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FUNDAMENTALS

Fundamentals of
Vacuum Technology

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Fundamentals of Vacuum Technology General

Fundamentals of
Vacuum Technology

revised and compiled by


Dr. Walter Umrath
with contributions from

Dr. Hermann Adam †, Alfred Bolz, Hermann Boy, Heinz Dohmen,


Karl Gogol, Dr. Wolfgang Jorisch, Walter Mönning,
Dr. Hans-Jürgen Mundinger, Hans-Dieter Otten, Willi Scheer,
Helmut Seiger, Dr. Wolfgang Schwarz, Klaus Stepputat, Dieter Urban,
Heinz-Josef Wirtzfeld, Heinz-Joachim Zenker

Preface
A great deal has transpired since the final reprint of the previous edition of Fundamen-
tals of Vacuum Technology appeared in 1987. LEYBOLD has in the meantime introduced
a number of new developments in the field. These include the dry-running ALL·ex
chemicals pump, the COOLVAC-FIRST cryopump systems with quick regeneration fea-
ture, turbomolecular pumps with magnetic bearings, the A-Series vacuum gauges, the
TRANSPECTOR and XPR mass spectrometer transmitters, leak detectors in the UL
series, and the ECOTEC 500 leak detector for refrigerants and many other gases. Moreo-
ver, the present edition of the “Fundamentals” goes into much greater detail on some
topics. Among these are residual gas analyses at low pressures, measurement of low
pressures, pressure monitoring, open- and closed-loop pressure control, and leaks and
their detection. Included for the first time are the sections covering the devices used to
measure and control the application of coatings and uses for vacuum technology in the
coating process. Naturally LEYBOLD’s “Vacuum Technology Training Center” at Cologne
was dependent on the invaluable support of numerous associates in collating the litera-
ture on hand and preparing new sections; I would like to expressly thank all those indi-
viduals at this juncture. A special word of appreciation is due the Communications
Department for its professional contribution in preparing this document for publishing.
Regrettably Dr. Hermann Adam, who at one time compiled the very first version of the
“Fundamentals”, did not live to see the publication of this edition. Though he had been
in retirement for many years, he nonetheless labored over the corrections and editing of
this current edition until shortly before his death.
I hope that this volume will enjoy a response as favorable as the previous version.

Dr. Walter Umrath


Cologne, August, 1998

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Contents Fundamentals of Vacuum Technology

1. Vacuum physics Quantities, 2.1.6.4 Pump fluid backstreaming 2.3.4 Evacuation of a chamber
their symbols, units of and its suppression where gases and vapors
measure and definitions . . .7 (Vapor barriers, baffles) . . .39 are evolved . . . . . . . . . . . . .66
1.1 Basic terms and concepts 2.1.6.5 Water jet pumps and 2.3.5 Selection of pumps for
in vacuum technology . . . . . .7 steam ejectors . . . . . . . . . .40 drying processes . . . . . . . .66
1.2 Atmospheric air . . . . . . . . .10 2.1.7 Turbomolecular pumps . . . .41 2.3.6 Flanges and their seals . . . .67
1.3 Gas laws and models . . . . .11 2.1.8 Sorption pumps . . . . . . . . .45 2.3.7 Choice of suitable valves . . .68
1.3.1 Continuum theory . . . . . . . .11 2.1.8.1 Adsorption pumps . . . . . . .45 2.3.8 Gas locks and seal-off
1.3.2 Kinetic gas theory . . . . . . . .11 2.1.8.2 Sublimation pumps . . . . . . .46 fittings . . . . . . . . . . . . . . . .69
1.4 The pressure ranges in 2.1.8.3 Sputter-ion pumps . . . . . . .46
vacuum technology and 2.1.8.4 Non evaporable getter 3. Vacuum measurement,
their characterization . . . . . 12 pumps (NEG pumps) . . . . .48 monitoring, control and
1.5 Types of flow and 2.1.9 Cryopumps . . . . . . . . . . . . .49 regulation . . . . . . . . . . . .70
conductance . . . . . . . . . . . .12 2.1.9.1 Types of cryopump . . . . . . .49 3.1 Fundamentals of low-
1.5.1 Types of flow . . . . . . . . . . .12 2.1.9.2 The cold head and its pressure measurement . . . .70
1.5.2 Calculating conductance operating principle . . . . . . .50 3.2 Vacuum gauges with
values . . . . . . . . . . . . . . . . .13 2.1.9.3 The refrigerator cryopump .51 pressure reading that is
1.5.3 Conductance for piping 2.1.9.4 Bonding of gases to cold independent of the type
and openings . . . . . . . . . . .14 surfaces . . . . . . . . . . . . . . .51 of gas . . . . . . . . . . . . . . . . .72
1.5.4 Conductance values for 2.1.9.5 Pumping speed and position 3.2.1 Bourdon vacuum gauges . . .72
other elements . . . . . . . . . .15 of the cryopanels . . . . . . . .52 3.2.2 Diaphragm vacuum
2.1.9.6 Characteristic quantities of a gauges . . . . . . . . . . . . . . . .72
2. Vacuum Generation . . . . .16 cryopump . . . . . . . . . . . . . .53 3.2.2.1 Capsule vacuum gauges . . .72
2.1 Vacuum pumps: A survey .16 2.2 Choice of pumping 3.2.2.2 DIAVAC diaphragm vacuum
2.1.1 Oscillation displacement process . . . . . . . . . . . . . . .56 gauge . . . . . . . . . . . . . . . . .72
vacuum pumps . . . . . . . . . .17 2.2.1 Survey of the most usual 3.2.2.3 Precision diaphragm
2.1.1.1 Diaphragm pumps . . . . . . .17 pumping processes . . . . . . .56 vacuum gauges . . . . . . . . . .72
2.1.2 Liquid sealed rotary 2.2.2 Pumping of gases 3.2.2.4 Capacitance diaphragm
displacement pumps . . . . . .17 (dry processes) . . . . . . . . .57 gauges . . . . . . . . . . . . . . . .73
2.1.2.1 Liquid ring pumps . . . . . . . .17 2.2.3 Pumping of gases and 3.2.3 Liquid-filled (mercury)
2.1.2.2 Oil sealed rotary vapors (wet processes) . . . .58 vacuum gauges . . . . . . . . . .74
displacement pumps . . . . . .18 2.2.4 Drying processes . . . . . . . .60 3.2.3.1 U-tube vacuum gauges . . . .74
2.1.2.2.1 Rotary vane pumps 2.2.5 Production of an oil-free 3.2.3.2 Compression vacuum
(TRIVAC A, TRIVAC B, (hydrocarbon-free) gauges (according to
TRIVAC E, SOGEVAC) . . . . .18 vacuum . . . . . . . . . . . . . . .60 McLeod) . . . . . . . . . . . . . . .74
2.1.2.2.2 Rotary plunger pumps 2.2.6 Ultrahigh vacuum working 3.3 Vacuum gauges with
(E-Pumps) . . . . . . . . . . . . .20 Techniques . . . . . . . . . . . . .61 gas-dependent pressure
2.1.2.2.3 Trochoid pumps . . . . . . . . .21 2.3 Evacuation of a vacuum reading . . . . . . . . . . . . . . . .75
2.1.2.2.4 The gas ballast . . . . . . . . . .21 chamber and determination 3.3.1 Spinning rotor gauge
2.1.3 Dry compressing rotary of pump sizes . . . . . . . . . . .62 (SRG) (VISCOVAC) . . . . . . .75
displacement pumps . . . . . .24 2.3.1 Evacuation of a vacuum 3.3.2 Thermal conductivity
2.1.3.1 Roots pumps . . . . . . . . . . .24 chamber (without additional vacuum gauges . . . . . . . . . .76
2.1.3.2 Claw pumps . . . . . . . . . . . .27 sources of gas or vapor) . . .62 3.3.3 Ionization vacuum gauges . .77
2.1.3.2.1 Claw pumps with internal 2.3.1.1 Evacuation of a chamber 3.3.3.1 Cold-cathode ionization
compression for the in the rough vacuum vacuum gauges (Penning
semiconductor industry region . . . . . . . . . . . . . . . . .62 vacuum gauges) . . . . . . . . .77
(“DRYVAC Series”) . . . . . . .28 2.3.1.2 Evacuation of a chamber 3.3.3.2 Hot-cathode ionization
2.1.3.2.2 Claw pump without internal in the high vacuum vacuum gauges . . . . . . . . . .78
compression for chemistry region . . . . . . . . . . . . . . . . .63 3.4 Adjustment and calibration;
applications (“ALL·ex”) . . . .31 2.3.1.3 Evacuation of a chamber in DKD, PTB national
2.1.4 Accessories for oil-sealed the medium vacuum standards . . . . . . . . . . . . . .81
rotary displacement region . . . . . . . . . . . . . . . . .63 3.4.1 Examples of fundamental
pumps . . . . . . . . . . . . . . . .33 2.3.2 Determination of a suitable pressure measurement
2.1.5 Condensers . . . . . . . . . . . .33 backing pump . . . . . . . . . . .64 methods (as standard
2.1.6 Fluid-entrainment pumps . .35 2.3.3 Determination of methods for calibrating
2.1.6.1
2.1.6.2
(Oil) Diffusion pumps . . . . .36
Oil vapor ejector pumps . . .38
pump-down time from
nomograms . . . . . . . . . . . .65 3.5
vacuum gauges . . . . . . . . . .81
Pressure monitoring, control D00
2.1.6.3 Pump fluids . . . . . . . . . . . .39 and regulation in vacuum
systems . . . . . . . . . . . . . . .83

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Fundamentals of Vacuum Technology Contents

3.5.1 Fundamentals of pressure 4.6.4 Quantitative gas analysis . .101 5.5.2.4 Leak detectors with
monitoring and control . . . .83 4.7 Software . . . . . . . . . . . . . .102 quadrupole mass
3.5.2 Automatic protection, 4.7.1 Standard SQX software spectrometer
monitoring and control (DOS) for stand-alone (ECOTEC II) . . . . . . . . . . .113
of vacuum systems . . . . . . .83 operation(1 MS plus, 5.5.2.5 Helium leak detectors
3.5.3 Pressure regulation and 1 PC, RS 232) . . . . . . . . . .102 with 180° sector mass
control in rough and 4.7.2 Multiplex/DOS software spectrometer
medium vacuum MQX (1 to 8 MS plus (UL 200, UL 500) . . . . . . .114
systems . . . . . . . . . . . . . . .84 1 PC, RS 485) . . . . . . . . . .102 5.5.2.6 Direct-flow and
3.5.4 Pressure regulation in 4.7.3 Process-oriented software – counter-flow leak
high and ultrahigh Transpector-Ware for detectors . . . . . . . . . . . . .115
vacuum systems . . . . . . . . .87 Windows . . . . . . . . . . . . .102 5.5.2.7 Partial flow operation . . . .115
3.5.5 Examples of applications 4.7.4 Development software 5.5.2.8 Connection to vacuum
with diaphragm TranspectorView . . . . . . . .102 systems . . . . . . . . . . . . . .116
controllers . . . . . . . . . . . . .88 4.8 Partial pressure 5.5.2.9 Time constants . . . . . . . .116
regulation . . . . . . . . . . . . .102 5.6 Limit values / Specifications
4. Analysis of gas at low 4.9 Maintenance . . . . . . . . . . .103 for the leak detector . . . . .117
pressures using mass 5.7 Leak detection techniques
spectrometry . . . . . . . . . .89 5. Leaks and their using helium leak
4.1 General . . . . . . . . . . . . . . . .89 detection . . . . . . . . . . .104 detectors . . . . . . . . . . . . .117
4.2 A historical review . . . . . . . .89 5.1 Types of leaks . . . . . . . . . .104 5.7.1 Spray technique
4.3 The quadrupole mass 5.2 Leak rate, leak size, (local leak test) . . . . . . . . .117
spectrometer mass flow . . . . . . . . . . . . .104 5.7.2 Sniffer technology
(TRANSPECTOR) . . . . . . . .89 5.2.1 The standard helium (local leak testing using
4.3.1 Design of the sensor . . . . . .90 leak rate . . . . . . . . . . . . . .106 the positive pressure
4.3.1.1 The normal (open) 5.2.2 Conversion equations . . . .106 method) . . . . . . . . . . . . . .118
ion source . . . . . . . . . . . . .90 5.3 Terms and definitions . . . .106 5.7.3 Vacuum envelope test
4.3.1.2 The quadrupole 5.4 Leak detection methods (integral leak test) . . . . . . .118
separation system . . . . . . . .91 without a leak detector 5.7.3.1 Envelope test – test
4.3.1.3 The measurement unit . . . . . . . . . . . . . . . . . .107 specimen pressurized
system (detector) . . . . . . . .92 5.4.1 Pressure rise test . . . . . . .107 with helium . . . . . . . . . . . .118
4.4 Gas admission and 5.4.2 Pressure drop test . . . . . .108 a) Envelope test with
pressure adaptation . . . . . .93 5.4.3 Leak test using vacuum concentration measur
4.4.1 Metering valve . . . . . . . . . .93 gauges which are sensitive ement and subsequent
4.4.2 Pressure converter . . . . . . .93 to the type of gas . . . . . . .108 leak rate calculation . . .118
4.4.3 Closed ion source (CIS) . . .93 5.4.4 Bubble immersion test . . .109 b) Direct measurement of
4.4.4 Aggressive gas monitor 5.4.5 Foam-spray test . . . . . . . .109 the leak rate with the
(AGM) . . . . . . . . . . . . . . . .94 5.4.6 Vacuum box check bubble .109 leak detector
4.5 Descriptive values in 5.4.7 Krypton 85 test . . . . . . . . .109 (rigid envelope) . . . . . .118
mass spectrometry 5.4.8 High-frequency vacuum 5.7.3.2 Envelope test with test
(specifications) . . . . . . . . . .94 test . . . . . . . . . . . . . . . . . .109 specimen evacuated . . . . .118
4.5.1 Line width (resolution) . . . .94 5.4.9 Testing with chemical a) Envelope =
4.5.2 Mass range . . . . . . . . . . . . .95 reactions and dye “plastic tent” . . . . . . . .118
4.5.3 Sensitivity . . . . . . . . . . . . . .95 penetration . . . . . . . . . . . .110 b) Rigid envelope . . . . . . .119
4.5.4 Smallest detectable 5.5 Leak detectors and how 5.7.4 “Bombing” test,
partial pressure . . . . . . . . . .95 they work . . . . . . . . . . . . .110 “Storage under pressure” .119
4.5.5 Smallest detectable 5.5.1 Halogen leak detectors 5.8 Industrial leak testing . . . .119
partial pressure ratio (HLD 4000, D-Tek) . . . . . .110
(concentration) . . . . . . . . . .95 5.5.2 Leak detectors with 6. Thin film controllers and
4.5.6 Linearity range . . . . . . . . . .95 mass spectrometers (MS) .110 control units with quartz
4.5.7 Information on surfaces 5.5.2.1 The operating principle oscillators . . . . . . . . . . .120
and amenability to for a MSLD . . . . . . . . . . . .111 6.1 Introduction . . . . . . . . . . .120
bake-out . . . . . . . . . . . . . . .95 5.5.2.2 Detection limit, background, 6.2 Basic principles of coating
4.6 Evaluating spectra . . . . . . . .96 gas storage in oil (gas ballast), thickness measurement
4.6.1 Ionization and fundamental floating zero-point with quartz oscillators . . . .120
problems in gas analysis . . .96 suppression . . . . . . . . . . .111 6.3 The shape of quartz
4.6.2 Partial pressure 5.5.2.3 Calibrating leak detectors; oscillator crystals . . . . . . .121
measurement . . . . . . . . . .100 test leaks . . . . . . . . . . . . .112 6.4 Period measurement . . . . .122
4.6.3 Qualitative gas analysis . . .100 6.5 The Z match technique . . .122

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Contents Fundamentals of Vacuum Technology

6.6 The active oscillator . . . . .122 8.3.1.4 Operating defects while Tab VI Conversion of pumping
6.7 The mode-lock oscillator . .123 pumping with gas ballast – speed (volume flow rate)
6.8 Auto Z match technique . .124 potential sources of error units . . . . . . . . . . . . . . . . .144
6.9 Coating thickness where the required ultimate Tab VII Conversion of throughput
regulation . . . . . . . . . . . . .125 pressure is not achieved . .137 (a,b) QpV units; leak rate
6.10 INFICON instrument 8.3.2 Roots pumps . . . . . . . . . .137 units . . . . . . . . . . . . . . . . .144
variants . . . . . . . . . . . . . .127 8.3.2.1 General operating Tab VIII Composition of
instructions, installation atmospheric air . . . . . . . . .145
7. Application of vacuum and commissioning . . . . . .137 Tab IX Pressure ranges used in
technology for coating 8.3.2.2 Oil change, maintenance vacuum technology and their
techniques . . . . . . . . . .128 work . . . . . . . . . . . . . . . . .137 characteristics . . . . . . . . . .145
7.1 Vacuum coating 8.3.2.3 Actions in case of Tab X Outgassing rate of
technique . . . . . . . . . . . . .128 operational disturbances . .138 materials . . . . . . . . . . . . . .145
7.2 Coating sources . . . . . . . .128 8.3.3 Turbomolecular pumps . . .138 Tab XI Nominal internal diameters
7.2.1 Thermal evaporators 8.3.3.1 General operating (DN) and internal diameters
(boats, wires etc.) . . . . . . .128 instructions . . . . . . . . . . . .138 of tubes, pipes and apertures
7.2.2 Electron beam 8.3.3.2 Maintenance . . . . . . . . . . .138 with circular cross-section
evaporators 8.3.4 Diffusion and vapor-jet (according to PNEUROP). .146
(electron guns) . . . . . . . . .129 vacuum pumps . . . . . . . . .139 Tab XII Important data for
7.2.3 Cathode sputtering . . . . . .129 8.3.4.1 Changing the pump fluid common solvents . . . . . . .146
7.2.4 Chemical vapor and cleaning the pump . . .139 Tab XIII Saturation pressure and
deposition . . . . . . . . . . . . .129 8.3.4.2 Operating errors with density of water . . . . . . . .147
7.3 Vacuum coating diffusion and vapor-jet Tab XIV Hazard classificationof
technology/coating pumps . . . . . . . . . . . . . . .139 fluids . . . . . . . . . . . . . . . .148
systems . . . . . . . . . . . . . .130 8.3.5 Adsorption pumps . . . . . .139 Tab XV Chemical resistance of
7.3.1 Coating of parts . . . . . . . .130 8.3.5.1 Reduction of adsorption commonly used elastomer
7.3.2 Web coating . . . . . . . . . . .130 capacity . . . . . . . . . . . . . .139 gaskets and sealing
7.3.3 Optical coatings . . . . . . . .131 8.3.5.2 Changing the molecular materials . . . . . . . . . . . . .149
7.3.4 Glass coating . . . . . . . . . .132 sieve . . . . . . . . . . . . . . . . .139 Tab XVI Symbols used invacuum
7.3.5 Systems for producing 8.3.6 Titanium sublimation technology . . . . . . . . . . . .152
data storage disks . . . . . . .132 pumps . . . . . . . . . . . . . . .140 Tab XVII Temperature comparison
8.3.7 Sputter-ion pumps . . . . . .140 and conversion table . . . . .154
8. Instructions for vacuum 8.4 Information on working Fig. 9.1 Variation of mean free path
equipment operation . . . .134 with vacuum gauges . . . . .140 l (cm) with pressure for
8.1 Causes of faults where the 8.4.1 Information on installing various gases . . . . . . . . . .154
desired ultimate pressure vacuum sensors . . . . . . . .140 Fig. 9.2 Diagram of kinetics of
is not achieved or is 8.4.2 Contamination at the gases for air at 20 °C . . . .154
achieved too slowly . . . . .134 measurement system and Fig. 9.3 Decrease in air pressure
8.2 Contamination of vacuum its removal . . . . . . . . . . . .141 and change in
vessels and eliminating 8.4.3 The influence of magnetic temperature as a
contamination . . . . . . . . . .134 and electrical fields . . . . . .141 function of altitude . . . . . .155
8.3 General operating infor- 8.4.4 Connectors, power pack, Fig. 9.4 Change in gas composition
mation for vacuum measurement systems . . .141 of the atmosphere as a
pumps . . . . . . . . . . . . . . .134 function of altitude . . . . . .155
8.3.1 Oil-sealed rotary vacuum 9. Tables, formulas, Fig. 9.5 Conductance values for
pumps (Rotary vane nomograms, diagrams piping of commonly used
pumps and rotary piston and symbols . . . . . . . . .142 nominal internal diameters
pumps) . . . . . . . . . . . . . . .135 Tab I Permissible pressure units with circular cross-section
8.3.1.1 Oil consumption, oil including the torr and its for molecular flow . . . . . . .155
contamination, oil conversion . . . . . . . . . . . .142 Fig. 9.6 Conductance values for
change . . . . . . . . . . . . . . .135 Tab II Conversion of pressure piping of commonly used
8.3.1.2 Selection of the pump oil units . . . . . . . . . . . . . . . . .142 nominal internal diameters
when handling Tab III Mean free path . . . . . . . . .142 with circular cross-section
aggressive vapors . . . . . . .135 Tab IV Compilation of important for molecular flow . . . . . . .155
8.3.1.3 Measures when pumping formulas pertaining to the Fig. 9.7 Nomogram for
various chemical
substances . . . . . . . . . . . .136 Tab V
kinetic theory of gases . . .143
Important values . . . . . . . .143
determination of
pump-down time tp of a D00
vessel in the rough
vacuum pressure range . . .156

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Fundamentals of Vacuum Technology Contents

Fig. 9.8 Nomogram for 10.3 Remarks on alphabetical


determination of the list in Section 10.2 . . . . . .168
conductance of tubes with 10.4 Tables . . . . . . . . . . . . . . . .170
a circular cross-section 10.4.1 Basic SI units . . . . . . . . . .170
for air at 20 °C in the 10.4.2 Derived coherent SI units
region of molecular flow . .157 with special names
Fig. 9.9 Nomogram for and symbols . . . . . . . . . . .170
determination of 10.4.3 Atomic units . . . . . . . . . .170
conductance of tubes in 10.4.4 Derived noncoherent SI
the entire pressure range .158 units with special names
Fig. 9.10 Determination of and symbols . . . . . . . . . . .170
pump-down time in the
medium vacuum range 11. National and international
taking into account the standards and
evolution of gas from recommendations
the walls . . . . . . . . . . . . . .159 particularly relevant to
Fig.9.11 Saturation vapor vacuum technology . . . . .171
pressure of various 11.1 National and international
substances . . . . . . . . . . . .160 standards and
Fig. 9.12 Saturation vapor pressure recommendations of
of pump fluids for oil and special relevance to
mercury fluid entrainment vacuum technology . . . . . .171
pumps . . . . . . . . . . . . . . .160
Fig. 9.13 Saturation vapor pressure 12. References . . . . . . . . . .174
of major metals used in
vacuum technology . . . . . .160 13. Index . . . . . . . . . . . . . .184
Fig. 9.14 Vapor pressure of
nonmetallic sealing
materials (the vapor
pressure curve for fluoro
rubber lies between the
curves for silicone
rubber and Teflon). . . . . . .161
Fig. 9.15 Saturation vapor pressure
ps of various substances
relevant for cryogenic
technology in a
temperaturerange of
T = 2 – 80 K. . . . . . . . . . . .161
Fig. 9.16 Common working ranges
of vacuum pumps . . . . . . .161
Fig. 9.16a Measurement ranges of
common vacuum
gauges . . . . . . . . . . . . . . .162
Fig. 9.17 Specific volume of
saturated water vapor . . . .163
Fig. 9.18 Breakdown voltage
between electrodes for air
(Paschen curve) . . . . . . . .163
Fig 9.19 Phase diagram of water . . .164

10. The statutory units used in


vacuum technology . . . . .165
10.1 Introduction . . . . . . . . . . .165
10.2 Alphabetical list of variables,
symbols and units frequently
used in vacuum technology
and its applications . . . . . .165

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Vacuum Physics Fundamentals of Vacuum Technology

1. Quantities, all the non-condensable components


present in the mix – in case of the “parti-
temperature is gas in equilibrium with the
liquid phase of the same substance. A
their symbols, al ultimate pressure” at a rotary vane
pump, for example.
strict differentiation between gases and
vapors will be made in the comments
units of Saturation vapor pressure ps
which follow only where necessary for
complete understanding.
measure and The pressure of the saturated vapor is
referred to as saturation vapor pressure Particle number density n (cm-3)
definitions ps. ps will be a function of temperature for
any given substance.
According to the kinetic gas theory the
number n of the gas molecules, referenced
to the volume, is dependent on pressure p
Vapor pressure pd and thermodynamic temperature T as
(cf. DIN 28 400, Part 1, 1990, Partial pressure of those vapors which can
DIN 1314 and DIN 28 402) expressed in the following:
be liquefied at the temperature of liquid
nitrogen (LN2). p=n·k·T (1.1)
n = particle number density
1.1 Basic terms and Standard pressure pn k = Boltzmann’s constant
Standard pressure pn is defined in DIN
concepts in 1343 as a pressure of pn = 1013.25 mbar. At a certain temperature, therefore, the
pressure exerted by a gas depends only on
vacuum technology the particle number density and not on the
Ultimate pressure pend
Pressure p (mbar) The lowest pressure which can be achie- nature of the gas. The nature of a gaseous
of fluids (gases and liquids). (Quantity: ved in a vacuum vessel. The socalled ulti- particle is characterized, among other
pressure; symbol: p; unit of measure: mate pressure pend depends not only on factors, by its mass mT.
millibar; abbreviation: mbar.) Pressure is the pump’s suction speed but also upon
defined in DIN Standard 1314 as the the vapor pressure pd for the lubricants, Gas density ρ (kg · m-3, g · cm-3)
quotient of standardized force applied to a sealants and propellants used in the pump. The product of the particle number densi-
surface and the extent of this surface If a container is evacuated simply with an ty n and the particle mass mT is the gas
(force referenced to the surface area). oil-sealed rotary (positive displacement) density ρ:
Even though the Torr is no longer used as vacuum pump, then the ultimate pressure ρ = n · mT (1.2)
a unit for measuring pressure (see Section which can be attained will be determined
10), it is nonetheless useful in the interest primarily by the vapor pressure of the
of “transparency” to mention this pressure pump oil being used and, depending on The ideal gas law
unit: 1 Torr is that gas pressure which is the cleanliness of the vessel, also on the The relationship between the mass mT of a
able to raise a column of mercury by 1 mm vapors released from the vessel walls and, gas molecule and the molar mass M of this
at 0 °C. (Standard atmospheric pressure is of course, on the leak tightness of the gas is as follows:
760 Torr or 760 mm Hg.) Pressure p can vacuum vessel itself. M = NA · mT (1.3)
be more closely defined by way of sub-
scripts: Ambient pressure pamb Avogadro’s number (or constant) NA
or (absolute) atmospheric pressure indicates how many gas particles will be
Absolute pressure pabs contained in a mole of gas. In addition to
Absolute pressure is always specified in Overpressure pe or gauge pressure this, it is the proportionality factor between
vacuum technology so that the “abs” index (Index symbol from “excess”) the gas constant R and Boltzmann’s
can normally be omitted. constant k:
pe = pabs – pamb
R = NA · k (1.4)
Total pressure pt Here positive values for pe will indicate
The total pressure in a vessel is the sum of overpressure or gauge pressure; negative Derivable directly from the above
the partial pressures for all the gases and values will characterize a vacuum. equations (1.1) to (1.4) is the correlation
vapors within the vessel. between the pressure ρ and the gas
Working pressure pW density ρ of an ideal gas.
Partial pressure pi During evacuation the gases and/or vapors
The partial pressure of a certain gas or are removed from a vessel. Gases are R·T
p = ρ ⋅ ––––– (1.5)
vapor is the pressure which that gas or understood to be matter in a gaseous state M
vapor would exert if it alone were present which will not, however, condense at
in the vessel. working or operating temperature. Vapor In practice we will often consider a certain
is also matter in a gaseous state but it may enclosed volume V in which the gas is
Important note: Particularly in rough
vacuum technology, partial pressure in a
be liquefied at prevailing temperatures by
increasing pressure. Finally, saturated
present at a certain pressure p. If m is the
mass of the gas present within that
D00
mix of gas and vapor is often understood vapor is matter which at the prevailing volume, then
to be the sum of the partial pressures for

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m ture this is always equivalent to reducing Quantity of gas (pV value), (mbar ⋅ l)
ρ = ––– (1.6) the gas pressure p. Explicit attention must The quantity of a gas can be indicated by
V
at this point be drawn to the fact that a way of its mass or its weight in the units of
The ideal gas law then follows directly reduction in pressure (maintaining the measure normally used for mass or
from equation (1.5): volume) can be achieved not only by weight. In practice, however, the product
reducing the particle number density n but of p · V is often more interesting in vacu-
m
p ⋅ V = ––– ⋅ R ⋅ T = ν ⋅ R ⋅ T (1.7) also (in accordance with Equation 1.5) by um technology than the mass or weight of
M reducing temperature T at constant gas a quantity of gas. The value embraces an
density. This important phenomenon will energy dimension and is specified in
Here the quotient m / M is the number of
always have to be taken into account millibar·liters (mbar·l) (Equation 1.7).
moles u present in volume V.
where the temperature is not uniform Where the nature of the gas and its
The simpler form applies for m / M = 1, i.e. throughout volume V. temperature are known, it is possible to
for 1 mole: use Equation 1.7b to calculate the mass m
The following important terms and
for the quantity of gas on the basis of the
p·V=R·T (1.7a) concepts are often used in vacuum
product of p · V:
technology:
The following numerical example is
intended to illustrate the correlation p ·V = m · R · T (1.7)
Volume V (l, m3, cm3) M
between the mass of the gas and pressure
The term volume is used to designate
for gases with differing molar masses,
a) the purely geometric, usually predeter- p· V ·M
drawing here on the numerical values in
mined, volumetric content of a vacuum m= (1.7b)
Table IV (Chapter 9). Contained in a R ·T
chamber or a complete vacuum system
10-liter volume, at 20 °C, will be
including all the piping and connecting
a) 1g of helium Although it is not absolutely correct,
spaces (this volume can be calculated);
b) 1g of nitrogen reference is often made in practice to the
b) the pressure-dependent volume of a
When using the equation (1.7) there “quantity of gas” p · V for a certain gas.
gas or vapor which, for example, is
results then at V = 10 l , m = 1 g, This specification is incomplete; the
moved by a pump or absorbed by an
R = 83.14 mbar·l·mol-1·K-1, temperature of the gas T, usually room
adsorption agent.
T = 293 K (20 °C) temperature (293 K), is normally implicitly
Volumetric flow (flow volume) qv assumed to be known.
In case a) where M = 4 g · mole-1
(monatomic gas): (l/s, m3/h, cm3/s) Example:
The term “flow volume” designates the The mass of 100 mbar · l of nitrogen (N2)
1·g · 83.14 · mbar · ` · mol – 1· K– 1 · 293 · K volume of the gas which flows through a at room temperature (approx. 300 K) is:
p= =
10 · `· K · 4 · g · mol –1 piping element within a unit of time, at the

= 609 mbar pressure and temperature prevailing at the 100 mbar · ` · 28 g · mol 1
particular moment. Here one must realize m= − − =
83 mbar · ` · mol 1 · K 1 · 300 K
In case b), with M = 28 ≠ g mole-1 (diato- that, although volumetric flow may be
mic gas): identical, the number of molecules moved 2800
= g = 0.113 g
may differ, depending on the pressure and 300 · 83
1·g · 83.14 · mbar · ` · mol – 1· K– 1 · 293 · K
p= = temperature.
10 · `· K · 28 · g · mol –1 Analogous to this, at T = 300 K:
= 87 mbar Pumping speed S (l/s, m3/h, cm3/s)
The pumping speed is the volumetric flow 1 mbar · l O2 = 1.28 · 10-3 g O2
The result, though appearing to be
through the pump’s intake port.
paradoxical, is that a certain mass of a
dV 70 mbar · l Ar = 1.31 · 10-1 g Ar
light gas exerts a greater pressure than the S = –––– (1.8a)
same mass of a heavier gas. If one takes dt The quantity of gas flowing through a
into account, however, that at the same piping element during a unit of time – in
If S remains constant during the pumping accordance with the two concepts for gas
gas density (see Equation 1.2) more
process, then one can use the difference quantity described above – can be indica-
particles of a lighter gas (large n, small m)
quotient instead of the differential quoti- ted in either of two ways, these being:
will be present than for the heavier gas
ent:
(small n, large m), the results become
more understandable since only the ∆V Mass flow qm (kg/h, g/s),
particle number density n is determinant S = ––– (1.8b) this is the quantity of a gas which flows
∆t
for the pressure level, assuming equal through a piping element, referenced to
temperature (see Equation 1.1). (A conversion table for the various units of time
measure used in conjunction with m
The main task of vacuum technology is to qm = ––– or as
pumping speed is provided in Section 9,
reduce the particle number density n insi- t
Table VI).
de a given volume V. At constant tempera-

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Vacuum Physics Fundamentals of Vacuum Technology

pV flow qpV (mbar·l·s-1). Conductance C (l · s-1) Leak rate qL (mbar·l·s-1)


pV flow is the product of the pressure and The pV flow through any desired piping According to the definition formulated
volume of a quantity of gas flowing element, i.e. pipe or hose, valves, nozzles, above it is easy to understand that the size
through a piping element, divided by time, openings in a wall between two vessels, of a gas leak, i.e. movement through unde-
i.e.: etc., is indicated with sired passages or “pipe” elements, will
also be given in mbar·l·s-1. A leak rate is
p·V d (p · V) qpV = C(p1 – p2) = ∆p · C (1.11)
qpV = –––––– = –––––––– often measured or indicated with atmos-
t dt Here ∆p = (p1 – p2) is the differential bet- pheric pressure prevailing on the one side
ween the pressures at the inlet and outlet of the barrier and a vacuum at the other
pV flow is a measure of the mass flow of ends of the piping element. The proportio- side (p < 1 mbar). If helium (which may be
the gas; the temperature to be indicated nality factor C is designated as the con- used as a tracer gas, for example) is pas-
here. ductance value or simply “conductance”. It sed through the leak under exactly these
is affected by the geometry of the piping conditions, then one refers to “standard
Pump throughput qpV element and can even be calculated for helium conditions”.
The pumping capacity (throughput) for a some simpler configurations (see Section
pump is equal either to the mass flow Outgassing (mbar·l)
1.5).
through the pump intake port: The term outgassing refers to the liberati-
In the high and ultrahigh vacuum ranges, on of gases and vapors from the walls of a
m C is a constant which is independent of vacuum chamber or other components on
qm = –––– (1.9)
pressure; in the rough and medium-high the inside of a vacuum system. This quan-
t
regimes it is, by contrast, dependent on tity of gas is also characterized by the pro-
or to the pV flow through the pump’s inta- pressure. As a consequence, the calculati- duct of p · V, where V is the volume of the
ke port: on of C for the piping elements must be vessel into which the gases are liberated,
carried out separately for the individual and by p, or better ∆p, the increase in
p·V
qpV = –––––– pressure ranges (see Section 1.5 for more pressure resulting from the introduction of
t detailed information). gases into this volume.

It is normally specified in mbar·l·s-1. Here From the definition of the volumetric flow
Outgassing rate (mbar·l·s-1)
p is the pressure on the intake side of the it is also possible to state that: The
This is the outgassing through a period of
conductance value C is the flow volume
pump. If p and V are constant at the intake time, expressed in mbar·l·s-1.
side of the pump, the throughput of this through a piping element. The equation
(1.11) could be thought of as “Ohm’s law
pump can be expressed with the simple Outgassing rate (mbar·l·s-1 · cm-2)
equation for vacuum technology”, in which qpV
(referenced to surface area)
corresponds to current, ∆p the voltage and
In order to estimate the amount of gas
qpV = p · S (1.10a) C the electrical conductance value. Analo-
which will have to be extracted, knowledge
gous to Ohm’s law in the science of elec-
where S is the pumping speed of the pump of the size of the interior surface area, its
tricity, the resistance to flow
at intake pressure of p. material and the surface characteristics,
1 their outgassing rate referenced to the sur-
(The throughput of a pump is often indica- R = –––
C face area and their progress through time
ted with Q, as well.) are important.
The concept of pump throughput is of has been introduced as the reciprocal
major significance in practice and should value to the conductance value. The Mean free path of the molecules λ (cm)
not be confused with the pumping speed! equation (1.11) can then be re-written as: and collision rate z (s-1)
The pump throughput is the quantity of 1 The concept that a gas comprises a large
gas moved by the pump over a unit of qpV = —— ⋅ ∆p (1.12) number of distinct particles between which
time, expressed in mbar ≠ l/s; the pum- R – aside from the collisions – there are no
ping speed is the “transportation capacity” The following applies directly for connec- effective forces, has led to a number of
which the pump makes available within a tion in series: theoretical considerations which we sum-
specific unit of time, measured in m3/h marize today under the designation “kine-
or l/s. R∑ = R1 + R2 + R3 . . . (1.13) tic theory of gases”.
The throughput value is important in deter- When connected in parallel, the following One of the first and at the same time most
mining the size of the backing pump in applies: beneficial results of this theory was the
relationship to the size of a high vacuum calculation of gas pressure p as a function
pump with which it is connected in series 1 1 1 1 of gas density and the mean square of
––– = –– + –– + –– + ⋅ ⋅ ⋅ ⋅ (1.13a)
in order to ensure that the backing pump R∑ R1 R2 R3 velocity c2 for the individual gas molecules
will be able to “take off” the gas moved by
the high vacuum pump (see Section 2.32).
in the mass of molecules mT: D00

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1 --- 1 --- Impingement rate zA (cm-2 ⋅ s-1) and 1.2 Atmospheric air
p = –– ρ ⋅ c2 = –– ⋅ n ⋅ mT ⋅ c2 (1.14)
3 3 monolayer formation time τ (s)
A technique frequently used to characteri- Prior to evacuation, every vacuum system
where ze the pressure state in the high vacuum on earth contains air and it will always be
regime is the calculation of the time requi- surrounded by air during operation. This
k·T red to form a monomolecular or monoato- makes it necessary to be familiar with the
c2 = 3 ⋅ ——– (1.15) mic layer on a gas-free surface, on the physical and chemical properties of
mT
assumption that every molecule will stick atmospheric air.
The gas molecules fly about and among to the surface. This monolayer formation
The atmosphere is made up of a number of
each other, at every possible velocity, and time is closely related with the so-called
gases and, near the earth’s surface, water
bombard both the vessel walls and collide impingement rate zA. With a gas at rest the
vapor as well. The pressure exerted by
(elastically) with each other. This motion of impingement rate will indicate the number
atmospheric air is referenced to sea level.
the gas molecules is described numerical- of molecules which collide with the surfa-
Average atmospheric pressure is
ly with the assistance of the kinetic theory ce inside the vacuum vessel per unit of
1013 mbar (equivalent to the “atmos-
of gases. A molecule’s average number of time and surface area:
phere”, a unit of measure used earlier).
collisions over a given period of time, the Table VIII in Chapter 9 shows the compo-
so-called collision index z, and the mean n· c
zA = (1.20) sition of the standard atmosphere at relati-
path distance which each gas molecule 4
ve humidity of 50 % and temperature of
covers between two collisions with other If a is the number of spaces, per unit of 20 °C. In terms of vacuum technology the
molecules, the so-called mean free path surface area, which can accept a specific following points should be noted in regard
length λ, are described as shown below as gas, then the monolayer formation time is to the composition of the air:
a function of the mean molecule velocity -c a) The water vapor contained in the air,
a 4 ·a
the molecule diameter 2r and the particle τ= = (1.21) varying according to the humidity level,
number density molecules n – as a very zA n · c
plays an important part when evacua-
good approximation: ting a vacuum plant (see Section 2.2.3).
C Collision frequency zv (cm-3 · s-1) b) The considerable amount of the inert
Z= (1.16) This is the product of the collision rate z gas argon should be taken into account
λ in evacuation procedures using sorpti-
and the half of the particle number density
where n, since the collision of two molecules is to on pumps (see Section 2.1.8).
be counted as only one collision: c) In spite of the very low content of heli-
8· k ·T 8· R ·T um in the atmosphere, only about 5
c= =
π · mT π ·M
(1.17) zV = n ·z (1.21a) ppm (parts per million), this inert gas
2 makes itself particularly obvious in
ultrahigh vacuum systems which are
and sealed with Viton or which incorporate
1 glass or quartz components. Helium is
λ= (1.18) able to permeate these substances to a
π · 2 · n · (2r)2
measurable extent.
Thus the mean free path length λ for the The pressure of atmospheric air falls with
particle number density n is, in accordan- rising altitude above the earth’s surface
ce with equation (1.1), inversely proportio- (see Fig. 9.3 in Chapter 9). High vacuum
nal to pressure p. Thus the following rela- prevails at an altitude of about 100 km and
tionship holds, at constant temperature T, ultrahigh vacuum above 400 km. The com-
for every gas position of the air also changes with the
distance to the surface of the earth (see
λ ⋅ p = const (1.19) Fig. 9.4 in Chapter 9).
Used to calculate the mean free path
length λ for any arbitrary pressures and
various gases are Table III and Fig. 9.1 in
Chapter 9. The equations in gas kinetics
which are most important for vacuum
technology are also summarized (Table IV)
in chapter 9.

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1.3 Gas laws and Ideal gas Law change of direction through 180 °, will be
equal to 2 · mT · c. The sum of the pulse
m
models p ·V =
M
· R · T = ν · R ·T changes for all the molecules impinging on
the wall will result in a force effective on
1.3.1 Continuum theory this wall or the pressure acting on the wall,
Also: Equation of state for ideal gases per unit of surface area.
Model concept: Gas is “pourable” (fluid) (from the continuum theory)
n 1
and flows in a way similar to a liquid. The · c · 2 · m T · c = · n · c2 · m T = p
continuum theory and the summarization van der Waals’ Equation 6 3
of the gas laws which follows are based on a
experience and can explain all the proces- (p + ) · ( Vm − b) = R · T where
Vm2
ses in gases near atmospheric pressure.
N
Only after it became possible using ever n=
a, b = constants V
better vacuum pumps to dilute the air to
the extent that the mean free path rose far (internal pressure, covolumes)
beyond the dimensions of the vessel were Vm = Molar volume Derived from this is
more far-reaching assumptions necessary; Also: Equation of state for real gases
1
these culminated in the kinetic gas theory. p ·V = · N · mT · c2
Clausius-Clapeyron Equation 3
The kinetic gas theory applies throughout
the entire pressure range; the continuum dp
theory represents the (historically older) L =T· · ( V − Vm, l ) Ideal gas law (derived from the kinetic
dT m, v
special case in the gas laws where atmos- gas theory)

pheric conditions prevail. L = Enthalpy of evaporation, If one replaces c2 with c2 then a compari-
T = Evaporation temperature, son of these two “general” gas equations
Summary of the most important gas laws Vm,v, Vm,l = Molar volumes of vapor will show:
(continuum theory)
or liquid
m 1
p ·V = · R · T = · N · m T · c2 or
Boyle-Mariotte Law M 3
p ⋅ V = const. 1.3.2 Kinetic gas theory
for T = constant (isotherm) mT · R 2 m · c2
With the acceptance of the atomic view of p·V = N · ( ) ·T = ·N·( T )
the world – accompanied by the necessity M 3 2
Gay-Lussac’s Law (Charles’ Law) to explain reactions in extremely dilute
V = V0 (1 + β · t ) gases (where the continuum theory fails) – The expression in brackets on the left-
the “kinetic gas theory” was developed. hand side is the Boltzmann constant k; that
Using this it is possible not only to derive on the right-hand side a measure of the
for p = constant (isobar)
the ideal gas law in another manner but molecules’ mean kinetic energy:
also to calculate many other quantities
Amonton’s Law Boltzmann constant
involved with the kinetics of gases – such
p = p0 (1 + γ · t ) as collision rates, mean free path lengths, mT · R J
monolayer formation time, diffusion con- k= = 1.38 · 10 −23
M K
for V = constant (isochor) stants and many other quantities.
Model concepts and basic assumptions: Mean kinetic energy of the molecules
Dalton’s Law 1. Atoms/molecules are points.
2. Forces are transmitted from one to mT · c 2
∑ pi = p total E kin =
i another only by collision. 2
3. The collisions are elastic.
thus
4. Molecular disorder (randomness)
Poisson’s Law prevails. 2
p · V = N· k · T = · N · E kin
3
p ⋅ Vk = const A very much simplified model was develo-
(adiabatic) ped by Krönig. Located in a cube are N In this form the gas equation provides a
particles, one-sixth of which are moving gas-kinetic indication of the temperature!
Avogadro’s Law toward any given surface of the cube. If
m1 m 2 the edge of the cube is 1 cm long, then it The mass of the molecules is
: = M1 : M 2
V1 V2 will contain n particles (particle number
density); within a unit of time n · c · ∆t/6 mT = M = Mass / mol
NA Molecules / mol
D00
molecules will reach each wall where the
change of pulse per molecule, due to the

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Fundamentals of Vacuum Technology Vacuum Physics

where NA is Avogadro’s number 1.5 Types of flow and


(previously: Loschmidt number).  p  
Avogadro constant conductance ∆pcrit = p1 1−  2 
  p1 crit  (1.22)
NA = 6.022 ⋅ 1023 mol–1 Three types of flow are mainly encounte-
red in vacuum technology: viscous or con- A further rise in ∆p > ∆pcrit would not
For 1 mole, zV = n · and tinuous flow, molecular flow and – at the result in any further rise in gas flow; any
2
transition between these two – the so-cal- increase is inhibited. For air at 20,°C the
V = Vm = 22.414 l (molar volume); led Knudsen flow. gas dynamics theory reveals a critical
value of
Thus from the ideal gas law at standard
conditions 1.5.1 Types of flow  p2 
  = 0528 . (1.23)
(Tn = 273.15 K and pn = 1013.25 mbar):  p1  crit
Viscous or continuum flow
m This will be found almost exclusively in the
p ·V = · R ·T The chart in Fig. 1.1 represents sche-
M rough vacuum range. The character of this matically the venting (or airing) of an eva-
type of flow is determined by the interac- cuated container through an opening in the
For the general gas constant: tion of the molecules. Consequently inter- envelope (venting valve), allowing ambient
nal friction, the viscosity of the flowing
1013.25 mbar · 22.4 ` · mol −1 air at p = 1000 mbar to enter. In accordan-
R= = substance, is a major factor. If vortex moti- ce with the information given above, the
273.15 K on appears in the streaming process, one resultant critical pressure is
mbar · ` speaks of turbulent flow. If various layers ∆pcrit = 1000 ⋅ (1–0.528) mbar ≈ 470 mbar;
= 83.14 of the flowing medium slide one over the
mol · K i.e. where ∆p > 470 mbar the flow rate will
other, then the term laminar flow or layer be choked; where ∆p < 470 mbar the gas
flux may be applied. flow will decline.
Laminar flow in circular tubes with para-
1.4 The pressure bolic velocity distribution is known as Poi- ∆p qm
seuille flow. This special case is found mbar %

ranges in vacuum frequently in vacuum technology. Viscous 1


flow will generally be found where the 100
technology and their molecules’ mean free path is considerab-
characterization ly shorter than the diameter of the pipe: 2 75
λ « d. 1000
qm
(See also Table IX in Chapter 9.) It is com- ∆p

mon in vacuum technology to subdivide its A characteristic quantity describing the 50

wide overall pressure range – which spans viscous flow state is the dimensionless
470
more than 16 powers of ten – into smaller Reynolds number Re. 25

individual regimes. These are generally Re is the product of the pipe diameter, flow
defined as follows: velocity, density and reciprocal value of the 0
s

Rough vacuum (RV) 1000 – 1 mbar viscosity (internal friction) of the gas venting time (t)
which is flowing. Flow is turbulent where
Medium vacuum (MV) 1 – 10-3.mbar
Re > 2200, laminar where Re < 2200. 1 Gas flow rate qm choked = constant
High vacuum (HV) 10 – 10-7 mbar
-3
(maximum value)
Ultrahigh vacuum (UHV) The phenomenon of choked flow may also
2 Gas flow not impeded, qm drops to ∆p = 0
10-7 – (10-14) mbar be observed in the viscous flow situation.
It plays a part when venting and evacua-
This division is, naturally, somewhat arbit- ting a vacuum vessel and where there are Fig. 1.1 Schematic representation of venting an
rary. Chemists in particular may refer to leaks. evacuated vessel
the spectrum of greatest interest to them,
lying between 100 and 1 mbar, as “inter- Gas will always flow where there is a diffe- Molecular flow
mediate vacuum”. Some engineers may rence in pressure ∆p = (p1 – p2) > 0. The Molecular flow prevails in the high and
not refer to vacuum at all but instead speak intensity of the gas flow, i.e. the quantity of ultrahigh vacuum ranges. In these regimes
of “low pressure” or even “negative pres- gas flowing over a period of time, rises the molecules can move freely, without
sure”. The pressure regimes listed above with the pressure differential. In the case any mutual interference. Molecular flow is
can, however, be delineated quite satisfac- of viscous flow, however, this will be the present where the mean free path length
torily from an observation of the gas-kine- case only until the flow velocity, which also for a particle is very much larger than the
tic situation and the nature of gas flow. The rises, reaches the speed of sound. This is diameter of the pipe: λ >> d.
operating technologies in the various ran- always the case at a certain pressure diffe-
ges will differ, as well. rential and this value may be characterized
as “critical”:

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Knudsen flow ratory equipment the collisions of the gas 1.5.2 Calculating
The transitional range between viscous particles among each other will predomi- conductance values
flow and molecular flow is known as Knud- nate in the rough vacuum range whereas
sen flow. It is prevalent in the medium in the high and ultrahigh vacuum ranges The effective pumping speed required to
vacuum range: λ ≈ d. impact of the gas particles on the contai- evacuate a vessel or to carry out a process
ner walls will predominate. inside a vacuum system will correspond to
The product of pressure p and pipe diame- the inlet speed of a particular pump (or the
ter d for a particular gas at a certain tem- In the high and ultrahigh vacuum ranges pump system) only if the pump is joined
perature can serve as a characterizing the properties of the vacuum container directly to the vessel or system. Practically
quantity for the various types of flow. wall will be of decisive importance since speaking, this is possible only in rare situa-
Using the numerical values provided in below 10-3 mbar there will be more gas tions. It is almost always necessary to
Table III, Chapter 9, the following equiva- molecules on the surfaces than in the include an intermediate piping system com-
lent relationships exist for air at 20 °C: chamber itself. If one assumes a mono- prising valves, separators, cold traps and
molecular adsorbed layer on the inside the like. All this represents an resistance to
Rough vacuum – Viscous flow wall of an evacuated sphere with 1 l volu- flow, the consequence of which is that the
me, then the ratio of the number of effective pumping speed Seff is always less
d
λ< ⇔ p ⋅ d > 6.0 ⋅ 10-1 mbar ⋅ cm adsorbed particles to the number of free than the pumping speed S of the pump or
100 molecules in the space will be as follows: the pumping system alone. Thus to ensure
at 1 mbar 10-2 a certain effective pumping speed at the
Medium vacuum – Knudsen flow vacuum vessel it is necessary to select a
at 10-6 mbar 10+4
d d at 10-11 mbar 10+9 pump with greater pumping speed. The
<λ< ⇔
100 2 correlation between S and Seff is indicated
For this reason the monolayer formation
by the following basic equation:
time t (see Section 1.1) is used to charac-
⇔ 6 ⋅ 10-1 > p ⋅ d > 1.3 ⋅ 10-2 mbar ⋅ cm terize ultrahigh vacuum and to distinguish 1 1 1
= + (1.24)
this regime from the high vacuum range. Seff S C
High and ultrahigh vacuum – Molecular The monolayer formation time τ is only a
flow fraction of a second in the high vacuum Here C is the total conductance value for
range while in the ultrahigh vacuum range the pipe system, made up of the individual
d ⇔ p ⋅ d < 1.3 ⋅ 10-2 mbar · cm it extends over a period of minutes or
λ> values for the various components which
2 hours. Surfaces free of gases can therefo- are connected in series (valves, baffles,
In the viscous flow range the preferred re be achieved (and maintained over lon- separators, etc.):
speed direction for all the gas molecules ger periods of time) only under ultrahigh
vacuum conditions. 1 1 1 1 1
will be identical to the macroscopic direc- = + + + . . . (1.25)
C C1 C2 C3 Cn
tion of flow for the gas. This alignment is Further physical properties change as
compelled by the fact that the gas particles pressure changes. For example, the ther-
are densely packed and will collide with Equation (1.24) tells us that only in the
mal conductivity and the internal friction of
one another far more often than with the situation where C = ∞ (meaning that the
gases in the medium vacuum range are
boundary walls of the apparatus. The flow resistance is equal to 0) will S = Seff.
highly sensitive to pressure. In the rough
macroscopic speed of the gas is a “group A number of helpful equations is available
and high vacuum regimes, in contrast,
velocity” and is not identical with the “ther- to the vacuum technologist for calculating
these two properties are virtually indepen-
mal velocity” of the gas molecules. the conductance value C for piping sec-
dent of pressure.
tions. The conductance values for valves,
In the molecular flow range, on the other Thus, not only will the pumps needed to cold traps, separators and vapor barriers
hand, impact of the particles with the walls achieve these pressures in the various will, as a rule, have to be determined empi-
predominates. As a result of reflection (but vacuum ranges differ, but also different rically.
also of desorption following a certain resi- vacuum gauges will be required. A clear It should be noted that in general that the
dence period on the container walls) a gas arrangement of pumps and measurement conductance in a vacuum component is
particle can move in any arbitrary direction instruments for the individual pressure not a constant value which is independent
in a high vacuum; it is no longer possible ranges is shown in Figures 9.16 and 9.16a of prevailing vacuum levels, but rather
to speak of “flow” in the macroscopic in Chapter 9. depends strongly on the nature of the flow
sense.
(continuum or molecular flow; see below)
It would make little sense to attempt to and thus on pressure. When using con-
determine the vacuum pressure ranges as ductance indices in vacuum technology
a function of the geometric operating calculations, therefore, it is always neces-
situation in each case. The limits for the sary to pay attention to the fact that only
individual pressure regimes (see Table IX
in Chapter 9) were selected in such a way
the conductance values applicable to a cer-
tain pressure regime may be applied in
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that when working with normal-sized labo- that regime.

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Fundamentals of Vacuum Technology Vacuum Physics

1.5.3 Conductance for piping d3 (1.28b) pumping speeds S*visc and S*mol refer-
C = 12.1 · ` /s enced to the area A of the opening and as
and orifices l
a function of δ = p2/p1. The equations
Conductance values will depend not only given apply to air at 20 °C. The molar mas-
on the pressure and the nature of the gas In the molecular flow region the conduc-
ses for the flowing gas are taken into con-
which is flowing, but also on the sectional tance value is independent of pressure!
sideration in the general equations, not
shape of the conducting element (e.g. cir- The complete Knudsen equation (1.26) will
shown here.
cular or elliptical cross section). Other fac- have to be used in the transitional area
tors are the length and whether the ele- 10–2 < d · –p < 6 · 10-1 mbar · cm. Conduc- l á sÐ1 á cmÐ2

ment is straight or curved. The result is tance values for straight pipes of standard
that various equations are required to take nominal diameters are shown in Figure 9.5
into account practical situations. Each of (laminar flow) and Figure 9.6 (molecular
these equations is valid only for a particu- flow) in Chapter 9. Additional nomograms
lar pressure range. This is always to be for conductance determination will also be
considered in calculations. found in Chapter 9 (Figures 9.8 and 9.9).
a) Conductance for a straight pipe, which
is not too short, of length l, with a cir-
cular cross section of diameter d for the
laminar, Knudsen and molecular flow
ranges, valid for air at 20 °C (Knudsen
equation):

d4 d 3 1 + 192 · d · p
C = 135 p +12.1 ·
l 1 + 237 · d · p
`/s (1.26)
l Fig. 1.2 Flow of a gas through an opening (A) at high
pressures (viscous flow)
where
b) Conductance value C for an orifice A
p +p (A in cm2): For continuum flow (viscous
p= 1 2
2 flow) the following equations (after
Prandtl) apply to air at 20 °C where
d = Pipe inside diameter in cm p2/p1 = δ:
l = Pipe length in cm (l ≥ 10 d)
p1 = Pressure at start of pipe for δ ≥ 0.528 (1.29)
(along the direction of flow) in mbar
A `
p2 = Pressure at end of pipe Cvisc = 76.6 · δ 0.712 · 1 − δ 0.288 · Fig. 1.3 Conductance values relative to the area,
(along the direction of flow) in mbar 1− δ s C*visc, C*mol, and pumping speed S*visc
and S*mol for an orifice A, depending on the
If one rewrites the second term in (1.26) in for δ ≤ 0.528 (1.29a) pressure relationship p2/p1 for air at 20 °C.
the following form
A ` When working with other gases it will be
C visc = 20 ·
d 3 1− δ s necessary to multiply the conductance
C = 12.1· · f (d · p ) (1.26a) values specified for air by the factors
l
and for δ ≤ 0,03 (1.29b) shown in Table 1.1.
with
` Gas (20 °C) Molecular flow Laminar flow
1 + 203 · d · p + 2.78 ·10 3 · d 2 · p 2 Cvisc = 20 · A Air 1.00 1.00
f (d · p ) = (1.27) s
1 + 237 · d · p Oxygen 0.947 0.91
Neon 1.013 1.05
it is possible to derive the two important δ = 0.528 is the critical pressure
Helium 2.64 0.92
limits from the course of the function f situation for air Hydrogen 3.77 2.07
(d · –p ): Carbon dioxide 0.808 1.26
p 
2 Water vapor 1.263 1.7
 
Limit for laminar flow  p1  crit
Table 1.1 Conversion factors (see text)
(d · –p > 6 · 10-1 mbar · cm):
Flow is choked at δ < 0.528; gas flow is
d4 (1.28a) thus constant. In the case of molecular
C = 135 · · p ` / s
l flow (high vacuum) the following will apply
for air:
Limit for molecular flow
(d · –p < 6 · 10-2 mbar · cm): Cmol = 11,6 · A · l · s-1 (A in cm2) (1.30)
Given in addition in Figure 1.3 are the

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Vacuum Physics Fundamentals of Vacuum Technology

Nomographic determination of conduc- The technical data in the Leybold catalog


tance values states the conductance values for vapor
The conductance values for piping and barriers, cold traps, adsorption traps and
openings through which air and other valves for the molecular flow range. At hig-
gases pass can be determined with nomo- her pressures, e.g. in the Knudsen and
graphic methods. It is possible not only to laminar flow ranges, valves will have about
determine the conductance value for the same conductance values as pipes of
piping at specified values for diameter, corresponding nominal diameters and
length and pressure, but also the size of axial lengths. In regard to right-angle val-
the pipe diameter required when a pum- ves the conductance calculation for an
ping set is to achieve a certain effective elbow must be applied.
pumping speed at a given pressure and
In the case of dust filters which are used to
given length of the line. It is also possible
protect gas ballast pumps and roots
to establish the maximum permissible pipe
pumps, the percentage restriction value
length where the other parameters are
for the various pressure levels are listed in
known. The values obtained naturally do
the catalog. Other components, namely the
not apply to turbulent flows. In doubtful
condensate separators and condensers,
situations, the Reynolds number Re (see
are designed so that they will not reduce
Section 1.5.) should be estimated using
pumping speed to any appreciable extent.
the relationship which is approximated
below The following may be used as a rule of
q thumb for dimensioning vacuum lines:
Re = 15 · pV (1.31)
d The lines should be as short and as wide
as possible. They must exhibit at least the
Here qpV = S · p is the flow output in mbar same cross-section as the intake port at
l/s, d the diameter of the pipe in cm. the pump. If particular circumstances pre-
A compilation of nomograms which have vent shortening the suction line, then it is
proved to be useful in practice will be advisable, whenever this is justifiable from
found in Chapter 9. the engineering and economic points of
view, to include a roots pump in the suc-
tion line. This then acts as a gas entrain-
1.5.4 Conductance values for ment pump which reduces line impedance.
other elements
Where the line contains elbows or other
curves (such as in right-angle valves),
these can be taken into account by assu-
ming a greater effective length leff of the
line. This can be estimated as follows:

θ
leff = laxial +133
. · ·d (1.32)
180°

Where
laxial : axial length of the line (in cm)
leff : Effective length of the line (in cm)
d : Inside diameter of the line (in cm)
θ : Angle of the elbow
(degrees of angle)

Axial length
D00

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Fundamentals of Vacuum Technology Vacuum Generation

2. Vacuum the atmosphere (compression pumps).


The gas particles are pumped by means
2. Pumps which transport quantities of
gas from the low pressure side to the
generation of displacement or pulse transfer.
b) Vacuum pumps where the gas particles
high pressure side without changing
the volume of the pumping chamber
which are to be removed condense on (Roots pumps, turbomolecular pumps)
or are bonded by other means (e.g. 3. Pumps where the pumping effect is
2.1. Vacuum pumps: A chemically) to a solid surface, which
often is part of the boundary forming
based mainly on the diffusion of gases
into a gas-free high speed vapor jet
survey volume itself. (vapor pumps)
4. Pumps which pump vapors by means of
Vacuum pumps are used to reduce the gas A classification which is more in line with
condensation (condensers) and pumps
pressure in a certain volume and thus the the state-of-the-art and practical applica-
which pump permanent gases by way
gas density (see equation 1.5). Conse- tions makes a difference between the
of condensation at very low tempera-
quently consider the gas particles need to following types of pumps, of which the
tures (cryopumps)
be removed from the volume. Basically first three classes belong to the compres-
5. Pumps which bond or incorporate ga-
differentiation is made between two sion pumps and where the two remaining
ses by adsorption or absorption to
classes of vacuum pumps: classes belong to the condensation and
surfaces which are substantially free of
a) Vacuum pumps where – via one or getter pumps:
gases (sorption pumps).
several compression stages – the gas 1. Pumps which operate with periodically
particles are removed from the volume increasing and decreasing pump cham- A survey on these classes of vacuum
which is to be pumped and ejected into ber volumes (rotary vane and rotary pumps is given in the diagram of Table 2.1.
plunger pumps; also trochoid pumps)

Vacuum pump
(Operating principle)

Gas transfer Entrapment


vacuum pump vacuum pump
Positive displacement Kinetic
vacuum pump vacuum pump

Reciprocating
Rotary Drag Fluid entrainment Ion transfer Adsorption
positive displacement vacuum pump vacuum pump vacuum pump vacuum pump pump
vacuum pump

Diaphragm Liquid sealed Gaseous ring Ejector Getter pump


vacuum pump vacuum pump vacuum pump vacuum pump

Liquid ring
Piston vacuum pump Turbine Liquid jet
Bulk getter pump
vacuum pump vacuum pump vacuum pump

Rotary vane
vacuum pump Axial flow Gas jet Sublimation
vacuum pump vacuum pump pump

Multiple vane
vacuum pump
Radial flow Vapor jet
Getter ion pump
vacuum pump vacuum pump

Rotary piston
vacuum pump
Molecular drag
vacuum pump Diffusion pump Evaporation ion pump

Rotary plunger
vacuum pump

Turbomolecular pump Self-purifying Sputter-ion pump


diffusion pump

Dry compressing
vacuum pump

Fractionating
diffusion pump Cryopump
Roots
vacuum pump

Diffusion ejector Condenser


pump
Claw
vacuum pump

Scroll pump

Table 2.1 Classification of vacuum pumps

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Vacuum Generation Fundamentals of Vacuum Technology

2.1.1 Oscillation displacement pumping chamber so that it remains free mbar. Two-stage pumps such as the
vacuum pumps of oil and lubricants (dry compressing DIVAC from LEYBOLD can attain about
vacuum pump). Diaphragm and valves are 10 mbar (see Fig. 2.2), three-stage pumps
2.1.1.1 Diaphragm pumps the only components in contact with the can attain about 2 mbar and four-stage
medium which is to be pumped. When diaphragm pumps can reach about
Recently, diaphragm pumps have coating the diaphragm with PTFE (Teflon) 5·10-1 mbar.
becoming ever more important, mainly for and when manufacturing the inlet and
environmental reasons. They are alterna- exhaust valves of a highly fluorinated Diaphragm pumps offering such a low
tives to water jet vacuum pumps, since elastomer as in the case of the DIVAC from ultimate pressure are suited as backing
diaphragm pumps do not produce any LEYBOLD, it is then possible to pump pumps for turbomolecular pumps with fully
waste water. Overall, a diaphragm vacuum aggressive vapors and gases. It is thus integrated Scroll stages (compound or wide
pump can save up to 90 % of the operating well suited for vacuum applications in the range turbomolecular pumps, such as the
costs compared to a water jet pump. chemistry lab. TURBOVAC 55 from LEYBOLD). In this way
Compared to rotary vane pumps, the a pump system is obtained which is ab-
pumping chamber of diaphragm pumps Due to the limited elastic deformability of solutely free of oil, this being of great im-
are entirely free of oil. By design, no oil the diaphragm only a comparatively low portance to measurement arrangements
immersed shaft seals are required. pumping speed is obtained. In the case of involving mass spectrometer systems and
Diaphragm vacuum pumps are single or this pumping principle a volume remains leak detectors. In contrast to rotary vane
multi-stage dry compressing vacuum at the upper dead center – the so called pumps this combination of pumps for leak
pumps (diaphragm pumps having up to “dead space” – from where the gases can detectors offers the advantage that
four stages are being manufactured). Here not be moved to the exhaust line. The naturally no helium is dissolved in the
the circumference of a diaphragm is quantity of gas which remains at the ex- diaphragm pump thereby entirely avoiding
tensioned between a pump head and the haust pressure expands into the expanding a possible build up of a helium background.
casing wall (Fig. 2.1). It is moved in an pumping chamber during the subsequent
oscillating way by means of a connecting suction stroke thereby filling it, so that as
rod and an eccentric. The pumping or the intake pressure reduces the quantity of 2.1.2 Liquid sealed rotary
inflowing new gas reduces more and
compression chamber, the volume of displacement pumps
which increases and decreases periodi- more. Thus volumetric efficiency worsens
cally, effects the pumping action. The continuously for this reason. Diaphragm
valves are arranged in such a way that vacuum pumps are not capable of 2.1.2.1 Liquid ring pumps
during the phase where the volume of the attaining a higher compression ratio than
Due to the pumping principle and the
pumping chamber increases it is open to the ratio between “dead space” and
simple design, liquid ring vacuum pumps
the intake line. During compression, the maximum volume of the pumping cham-
are particularly suited to pumping gases
pumping chamber is linked to the exhaust ber. In the case of single-stage diaphragm
and vapors which may also contain small
line. The diaphragm provides a hermetic vacuum pumps the attainable ultimate
amounts of liquid. Air, saturated with water
seal between the gear chamber and the pressure amounts to approximately 80
vapors or other gases containing conden-

IN EX

a)

b)

c)

d)

(1) Casing lid (5) Diaphragm 2nd stage


1st stage
(2) Valves (6) Diaphragm support disk
(3)
(4)
Lid
Diaphragm disk
(7)
(8)
Connecting rod
Eccentric disk
Opening and closing of the valves, path and pumping mechanism
during four subsequent phases of a turn of the connecting rod (a-d)
D00
Fig. 2.1 Schematic on the design of a diaphragm pump stage (Vacuubrand) Fig. 2.2 Principle of operation for a two-stage diaphragm pump (Vacuubrand)

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Fundamentals of Vacuum Technology Vacuum Generation

sable constituents, may be pumped 2.1.2.2.1 Rotary vane pumps


without problems. By design, liquid ring (TRIVAC A, TRIVAC B,
pumps are insensitive to any contamina- TRIVAC E, SOGEVAC)
tion which may be present in the gas flow.
Rotary vane pumps (see also Figs. 2.5 and
The attainable intake pressures are in the
2.6) consist of a cylindrical housing
region between atmospheric pressure and
(pump-ing ring) (1) in which an eccentri-
the vapor pressure of the operating liquid
cally suspended and slotted rotor (2) turns
used. For water at 15 °C it is possible to
in the direction of the arrow. The rotor has
attain an operating pressure of 33 mbar. A
vanes (16) which are forced outwards
typical application of water ring vacuum
usually by centrifugal force but also by
pumps is venting of steam turbines in
springs so that the vanes slide inside the
power plants. Liquid ring vacuum pumps Constant, minimum clearance a for the entire housing. Gas entering through the intake
(Fig. 2.3) are rotary displacement pumps sealing passage b
(4) is pushed along by the vanes and is
which require an operating liquid which
Fig. 2.4 Arrangement of the sealing passage in rotary finally ejected from the pump by the oil
rotates during operation to pump the gas.
vane pumps sealed exhaust valve (12).
also known as “duo seal”
The older range of TRIVAC A pumps (Fig.
1. Removal of the heat produced by the 2.5) from LEYBOLD has three radial vanes
compression process. offset by 120°. The TRIVAC B range (Fig.
2. Uptake of liquids and vapors 2.6) has only two vanes offset by 180°. In
(condensate).
3. Providing the seal between the blade
wheel and the casing.

2.1.2.2 Oil sealed rotary displacement


1 Rotor 4 Intake channel
pumps
2 Rotor shaft 5 Liquid ring A displacement vacuum pump is generally
3 Casing 6 Flex. discharge channel
a vacuum pump in which the gas which is
Fig. 2.3 Liquid ring vacuum pump, schematic to be pumped is sucked in with the aid of
(Siemens) pistons, rotors, vanes and valves or
similar, possibly compressed and then
The blade wheel is arranged eccentrically discharged. The pumping process is
in a cylindrical casing. When not in opera- effected by the rotary motion of the piston
tion, approximately half of the pump is inside the pump. Differentiation should be
filled with the operating fluid. In the axial made between oiled and dry compressing
direction the cells formed by the blade displacement pumps. By the use of sealing
oil it is possible to attain in a single-stage 1 Pump housing 9 Exhaust port
wheel are limited and sealed off by 2 Rotor 10 Air inlet silencer
“control discs”. These control discs are high compression ratios of up to about 3 Oil-level sight glass 11 Oil filter
equipped with suction and ejection slots 105. Without oil, “inner leakiness” is 4 Suction duct 12 Exhaust valve
which lead to the corresponding ports of considerably greater and the attainable 5 Anti-suckback valve 13 Exhaust duct
compression ratio is correspondingly less, 6 Dirt trap 14 Gas ballast duct
the pump. After having switched on such a 7 Intake port 15 Oil injection
pump the blade wheel runs eccentrically about 10. 8 Lid of gas ballast 16 Vane
within the casing; thus a concentrically As shown in the classification Table 2.1, valve
rotating liquid ring is created which at the the oil sealed displacement pumps include
narrowest point fully fills the space rotary vane and rotary plunger pumps of Fig. 2.5 Cross section of a single-stage rotary vane
between the casing and the blade wheel single and two-stage design as well as pump (TRIVAC A)
and which retracts from the chambers as single-stage trochoid pumps which today
the rotation continues. The gas is sucked are only of historic interest. Such pumps both cases the vanes are forced outwards
in as the chambers empty and compres- are all equipped with a gas ballast facility by the centrifugal forces without the use of
sion is obtained by subsequent filling. The which was described in detail (for details springs. At low ambient temperatures this
limits for the intake or discharge process see 2.1.2.2.4) for the first time by Gaede possibly requires the use of a thinner oil.
are set by the geometry of the openings in (1935). Within specified engineering The A-Series is lubricated through the
the control discs. limits, the gas ballast facility permits arising pressure difference whereas the B-
pumping of vapors (water vapor in Series pumps have a geared oil pump for
In addition to the task of compression, the
particular) without condensation of the pressure lubrication. The TRIVAC B-Series
operating fluid fulfills three further
vapors in the pump. is equipped with a particularly reliable anti-
important tasks:
suckback valve; a horizontal or vertical

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Vacuum Generation Fundamentals of Vacuum Technology

the oil box (user friendly design). In


combination with the TRIVAC BCS system
it may be equipped with a very com- Valve stop
prehensive range of accessories, designed
chiefly for semiconductor applications.
The oil reservoir of the rotary vane pump
and also that of the other oil sealed Leaf
spring
displacement pumps serves the purpose of the
of lubrication and sealing, and also to fill valve
dead spaces and slots. It removes the heat
of gas compression, i.e. for cooling I High vacuum stage
II Second forevacuum stage
purposes. The oil provides a seal between
rotor and pump ring. These parts are Fig. 2.7 Cross section of a two-stage rotary vane
“almost” in contact along a straight line pump, schematic
(cylinder jacket line). In order to increase
the oil sealed surface area a so-called
two-stage oil sealed pumps it is possible
1 Intake port 8 Orifice, connec- sealing passage is integrated into the
to attain lower operating and ultimate
2 Dirt trap tion for inert gas pumping ring (see Fig. 2.4). This provides
3 Anti-suckback ballast pressures ompared to the corresponding
a better seal and allows a higher com-
valve 9 Exhaust duct single-stage pumps. The reason for this is
4 Intake duct 10 Exhaust valve pression ratio or a lower ultimate pres-
that in the case of single-stage pumps, oil
5 Vane 11 Demister sure. LEYBOLD manufactures three
is unavoidably in contact with the
6 Pumping cham- 12 Spring different ranges of rotary vane pumps
ber 13 Orifice; connec- atmosphere outside, from where gas is
which are specially adapted to different
7 Rotor tion for oil filter taken up which partially escapes to the
applications such as high intake pressure,
vacuum side thereby restricting the
Fig. 2.6 Cross section of a single-stage rotary vane low ultimate pressure or applications in
attainable ultimate pressure. In the oil
pump (TRIVAC B) the semiconductor industry. A summary of
sealed two-stage displacement pumps
the more important characteristics of
manufactured by LEYBOLD, oil which has
arrangement for the intake and exhaust these ranges is given in Table 2.2. The
already been degassed is supplied to the
ports. The oil level sight glass and the gas TRIVAC rotary vane pumps are produced
stage on the side of the vacuum (stage 1 in
ballast actuator are all on the same side of as single-stage (TRIVAC S) and two-stage
Fig. 2.7): the ultimate pressure lies almost
(TRIVAC D) pumps (see Fig. 2.7). With the

TRIVAC A TRIVAC B TRIVAC BCS TRIVAC E SOGEVAC

Vanes per stage 3 2 2 2 3 (tangential)

1 – 1.5 1.6 – – 16 – 25
Pumping speed 2–4 4–8 16 – 25 2.5 40 – 100
[m3/h] 8 – 16 16 – 25 40 – 65 – 180 – 280
30 – 60 40 – 65 – – 585 – 1200

Sealing passage yes yes yes yes no

Ultimate pressure, < 2 · 10–2 < 2 · 10–2 < 2 · 10–2 – < 5 · 10–1
single-stage [mbar]

Ultimate pressure < 2.5 · 10–4 < 1 · 10–4 < 1 · 10–4 < 1 · 10–4 –
two-stage [mbar]

Oil supply Pressure difference Gear pump Gear pump Eccentric pump Pressure difference

Slots Comparable for all types: about 0.01 to 0.05 mm

Bearing/lubrication Axial face / oil Axial face / oil Axial face / oil Ball / grease Ball / oil

Special – Hydropneumatic Coated parts in Many Cost-effective


characteristics anti-suckback valve contact with medium accessories

Media No ammonia Clean to Aggressive and Clean to Clean


light particles corrosive light particles

Main areas of
application
Multi-
purpose
Multi-
purpose
Semiconductor
industry
Multi-
purpose
Packaging
industry
D00
Table 2.2 Rotary vacuum pump ranges

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Fundamentals of Vacuum Technology Vacuum Generation

Fig. 2.8a Cross section of a two-stage rotary vane Fig. 2.8b SOGEVAC pump SV 300 with three tangen-
pump (TRIVAC E) tial vanes

in the high vacuum range, the lowest direction of the arrow moves along the
operating pressures lie in the range chamber wall. The gas which is to be
between medium vacuum / high vacuum. pumped flows into the pump through the
Note: operating the so called high vacuum intake port (11), passes through the intake
1 Casing 8 Exhaust pot
stage (stage 1) with only very little oil or channel of the slide valve (12) into the 2 Cylindrical piston 9 Gas ballast valve
no oil at all will – in spite of the very low pumping chamber (14). The slide valve 3 Eccentric 10 Dirt trap
ultimate pressure – in practice lead to forms a unit with the piston and slides to 4 Compression 11 Intake port
considerable difficulties and will signifi- and fro between the rotatable valve guide chamber 12 Slide valve
5 Oil sealed pressure 13 Hinge bar
cantly impair operation of the pump. in the casing (hinge bar 13). The gas valve 14 Pumping chamber
drawn into the pump finally enters the 6 Oil-level sight glass (air is flowing in)
compression chamber (4). While turning, 7 Gas ballast channel
2.1.2.2.2 Rotary plunger pumps the piston compresses this quantity of gas
(E-Pumps) until it is ejected through the oil sealed Fig. 2.9 Cross section of a single-stage rotary plun-
ger pump (monoblock design)
valve (5). As in the case of rotary vane
Shown in Fig. 2.9 is a sectional view of a
pumps, the oil reservoir is used for
rotary plunger pump of the single block
lubrication, sealing, filling of dead spaces each turn completes an operating cycle
type. Here a piston (2) which is moved
and cooling. Since the pumping chamber (see Fig. 2.10). Rotary plunger pumps are
along by an eccentric (3) turning in the
is divided by the piston into two spaces, manufactured as single and two-stage
pumps. In many vacuum processes
combining a Roots pump with a single-
stage rotary plunger pump may offer more
advantages than a two-stage rotary
plunger pump alone. If such a combination
or a two-stage pump is inadequate, the
use of a Roots pump in connection with a
two-stage pump is recommended. This
does not apply to combinations involving
rotary vane pumps and Roots pumps.

Motor power
The motors supplied with the rotary vane
and rotary plunger pumps deliver enough
power at ambient temperatures of 12 °C
and when using our special oils to cover
1 Upper dead point 4 Slot in suction channel is clo- – commencement of gas bal- the maximum power requirement (at about
2 Slot in suction channel of sed again by swivelling hinge last inlet
400 mbar). Within the actual operating
slide valve is freed – begin- bar – end of suction period 7 Gas ballast opening is quite
ning of suction period 5 Upper dead point – maximum free range of the pump, the drive system of the
3 Lower dead point – slot in space between rotating 8 End of gas ballast inlet warmed up pump needs to supply only
suction channel is quite free, piston and stator 9 End of pumping period. about one third of the installed motor
and pumped-in gas (arrow) 6 Shortly before beginning of
power (see Fig. 2.11).
enters freely into the pum- compression period, the front
ping chamber (shown sha- surface of the rotating plun-
ded) ger frees gas ballast opening

Fig. 2.10 Operating cycle of a rotary plunger pump (for positions 1 to 9 of the plunger)

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Vacuum Generation Fundamentals of Vacuum Technology


Power of the drive motor [Watt]

Di
sc
ha

ion
rg

ss
e

t
inle
pre

st
alla
Com

sb
Ga
Gas ballast Position
inlet of the
leading
vane

on
Sucti

Pressure [mbar]

1 Operating temp. 5 Theoretic curve for


1 Toothed wheel fixed to the driving shaft
curve 1 32°C, adiabatic compres-
2 Toothed wheel fixed to the piston 1–2 Suction
2 Operating temp. sion
3 Elliptic piston 2–5 Compression
curve 2 40°C, 6 Theoretic curve for
4 Inner surface of the pump 3–4 Gas ballast inlet
3 Operating temp. isotherm compres-
5 Driving shaft 5–6 Discharge
curve 3 60°C, sion
6 Eccentric
4 Operating temp.
curve 4 90°C,

Fig. 2.11 Motor power of a rotary plunger pump (pum-


ping speed 60 m3/h) as a function of intake
pressure and operating temperature. The cur-
ves for gas ballast pumps of other sizes are Fig. 2.13 Working process within a rotary vane pump
similar. Fig. 2.12 Cross section of a trochoid pump with gas ballast

2.1.2.2.3 Trochoid pumps the area of manufacturing, so that today the pump’s oil. This very rapidly impairs
LEYBOLD does not produce trochoid the lubricating properties of the oil and the
Trochoid pumps belong to the class of so
pumps any more. Operation of such a pump may even seize when it has taken up
called rotary piston pumps, which (see
pump is shown in the sectional diagram of too much water. The gas ballast facility
overview of Table 2.1) in turn belong to the
Fig. 2.12. developed in 1935 by Wolfgang Gaede
group of rotary pumps. With rotary piston
inhibits the occurrence of condensation of
pumps, the piston’s center of gravity runs
the vapor in the pump as follows. Before
along a circular path about the rotational
2.1.2.2.4 The gas ballast the actual compression process begins
axis (hence rotary piston machines). A
(see Fig. 2.13), a precisely defined quantity
rotary piston pump can – in contrast to the The gas ballast facility as used in the rotary
of air (“the gas ballast”) is admitted into
rotary plunger pump – be completely vane, rotary plunger and trochoid pumps
the pumping chamber of the pump. The
balanced dynamically. This offers the permits not only pumping of permanent
quantity is such that the compression ratio
advantage that larger pumps can operate gases but also even larger quantities of
of the pump is reduced to 10:1 max. Now
without vibration so that they can be condensable gases.
vapors which have been taken in by the
installed without needing foundations.
The gas ballast facility (see Fig. 2.13) pump may be compressed together with
Moreover, such pumps may be operated at
prevents condensation of vapors in the the gas ballast, before reaching their
higher speed, compared to rotary plunger
pump chamber of the pump. When condensation point and ejected from the
pumps (see below). The volume of the
pumping vapors these may only be pump. The partial pressure of the vapors
pumping chamber with respect to the
compressed up to their saturation vapor which are taken in may however not
volume of the entire pump – the so called
pressure at the temperature of the pump. exceed a certain value. It must be so low
specific volume – is, in the case of
If pumping water vapor, for example, at a that in the case of a compression by a
trochoid pumps, approximately twice of
pump temperature of 70 °C, the vapor may factor of 10, the vapors can not condense
that of rotary plunger pumps. Larger
only be compressed to 312 mbar at the operating temperature of the pump.
rotary plunger pumps run at speeds of
(saturation vapor pressure of water at When pumping water vapor this critical
500 rpm. The trochoid pump may run at
70 °C (see Table XIII in Section 9)). When value is termed the “water vapor
1000 rpm and this applies also to larger
compressing further, the water vapor tolerance”.
designs. It is thus about four times smaller
condenses without increasing the
compared to a rotary plunger pump having Shown schematically in Fig. 2.14 is the
pressure. No overpressure is created in
the same pumping speed and runs without
producing any vibrations. Unfortunately
the pump and the exhaust valve is not
opened. Instead the water vapor remains
pumping process with and without gas
ballast as it takes place in a rotary vane D00
the advantages in the area of engineering pump when pumping condensable vapors.
as water in the pump and emulsifies with
are combined with great disadvantages in

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Fundamentals of Vacuum Technology Vacuum Generation

Two requirements must be met when ∆pexhaust filter = is the pressure difference
pumping vapors: across the exhaust filter
1) the pump must be at operating amounting to 0 ... 0.5 bar
temperature.
2) the gas ballast valve must be open. Example 1:
With a rotary vane pump with an external
(With the gas ballast valve open the oil mist filter in series, a mixture of water
temperature of the pump increases by vapor and air is being pumped. The follo-
about 10 °C. Before pumping vapors the wing values are used for applying eq. (2.1):
pump should be operated for half an hour
with the gas ballast valve open). pexhaust = 1 bar

∆pvalve + ∆pexhaust filter = 0.35 bar,


Simultaneous pumping of gases and
vapors temperature of the pump 70 °C
When simultaneously pumping permanent Hence:
gases and condensable vapors from a
vacuum system, the quantity of permanent psum = 1.35 bar; pvapor sat (H2O)
gas will often suffice to prevent any = 312 mbar
condensation of the vapors inside the
(see Table XIII in chapter 9)
pump. The quantity of vapor which may be
pumped without condensation in the Using eq. (2.1) follows:
pump can be calculated as follows:
a) Without gas bal- b) With gas ballast pvapour , H O 312
pvapour p 2
< = 0. 23
last 1) Pump is connected
< vapour, sat (2.1) pvapour , H O + pair 1350
1) Pump is connected to the vessel, which pvapour + pperm p sum 2

to the vessel, which is already almost


is already almost empty of air The pressure of the water vapor in the
empty of air (70 mbar) – it must Where: air/water vapor mixture must not exceed
(70 mbar) – it must thus transport pvapor = is the partial pressure of 23 % of the total pressure of the mixture.
thus transport mostly vapor
vapor at the intake of the
mostly vapor particles
particles 2) Pump chamber is pump Example 2:
2) Pump chamber is separated from the pperm = is the total pressure of all Ethanoic acid is to be pumped with a
separated from the vessel – now the pumped permanent gases rotary plunger pump.
vessel – compres- gas ballast valve,
at the intake of the pump
sion begins through which the pexhaust = 1.1 bar (taking into
3) Content of pump pump chamber is pvapor, sat = is the saturation pressure
chamber is already filled with additio- of the pumped vapor, consideration the flow
so far compressed nal air from outsi- depending on temperatu- resistance of the pipes)
that the vapor con- de, opens – this
re (see Fig. 2.15) ∆pvalve = 0.25 bar
denses to form additional air is cal-
droplets – over- led gas ballast psum = pexhaust + ∆pvalve +
pressure is not yet 3) Discharge valve is ∆pexhaust filter ∆pexhaust filter = 0.15 bar
reached pressed open, and ∆pvalve = is the pressure difference (pressure loss in the oil
4) Residual air only particles of vapor
across the exhaust valve mist trap)
now produces the and gas are pushed
required overpres- out – the overpres- which amounts depen-
sure and opens the sure required for ding on type of pump and Hence:
discharge valve, this to occur is rea- operating conditions to
but the vapor has ched very early
psum = 1.5 bar.
0.2 ... 0.4 bar
already condensed because of the sup-
and the droplets plementary gas By controlled cooling the pump and oil
are precipitated in ballast air, as at the temperature is set at 100 °C. The saturati-
the pump. beginning the enti- on pressure of the acid therefore is – see
Saturation vapor pressure [mbar]

re pumping pro-
Saturation vapor pressure [Torr]

Fig. 2.15 – pvapor, sat = 500 mbar.


cess condensation
cannot occur
4) The pump dischar- From eq. (2.1) follows:
ges further air and
vapor pvapour, acid 0.5 1
=< =
pvapour, acid + pair 1.5 3

Returning to the question of pumping


water vapor in a mixture with air, the ratio
Fig. 2.14 Diagram of pumping process in a rotary vane
pump without (left) and with (right) gas bal-
Temperature [° C] 3 parts of permanent gases to 1 part of
last device when pumping condensable sub- water vapor, as indicated in example 1, can
stances Fig. 2.15 Saturation vapor pressures be for guidance only. In actual practice it is

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Vacuum Generation Fundamentals of Vacuum Technology

recommended to run up a rotary pump of Water vapor tolerance the gas ballast B would result in an increa-
the types described hitherto always with An important special case in the general sed water vapor tolerance pW,0. In prac-
the gas ballast valve open, because it takes considerations made above relating to the tice, an increase in B, especially in the case
some time until the pump has reached its topic of vapor tolerance is that of pumping of single-stage gas ballast pumps is
final working temperature. water vapor. According to PNEUROP water restricted by the fact that the attainable
vapor tolerance is defined as follows: ultimate vacuum for a gas ballast pump
From eq. (2.1) follows for the permissible
operated with the gas ballast valve open
partial pressure pvapor of the pumped “Water vapor tolerance is the highest
becomes worse as the gas ballast B
vapor the relation pressure at which a vacuum pump, under
increases. Similar considerations also
normal ambient temperatures and
apply to the general equation 2.3 for the
pvapour, sat pressure conditions (20 °C, 1013 mbar),
pvapour ≤ ·p vapor tolerance pvapor.
psum − pvapour, sat perm (2.2) can continuously take in and transport
pure water vapor. It is quoted in mbar”. It At the beginning of a pump down process,
This relation shows that with pperm = 0 no is designated as pW,O. the gas ballast pump should always be
vapors can be pumped without condensa- operated with the gas ballast valve open.
Applying eq. (2.3) to this special case In almost all cases a thin layer of water will
tion in the pump, unless the gas-ballast
means: be present on the wall of a vessel, which
concept is applied. The corresponding for-
mula is: pperm = 0 and pvapor, sat = ps (H2O), thus: only evaporates gradually. In order to
(p −p ) attain low ultimate pressures the gas
p vapour ≤ B p su m· Va pour, sat vapour , g.b. +
S psum − p vapour , sat B p ( H O ) − pvapour, g.b. ballast valve should only be closed after
p (2.3) p W, O = p sum s 2 (2.4) the vapor has been pumped out. LEYBOLD
+ p vapour sat
p perm S psum − ps ( H 2O )
sum − p vapour sat pumps generally offer a water vapor tole-
rance of between 33 and 66 mbar. Two-
If for the gas ballast gas atmospheric air of
Where: stage pumps may offer other levels of
50 % humidity is used, then
B = is the volume of air at water vapor tolerance corresponding to
pvapor, g.b. = 13 mbar; with B/S = 0.10
1013 mbar which is admitted the compression ratio between their
– a usual figure in practice – and psum
to the pump chamber per unit stages – provided they have pumping
(total exhaust pressure) = 1330 mbar, the
time, called in brief the “gas chamber of different sizes.
water vapor tolerance pW,0 as function of
ballast”
the temperature of the pump is represen-
S = is the nominal speed of the Other gases as ballast
ted by the lowest curve in diagram Fig.
pump (volume flow rate) Generally atmospheric air is used as the
2.16. The other curves correspond to the
psum = is the pressure at the gas ballast medium. In special cases,
pumping of water vapor-air mixtures,
discharge outlet of the pump, when pumping explosive or toxic gases,
hence pperm = pair ≠ O), indicated by the
assumed to be a maximum at for example, other permanent gases like
symbol pL in millibar. In these cases a hig-
1330 mbar noble gases or nitrogen, may be used (see
her amount of water vapor partial pressu-
pvapor, sat = Saturation vapor pressure of Section 8.3.1.3).
re pw can be pumped as shown in the dia-
the vapor at the pump’s
gram. The figures for pW,0 given in the
exhaust port
catalogue therefore refer to the lower limit
pvapor, g.b. = is the partial pressure of any
and are on the safe side.
vapor that might be present
in the gas used as gas ballast According to equation 2.4 an increase in
(e.g. water vapor contained in
the atmospheric air when pL [mbar]
used as gas ballast)
pperm = is the total pressure of all per-
manent gases at the inlet port
of the pump
pW [mbar]

Eq. (2.3) shows that when using gas


ballast (B ≠ 0) vapors can also be pumped
without condensation if no gas is present
at the intake of the pump. The gas ballast Temperature of the pump
may also be a mixture of non-condensable
gas and condensable vapor as long as the
partial pressure of this vapor (pvapor, g.b.) is Fig. 2.16 Partial pressure pW of water vapor that can
less than the saturation pressure pvapor, sat be pumped with the gas ballast valve open
without condensation in the pump, as a fun-
of the pumped vapor at the temperature of
the pump.
ction of the pump temperature for various
partial pressures pL of air. The lowest curve
D00
corresponds to the water vapor tolerance
pW, O of the pump

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Fundamentals of Vacuum Technology Vacuum Generation

2.1.3 Dry compressing rotary without mechanical wear. In contrast to SiR = n · ViR (2.9)
displacement pumps rotary vane and rotary plunger pumps,
Roots pumps are not oil sealed, so that the i.e. the product of speed n and internal lea-
internal leakage of dry compressing kage volume ViR.
2.1.3.1 Roots pumps
pumps by design results in the fact that
The design principle of the Roots pumps Volumetric efficiency of a Roots pumps is
compression ratios only in the range 10 –
was already invented in 1848 by Isaiah given by
100 can be attained. The internal leakage
Davies, but it was 20 years later before it of Roots pumps, and also other dry Q eff
was implemented in practice by the compressing pumps for that matter, is η= (2.10)
Q th
Americans Francis and Philander Roots. mainly based on the fact that owing to the
Initially such pumps were used as blowers operating principle certain surface areas of By using equations 2.5, 2.6, 2.7 and 2.8
for combustion motors. Later, by inverting the pump chamber are assigned to the one obtains
the drive arrangement, the principle was intake side and the compression side of
employed in gas meters. Only since 1954 pV SiR
the pump in alternating fashion. During the η = 1− · (2.11)
has this principle been employed in compression phase these surface areas pa Sth
vacuum engineering. Roots pumps are (rotors and casing) are loaded with gas
used in pump combinations together with (boundary layer); during the suction phase When designating the compression pv/pa
backing pumps (rotary vane- and rotary this gas is released. The thickness of the as k one obtains
plunger pumps) and extend their operating traveling gas layer depends on the SiR
range well into the medium vacuum range. clearance between the two rotors and η = 1− k (2.11a)
Sth
With two stage Roots pumps this extends between the rotors and the casing wall.
into the high vacuum range. The operating Due to the relatively complex thermal Maximum compression is attained at zero
principle of Roots pumps permits the conditions within the Roots pump it is not throughput (see PNEUROP and
assembly of units having very high possible to base one’s consideration on DIN 28 426, Part 2). It is designated as k0:
pumping speeds (over 100,000 m3/h) the cold state. The smallest clearances and
which often are more economical to thus the lowest back flows are attained at Sth
k0 = ( ) =
operate than steam ejector pumps running operating pressures in the region of SiR η 0 (2.12)
in the same operating range. 1 mbar. Subsequently it is possible to
A Roots vacuum pump (see Fig. 2.17) is a attain in this region the highest com- k0 is a characteristic quantity for the Roots
rotary positive-displacement type of pump pression ratios, but this pressure range is pump which usually is stated as a function
where two symmetrically-shaped impel- also most critical in view of contacts of the forevacuum pressure pV (see Fig.
lers rotate inside the pump casing past between the rotors and the casing. 2.18). k0 also depends (slightly) on the
each other in close proximity. The two type of gas.
rotors have a cross section resembling Characteristic quantities of roots pumps For the efficiency of the Roots pump, the
approximately the shape of a figure 8 and The quantity of gas Qeff effectively pumped
are synchronized by a toothed gear. The by a Roots pump is calculated from the
clearance between the rotors and the theoretically pumped quantity of gas Qth
casing wall as well as between the rotors and the internal leakage QiR (as the
themselves amounts only to a few tenths quantity of gas which is lost) as:
of a millimeter. For this reason Roots Qeff = Qth – QiR (2.5)
pumps may be operated at high speeds
The following applies to the theoretically
pumped quantity of gas:

1 Qth = pa · Sth (2.6)


2 2 Fig. 2.18 Maximum compression k0 of the Roots pump
where pa is the intake pressure and Sth is RUVAC WA 2001 as a function of fore vacu-
the theoretical pumping speed. This in turn um pressure pV
is the product of the pumping volume VS
and the speed n: generally valid equation applies:
Sth = n · VS (2.7)
η = 1− k (2.13)
Similarly the internal leakage QiR is ko
3
5 calculated as:
4 Normally a Roots pump will be operated in
QiR = n · ViR (2.8)
connection with a downstream rough
1 Intake flange 4 Exhaust flange where pV is the forevacuum pressure vacuum pump having a nominal pumping
2 Rotors 5 Casing
(pressure on the forevacuum side) and SiR speed SV. The continuity equation gives:
3 Chamber
is a (notional) “reflow” pumping speed
with SV · pV = Seff · pa = η · Sth · pa (2.14)
Fig. 2.17 Schematic cross section of a Roots pump

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Vacuum Generation Fundamentals of Vacuum Technology

From this b) the max. compression as a function of Power requirement of a roots pump
p S the fore vacuum pressure: k0 (pV) Compression in a Roots pump is perfor-
k = V = η · th (2.15) med by way of external compression and
pa SV c) the pumping speed characteristic of the
backing pump SV (pV) is termed as isochoric compression.
Experience shows that the following equa-
The ratio Sth/SV (theoretical pumping
The way in which the calculation is carried tion holds approximately:
speed of the Roots pump / pumping speed
out can be seen in Table 2.3 giving the data
of the backing pump) is termed the Ncompression = Sth (pv – pa) (2.18)
for the combination of a Roots pump
gradation kth. From (2.15) one obtains
RUVAC WA 2001 / E 250 (single-stage ro- In order to determine the total power (so-
k = η · kth (2.16) tary plunger pump, operated without gas called shaft output) of the pump, mecha-
ballast). In this the following is taken for nical power losses NV (for example in the
Equation (2.16) implies that the compres-
Sth: bearing seals) must be considered:
sion k attainable with a Roots pump must
always be less than the grading kth Ntot = Ncompression + ∑ NV (2.19)
Sth = 2050 – 2.5 % = 2000 m3/h
between Roots pump and backing pump The power losses summarized in NV are –
since volumetric efficiency is always < 1. The method outlined above may also be as shown by experience – approximately
When combining equations (2.13) and applied to arrangements which consist of a proportional to Sth, i.e.:
(2.16) one obtains for the efficiency the rotary pump as the backing pump and
well known expression several Roots pumps connected in series, ∑ Nv = const · Sth (2.20)
k0 for example. Initially one determines – in
η= Depending on the type of pump and its
ko + k th (2.17) line with an iteration method – the
design the value of the constant ranges
pumping characteristic of the backing
between 0.5 and 2 Wh / m3 .
pump plus the first Roots pump and then
The characteristic quantities to be found in The total power is thus:
considers this combination as the backing
equation 2.17 are only for the combination
pump for the second Roots pump and so Ntot = Sth (pv – pa + const.)
of the Roots pump and the backing pump,
on. Of course it is required that the
namely maximum compression k0 of the
theoretical pumping speed of all pumps of The corresponding numerical value equa-
Roots pump and gradation kth between
the arrangement be known and that the tion which is useful for calculations is:
Roots pump and backing pump.
compression at zero throughput k0 as a
With the aid of the above equations the function of the backing pressure is also Ntot = Sth (pv – pa + const.) · 3 · 10-2 Watt
pumping speed curve of a given combi- known. As already stated, it depends on (2.21)
nation of Roots pump and backing pump the vacuum process which grading will be
may be calculated. For this the following with pv, pa in mbar, Sth in m3 / h and
most suitable. It may be an advantage
must be known: when backing pump and Roots pump both the constant “const.” being between
a) the theoretical pumping speed of the have the same pumping speed in the 18 and 72 mbar.
Roots pump: Sth rough vacuum range.

Forevacuum Pumping speed kth = Sth / Sv k0 (pv) of η = k0 / k0+kth Intake pressure


pressure Sv of the = 2001/Sv the RUVAC (Volumetric. Seff = η Sth pa = pv · Sv / Seff
Pv E 250 WA 2001 efficiency) (equation 2.14)

100 250 8.0 12.5 0.61 1.220 21

40 250 8.0 18 0.69 1.380 7.2

10 250 8.0 33 0.8 1.600 1.6

5 250 8.0 42 0.84 1.680 0.75

1 250 8.0 41 0.84 1.680 0.15

5 · 10–1 220 9.1 35 0.79 1.580 7 · 10–2

1 · 10–1 120 16.6 23 0.6 1.200 1 · 10–2

4 · 10–2 30 67 18 0.21 420 3 · 10–3


↓ ↓

The values taken from the two right-hand columns give point by point the pumping speed curve for Pumping speed characteristic
the combination WA 2001/E250 (see Fig. 2.19, topmost curve) for the combination
WA 2001 / E250
D00
Table 2.3

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Fundamentals of Vacuum Technology


Pumping speed S
Vacuum Generation

Intake pressure pa →

Fig. 2.19 Pumping speed curves for different pump combinations with the corresponding backing pumps

Load rating of a roots pump Integral leak tightness of this version is Maintaining the allowed pressure
The amount of power drawn by the pump < 10-4 mbar·l·s-1. difference
determines its temperature. If the tempe- In the case of standard Roots pumps,
In the case of better leak tightness
rature increases over a certain level, measures must be introduced to ensure
requirements of < 10-5 mbar·l·s-1 the
determined by the maximum permissible that the maximum permissible pressure
Roots pump is equipped with a canned
pressure difference pV – pa, the danger difference between intake and exhaust port
motor. The rotor is seated in the vacuum
exists that the rotors may seize in the due to design constraints is not exceeded.
on the drive shaft of the pump and is
casing due to their thermal expansion. The This is done either by a pressure switch,
separated from the stator by a vacuum-
maximum permissible pressure difference which cuts the Roots pump in and out
tight non-magnetic tube. The stator coils
∆pmax is influenced by the following fac- depending on the intake pressure, or by
are cooled by a fan having its own drive
tors: forevacuum or compression pressure using a pressure difference or overflow
motor. Thus shaft seals which might be
pV, pumping speed of the backing pump valve in the bypass of the Roots pumps
subject to wear are no longer required. The
SV, speed of the Roots pump n, gradation (Fig. 2.20 and 2.21). The use of an
use of Roots pumps equipped with canned
kth and the adiabatic exponent κ of the overflow valve in the bypass of the Roots
motors is especially recommended when
pumped gas. ∆pmax increases when pV pump is the better and more reliable
pumping high purity-, toxic- or radioactive
and SV increase and decreases when n and solution. The weight and spring loaded
gases and vapors.
kth increase. Thus the maximum difference valve is set to the maximum permissible
between forevacuum pressure and intake
pressure, pV – pa must – during conti-
nuous operation – not exceed a certain
value depending on the type of pump.
Such values are in the range between 130
and 50 mbar. However, the maximum
permissible pressure difference for conti-
nuous operation may be exceed for brief WAU 2001
periods. In the case of special designs,
which use gas cooling, for example, high
pressure differences are also permissible
during continuous operation.

Types of motors used with roots pumps SOGEVAC SV 1200


Standard flange-mounted motors are used
as the drive. The shaft feedthroughs are
sealed by two oil sealed radial shaft seals
running on a wear resistant bushing in
order to protect the drive shaft. Flange
motors of any protection class, voltage or Fig. 2.20 Cross section of a Roots pumps with Fig. 2.21 Vacuum diagram – Roots pump with integra-
bypass line ted bypass line and backing pump
frequency may be used.

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Vacuum Generation Fundamentals of Vacuum Technology

1 a

4 b
4 Z
P
Z
P
3 Z
P
c

1 Intake port
2 Discharge port
3 Gas cooler 1 Rotors 4 Exhaust slot
4 Flow of cold gas 2 Compression 5 Intake slot
chamber 6 Intermediate stage purge
Fig. 2.24 Arrangement of the pumps and guiding of
3 Intake space gas
Fig. 2.22 Diagram of a Roots pump with pre-admis- the gas flow. P = Pump stage Z = Interme-
sion cooling Fig. 2.23 Principle of operation diate ring

pressure difference of the particular pump. the case of single-stage compression is work cycle in position a, the right rotor just
This ensures that the Roots pump is not taken from the atmosphere and admitted opens the intake slot (5). Gas now flows
overloaded and that it may be operated in from the pre-admission cooler, and which into the continually increasing intake space
any pressure range. In practice this means in the case of multi-stage pump systems is (3) in position b until the right rotor seals
that the Roots pump can be switched on, taken from downstream gas coolers, off the intake slot (5) in position c. After
together with the backing pump, at performs a pre-compression and removes both claws have passed through the center
atmospheric pressure. In the process any by “inner cooling” the heat of compression position, the gas which has entered is then
pressure increases will not adversely affect at the point of time it occurs. compressed in the compression chamber
combined operation, i.e. the Roots pump (2) (position a) so long until the left rotor
is not switched off in such circumstances. releases the discharge slot (4) (position b)
2.1.3.2 Claw pumps thereby discharging the gas. Immediately
Pre-admission cooling (Fig. 2.22) after the compression process has started
Like Roots pumps, claw pumps belong to
In the case of Roots pumps with pre- (position a) the intake slot (5) is opened
the group of dry compressing rotary
admission cooling, the compression pro- simultaneously and gas again flows into
piston vacuum pumps (or rotary vacuum
cess basically is the same as that of a nor- the forming intake space (3) (position b).
pumps). These pumps may have several
mal Roots pump. Since greater pressure Influx and discharge of the gas is
stages; their rotors have the shape of
differences are allowed more installed performed during two half periods. Each
claws.
power is needed, which at the given speed rotor turns twice during a full work cycle.
and the pressure difference between inlet The design principle of a claw pump is Located between the pumping stages are
and discharge port is directly proportional explained by first using an example of a intermediate discs with flow channels
and is composed of the theoretical work four-stage design. The cross section inside which run from the discharge side of the
done on compression and various power the pump’s casing has the shape of two upper stage to the intake side of the next
losses. The compression process ends partly overlapping cylinders (Fig. 2.23). stage, so that all inlet or exhaust sides are
normally after opening of the pumping Within these cylinders there are two freely arranged vertically above each other (Fig.
chamber in the direction of the discharge rotating rotors in each pump stage: (1) 2.24). Whereas in a Roots pump the in-
port. At this moment warmed gas at higher with their claws and the matching recesses coming gas is pumped through the pump
pressure flows into the pumping chamber rotating in opposing directions about their at a constant volume and compression is
and compresses the transported volume of vertical axes. The rotors are synchronized only performed in the forevacuum line
gas. This compression process is perfor- by a gear just like a Roots pump. In order (see Section 2.1.3.1), the claw pump
med in advance in the case of pre-admis- to attain an optimum seal, the clearance compresses the gas already within the
sion cooling. Before the rotor opens the between the rotor at the center of the pumping chamber until the rotor releases
pumping chamber in the direction of the casing and the amount of clearance with the discharge slot. Shown in Fig. 2.25 are
discharge port, compressed and cooled respect to the inside casing wall is very the average pressure conditions in the
gas flows into the pumping chamber via small; both are in the order of magnitude individual pumping stages of a DRYVAC at
the pre-admission channel. Finally the
rotors eject the pumped medium via the
of a few 0.01 mm. The rotors periodically
open and close the intake and discharge
an intake pressure of 1 mbar. In order to
meet widely differing requirements
D00
discharge port. The cooled gas, which in slots (5) and (4). At the beginning of the LEYBOLD manufactures two different

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Fundamentals of Vacuum Technology Vacuum Generation

IN 1 mbar OUT P P
Stage 1 W Compr. W Compr.
3 mbar 1 1 2
2

IN 3 mbar OUT 15 mbar Stage 2

IN 15 mbar OUT 150 mbar Stage 3


3

IN 150 mbar OUT 1000 mbar Stage 4 4 3

V V

Fig. 2.27 Compression curve for a claw pump without


Fig. 2.26 Compression curve for a claw pump with internal compression
Fig. 2.25 Pressures in pump stages 1 to 4 internal compression (“isochoric compression”)

series of claw pumps, which chiefly differ which is applied from the outside after 2.1.3.2.1 Claw pumps with internal
in the type of compression process used: completion of the intake process. This is compression for the
1) Pumps with internal compression, similar to the admission of a gas ballast semiconductor industry
multi-stage for the semiconductor when opening the gas ballast valve after (“DRYVAC series”)
industry (DRYVAC Series) and completion of the intake phase. From the
2) Pumps without internal compression, diagram it is apparent that in the case of Design of DRYVAC Pumps
two-stage for chemistry applications isochoric compression the work done on Due to the work done on compression in
(“ALL·ex”). compression must be increased, but cold the individual pumping stages, multi-stage
gas instead of hot exhaust gas is used for claw pumps require water cooling for the
Figs. 2.26 and 2.27 demonstrate the
venting. This method of direct gas cooling four stages to remove the compression
differences in design. Shown is the course
results in considerably reduced rotor heat. Whereas the pumping chamber of
of the pressure as a function of the volume
temperatures. Pumps of this kind are dis- the pump is free of sealants and lubri-
of the pumping chamber by way of a pV
cussed as “ALL·ex” in Section 2.1.3.2.2. cants, the gear and the lower pump shaft
diagram.
are lubricated with perfluoropolyether
Fig. 2.26 shows the (polytropic) course of (PFPE). The gear box is virtually herme-
the compression for pumps with internal tically sealed from the pumping chamber
compression. The pressure increases until by piston rings and a radial shaft seal. The
the discharge slot is opened. If at that bearings in the upper end disk are
point the exhaust back pressure has not lubricated with PFPE grease. In order to
been reached, the compression space is protect the bearings and shaft seals
suddenly vented with hot exhaust gas. As against aggressive substances, a barrier
1
the volume is reduced further, the gas at gas facility is provided. A controlled water
exhaust pressure is ejected. The work 2 cooling system allows the control of the
done on compression is represented by casing temperature over a wide range as
the area under the p-v curve 1-2-3-4. It is the pump is subjected to differing gas
almost completely converted into heat. In loads coming from the process. The four
the case of dry compressing vacuum stage design is available in several
pumps not much of this heat can be lost to pumping speed and equipment grades of
3
the cooled casing due to the low density of 25, 50 and 100 m3/h DRYVAC pumps:
the gas. This results in high gas tempe- a) as the basic version for non-aggressive
ratures within the pump. Experiences with clean processes: DRYVAC 25 B, 50 B
claw pumps show that the highest tem- and 100 B (Fig. 2.29a)
peratures occur at the rotors. b) as a version for semiconductor
processes: DRYVAC 25 P, 50 P and
Shown in Fig. 2.27 is the principle of 100 P (Fig. 2.29b)
isochoric compression in a p-v diagram. 1 Intake port
c) as a system version with integrated self
Here the compression is not performed by 2 Front panel / electronics
3 Main switch monitoring: DRYVAC 50 S and 100 S
reducing the volume of the pumping d) as a system version with integrated self
chamber, but by venting with cold gas Fig. 2.28 DRYVAC pump

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Vacuum Generation Fundamentals of Vacuum Technology

Casing Intake Intake


Casing
suction line line
suction
Cooling 100 P only Cooling
water water

Exhaust Exhaust
line line

Inert
gas

Fig. 2.29a Vacuum diagram for the DRYVAC B Fig. 2.29b Vacuum diagram for the DRYVAC P Fig. 2.29c Vacuum diagram for the DRYVAC S

monitoring offering an increased need to meet a variety of special require- strongly on their size. The mean velocity
pumping speed in the lower pressure ments. In semiconductor processes, as in (VGas) of the flowing gas during the
range: DRYVAC 251 S and 501 S (Fig. many other vacuum applications, the compression phase is given by the
2.29c) formation of particles and dusts during the following equation:
process and/or in the course of compres- q pV mbar · `· s −1
The ultimate pressure attainable with the
sing the pumped substances to atmos- v = · =
DRYVAC 251 S or 501 S is – compared to Gas p · A mbar · cm2
pheric pressure within the pump, is una- (2.22)
the versions without integrated Roots 10 · q pV m
voidable. In the case of vacuum pumps = ·
pump – by approximately one order of p·A s
operating on the claw principle it is
magnitude lower (from 2·10-2 mbar to
possible to convey particles through the
3·10-3 mbar) and the attainable throughput qpV = gas throughput
pump by means of so called “pneumatic
is also considerably increased. It is of
conveying”. This prevents the deposition p = pressure
course possible to directly flange mount
of particles and thus the formation of A = surface area
LEYBOLD RUVAC pumps on to the
layers within the pump and reduces the
DRYVAC models (in the case of semi- One can see that with increasing pressure
risk that the claw rotor may seize. Care
conductor processes also mostly with a the velocity of the pumped gas flow slows
must be taken to ensure that the velocity of
PFPE oil filling for the bearing chambers). down and attains the order of magnitude
the gas flow within the individual pumping
of the settling speed of the particles in the
The pumps of the DRYVAC family are the stages is at all times greater than the
gas flow (Fig. 2.32). This means that the
classic dry compressing claw vacuum settling speed of the particles entrained in
risk of depositing particles in the operating
pumps that are preferably used in the se- the gas flow. As can be seen in Fig. 2.31,
chamber of the pump and the resulting
miconductor industry, whereby the pumps the settling speed of the particles depends

To be provided by the customer Stage 2 Stage 3 Stage 4


2 500 mbar·l/s 8 300 mbar·l/s 20 000 mbar·l/s

TSH Temperature switch

PSL Pressure switch Particle size

PSH Pressure switch


Gas velocity
Limit speed

FSL Flow switch


Throughput in
MPS Motor protection switch mbar·l/s

PT 100 Temperature sensor


Throughput cross sec-
For DRYVAC with LIMS
tion 6.5 cm2, constant
Pressure
CS Current sensor

EPS Exhaust pressure sensor


Pressure
Fig. 2.32 Mean gas velocity vg during compression
D00
Fig. 2.31 Settling speed as a function of pressure p. without purge gas (left) and with purge gas
Fig. 2.30 Key to Figures 2.29a – 2.29c Parameter: particle size (right) in stages 2, 3 and 4

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Fundamentals of Vacuum Technology Vacuum Generation

mbar
Ultimate pressure

Pumping speed
Stage 2 2 500 mbar · l/s
Stage 3 8 300 mbar · l/s
Stage 4 20 000 mbar · l/s
Purge gas flow

Pressure
Fig. 2.33 Ultimate pressure of the DRYVAC 100S as a function of pure gas flow
in stages 2 – 4 Fig. 2.34 Pumping speed with and without purge gas

impairment increases with increasing ate discs to the exhaust, it is possible to method several effects can be noted:
pressure. In parallel to this the potential reduce the influence of the purge gas on • The admitted purge gas dilutes the
for the formation of particles from the the ultimate pressure to a minimum. Test pumped mixture of substances, par-
gaseous phase increases at increasing results (Fig. 2.33) indicate that the in- ticle-forming reactions will not occur, or
compression levels. In order to keep the fluence of purge gas in the fourth stage is are at least delayed.
size of the forming particles small and thus – as to be expected – of the lowest level • The risk of an explosion through self-
their settling speed low and to maintain a since there are located between this stage igniting substances is significantly
high velocity for the gas, an additional and the intake side the three other pum- reduced.
quantity of gas is supplied into the pump ping stages. The admission of purge gas • Particles which have formed are con-
via the individual intermediate discs (purge via the second and third stages (Fig. 2.33) veyed pneumatically through the pump
gas). For this, the inflowing quantity of has a comparatively small influence on the • Losses in pumping speed and a reduc-
purge gas is matched to the pressure ultimate pressure as can be seen from the tion in ultimate pressure can be kept
conditions prevailing in the individual pumping speed curve in Fig. 2.34. Finally it very small due to the special way in
pumping stages (see top right part of Fig. can be said that the formation of particles which the gas is made to pass through
2.32). This keeps the velocity of the gas is to be expected in most CVD processes. the pump.
flow high enough within the entire pump When using dry compressing claws
by so-called pneumatic pumping. Through vacuum pumps, the controlled admission
the way in which the gas is lead within the of purge gas via the individual intermediate
pump, i.e. from the intake through the four discs is the best approach to avoid the
pumping stages with the related intermedi- formation of layers. When applying this

Intake port
Motor

1st stage
Claws
2nd stage

Coupling
Axial face seals

Gear, complete
with shafts and
bearings

Fig. 2.35 Simple arrangement of the dry compression “ALL·ex” pump

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Vacuum Generation Fundamentals of Vacuum Technology

2.1.3.2.2 Claw pumps without internal view of protection against internal explo-
compression for chemistry sions, something which was also taken
applications (“ALL·ex” ) into account by direct cooling with cold
gas (see operating principle). A special Cooling gas
The chemical industry requires vacuum
feature of the “ALL·ex” is that both shafts
pumps which are highly reliable and which
have their bearings exclusively in the gear.
do not produce waste materials such as
On the pumping side, the shafts are free
contaminated waste oil or waste water. If
(cantilevered). This simple design allows
this can be done, the operating costs of
the user to quickly disassemble the pump
such a vacuum pump are low in view of
for cleaning and servicing without the Exhaust gas
the measures otherwise required for pro-
need for special tools.
tecting the environment (disposal of waste
oil and water, for example). For operation In order to ensure a proper seal against
of the simple and rugged “ALL·ex” pump the process medium in the pumping Fig. 2.37 Circulation of the cold gas in the “ALL·ex”
from LEYBOLD there are no restrictions as chamber the shaft seal is of the axial face with cooler / condenser
to the vapor flow or the pressure range seal type – a sealing concept well proven
during continuous operation. The “ALL·ex” in chemistry applications. This type of seal
rotor. The process gas then flows into the
may be operated within the entire pressure is capable of sealing liquids against
intake chamber which increases in size. The
range from 5 to 1000 mbar without liquids, so that the pump becomes
intake process is caused by the pressure
restrictions. rinseable and insensitive to forming
gradient produced by increasing the
condensate. Fig. 2.36 shows the compo-
volume of the pumping chamber. The
Design of the “ALL·ex” pump nents supplied with the “ALL·ex”, together
maximum volume is attained after 3/4 of a
The design of the two-stage “ALL·ex” is with a gas cooler and a receiver.
revolution of the rotors (Fig. 2.38-2). After
shown schematically in Fig. 2.35. The gas
the end of the intake process, the control
flows from top to bottom through the Operating principle
edge of the left rotor opens the cold gas
vertically arranged pumping stages in Isochoric compression, which also serves
inlet and at the same time the control edge
order to facilitate the ejection of con- the purpose of limiting the temperature
of the right rotor opens the intake slot (Fig.
densates and rinsing liquids which may ultimately attained during compression,
2.38-3) once more. In Fig. 2.38-4 the
have formed. The casing of the pump is especially in the stage on the side of the
control edge of the left rotor terminates the
water cooled and permits cooling of the atmosphere, and which ensures protection
discharge of the gas which has been
first stage. There is no sealed link between against internal explosions, is performed
compressed to 1000 mbar with the cold
gas chamber and cooling channel so that by venting the pumping chamber with cold
gas; at the same time the control edge of
the entry of cooling water into the gas from a closed refrigerating gas cycle
the right rotor completes an intake process
pumping chamber can be excluded. The (Fig. 2.37). Fig. 2.38-1 indicates the start of
again.
pressure-burst resistant design of the the intake process by opening the intake
entire unit underlines the safety concept in slot through the control edge of the right The total emissions from the system are

1
3

1000
4

m
3 . h-1
2
5
Saugvermˆgen

100
Pumping speed

6
10
7 8
6
4
2

1 2 4 6 8
1 10 100 mbar 1000
Intake pressure
Ansaugdruck
1 Motor 5 Exhaust cooler
2
3
4
Pump
Intake port
Exhaust port
6 Cooling water
connection
7 Cooling receiver
D00
Fig. 2.36 “ALL·ex” pump Fig. 2.39 Pumping speed characteristic of an ALL·ex” 250

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Fundamentals of Vacuum Technology Vacuum Generation

Vmax

Exhaust slot Intake


Volume of the pump slot
chamber starts to increase
1
Suction
Cold gas inlet Vmin
100 1000 Pmbar
(10) (100)

Vmax

Volume of the pump


chamber at maximum
2
End of suction
Vmin
100 1000 Pmbar
(10) (100)

Cold gas inlet


Vmax

Volume of the pump chamber


stars to decrease (without
compression). Pressure
increase to 1000 mbar
3 only by admitting cold gas.

Vmin

Beginning of admitting cold gas 100 1000 Pmbar


(10) (100)

Vmax

Ejection of the mixture Exhaust slot


composed of sucked
in gas and cold gas.
4
Cold gas inlet Vmin
100 1000 Pmbar
(10) (100)

Fig. 2.38 Diagrams illustrating the pumping principle of the ALL·ex” pump (claw pump without inner compression)

not increased by the large quantities of cold solvent recovery. The method of direct gas ly. The rinsing liquids are usually applied to
gas, since a closed refrigerating cycle is cooling, i.e. venting of the pumping cham- the pump after completion of the connec-
maintained by way of an externally arran- ber with cold gas supplied from outside ted process (batch operation) or while the
ged gas cooler and condenser (Fig. 2.37). (instead of hot exhaust gas) results in the process is in progress during brief blocking
The hot exhaust gas is made to pass case of the “ALL·ex” in rotor temperatures phases. Even while the “ALL·ex” is at
through the cooler and is partly returned in which are so low that mixtures of substa- standstill and while the pumping chamber
the form of cold gas for pre-admission nces rated as ExT3 can be pumped reliably is completely filled with liquid it is possible
cooling into the pump. The pump takes in under all operating conditions. The to start this pump up. Shown in Fig. 2.39 is
the quantity of cold process gas needed for “ALL·ex” thus fully meets the requirements the pumping speed characteristic of an
venting the pumping chamber back into the of the chemical industry concerning the “ALL·ex” 250. This pump has a nominal
compression space on its own. This pro- protection against internal explosions. A pumping speed of 250 m3/h and an
cess, however, has no influence on the certain degree of liquid compatibility makes ultimate pressure of < 10 mbar. At
pumping speed of the “ALL·ex” because the the “ALL·ex” rinseable, thus avoiding the 10 mbar it still has a pumping speed of
intake process has already ended when the formation of layers in the pump, for examp- 100 m3/h. The continuous operating
venting process starts. Designing the le, or the capability of dissolving layers pressure of the pump may be as high as
cooler as a condenser allows for simple which may already have formed respective- 1000 mbar; it consumes 13.5 kW of
electric power.

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Vacuum Generation Fundamentals of Vacuum Technology

2.1.4 Accessories for Elimination of oil vapor


oil-sealed rotary The attainable ultimate pressure with oil-
sealed rotary pumps is strongly influenced
displacement pumps by water vapor and hydrocarbons from the
During a vacuum process, substances pump oil. Even with two-stage rotary vane
harmful to rotary pumps can be present in pumps, a small amount of back-streaming
a vacuum chamber. of these molecules from the pump interior
into the vacuum chamber cannot be
Elimination of water vapor avoided. For the production of hydrocar-
Water vapor arises in wet vacuum proces- bon-free high and ultrahigh vacuum, for
ses. This can cause water to be deposited example, with sputter-ion or turbomolecu-
in the inlet line. If this condensate reaches lar pumps, a vacuum as free as possible of
the inlet port of the pump, contamination oil is also necessary on the forevacuum
of the pump oil can result. The pumping side of these pumps. To obtain this, me-
performance of oil-sealed pumps can be dium vacuum adsorption traps (see Fig.
significantly impaired in this way. More- 2.40) filled with a suitable adsorption
over, water vapor discharged through the material (e.g., LINDE molecular sieve 13X)
outlet valve of the pump can condense in are installed in the inlet line of such oil-
the discharge outlet line. The condensate sealed forepumps. The mode of action of a
can, if the outlet line is not correctly ar- sorption trap is similar to that of an ad-
ranged, run down and reach the interior of sorption pump. For further details, see
the pump through the discharge outlet Section 2.1.8. If foreline adsorption traps
valve. Therefore, in the presence of water are installed in the inlet line of oil-sealed
vapor and other vapors, the use of rotary vane pumps in continuous opera-
condensate traps is strongly recommen- tion, two adsorption traps in parallel are
ded. If no discharge outlet line is connec- recommended, each separated by valves.
ted to the gas ballast pump (e.g., with Experience shows that the zeolite used as
the adsorption material loses much of its 1 Housing
smaller rotary vane pumps), the use of 2 Basket holding the sieve
discharge filters is recommended. These adsorption capacity after about 10 – 14 3 Molecular sieve (filling)
catch the oil mist discharged from the days of running time, after which the 4 Sealing flanges
pump. other, now-regenerated, adsorption trap 5 Intake port with small flange
can be utilized; hence the process can 6 Upper section
Some pumps have easily exchangeable fil- continue uninterrupted. By heating the
7 Vessel for the heater or refrigerant
ter cartridges that not only hold back oil 8 Connection on the side of the pump with
adsorption trap, which is now not connec- small flange
mist, but clean the circulating pump oil. ted in the pumping line, the vapors
Whenever the amount of water vapor pre- escaping from the surface of the zeolite
sent is greater than the water vapor tole- can be most conveniently pumped away Fig. 2.40 Cross section of a medium vacuum
rance of the pump, a condenser should with an auxiliary pump. In operation, pum- adsorption trap
always be installed between the vessel and ping by the gas ballast pump generally
the pump. (For further details, see Section leads to a covering of the zeolite in the
2.1.5)
2.1.5 Condensers
other, unheated adsorption trap and thus
to a premature reduction of the adsorption For pumping larger quantities of water
Elimination of dust capacity of this trap. vapor, the condenser is the most econo-
Solid impurities, such as dust and grit, mical pump. As a rule, the condenser is
significantly increase the wear on the Reduction of the effective pumping cooled with water of such temperature that
pistons and the surfaces in the interior of speed the condenser temperature lies sufficiently
the pump housing. If there is a danger that All filters, separators, condensers, and below the dew point of the water vapor and
such impurities can enter the pump, a dust valves in the inlet line reduce the effective an economical condensation or pumping
separator or a dust filter should be in- pumping speed of the pump. On the basis action is guaranteed. For cooling, however,
stalled in the inlet line of the pump. Today of the values of the conductances or media such as brine and refrigerants (NH3,
not only conventional filters having fairly resistances normally supplied by Freon) can also be used.
large casings and matching filter inserts manufacturers, the actual pumping speed When pumping water vapor in a large
are available, but also fine mesh filters of the pump can be calculated. For further industrial plant, a certain quantity of air is
which are mounted in the centering ring of details, see Section 1.5.2. always involved, which is either contained
the small flange. If required, it is recom- in the vapor or originates from leaks in the
mended to widen the cross section with KF
adaptors.
plant (the following considerations for air
and water vapor obviously apply also in D00
general for vapors other than water vapor).
Therefore, the condenser must be backed

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Fundamentals of Vacuum Technology Vacuum Generation

of the gas ballast pump – should not condenser, the water vapor pressure pD2 at
(when the quantity of permanent gas the exit of the condenser is always lower
described in more detail in Section than that at the entrance; for (2.23) to be
2.2.3 is not pumped simultaneously) be fulfilled, the partial pressure of air pp2 at
greater than the water vapor tolerance the exit must be higher than at the
for the gas ballast pump involved. If – entrance pp1, (see Fig. 2.43), even when
as cannot always be avoided in practice no throttle is present.
– a higher water vapor partial pressure
The higher air partial pressure pp2 at the
is to be expected at the condenser exit,
condenser exit is produced by an accumu-
it is convenient to insert a throttle bet-
1 Inlet of the condenser lation of air, which, as long as it is present
2 Discharge of the condenser ween the condenser exit and the inlet
at the exit, results in a stationary flow
3 See text port of the gas ballast pump. The
equilibrium. From this accumulation of air,
conductance of this throttle should be
the (eventually throttled) gas ballast pump
variable and regulated (see Section
Fig. 2.41 Condenser (I) with downstream gas ballast in equilibrium removes just so much as
pump (II) for pumping of large quantities of 1.5.2) so that, with full throttling, the
streams from the entrance (1) through the
water vapor in the rough vacuum range (III) pressure at the inlet port of the gas
– adjustable throttle
condenser.
ballast pump cannot become higher
than the water vapor tolerance. Also, All calculations are based on (2.23a) for
by a gas ballast pump (see Fig. 2.41) and the use of other refrigerants or a de- which, however, information on the
hence always works – like the Roots pump crease of the cooling water temperature quantity of pumped vapors and permanent
– in a combination. The gas ballast pump may often permit the water vapor pres- gases, the composition, and the pressure
has the function of pumping the fraction of sure to fall below the required value. should be available. The size of the
air, which is often only a small part of the condenser and gas ballast pump can be
For a mathematical evaluation of the
water-vapor mixture concerned, without calculated, where these two quantities are,
combination of condenser and gas ballast
simultaneously pumping much water indeed, not mutually independent. Fig. 2.42
pump, it can be assumed that no loss of
vapor. It is, therefore, understandable that, represents the result of such a calculation
pressure occurs in the condenser, that the
within the combination of condenser and as an example of a condenser having a
total pressure at the condenser entrance
gas ballast pump in the stationary con- condensation surface of 1 m2, and at an
ptot 1, is equal to the total pressure at the
dition, the ratios of flow, which occur in the inlet pressure pv1, of 40 mbar, a
condenser exit, ptot 2:
region of rough vacuum, are not easily condensation capacity that amounts to
assessed without further consideration. ptot 1 = ptot 2 (2.23) 15 kg / h of pure water vapor if the fraction
The simple application of the continuity of the permanent gases is very small. 1 m3
The total pressure consists of the sum of of cooling water is used per hour, at a line
equation is not adequate because one is no the partial pressure portions of the air pp
longer concerned with a source or sink-free overpressure of 3 bar and a temperature of
and the water vapor pv: 12 °C. The necessary pumping speed of the
field of flow (the condenser is, on the basis
of condensation processes, a sink). This is pp1 + pv1 = pp2 + pv2 (2.23a) gas ballast pump depends on the existing
emphasized especially at this point. In a operating conditions, particularly the size of
As a consequence of the action of the the condenser. Depending on the efficiency
practical case of “non-functioning” of the
condenser – gas ballast pump combination,
it might be unjustifiable to blame the
condenser for the failure.
Condensation capacity [kg · h-1]

In sizing the combination of condenser


and gas ballast pump, the following points P’v2
must be considered: Pv1 Pv2
a) the fraction of permanent gases (air)
pumped simultaneously with the water
vapor should not be too great. At partial P’p2
Pp2
pressures of air that are more than Pp1
about 5 % of the total pressure at the
exit of the condenser, a marked accu-
Intake pressure pD1
mulation of air is produced in front of
the condenser surfaces. The condenser Fig. 2.43 Schematic representation of the pressure dis-
then cannot reach its full capacity (See Fig. 2.42 Condensation capacity of the condenser tribution in the condenser. The full lines corre-
also the account in Section 2.2.3 on the (surface area available to condensation 1 m2) spond to the conditions in a condenser in
simultaneous pumping of gases and as a function of intake pressure pD1 of the which a small pressure drop takes place
water vapor. Curve a: Cooling water tempera- (ptot 2 < ptot 1). The dashed lines are those for
vapors).
ture 12 °C. Curve b: Temperature 25 °C. an ideal condenser (ptot 2 ≈ ptot 1). pD: Partial
b) the water vapor pressure at the Consumption in both cases 1 m3/h at 3 bar pressure of the water vapor, pL: Partial pressu-
condenser exit – that is, at the inlet side overpressure re of the air

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of the condenser, the water vapor partial front, but generally only behind the 2.1.6 Fluid-entrainment pumps
pressure pv2 lies more or less above the condenser.
saturation pressure pS which corresponds Basically, a distinction is made between
If the starting time of a process is shorter ejector pumps such as water jet pumps
to the temperature of the refrigerant. (By
than the total running time, technically the (17 mbar < p < 1013 mbar), vapor ejector
cooling with water at 12 °C, pS, would be
simplest method – the roughing and the vacuum pumps
15 mbar (see Table XIII in Section 9)).
Correspondingly, the partial air pressure
holding pump – is used. Processes with (10-3 mbar < p < 10-1 mbar) and diffusion
pp2 that prevails at the condenser exit also
strongly varying conditions require an pumps (p < 10-3 mbar). Ejector vacuum
adjustable throttle section and, if needed, pumps are used mainly for the production
varies. With a large condenser,
an adjustable air admittance. of medium vacuum. Diffusion pumps
pv2 ≈ pS, the air partial pressure pp,2 is thus
large, and because pp · V = const, the On the inlet side of the gas ballast pump a produce high and ultrahigh vacuum. Both
volume of air involved is small. Therefore, water vapor partial pressure pv2 is always types operate with a fast-moving stream of
only a relatively small gas ballast pump is present, which is at least as large as the pump fluid in vapor or liquid form (water
necessary. However, if the condenser is saturation vapor pressure of water at the jet as well as water vapor, oil or mercury
small, the opposite case arises: coolant temperature. This ideal case is vapor). The pumping mechanism of all
pv2 > pS · pp2, is small. Here a relatively realizable in practice only with a very large fluid-entrainment pumps is basically the
large gas ballast pump is required. Since condenser (see above). same. The pumped gas molecules are
the quantity of air involved during a removed from the vessel and enter into the
With a view to practice and from the stated pump fluid stream which expands after
pumping process that uses condensers is fundamental rules, consider the two
not necessarily constant but alternates passing through a nozzle. The molecules
following cases: of the pump fluid stream transfer by way
within more or less wide limits, the
considerations to be made are more 1. Pumping of permanent gases with of impact impulses to the gas molecules in
difficult. Therefore, it is necessary that the small amounts of water vapor. Here the the direction of the flow. Thus the gas
pumping speed of the gas ballast pump size of the condenser – gas ballast pump which is to be pumped is moved to a space
effective at the condenser can be regulated combination is decided on the basis of the having a higher pressure.
within certain limits. pumped-off permanent gas quantity. The In fluid-entrainment pumps corresponding
condenser function is merely to reduce the vapor pressures arise during operation
In practice, the following measures are
water vapor pressure at the inlet port of depending on the type of pump fluid and
usual:
the gas ballast pump to a value below the the temperature as well as the design of
a) A throttle section is placed between the
water vapor tolerance. the nozzle. In the case of oil diffusion
gas ballast pump and the condenser,
which can be short-circuited during 2. Pumping of water vapor with small pumps this may amount to 1 mbar in the
rough pumping. The flow resistance of amounts of permanent gases. Here, to boiling chamber. The backing pressure in
the throttle section must be adjustable make the condenser highly effective, as the pump must be low enough to allow the
so that the effective speed of the pump small as possible a partial pressure of the vapor to flow out. To ensure this, such
can be reduced to the required value. permanent gases in the condenser is pumps require corresponding backing
This value can be calculated using the sought. Even if the water vapor partial pumps, mostly of the mechanical type. The
equations given in Section 2.2.3. pressure in the condenser should be vapor jet cannot enter the vessel since it
b) Next to the large pump for rough pum- greater than the water vapor tolerance of condenses at the cooled outer walls of the
ping a holding pump with low speed is the gas ballast pump, a relatively small gas pump after having been ejected through
installed, which is of a size corres- ballast pump is, in general, sufficient with the nozzle.
ponding to the minimum prevailing gas the then required throttling to pump away Wolfgang Gaede was the first to realize
quantity. The objective of this holding the prevailing permanent gases. that gases at comparatively low pressure
pump is merely to maintain optimum can be pumped with the aid of a pump
Important note: During the process, if the
operating pressure during the process. fluid stream of essentially higher pressure
pressure in the condenser drops below the
c) The necessary quantity of air is ad- and that, therefore, the gas molecules
saturation vapor pressure of the conden-
mitted into the inlet line of the pump from a region of low total pressure move
sate (dependent on the cooling water
through a variable-leak valve. This into a region of high total pressure. This
temperature), the condenser must be
additional quantity of air acts like an apparently paradoxical state of affairs
blocked out or at least the collected
enlarged gas ballast, increasing the develops as the vapor stream is initially
condensate isolated. If this is not done, the
water vapor tolerance of the pump. entirely free of gas, so that the gases from
gas ballast pump again will pump out the
However, this measure usually results a region of higher partial gas pressure (the
vapor previously condensed in the
in reduced condenser capacity. More- vessel) can diffuse into a region of lower
condenser
over, the additional admitted quantity of partial gas pressure (the vapor stream).
air means additional power consump- This basic Gaede concept was used by
tion and (see Section 8.3.1.1) increased Langmuir (1915) in the construction of the
oil consumption. As the efficiency of the
condenser deteriorates with too great a
first modern diffusion pump. The first
diffusion pumps were mercury diffusion
D00
partial pressure of air in the condenser, pumps made of glass, later of metal. In the
the admission of air should not be in Sixties, mercury as the medium was
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Fundamentals of Vacuum Technology Vacuum Generation

almost completely replaced by oil. To generally with water. Smaller oil diffusion 2.1.6.1 (Oil) Diffusion pumps
obtain as high a vapor stream velocity as pumps can, however, also be cooled with
These pumps consist basically (see Fig.
possible, he allowed the vapor stream to an air stream because a low wall tempe-
2.44) of a pump body (3) with a cooled
emanate from a nozzle with supersonic rature is not so decisive to the efficiency as
wall (4) and a three- or four-stage nozzle
speed. The pump fluid vapor, which con- for mercury diffusion pumps. Oil diffusion
system (A – D). The oil serving as pump
stitutes the vapor jet, is condensed at the pumps can operate well with wall tempera-
fluid is in the boiler (2) and is vaporized
cooled wall of the pump housing, whereas tures of 30 °C, whereas the walls of mer-
from here by electrical heating (1). The
the transported gas is further compressed, cury diffusion pumps must be cooled to
pump fluid vapor streams through the
usually in one or more succeeding stages, 15 °C. To protect the pumps from the
riser tubes and emerges with supersonic
before it is removed by the backing pump. danger of failure of the cooling water –
speed from the ring-shaped nozzles (A –
The compression ratios, which can be insofar as the cooling-water coil is not
D). Thereafter the jet so-formed widens
obtained with fluid entrainment pumps, controlled by thermally operated protec-
like an umbrella and reaches the wall
are very high: if there is a pressure of 10-9 tive switching – a water circulation moni-
where condensation of the pump fluid
mbar at the inlet port of the fluid- tor should be installed in the cooling water
occurs. The liquid condensate flows
entrainment pump and a backing pressure circuit; hence, evaporation of the pump
downward as a thin film along the wall and
of 10-2 mbar, the pumped gas is com- fluid from the pump walls is avoided.
finally returns into the boiler. Because of
pressed by a factor of 107!
this spreading of the jet, the vapor density
Basically the ultimate pressure of fluid is relatively low. The diffusion of air or any
entrainment pumps is restricted by the pumped gases (or vapors) into the jet is so
value for the partial pressure of the fluid rapid that despite its high velocity the jet
used at the operating temperature of the
pump. In practice one tries to improve this
by introducing baffles or cold traps. These
are “condensers” between fluid entrain-
ment pump and vacuum chamber, so that
the ultimate pressure which can be
attained in the vacuum chamber is now
only limited by the partial pressure of the
fluid at the temperature of the baffle.
The various types of fluid entrainment
pumps are essentially distinguished by the
density of the pump fluid at the exit of the
top nozzle facing the high vacuum side of
the pump:
1. Low vapor density:
Diffusion pumps
Oil diffusion pumps
(Series: LEYBODIFF, DI and DIP)
Mercury diffusion pumps
2. High vapor density:
Vapor jet pumps
Water vapor pumps
Oil vapor jet pumps
Mercury vapor jet pumps
3. Combined
oil diffusion/ vapor jet pumps
4. Water jet pumps

Cooling of fluid entrainment pumps


The heater power that is continuously

H
supplied for vaporizing the pump fluid in 1 Heater 5 High vacuum flange A
2 Boiler 6 Gas molecules B
fluid-entrainment pumps must be dissipa- 3 Pump body 7 Vapor jet C Nozzles
ted by efficient cooling. The energy 4 Cooling coil 8 Backing vacuum connection D
required for pumping the gases and
vapors is minimal. The outside walls of the Fig. 2.44 Mode of operation of a diffusion pump
casing of diffusion pumps are cooled,

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Vacuum Generation Fundamentals of Vacuum Technology

becomes virtually completely saturated lowest diffusion stage, to allow the volatile To characterize the effectiveness of a
with the pumped medium. Therefore, over components to evaporate and be removed diffusion pump, the so called HO factor is
a wide pressure range diffusion pumps by the backing pump. Therefore, the re- defined. This is the ratio of the actually
have a high pumping speed. This is evaporating pump fluid consists of only obtained specific pumping speed to the
practically constant over the entire the less volatile components of the pump theoretical maximum possible specific
working region of the diffusion pump oil. pumping speed. In the case of diffusion
(≤ 10-3 mbar) because the air at these low pumps from LEYBOLD optimum values
pressures cannot influence the jet, so its Pumping speed are attained (of 0.3 for the smallest and up
course remains undisturbed. At higher The magnitude of the specific pumping to 0.55 for the larger pumps).
inlet pressures, the course of the jet is speed S of a diffusion pump – that is, the
The various oil diffusion pumps manufac-
altered. As a result, the pumping speed pumping speed per unit of area of the
tured by LEYBOLD differ in the following
decreases until, at about 10-1 mbar, it actual inlet surface – depends on several
design features (see Fig. 2.45 a and b).
becomes immeasurably small. parameters, including the position and
The forevacuum pressure also influences dimensions of the high vacuum stage, the a) LEYBODIFF series
the vapor jet and becomes detrimental if velocity of the pump fluid vapor, and the This series of pumps is equipped with a
its value exceeds a certain critical limit. mean molecular velocity -c of the gas being fractionating device. The various consti-
This limit is called maximum backing pumped (see equation 1.17 in Section tuents of the pump fluid are selected so
pressure or critical forepressure. The 1.1). With the aid of the kinetic theory of that the high vacuum nozzle is supplied
capacity of the chosen backing pump must gases, the maximum attainable specific only by the fraction of the pump fluid that
be such (see 2.3.2) that the amount of gas pumping speed at room temperature on has the lowest vapor pressure. This
discharged from the diffusion pump is pumping air is calculated to assures a particularly low ultimate pres-
pumped off without building up a backing Smax = 11.6 l · s-1 · cm-2. This is the spe- sure. Fractionating occurs because the
pressure that is near the maximum cific (molecular) flow conductance of the degassed oil first enters the outer part of
backing pressure or even exceeding it. intake area of the pump, resembling an the boiler, which serves the nozzle on the
aperture of the same surface area (see backing vacuum side. Here a part of the
The attainable ultimate pressure depends equation 1.30 in Section 1.5.3). Quite more volatile constituents evaporates.
on the construction of the pump, the vapor generally, diffusion pumps have a higher Hence the already purified pump fluid
pressure of the pump fluid used, the pumping speed for lighter gases compared reaches the intermediate part of the boiler,
maximum possible condensation of the to heavier gases. which serves the intermediate nozzle. Here
pump fluid, and the cleanliness of the
vessel. Moreover, backstreaming of the
pump fluid into the vessel should be
reduced as far as possible by suitable
baffles or cold traps (see Section 2.1.6.4).

Degassing of the pump oil


In oil diffusion pumps it is necessary for
the pump fluid to be degassed before it is
returned to the boiler. On heating of the
pump oil, decomposition products can
arise in the pump. Contamination from the
vessel can get into the pump or be
contained in the pump in the first place.
These constituents of the pump fluid can
significantly worsen the ultimate pressure
attainable by a diffusion pump, if they are
not kept away from the vessel. Therefore,
the pump fluid must be freed of these
1
impurities and from absorbed gases.
2
This is the function of the degassing
section, through which the circulating oil
passes shortly before re-entry into the a) LEYBODIFF-Pump with fractionating b) DI pump; side view on to the
boiler. In the degassing section, the most facility internal heater
volatile impurities escape. Degassing is 1 Center 1 Thermostat sensor
2 Middle section 2 Heating cartridge
obtained by the carefully controlled
temperature distribution in the pump. The
condensed pump fluid, which runs down
3 Outer part of the boiler
(fractionation) D00
the cooled walls as a thin film, is raised to Fig. 2.45 Diagram showing the basic differences in LEYBOLD oil diffusion pumps
a temperature of about 130 °C below the

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Fundamentals of Vacuum Technology Vacuum Generation

boiling. Those parts of the thermal


conductivity panels above the oil level
supply additional energy to the vapor.
Owing to the special design of the heating
system, the heater cartridges may be
exchanged also while the pump is still hot.

1 Nozzle (Laval) 2.1.6.2 Oil vapor ejector pumps


2 Diffuser nozzle (Venturi)
3 Mixing chamber The pumping action of a vapor ejector
4 Connection to the vacuum chamber stage is explained with the aid of Fig. 2.46.
The pump fluid enters under high pressure
Fig. 2.46 Operation of a vapor jet pump p1 the nozzle (1), constructed as a Laval
nozzle. There it is expanded to the inlet
the lighter constituents are evaporated in pressure p2. On this expansion, the
greater quantities than the heavier con- sudden change of energy is accompanied
stituents. When the oil enters the central by an increase of the velocity. The
region of the boiler, which serves the high consequently accelerated pump fluid
vacuum nozzle, it has already been freed of vapor jet streams through the mixer region
1 High vacuum port
the light volatile constituents. (3), which is connected to the vessel (4) 2 Diffusion stages
being evacuated. Here the gas molecules 3 Ejector stages
b) DI series emerging from the vessel are dragged
In these pumps an evaporation process for along with the vapor jet. The mixture, Fig. 2.47 Diagram of an oil jet (booster) pump
the pump fluid which is essentially free of pump fluid vapor – gas, now enters the
bursts is attained by the exceptional heater diffuser nozzle constructed as a Venturi The oil vapor ejector pumps used in
design resulting in a highly constant nozzle (2). Here the vapor – gas mixture is present-day vacuum technology have, in
pumping speed over time. The heater is of compressed to the backing pressure p3 general, one or more diffusion stages and
the internal type and consists of heating with simultaneous diminution of the several subsequent ejector stages. The
cartridges into which tubes with soldered velocity. The pump fluid vapor is then con- nozzle system of the booster is construc-
on thermal conductivity panels are densed at the pump walls, whereas the ted from two diffusion stages and two
introduced. The tubes made of stainless entrained gas is removed by the backing ejector stages in cascade (see Fig. 2.47).
steel are welded horizontally into the pump. Oil vapor ejector pumps are ideally The diffusion stages provide the high
pump’s body and are located above the oil suited for the pumping of larger quantities pumping speed between 10-4 and 10-3
level. The thermal conductivity panels of gas or vapor in the pressure region mbar (see Fig. 2.48), the ejector stages,
made of copper are only in part immersed between 1 and 10-3 mbar. The higher the high gas throughput at high pressures
in the pump fluid. Those parts of the density of the vapor stream in the nozzles (see Fig. 2.49) and the high critical backing
thermal conductivity panels are so rated ensures that the diffusion of the pumped pressure. Insensitivity to dust and vapors
that the pump fluid can evaporate gas in the vapor stream takes place much dissolved in the pump fluid is obtained by
intensively but without any retardation of more slowly than in diffusion pumps, so a spacious boiler and a large pump fluid
that only the outer layers of the vapor
stream are permeated by gas. Moreover,
the surface through which the diffusion
occurs is much smaller because of the
special construction of the nozzles. The
Pumping speed [Torr · l · s–1]

specific pumping speed of the vapor


Pumping speed [l · s–1]

Pumping speed [mbar ·l · s–1]

ejector pumps is, therefore, smaller than


that of the diffusion pumps. As the pum-
ped gas in the neighborhood of the jet
under the essentially higher inlet pressure
decisively influences the course of the flow
lines, optimum conditions are obtained
only at certain inlet pressures. Therefore,
the pumping speed does not remain con-
Intake pressure pa stant toward low inlet pressures. As a
Intake pressure pa
Fig. 2.48 Pumping speed of various vapor pumps as a consequence of the high vapor stream
function of intake pressure related to a nomi- velocity and density, oil vapor ejector
nal pumping speed of 1000 l/s. pumps can transport gases against a rela-
End of the working range of oil vapor ejector tively high backing pressure. Their critical Fig. 2.49 Pumping speed of various vapor pumps
pumps (A) and diffusion pumps (B) (derived from Fig. 2.48)
backing pressure lies at a few millibars.
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Vacuum Generation Fundamentals of Vacuum Technology

reservoir. Large quantities of impurities tion neither decomposes nor becomes sed at) the inner cooled surfaces of these
can be contained in the boiler without de- strongly oxidized when air is admitted. devices. Second, the condensation sur-
terioration of the pumping characteristics. However, at room temperature it has a faces must be so constructed and geome-
comparatively high vapor pressure of trically arranged that the flow conductance
10-3 mbar. If lower ultimate total pressures of the baffles or cold traps is as large as
2.1.6.3 Pump fluids are to be reached, cold traps with liquid possible for the pumped gas. These two
nitrogen are needed. With their aid, requirements are summarized by the term
a) Oils ultimate total pressures of 10-10 mbar can “optically opaque”. This means that the
The suitable pump fluids for oil diffusion be obtained with mercury diffusion pumps. particles cannot enter the baffle without
pumps are mineral oils, silicone oils, and Because mercury is toxic, as already hitting the wall, although the baffle has a
oils based on the polyphenyl ethers. mentioned, and because it presents a high conductance. The implementation of
Severe demands are placed on such oils hazard to the environment, it is nowadays this idea has resulted in a variety of
which are met only by special fluids. The hardly ever used as a pump fluid. designs that take into account one or the
properties of these, such as vapor pres- LEYBOLD supplies pumps with mercury as other requirement.
sure, thermal and chemical resistance, the pump fluid only on request. The vapor
particularly against air, determine the A cold cap baffle is constructed so that it
pressure curves of pump fluids are given in
choice of oil to be used in a given type of can be mounted immediately above the
Fig. 9.12, Section 9.
pump or to attain a given ultimate vacuum. high vacuum nozzle. The cold cap baffle is
The vapor pressure of the oils used in made of metal of high thermal conductivity
vapor pumps is lower than that of mer- 2.1.6.4 Pump fluid backstreaming and in good thermal contact with the cooled
cury. Organic pump fluids are more sen- its suppression (vapor pump wall, so that in practice it is main-
sitive in operation than mercury, because barriers, baffles) tained at the cooling-water temperature or,
the oils can be decomposed by long-term with air-cooled diffusion pumps, at ambi-
In the vapor stream from the topmost ent temperature. In larger types of pumps,
admission of air. Silicone oils, however,
nozzle of a diffusion pump, pump fluid the cold cap baffle is water cooled and
withstand longer lasting frequent admis-
molecules not only travel in the direction permanently attached to the pump body.
sions of air into the operational pump.
of streaming to the cooled pump wall, but The effective pumping speed of a diffusion
Typical mineral oils are DIFFELEN light, also have backward components of pump is reduced by about 10 % on
normal and ultra. The different types of velocity because of intermolecular colli- installation of the cold cap baffle, but the
DIFFELEN are close tolerance fractions of a sions. They can thus stream in the direc- oil backstreaming is reduced by about 90
high quality base product (see our cata- tion of the vessel. In the case of to 95 %.
log). LEYBODIFF and DI pumps, the oil-back-
streaming amounts to a few micrograms Shell baffles consist of concentrically
Silicone oils (DC 704, DC 705, for examp- arranged shells and a central baffle plate.
per minute for each square centimeter of
le) are uniform chemical compounds With appropriate cooling by water or
inlet cross-sectional area. To reduce this
(organic polymers). They are highly refrigeration, almost entirely oil vapor-free
backstreaming as much as possible,
resistant to oxidation in the case of air vacua can be produced by this means. The
various measures must be undertaken
inrushes and offer special thermal stability effective pumping speed of the diffusion
simultaneously:
characteristics. pump remains at least at 50 %, although
a) the high vacuum-side nozzle and the
DC 705 has an extremely low vapor pres- shape of the part of the pump body shell baffles are optically opaque. This type
sure and is thus suited for use in diffusion surrounding this nozzle must be of baffle has been developed by LEYBOLD
pumps which are used to attain extremely constructed so that as few as possible in two different forms: with a stainless-
low ultimate pressures of < 10-10 mbar. vapor molecules emerge sideways in steel cooling coil or – in the so-called
the path of the vapor stream from the Astrotorus baffles – with cooling inserts of
ULTRALEN is a polyphenylether. This fluid
nozzle exit to the cooled pump wall. copper. The casing of the former type is
is recommended in all those cases where a
b) the method for cooling the pump wall made entirely of stainless steel.
particularly oxidation-resistant pump fluid
must be used and where silicone oils must allow as complete as possible For the smaller air-cooled, oil diffusion
would interfere with the process. condensation of the pump fluid vapor pumps, plate baffles are used. The air-
and, after condensation, the fluid must cooled arrangement consists of a copper
APIEZON AP 201 is an oil of exceptional be able to drain away readily. plate with copper webs to the housing
thermal and chemical resistance capable c) one or more pump-fluid traps, baffles, wall. The temperature of the plate baffle
of delivering the required high pumping or cold traps must be inserted between remains nearly ambient during the
speed in connection with oil vapor ejector the pump and the vessel, depending on operation of the diffusion pump.
pumps operating in the medium vacuum the ultimate pressure that is required.
range. The attainable ultimate total pres-
Two chief requirements must be met in the Hydrocarbon-free vacuum
sure amounts to about 10-4 mbar.
If extreme demands are made on freedom
b) Mercury
construction of baffles or cold traps for oil
diffusion pumps. First, as far as possible, from oil vapor with vacuum produced by
oil diffusion pumps, cold traps should be
D00
Mercury is a very suitable pump fluid. It is all backstreaming pump-fluid vapor mole-
a chemical element that during vaporiza- cules should remain attached to (conden- used that are cooled with liquid nitrogen

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The temperature increase at the vessel Note:


containing the refrigerant is so slight over It must be noted that data on back-
the operating time that – as the liquid level streaming as specified in catalogs apply
drops – no significant desorption of the only to continuously-operated oil diffusion
condensate takes place. Located on the pumps. Shortly after starting a pump the
pumping side is an impact panel made of uppermost nozzle will not eject a well
copper. The low temperature of this panel directed vapor jet. Instead oil vapor
ensures that the greater part of the spreads in all directions for several se-
condensed pump fluid remains in the conds and the backstreaming effect is
liquid state and may drip back into the strong. When switching a diffusion pump
pump. Today the oils used to operate dif- on and off frequently the degree of oil
fusion pumps have a very low vapor pres- brackstreaming will be greater.
sure at room temperature (for example
DIFFELEN light, 2 · 10-8 mbar; DC 705,
4 · 10-10 mbar). The specified provisions 2.1.6.5 Water jet pumps and steam
with a liquid-nitrogen-cooled baffle or cold ejectors
trap would enable an absolutely oil-free
Included in the class of fluid-entrainment
vacuum to be produced.
pumps are not only pumps that use a fast-
In practice, however, complete suppres- streaming vapor as the pump fluid, but
sion of oil-backstreaming is never at- also liquid jet pumps. The simplest and
tained. There are always a few pump-fluid cheapest vacuum pumps are water jet
molecules that, as a result of collisions pumps. As in a vapor pump (see Fig. 2.46
with one another, reach the vessel without or 2.51), the liquid stream is first released
having hit one of the cooled surfaces of the from a nozzle and then, because of
baffle or the cold trap. Moreover, there are turbulence, mixes with the pumped gas in
1 Diffusion pump with cold
always a few highly volatile components of the mixing chamber. Finally, the movement
cap baffle (cooled by contact), the pump fluid that do not remain attached of the water – gas mixture is slowed down
2 Shell or chevron baffle to the very low temperature surfaces. The in a Venturi tube. The ultimate total
3 Anticreep barrier temperature and the vapor molecules
4 Sealing gasket
pressure in a container that is pumped by
5 Bearing ring
adsorbed at the surface of the vessel a water jet pump is determined by the
6 LN2 cold trap, determine exactly the pressure in the vapor pressure of the water and, for
7 Vacuum chamber vessel. If, the surfaces are not fully cove- example, at a water temperature of 15 °C
red with adsorbed pump-fluid molecules amounts to about 17 mbar.
Fig. 2.50 Schematic arrangement of baffle, anticreep after a bake-out process, their vapor
barrier and cold trap above a diffusion pump pressure contributes only insignificantly to Essentially higher pumping speeds and
the pressure in the vessel. lower ultimate pressures are produced by
steam ejector pumps. The section
so that they are maintained at a tempera- After a certain time, the “stay-down time”, through one stage is shown in Fig. 2.51.
ture of -196 °C. a continuous layer of oil molecules builds The markings correspond with those
Low-temperature baffles or cold traps up, and the ultimate pressure is practically shown in Fig. 2.46. In practice, several
should always be used with a cold cap in determined by the vapor pressure of the pumping stages are usually mounted in
place. On this the greatest part of the pump fluid at the temperature of the vessel cascade. For laboratory work, two-stage
backstreaming oil is condensed, so that walls. This “stay-down” time can even pump combinations are suitable and
the inevitable loss of pump fluid from the amount to several hours, indeed even to consist of a steam ejector stage and a
condensation of the pump fluid on the low- days, with the use of low-temperature water jet (backing) stage, both made of
temperature surface is kept at a minimum. baffles. glass. The water jet backing stage enables
With longer-term operation it is always ad- Oil can reach the vessel not only as vapor, operation without other backing pumps.
visable to install, in place of the cold cap, a but also as a liquid film, because oil wets With the help of a vapor stream at
water-cooled shell or chevron baffle readily and thus creeps up the wall. overpressure, the vacuum chamber can be
between the diffusion pump and the low- evacuated to an ultimate pressure of about
temperature baffle or cold trap (see Fig. By installation of an anticreep barrier (see 3 mbar. The condensate from the steam is
2.50). Fig. 2.50) made of Teflon polymer, a mate- led off through the drain attachment. The
rial that is not wetted by oil and can stand water jet stage of this pump is cooled with
LEYBOLD manufactures cold traps made a bake-out temperature up to 200 °C, water to increase its efficiency. Steam
of metal so called LN2 cold traps. These further creeping of the oil can be effecti- ejector pumps are especially suitable for
cold traps are to be used in those cases vely prevented. It is most appropriate to work in laboratories, particularly if very
where a cold trap is to be operated for arrange the anticreep barrier above the aggressive vapors are to be pumped.
prolonged periods of time without re- upper baffle (see Fig. 2.50). Steam ejector pumps, which will operate
quiring a filling facility for liquid nitrogen. at a pressure of a few millibars, are

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2.1.7 Turbomolecular pumps Whereas the dependence of the pumping


speed_ on the __ type of gas is fairly low
The principle of the molecular pump – well (S ∼ c ∼ 1 / EE M ), the dependence of the
known since 1913 – is that the gas par- compression k0 at zero throughput and
ticles to be pumped receive, through thus also the compression k, because
__
impact with the rapidly moving surfaces of of k0 ∼ eEM log k0 ∼ E M , is greater as
a rotor, an impulse in a required flow direc- shown by the experimentally-determined
tion. The surfaces of the rotor – usually relationship in Fig. 2.55.
disk-shaped – form, with the stationary
Example:
surfaces of a stator, intervening spaces in
which the gas is transported to the backing from theory it follows that
port. In the original Gaede molecular
pump and its modifications, the inter- log k0(He) 4 1 1
= = =
vening spaces (transport channels) were log k0(N2) 28 7 2.65
very narrow, which led to constructional ⇒ log k0(N 2) = 2.65 · log k0(He)
difficulties and a high degree of sus-
ceptibility to mechanical contamination.
this with k0 (He) = 3 · 103 from Fig. 2.55
At the end of the Fifties, it became possible results in:
– through a turbine-like design and by
modification of the ideas of Gaede – to log k0 (N2) = 2.65 · log (3 · 103) = 9.21
produce a technically viable pump the so- or k0 (N2) = 1.6 · 109.
called “turbomolecular pump”. The
spaces between the stator and the rotor This agrees – as expected – well (order of
disks were made in the order of magnitude) with the experimentally
1 Steam inlet millimeters, so that essentially larger determined value for k0 (N2) = 2.0 · 108
2 Jet nozzle tolerances could be obtained. Thereby, from Fig. 2.55. In view of the optimizations
3 Diffuser greater security in operation was achieved. for the individual rotor stages common
4 Mixing region today, this consideration is no longer
5 Connection to the vacuum chamber
However, a pumping effect of any
significance is only attained when the correct for the entire pump. Shown in Fig.
circumferential velocity (at the outside 2.56 are the values as measured for a
Fig. 2.51 Schematic representation of the operation rim) of the rotor blades reaches the order modern TURBOVAC 340 M.
of a steam ejector pump
of magnitude of the average thermal In order to meet the condition, a circumfe-
velocity of the molecules which are to be rential velocity for the rotor of the same
especially recommended for pumping pumped. Kinetic gas theory supplies for -c order of magnitude as -c high rotor speeds
laboratory distillation apparatus and of the equation 1.17: are required for turbomolecular pumps.
similar plants when the pressure from a They range from about 36,000 rpm for
simple water jet pump is insufficient. In 8· R ·T pumps having a large diameter rotor
c=
this instance, the use of rotary pumps π ·M (TURBOVAC 1000) to 72,000 rpm in the
would not be economical. case of smaller rotor diameters
in which the dependency on the type of gas (TURBOVAC 35 / 55). Such high speeds
Even in spite of their low investment costs
as a function of molar mass M is contained. naturally raise questions as to a reliable
water jet pumps and steam ejectors are
The calculation involving cgs-units bearing concept. LEYBOLD offers three
being replaced in the laboratories more
(where R = 83.14 · 106 mbar · cm3/mol · K) concepts, the advantages and disadvan-
and more by diaphragm pumps because of
results in the following Table: tages of which are detailed in the follo-
the environmental problems of using water
as the pump fluid. Solvent entering the Gas Molar Mean thermal wing:
water can only be removed again through Mass M velocity (m/s) • Oil lubrication / steel ball bearings
————————————–———— + Good compatibility with particles by
complex cleaning methods (distillation). H2 2 1761 circulating oil lubricant
He 4 1245 - Can only be installed vertically
H2O 18 587 + Low maintenance
Ne 20 557 • Grease lubrication / hybrid bearings
CO 28 471
+ Installation in any orientation
N2 28 471
+ Suited for mobile systems
Air 28.96 463
± Air cooling will do for many applica-
O2 32 440
tions
Ar
CO2
40
44
394
375
+ Lubricated for life (of the bearings) D00
CC13F (F11) 134.78 68
Table 2.4 -c as a function of molar mass M

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Fundamentals of Vacuum Technology Vacuum Generation

• Free of lubricants / magnetic suspen- Jülich” permitted the magnetic suspen- stages, whose blades have shorter radial
sion sion concept to spread widely. In this spans, where the gas is compressed to
+ No wear system the rotor is maintained in a stable backing pressure or rough vacuum pres-
+ No maintenance position without contact during operation, sure. The turbine rotor (6) is mounted on
+ Absolutely free of hydrocarbons by magnetic forces. Absolutely no lubri- the drive shaft, which is supported by two
+ Low noise and vibration levels cants are required. So-called touch down precision ball bearings (8 and 11), accom-
+ Installation in any orientation bearings are integrated for shutdown. modated in the motor housing. The rotor
shaft is directly driven by a medium-fre-
Steel ball bearings / hybrid ball bearings Fig. 2.52 shows a sectional drawing of a
quency motor housed in the forevacuum
(ceramic ball bearings): Even a brief tear typical turbomolecular pump. The pump is
space within the rotor, so that no rotary
in the thin lubricating film between the an axial flow compressor of vertical
shaft lead-through to the outside atmos-
balls and the races can – if the same type design, the active or pumping part of
phere is necessary. This motor is powered
of material is used – result in microwelding which consists of a rotor (6) and a stator
and automatically controlled by an external
at the points of contact. This severely re- (2). Turbine blades are located around the
frequency converter, normally a solid-state
duces the service life of the bearings. By circumferences of the stator and the rotor.
frequency converter that ensures a very
using dissimilar materials in so called hy- Each rotor – stator pair of circular blade
low noise level. For special applications,
brid bearings (races: steel, balls: ceramics) rows forms one stage, so that the
for example, in areas exposed to radiation,
the effect of microwelding is avoided. assembly is composed of a multitude of
motor generator frequency converters are
stages mounted in series. The gas to be
The most elegant bearing concept is that used.
pumped arrives directly through the
of the magnetic suspension. As early as
aperture of the inlet flange (1), that is, The vertical rotor – stator configuration
1976 LEYBOLD delivered magnetically
without any loss of conductance, at the provides optimum flow conditions of the
suspended turbomolecular pumps – the
active pumping area of the top blades of gas at the inlet.
legendary series 550M and 560M. At that
the rotor – stator assembly. This is equip-
time a purely active magnetic suspension To ensure vibration-free running at high
ped with blades of especially large radial
(i.e. with electromagnets) was used. Ad- rotational speeds, the turbine is dyna-
span to allow a large annular inlet area.
vances in electronics and the use of per- mically balanced at two levels during its
The gas captured by these stages is
manent magnets (passive magnetic assembly.
transferred to the lower compression
suspension) based on the “System KFA

Turbomole-
cular
pump stage 3

Siegbahn
stage 5

8
1

1 High vacuum inlet flange 7 Pump casing 1 Vacuum port 5 Bearing


2 Stator pack 8 Ball bearings 2 High vacuum flange 6 Motor
3 Venting flange 9 Cooling water connection 3 Rotor 7 Fan
4 Forevacuum flange 10 3-phase motor 4 Stator 8 Bearing
5 Splinter guard 11 Ball bearings
6 Rotor

Fig. 2.52 Schematic diagram of a grease lubricated TURBOVAC 151 Fig. 2.52a Cross section of a HY.CONE turbomolecular pump
turbomolecular pump

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Vacuum Generation Fundamentals of Vacuum Technology

10000
l · s–1
l · s–1

600 1000/1000 MC
1000
500
S
200 340M 361
151
100
50/55

10 2 4 6 8
ñ6 ñ5 ñ4 ñ3 ñ2 ñ1
10 10 10 p 10 10 mbar 10

Fig. 2.53 Pumping speed for air of different turbomolecular pumps Fig. 2.54 Pumping speed curves of a TURBOVAC 600 for H2, He, N2 and Ar

The pumping speed (volume flow rate) forevacuum flange of the pump and that at the aid of one or more cooled baffles or
characteristics of turbomolecular pumps the high vacuum flange: maximum com- traps and without the risk of a measurable
are shown in Fig. 2.53. The pumping pression k0 is to be found at zero partial pressure for hydrocarbons in the
speed remains constant over the entire throughput. For physical reasons, the vacuum chamber (hydrocarbon-free
working pressure range. It decreases at compression ratio of turbomolecular vacuum! – see also Fig. 2.57: residual gas
intake pressures above 10-3 mbar, as this pumps is very high for heavy molecules spectrum above a TURBOVAC 361). As the
threshold value marks the transition from but considerably lower for light molecules. hydrogen partial pressure attained by the
the region of molecular flow to the region The relationship between compression rotary backing pump is very low, the
of laminar viscous flow of gases. Fig. 2.54 and molecular mass is shown in Fig. 2.55. turbomolecular pump is capable of
shows also that the pumping speed Shown in Fig. 2.56 are the compression attaining ultimate pressures in the 10-11
depends on the type of gas. curves of a TURBOVAC 340 M for N2, He mbar range in spite of its rather moderate
and H2 as a function of the backing pres- compression for H2. To produce such ex-
The compression ratio (often also simply
sure. Because of the high compression tremely low pressures, it will, of course, be
termed compression) of turbomolecular
ratio for heavy hydrocarbon molecules, necessary to strictly observe the general
pumps is the ratio between the partial
turbomolecular pumps can be directly rules of UHV technology: the vacuum
pressure of one gas component at the
connected to a vacuum chamber without chamber and the upper part of the turbo-

k0

M = Mass number = Relative molar mass at


an ionization 1
√M
Fig. 2.56 Maximum compression k0 of a turbomolecular
I = Ion current
D00
Fig. 2.55 TURBOVAC 450 – Maximum compression pump TURBOVAC 340 M for H2, He and N2 as
k0 as a function of molar mass M a function of backing pressure Fig. 2.57 Spectrum above a TURBOVAC 361

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Fundamentals of Vacuum Technology Vacuum Generation

molecular pump must be baked out, and pump should be vented (except in the case
metal seals must be used. At very low of operation with a barrier gas) via the
pressures the residual gas is composed venting flange which already contains a
mainly of H2 originating from the metal sintered metal throttle, so that venting may
walls of the chamber. The spectrum in Fig. be performed using a normal valve or a
2.57 shows the residual gas composition power failure venting valve.
in front of the inlet of a turbomolecular
pump at an ultimate pressure of 7 · 10-10 Barrier gas operation
mbar nitrogen equivalent. It appears that In the case of pumps equipped with a
the portion of H2 in the total quantity of barrier gas facility, inert gas – such as dry
gas amounts to approximately 90 to 95 %. nitrogen – may be applied through a
The fraction of “heavier” molecules is con- special flange so as to protect the motor
siderably reduced and masses greater than space and the bearings against aggressive
44 were not detected. An important crite- media. A special barrier gas and venting
rion in the assessment of the quality of a valve meters the necessary quantity of
residual gas spectrum are the measurable barrier gas and may also serve as a ven-
hydrocarbons from the lubricants used in ting valve.
the vacuum pump system. Of course an Fig. 2.58 Determination of the cut-in pressure for
turbomolecular pumps when evacuating
“absolutely hydrocarbon-free vacuum” large vessels
Decoupling of vibrations
can only be produced with pump systems TURBOVAC pumps are precisely balanced
which are free of lubricants, i.e. for exam- and may generally be connected directly to
ple with magnetically-suspended turbo- pump sets and large vacuum chambers. At the apparatus. Only in the case of highly
molecular pumps and dry compressing a known pumping speed for the backing sensitive instruments, such as electron
backing pumps. When operated correctly pump SV (m3/h) and a known volume for microscopes, is it recommended to install
(venting at any kind of standstill) no hy- the vacuum chamber (m3) it is possible to vibration absorbers which reduce the
drocarbons are detectable also in the spec- estimate the cut-in pressure for the present vibrations to a minimum. For mag-
trum of normal turbomolecular pumps. turbomolecular pump: netically suspended pumps a direct
A further development of the turbomo- Simultaneous start when connection to the vacuum apparatus will
lecular pump is the hybrid or compound usually do because of the extremely low
Sv vibrations produced by such pumps.
turbomolecular pump. This is actually two > 40 h−1
V
pumps on a common shaft in a single For special applications such as opera-
casing. The high vacuum stage for the mo- and delayed start when tion in strong magnetic fields, radiation
lecular flow region is a classic turbo- hazard areas or in a tritium atmosphere,
molecular pump, the second pump for the Sv
< 40 h−1 please contact our Technical Sales Depart-
viscous flow range is a molecular drag or V ment which has the necessary experience
friction pump. and which is available to you at any time.
at a cut-in pressure of:
LEYBOLD manufactures pumps such as
the TURBOVAC 55 with an integrated  SV 
 
pV, Start = e  6 · V  mbar (2.24)
Holweck stage (screw-type compressor)
and, for example, the HY.CONE 60 or
HY.CONE 200 with an integrated Siegbahn When evacuating larger volumes the cut-in
stage (spiral compressor). The required pressure for turbomolecular pumps may
backing pressure then amounts to a few also be determined with the aid of the
mbar so that the backing pump is only diagram of Fig. 2.58.
required to compress from about 5 to 10
mbar to atmospheric pressure. A sectional Venting
view of a HY.CONE is shown in Fig. 2.52a. After switching off or in the event of a
power failure, turbomolecular pumps
Information on the operation of turbomo- should always be vented in order to
lecular pumps prevent any backdiffusion of hydrocarbons
from the forevacuum side into the vacuum
Starting chamber. After switching off the pump the
As a rule turbomolecular pumps should cooling water supply should also be
generally be started together with the switched off to prevent the possible
backing pump in order to reduce any condensation of water vapor. In order to
backstreaming of oil from the backing protect the rotor it is recommended to
pump into the vacuum chamber. A delayed comply with the (minimum) venting times
start of the turbomolecular pump, makes stated in the operating instructions. The
sense in the case of rather small backing

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Vacuum Generation Fundamentals of Vacuum Technology

2.1.8 Sorption pumps particle diameter compared with the pore


size of 13 Å for zeolite 13X. These gases
The term “sorption pumps” includes all
are, therefore, very poorly adsorbed.
arrangements for the removal of gases and
vapors from a space by sorption means. The adsorption of gases at surfaces is
The pumped gas particles are thereby dependent not only on the temperature,
bound at the surfaces or in the interior of but more importantly on the pressure
these agents, by either physical tempera- above the adsorption surface. The
ture-dependent adsorption forces (van der dependence is represented graphically for
Waals forces), chemisorption, absorption, a few gases by the adsorption isotherms
or by becoming embedded during the given in Fig. 2.60. In practice, adsorption
course of the continuous formation of new pumps are connected through a valve to
sorbing surfaces. By comparing their ope- the vessel to be evacuated. It is on
rating principles, we can distinguish immersing the body of the pump in liquid
between adsorption pumps, in which the nitrogen that the sorption effect is made
sorption of gases takes place simply by technically useful. Because of the different
temperature-controlled adsorption pro- adsorption properties, the pumping speed
cesses, and getter pumps, in which the and ultimate pressure of an adsorption
1 Inlet port 5 Thermal conducting
sorption and retention of gases are pump are different for the various gas
2 Degassing port vanes
essentially caused by the formation of 3 Support 6 Adsorption material molecules: the best values are achieved for
chemical compounds. Gettering is the 4 Pump body (e.g. Zeolith) nitrogen, carbon dioxide, water vapor, and
bonding of gases to pure, mostly metallic hydrocarbon vapors. Light noble gases are
surfaces, which are not covered by oxide Fig. 2.59 Cross section of an adsorption pump hardly pumped at all because the diameter
or carbide layers. Such surfaces always of the particles is small compared to the
form during manufacture, installation or 1 m2. For nitrogen molecules with a pores of the zeolite. As the sorption effect
while venting the system. The mostly relative molecular mass Mr = 28 that decreases with increased coverage of the
metallic highest purity getter surfaces are corresponds to about 2 · 10-4 g or 0.20 zeolite surfaces, the pumping speed falls
continuously generated either directly in mbar · l (see also Section 1.1). Therefore, off with an increasing number of the
the vacuum by evaporation (evaporator an adsorption surface of 1000 m2 is particles already adsorbed. The pumping
pumps) or by sputtering (sputter pumps) capable of adsorbing a monomolecular speed of an adsorption pump is, therefore,
or the passivating surface layer of the layer in which more than 133 mbar · l of dependent on the quantity of gas already
getter (metal) is removed by degassing the gas is bound. pumped and so is not constant with time.
vacuum, so that the pure material is
Hydrogen and light noble gases, such as The ultimate pressure attainable with
exposed to the vacuum. This step is called
helium and neon, have a relatively small adsorption pumps is determined in the
activation (NEG pumps NEG = Non Eva-
porable Getter).

Pressure [Torr]
2.1.8.1 Adsorption pumps
Adsorbed quantity of gas per quantity of adsorbent [mbar ·l · g–1]

Adsorption pumps (see Fig. 2.59) work


according to the principle of the physical
adsorption of gases at the surface of
molecular sieves or other adsorption
materials (e.g. activated Al2O3). Zeolite
13X is frequently used as an adsorption
material. This alkali aluminosilicate
possesses for a mass of the material an
extraordinarily large surface area, about
1000 m2/g of solid substance. Corres-
pondingly, its ability to take up gas is con-
siderable.
The pore diameter of zeolite 13X is about
13 Å, which is within the order of size of
water vapor, oil vapor, and larger gas
molecules (about 10 Å). Assuming that the
mean molecular diameter is half this value,
5 · 10-8 cm, about 5 · 1018 molecules are
Pressure [mbar]
D00
Fig. 2.60 Adsorption isotherms of zeolite 13X for nitrogen at -195 °C and 20 °C, as well as for helium and
adsorbed in a monolayer on a surface of neon at -195 °C

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Fundamentals of Vacuum Technology Vacuum Generation

first instance by those gases that prevail in an extraordinarily high pumping speed for
the vessel at the beginning of the pumping active gases, which, particularly on star-
process and are poorly or not at all ting processes or on the sudden evolution
adsorbed (e.g. neon or helium) at the of greater quantities of gas, can be rapidly
zeolite surface. In atmospheric air, a few pumped away. As sublimation pumps
parts per million of these gases are function as auxiliary pumps (boosters) to
present. Therefore, pressures < 10-2 mbar sputter-ion pumps and turbomolecular
can be obtained. pumps, their installation is often indi-
spensable (like the “boosters” in vapor
If pressures below 10-3 mbar exclusively
ejector pumps; see Section 2.1.6.2).
are to be produced with adsorption pumps,
as far as possible no neon or helium PZ
should be present in the gas mixture.
2.1.8.3 Sputter-ion pumps
After a pumping process, the pump must
be warmed only to room temperature for The pumping action of sputter-ion pumps
←⊕ Direction of motion of the ionized gas
the adsorbed gases to be given off and the is based on sorption processes that are molecules
zeolite is regenerated for reuse. If air (or initiated by ionized gas particles in a Pen- •→ Direction of motion of the sputtered
damp gas) containing a great deal of water ning discharge (cold cathode discharge). titanium
By means of “paralleling many individual -––- Spiral tracks of the electrons
vapor has been pumped, it is recom- PZ Penning cells
mended to bake out the pump completely Penning cells” the sputter ion pump
dry for a few hours at 200 °C or above. attains a sufficiently high pumping speed
for the individual gases. Fig. 2.61 Operating principle of a sputter-ion pump
To pump out larger vessels, several
adsorption pumps are used in parallel or in Operation of sputter-ion pumps
series. First, the pressure is reduced from The ions impinge upon the cathode of the sures) is sufficient to maintain a self-
atmospheric pressure to a few millibars by cold cathode discharge electrode system sustained gas discharge. A supply of elec-
the first stage in order to “capture” many and sputter the cathode material (titanium). trons from a hot cathode is not required.
noble gas molecules of helium and neon. The titanium deposited at other locations Because of their great mass, the
After the pumps of this stage have been acts as a getter film and adsorbs reactive movement of the ions is unaffected by the
saturated, the valves to these pumps are gas particles (e.g., nitrogen, oxygen, hydro- magnetic field of the given order of mag-
closed and a previously closed valve to a gen). The energy of the ionized gas par- nitude; they flow off along the shortest
further adsorption pump still containing ticles is not only high enough to sputter the path and bombard the cathode.
clean adsorbent is opened so that this cathode material but also to let the The discharge current i is proportional to
pump may pump down the vacuum impinging ions penetrate deeply into the the number density of neutral particles n0,
chamber to the next lower pressure level. cathode material (ion implantation). This the electron density n-, and the length l of
This procedure can be continued until the sorption process “pumps” ions of all types, the total discharge path:
ultimate pressure cannot be further including ions of gases which do not
improved by adding further clean adsorp- chemically react with the sputtered titanium i = n0 · n– · σ · l (2.25)
tion pumps. film, i.e. mainly noble gases. The effective cross section s for ionizing
The following arrangement is used to collisions depends on the type of gas.
produce the ions: stainless-steel, cylindri- According to (2.25), the discharge current
2.1.8.2 Sublimation pumps i is a function of the number particle
cal anodes are closely arranged between,
Sublimation pumps are sorption pumps in with their axes perpendicular to, two density n0, as in a Penning gauge, and it
which a getter material is evaporated and parallel cathodes (see Fig. 2.61). The can be used as a measure of the pressure
deposited on a cold inner wall as a getter cathodes are at negative potential (a few in the range from 10-4 to 10-8 mbar. At
film. On the surface of such a getter film kilovolts) against the anode. The entire lower pressures the measurements are not
the gas molecules form stable com- electrode system is maintained in a strong, reproducible due to interferences from
pounds, which have an immeasurably low homogeneous magnetic field of a flux field emission effects.
vapor pressure. The active getter film is density of B = 0.1 T, (T = Tesla = 104 In diode-type, sputter-ion pumps, with an
renewed by subsequent evaporations. Gauss) produced by a permanent magnet electrode system configuration as shown
Generally titanium is used in sublimation attached to the outside of the pump’s in Fig. 2.62, the getter films are formed on
pumps as the getter. The titanium is casing. The gas discharge profduced by the anode surfaces and between the
evaporated from a wire made of a special the high tension contains electrons and sputtering regions of the opposite
alloy of a high titanium content which is ions. Under the influence of the magnetic cathode. The ions are buried in the
heated by an electric current. Although the field the electrons travel along long spiral cathode surfaces. As cathode sputtering
optimum sorption capacity (about one tracks (see Fig. 2.61) until they impinge on proceeds, the buried gas particles are set
nitrogen atom for each evaporated tita- the anode cylinder of the corresponding free again. Therefore, the pumping action
nium atom) can scarcely be obtained in cell. The long track increases ion yield, for noble gases that can be pumped only
practice, titanium sublimation pumps have which even at low gas densities (pres- by ion burial will vanish after some time

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pumping speed Sn is given by the maxi-


mum of the pumping speed curve for air
whereby the corresponding pressure must
be stated.
For air, nitrogen, carbon dioxide and water
vapor, the pumping speed is practically the
• Titanium atoms same. Compared with the pumping speed
Ö Gas molecules for air, the pumping speeds of sputter-ion
⊕ Ions pumps for other gases amount to
ü Electrons approximately:
B Magnetic field Hydrogen 150 to 200 %
Methane 100 %
Other light
hydrocarbons 80 to 120 %
Oxygen 80 %
Fig. 2.62 Electrode configuration in a diode sputter-ion pump
Argon 30 %
Helium 28 %
and a “memory effect” will occur. and from which they travel to the target Sputter-ion pumps of the triode type excel
plate at an energy still considerably higher in contrast to the diode-type pumps in
Unlike diode-type pumps, triode sputter- high-noble gas stability. Argon is pumped
than the thermal energy 1/2 · k · T of the
ion pumps exhibit excellent stability in stably even at an inlet pressure of
gas particles. The energetic neutral
their pumping speed for noble gases 1 · 10-5 mbar. The pumps can be started
particles can penetrate into the target
because sputtering and film forming without difficulties at pressures higher than
surface layer, but their sputtering effect is
surfaces are separated. Fig. 2.63 shows 1 · 10-2 mbar and can operate continuously
only negligible. These buried or implanted
the electrode configuration of triode at an air inlet producing a constant air
particles are finally covered by fresh
sputter-ion pumps. Their greater efficiency pressure of 5 · 10-5 mbar. A new kind of
titanium layers. As the target is at positive
for pumping noble gases is explained as design for the electrodes extends the
potential, any positive ions arriving there
follows: the geometry of the system favors service life of the cathodes by 50 %.
are repelled and cannot sputter the target
grazing incidence of the ions on the
layers. Hence the buried noble gas atoms
titanium bars of the cathode grid, whereby Influence on processes in the vacuum
are not set free again. The pumping speed
the sputtering rate is considerably higher chamber by magnetic stray fields and
of triode sputter-ion pumps for noble
than with perpendicular incidence. The stray ions from the sputter-ion pump.
gases does not decrease during the
sputtered titanium moves in about the The high-magnetic-field strength required
operation of the pump.
same direction as the incident ions. The for the pumping action leads inevitably to
getter films form preferentially on the third The pumping speed of sputter-ion pumps stray magnetic fields in the neighborhood
electrode, the target plate, which is the depends on the pressure and the type of of the magnets. As a result, processes in
actual wall of the pump housing. There is gas. It is measured according to the the vacuum chamber can be disturbed in
an increasing yield of ionized particles that methods stated in DIN 28 429 and some cases, so the sputter-ion pump
are grazingly incident on the cathode grid PNEUROP 5615. The pumping speed concerned should be provided with a
where they are neutralized and reflected curve S(p) has a maximum. The nominal screening arrangement. The forms and
kinds of such a screening arrangement can
be regarded as at an optimum if the
processes taking place in the vacuum
chamber are disturbed by no more than
• Titanium atoms
the earth’s magnetic field which is present
in any case.
Ö Gas molecules
⊕ Ions Fig. 2.64 shows the magnetic stray field at
ü Electrons the plane of the intake flange of a sputter-
A Anode cylinder ion pump IZ 270 and also at a parallel
(same as in the diode
pump) plane 150 mm above. If stray ions from the
B Magnetic field discharge region are to be prevented from
F Target plate reaching the vacuum chamber, a suitable
(pump housing) screen can be set up by a metal sieve at
as the third electrode
K Cathode grid opposite potential in the inlet opening of
the sputter-ion pump (ion barrier). This,
however, reduces the pumping speed of D00
the sputter-ion pump depending on the
Fig. 2.63 Electrode configuration in a triode sputter-ion pump mesh size of the selected metal sieve.

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Fundamentals of Vacuum Technology Vacuum Generation

then need no electrical energy


• no interference by magnetic fields
• hydrocarbon-free vacuum
• free of vibrations
• low weight
NEG pumps are mostly used in
combination with other UHV pumps (tur-
bomolecular and cryopumps). Such com-
binations are especially useful when
wanting to further reduce the ultimate
pressure of UHV systems, since hydrogen
contributes mostly to the ultimate pres-
sure in an UHV system, and for which NEG
pumps have a particularly high pumping
speed, whereas the pumping effect for H2
of other pumps is low. Some typical
examples for applications in which NEG
pumps are used are particle accelerators
and similar research systems, surface
Fig. 2.64 Stray magnetic field of a sputter-ion pump analysis instruments, SEM columns and
in two places parallel to the inlet flange
(inserts) curves show lines of constant
sputtering systems. NEG pumps are
magnetic induction B in Gauss. manufactured offering pumping speeds of
1 Gauss = 1 · 10–4 Tesla several l/s to about 1000 l/s. Custom
pumps are capable of attaining a pumping
2.1.8.4 Non evaporable getter pumps speed for hydrogen which is by several
(NEG Pumps) orders of magnitude higher.

The non evaporable getter pump operates


with a non evaporable, compact getter
material, the structure of which is porous
at the atomic level so that it can take up
large quantities of gas. The gas molecules
adsorbed on the surface of the getter
material diffuse rapidly inside the material
thereby making place for further gas
molecules impinging on the surface. The
non evaporable getter pump contains a
heating element which is used to heat the
getter material to an optimum temperature
depending on the type of gas which is
preferably to be pumped. At a higher
temperature the getter material which has
been saturated with the gas is regenerated
(activated). As the getter material, mostly
zirconium-aluminum alloys are used in the
form of strips. The special properties of
NEG pumps are:
• constant pumping speed in the HV and
UHV ranges
• no pressure restrictions up to about 12
mbar
• particularly high pumping speed for
hydrogen and its isotopes
• after activation the pump can often
operate at room temperature and will

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2.1.9 Cryopumps engineering in that the temperatures pumped by way of condensation. A


involved in cryo engineering are in the surface cooled with liquid helium
As you may have observed water range below 120 K (< -153 °C). Here we (T ≈ 4.2 K) is capable of condensing all
condenses on cold water mains or are dealing with two questions: gases except helium.
windows and ice forms on the evaporator a) What cooling principle is used in cryo In continuous flow cryopumps the cold
unit in your refrigerator. This effect of engineering or in cryopumps and how surface is designed to operate as a heat
condensation of gases and vapors on cold is the thermal load of the cold surface exchanger. Liquid helium in sufficient
surfaces, water vapor in particular, as it is lead away or reduced? quantity is pumped by an auxiliary pump
known in every day life, occurs not only at b) What are the operating principles of the from a reservoir into the evaporator in order
atmospheric pressure but also in vacuum. cryopumps? to attain a sufficiently low temperature at
This effect has been utilized for a long time the cold surface (cryopanel).
in condensers (see 2.1.5) mainly in
2.1.9.1 Types of cryopump The liquid helium evaporates in the heat
connection with chemical processes;
exchanger and thus cools down the
previously the baffle on diffusion pumps Depending on the cooling principle a cryopanel. The waste gas which is
used to be cooled with refrigerating difference is made between generated (He) is used in a second heat
machines. Also in a sealed space (vacuum • Bath cryostats exchanger to cool the baffle of a thermal
chamber) the formation of condensate on • Continuous flow cryopumps radiation shield which protects the system
a cold surface means that a large number • Refrigerator cryopumps from thermal radiation coming from the
of gas molecules are removed from the
In the case of bath cryostats – in the most outside. The cold helium exhaust gas
volume: they remain located on the cold
simple case a cold trap filled with LN2 (li- ejected by the helium pump is supplied to
surface and do not take part any longer in
quid nitrogen) – the pumping surface is a helium recovery unit. The temperature at
the hectic gas atmosphere within the
cooled by direct contact with a liquefied the cryopanels can be controlled by
vacuum chamber. We then say that the
gas. On a surface cooled with LN2 controlling the helium flow.
particles have been pumped and talk of
cryopumps when the “pumping effect” is (T ≈ 77 K) H2O and CO2 are able to Today refrigerator cryopumps are being
attained by means of cold surfaces. condense. On a surface cooled to ≈ 10 K used almost exclusively (cold upon
all gases except He and Ne may be demand). These pumps operate basically
Cryo engineering differs from refrigeration
much in the same way as a common
household refrigerator, whereby the
following thermodynamic cycles using
1
helium as the refrigerant may be employed:
3 • Gifford-McMahon process
• Stirling process
2 • Brayton process
• Claude process
The Gifford-McMahon process is mostly
used today and this process is that which
has been developed furthest. It offers the
possibility of separating the locations for
the large compressor unit and the
expansion unit in which the refrigeration
process takes place. Thus a compact and
low vibration cold source can be designed.
The cryopumps series-manufactured by
LEYBOLD operate with two-stage cold
heads according to the Gifford-McMahon
process which is discussed in detail in the
following.
The entire scope of a refrigerator cryopump
is shown in Fig. 2.65 and consists of the
compressor unit (1) which is linked via
flexible pressure lines (2) – and thus
vibration-free – to the cryopump (3). The
cryopump itself consists of the pump
1 Compressor unit
2 Flexible pressure
lines
3 Cold head (without
condensation
surfaces)
casing and the cold head within. Helium is
used as the refrigerant which circulates in a
D00
closed cycle with the aid of the compressor.
Fig. 2.65 All items of a refrigerator cryopump

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2.1.9.2 The cold head and its opera- located inside the displacer. The regenera- In two series connected stages the
ting principle (Fig. 2.66) tor is a heat accumulator having a large temperature of the helium is reduced to
heat exchanging surface and capacity, about 30 K in the first stage and further to
Within the cold head, a cylinder is divided
which operates as a heat exchanger within about 10 K in the second stage. The
into two working spaces V1 and V2 by a
the cycle. Outlined in Fig. 2.66 are the four attainable low temperatures depend
displacer. During operation the right space
phases of refrigeration in a single-stage among other things on the type of
V1 is warm and the left space V2 is cold. At
refrigerator cold head operating according regenerator. Commonly copperbronze is
a displacer frequency f the refrigerating
to the Gifford-McMahon principle. used in the regenerator of the first stage
power W of the refrigerator is:
and lead in the second stage. Other
W = (V2,max – V2,min) · (pH – pN) · f (2.26) The two-stage cold head materials are available as regenerators for
The series-manufactured refrigerator special applications like cryostats for
The displacer is moved to and fro pneuma-
cryopumps from LEYBOLD use a two- extremely low temperatures (T < 10 K).
tically so that the gas is forced through the
stage cold head operating according to the The design of a two-stage cold head is
displacer and thus through the regenerator
Gifford-McMahon principle (see Fig. 2.67). shown schematically in Fig. 2.67. By

V2 (cold) V1 (warm) Phase 1:


The displacer is at the left dead center;
V2 where the cold is produced has its
minimum size. Valve N remains closed,
H is opened. Gas at the pressure pH
Regenerator Displacer flows through the regenerator into V2.
There the gas warms up by the pressure
increase in V1.

V2 (cold) V1 (warm)
Phase 2:
Valve H remains open, valve N closed:
the displacer moves to the right and
ejects the gas from V1 through the rege-
nerator to V2 where it cools down at the
Regenerator Displacer cold regenerator.; V2 has its maximum
volume.

V2 (cold) V1 (warm)
Phase 3:
Valve H is closed and the valve N to the
low pressure reservoir is opened. The
gas expands from pH to pN and thereby
cools down. This removes heat from the
Regenerator Displacer vicinity and it is transported with the
expanding gas to the compressor.

V2 (cold) V1 Phase 4:
With valve N open the displacer moves
to the left; the gas from V2,max flows
through the regenerator, cooling it down
and then flows into the volume V1 and
Regenerator Displacer into the low pressure reservoir. This
completes the cycle.

Fig. 2.66 Refrigerating phases using a single-stage cold head operating according to the Gifford-McMahon process

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1 Electric connections and current 11 Regenerator, 2nd stage 1 High vacuum flange 9 1st stage of the cold head
feedthrough for the motor in the 12 Expansion volume, 2nd stage 2 Pump casing (≈ 50 – 80 K)
cold head 13 2nd (cooling) stage 3 Forevacuum flange 10 Gauge for the hydrogen vapor
2 He high pressure connection (copper flange) 4 Safety valve for gas discharge pressure thermometer
3 He low pressure connection 14 Measurement chamber for the 5 Thermal radiation shield 11 Helium gas connections
4 Cylinder, 1st stage vapor pressure 6 Baffle 12 Motor of the cold head
5 Displacer, 1st stage 15 Control piston 7 2nd stage of the cold head with casing and electric
6 Regenerator, 1st stage 16 Control volume (≈10 K); connections
7 Expansion volume, 1st stage 17 Control disk 8 Cryopanels
8 1st (cooling) stage (copper 18 Control valve
flange) 19 Gauge for the hydrogen vapor
9 Cylinder, 2nd stage pressure thermometer
10 Displacer, 2nd stage 20 Motor in the cold head
Fig. 2.67 Two-stage cold head Fig. 2.68 Design of a refrigerator cryopump (schematic)

means of a control mechanism with a is surrounded by the thermal radiation stage (7) of the cold head are coated with
motor driven control valve (18) with shield (5) which is black on the inside and activated charcoal on the inside in order to
control disk (17) and control holes first the polished as well as nickel plated on the be able to pump gases which do not easily
pressure in the control volume (16) is outside. Under no-load conditions the condense and which can only be pumped
changed which causes the displacers (6) baffle and the thermal radiation shield by cryosorption (see 2.1.9.4).
of the first stage and the second stage (11) (first stage) attain a temperature ranging
to move; immediately thereafter the between 50 to 80 K at the cryopanels and
pressure in the entire volume of the about 10 K at the second stage. The 2.1.9.4 Bonding of gases to cold
cylinder is equalized by the control surface temperatures of these cryopanels surfaces
mechanism. The cold head is linked via are decisive to the actual pumping The thermal conductivity of the condensed
flexible pressure lines to the compressor. process. These surface temperatures (solid) gases depends very much on their
depend on the refrigerating power structure and thus on the way in which the
supplied by the cold head, and the thermal condensate is produced. Variations in
2.1.9.3 The refrigerator cryopump conduction properties in the direction of thermal conductivity over several orders of
the pump’s casing. During operation of the magnitude are possible! As the condensa-
Fig. 2.68 shows the design of a cryopump.
cryopump, loading caused by the gas and te increases in thickness, thermal resis-
It is cooled by a two-stage cold head. The
the heat of condensation results in further tance and thus the surface temperature
thermal radiation shield (5) with the baffle
warming of the cryopanels. The surface increase subsequently reducing the pum-
(6) is closely linked thermally to the first
temperature does not only depend on the ping speed. The maximum pumping speed
stage (9) of the cold head. For pressures
temperature of the cryopanel, but also on
below 10-3 mbar the thermal load is
caused mostly by thermal radiation. For
the temperature of the gas which has
already been frozen on to the cryopanel.
of a newly regenerated pump is stated as
its nominal pumping speed. The bonding D00
this reason the second stage (7) with the process for the various gases in the
The cryopanels (8) attached to the second cryopump is performed in three steps: first
condensation and cryosorption panels (8)

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not arrive at the second stage and


consume capacity there), the situation
arises as shown in Fig. 2.69.
The gas molecules entering the pump pro-
duce the area related theoretical pumping
speed according the equation 2.29a with T
= 293 K. The different pumping speeds
have been combined for three representa-
tive gases H2, N2 and H20 taken from each
of the aforementioned groups. Since water
Hydrogen Water vapor Nitrogen vapor is pumped on the entire entry area of
Area related conductance of the intake flange in l / s · cm2: the cryopump, the pumping speed
43.9 14.7 11.8 measured for water vapor corresponds
Area related pumping speed of the cryopump in l / s · cm2: almost exactly to the theoretical pumping
13.2 14.6 7.1 speed calculated for the intake flange of
Ratio between pumping speed and conductance:
30 % 99 % 60 %
the cryopump. N2 on the other hand must
first overcome the baffle before it can be
Fig. 2.69 Cryopanels – temperature and position define the efficiency in the cryopump bonded on to the cryocondensation panel.
Depending on the design of the baffle, 30
the mixture of different gases and vapors pressure. Cryosorption is the physical and to 50 percent of all N2 molecules are
meets the baffle which is at a temperature reversible bonding of gas molecules reflected.
of about 80 K. Here mostly H2O and CO2 through Van der Waals forces on suffici- H2 arrives at the cryosorption panels after
are condensed. The remaining gases ently cold surfaces of other materials. The further collisions and thus cooling of the
penetrate the baffle and impinge in the bond energy is equal to the heat of gas. In the case of optimally designed
outside of the cryopanel of the second adsorption which is greater than the heat cryopanels and a good contact with the ac-
stage which is cooled to about 10 K. Here of vaporization. As soon as a monolayer tive charcoal up to 50 percent of the H2
gases like N2, O2 or Ar will condense. Only has been formed, the following molecules which has overcome the baffle can be
H2, He and Ne will remain. These gases impinge on a surface of the same kind bonded. Due to the restrictions regarding
can not be pumped by the cryopanels and (sorbent) and the process transforms into access to the pumping surfaces and
these pass after several impacts with the cryocondensation. The higher bond energy cooling of the gas by collisions with the
thermal radiation shield to the inside of for cryocondensation prevents the further walls inside the pump before the gas
these panels which are coated with an growth of the condensate layer thereby reaches the pumping surface, the measu-
adsorbent (cryosorption panels) where restricting the capacity for the adsorbed red pumping speed for these two gases
they are bonded by cryosorption. Thus for gases. However, the adsorbents used, like amounts only to a fraction of the theoreti-
the purpose of considering a cryopump activated charcoal, silica gel, alumina gel cal pumping speed. The part which is not
the gases are divided into three groups and molecular sieve, have a porous pumped is reflected chiefly by the baffle.
depending at which temperatures within structure with very large specific surface Moreover, the adsorption probability for
the cryopump their partial pressure drops areas of about 106 m2/kg. Cryotrapping is H2 differs between the various adsorbents
below 10-9 mbar: understood as the inclusion of a low and is < 1, whereas the probabilities for the
boiling point gas which is difficult to pump condensation of water vapor and N2 ≈ 1.
1st group:
such as hydrogen, in the matrix of a gas
ps < 10-9 mbar at T ≈ 77K (LN2): H2O, CO2 Three differing capacities of a pump for the
having a higher boiling point and which
2nd group: can be pumped easily such as Ar, CH4 or gases which can be pumped result from
ps < 10-9 mbar at T ≈ 20K: N2, O2, Ar CO2. At the same temperature the the size of the three surfaces (baffle,
condensate mixture has a saturation vapor condensation surface at the outside of the
3rd group: second stage and sorption surface at the
pressure which is by several orders of
ps < 10-9 mbar at T < 4.2K: H2, He, Ne inside of the second stage). In the design
magnitude lower than the pure condensate
A difference is made between the different of the gas with the lower boiling point. of a cryopump, a mean gas composition
bonding mechanisms as follows: (air) is assumed which naturally does not
apply to all vacuum processes (sputtering
Cryocondensation is the physical and re- 2.1.9.5 Pumping speed and position of processes, for example. See 2.1.9.6
versible bonding of gas molecules through the cryopanels “Partial Regeneration”).
Van der Waals forces on sufficiently cold
surfaces of the same material. The bond Considering the position of the cryopanels
energy is equal to the energy of vaporiza- in the cryopump, the conductance from
tion of the solid gas bonded to the surface the vacuum flange to this surface and also
and thus decreases as the thickness of the the subtractive pumping sequence (what
condensate increases as does the vapor has already condensed at the baffle can

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2.1.9.6 Characteristic quantities of a TK (K) Ultimate pressure Ult. press. (mbar) Ult. press.(mbar)
cryopump (according to equ. 2.28) H2 N2
The characteristic quantities of a cryo- 2.5 10.95 · ps 3.28 · 10–14 immeasurably low
pump are as follows (in no particular 4.2 8.66 · ps 4.33 · 10–9 immeasurably low
order): 20 3.87 · ps 3.87 · 10+3 3.87 · 10–11
• Cooldown time
Table 2.6 Ultimate temperatures at a wall temperature of 300 K
• Crossover value
• Ultimate pressure Ultimate pressure pend: For the case of refrigerating power for the first stage at 80
cryocondensation (see Section 2.1.9.4) K and for the second stage at 20 K when
• Capacity simultaneously loading both stages
the ultimate pressure can be calculated by:
• Refrigerating power and net thermally. During the measurement of
refrigerating power TG refrigerating power the thermal load is
pend = ps( TK ) · (2.28)
TK generated by electric heaters. The refrige-
• Regeneration time rating power is greatest at room tempe-
• Throughput and maximum pV flow pS is the saturation vapor pressure of the rature and is lowest (Zero) at ultimate tem-
gas or gases which are to be pumped at perature.
• Pumping speed the temperature TK of the cryopanel and TG
.
Net refrigerating power Q (W): In the
• Service life / duration of operation is the gas temperature (wall temperature in case of refrigerator cryopumps the net
the vicinity of the cryopanel). refrigerating power available at the usual
• Starting pressure
Example: With the aid of the vapor operating temperatures
Cooldown time: The cooldown time of pressure curves in Fig. 9.15 for H2 and N2 (T1 < 80 K, T2 < 20 K) substantially defines
cryopumps is the time span from start-up the ultimate pressures summarized in the throughput and the crossover value.
until the pumping effect sets in. In the case Table 2.6 at TG = 300 K result. The net. refrigerating power is – depen-
of refrigerator cryopumps the cooldown ding on the configuration of the pump –
time is stated as the time it takes for the The Table shows that for hydrogen at much lower than the refrigerating power of
second stage of the cold head to cool temperatures T < 3 K at a gas temperature the cold head used without the pump.
down from 293 K to 20 K. of TG= 300 K (i.e. when the cryopanel is
exposed to the thermal radiation of the pV flow see 1.1
Crossover value: The crossover value is a wall) sufficiently low ultimate pressures Regeneration time: As a gas trapping
characteristic quantity of an already cold can be attained. Due to a number of inter- device, the cryopump must be regenerated
refrigerator cryopump. It is of significance fering factors like desorption from the wall after a certain period of operation. Rege-
when the pump is connected to a vacuum and leaks, the theoretical ultimate pres- neration involves the removal of condens-
chamber via an HV / UHV valve. The sures are not attained in practice. ed and adsorbed gases from the cryopa-
crossover value is that quantity of gas with
Capacity C (mbar · l): The capacity of a nels by heating. The regeneration can be
respect to Tn = 293 K which the vacuum
cryopump for a certain gas is that quantity run fully or only partially and mainly differs
chamber may maximally contain so that
of gas (pV value at Tn = 293 K) which can by the way in which the cryopanels are
the temperature of the cryopanels does
be bonded by the cryopanels before the heated.
not increase above 20 K due to the gas
burst when opening the valve. The pumping speed for this type of gas G In the case of total regeneration a diffe-
crossover value is usually stated as a pV drops to below 50 % of its initial value. rence is made between:
value in in mbar · l. The capacity for gases which are pumped 1. Natural warming: after switching off the
The crossover value and the chamber by means of cryosorption depends on the compressor, the cryopanels at first
volume V result in the crossover pressure quantity and properties of the sorption warm up only very slowly by thermal
pc to which the vacuum chamber must be agent; it is pressure dependent and conduction and then in addition
evacuated first before opening the valve generally by several orders of magnitude through the released gases.
leading to the cryopump. The following lower compared to the pressure 2. Purge gas method: the cryopump is
may serve as a guide: independent capacity for gases which are warmed up by admitting warm purging
pumped by means of cryocondensation. gas.
35 · .
pc ≤ · Q 2 (20 K ) mbar (2.27) 3. Electric heaters: the cryopanels of the
V Refrigerating power Q (W): The refrige-
cryopump are warmed up by heaters at
rating power of a refrigeration source at a
V = Volume of the vacuum chamber (l), the first and second stages. The
temperature T gives the amount of heat
. released gases are discharged either
Q2(20K) = Net refrigerating capacity in that can be extracted by the refrigerating
through an overpressure valve (purge
Watts, available at the second stage of the source whilst still maintaining this
cold head at 20 K. temperature. In the case of refrigerators it
has been agreed to state for single-stage
gas method) or by mechanical backing
pumps. Depending on the size of the D00
pump one will have to expect a
cold heads the refrigerating power at 80 K
regeneration time of several hours.
and for two-stage cold heads the

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Fundamentals of Vacuum Technology Vacuum Generation

p >> pend the expression in brackets


approaches 1 so that in the oversaturated
case
p >> pend > Ps so that:
Temperature (K)

Sth = AK · SA (2.29a)
2 1 with
R · TG TG
SA = c = = 365
. `/ s · cm2
4 2· π · M M
(2) (1)
TG Gas temperature in K
40 minutes Time about 6 hours
M Molar mass
Fig. 2.70 Comparison between total (1) and partial (2) regeneration Given in Table 2.7 is the surface area-
related pumping speed SA in l · s-1 · cm-2
Partial regeneration: Since the limitation The maximum pV flow at which the for some gases at two different gas
in the service life of a cryopump depends cryopanels are warmed up to T ≈ 20 K in temperatures TG in K determined accor-
in most applications on the capacity limit the case of continuous operation, de- ding to equation 2.29a. The values stated
for the gases nitrogen, argon and pends on the net refrigerating power of the in the Table are limit values. In practice the
hydrogen pumped by the second stage, it pump at this temperature and the type of condition of an almost undisturbed
will often be required to regenerate only gas. For refrigerator cryopumps and equilibrium (small cryopanels compared
this stage. Water vapor is retained during condensable gases the following may be to a large wall surface) is often not true,
partial regeneration by the baffle. For this, taken as a guide: because large cryopanels are required to
the temperature of the first stage must be . attain short pumpdown times and a good
Qmax = 2.3 Q 2 (20 K) mbar · l/s
maintained below 140 K or otherwise the . end vacuum. Deviations also result when
partial pressure of the water vapor would Q 2 (20 K) is the net refrigerating power in the cryopanels are surrounded by a cooled
become so high that water molecules Watts available at the second stage of the baffle at which the velocity of the
would contaminate the adsorbent on the cold heat at 20 K. In the case of inter- penetrating molecules is already reduced
second stage. mittent operation, a higher pV flow is per- by cooling.
missible (see crossover value).
In 1992, LEYBOLD was the first manufac- Service life / duration of operation top (s):
turer of cryopumps to develop a method The duration of operation of the cryopump
Pumping speed Sth: The following applies
permitting such a partial regeneration. for a particular gas depends on the
to the (theoretical) pumping speed of a
This fast regeneration process is micro- equation:
cryopump:
processor controlled and permits a partial t op, G
regeneration of the cryopump in about 40  p 
S th = A K · SA · α · 1 − end (2.29) CG = ∫Q G (t)dt with
minutes compared to 6 hours needed for a  p  0

total regeneration based on the purge gas


method. A comparison between the typical CG = Capacity of the cryopump for the
AK Size of the cryopanels
cycles for total and partial regeneration is gas G
shown in Fig. 2.70. The time saved by the SA Surface area related pumping speed
QG(t) =Throughput of the cryopump for
Fast Regeneration System is apparent. In a (area related impact rate according to
the gas at the point of time t
production environment for typical sput- equations 1.17 and 1.20, proportional
tering processes one will have to expect to the mean velocity of the gas If the constant __ mean over time for the
one total regeneration after 24 partial molecules in the direction of the throughput QG is known, the following
regenerations. cryopanel) applies:
a Probability of condensation C C
Throughput and maximum pV flow: t op, G = G = G (2.30)
(mbar l/s): the throughput of a cryopump (pumping) QG pG · SG
for a certain gas depends on the pV flow of pend Ultimate pressure (see above)
the gas G through the intake opening of After the period of operation top,G has
the pump: p Pressure in the vacuum chamber elapsed the cryopump must be rege-
The equation (2.29) applies to a cryopanel nerated with respect to the type of gas G.
QG = qpV,G; the following equation
applies built into the vacuum chamber, the surface Starting pressure po: Basically it is
area of which is small compared to the possible to start a cryopump at atmosphe-
QG = pG · SG with surface of the vacuum chamber. At ric pressure. However, this is not desirable
pG = intake pressure, sufficiently low temperatures α = 1 for all for several reasons. As long as the mean
gases. The equation (2.29) shows that for free path of the gas molecules is smaller
SG = pumping capacity for the gas G

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M SA SA TS Triple point
Symbol Gas Molar at 293 K at 80 K Boiling point (= melting point)
mass gas temp. gas temp. 1013 mbar Tt pt
g/mol l/s · cm2 l/s · cm2 K K mbar
H2 Hydrogen 2.016 43.88 22.93 20.27 13.80 70.4
He Helium 4.003 31.14 16.27 4.222 2.173 50.52
CH4 Methane 4.003 15.56 8.13 111.67 90.67 116.7
H2O Water 18.015 14.68 – 373.15 273.16 6.09
Ne Neon 20.183 13.87 7.25 27.102 24.559 433.0
CO Carbon monoxide 28.000 11.77 6.15 81.67 68.09 153.7
N2 Nitrogen 28.013 11.77 6.15 77.348 63.148 126.1
Air 28.96 11.58 6.05 ≈ 80.5 ≈ 58.5 –
O2 Oxygen 31.999 11.01 5.76 90.188 54.361 1.52
Ar Argon 39.948 9.86 5.15 87.26 83.82 687.5
Kr Krypton 83.80 6.81 3.56 119.4 115.94 713.9
Xe Xenon 131.3 5.44 2.84 165.2 161.4

Table 2.7 Surface-related pumping speeds for some gases

than the dimensions of the vacuum cham-


ber (p > 10-3 mbar), thermal conductivity
of the gas is so high that an unacceptably
large amount of heat is transferred to the
cryopanels. Further, a relatively thick layer
of condensate would form on the cryo-
panel during starting. This would markedly
reduce the capacity of the cryopump
available to the actual operating phase.
Gas (usually air) would be bonded to the
adsorbent, since the bonding energy for
this is lower than that for the condensation
surfaces. This would further reduce the
already limited capacity for hydrogen. It is
recommended that cryopumps in the high
vacuum or ultrahigh vacuum range are
started with the aid of a backing pump at
pressures of p < 5 · 10-2 mbar. As soon as
the starting pressure has been attained the
backing pump may be switched off.

D00

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2.2 Choice of pumping Dry processes work primarily in a narrow resin-casting plants, as well as in
and limited pressure region. molecular distillation, the production of as
process The system is usually evacuated to a large a liquid surface as possible is
suitable characteristic pressure before the important. In all wet processes the provi-
2.2.1 Survey of the most usual actual working process begins. This sion of the necessary heat for evapo-
happens, for example, in plants for evapo- ration of the moisture is of great impor-
pumping processes rative coating, electron-beam welding, and tance.
Vacuum technology has undergone rapid crystal pulling; in particle accelerators,
Basic pumping procedures are given in the
development since the Fifties. In research mass spectrometers, electron micro-
following paragraphs.
and in most branches of industry today, it scopes; and others.
is indispensable. If you have specific questions, you should
Further, there are dry processes in which
get in touch with a specialist department in
Corresponding to the many areas of ap- degassing in vacuum is the actual
LEYBOLD where experts are available to
plication, the number of technical proce- technical process. These include work in
you who can draw on many years of
dures in vacuum processes is extraordi- induction- and arc furnaces, steel degas-
experience.
narily large. These cannot be described sing plants, and plants for the manufacture
within the scope of this section, because of pure metals and electron tubes.
Classifications of typical vacuum proces-
the basic calculations in this section cover ses and plants according to the pressure
mainly the pumping process, not the Wet processes are undertaken primarily
regions.
process taking place in the vessel. A in a prescribed working operation that
Rough vacuum 1013 mbar – 1 mbar
survey of the most important processes in covers a wider pressure region.
• Drying, distillation, and steel degassing.
vacuum technology and the pressure This is especially important in the drying of
solid materials. If, for instance, work is Medium vacuum 1 -10-3 mbar
regions in which these processes are
chiefly carried out is given in the diagrams undertaken prematurely at too low a • Molecular distillation, freeze-drying,
(Figures 2.71 and 2.72). pressure, the outer surfaces dry out too impregnation, melting and casting
quickly. As a result, the thermal contact to furnaces, and arc furnaces.
Generally, the pumping operation for these the moisture to be evaporated is impaired High vacuum 10-3 – 10-7 mbar
processes can be divided into two and the drying time is considerably • Evaporative coating, crystal pulling,
categories – dry- and wet – vacuum proce- increased. Predominantly processes that mass spectrometers, tube production,
dures, that is, into processes in which no are carried out in drying, impregnating, electron microscopes, electron beam
significant amounts of vapor have to be and freeze-drying plants belong in this plants, and particle accelerators.
pumped and those in which vapors category. Ultrahigh vacuum: < 10-7 mbar
(mostly water or organic) arise.
• Nuclear fusion, storage rings for
In the removal of water vapor from liquids
Distinctions between the two categories or in their distillation, particularly in accelerators, space research, and
are described briefly: degassing columns, vacuum filling, and surface physics.

Ultrahigh vacuum High vacuum Medium vacuum Rough vacuum

Mass spectrometers
Molecular beam apparatus
Ion sources
Particle accelerators
Electron microscopes
Electron diffraction apparatus
Vacuum spectographs
Low-temperature research
Production of thin films
Surface physics
Plasma research
Nuclear fusion apparatus
Space simulation
Material research
Preparations for
electron microscopy

10–13 10–10 10–7 10–3 100 103

Pressure [mbar]

Fig. 2.71 Pressure ranges (p < 1000 mbar) of physical and chemical analytical methods

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Ultrahigh vacuum High vacuum Medium vacuum Rough vacuum

Annealing of metals
Melting of metals
Degassing of molten metals
Steel degassing
Electron-beam melting
Electron-beam welding
Evaporation coating
Sputtering of metals
Zone melting and crystal growing in high-vacuum
Molecular distillation
Degassing of liquids
Sublimation
Casting of resins and lacquers
Drying of plastics
Drying of insulating papers
Freeze-drying of mass materials
Freeze-drying of pharmaceutical products
Production of incandescent lamps
Production of electron tubes
Production of gas-discharge tubes

10–10 10–7 10–3 100 103

Pressure [mbar]
Fig. 2.72 Pressure ranges of industrial vacuum processes

2.2.2 Pumping of gases be pumped above 80 mbar over long still amounts to about 50 % of the nominal
(dry processes) periods, one should use, particularly on pumping speed.
economic grounds, jet pumps, water ring
For dry processes in which a non conden- pumps or dry running, multi-vane pumps. Between 1 and 10-2 mbar at the onset of
sable gas mixture (e.g., air) is to be Rotary vane and rotary piston pumps are large quantities of gas, Roots pumps with
pumped, the pump to be used is clearly especially suitable for pumping down rotary pumps as backing pumps have
characterized by the required working vessels from atmospheric pressure to optimum pumping properties (see Section
pressure and the quantity of gas to be pressures below 80 mbar, so that they can 2.1.3.1). For this pressure range, a single-
pumped away. The choice of the required work continuously at low pressures. If stage rotary pump is sufficient, if the chief
working pressure is considered in this large quantities of gas arise at inlet working region lies above 10-1 mbar. If it
section. The choice of the required pump pressures below 40 mbar, the connection lies between 10-1 and 10-2 mbar, a two-
is dealt with in Section 2.3. in series of a Roots pump is recommen- stage backing pump is recommended.
Each of the various pumps has a charac- ded. Then, for the backing pump speed Below 10-2 mbar the pumping speed of
teristic working range in which it has a required for the process concerned, a single-stage Roots pumps in combination
particularly high efficiency. Therefore, the much smaller rotary vane or piston pump with two-stage rotary pumps as backing
most suitable pumps for use in the follo- can be used. pumps decreases. However, between 10-2
wing individual pressure regions are des- and 10-4 mbar, two-stage Roots pumps (or
cribed. For every dry-vacuum process, the b) Medium vacuum (1 – 10-3 mbar) two single-stage Roots pumps in series)
vessel must first be evacuated. It is quite If a vacuum vessel is merely to be eva- with two-stage rotary pumps as backing
possible that the pumps used for this may cuated to pressures in the medium vacu- pumps still have a very high pumping
be different from those that are the um region, perhaps to that of the required speed. Conversely, this pressure region is
optimum choices for a process that is backing pressure for diffusion or sputter- the usual working region for vapor ejector
undertaken at definite working pressures. ion pumps, single- and two-stage rotary pumps. For work in this pressure region,
In every case the choice should be made pumps are adequate for pressures down to they are the most economical pumps to
with particular consideration for the 10-1 and 10-3 mbar, respectively. It is es- purchase. As backing pumps, single-stage
pressure region in which the working sentially more difficult to select the rotary positive displacement pumps are
process predominantly occurs. suitable type of pump if medium vacuum suitable. If very little maintenance and val-
processes are concerned in which gases veless operation are convenient (i.e., small
a) Rough vacuum (1013 – 1 mbar) or vapors are evolved continuously and vessels in short operation cycles are to be
The usual working region of the rotary must be pumped away. An important hint pumped to about 10-4 mbar or large
pumps described in Section 2 lies below may be given at this point. Close to the vessels are to be maintained at this pres-
80 mbar. At higher pressures these pumps attainable ultimate pressure, the pumping sure unattended for weeks), the previously
have a very high power consumption (see
Fig. 2.11) and a high oil consumption (see
speed of all rotary pumps falls off rapidly.
Therefore, the lowest limit for the normal
mentioned two-stage Roots pumps with
two-stage rotary pumps as backing pumps
D00
Section 8.3.1.1). Therefore, if gases are to working pressure region of these pumps are the suitable combinations. Allthough,
should be that at which the pumping speed such a combination does not work as

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economically as the corresponding vapor 2.2.3 Pumping of gases and sisting of a Roots pump, condenser, and
ejector pump, it can operate for a much vapors (wet processes) backing pump, which can transport 100
longer time without maintenance. kg/h of vapor and 18 kg/h of air at an inlet
When vapors must be pumped, in addition pressure of 50 mbar, has a power
c) High vacuum (10-3 to 10-7 mbar) to the factors working pressure and requirement of 4 – 10 kW (depending on
Diffusion, sputter-ion, and turbomolecular pumping speed, a third determining factor the quantity of air involved). A steam
pumps typically operate in the pressure is added namely the vapor partial pressure ejector pump of the same performance
region below 10-3 mbar. If the working – which may vary considerably in the requires about 60 kW without altering the
region varies during a process, different course of a process. This factor is decisive quantity of air involved.
pumping systems must be fitted to the in determining the pumping arrangement
to be installed. In this regard, the con- For the pumping of water vapor, gas ballast
vessel. There are also special diffusion
densers described in Section 2.15 are very pumps and combinations of gas ballast
pumps that combine the typical properties
important adjuncts to rotary displacement pumps, Roots pumps, and condensers are
of a diffusion pump (low ultimate pres-
pumps. They have a particularly high especially suitable.
sure, high pumping speed in the high
vacuum region) with the outstanding pumping speed when pumping vapors.
The next section covers pumping of water Pumping of water vapor with gas ballast
properties of a vapor ejector pump (high
vapor (the most frequent case). The pumps
throughput in the medium vacuum region,
considerations apply similarly to other The ratio of vapor partial pressure pv to air
high critical backing pressure). If the
partial pressure pp is decisive in the
working region lies between 10-2 and 10-6 non-aggressive vapors.
evaluation of the correct arrangement of
mbar, these diffusion pumps are, in
Pumping of Water Vapor gas ballast pumps, as shown previously by
general, specially recommended.
Water vapor is frequently removed by equations 2.2 and 2.3. Therefore, if the
water vapor tolerance of the gas ballast
d) Ultrahigh vacuum (< 10-7 mbar) pumps that operate with water or steam as
a pump fluid, for example, water ring pump is known, graphs may be obtained
For the production of pressures in the
pumps or steam ejector pumps. This de- that clearly give the correct use of gas
ultrahigh vacuum region, sputter-ion, and
pends considerably on circumstances, ballast pumps for pumping water vapor
sublimation pumps, as well as turbomole-
however, because the economy of steam (see Fig. 2.73). Large single-stage rotary
cular pumps and cryopumps, are used in
ejector pumps at low pressures is gene- plunger pumps have, in general, an
combination with suitable forepumps. The
rally far inferior to that of rotary pumps. operating temperature of about 77 °C and
pump best suited to a particular UHV
For pumping a vapor – gas mixture in hence a water vapor tolerance of about 60
process depends on various conditions
which the vapor portion is large but the air mbar. This value is used to determine the
(for further details, see Section 2.5).
portion is small, the vapor can be pumped different operating regions in Fig. 2.73. In
by condensers and the permanent gases, addition it is assumed that the pressure at
by relatively small gas ballast pumps (see the discharge outlet port of the gas ballast
Section 2.1.5). pump can increase to a maximum of 1330
mbar until the discharge outlet valve
Comparatively, then, a pump set con- opens.

Region A: Single-stage, rotary plunger


pumps without gas ballast inlet.
At a saturation vapor pressure pS of 419
mbar at 77 °C, according to equation 2.2,
the requirement is given that pv < 0.46 pp,
where
pv is the water vapor partial pressure
Water vapor partial pressure pv

pp is the partial pressure of air


pv + pp = ptot total pressure

46 This requirement is valid in the whole


0.
= working region of the single-stage rotary
/ pp
pv plunger pump – hence, at total pressures
between 10-1 and 1013 mbar.

Region B: Single-stage rotary plunger


pumps with gas ballast and an inlet
condenser.
Air partial pressure pp In this region the water vapor pressure
exceeds the admissible partial pressure at
Fig. 2.73 Areas of application for gas ballast pumps and condensers pumping water vapor (o.G. = without gas ballast) the inlet. The gas ballast pump must,

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therefore, have a condenser inserted at the Pumping of water vapor with roots pumps denser must decrease the vapor partial
inlet, which is so rated that the water vapor Normally, Roots pumps are not as pressure below 60 mbar. Hence, the gas
partial pressure at the inlet port of the economical as gas ballast pumps for ballast pump should be large enough only
rotary pump does not exceed the continuous operation at pressures above to prevent the air partial pressure behind
admissible value. The correct dimensions 40 mbar. With very large pump sets, which the intermediate condenser from ex-
of the condenser are selected depending work with very specialized gear ratios and ceeding a certain value; for example, if the
on the quantity of water vapor involved. are provided with bypass lines, however, total pressure behind the Roots pump
For further details, see Section 2.1.5. At a the specific energy consumption is indeed (which is always equal to the total
water vapor tolerance of 60 mbar, the more favorable. If Roots pumps are pressure behind the intermediate conden-
lower limit of this region is installed to pump vapors, as in the case of ser) is 133 mbar, the gas ballast pump
gas ballast pumps, a chart can be given must pump at least at a partial air pressure
pv > 6O + 0.46 pp mbar
that includes all possible cases (see Fig. of 73 mbar, the quantity of air transported
2.74). to it by the Roots pump. Otherwise, it must
Region C: Single-stage rotary plunger take in more water vapor than it can
pumps with a gas ballast. Region A: A Roots pump with a single- tolerate. This is a basic requirement: the
The lower limit of region C is characterized stage rotary plunger pump without gas use of gas ballast pumps is wise only if
by the lower limit of the working region of ballast. air is also pumped!
this pump. It lies, therefore, at about As there is merely a compression between
ptot = 1 mbar. If large quantities of vapor With an ideally leak-free vessel, the gas
the Roots pump and the rotary plunger
arise in this region, it is often more ballast pump should be isolated after the
pump, the following applies here too:
economical to insert a condenser: 20 kg of required operating pressure is reached and
vapor at 28 mbar results in a volume of pv < 0.46 pp pumping continued with the condenser
about 1000 m3. It is not sensible to pump only. Section 2.1.5 explains the best
The requirement is valid over the entire
this volume with a rotary pump. As a rule possible combination of pumps and
working region of the pump combination
of thumb: condensers.
and, therefore, for total pressures between
10-2 and 40 mbar (or 1013 mbar for Roots
A condenser should always be inserted at Region C: A Roots pump, an intermediate
pumps with a bypass line).
the pump’s inlet if saturated water vapor condenser, and a gas ballast pump.
arises for a considerable time. Region B: A main condenser, a Roots The lower limit of the water vapor partial
As a precaution, therefore, a Roots pump pump with a bypass line, an intermediate pressure is determined through the
should always be inserted in front of the condenser, and a gas ballast pump. compression ratio of the Roots pump at
condenser at low inlet pressures so that This combination is economical only if the backing pressure, which is determined
the condensation capacity is essentially large water vapor quantities are to be by the saturation vapor pressure of the
enhanced. The condensation capacity does pumped continuously at inlet pressures condensed water. Also, in this region the
not depend only on the vapor pressure, above about 40 mbar. The size of the main intermediate condenser must be able to
but also on the refrigerant temperature. At condenser depends on the quantity of reduce the vapor partial pressure to at
low vapor pressures, therefore, effective vapor involved. The intermediate con- least 60 mbar. The stated arrangement is
condensation can be obtained only if the
refrigerant temperature is correspondingly
low. At vapor pressures below 6.5 mbar,
for example, the insertion of a condenser
is sensible only if the refrigerant tempera-
ture is less than 0 °C. Often at low pres-
sures a gas – vapor mixture with
Water vapor partial pressure pv

unsaturated water vapor is pumped (for


further details, see Section 2.1.5). In
general, then, one can dispense with the
condenser.

Region D: Two-stage gas ballast pumps,


Roots pumps, and vapor ejector pumps,
always according to the total pressure 46
0.
=
concerned in the process. /p p
pv
It must again be noted that the water vapor
tolerance of two-stage gas ballast pumps
is frequently lower than that of correspon-
ding single-stage pumps.
Air
Air partial
partialpressure
pressurepp pp
D00
Fig. 2.74 Areas of application for Roots pumps and condensers pumping water vapor (o.G. = without gas ballast)

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suitable – when cooling the condenser E. If the drying process should terminate with known properties with that of a
with water at 15 °C – for water vapor at still lower pressures material with different properties.
pressures between about 4 and 40 mbar. When a pressure below 10-2 mbar is
reached a previously bypassed oil vapor Fundamentally, in the drying of a
Region D: A roots pump and a gas ballast ejector pump should be switched on in material, a few rules are noteworthy:
pump. addition. Experience has shown that shorter drying
In this region D the limits also depend times are obtained if the water vapor
essentially on the stages and ratios of Drying of solid substances partial pressure at the surface of the
sizes of the pumps. In general, however, As previously indicated, the drying of solid material is relatively high, that is, if the
this combination can always be used substances brings about a series of further surface of the material to be dried is not
between the previously discussed limits – problems. It no longer suffices that one yet fully free of moisture. This is possible
therefore, between 10-2 and 4 mbar. simply pumps out a vessel and then waits because the heat conduction between the
until the water vapor diffuses from the source of heat and the material is greater
solid substance. This method is indeed at higher pressures and the resistance to
technically possible, but it would intorably diffusion in a moist surface layer is smaller
increase the drying time. than in a dry one. To fulfill the conditions
2.2.4 Drying processes It is not a simple technical procedure to
of a moist surface, the pressure in the
drying chamber is controlled. If the neces-
Often a vacuum process covers several of keep the drying time as short as possible.
sary relatively high water vapor partial
the regions quoted here. In batch drying Both the water content and the layer thick-
pressure cannot be maintained perma-
the process can, for example (see Fig. ness of the drying substance are im-
nently, the operation of the condenser is
2.74), begin in region A (evacuation of the portant. Only the principles can be stated
temporarily discontinued. The pressure in
empty vessel) and then move through here. In case of special questions we
the chamber then increases and the
regions B, C, and D in steps. Then the advise you to contact our experts in our
surface of the material becomes moist
course of the process would be as follows: Cologne factory.
again. To reduce the water vapor partial
A. Evacuating the vessel by a gas ballast The moisture content E of a material to be pressure in the vessel in a controlled way,
pump and a Roots pump with a bypass dried of which the diffusion coefficient it may be possible to regulate the re-
line. depends on the moisture content (e.g. with frigerant temperature in the condenser. In
plastics) as a function of the drying time t this way, the condenser temperature
B. Connecting the two condensers is given in close approximation by the attains preset values, and the water vapor
because of the increasing vapor pressure following equation: partial pressure can be reduced in a con-
produced by heating the material. trolled manner.
The choice of the pumping System is E0
decided by the highest vapor partial E= % (2.31)
(1 + K · t )q
pressure occurring and the lowest air
partial pressure at the inlet.
E0 where E is the moisture content before
C. Bypassing the main condenser drying 2.2.5 Production of an oil-free
It will now not have an effect. Instead it q is the temperature-dependent coef- (hydrocarbon-free)
would only be pumped empty by the ficient. Thus equation (2.31) serves vacuum
pumping system with a further drop in only for the temperature at which q
vapor pressure. was determined Backstreaming vapor pump fluids, vapors
K is a factor that depends on the of oils, rotary pump lubricants, and their
D. Bypassing the intermediate condenser cracking products can significantly disturb
Roots pumps and gas ballast pumps alone temperature, the water vapor partial
pressure in the vicinity of the material, various working processes in vacuum.
can now continue pumping. With short- Therefore, it is recommended that certain
term drying, the separation of the the dimensions, and the properties of
the material. applications use pumps and devices that
condenser filled with condensed water is reliably exclude the presence of hydro-
particularly important, because the gas With the aid of this approximate equation, carbon vapors.
ballast pump would continue to pump the drying characteristics of many
from the condenser the previously substances can be assessed. If K and q a) Rough vacuum region
condensed water vapor at the saturation have been determined for various (1013 to 1 mbar)
vapor pressure of water. temperatures and water vapor partial Instead of rotary pumps, large water jet,
With longer-term drying processes, it pressures, the values for other steam ejector, or water ring pumps can be
suffices to shut off the condensate temperatures are easily interpolated, so used. For batch evacuation, and the pro-
collector from the condenser. Then only that the course of the drying process can duction of hydrocarbon-free fore vacuum
the remaining condensate film on the be calculated under all operating for sputter-ion pumps, adsorption pumps
cooling tubes can reevaporate. Depending conditions. With the aid of a similarity (see Section 2.1.8.1) are suitable. If the
on the size of the gas ballast pump, this transformation, one can further compare use of oil-sealed rotary vane pumps
reevaporation ensues in 30 – 60 min. the course of drying process of a material cannot be avoided, basically two-stage

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rotary vane pumps should be used. The pumps with diaphragm pumps or classic of the vacuum vessel and of the
small amount of oil vapor that back- turbomolecular pumps combined with attached components (e.g., connecting
streams out of the inlet ports of these scroll pumps should be used as oil-free tubulation; valves, seals) can be made
pumps can be almost completely removed backing pumps. extremely small,
by a sorption trap (see Section 2.1.4) c) suitable means (cold traps, baffles) are
inserted in the pumping line. provided to prevent gases or vapors or
their reaction products that have origi-
b) Medium vacuum region nated from the pumps used from
(1 to 10-3 mbar) 2.2.6 Ultrahigh vacuum reaching the vacuum vessel (no
For the pumping of large quantities of gas working Techniques backstreaming).
in this pressure region, vapor ejector
The boundary between the high and ultra- To fulfill these conditions, the individual
pumps are by far the most suitable. With
high vacuum region cannot be precisely components used in UHV apparatus must
mercury vapor ejector pumps, completely
defined with regard to the working me- be bakeable and extremely leaktight.
oil-free vacua can be produced. As a pre-
thods. In practice, a border between the Stainless steel is the preferred material for
caution, the insertion of a cold trap chilled
two regions is brought about because UHV components.
with liquid nitrogen is recommended so
that the harmful mercury vapor does not pressures in the high vacuum region may The construction, start-up, and operation
enter the vessel. With the medium vacuum be obtained by the usual pumps, valves, of an UHV system also demands special
sorption traps described under a), it is seals, and other components, whereas for care, cleanliness, and, above all, time. The
possible with two-stage rotary vane pressures in the UHV region, another assembly must be appropriate; that is, the
pumps to produce almost oil-free vacua technology and differently constructed individual components must not be in the
down to below 10-4 mbar. components are generally required. The least damaged (i.e. by scratches on
“border” lies at a few 10-8 mbar. Therefore, precision-worked sealing surfaces). Fun-
Absolutely oil-free vacua may be produced pressures below 10-7 mbar should ge- damentally, every newly-assembled UHV
in the medium vacuum region with nerally be associated with the UHV region. apparatus must be tested for leaks with a
adsorption pumps. Since the pumping
The gas density is very small in the UHV helium leak detector before it is operated.
action of these pumps for the light noble
region and is significantly influenced by Especially important here is the testing of
gases is only small, vessels initially filled
outgasing rate of the vessel walls and by demountable joints (flange connections),
with air can only be evacuated by them to
the tiniest leakages at joints. Moreover, in glass seals, and welded or brazed joints.
about 10-2 mbar. Pressures of 10-3 mbar
connection with a series of important After testing, the UHV apparatus must be
or lower can then be produced with
technical applications to characterize the baked out. This is necessary for glass as
adsorption pumps only if neither neon nor
UHV region, generally the monolayer time well as for metal apparatus. The bake-out
helium is present in the gas mixture to be
(see also equation 1.21) has become extends not only over the vacuum vessel,
pumped. In such cases it can be useful to
important. This is understood as the time t but frequently also to the attached parts,
expel the air in the vessel by first flooding
that elapses before a monomolecular or particularly the vacuum gauges. The
with nitrogen and then pumping it away.
monatomic layer forms on an initially individual stages of the bake-out, which
c) High- and ultrahigh vacuum region ideally cleaned surface that is exposed to can last many hours for a larger system,
and the bake-out temperature are arranged
(< 10-3 mbar) the gas particles. Assuming that every gas
particle that arrives at the surface finds a according to the kind of plant and the
When there is significant evolution of gas
free place and remains there, a convenient ultimate pressure required. If, after the
in the pressure regions that must be pum-
formula for τ is apparatus has been cooled and the other
ped, turbomolecular pumps, or cryo-
necessary measures undertaken (e.g.,
pumps should be used. A sputter-ion 3.2 – 6
pump is especially suitable for maintaining τ= · 10 s (p in mbar) cooling down cold traps or baffles), the
p
ultimate pressure is apparently not
the lowest possible pressure for long
obtained, a repeated leak test with a
periods in a sealed system where the Therefore, in UHV (p < 10-7 mbar) the helium leak detector is recommended.
process does not release large quantities monolayer formation time is of the order Details on the components, sealing
of gas. Magnetically-suspended turbomo- of minutes to hours or longer and thus of methods and vacuum gauges are provided
lecular pumps also guarantee hydrocar- the same length of time as that needed for in our catalog.
bon-free vacua. However, while these experiments and processes in vacuum.
pumps are switched off, oil vapors can The practical requirements that arise have
enter the vessel through the pump. By become particularly significant in solid-
suitable means (e.g., using an isolating state physics, such as for the study of thin
valve or venting the vessel with argon), films or electron tube technology. A UHV
contamination of the vessel walls can be system is different from the usual high
impeded when the pump is stationary. If vacuum system for the following reasons:
the emphasis is on generating a “hydroc-
arbon-free vacuum” with turbomolecular
a) the leak rate is extremely small (use of
metallic seals),
D00
pumps, then hybrid turbomolecular b) the gas evolution of the inner surfaces

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2.3. Evacuation of a quantities of gas and vapor at a certain


pressure.
V
Seff = · `n
t
1013 V
p
= · 2.3 · log
t
1013
p (2.34)
vacuum chamber 3. Pumping of the gases and vapors
produced during a process by variation Introducing the dimensionless factor
and determination of temperature and pressure.
1013 1013
of pump sizes Initial evacuation of a vacuum chamber is
σ = `n p = 2.3 · log p (2.34a)
influenced in the medium-, high-, and
Basically, two independent questions ultrahigh vacuum regions by continually into equation (2.34), the relationship
arise concerning the size of a vacuum evolving quantities of gas, because in between the effective pumping speed Seff,
system: these regions the escape of gases and and the pump-down time t is given by
1. What effective pumping speed must the vapors from the walls of the vessel is so V
pump arrangement maintain to reduce significant that they alone determine the Seff = · σ (2.35)
t
the pressure in a given vessel over a dimensions and layout of the vacuum
given time to a desired value? system. The ratio V/Seff is generally designated as
2. What effective pumping speed must the a time constant τ. Thus the pump-down
pump arrangement reach during a time of a vacuum chamber from
vacuum process so that gases and atmospheric pressure to a pressure p is
2.3.1 Evacuation of a vacuum given by:
vapors released into the vessel can be
quickly pumped away while a given chamber (without t=τ·s (2.36)
pressure (the operating pressure) in the additional sources of gas
vessel, is maintained and not or vapor) τ= V
with
exceeded? Seff
Because of the factors described above, an
During the pumping-out procedure of assessment of the pump-down time must
certain processes (e.g., drying and hea- be basically different for the evacuation of and σ = `n 1013
ting), vapors are produced that were not p
a container in the rough vacuum region
originally present in the vacuum chamber, from evacuation in the medium- and high The dependence of the factor from the
so that a third question arises: vacuum regions. desired pressure is shown in Fig. 2.75. It
3. What effective pumping speed must the should be noted that the pumping speed of
pump arrangement reach so that the single-stage rotary vane and rotary piston
process can be completed within a 2.3.1.1 Evacuation of a chamber in the pumps decreases below 10 mbar with gas
certain time? rough vacuum region ballast and below 1 mbar without gas
In this case the required effective pumping ballast. This fundamental behavior is
The effective pumping speed of a pump
speed Seff, of a vacuum pump assembly is different for pumps of various sizes and
arrangement is understood as the actual
pumping speed of the entire pump ar- dependent only on the required pressure
rangement that prevails at the vessel. p, the volume V of the container, and the
The nominal pumping speed of the pump pump-down time t.
can then be determined from the effective With constant pumping speed Seff and
pumping speed if the flow resistance assuming that the ultimate pressure pend
(conductances) of the baffles, cold traps, attainable with the pump arrangement is
filters, valves, and tubulations installed such that pend << p, the decrease with time
between the pump and the vessel are of the pressure p(t) in a chamber is given
known (see Sections 1.5.2 to 1.5.4). In the by the equation:
Pressure →

determination of the required nominal


pumping speed it is further assumed that dp Seff
− = ·p (2.32)
the vacuum system is leaktight; therefore, dt V
the leak rate must be so small that gases
Beginning at 1013 mbar at time t = 0, the
flowing in from outside are immediately
effective pumping speed is calculated
removed by the connected pump arrange-
depending on the pump-down time t from
ment and the pressure in the vessel does
equation (2.32) as follows:
not alter (for further details, see Section
5). The questions listed above under 1., 2. p dp Seff
and 3. are characteristic for the three most ∫ p =− ·t (2.33a) Dimensionless factor σ
1013 V
essential exercises of vacuum technology
Fig. 2.75 Dependency of the dimensionless factor s for
1. Evacuation of the vessel to reach a calculation of pumpdown time t according to
p S equation 2.36. The broken line applies to
specified pressure. `n = − eff · t (2.33b) single-stage pumps where the pumping
2. Pumping of continuously evolving 1013 V speed decreases below 10 mbar

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types but should not be ignored in the condition. Useful data are collected in A pumping speed of 100 l/s alone is
determination of the dependence of the Table X (Section 9). The gas evolution can required to continuously pump away the
pump-down time on pump size. It must be be determined experimentally only from quantity of gas flowing in through the
pointed out that the equations (2.32 to case to case by the pressure-rise method: leaks or evolving from the chamber walls.
2.36) as well Fig. 2.75 only apply when the the system is evacuated as thoroughly as Here the evacuation process is similar to
ultimate pressure attained with the pump possible, and finally the pump and the the examples given in Sections 2.3.1.1.
used is by several orders of magnitude chamber are isolated by a valve. Now the However, in the case of a diffusion pump
lower than the desired pressure. time is measured for the pressure within the pumping process does not begin at
the chamber (volume V) to rise by a atmospheric pressure but at the forevacu-
Example: A vacuum chamber having a
certain amount, for example, a power of um pressure pV instead. Then equation
volume of 500 l shall be pumped down to
10. The gas quantity Q that arises per unit (2.34) transforms into:
1 mbar within 10 minutes. What effective
time is calculated from:
pumping speed is required? p
Seff = V · `n V = V · `n K
500 l = 0.5 m3; 10 min = 1/6 h Q=
∆p · V t p t
t (2.37)
According to equation (2.34) it follows At a backing pressure of pV = 2 · 10-3 mbar
that: (∆p = measured pressure rise ) “compression” K is in our example:
0.5 1013 The gas quantity Q consists of the sum of 2 ⋅10 – 3
Seff = · 2.3 · log all the gas evolution and all leaks possibly K= = 200
1/ 6 1 1⋅10 – 5
= 3 · 2.3 · 3.01 = 20.8 m3/h present. Whether it is from gas evolution
or leakage may be determined by the In order to attain an ultimate pressure of
following method: 1 · 10-5 mbar within 5 minutes after
For the example given above one reads off
The gas quantity arising from gas evolu- starting to pump with the diffusion pump
the value of 7 from the straight line in Fig.
tion must become smaller with time, the an effective pumping speed of
2.75. However, from the broken line a
quantity of gas entering the system from 500 `
value of 8 is read off. According to Seff = · 2.3 · log 200 ≈ 9 s
equation (2.35) the following is obtained: leakage remains constant with time. 5 · 60
Experimentally, this distinction is not
0.5 always easily made, since it often takes a is required. This is much less compared to
Seff = · 7 = 21 m 3/ h or
1 considerable length of time – with pure the effective pumping speed needed to
6 gas evolution – before the measured pres- maintain the ultimate pressure. Pump-
0.5 sure-time curve approaches a constant (or
Seff = ·8 = 24 m 3/ h down time and ultimate vacuum in the
1 almost a constant) final value; thus the
6 high vacuum and ultrahigh vacuum ranges
beginning of this curve follows a straight depends mostly on the gas evolution rate
line for long times and so simulates and the leak rates. The underlying mathe-
under consideration of the fact that the
leakage (see Section 5, Leaks and Leak matical rules can not be covered here. For
pumping speed reduces below 10 mbar.
Detection). these please refer to books specializing on
The required effective pumping speed thus
that topic.
amounts to about 24 m3/h. If the gas evolution Q and the required
pressure pend are known, it is easy to de-
termine the necessary effective pumping
2.3.1.2 Evacuation of a chamber in the speed: 2.3.1.3 Evacuation of a chamber in the
high vacuum region medium vacuum region
Q In the rough vacuum region, the volume of
It is considerably more difficult to give Seff = (2.38)
pend the vessel is decisive for the time involved
general formulas for use in the high vacu-
um region. Since the pumping time to in the pumping process. In the high and
reach a given high vacuum pressure Example: A vacuum chamber of 500 l may ultrahigh vacuum regions, however, the
depends essentially on the gas evolution have a total surface area (including all gas evolution from the walls plays a
from the chamber’s inner surfaces, the systems) of about 5 m2. A steady gas significant role. In the medium vacuum
condition and pre-treatment of these evolution of 2 · 10-4 mbar · l/s is assumed region, the pumping process is influenced
surfaces are of great significance in per m2 of surface area. This is a level by both quantities. Moreover, in the
vacuum technology. Under no circums- which is to be expected when valves or medium vacuum region, particularly with
tances should the material used exhibit rotary feedthroughs, for example are rotary pumps, the ultimate pressure pend
porous regions or – particularly with connected to the vacuum chamber. In attainable is no longer negligible. If the
regard to bake-out – contain cavities; the order to maintain in the system a pressure quantity of gas entering the chamber is
inner surfaces must be as smooth as of 1 · 10-5 mbar, the pump must have a known to be at a rate Q (in millibars liter
possible (true surface = geometric sur-
face) and thoroughly cleaned (and
pumping speed of
5 · 2 ·10 – 4 mbar · `/ s
per second) from gas evolution from the
walls and leakage, the differential equation D00
degreased). Gas evolution varies greatly Seff = = 100 ` / s (2.32) for the pumping process becomes
1·10 – 5 mbar
with the choice of material and the surface

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S eff  p − p 
−Q
The required pumping speed of the 1·10 – 4
dp end  (2.39) backing pump is calculated from: SV = · 200 = 0.1 `/s = 0. 36 m 3/h
=− 2 ·10 – 1
dt V
pA
SV = ·S (2.41a)
Integration of this equation leads to pV eff Theoretically in this case a smaller backing
pump having a pumping speed of about 1
p − p  m3/h could be used. But in practice a
end  − Q / Seff
 o  Example: In the case of a diffusion pump
V 
t= `n larger backing pump should be installed
S p− p  − Q/S (2.40) having a pumping speed of 400 l/s the
eff   eff because, especially when starting up a
 end  effective pumping speed is 50 % of the
vacuum system, large amounts of gas may
value stated in the catalog when using a
where occur for brief periods. Operation of the
shell baffle. The max. permissible backing
p0 is the pressure at the beginning of the high vacuum pump is endangered if the
pressure is 2 · 10-1 mbar. The pumping
pumping process quantities of gas can not be pumped away
speed required as a minimum for the
p is the desired pressure immediately by the backing pump. If one
backing pump depends on the intake
works permanently at very low inlet pres-
In contrast to equation 2.33b this equation pressure pA according to equation 2.41a.
sures, the installation of a ballast volume
does not permit a definite solution for Seff,
At an intake pressure of pA = 1 · 10-2 mbar (backing-line vessel or surge vessel)
therefore, the effective pumping speed for
the pumping speed for the high vacuum between the high vacuum pump and the
a known gas evolution cannot be deter-
pump as stated in the catalog is about 100 backing pump is recommended. The
mined from the time – pressure curve
l/s, subsequently 50 % of this is 50 l/s. backing pump then should be operated for
without further information.
Therefore the pumping speed of the short times only. The maximum admis-
In practice, therefore, the following backing pump must amount to at least sible backing pressure, however, must
method will determine a pump with never be exceeded.
1·10 – 2
sufficiently high pumping speed: SV = · 50 = 2.5 `/s = 9 m 3/ h The size of the ballast volume depends on
a) The pumping speed is calculated from 2 ·10 – 1
the total quantity of gas to be pumped per
equation 2.34 as a result of the volume
At an intake pressure of pA = 1 · 10-3 mbar unit of time. If this rate is very low, the rule
of the chamber without gas evolution
the pump has already reached its nominal of thumb indicates that 0.5 l of ballast
and the desired pump-down time.
pumping speed of 400 l/s; the effective volume allows 1 min of pumping time with
b The quotient of the gas evolution rate
pumping speed is now Seff = 200 l/s; thus the backing pump isolated.
and this pumping speed is found. This
the required pumping speed for the
quotient must be smaller than the For finding the most adequate size of
backing pump amounts to
required pressure; for safety, it must be backing pump, a graphical method may be
about ten times lower. If this condition 1·10 – 3 used in many cases. In this case the
SV = · 200 = 1`/s = 3. 6 m 3/h
is not fulfilled, a pump with corres- 2 ·10 – 1 starting point is the pumping speed cha-
pondingly higher pumping speed must racteristic of the pumps according to
be chosen. If the high vacuum pump is to be used for equation 2.41.
pumping of vapors between 10-3 and
10-2 mbar, then a backing pump offering a The pumping speed characteristic of a
nominal pumping speed of 12 m3/h must pump is easily derived from the measured
be used, which in any case must have a pumping speed (volume flow rate)
2.3.2 Determination of a pumping speed of 9 m3/h at a pressure of characteristic of the pump as shown for a
suitable backing pump 2 · 10-1 mbar. If no vapors are to be 6000 l/s diffusion pump (see curve S in
pumped, a single-stage rotary vane pump Fig. 2.76). To arrive at the throughput
The gas or vapor quantity transported characteristic (curve Q in Fig. 2.76), one
through a high vacuum pump must also be operated without gas ballast will do in
most cases. If (even slight) components of must multiply each ordinate value of S by
handled by the backing pump. Moreover, its corresponding pA value and plotted
in the operation of the high vacuum pump vapor are also to be pumped, one should
in any case use a two-stage gas ballast against this value. If it is assumed that the
(diffusion pump, turbomolecular pump), inlet pressure of the diffusion pump does
the maximum permissible backing pump as the backing pump which offers –
also with gas ballast – the required not exceed 10-2 mbar, the maximum
pressure must never, even for a short time, throughput is 9.5 mbar · l/s
be exceeded. If Q is the effective quantity pumping speed at 2 · 10-1 mbar.
of gas or vapor, which is pumped by the If the high vacuum pump is only to be Hence, the size of the backing pump must
high vacuum pump with an effective used at intake pressures below 10-3 mbar, be such that this throughput can be
pumping speed Seff at an inlet pressure pA, a smaller backing pump will do; in the case handled by the pump at an intake pressure
this gas quantity must certainly be trans- of the example given this will be a pump (of the backing pump) that is equal to or
ported by the backing pump at a pumping offering a pumping speed of 6 m3/h. If the preferably lower than the maximum
speed of SV at the backing pressure pV. For continuous intake pressures are even permissible backing pressure of the dif-
the effective throughput Q, the continuity lower, below 10-4 mbar, for example, the fusion pump; that is, 4 · 10-1 mbar for the
equation applies: required pumping speed for the backing 6000 l/s diffusion pump.
Q = pA · Seff = pv · SV (2.41) pump can be calculated from equation After accounting for the pumping speed
2.41a as:
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characteristics of commercially available 2.3.3 Determination of pump- the pressure at which the Roots pump is
two-stage rotary plunger pumps, the down time from switched on.
throughput characteristic for each pump is
calculated in a manner similar to that used
nomograms In the medium vacuum region, the gas
evolution or the leak rate becomes
to find the Q curve for the diffusion pump In practice, for instance, when estimating
significantly evident. From the nomogram
in Fig. 2.76 a. The result is the group of Q the cost of a planned vacuum plant, cal-
9.10 in Section 9, the corresponding
curves numbered 1 – 4 in Fig. 2.76 b, culation of the pump-down time from the
calculations of the pump-down time in this
whereby four 2-stage rotary-plunger effective pumping speed Seff, the required
vacuum region can be approximated.
pumps were considered, whose nominal pressure p, and the chamber volume V by
speeds were 200, 100, 50, and 25 m3/h, formulas presented would be too trouble- In many applications it is expedient to
respectively. The critical backing pressure some and time-consuming. Nomograms relate the attainable pressures at any given
of the 6000 l/s diffusion pump is marked as are very helpful here. By using the nomo- time to the pump-down time. This is easily
V.B. (p = 4 · 10-1 mbar). Now the maximum gram in Fig. 9.7 in Section 9, one can possible with reference to the nomogram
throughput Q = 9.5 mbar · l/s is shown as quickly estimate the pump-down time for 9.7 in Section 9.
horizontal line a. This line intersects the vacuum plants evacuated with rotary
As a first example the pump-down cha-
four throughput curves. Counting from pumps, if the pumping speed of the pump
racteristic – that is, the relationship pres-
right to left, the first point of intersection concerned is fairly constant through the
sure p (denoted as desired pressure pend)
that corresponds to an intake pressure pressure region involved. By studying the
versus pumping time tp – is derived from
below the critical backing pressure of examples presented, one can easily under-
the nomogram for evacuating a vessel of
4 · 10-1 mbar is made with throughput stand the application of the nomogram.
5 m3 volume by the single-stage rotary
characteristic 2. This corresponds to the The pump-down times of rotary vane and plunger pump E 250 with an effective
two-stage rotary plunger pump with a rotary piston pumps, insofar as the pum- pumping speed of Seff = 250 m3/h and an
nominal pumping speed of 100 m3/h. ping speed of the pump concerned is con- ultimate pressure pend,p = 3 · 10-1 mbar
Therefore, this pump is the correct backing stant down to the required pressure, can when operated with a gas ballast and at
pump for the 6000 l/s diffusion pump be determined by reference to example 1. pend,p = 3 · 10-2 mbar without a gas ballast.
under the preceding assumption.
In general, Roots pumps do not have The time constant τ = V / Seff (see equation
However, if the pumping process is such constant pumping speeds in the working 2.36) is the same in both cases and
that the maximum throughput of 9.5 region involved. For the evaluation of the amounts as per nomogram 9.7 to about
mbar · l/s is unlikely, a smaller backing pump-down time, it usually suffices to 70 s (column 3). For any given value of
pump can, of course, be used. This is self- assume the mean pumping speed. pend > pend,p the straight line connecting
explanatory, for example, from line b in Examples 2 and 3 of the nomogram show, the “70 s point” on column 3 with the
Fig. 2.76 b, which corresponds to a in this context, that for Roots pumps, the (pend – pend,p) value on the right-hand
maximum throughput of only 2 mbar l/s. compression ratio K refers not to the scale of column 5 gives the corresponding
In this case a 25 m3/h two-stage rotary- atmospheric pressure (1013 mbar), but to tp value. The results of this procedure are
plunger pump would be sufficient. shown as curves a and b in Fig. 2.77.
Throughput Q [mbar · l · s–1]
Pumping speed S [l · s–1]

Q [mbar · l · s–1]

Intake pressure pa [mbar]

a) Pumping speed characteristic of a 6000 l/s diffusion pump b) Series of throughput curves for two-stage rotary
plunger pumps (V.B. = critical forevacuum pressure)
D00
Fig. 2.76 Diagram for graphically determining a suitable backing pump

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2001 / E 250 in Fig. 2.19), one introduces, evolving and pumped vapors is known.
as an approximation, average values of However, since this is seldom the case
Seff, related to defined pressure ranges. In except with drying processes, a quantita-
the case of the WA 1001/ E 250 tive consideration of this question is
combination the following average figures abandoned within the scope of this
apply: publication.
Seff = 800 m3/h in the range 10 – 1 mbar,
Seff = 900 m3/h in the range 1 mbar
to 5 · 10-2 mbar,
2.3.5 Selection of pumps for
Seff = 500 m3/h in the range 5 · 10-2 to drying processes
5 · 10-3 mbar
Fundamentally, we must distinguish bet-
The ultimate pressure of the combination
ween short-term drying and drying pro-
WA 1001 / E 250 is: Pend,p = 3 · 10-3 mbar.
cesses that can require several hours or
From these figures the corresponding time
even days. Independently of the duration
constants in the nomogram can be
of drying, all drying processes proceed
determined; from there, the pump-down
approximately as in Section 2.24
time tp can be found by calculating the
pressure reduction R on the left side of As an example of an application, the drying
column 5. The result is curve c in Fig. 2.77. of salt (short-term drying) is described,
this being an already well-proven drying
Computer aided calculations at LEYBOLD process.
Of course calculations for our industrial
systems are performed by computer Drying of salt
programs. These require high per- First, 400 kg of finely divided salt with a
formance computers and are thus usually water content of about 8 % by mass is to
not available for simple initial calculations. be dried in the shortest possible time
(about 1 h) until the water content is less
than 1 % by mass. The expected water
evolution amounts to about 28 kg. The salt
in the chamber is continuously agitated
2.3.4 Evacuation of a chamber
during the drying process and heated to
where gases and vapors about 80 °C. The vacuum system is
Fig. 2.77 Pumpdown time, tp, of a 5 m3 vessel using a are evolved schematically drawn in Fig. 2.78.
rotary plunger pump E 250 having a nominal
pumping speed of 250 m3/h with (a) and The preceding observations about the During the first quarter of drying time far
without (b) gas ballast, as well as pump-down time are significantly altered if more than half the quantity of water vapor
Roots/rotary plunger pump combination WA vapors and gases arise during the is evolved. Then the condenser is the
1001 / E250 for a cut-in pressure of 10 mbar evacuation process. With bake-out pro- actual main pump. Because of the high
for the WA 1001 (e)
cesses particularly, large quantities of water vapor temperature and, at the
vapor can arise when the surfaces of the beginning of the drying, the very high
It is somewhat more tedious to determine chamber are cleared of contamination. The water vapor pressure, the condensation
the (pend,tp) relationship for a combination resulting necessary pump-down time efficiency of the condenser is significantly
of pumps. The second example discussed depends on very different parameters. increased. In Fig. 2.78 it is understood that
in the following deals with evacuating a Increased heating of the chamber walls is two parallel condensers each of 1 m2 con-
vessel of 5 m3 volume by the pump accompanied by increased desorption of densation surface can together condense
combination Roots pump WA 1001 and gases and vapors from the walls. However, about 15 l of water at an inlet pressure of
the backing pump E 250 (as in the because the higher temperatures result in 100 mbar in 15 min. However, during this
preceding example). Pumping starts with an accelerated escape of gases and vapors initial process, it must be ensured that the
the E 250 pump operated without gas from the walls, the rate at which they can water vapor pressure at the inlet port of
ballast alone, until the Roots pump is be removed from the chamber is also in- the rotary piston pump does not exceed 60
switched on at the pressure of 10 mbar. As creased. mbar (see Section 2.15 for further details).
the pumping speed characteristic of the Since the backing pump has only to pump
combination WA 1001/ E 250 – in contrast The magnitude of the allowable tempera-
away the small part of the noncondensable
to the characteristic of the E 250 – is no ture for the bake-out process in question
gases at this stage, a single-stage rotary
longer a horizontal straight line over the will, indeed, be determined essentially by
piston pump TRIVAC S 65 B will suffice.
best part of the pressure range (compare the material in the chamber. Precise pump-
With increasing process time, the water
this to the corresponding course of the down times can then be estimated by
vapor evolution decreases, as does the
characteristic for the combination WA calculation only if the quantity of the

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water vapor pressure in the condenser. the desired pump-down time. This pump- pressure. The relationship between the
After the water pressure in the chamber down time is arranged according to the ultimate pressure and the remaining
falls below 27 mbar, the Roots pump (say, desired process duration: if the process is moisture is fixed for every product but dif-
a Roots pump RUVAC WA 501) is to be finished after 12 – 15 h, the pump- ferent from product to product. LEYBOLD
switched in. Thereby the water vapor is down time should not last longer than 1 h. has many years of experience to its record
pumped more rapidly out of the chamber, The size of the backing pump may be regarding applications in this area.
the pressure increases in the condensers, easily calculated according to Section Assume that a 0.1 % residual moisture
and their condensation efficiency again 2.3.1. content is required, for which the neces-
increases. The condensers are isolated by sary ultimate pressure is 6 · 10-2 mbar.
a valve when their water vapor reaches its 2. Predrying During the last 5 h the remaining 6 % of
saturation vapor pressure. At this point, During predrying – depending on the the moisture content, or 5 kg of water, is
there is a water vapor pressure in the pressure region in which the work is removed. At a mean pressure of about
chamber of only about 4 mbar, and carried out – about 75 % of the moisture is 0.65 mbar, 2000 m3/h of vapor is evolved.
pumping is accomplished by the Roots drawn off. This predrying should occupy Two possibilities are offered:
pump with a gas ballast backing pump the first third of the drying time. The rate at a) One continues working with the above-
until the water vapor pressure reaches which predrying proceeds depends almost mentioned Roots pump WA 1001. The
about 0.65 mbar. From experience it can exclusively on the sufficiency of the heat ultimate total pressure settles at a value
be assumed that the salt has now reached supply. For predrying 1 ton of paper in 5 h, according to the water vapor quantity
the desired degree of dryness. 60 kg of water must be evaporated; that is, evolving. One waits until a pressure of
an energy expenditure of about 40 kWh is about 6.5 · 10-2 mbar is reached, which
Drying of paper needed to evaporate water. Since the paper naturally takes a longer time.
If the pumps are to be of the correct size must be heated to a temperature of about b From the beginning, a somewhat larger
for a longer process run, it is expedient to 120 °C at the same time, an average of Roots pump is chosen (e.g., the
break down the process run into charac- about 20 kW must be provided. The mean RUVAC WA 2001 with a pumping speed
teristic sections. As an example, paper vapor evolution per hour amounts to of 2000 m3/h is suitable). For larger
drying is explained in the following where 12 kg. Therefore, a condenser with a capa- quantities of paper (5000 kg, for
the paper has an initial moisture content of city of 15 kg/h should be sufficient. If the example) such a pumping system will
8 %, and the vessel has the volume V. paper is sufficiently preheated (perhaps by be suitable which at a pumping speed
air-circulation drying) before evacuation, for water vapor of up to 20,000 m3/h
1. Evacuation in the first hour of drying, double vapor automatically lowers the pressure from
The backing pump must be suitably rated evolution must be anticipated. 27 to 10-2 mbar. The entire time need
with regard to the volume of the vessel and for drying is significantly reduced when
3. Main drying using such pumps.
If, in the second stage, the pressure in a
further 5 h is to fall from 20 to about
5.3 mbar and 75 % of the total moisture
(i.e., 19 % of the total moisture of 15 kg)
is to be drawn off, the pump must, accor- 2.3.6 Flanges and their seals
ding to equations (2.37) and (2.38), have a
In general, demountable joints in metallic
pumping speed of
vacuum components, pumps, valves,
V · ∆p tubulations, and so on are provided with
Seff = flanges. Vacuum components for rough,
t·p
medium, and high vacuum from LEYBOLD
According to equation 1.7, 15 kg of water are equipped with the following stan-
vapor corresponds at 15 °C to a quantity of dardized flange systems:
water vapor of • Small flanges (KF) (quick-action con-
m · R · T 15 ·83.14 · 288 ≈ nections to DIN 28 403) of nominal
V · ∆p = = widths 10, 16, 20, 25, 32, 40 and 50
M 18
mm. The values 10, 16, 25 and 40 are
1 Vacuum chamber with salt filling
≈ 20000 mbar · m3 subsequently
preferred widths according to the
2 RUVAC WA 501
PNEUROP recommendations and the
3 Condensers
20000 ISO recommendations of the technical
4 Throttle valve Seff = = 750 m 3/h
5 Rotary plunger pump 5 · 5. 3 committee ISO/TC 112 (see also Sec-
tion 11). For a complete connection of
Fig. 2.78 Vacuum diagram for drying of salt. Pump
combination consisting of Roots pump, con-
Hence the Roots pump RUVAC WA 1001
would be the suitable pump. The
two identical flanges one clamping ring
and one centering ring are required. D00
denser and rotary plunger pump for stepwise permissible remaining moisture in the
switching of the pumping process (see text) • Clamp flanges (ISO-K) of nominal
product determines the attainable ultimate
widths 65, 100, 160, 250, 320, 400,
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500 and 630 mm. Also, these flanges impairment. However, then Perbunan Valves are constructed so that they will not
correspond to the nominal widths and sealing material is not suitable as a flange throttle pumping speed. Hence, when
construction of the PNEUROP and sealant. Rather, VITILAN® (a special FPM) opened fully, their conductance in the
ISO/TC 112 recommendations. Clamp sealing rings and also aluminum seals, rough and medium vacuum regions equals
flanges are joined together by clamps which allow heating processes up to that of corresponding tube components.
or collar rings. Centering rings or gas- 150 °C and 200 °C respectively, should be For example, the conductance of a right-
kets are needed for sealing. used. After such degassing, pressures angle valve will equal the conductance of a
down to 10-8 mbar, i.e. down to the UHV bent tube of the same nominal bore and
• Bolted flanges (ISO-F) for the same
range, can be attained in vacuum systems. angle. Similarly, the conductance of the
nominal widths as above (according to
valve for molecular flow (i. e., in the high
PNEUROP and ISO/TC 112). In special Generating pressures below 10-8 mbar
and ultrahigh vacuum regions), is so high
cases bolted flanges having a smaller requires higher bake-out temperatures. As
that no significant throttling occurs. Actual
nominal width are used. Clamp flanges explained above (see Section 2.2.6) work
values for the conductance of various
and bolted flanges are in accordance in the UHV range requires a basically
components are given in the catalog.
with DIN 28 404. different approach and the use of CF
flanges fitted with metallic sealing rings. To meet stringent leak-tightness demands,
The nominal width is approximately equal
high-quality vacuum valves are designed
to the free inner diameter of the flange in
so that gas molecules adhering to the
millimeters; greater deviations are excep-
surface of the valve shaft are not
tions, so the clamp flange DN 63 has an
transferred from the outer atmosphere into
inner diameter of 70 mm. See also Table XI 2.3.7 Choice of suitable valves the vacuum during operation. Such valves
in Section 9).
are therefore equipped with metal bellows
Vacuum technology puts great demands
for isolating the valve shaft from the
High vacuum components are made of on the functioning and reliability of the
atmosphere, or alternatively, they are fully
aluminum or stainless steel. Stainless valves, which are often needed in large
encapsulated, that is, only static seals exist
steel is slightly more expensive but offers numbers in a plant. The demands are
between atmosphere and vacuum. This
a variety of advantages: lower degassing fulfilled only if correct shut-off devices are
group is comprised of all medium and high
rate, corrosion resistant, can be degassed installed for each application, depending
vacuum valves from LEYBOLD that are
at temperatures up to 200 °C, metal seals on the method of construction, method of
operated either manually or electro-
are possible and stainless steel is much operation, and size. Moreover, in the
pneumatically (Fig. 2.80) and (Fig. 2.79).
more resistant to scratching compared to construction and operation of vacuum
The leak rate of these valves is less than
aluminum. plants, factors such as the flow
10-9 mbar · l/s.
conductance and leak-tightness of valves
Ultrahigh vacuum components are made are of great importance. Valves sealed with oil or grease can be
of stainless steel and have CF flanges
bakeable to a high temperature. These
components, including the flanges, are
manufactured in a series production,
starting with a nominal width of 16 up to
250 mm. CF flanges are available as fixed
flanges or also with rotatable collar
flanges. They may be linked with CONFLAT
flanges from almost all manufacturers.
Copper gaskets are used for sealing
purposes.
Basically, the flanges should not be
smaller than the connecting tubes and the
components that are joined to them. When
no aggressive gases and vapors are
pumped and the vacuum system is not
exposed to a temperature above 80 °C,
sealing with NBR (Perbunan) or CR (Neo-
prene) flange O-rings is satisfactory for
work in the rough-, medium-, and high
vacuum regions. This is often the case 1 Casing 3 Compression spring 1 Casing 4 Compressed air supply
when testing the operation of vacuum 2 Valve disk 4 Solenoid coil 2 Valve disk 5 Piston
systems before they are finally assembled. 3 Bellows

All stainless steel flanges may be degassed Fig. 2.79 Right angle vacuum valve with Fig. 2.80 Right angle vacuum valve with
at temperatures up to 200 °C without solenoid actuator electropneumatic actuator

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Vacuum Generation Fundamentals of Vacuum Technology

used for highly stringent demands. Their Typical are variable leak valves, which 2.3.8 Gas locks and seal-off
leakage rate is also about 10-9 mbar · l/s. cover the leakage range from 10-10 cm3/s fittings
However, a special case is the pendulum- (NTP) up to 1.6 · 103 cm3/s (NTP). These
type gate valve. Despite its grease-covered valves are usually motor driven and In many cases it is desirable not only to be
seal, the leak rate between vacuum and suitable for remote control and when they able to seal off gas-filled or evacuated ves-
external atmosphere is virtually the same are connected to a pressure gauge, the sels, but also to be in a position to check
as for bellows-sealed valves because when process pressures can be set and the pressure or the vacuum in these
the valve is in operation the shaft carries maintained. Other special valves fulfill vessels at some later time and to post-eva-
out only a rotary motion so that no gas safety functions, such as rapid, automatic cuate or supplement or exchange the gas
molecules are transferred into the vacuum. cut-off of diffusion pumps or vacuum filling.
Pendulum-type gate valves are not manu- systems in the event of a power failure. For This can be done quite easily with a seal-off
factured by LEYBOLD. example, SECUVAC valves belong to this fitting from LEYBOLD which is actuated via
group. In the event of a power failure, they a corresponding gas lock. The small flange
For working pressures down to 10-7 mbar,
cut off the vacuum system from the connection of the evacuated or gas-filled
valves of standard design suffice because
pumping system and vent the forevacuum vessel is hermetically sealed off within the
their seals and the housing materials are
system. The vacuum system is enabled tube by a small closure piece which forms
such that permeation and outgassing are
only after a certain minimum pressure the actual valve. The gas lock required for
insignificant to the actual process. If
(about 200 mbar) has been attained once actuation is removed after evacuation or
pressures down to 10-9 mbar are required,
the power has been restored. filling with gas. Thus one gas lock will do to
baking up to 200 °C is usually necessary,
which requires heat resistant sealing When aggressive gases or vapors have to actuate any number of seal-off fittings.
materials (e.g., VITILAN®) and materials be pumped, valves made of stainless steel Shown in Fig. 2.81 is a sectional view of
of high mechanical strength, with prepared and sealed with VITILAN® sealant are such an arrangement. Gas locks and seal-
(inner) surfaces and a low outgassing rate. usually used. For nuclear technology, off fittings are manufactured by LEYBOLD
Such valves are usually made of stainless valves have been developed that are sealed having a nominal width of DN 16 KF, DN 25
steel. Flange connections are sealed with with special elastomer or metal gaskets. KF and DN 40 KF. They are made of stain-
aluminum gaskets, so permeation pro- We will be pleased to provide further less steel. The leak rate of the seal-off fit-
blems of elastomer seals are avoided. In design information for your area of tings is less than 1 · 10-9 mbar l/s. They
the UHV range these issues are of special application upon request. can sustain overpressures up to 2.5 bar,
significance so that mainly metallic seals are temperature resistant up to 150 °C and
must be used. The gas molecules bonded may be protected against dirt by a standard
to the surface of the materials have, at blank flange.
pressures below 10-9 mbar, a very great Typical application examples are double-
influence. They can only be pumped away walled vessels with an insulating vacuum,
within a reasonable period of time by like Dewar vessels, liquid gas vessels
simultaneous degassing. Degassing (tanks) or long distance energy pipelines
temperatures up to 500 °C required in UHV and many more. They are also used for
systems, pose special requirements on the evacuation or post-evacuation of reference
sealing materials and the entire sealing and support vacua in scientific instruments
geometry. Gaskets made of gold or copper seal-off fittings with gas locks are often
must be used. used. Previously it was necessary to have a
The various applications require valves pump permanently connected in order to
with different drives, that is, valves that are post-evacuate as required. Through the
manually operated, electropneumatically- use of gas locks with seal-off fittings a
or magnetically-operated, and motor vacuum-tight seal is provided for the
driven, such as variable-leak valves. The vessel and the pump is only required from
h
variety is even more enhanced by the time to time for checking or post-
various housing designs. In addition to the evacuation.
various materials used, right-angle and DN
straight-through valves are required.
a
Depending on their nominal width and
intended application, flanges fitted to
valves may be small (KF), clamp (ISO-K), a
bolted (ISO-F), or UHV (CF).
In addition to the vacuum valves, which h1 h2
perform solely an isolation function (fully
open – fully closed position), special
d D00
valves are needed for special functions. Fig. 2.81 Gas lock with centering ring and seal-off
fitting, sectional view

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Fundamentals of Vacuum Technology Vacuum Measurement

3. Vacuum 3.1 Fundamentals of


low-pressure
measurement,
measurement
monitoring,
Vacuum gauges are devices for measuring
control and gas pressures below atmospheric pressu-
re (DIN 28 400, Part 3, 1992 issue). In
regulation many cases the pressure indication
The pressures measured in vacuum tech- depends on the nature of the gas. With
Analogy analysis compression vacuum gauges it should be
nology today cover a range from 1013
mbar to 10-12 mbar, i.e. over 15 orders of
Determination by Absolute noted that if vapors are present, condensa-
means of pressure Length tion may occur due to the compression, as
magnitude. The enormous dynamics invol-
ved here can be shown through an analo-
empirical world a result of which the pressure indication is
of human beings 1 bar 1m falsified. Compression vacuum gauges
gy analysis of vacuum pressure measure-
simple measuring measure the sum of the partial pressures
ment and length measurement, as depic- methods > 1 mbar > 1 mm
ted in Table 3.1. of all gas components that do not conden-
mechanical se during the measurement procedure. In
Measuring instruments designated as measuring
the case of mechanically compressing
vacuum gauges are used for measurement methods > 10–3 mbar > 1 mm
pumps, the final partial pressure can be
in this broad pressure range. Since it is indirect measured in this way (see 1.1). Another
impossible for physical reasons to build a methods 10–9 mbar ≈ 1/100
way of measuring this pressure, is to free-
vacuum gauge which can carry out quanti- atom ∅
ze out the condensable components in an
tative measurements in the entire vacuum extreme indirect ≈ 0.18
LN2 cold trap. Exact measurement of par-
range, a series of vacuum gauges is avai- methods 10–12 mbar electron ∅
tial pressures of certain gases or vapors is
lable, each of which has a characteristic carried out with the aid of partial pressure
measuring range that usually extends over Table 3.1
measuring instruments which operate on
several orders of magnitude (see Fig. the mass spectrometer principle (see sec-
9.16a). In order to be able to allocate the tion 4).
largest possible measuring ranges to the
individual types of vacuum gauges, one Dependence of the pressure indication
accepts the fact that the measurement on the type of gas
uncertainty rises very rapidly, by up to A distinction must be made between the
100 % in some cases, at the upper and following vacuum gauges:
lower range limits. This interrelationship is 1. Instruments that by definition measure
shown in Fig. 3.1 using the example of the the pressure as the force which acts on
VISCOVAC. Therefore, a distinction must an area, the so-called direct or absolu-
be made between the measuring range as te vacuum gauges. According to the
stated in the catalogue and the measuring kinetic theory of gases, this force,
range for “precise” measurement. The which the particles exert through their
measuring ranges of the individual vacu- impact on the wall, depends only on the
um gauges are limited in the upper and number of gas molecules per unit volu-
lower range by physical effects. me (number density of molecules n)
and their temperature, but not on their
molar mass. The reading of the measu-
ring instrument is independent of the
Relative measurement uncertainty (%)

20 type of gas. Such units include liquid-


filled vacuum gauges and mechanical
“favorable measuring range”
15 vacuum gauges.
(relative measurement uncertainty < 5%)
2. Instruments with indirect pressure
10 measurement. In this case, the pressu-
re is determined as a function of a pres-
5
sure-dependent (or more accurately,
density-dependent) property (thermal
1 conductivity, ionization probability,
–6
10 10–5 10–4 10–3 10–2 10–1 1 electrical conductivity) of the gas.
Pressure (mbar) These properties are dependent on the
molar mass as well as on the pressure.
Fig. 3.1 Measurement uncertainty distribution over the measuring range: VISCOVAC

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Vacuum Measurement Fundamentals of Vacuum Technology

The pressure reading of the measuring vacuum ranges with a measurement (of the order of 10-2 to 10-1 l/s). Contami-
instrument depends on the type of gas. uncertainty of less than 50 %, the person nation of the measuring system, interfe-
conducting the experiment must proceed ring electrical and magnetic fields, insula-
The scales of these pressure measuring
with extreme care. Pressure measure- tion errors and inadmissibly high ambient
instruments are always based on air or
ments that need to be accurate to a few temperatures falsify pressure measure-
nitrogen as the test gas. For other gases or
percent require great effort and, in general, ment. The consequences of these avoida-
vapors correction factors, usually based
the deployment of special measuring ble errors and the necessary remedies are
on air or nitrogen, must be given (see
instruments. This applies particularly to all indicated in the discussion of the individu-
Table 3.2). For precise pressure measure-
pressure measurements in the ultrahigh al measuring systems and in summary
ment with indirectly measuring vacuum
vacuum range (p < 10-7 mbar). form in section 8.4.
gauges that determine the number density
through the application of electrical energy To be able to make a meaningful statement Selection of vacuum gauges
(indirect pressure measurement), it is about a pressure indicated by a vacuum The desired pressure range is not the only
important to know the gas composition. In gauge, one first has to take into account at factor considered when selecting a suita-
practice, the gas composition is known what location and in what way the measu- ble measuring instrument. The operating
only as a rough approximation. In many ring system is connected. In all pressure conditions under which the gauge works
cases, however, it is sufficient to know areas where laminar flows prevail also play an important role. If measure-
whether light or heavy molecules predomi- (1013 > p > 10-1 mbar), note must be ments are to be carried out under difficult
nate in the gas mixture whose pressure is taken of pressure gradients caused by operating conditions, i.e. if there is a high
to be measured (e.g. hydrogen or pump pumping. Immediately in front of the risk of contamination, vibrations in the
fluid vapor molecules). pump (as seen from the vessel), a lower tubes cannot be ruled out, air bursts can
pressure is created than in the vessel. Even be expected, etc., then the measuring
Given the presence Correction factor
components having a high conductance instrument must be robust. In industrial
of predominantly based on N2
may create such a pressure gradient. facilities, Bourdon gauges, diaphragm
(type of gas) (nitrogen = 1) Finally, the conductance of the connecting
He 6.9 vacuum gauges, thermal conductivity
line between the vacuum system and the vacuum gauges, hot cathode ionization
Ne 4.35 measuring system must not be too small
Ar 0.83 vacuum gauges and Penning vacuum gau-
because the line will otherwise be evacua- ges are used. Some of these measuring
Kr 0.59 ted too slowly in the pressure region of
Xe 0.33 instruments are sensitive to adverse ope-
laminar flow so that the indicated pressure rating conditions. They should and can
Hg 0.303 is too high.
H2 2.4 only be used successfully if the above
The situation is more complicated in the mentioned sources of errors are excluded
CO 0.92
case of high and ultrahigh vacuum. as far as possible and the operating
CO2 0.69
According to the specific installation fea- instructions are followed.
CH4 0.8
tures, an excessively high pressure or, in
higher the case of well-degassed measuring
hydrocarbons 0.1 – 0.4 tubes, an excessively low pressure may be
recorded due to outgassing of the walls of
Table 3.2 Correction factors the vacuum gauge or inadequate degas-
sing of the measuring system. In high and
Example: If the pressure of a gas essenti- ultrahigh vacuum, pressure equalization
ally consisting of pump fluid molecules is between the vacuum system and the mea-
measured with an ionization vacuum suring tubes may take a long time. If pos-
gauge, then the pressure reading (applying sible, so-called nude gauges are used. The
to air or N2), as shown in Table 3.2, is too latter are inserted directly in the vacuum
high by a factor of about 10. system, flange-mounted, without a
connecting line or an envelope. Special
Measurement of pressures in the rough consideration must always be given to the
vacuum range can be carried out relatively influence of the measuring process itself
precisely by means of vacuum gauges with on the pressure measurement. For exam-
direct pressure measurement. Measure- ple, in ionization vacuum gauges that work
ment of lower pressures, on the other with a hot cathode, gas particles, especial-
hand, is almost always subject to a num- ly those of the higher hydrocarbons, are
ber of fundamental errors that limit the thermally broken down. This alters the gas
measuring accuracy right from the start so composition. Such effects play a role in
that it is not comparable at all to the
degree of accuracy usually achieved with
connection with pressure measurement in
the ultrahigh vacuum range. The same D00
measuring instruments. In order to mea- applies to gas clean-up in ionization vacu-
sure pressure in the medium and high um gauges, in particular Penning gauges

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Fundamentals of Vacuum Technology Vacuum Measurement

3.2 Vacuum gauges 3.2.2 Diaphragm vacuum The closure to the vessel is in the form of a
corrugated diaphragm (4) of special steel.
gauges
with pressure As long as the vessel is not evacuated, this
diaphragm is pressed firmly against the
reading that is 3.2.2.1 Capsule vacuum gauges
wall (1). As evacuation increases, the diffe-
independent of the The best-known design of a diaphragm rence between the pressure to be measu-
vacuum gauge is a barometer with an red px and the reference pressure decrea-
type of gas aneroid capsule as the measuring system. ses. The diaphragm bends only slightly at
It contains a hermetically sealed, evacu- first, but then below 100 mbar to a greater
Mechanical vacuum gauges measure the ated, thin-walled diaphragm capsule made degree. With the DIAVAC the diaphragm
pressure directly by recording the force of a copper-beryllium alloy. As the pressu- deflection is again transmitted to a pointer
which the particles (molecules and atoms) re drops, the capsule diaphragm expands. (9). In particular the measuring range bet-
in a gas-filled space exert on a surface by This movement is transmitted to a point by ween 1 and 20 mbar is considerably exten-
virtue of their thermal velocity. a lever system. The capsule vacuum ded so that the pressure can be read quite
gauge, designed according to this princi- accurately (to about 0.3 mbar). The sensi-
ple, indicates the pressure on a linear tivity to vibration of this instrument is
scale, independent of the external atmos- somewhat higher than for the capsule
3.2.1 Bourdon vacuum gauges pheric pressure. vacuum gauge.

The interior of a tube bent into a circular


arc (so-called Bourdon tube) (3) is 3.2.2.2 DIAVAC diaphragm vacuum 3.2.2.3 Precision diaphragm vacuum
connected to the vessel to be evacuated gauge gauges
(Fig. 3.2). Through the effect of the exter-
The most accurate pressure reading possi- A significantly higher measuring accuracy
nal air pressure the end of the tube is
ble is frequently required for levels below than that of the capsule vacuum gauge and
deflected to a greater or lesser extent
50 mbar. In this case, a different diaphragm the DIAVAC is achieved by the precision
during evacuation and the attached pointer
vacuum gauge is more suitable, i.e. the diaphragm vacuum gauge. The design of
mechanism (4) and (2) is actuated. Since
DIAVAC, whose pressure scale is consider- these vacuum gauges resembles that of
the pressure reading depends on the exter-
ably extended between 1 and 100 mbar. capsule vacuum gauges. The scale is line-
nal atmospheric pressure, it is accurate
The section of the interior in which the ar. The obtainable degree of precision is
only to approximately 10 mbar, provided
lever system (2) of the gauge head is loca- the maximum possible with present-day
that the change in the ambient atmosphe-
ted (see Fig. 3.3) is evacuated to a referen- state-of-the-art equipment. These instru-
ric pressure is not corrected.
ce pressure pref of less than 10-3 mbar. ments permit measurement of 10-1 mbar
with a full-scale deflection of 20 mbar. The
greater degree of precision also means a
higher sensitivity to vibration.
Capsule vacuum gauges measure pressu-
re accurately to 10 mbar (due to the linear
scale, they are least accurate at the low
pressure end of the scale). If only pressu-
res below 30 mbar are to be measured, the
DIAVAC is recommended because its rea-
ding (see above) is considerably more
accurate. For extremely precise measuring
accuracy requirements precision dia-
phragm vacuum gauges should be used. If
low pressures have to be measured accu-
rately and for this reason a measuring
range of, for example, up to 20 mbar is
selected, higher pressures can no longer
be measured since these gauges have a
1 Base plate 7 Mirror sheet linear scale. All mechanical vacuum gau-
1 Connecting tube to 2 Lever system 8 Plexiglass sheet ges are sensitive to vibration to some
connection flange 3 Connecting flange 9 Pointer
2 Pointer 4 Diaphragm 10 Glass bett
extent. Small vibrations, such as those that
3 Bourdon tube 5 Reference 11 Mounting plate arise in the case of direct connection to a
4 Lever system pressure pref, 12 Housing backing pump, are generally not detrimen-
6 Pinch-off end tal.
Fig. 3.3 Cross-section of DIAVAC DV 1000
Fig. 3.2 Cross-section of a Bourdon gauge diaphragm vacuum gauge

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Vacuum Measurement Fundamentals of Vacuum Technology

1 2

C1 C2

p1 p2

Fig. 3.4 Piezoelectric sensor (basic diagram) Fig. 3.5 Capacitive sensor (basic diagram)

3.2.2.4 Capacitance diaphragm capacitance of a plate capacitor: one elec- If the pressures to be measured exceed
gauges trode is fixed, the other is formed by the these range limits, it is recommended that
diaphragm. When the diaphragm is deflec- a multichannel unit with two or three sen-
Deflection of a diaphragm can also be elec-
ted, the distance between the electrodes sors be used, possibly with automatic
trically measured as “strain” or as a chan-
and thus capacitance of the capacitor is channel changeover. The capacitance dia-
ge in capacitance. In the past, four strain
altered. Fig. 3.5 illustrates the principle of phragm gauge thus represents, for all
gauges, which change their resistance
this arrangement. A distinction is made practical purposes, the only absolute pres-
when the diaphragm is deflected, i.e.
between sensors with metallic and those sure measuring instrument that is inde-
under tensile load, were mounted on a
with ceramic diaphragms. The structure of pendent of the type of gas and designed
metallic diaphragm in a bridge circuit. At
the two types is similar and is shown on for pressures under 1 mbar. Today two
LEYBOLD such instruments have been
the basis of two examples in Fig. 3.6. types of capacitive sensors are available:
given a special designation, i.e.
Capacitance diaphragm gauges are used 1) Sensors DI 200 and DI 2000 with
MEMBRANOVAC. Later, silicon dia-
from atmospheric pressure to 1·10-3 mbar aluminum oxide diaphragms, which are
phragms that contained four such “strain
(from 10-4 mbar the measurement uncer- particularly overload-free, with the
resistances” directly on their surface were
tainty rises rapidly). To ensure sufficient MEMBRANOVAC DM 11 and DM 12
used. The electrical arrangement again
deflection of the diaphragms at such low units.
consisted of a bridge circuit, and a con-
pressures, diaphragms of varying thickn- 2) Sensors with Inconel diaphragms CM 1,
stant current was fed in at two opposite
esses are used for the various pressure DM 10, CM 100, CM 1000 with extre-
corner points while a linear voltage signal
levels. In each case, the pressure can be mely high resolution, with the DM 21
proportional to the pressure was picked up
measured with the sensors to an accuracy and DM 22 units.
at the two other corner points. Fig. 3.4 illu-
of 3 powers of ten:
strates the principle of this arrangement.
1013 to 1 mbar
Such instruments were designated as
100 to 10–1 mbar
PIEZOVAC units and are still in use in
10 to 10–2 mbar und
many cases. Today the deflection of the
1 to 10–3 mbar.
diaphragm is measured as the change in

C ~ A/d
C = capacitance Diaphragm
A = area (Inconel) Reference chamber closure
d = distance C ~ A/d
C = capacitance
Grid + reference chamber A = area
closure d = distance
Amplifier + 15 V DC Capacitor plates
Diaphragm
Sensor body Signal converter
– 15 V DC (ceramic)
(ceramic) + amplifier
0 – 10 V

Electrode 24 V DC, 4 – 20 mA

left: CAPACITRON (Inconel diaphragm) right: MEMBRANOVAC (aluminum oxide diaphragm)


D00
Fig. 3.6 Capacitive sensors (basic diagram)

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Fundamentals of Vacuum Technology Vacuum Measurement

3.2.3 Liquid-filled (mercury) racy. The pressure is measured by com- Principle of measurement with compres-
vacuum gauges pressing a quantity of gas that initially sion vacuum gauges
occupies a large volume into a smaller If h is the difference in the mercury level
3.2.3.1 U-tube vacuum gauges volume by raising a mercury level. The between the measurement capillary and
increased pressure obtained in this man- the reference capillary (measured in mm),
U-tube vacuum gauges filled with mercury ner can be measured in the same way as in then it follows from the Boyle-Mariotte
are the simplest and most exact instru- a U-tube manometer and from it the origi- law:
ments for measuring pressure in the rough nal pressure is calculated (see equations
vacuum range (1013 to a few mbar). p · V = (p + h) · Vc (3.1)
below).
Unfortunately their use in technical plants
According to the type of scale division, a Vc
is limited because of their size and pro- p = h⋅ (3.1a)
distinction is made between two forms of V − Vc
neness to breakage (see 3.4.1a).
compression vacuum gauges: those with a
In the evacuated limb of the U-tube vacu- linear scale (see Fig. 3.7) and those with a p measured in mm of mercury (= torr).
um gauge a constant pressure is maintai- square-law scale (see Fig. 3.8). In the case If Vc << V, then:
ned equal to the vapor pressure of mercu- of the compression vacuum gauges of the
ry at room temperature (about 10-3 mbar). Vc
McLeod linear-scale type, the ratio of the p = h⋅ (3.1b)
The other limb is connected to the volume enclosed residual volume Vc to the total V
in which the pressure is to be measured. volume V must be known for each height Vc and V must be known, h is read off
From the difference in the levels of the two of the mercury level in the measurement
columns, the pressure to be measured can (linear scale).
capillary; this ratio is shown on the scale
be determined on the mbar scale provided. provided with the instrument. In the case These relationships remain unchanged if
The reading is independent of the atmos- of compression vacuum gauges with a the difference in level is read off a scale
pheric pressure. square-law scale, the total volume and the with mbar division. The pressure is then
capillary diameter d must be known. obtained in mbar:
3.2.3.2 Compression vacuum gauges Nowadays a “shortened” McLeod type
compression vacuum gauge according to p = 4 ⋅ h ⋅ Vc h in mm (3.1c)
(according to McLeod) 3 V
Kammerer is used to measure the “partial
The compression vacuum gauge develo- final pressure” of mechanically com- If during measurement the mercury level
ped by McLeod in 1874 is a very rarely pressing pumps. Through the high degree in the measurement capillary is always set
used type of vacuum gauge today. In its of compression the condensable gas com- so that the mercury level in the reference
refined form the instrument can be used ponents (vapors) are discharged as liquid capillary corresponds to the upper end of
for absolute pressure measurement in the (the volume of the same mass is then the measurement capillary (see Figs. 3.7
high vacuum range down to 10-5 mbar. In smaller by a factor of around 105 and can and 3.8), the volume Vc is always given by:
the past it was frequently used as a refe-
rence instrument for the calibration of
be neglected in the measurement) so that Vc = h ⋅ π ⋅ d 2 (3.1d)
only the pressure of the permanently 4
medium and sometimes also of high vacu- gaseous components is measured (this is
um gauges. For such measurements, where the expression permanent gases h ....difference in level, see Fig. 3.5
however, numerous precautionary rules comes from). d ....inside diameter of measurement
had to be taken into account before it was capillary
possible to assess the measuring accu-

torr Upper limit for: torr


Vcmax. = 1 cm3
hmax. = 100 mm Upper limit for:
d = 2.5 mm
Upper limit for:
Vcmax. = 0.1 cm3 Upper limit for:
measuring
measuring

hmax. = 100 mm d = 1 mm
range
range
Pressure p

Lower limit for:


d = 2.5 mm
measuring
range

measuring
range

Lower limit for:


Lower limit for:
Vcmin. = 5 · 10–3 cm3
d = 1 mm
hmin. = 1 mm

Volume V [cm3] Volume V [cm3]

Fig. 3.7 McLeod compression vacuum gauge with linear scale (equation 3.1b) Fig. 3.8 McLeod compression vacuum gauge with square-law scale (equation 3.1f)

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If this term is substituted for Vc in equati- 3.3 Vacuum gauges vided until after supply of this signal to the
on (3.1b), the result is: computer and processing by the appro-
with priate software and is then displayed direc-
p = h2 ⋅ π ⋅ d
2
(3.1e) tly on the screen.
4 V gas-dependent
that is, a square-law scale in mm (torr) if d
pressure reading
and V are measured in mm or mm3. If the This type of vacuum gauge does not mea- 3.3.1 Spinning rotor gauge
scale is to be divided into mbar, then the sure the pressure directly as an area-rela-
equation is: (SRG) (VISCOVAC)
ted force, but indirectly by means of other
physical variables that are proportional to Pressure-dependent gas friction at low gas
p = h2 ⋅ π ⋅ d
2
(3.1f) the number density of particles and thus to pressures can be utilized to measure pres-
3 V
the pressure. The vacuum gauges with sures in the medium and high vacuum
where h in mm gas-dependent pressure reading include: range. In technical instruments of this kind
d in mm the decrement gauge (3.3.1), the thermal a steel ball that has a diameter of several
and V in mm3 conductivity vacuum gauge (3.3.2) and the millimeters and is suspended without
ionization vacuum gauge having different contact in a magnetic field (see Fig. 3.9) is
Compression vacuum gauges ensure a designs (3.3.3). used as the measuring element. The ball is
reading of the sum of all partial pressures set into rotation through an electro-
of the permanent gases, provided that no The instruments consist of the actual sen-
magnetic rotating field: after reaching a
vapors are present that condense during sor (gauge head, sensor) and the control
starting speed (around 425 Hz), the ball is
the compression procedure. unit required to operate it. The pressure
left to itself. The speed then declines at a
scales or digital displays are usually based
The measuring range between the top and rate that depends on the prevailing pressu-
on nitrogen pressures; if the true pressure
bottom ends is limited by the maximum re under the influence of the pressure-
pT of a gas (or vapor) has to be determi-
and minimum ratios of the capillary volu- dependent gas friction. The gas pressure
ned, the indicated pressure pI must be
me to the total volume (see Figs. 3.7 and is derived from the relative decline of the
multiplied by a factor that is characteristic
3.8). The accuracy of the pressure mea- speed f (slowing down) using the follo-
for this gas. These factors differ, depen-
surement depends to a great extent on the wing equation:
ding on the type of instrument, and are eit-
reading accuracy. By using a vernier and her given in tabular form as factors inde- df 10 p ⋅ σ
−f ⋅ = ⋅
mirror, pressure measurements with an pendent of pressure (see Table 3.2) or, if dt π c ⋅ r ⋅ ρ (3.2)
accuracy of ± 2 % can be achieved. In the they depend on the pressure, must be
low pressure range, where h is very small, determined on the basis of a diagram (see p =
gas pressure
this accuracy is no longer attainable, chief- Fig. 3.11). r =
radius of the ball
ly because small geometric deviations ρ =
density of the ball material
have a very noticeable effect at the closed In general, the following applies: -c =
mean speed of the gas particles,
end of the capillary (systematic error). True pressure dependent on type of gas
The presence of vapors that may conden- pT = indicated pressure pI · correction factor σ = coefficient of friction of the ball, inde-
se during compression influences the pendent of the type of gas, nearly 1.
If the pressure is read off a “nitrogen
measurement, often in an indefinite man-
scale” but not corrected, one refers to
ner. One can easily determine whether
“nitrogen equivalent” values.
vapors having a pressure that is not negli-
gible are present. This can be done by set- In all electrical vacuum gauges (they inclu-
ting different heights h in the measure- de vacuum gauges that are dependent on
ment capillary under constant pressure the type of gas) the increasing use of com-
while using the linear scale and then cal- puters has led to the wish to display the
culating p according to equation 3.1b. If no pressure directly on the screen, e.g. to ins-
vapors are present, or only those whose ert it at the appropriate place in a process
pressure is negligible at room temperature flow diagram. To be able to use the most
(such as mercury), then the same value of standardized computer interfaces possi-
p must result for each h. ble, so-called transmitters (signal conver-
ters with standardized current outputs) are
The scale of compression vacuum gauges
built instead of a sensor and display unit 1 Ball 3 Permanent magnets
can be calculated from the geometric 2 Measuring tube, 4 Stabilization coils
(e.g. THERMOVAC transmitter, Penning
dimensions. This is why they were used in closed at one end, 5 4 drive coils
transmitter, IONIVAC transmitter). Trans- welded into 6 Bubble level
the past by official calibration stations as
mitters require a supply voltage (e.g. +24 connection flange 7 7 Connection flange
normal pressure (see equation 3.4.1a).
volts) and deliver a pressure-dependent
current signal that is linear over the entire Fig. 3.9 Cross-section of the gauge head of a
D00
measuring range from 4 to 20 mA or VISCOVAC VM 212 spinning rotor gauge
(SRG)
0 – 10 V. The pressure reading is not pro-
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Fundamentals of Vacuum Technology Vacuum Measurement

As long as a measurement uncertainty of 3.3.2 Thermal conductivity dent on the density and thus on the pres-
3 % is sufficient, which is usually the case, vacuum gauges sure. Below 10-3 mbar the mean free path
one can apply σ = 1 so that the sensitivity of a gas roughly corresponds to the size of
of the spinning rotor gauge (SRG) with Classical physics teaches and provides radius r2 of the measuring tubes. The sen-
rotating steel ball is given by the calculable experimental confirmation that the thermal sing filament in the gauge head forms a
physical size of the ball, i.e. the product conductivity of a static gas is independent branch of a Wheatstone bridge. In the
radius x density r · ρ (see equation 3.2). of the pressure at higher pressures (par- THERMOTRON thermal conductivity gau-
Once a ball has been “calibrated”, it is sui- ticle number density), p > 1 mbar. At lower ges with variable resistance which were
table for use as a “transfer standard”, i.e. pressures, p < 1 mbar, however, the ther- commonly used in the past, the sensing
as a reference device for calibrating ano- mal conductivity is pressure-dependent filament was heated with a constant cur-
ther vacuum gauge through comparison, (approximately proportional 1 / AD M). It de- rent. As gas pressure increases, the tem-
and is characterized by high long-term sta- creases in the medium vacuum range star- perature of the filament decreases because
bility. Measurements with the VISCOVAC ting from approx. 1 mbar proportionally to of the greater thermal conduction through
are not limited to measurement of the the pressure and reaches a value of zero in the gas so that the bridge becomes out of
pressure, however. Other variables invol- the high vacuum range. This pressure balance. The bridge current serves as a
ved in the kinetic theory of gases, such as dependence is utilized in the thermal con- measure for the gas pressure, which is
mean free path, monolayer time, particle ductivity vacuum gauge and enables preci- indicated on a measuring scale. In the
number density and impingement rate, can se measurement (dependent on the type of THERMOVAC thermal conductivity gau-
also be measured. The instrument permits gas) of pressures in the medium vacuum ges with constant resistance which are
storage of 10 programs and easy change- range. almost exclusively built today, the sensing
over between these programs. The measu- The most widespread measuring instru- filament is also a branch of a Wheatstone
ring time per slowing-down operation is ment of this kind is the Pirani vacuum bridge. The heating voltage applied to this
between 5 seconds for high pressures and gauge. A current-carrying filament with a bridge is regulated so that the resistance
about 40 seconds for lower pressures. The radius of r1 heated up to around 100 to and therefore the temperature of the fila-
measurement sequence of the instrument 150 °C (Fig. 3.10) gives off the heat gene- ment remain constant, regardless of the
is controlled fully automatically by a rated in it to the gas surrounding it heat loss. This means that the bridge is
microprocessor so that a new value is dis- through radiation and thermal conduction always balanced. This mode of regulation
played after every measurement (slowing- (as well as, of course, to the supports at involves a time constant of a few millise-
down procedure). The programs additio- the filament ends). In the rough vacuum conds so that such instruments, in con-
nally enable calculation of a number of sta- range the thermal conduction through gas trast to those with variable resistance, res-
tistical variables (arithmetic mean, stan- convection is virtually independent of pond very quickly to pressure changes.
dard deviation) after a previously specified pressure (see Fig. 3.10). If, however, at a The voltage applied to the bridge is a mea-
number of measurements. few mbar, the mean free path of the gas is sure of the pressure. The measuring volta-
of the same order of magnitude as the fila- ge is corrected electronically such that an
While in the case of the kinetic theory of
ment diameter, this type of heat transfer approximately logarithmic scale is obtai-
gases with VISCOVAC the counting of par-
declines more and more, becoming depen- ned over the entire measuring range. Ther-
ticles directly represents the measuring
principle (transferring the particle pulses
to the rotating ball, which is thus slowed
down). With other electrical measuring I II III
methods that are dependent on the type of
gas, the particle number density is measu-
r2 -
red indirectly by means of the amount of l ‹‹ r – r
Wärmefluß

r1 - 2 1
heat lost through the particles (thermal - l ‹‹ r1
l # r2
conductivity vacuum gauge) or by means
Heat loss

-
of the number of ions formed (ionization l ›› r1
Abgeführter

vacuum gauge).

10–5 10–4 10–3 10–2 10–1 1 10 100


Druck
Pressure [mbar]
[mbar]

I Thermal dissipation due to radiation and conduction in the metallic ends


II Thermal dissipation due to the gas, pressure-dependent
III Thermal dissipation due to radiation and convection
Fig. 3.10 Dependence of the amount heat dissipated by a heated filament (radius r1) in a tube (radius r2) at a constant
temperature difference on the gas pressure (schematic diagram)

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mal conductivity vacuum gauges with con- pheric pressure” pT with a THERMOVAC as is proportional to the particle number den-
stant resistance have a measuring range a pressure measuring instrument. Argon sity and thus to the pressure.
from 10-4 to 1013 mbar. Due to the very might escape from the vessel (cover
The formation of ions is a consequence of
short response time, they are particularly opens, bell jar rises). For such and similar
either a discharge at a high electric field
suitable for controlling and pressure moni- applications, pressure switches or vacuum
strength (so-called cold-cathode or Pen-
toring applications (see section 3.5). The gauges that are independent of the type of
ning discharge, see 3.3.3.1) or the impact
measurement uncertainty varies in the dif- gas must be used (see section 3.2).
of electrons that are emitted from a hot
ferent pressure ranges. The maximum
cathode (see 3.3.3.2).
error at full-scale deflection is about 1 to
2 %. In the most sensitive range, i.e. bet- Under otherwise constant conditions, the
ween 10-3 and 1 mbar, this corresponds to ion yield and thus the ion current depend
around 10 % of the pressure reading. The 3.3.3 Ionization vacuum on the type of gas since some gases are
measurement uncertainty is significantly gauges easier to ionize than others. As all vacuum
greater outside this range. gauges with a pressure reading that is
Ionization vacuum gauges are the most dependent on the type of gas, ionization
As in all vacuum gauges dependent on the important instruments for measuring gas vacuum gauges are calibrated with nitro-
type of gas, the scales of the indicating pressures in the high and ultrahigh vacu- gen as the reference gas (nitrogen equiva-
instruments and digital displays in the um ranges. They measure the pressure in lent pressure, see 3.3). To obtain the true
case of thermal conductivity vacuum gau- terms of the number density of particles pressure for gases other than nitrogen, the
ges also apply to nitrogen and air. Within proportional to the pressure. The gas read-off pressure must be multiplied by
the limits of error, the pressure of gases whose pressure is to be measured enters the correction factor given in Table 3.2 for
with similar molecular masses, i.e. O2, CO the gauge heads of the instruments and is the gas concerned. The factors stated in
and others, can be read off directly. Cali- partially ionized with the help of an electric Table 3.2 are assumed to be independent
bration curves for a series of gases are field. Ionization takes place when electrons of the pressure, though they depend
shown in Fig. 3.11. are accelerated in the electric field and somewhat on the geometry of the electro-
An extreme example of the discrepancy attain sufficient energy to form positive de system. Therefore, they are to be regar-
between true pressure pT and indicated ions on impact with gas molecules. These ded as average values for various types of
pressure pI in pressure measurement is ions transmit their charge to a measuring ionization vacuum gauges (see Fig. 3.16).
the admission of air to a vacuum system electrode (ion collector) in the system. The
with argon from a pressure cylinder to ion current, generated in this manner (or,
avoid moisture (pumping time). According more precisely, the electron current in the 3.3.3.1 Cold-cathode ionization
to Fig. 3.11, one would obtain a pI reading feed line of the measuring electrode that is vacuum gauges (Penning
of only 40 mbar on reaching an “Ar atmos- required to neutralize these ions) is a mea- vacuum gauges)
sure of the pressure because the ion yield
Ionization vacuum gauges which operate
with cold discharge are called cold-catho-
de- or Penning vacuum gauges. The
discharge process in a measuring tube is,
N2, O2 air – pI = pT in principle, the same as in the electrode
system of a sputter ion pump (see section
2.1.8.3). A common feature of all types of
cold-cathode ionization vacuum gauges is
pI < pT
that they contain just two unheated
electrodes, a cathode and an anode, bet-
ween which a so-called cold discharge is
True pressure [mbar] pW

initiated and maintained by means of a d.c.


voltage (of around 2 kV) so that the
discharge continues at very low pressures.
This is achieved by using a magnetic field
to make the paths of the electrons long
pI > pT enough so that the rate of their collision
with gas molecules is sufficiently large to
form the number of charge carriers requi-
red to maintain the discharge. The magne-
tic field (see Fig. 3.12) is arranged such
that the magnetic field lines of force cross

Indicated pressure [mbar] pI


the electric field lines. In this way the elec-
trons are confined to a spiral path. The
D00
Fig. 3.11 Calibration curves of THERMOVAC gauges for various gases, based on nitrogen equivalent reading
positive and negative charge carriers pro-

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Fundamentals of Vacuum Technology Vacuum Measurement

duced by collision move to the correspon- tive to the sudden admission of air and to i+ produced in the measuring system is
ding electrodes and form the pressure- vibrations; and third, the instrument is defined by:
dependent discharge current, which is easy to operate.
i+ = C · i– · p und (3.3)
indicated on the meter. The reading in
mbar depends on the type of gas. The i+
p= (3.3a)
upper limit of the measuring range is given
3.3.3.2 Hot-cathode ionization vacuum i ⋅C

by the fact that above a level of several


gauges
10-2 mbar the Penning discharge changes The variable C is the vacuum gauge con-
to a glow discharge with intense light out- Generally speaking, such gauges refer to stant of the measuring system. For nitro-
put in which the current (at constant volta- measuring systems consisting of three gen this variable is generally around
ge) depends only to a small extent on the electrodes (cathode, anode and ion collec- 10 mbar-1. With a constant electron cur-
pressure and is therefore not suitable for tor) where the cathode is a hot cathode. rent the sensitivity S of a gauge head is
measurement purposes. In all Penning Cathodes used to be made of tungsten but defined as the quotient of the ion current
gauges there is considerably higher gas are now usually made of oxide-coated iri- and the pressure. For an electron current
sorption than in ionization vacuum gauges dium (Th2O3, Y2O3) to reduce the electron of 1 mA and C = 10 mbar-1, therefore, the
that operate with a hot cathode. A Penning output work and make them more resi- sensitivity S of the gauge head is:
measuring tube pumps gases similarly to a stant to oxygen. Ionization vacuum gauges
S = i+ / p = C · i- = 10 mbar-1 · 1 mA
sputter ion pump (S ≈ 10-2 l/s). Here again of this type work with low voltages and
without an external magnetic field. The hot = 10 mbar-1 · 10-3 A
the ions produced in the discharge are
accelerated towards the cathode where cathode is a very high-yield source of elec- = 1 · 10-2 A/mbar.
they are partly retained and partly cause trons. The electrons are accelerated in the Hot-cathode ionization vacuum gauges
sputtering of the cathode material. The electric field (see Fig. 3.13) and receive also exhibit gas sorption (pumping
sputtered cathode material forms a gette- sufficient energy from the field to ionize action), which, however, is considerably
ring surface film on the walls of the gauge the gas in which the electrode system is smaller than with Penning systems, i.e.
tube. In spite of these disadvantages, located. The positive gas ions formed are approx. 10-3 l/s. Essentially this gas sorp-
which result in a relatively high degree of transported to the ion collector, which is tion takes place on the glass wall of the
inaccuracy in the pressure reading (up to negative with respect to the cathode, and gauge head and, to a lesser extent, at the
around 50 %), the cold-cathode ionization give up their charge there. The ion current ion collector. Here use is made of nude
gauge has three very outstanding advanta- thereby generated is a measure of the gas gauges that are easy to operate because an
ges. First, it is the least expensive of all density and thus of the gas pressure. If i- external magnet is not needed. The upper
high vacuum measuring instruments. is the electron current emitted by the hot limit of the measuring range of the hot-
Second, the measuring system is insensi- cathode, the pressure-proportional current cathode ionization gauge is around
10-2 mbar (with the exception of special
designs). It is basically defined by the
scatter processes of ions at gas molecules
Anode
due to the shorter free path at higher pres-
sures (the ions no longer reach the ion
Cathode Ion collector collector = lower ion yield). Moreover,
uncontrollable glow or arc discharges may
form at higher pressures and electrostatic
discharges can occur in glass tubes. In
these cases the indicated pressure pI may
UC UA deviate substantially from the true pressu-
(+ 50V) (+ 200V) re pT.
At low pressures the measuring range is
limited by two effects: by the X-ray effect
and by the ion desorption effect. These
UA effects results in loss of the strict propor-
tionality between the pressure and the ion
current and produce a low pressure thres-
UC
hold that apparently cannot be crossed
(see Fig. 3.14).
1 Small flange 4 Ceramic washer
DN 25 KF; 5 Current leadthrough
DN 40 KF 6 Connecting bush i+: ion current The X-ray effect (see Fig. 3.15)
2 Housing 7 Anode pin i-: electron current The electrons emitted from the cathode
3 Ring anode with 8 Cathode plate impinge on the anode, releasing photons
ignition pin
(soft X-rays). These photons, in turn,
Fig. 3.13 Schematic diagram and potential curve in a
Fig. 3.12 Cross-section of PENNINGVAC PR 35 gauge hot-cathode ionization vacuum gauge
trigger photoelectrons from surfaces they

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strike. The photoelectrons released from collector and lead to a pressure indication the Bayard-Alpert system is usually the
the ion collector flow to the anode, i.e. the that is initially independent of the pressure standard system.
ion collector emits an electron current, but rises as the electron current increases.
which is indicated in the same manner as If such a small electron current is used so a) The conventional ionization vacuum
a positive ion current flowing to the ion that the number of electrons incident at the gauge
collector. This photocurrent simulates a surface is small compared to the number of A triode of conventional design (see Fig.
pressure. This effect is called the positive adsorbed gas particles, every electron will 3.16 a) is used as the gauge head, but it is
X-ray effect, and it depends on the anode be able to desorb positive ions. If the elec- slightly modified so that the outer electro-
voltage as well as on the size of the surfa- tron current is then increased, desorption de serves as the ion collector and the grid
ce of the ion collector. will initially increase because more elec- within it as the anode. With this arrange-
trons impinge on the surface. This finally ment the electrons are forced to take very
Under certain circumstances, however, long paths (oscillating around the grid
leads to a reduction in adsorbed gas par-
there is also a negative X-ray effect. Pho- wires of the anode) so that the probability
ticles at the surface. The reading falls again
tons which impinge on the wall surroun- of ionizing collisions and thus the sensiti-
and generally reaches values that may be
ding the gauge head release photoelec- vity of the gauge are relatively high. Becau-
considerably lower than the pressure rea-
trons there, which again flow towards the se the triode system can generally only be
ding observed with a small electron cur-
anode, and since the anode is a grid struc- used in high vacuum on account of its
rent. As a consequence of this effect in
ture, they also flow into the space within strong X-ray effect, the gas sorption (pum-
practice, one must ascertain whether the
the anode. If the surrounding wall has the ping) effect and the gas content of the
pressure reading has been influenced by a
same potential as the ion collector, e.g. electrode system have only a slight effect
desorption current. This can be done most
ground potential, a portion of the electrons on the pressure measurement.
simply by temporarily altering the electron
released at the wall can reach the ion
current by a factor of 10 or 100. The rea-
collector. This results in the flow of an
ding for the larger electron current is the
electron current to the ion collector, i.e. a a)
more precise pressure value.
negative current flows which can compen-
Conventional
sate the positive ion current. This negative In addition to the conventional ionization ionization
X-ray effect depends on the potential of the gauge, whose electrode structure resemb- vacuum gauge
outer wall of the gauge head. les that of a common triode, there are system

various ionization vacuum gauge systems


The ion desorption effect (Bayard-Alpert system, Bayard-Alpert
b)
Adsorbed gases can be desorbed from a system with modulator, extractor system) ionization vacu-
surface by electron impact. For an ionizati- which more or less suppress the two um gauge
system for higher
on gauge this means that, if there is a layer effects, depending on the design, and are pressures (up to
of adsorbed gas on the anode, these gases therefore used for measurement in the 1 mbar)
are partly desorbed as ions by the impin- high and ultrahigh vacuum range. Today
ging electrons. The ions reach the ion
c)

Bayard-Alpert
ionization
vacuum gauge
system
Indicated pressure mbar

d)

Bayard-Alpert
ionization
vacuum gauge
system with
modulator

e)
Actual pressure mbar
extractor
I Pressure reading without X-ray effect ionization
II Apparent low pressure limit due to X-ray effect C Cathode vacuum gauge
III Sum of I and II A Anode system
I Ion collector
I ion collector A anode
Fig. 3.15 Explanation of the X-ray effect in a conventio- Sc screen C cathode
nal ionization gauge. The electrons e- emitted M modulator R reflector
by the cathode C collide with anode A and
trigger a soft X-ray radiation (photons) there. Fig. 3.16 Schematic drawing of the electrode
D00
Fig. 3.14 Apparent low pressure limit due to X-ray This radiation strikes, in part, the ion collec- arrangement of various ionization vacuum
Ð
effect in a normal ionization vacuum gauge tor and generates photoelectrons e s there gauge measuring systems

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b) The high-pressure ionization vacuum as that on the ion collector, part of the ion Another advantage is that the measuring
gauge (up to 1 mbar) current formed flows to the modulator and system is designed as a nude gauge with a
A triode is again used as the electrode the current that flows to the ion collector diameter of only 35 mm so that it can be
system (see Fig. 3.16 b), but this time with becomes smaller. The indicated pressure installed in small apparatus.
an unmodified conventional design. Since pI of the ionization gauge with modulator
the gauge is designed to allow pressure set to the anode potential consists of the
measurements up to 1 mbar, the cathode portion due to the gas pressure pg and that
must be resistant to relatively high oxygen due to the X-ray effect pγ:
pressure. Therefore, it is designed as a so-
pA = pg + pγ (3.4)
called non-burnout cathode, consisting of
an yttria-coated iridium ribbon. To obtain a After switching the modulator from the
rectilinear characteristic (ion current as a anode potential over to the ion collector
linear function of the pressure) up to a potential, the modulated pressure reading
pressure of 1 mbar, a high-ohmic resistor pM is lower than the pI reading because a
is installed in the anode circuit. portion of the ions now reaches the modu-
lator. Hence:
c) Bayard-Alpert ionization vacuum pM = α · pg + pγ (3.5)
gauge (the standard measuring
system used today) with α < 1.
To ensure linearity between the gas pres-
sure and the ion current over as large a The pg share of the X-ray effect is the same
pressure range as possible, the X-ray in both cases. After determining the diffe-
effect must be suppressed as far as possi- rence between (3.4) and (3.5), we obtain
ble. In the electrode arrangement develo- the equation for the gas pressure pg:
ped by Bayard and Alpert, this is achieved p −p
A M (3.6)
pg =
by virtue of the fact that the hot cathode is 1− α
located outside the anode and the ion
collector is a thin wire forming the axis of α can immediately be determined by expe-
the electrode system (see Fig. 3.16 c). The riment at a higher pressure (around
X-ray effect is reduced by two to three 10-6 mbar) at which the X-ray effect and
orders of magnitude due to the great thus pγ are negligible. The pressure corre-
reduction in the surface area of the ion sponding to the two modulator potentials
collector. When pressures in the ultrahigh are read off and their ratio is formed. This
vacuum range are measured, the inner modulation method has the additional
surfaces of the gauge head and the advantage that the ion desorption effect is
connections to the vessel affect the pres- determined in this way. It permits pressu-
sure reading. The various effects of ad- re measurements up to the 10-11 mbar
sorption, desorption, dissociation and flow range with relatively little effort.
phenomena cannot be dealt with in this
context. By using Bayard-Alpert systems e) Extractor ionization vacuum gauge
as nude gauge systems that are placed Disruptive effects that influence pressure
directly in the vessel, errors in measure- measurement can also be extensively eli-
ment can be extensively avoided because minated by means of an ion-optical system
of the above mentioned effects. first suggested by Redhead. With this
extractor system (see Fig. 3.16 e) the ions
d) Bayard-Alpert ionization vacuum gauge from the anode cylinder are focused on a
with modulator very thin and short ion collector. The ion
The Bayard-Alpert system with modulator collector is set up in a space, the rear wall
(see Fig. 3.16 d), introduced by Redhead, of which is formed by a cup-shaped elec-
offers pressure measurement in which trode that is maintained at the anode
errors due to X-ray and ion desorption potential so that it cannot be reached by
effects can be quantitatively taken into ions emanating from the gas space. Due to
account. In this arrangement there is a the geometry of the system as well as the
second thin wire, the modulator, near the potential of the of individual electrodes,
anode in addition to the ion collector insi- the disruptive influences through X-ray
de the anode. If this modulator is set at the effects and ion desorption are almost com-
anode potential, it does not influence the pletely excluded without the need of a
measurement. If, on the other hand, the modulator. The extractor system measures
same potential is applied to the modulator pressures between 10-4 and 10-12 mbar.

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3.4 Adjustment and gauges), are calibrated directly by the PTB


at regular intervals. Vacuum gauges of all
3.4.1 Examples of fundamental
pressure measurement
calibration; DKD, makes are calibrated on an impartial basis
methods (as standard
by LEYBOLD in Cologne according to
PTB national customer order. A DKD calibration certifi- methods for calibrating
standards cate is issued with all characteristic data vacuum gauges)
on the calibration. The standards of the
Definition of terms: Since these terms are Federal Physical-Technical Institute are the a) Measuring pressure with a reference
often confused in daily usage, a clear defi- so-called national standards. To be able to gauge
nition of them will first be provided: guarantee adequate measuring accuracy An example of such an instrument is the
or as little measurement uncertainty as U-tube vacuum gauge, with which the
Adjustment or tuning refers to the correct possible in its calibrations, the PTB largely measurement of the pressure in the mea-
setting of an instrument. For example, set- carries out its measurements through the surement capillary is based on a measure-
ting 0 and 100 % in THERMOVACs or set- application of fundamental methods. This ment of the weight over the length of the
ting the mass spectrometer to mass 4 in means, for example, that one attempts to mercury column.
the helium leak detector. describe the calibration pressures through
In the past the McLeod vacuum gauge was
the measurement of force and area or by
also used for calibration purposes. With a
Calibration inspection refers to com- thinning the gases in strict accordance
precision-made McLeod and carefully exe-
parison with a standard in accordance with with physical laws. The chain of the recali-
cuted measurements, taking into account
certain statutory regulations by specially bration of standard instruments carried
all possible sources of error, pressures
out once a year at the next higher qualified
authorized personnel (Bureau of Stand- down to 10-4 mbar can be measured with
ards). If the outcome of this regular ins- calibration facility up to the PTB is called
considerable accuracy by means of such
pection is positive, an operating permit for “resetting to national standards”. In other
an instrument.
the next operation period (e.g. three years) countries as well, similar methods are car-
ried out by the national standards institu- Another reference gauge is the VISCOVAC
is made visible for outsiders by means of a decrement gauge with rotating ball (see
sticker or lead seal. If the outcome is nega- tes as those applied by the Federal Physi-
cal-Technical Institute (PTB) in Germany. 3.3.1) as well as the capacitance dia-
tive, the instrument is withdrawn from phragm gauge (see 3.2.2.4).
operation. Fig. 3.17 shows the pressure scale of the
PTB. Calibration guidelines are specified in
DIN standards (DIN 28 416) and ISO pro- b) Generation of a known pressure; static
Calibration refers to comparison with a expansion method
standard in accordance with certain posals.
On the basis of a certain quantity of gas
statutory regulations by specially authori- whose parameters p, V and T are known
zed personnel (calibration facility). The exactly – p lies within the measuring range
result of this procedure is a calibration cer- of a reference gauge such as a U-tube or
tificate which contains the deviations of
the readings of the instrument being cali-
brated from the standard.
Calibration facilities carry out this calibra- 30
tion work. One problem that arises is the Dynamic
question of how good the standards are
Relative uncertainly of the pressure determination [%]

expansion
and where they are calibrated. Such stan- 10
dards are calibrated in calibration facilities
of the German Calibration Service (DKD).
The German Calibration Service is mana- 3
ged by the Federal Physical-Technical Molecular
beam
Institute (PTB). Its function is to ensure Static expansion
that measuring and testing equipment 1
used for industrial measurement purposes U-Tube
is subjected to official standards. Calibrati-
on of vacuum gauges and test leaks within 0.3
the framework of the DKD has been assig-
ned to LEYBOLD, as well as other compa-
nies, by the PTB. The required calibration 0.1
pump bench was set up in accordance 10–12 10–9 10–6 10–3 100 103
with DIN 28 418 (see Table 11.1) and then
inspected and accepted by the PTB. The Pressure [mbar] D00
standards of the DKD facilities, so-called Fig. 3.17 Pressure scale of Federal Physical-Technical Institute (PTB), Berlin, (status as at August 1984) for inert gases,
transfer standards (reference vacuum nitrogen and methane

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McLeod vacuum gauge – a lower pressure c) Dynamic expansion method L1 = conductance of the valve. The pum-
within the working range of ionization gau- (see Fig. 3.19) ping system consists of a precisely mea-
ges is reached via expansion in several According to this method, the calibration sured aperture with the conductance L2 in
stages. pressure p is produced by admitting gas at a wall that is as thin as possible (screen
a constant throughput rate Q into a va- conductance) and a pump with a pumping
If the gas having volume V1 is expanded to
cuum chamber while gas is simultaneous- speed of PSp:
a volume (V1 + V2), and from V2 to
ly pumped out of the chamber by a pump
(V2 + V3), etc., one obtains, after n stages L 2 ⋅ Sp L2
unit with a constant pumping speed S. At S= =
of expansion: L + Sp L2 (3.8)
equilibrium the following applies accor- 2 1+
V1 V2 Vn −1 ding to equation 1.10 a: Sp
pn = p ⋅ ⋅ ⋅⋅ ⋅⋅ (3.7)
1 V1 + V2 V2 + V3 Vn −1 + Vn
p = Q/S and thus
p1 = initial pressure measured directly in Q is obtained either from the quantity of L1 L1 L2
mbar gas that flows into the calibration chamber p2 = p ⋅ =p⋅ ⋅ (1 + ) (3.9)
pn = calibration pressure from a supply vessel in which constant 1 S 1 L2 Sp
pressure prevails or from the quantity of
The volumes here must be known as pre- gas flowing into the calibration chamber at This method has the advantage that, after
cisely as possible (see Fig. 3.18) and the a measured pressure through a known reaching a state of equilibrium, sorption
temperature has to remain constant. This conductance. The pressure in front of the effects can be ignored and this procedure
method requires that the apparatus used inlet valve must be high enough so that it can therefore be used for calibrating gau-
be kept very clean and reaches its limit at can be measured with a reference gauge. ges at very low pressures.
pressures where the gas quantity can be The inlet apertures of the valve (small
altered by desorption or adsorption effects capillaries, sintered bodies) must be so
beyond the permissible limits of error. small that the condition d << λ is met, i.e.
According to experience, this lower limit is a molecular flow and hence a constant
around 5 · 10-7 mbar. This method is cal- conductance of the inlet valve are obtained
led the static expansion method because (see Section 1.5). The quantity of gas is
the pressure and volume of the gas at rest then defined by p1 · L1, where
are the decisive variables. p1 = pressure in front of the inlet valve and

IM IM

V2 = 1000 cm3
p1
+

p3 V4 =
3
13000 cm
+

p4
+

V1 = 25 cm3 V3 = 25 cm3
+

p2
L1
p2 = p1 (Sp >> L2)
S
+

1 Volume 1 10 LN2 cold trap 16 to pump


2 Volume 2 11 to pump system (pumping speed
3 Inlet valve 12 U-tube vacuum PSp)
(conductance L1) gauge 17 Gas inlet
4 Aperture with 13 McLeod vacuum 18 Mass spectrometer
conductance L2 gauge 19,20 Gauges to be
5 Valve 14 Valve calibrated
6 to pump system 15 Calibrated 21 Nude gauge to be
7 Valve ionization gauge calibrated
8 to gas reservoir tube 22 Bake-out furnace
9 Valve

Fig. 3.18 Generation of low pressures through static expansion Fig. 3.19 Apparatus for calibration according to the dynamic expansion method

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3.5 Pressure 3.5.2 Automatic protection, actuated from a control panel with push-
buttons. The pump system is to be protec-
monitoring and control of
monitoring, control vacuum systems
ted against the following malfunctions:
a) power failure
and regulation in Protection of a vacuum system against b) drop in pressure in the compressed air
vacuum systems malfunctions is extremely important. In network
the event of failure, very high material c) failure of cooling water to the diffusion
values may be at risk, whether through pump
3.5.1 Fundamentals of pressure d) fault in diffusion pump heating system
loss of the entire system or major compo-
monitoring and control nents of it, due to loss of the batch of e) failure of backing pump
In all vacuum processes the pressure in material to be processed or due to further f) pressure rise in the vessel above a
the system must be constantly checked production down time. Adequate operatio- maximum permissible value
and, if necessary, regulated. Modern plant nal control and protection should therefo- g) pressure rise above a maximum
control additionally requires that all mea- re be provided for, particularly in the case backing pressure (critical forepressure
sured values which are important for of large production plants. The individual of the diffusion pump)
monitoring a plant are transmitted to cen- factors to be taken into account in this The measures to be taken in order to fore-
tral stations, monitoring and control cen- connection are best illustrated on the basis stall such malfunctions will be discussed
ters and compiled in a clear manner. Pres- of an example: Fig. 3.20 shows the sche- in the same order:
sure changes are frequently recorded over matic diagram of a high vacuum pump a) Measures in the event of power failure:
time by recording equipment. This means system. The vessel (11) can be evacuated All valves are closed so as to prevent
that additional demands are placed on by means of a Roots pump (14) or a diffu- admission of air to the vacuum vessel
vacuum gauges: sion pump (15), both of which operate in and protect the diffusion pump against
a) continuous indication of measured conjunction with the backing pump (1). damage.
values, analog and digital as far as pos- The Roots pump is used in the medium b) Protection in the event of a drop in
sible vacuum range and the diffusion pump in pressure in the compressed air net-
b) clear and convenient reading of the the high vacuum range. The valves (3), (8) work: The compressed air is monitored
measured values and (16) are operated electropneuma- by a pressure monitoring device (5). If
c) recorder output to connect a recording tically. The individual components are
instrument or control or regulation
equipment
d) built-in computer interface (e.g. RS 232)
e) facility for triggering switching operati-
ons through built-in trigger points
These demands are generally met by all
vacuum gauges that have an electric mea-
sured value display, with the exception of
Bourdon, precision diaphragm and liquid-
filled vacuum gauges. The respective con-
trol units are equipped with recorder out-
puts that supply continuous voltages bet-
ween 0 and 10 V, depending on the pres-
sure reading on the meter scale, so that
the pressure values can be recorded over
time by means of a recording instrument.
If a pressure switching unit is connected to
the recorder output of the gauge, swit-
ching operations can be triggered when
the values go over or below specified set-
points. The setpoints or switch threshold
values for triggering switching operations
directly in the gauges are called trigger
1 Backing pump 6 Temperature monitoring device 12 High-vacuum gauge
values. Apart from vacuum gauges, there 2 Backing pressure 7 Cooling water monitoring device 13 Limit switches
are diaphragm pressure switches that trig- monitoring device 8 Electropneumatic valve 14 Roots pump
ger a switching operation (without display 3 Electropneumatic valve 9 Recorder 15 Diffusion pump
4 Compressed air connection 10 High-vacuum monitoring device 16 Electropneumatic valve
of a measured value) via a contact ampli-
fier when a certain pressure is reached. 5 Pressure monitoring device 11 Vessel 17 Venting valve D00
Valves, for example, can also be controlled Fig. 3.20 Schematic diagram of a high vacuum pump system with optional operation of a Roots pump or
through such switching operations. a diffusion pump

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Fundamentals of Vacuum Technology Vacuum Measurement

the pressure falls under a specified system protected against all malfunctions ce is the controller in which the setpoint
value, a signal can initially be emitted or to a fully automatic, program-controlled and the actual value are compared. The
the valves can be automatically closed. plant, though the complexity of the electri- totality of all elements involved in the con-
In this case, a sufficient reserve supply cal circuits, of course, increases signifi- trol process forms the control circuit. The
of compressed air is necessary (not cantly. terms and characteristic variables for
shown in Fig. 3.20), which allows all describing control processes are stipula-
valves to be actuated at least once. ted in DIN 19226.
c) Measures in the event of failure of coo-
Generally a distinction is made between
ling water to the diffusion pump: The
discontinuous control (e.g. two-step or
cooling water is monitored by a flow or 3.5.3 Pressure regulation and three-step control) with specification of a
temperature monitoring device (6) and control in rough and pressure window, within which the pressu-
(7). If the flow of cooling water is ina-
dequate, the heater of the diffusion
medium vacuum systems re may vary, and continuous control (e.g.
PID control) with a specified pressure set-
pump is switched off and a signal is Control and regulation have the function of point, which should be maintained as pre-
given; the valve (8) closes. giving a physical variable – in this case the cisely as possible. We have two possible
d) Protection against failure of the diffusi- pressure in the vacuum system – a certain ways of adjusting the pressure in a vacu-
on pump heater: Interruption of the dif- value. The common feature is the actuator um system: first, by changing the pumping
fusion pump heating system can be which changes the energy supply to the speed (altering the speed of the pump or
monitored by a relay. If the temperature physical variable and thus the variable its- throttling by closing a valve); second,
rises above a maximum permissible elf. Control refers to influencing a system through admission of gas (opening a
value, a temperature monitoring device or unit through commands. In this case valve). This results in a total of 4 procedu-
(6) responds. In both cases the valve the actuator and hence the actual value of res.
(8) closes and a signal is given. the physical variable is changed directly
e) Protection in the event of backing pump with a manipulated variable. Example: Discontinuous pressure regulation
failure: Belt-driven backing pumps Actuation of a valve by means of a pressu- Although continuous regulation undoub-
must have a centrifugal switch which re-dependent switch. The actual value may tedly represents the more elegant proce-
shuts down the entire system in the change in an undesirable way due to addi- dure, in many cases two-step or three-step
event of belt breakage or another tional external influences. The controlled regulation is fully adequate in all vacuum
malfunction. Monoblock pumps for unit cannot react to the control unit. For ranges. To specify the pressure window,
which the drive is mounted directly on this reason control systems are said to two or three variable, pressure-dependent
the shaft can be monitored by current have an open operating sequence. In the switch contacts are necessary. It does not
relays and the like. case of regulation, the actual value of the matter here whether the switch contacts
f) Protection against a pressure rise in the physical variable is constantly compared are installed in a gauge with display or in a
vessel above a certain limit value: The to the specified setpoint and regulated if downstream unit or whether it is a pressu-
high vacuum monitoring device (10) there is any deviation so that it completely re switch without display. Fig. 3.21 illust-
emits a signal when a specified pressu- approximates the setpoint as far as possi- rates the difference between two-step
re is exceeded. ble. For all practical purposes regulation regulation through pumping speed thrott-
g) Ensuring the critical forepressure of the always requires control. The main differen- ling, two-point regulation through gas
diffusion pump: When a certain backing
pressure is exceeded, all valves are clo-
sed by the backing pressure monitoring
device (2), the pumps are switched off
and again a signal is given. The position Two-step regulation through Three-step regulation through

of the valves (3), (8) and (16) is indica- pumping speed throttling gas admission pumping speed throttling
and gas admission
ted on the control panel by means of Pressure Pressure Pressure
limit switches (13). The pressure in the
pAtm pAtm pAtm
vessel is measured with a high vacuum
gauge (12) and recorded with a recor-
der (9). Protection against operating pmax
errors can be provided by interlocking
pmin pmax pmitte
the individual switches so that they can
only be actuated in a predetermined pmin pmin
sequence. The diffusion pump, for
Time Time Time
example, may not be switched on when
the backing pump is not running or the
required backing pressure is not main-
tained or the cooling water circulation is
not functioning.
Fig. 3.21 Schematic diagram of two-step and three-step regulation
In principle, it is not a big step from a
D00.84 LEYBOLD VACUUM PRODUCTS AND REFERENCE BOOK 2001/2002
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Vacuum Measurement Fundamentals of Vacuum Technology

➀ Gauge with two Fu Fuse ➀ Gauge with two Fu Fuse


switching points R, Mp Mains connection 220 V/50 Hz switching points R, Mp Mains connection 220 V/50 Hz
➁ Throttle valve Smax Switching point for maximum value ➁ Variable-leak valve Smax Switching point for maximum value
➂ Vacuum pump Smin Switching point for minimum value ➂ Inlet valve Smin Switching point for minimum value
➃ Pump valve PV Pump valve ➃ Gas supply EV Inlet valve
➄ Vacuum vessel R1 Auxiliary relay for pump valve ➄ Throttle valve R2 Auxiliary relay for inlet valve
K1 Relay contact of R1 ➅ Vacuum pump K2 Relay contact of R2
M Measuring and switching device ➆ Vacuum vessel M Measuring and switching device

Fig. 3.22 Two-step regulation through pumping speed throttling Fig. 3.23 Two-step regulation through gas admission

admission and three-point regulation In the case of two-step regulation through As the name indicates, two switching
through a combination of pumping speed gas admission, the inlet valve is initially points, the lower switching point of the
throttling and gas admission. Figures 3.22 closed. If the upper pressure switching regulation system through pumping speed
and 3.23 show the circuit and structure of point is not reached, nothing changes; throttling and the upper switching point of
the two two-step regulation systems. In only when the pressure falls below the the gas inlet regulation system, were com-
the case of two-step regulation through lower switching point, do the “make bined.
pumping speed throttling (Fig. 3.22), vol- contacts” open the gas inlet valve and
To avoid the complicated installation with
tage is supplied to pump valve 4, i.e. it is actuate the auxiliary relay with self-holding
auxiliary relays, many units offer a facility
open when the relay contacts are in the function simultaneously. Return to the idle
for changing the type of function of the
release condition. At a level below the state with closing of the gas inlet valve is
built-in trigger values via software. Initially
upper switching point the valve remains not effected until after the upper switching
one can choose between individual swit-
open because of the self-holding function point is exceeded due to the release of the
ching points (so-called “level triggers”)
of the auxiliary relay. Only at a level below relay self-holding function.
and interlinked switching points (“interval
the lower switching point is the relay lat-
Fig. 3.24 shows the corresponding three- triggers”). These functions are explained
ching released. If the pressure subse-
step regulation system which was created in Fig. 3.25. With interval triggers one can
quently rises, the valve is opened again at
with the two components just described. also select the size of the hysteresis and
the upper switching point.

Fu Fuse
➀ Gauge with three R, Mp Mains connection 220 V/50 Hz
switching points Smax Switching point for maximum value
➁ Variable-leak valve Smitte Switching point for mean value
➂ Variable-leak valve Smin Switching point for minimum value
T TORROSTAT® S 020
➃ Inlet valve
PV Pump valve
➄ Gas supply EV Inlet valve
➅ Throttle valve R1 Auxiliary relay for pump interval
➆ Vacuum pump
➇ Pump valve
➈ Vacuum vessel
R2
K1
K2
Auxiliary relay for inlet interval
Relay contact of R1
Relay contact of R2
D00
M Measuring and switching device
Fig. 3.24 Three-step regulation system Fig. 3.25 Diagram of level triggers and interval triggers

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Fundamentals of Vacuum Technology Vacuum Measurement

process chamber
connection
measuring
connection
for process pressure
reference chamber
control chamber
diaphragm controller seat
measuring
connection
for reference pump connection
chamber

reference pressure
adjustment valve

Fig. 3.26 LEYBOLD-A series, equipment with level and interval triggers Fig. 3.27 Principle of a diaphragm controller

the type of setpoint specification, i.e. either rence pressure > process pressure) or such a connection of 3 MR 50 diaphragm
fixed setting in the unit or specification released (for reference pressure < process controllers.
through an external voltage, e.g. from 0 – pressure) so that in the latter case, a
To control a vacuum process, it is fre-
10 volts. A three-step regulation system connection is established between the pro-
quently necessary to modify the pressure
(without auxiliary relay), for example, can cess side and the vacuum pump. This ele-
in individual process steps. With a dia-
be set up with the LEYBOLD MEMBRANOVAC gant and more or less “automatic” regula-
phragm controller this can be done either
of the A series. Fig. 3.26 shows different tion system has excellent control characte-
manually or via electric control of the refe-
units of the new LEYBOLD A series, which, ristics (see Fig. 3.28).
rence pressure.
although they function according to diffe-
To achieve higher flow rates, several dia-
rent measuring methods, all display a uni- Electric control of the reference pressure
phragm controllers can be connected in
form appearance. of a diaphragm controller is relatively easy
parallel. This means that the process
because of the small reference volume that
chambers and the reference chambers are
Continuous pressure regulation always remains constant. Fig. 3.31 shows
also connected in parallel. Fig. 3.29 shows
We have to make a distinction here bet- such an arrangement on the left as a pic-
ween electric controllers (e.g. PID con-
trollers) with a proportional valve as actua-
tor and mechanical diaphragm controllers.
In a regulation system with electric con-
trollers the coordination between control-
ler and actuator (piezoelectric gas inlet
valve, inlet valve with motor drive, butterf-
ly control valve, throttle valve) is difficult
because of the very different boundary
conditions (volume of the vessel, effective
pumping speed at the vessel, pressure
control range). Such control circuits tend
to vibrate easily when process mal-
functions occur. It is virtually impossible to
specify generally valid standard values.
Many control problems can be better sol-
ved with a diaphragm controller. The func-
tion of the diaphragm controller (see Fig.
3.27) can be easily derived from that of a
diaphragm vacuum gauge: the blunt end of
a tube or pipe is either closed off by means P1 = process pressure, P2 = pressure in pump, Pref = reference pressure
of an elastic rubber diaphragm (for refe-
Fig. 3.28 Control characteristics of a diaphragm controller

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3.5.4 Pressure regulation in


high and ultrahigh vacu-
um systems
If the pressure is to be kept constant wit-
hin certain limits, an equilibrium must be
established between the gas admitted to
the vacuum vessel and the gas simulta-
neously removed by the pump with the aid
of valves or throttling devices. This is not
very difficult in rough and medium vacu-
Fig. 3.29 Triple connection of diaphragm controllers um systems because desorption of adsor-
bed gases from the walls is generally neg-
ture and on the right schematically, see ligible in comparison to the quantity of gas
3.5.5 for application examples with flowing through the system. Pressure
diaphragm controllers. regulation can be carried out through gas
inlet or pumping speed regulation. Howe-
To be able to change the reference pressu- ver, the use of diaphragm controllers is DC Diaphragm controller
re and thus the process pressure towards P Vacuum pump
only possible between atmospheric pres- M Measuring and switching device
higher pressures, a gas inlet valve must sure and about 10 mbar. PS Pressure sensor
additionally be installed at the process V1 Pump valve
chamber. This valve is opened by means of In the high and ultrahigh vacuum range, V2 Gas inlet valve
a differential pressure switch (not shown on the other hand, the gas evolution from TH Throttle
the vessel walls has a decisive influence on RC Reference chamber
in Fig. 3.31) when the desired higher pro- PC Process chamber
cess pressure exceeds the current process the pressure. Setting of specific pressure CV Internal reference pressure control valve
pressure by more than the pressure diffe- values in the high and ultrahigh vacuum
rence set on the differential pressure range, therefore, is only possible if the gas Fig. 3.30 Control of vacuum drying processes by regu-
evolution from the walls is negligible in lation of the intake pressure of the vacuum
switch. pump according to the water vapor tolerance
relation to the controlled admission of gas
by means of the pressure-regulating unit.
For this reason, pressure regulation in this variable-leak valves are used as actuators.
range is usually effected as gas admission Only bakeable all-metal gas inlet valves
regulation with an electric PID controller. should be used for pressure regulation
Piezoelectric or servomotor-controlled below 10-6 mbar.

DC Diaphragm controller
PS Process pressure sensor
RS Reference pressure sensor
V1 Gas inlet valve
V2 Pump valve
V3 Gas inlet variable-leak valve
TH Throttle
M Measuring and switching device
PP Process pump
RC Reference chamber
PC
AP
Process chamber
Auxiliary pump
D00
CV Internal reference pressure control valve
Fig. 3.31 Diaphragm controller with external automatic reference pressure regulation

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3.5.5 Examples of applications The material to be dried is usually heated “caught” as the reference pressure in the
with diaphragm to intensify and speed up the drying pro- reference chamber (RC) of the diaphragm
cess. If a certain amount of water vapor is controller (DC). Now the process pressure
controllers produced, the intake pressure rises above is automatically maintained at a constant
1) Regulation of a drying/distillation pro- the two switching points. As a result, valve level according to the set reference pres-
cess, taking into account the maximum V2 first closes and V1 opens. Through sure by means of the diaphragm controller
water vapor tolerance of a vane type incoming air or protective gas the pressu- (DC). If the reference pressure should rise
rotary pump re in the reference chamber is raised and in the course of the process due to a leak,
the throughput at the diaphragm controller this is automatically detected by the mea-
In a drying process it is frequently desira- thus throttled until the intake pressure of suring and switching device and corrected
ble to carry out drying solely by means of the vacuum pump has dropped below the by briefly opening pump valve V2. This
vacuum pumps without inserting conden- set maximum switching point again. Then additional control function enhances the
sers. In view of the limited water vapor valve V1 closes. operational reliability and extends the
tolerance of vacuum pumps – approx. range of application. Correcting the increa-
30 mbar as a rule – this would result in Depending on the quantity of vapor that
sed reference pressure to the originally set
condensation of the vapors produced wit- accumulates, the throughput of the
value is of special interest for regulated
hin the vacuum pump, given non-throttled diaphragm controller is set by increasing
helium circuits because the pressure rise
or non-regulated pumping speed. One can or decreasing the reference pressure in
in the reference chamber (RC) of the dia-
avoid this through process-dependent each case so that the maximum permissi-
phragm controller can be compensated for
remote control of a diaphragm controller ble partial water vapor pressure at the inlet
through this arrangement as a consequen-
with auxiliary control valves and a measu- connection of the vacuum pump is never
ce of the unavoidable helium permeability
ring and switching device with a pressure exceeded.
of the controller diaphragm of FPM.
sensor at the inlet connection of the vacu- As soon as the pressure in the process
um pump if the intake pressure is adapted To be able to change the reference pressu-
chamber drops below the set minimum
to the pumps water vapor tolerance re and thus increase the process pressure
switching point towards the end of the dry-
through automatic monitoring of the inta- to higher pressures, a gas inlet valve must
ing process, valve V2 opens and remains
ke pressure of the vacuum pump and by be additionally installed at the process
open. In this way the unthrottled cross-
throttling the pumping speed. Fig. 3.30 chamber. This valve is opened by means of
section of the diaphragm controller is avai-
shows the principle of this arrangement. a differential pressure switch (not shown
lable again for rapid final drying. At the
in Fig. 3.31) when the desired higher pro-
Mode of operation: Starting from atmos- same time the final drying procedure can
cess pressure exceeds the current process
pheric pressure with the process heating be monitored by means of the pressure
pressure by more than the pressure diffe-
switched off, valve V1 is initially open sensor PS.
rential set at the differential pressure
(maximum switching point exceeded) so switch.
that atmospheric pressure also prevails in 2) Pressure regulation by means of dia-
the reference chamber. phragm controller with external
automatic reference pressure adjust-
The diaphragm controller is therefore clo- ment (see Fig. 3.31)
sed. When the system is started up, the
connecting line between the vacuum pump For automatic vacuum processes with
and pump valve V2 is first evacuated. As regulated process pressure, presetting of
soon as the pressure drops below the the desired set pressure must often func-
maximum switching point, valve V1 clo- tion and be monitored automatically. If a
ses. When the pressure falls below the diaphragm controller is used, this can be
minimum switching point, valve V2 opens. done by equipping the reference chamber
with a measuring and switching device and
In this manner the pressure in the referen- a control valve block at the reference
ce chamber is slowly lowered, the thrott- chamber. The principle of this arrange-
ling of the diaphragm controller is reduced ment is shown in Fig. 3.31.
accordingly and thus the process pressure
is lowered until the quantity of process gas Mode of operation: Starting with atmos-
is greater than the quantity conveyed by pheric pressure, gas inlet valve V1 is clo-
the pump so that the minimum switching sed at the beginning of the process. Pump
point is again exceeded. Valve V2 closes valve V2 opens. The process chamber is
again. This interaction repeats itself until now evacuated until the set pressure,
the pressure in the process chamber has which is preset at the measuring and swit-
dropped below the minimum switching ching device, is reached in the process
point. After that, valve V2 remains open so chamber and in the reference chamber.
that the process can be brought down to When the pressure falls below the set swit-
the required final pressure with a comple- ching threshold, pump valve V2 closes. As
tely open diaphragm controller. a result, the pressure value attained is

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Mass Spectrometry Fundamentals of Vacuum Technology

4. Analysis of gas which are in common use comprise the


measurement system proper (the sensor)
at low and the control device required for its ope-
ration. The sensor contains the ion source,
pressures the separation system and the ion trap.
The separation of ions differing in masses
using mass and charges is often effected by utilizing
phenomena which cause the ions to reso-
spectrometry nate in electrical and magnetic fields.
Initially, the control units were quite clum-
sy and offered uncountable manipulation
options. It was often the case that only
4.1 General physicists were able to handle and use
them. With the introduction of PCs the
Analyses of gases at low pressures are requirements in regard to the control units
useful not only when analyzing the residu- became ever greater. At first, they were fit-
al gases from a vacuum pump, leak testing ted with interfaces for linkage to the com-
at a flange connection or for supply lines puter. Attempts were made later to equip a c
(compressed air, water) in a vacuum. They a
PC with an additional measurement circuit b
are also essential in the broader fields of board for sensor operation. Today’s sen-
vacuum technology applications and pro- a: High-performance sensor with Channeltron
sors are in fact transmitters equipped with b: Compact sensor with Micro-Channelplate
cesses. For example in the analysis of pro- an electrical power supply unit attached c: High-performance sensor with Faraday cup
cess gases used in applying thin layers of direct at the atmosphere side; communica-
coatings to substrates. The equipment tion with a PC from that point is via the
Fig. 4.1a TRANSPECTOR sensors
used for qualitative and/or quantitative standard computer ports (RS 232, RS
analyses of gases includes specially deve- 485). Operating convenience is achieved metry in vacuum-assisted process techno-
loped mass spectrometers with extremely by the software which runs on the PC. logy applications presumably date back to
small dimensions which, like any other Backus’ work in the years 1943 / 44. He
vacuum gauge, can be connected directly carried out studies at the Radiographic
to the vacuum system. Their size distin- Laboratories at the University of California.
guishes these measurement instruments Seeking to separate uranium isotopes, he
from other mass spectrometers such as 4.2 A historical review used a 180° sector field spectrometer after
those used for the chemical analyses of Dempster (1918), which he referred to as
Following Thomson’s first attempt in 1897
gases. The latter devices are poorly suited, a “vacuum analyzer”. Even today a similar
to determine the ratio of charge to mass
for example, for use as partial pressure term, namely the “residual gas analyzer”
e/m for the electron, it was quite some
measurement units since they are too (RGA), is frequently used in the U.S.A. and
time (into the 1950s) before a large num-
large, require a long connector line to the the U.K. instead of “mass spectrometer”.
ber and variety of analysis systems came
vacuum chamber and cannot be baked out Today’s applications in process monitoring
into use in vacuum technology. These
with the vacuum chamber itself. The in- are found above all in the production of
included the Omegatron, the Topatron and
vestment for an analytical mass spectro- semiconductor components.
ultimately the quadrupole mass spectro-
meter would be unjustifiably great since,
meter proposed by Paul and Steinwedel in
for example, the requirements as to reso-
1958, available from INFICON in its stan-
lution are far less stringent for partial pres-
dard version as the TRANSPECTOR (see
sure measurements. Partial pressure is
understood to be that pressure exerted by
Fig. 4.1). The first uses of mass spectro- 4.3 The quadrupole
a certain type of gas within a mix of gases. mass spectrometer
The total of the partial pressures for all the
types of gas gives the total pressure. The (TRANSPECTOR)
distinction among the various types of
The ion beam extracted from the electron
gases is essentially on the basis of their
impact ion source is diverted into a qua-
molar masses. The primary purpose of
drupole separation system containing four
analysis is therefore to register qualita-
rod-shaped electrodes. The cross sections
tively the proportions of gas within a
of the four rods form the circle of curvatu-
system as regards the molar masses and
re for a hyperbola so that the surrounding
determine quantitatively the amount of the
electrical field is nearly hyperbolic. Each of
individual types of gases associated with
the various atomic numbers.
the two opposing rods exhibits equal
potential, this being a DC voltage and a
D00
Partial pressure measurement devices superimposed high-frequency AC voltage
Fig. 4.1b TRANSPECTOR XPR sensor

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Fundamentals of Vacuum Technology Mass Spectrometry

Anode
Quadrupole exit
Focussing plate diaphragm Cathode
(extractor diaphragm) Ion source exit
diaphragm
Cathode (total pressure measurement)
Anode

Shielding Reflec- Ion trap


tor

Ion source Quadrupole separation system Ion detector


Extractor measurement system

Transpector measurement head


Fig. 4.2 Schematic for quadrupole mass spectrometer Fig. 4.3 Quadrupole mass spectrometer – Extractor ionization vacuum gauge

(Fig. 4.2). The voltages applied induce XPR sensor had to be raised from about 2 of the cathode, anode and several baffles.
transverse oscillations in the ions traver- MHz to approximately 6 times that value, The electron emission, kept constant, cau-
sing the center, between the rods. The namely to 13 MHz. In spite of the reduction ses partial ionization of the residual gas,
amplitudes of almost all oscillations in the length of the rod system, ion yield is into which the ion source is “immersed” as
escalate so that ultimately the ions will still reduced due to dispersion processes completely as possible. The vacuum in the
make contact with the rods; only in the at such high pressures. Additional electro- vicinity of the sensor will naturally be influ-
case of ions with a certain ratio of mass to nic correction is required to achieve per- enced by baking the walls or the cathode.
charge m/e is the resonance condition fect depiction of the spectrum. The dimen- The ions will be extracted through the baf-
which allows passage through the system sions of the XPR sensor are so small that fles along the direction of the separation
satisfied. Once they have escaped from the it can “hide” entirely inside the tubulation system. One of the baffles is connected to
separation system the ions move to the ion of the connection flange (DN 40, CF) and a separate amplifier and – entirely inde-
trap (detector, a Faraday cup) which may thus occupies no space in the vacuum pendent of ion separation – provides con-
also take the form of a secondary electron chamber proper. Fig. 4.1a shows the size tinuous total pressure measurement (see
multiplier pick-up (SEMP). comparison for the normal high-perfor- Fig. 4.4). The cathodes are made of iridium
mance sensors with and without the Chan- wire and have a thorium oxide coating to
The length of the sensor and the sepa-
neltron SEMP, the normal sensor with reduce the work associated with electron
ration system is about 15 cm. To ensure
channel-plate SEMP. Fig. 4.1b shows the discharge. (For some time now the thori-
that the ions can travel unhindered from
XPR sensor. The high vacuum required for um oxide has gradually been replaced by
the ion source to the ion trap, the mean
the sensor is often generated with a yttrium oxide.) These coatings reduce the
free path length inside the sensor must be
TURBOVAC 50 turbomolecular pump and electron discharge work function so that
considerably greater than 15 cm. For air
a D 1.6 B rotary vane pump. With its great the desired emission flow will be achieved
and nitrogen, the value is about
compression capacity, a further advantage even at lower cathode temperatures. Avai-
p · λ = 6 · 10–3 mbar · cm. At p = 1 · 10-4
of the turbomolecular pump when lable for special applications are tungsten
bar this corresponds to a mean free path
handling high molar mass gases is that the cathodes (insensitive to hydrocarbons but
length of λ = 60 cm. This pressure is gene-
sensor and its cathode are ideally pro- sensitive to oxygen) or rhenium cathodes
rally taken to be the minimum vacuum for
tected from contamination from the (insensitive to oxygen and hydrocarbons
mass spectrometers. The emergency shut-
direction of the forepump. but evaporate slowly during operation due
down feature for the cathode (responding
to the high vapor pressure).
to excessive pressure) is almost always
set for about 5 · 10-4 mbar. The desire to
be able to use quadrupole spectrometers
Cathode
at higher pressures too, without special 4.3.1 Design of the sensor
pressure convertors, led to the develop-
ment of the XPR sensor at Inficon (XPR One can think of the sensor as having been Shielding
standing for extended pressure range). To derived from an extractor measurement Anode
enable direct measurement in the range of system (see Fig. 4.3), whereby the
Extractor
about 2 · 10-2 mbar, so important for sput- separation system was inserted between
diaphragm
ter processes, the rod system was reduced the ion source and the ion trap.
from 12 cm to a length of 2 cm. To ensure Total pressure
diaphragm
that the ions can execute the number of
transverse oscillations required for sharp 4.3.1.1 The normal (open) ion source
mass separation, this number being about
The ion source comprises an arrangement Fig. 4.4 Open ion source
100, the frequency of the current in the

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Mass Spectrometry Fundamentals of Vacuum Technology

4.3.1.2 The quadrupole separation the amplitude of the transverse oscilla-


system xz plane yz plane tions will be smaller than the clearance
+ Rod: - Rod:
between the rods and the ion can pass
Here the ions are separated on the basis of 1 +
+U
+
–U

+
Transmission:
-
Transmission:
to the collector at very large V.
their mass-to-charge ratio. We know from full none

+ Rod: - Rod:
physics that the deflection of electrically 2 +
+U+V, cos ω
+
–U–V · cos ω 3. Ion emission i+ = i+ (V) for a fixed mass
Transmission: Transmission:
charged particles (ions) from their trajec- + low-pass - high-pass
of M:
tory is possible only in accordance with i+ i+

their ratio of mass to charge, since the 3 xz plane (left): For voltages of V < V1 the
V1 V V1 V

attraction of the particles is proportional to deflection which leads to an escalation


i+ i+

the charge while the inertia (which resists 4


of the oscillations is smaller than V1, i.e.
change) is proportional to its mass. The
M1 M M1 M still in the “pass” range. Where V > V1
separation system comprises four cylin- Superimposition of the xy and yz planes the deflection will be sufficient to
drical metal rods, set up in parallel and iso- yz xz ( UV fixed)
induce escalation and thus blockage.
i+

lated one from the other; the two opposing 5 I


II
III
M
yz plane (right): For voltages of V < V1
rods are charged with identical potential. U .. Selectivity (resolution) Sensitivity the deflection which leads to the dam-
V
Fig. 4.2 shows schematically the arrange- ping of the oscillations is smaller than
ment of the rods and their power supply. V1, i.e. still in the “block” range. Where
The electrical field Φ inside the separation Fig. 4.5 Phenomenological explanation of the V > V1 the damping will be sufficient to
system is generated by superimposing a separation system settle oscillations, allowing passage.
DC voltage and a high-frequency AC volta-
ge: 4. Ion flow i+ = i+ (M) for a fixed ratio of
paration system and observe the deflec-
U / V:
tion of a singly ionized, positive ion with
Φ = (U + V ⋅ cos ωt) · (x2 – y2) / r02
atomic number M, moving in two planes, Here the relationships are exactly oppo-
r0 = radius of the cylinder which can be which are perpendicular one to the other site to those for i+ = i+ (V) since the
inscribed inside the system of rods and each passing through the centers of influence of V on light masses is great-
Exerting an effect on a single charged ion two opposing rods. We proceed step-by- er than on heavy masses.
moving near and parallel to the center line step and first observe the xz plane (Fig.
xz plane: For masses of M < M1 the
inside the separation system and perpen- 4.5, left) and then the yz plane (Fig.4.5,
deflection which results in escalation of
dicular to its movement are the forces right):
the oscillations is greater than at M1,
1. Only DC potential U at the rods:
which means that the ions will be
Fx = − 2e ⋅ x ⋅ cos (ω ⋅ t ) xz plane (left): Positive potential of +U blocked. At M > M1 the deflection is no
r02 longer sufficient for escalation, so that
at the rod, with a repellant effect on the
Fy = − 2e2 ⋅ y ⋅ cos (ω ⋅ t ) ion, keeping it centered; it reaches the the ion can pass.
r0 collector (→ passage).
Fz = 0 yz plane: For masses of M < M1 the
yz plane (right): Negative potential on deflection which results in damping of
the rod -U, meaning that at even the the oscillations is greater than at M1,
The mathematical treatment of these equa- tiniest deviations from the center axis which means that the ion will pass. At
tions of motion uses Mathieu’s differential the ion will be drawn toward the nearest M > M1 the damping is not sufficient to
equations. It is demonstrated that there rod and neutralized there; it does not calm the system and so the ion is
are stable and unstable ion paths. With the reach the collector (→ blocking). blocked.
stable paths, the distance of the ions from
2. Superimposition of high-frequency 5. Combination of the xz and yz planes. In
the separation system center line always
remains less than ro (passage condition). voltage V · cos ω t: the superimposition of the ion currents
i+ = i+ (M) for both pairs of rods (U / V
With unstable paths, the distance from the xz plane (left): being fixed) there are three important
axis will grow until the ion ultimately colli- Rod potential +U + V · cos ω t. With ranges:
des with a rod surface. The ion will be rising AC voltage amplitude V the ion
discharged (neutralized), thus becoming will be excited to execute transverse Range I : No passage for M due to the
unavailable to the detector (blocking con- oscillations with ever greater amplitu- blocking behavior of the xz pair of rods.
dition). des until it makes contact with a rod Range II : The pass factor of the rod
Even without solving the differential equa- and is neutralized. The separation systems for mass M is determined by
tion, it is possible to arrive at a purely phe- system remains blocked for very large the U/V ratio (other ions will not pass).
nomenological explanation which leads to values of V. We see that great permeability (corre-
an understanding of the most important sponding to high sensitivity) is bought
yz plane (right):
characteristics of the quadrupole sepa-
ration system.
Rod potential -U -V · cos ω t. Here again
superimposition induces an additional
at the price of low selectivity (= resolu-
tion, see Section 4.5). Ideal adjustment
D00
If we imagine that we cut open the se- force so that as of a certain value for V of the separation system thus requires
a compromise between these two prop-

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Positive ion
Separation system output
Collector
Electron suppressor

Faraday cup

Connection Amplifier
to front end
of the inside
surface Resistance of the inner surface

Amplifier Resistance ≈ 108 Ω


Negative high voltage
R ≈ 4 · 106 Ω

Fig. 4.6 Left: principle of the Faraday cup; right: configuration of the Channeltron

erties. To achieve constant resolution, Channeltrons or Channelplates can be TRANSPECTOR the otherwise unlimited
the U/V ratio will remain constant over used as SEMPs. SEMPs are virtually iner- selection of the scanning period and the
the entire measurement range. The tia-free amplifiers with gain of about 10+6 amplifier time constants will be restricted
“atomic number” M (see 4.6.1) of the at the outset; this will indeed drop off by microprocessor control to logical pairs
ions which can pass through the sepa- during the initial use phase but will then of values.
ration system must satisfy this condi- become virtually constant over a long peri-
tion: od of time. Fig. 4.6 shows at the left the
m V basic configuration of a Faraday ion trap
≈M= and, on the right, a section through a
e 14.438 ⋅ f 2 ⋅ ro2 Channeltron. When recording spectra the
scanning period per mass line t0 and the
V = High-frequency amplitude, time constants of the amplifier t should
rO = Quadrupole inscribed radius satisfy the condition that t0 = 10 τ. In
f = High-frequency modern devices such as the
As a result of this linear dependency
there results a mass spectrum with li-
near mass scale due to simultaneous,
proportional modification of U and V.
Non-segregating gas inlet system
Range III : M cannot pass, due to the
blocking characteristics of the yz pair of Stage B Stage A
rods.
p ≤ 10 –4 mbar p = 1 ... 10 mbar p = 10 ... 1000 mbar

L2 Capillary L3
Mass ^
4.3.1.3 The measurement system spectrometer _ QHV
^
_

(detector) L1
Seff QPumping
No
Once they have left the separation system Molecular flow Laminar flow
segregation
the ions will meet the ion trap or detector
L2 molecular → λ À dL
which, in the simplest instance, will be in 2

1 QHV ¿ QPumping
the form of a Faraday cage (Faraday cup). L2 ~ CD
M
In any case the ions which impinge on the (Transition laminar/molecular)
1
detector will be neutralized by electrons L1 ~ CD
M
from the ion trap. Shown, after electrical Seff À L1 → Seff ~ 1
amplification, as the measurement signal CD
M
itself is the corresponding “ion emission
Seff compensates for L2 → No segregation
S

stream”. To achieve greater sensitivity, a


secondary electron multiplier pickup
(SEMP) can be employed in place of the
Faraday cup. Fig. 4.7 Principle of the pressure converter (stage B only in the single-stage version and stages A and B in
two-stage units)

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Mass Spectrometry Fundamentals of Vacuum Technology

4.4 Gas admission and a. Process pressure < 1 mbar: Single- A falsification of the gas composition
stage pressure converter. resulting from adsorption and condensati-
pressure Gas is allowed to pass out of the vacuum on can be avoided by heating the pressure
vessel in molecular flow, through a dia- converter and the capillary.
adaptation phragm with conduc- tance value L2 and
To evaluate the influence on the gas com-
into the “sensor chamber” (with its own
position by the measurement unit itself,
4.4.1 Metering valve high vacuum system). Molecular flow cau-
information on the heating temperature,
ses segregation but this will be indepen-
The simplest way to adapt a classical mass the materials and surface areas for the
dent of the pressure level (see Section
spectrometer to pressures exceeding metallic, glass and ceramic components
1.5). A second diaphragm with molecular
1 · 10-4 mbar is by way of a metering will be needed along with specifications on
flow, located between the sensor chamber
valve. The inherent disadvantage is, howe- the material and dimensions of the catho-
and the turbomolecular pump, will com-
ver, that since the flow properties are not de (and ultimately regarding the electron
pensate for the segregation occurring at
unequivocally defined, a deviation from the impact energy for the ion source as well).
L2.
original gas composition might result.
b. Process pressure > 1 mbar: Two-stage
pressure converter. Using a small (rotary
vane) pump a laminar stream of gas is
diverted from the rough vacuum area 4.4.3 Closed ion source (CIS)
4.4.2 Pressure converter through a capillary or diaphragm (conduc- In order to curb – or avoid entirely – influ-
In order to examine a gas mix at total pres- tance value L3). Prior to entry into the ences which could stem from the sensor
sure exceeding 1 · 10-4 mbar it is neces- pump, at a pressure of about 1 mbar, a chamber or the cathode (e.g. disturbance
sary to use pressure converters which will small part of this flow is again allowed to of the CO-CO2 equilibrium by heating the
not segregate the gases. Figure 4.7 is used enter the sensor chamber through the dia- cathode) a closed ion source (CIS) will be
to help explain how such a pressure con- phragm with conductance value L2, again used in many cases (see Fig 4.8).
verter works: as molecular flow.

Process: 10 -2 mbar Process: 10 -2 mbar

(Elastomer) Valve (Metal)


Inlet diaphragm

Impact chamber
10 -5
10 -5
10 -5
10 -3 Cathode chamber
Example of the sputter „Exit diaphragm“
process
To be detected is 1 ppm N2 as
contamination in argon,
the working gas
10 -5 10 -5 10 -5 10 -5

1 ppm N 2 at the inlet: 1 ppm N 2 at the inlet:

10 -6 ·10 -5 mbar = 10 -11 mbar 10 -6 · 10 -3 mbar = 10 -9 mbar


Exit diaphragm
Background: Background:
Residual gas (valve closed) 10 -6 mbar total Residual gas (valve closed) 10 -7 mbar total
total, including 1% by mass 28 : 10 -8 mbar Pump Pump total, including 1% by mass 28 : 10 -9 mbar

Background noise 1 ppm

Signal at 1‰ of background Background noise


cannot be detected Signal twice the background noise
amplitude; can just be clearly detected D00
Fig. 4.8 Open ion source (left) and closed ion source (right)

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Fundamentals of Vacuum Technology Mass Spectrometry

Impact chamber
Working gas for the process (Ar)
Cathode chamber
“Exit diaphragms”
AGM protective gas valve

10 -5

Process:
e. g. 50 mbar 10 -3 10 -5

Diaphragm Pump
10 -5

Fig. 4.9 Principle behind the aggressive gas monitor (AGM)

The CIS is divided into two sections: a 4.4.4 Aggressive gas monitor
cathode chamber where the electrons are
4.5 Descriptive values
(AGM)
emitted, and an impact chamber, where in mass
the impact ionization of the gas particles In many cases the process gas to be
takes place. The two chambers are pum- examined is so aggressive that the catho- spectrometry
ped differentially: the pressure in the de would survive for only a short period of (specifications)
cathode chamber comes to about time. The AGM uses the property of lami-
10-5 mbar, that in the impact room about nar flow by way of which there is no A partial pressure measurement unit is
10-3 mbar. The gas from the vacuum “reverse” flow of any kind. Controlled with characterized essentially by the following
chamber is allowed to pass into the impact a separate AGM valve, a part of the wor- properties (DIN 28 410):
chamber by way of a metal-sealed, bakea- king gas fed to the processes is introduced
ble valve (pressure converter, ultrahigh as “purging gas”, ahead of the pressure
vacuum technology). There high-yield converter, to the TRANSPECTOR; this sets
ionization takes place at about 10-3 mbar. up a flow toward the vacuum chamber.
The electrons exerting the impact are emit- Thus process gas can reach the TRANS- 4.5.1 Line width (resolution)
ted in the cathode chamber at about PECTOR only with the AGM valve closed.
10-5 mbar and pass through small ope- When the valve is open the TRANSPEC- The line width is a measure of the degree
nings from there into the impact chamber. TOR sees only pure working gas. Fig. 4.9 to which differentiation can be made bet-
The signal-to-noise ratio (residual gas) via shows the AGM principle. ween two adjacent lines of the same
à vis the open ion source will be increased height. The resolution is normally indica-
overall by a factor of 10+3 or more. Figure ted. It is defined as: R = M / ∆M and is con-
4.8 shows the fundamental difference bet- stant for the quadrupole spectrometer
ween the configurations for open and clo- across the entire mass range, slightly
sed ion sources for a typical application in greater than 1 or ∆M < 1.
sputter technology. With the modified Often an expression such as “unit resoluti-
design of the CIS compared with the open on with 15% valley” is used. This means
ion source in regard to both the geometry that the “bottom of the valley” between
and the electron energy (open ion source two adjacent peaks of identical height
102 eV, CIS 75 or 35 eV), different frag- comes to 15 % of the height of the peak or,
ment distribution patterns may be found put another way, at 7.5 % of its peak
where a lower electron energy level is sel- height the line width DM measured across
ected. For example, the argon36++ isotope an individual peak equals 1 amu (atomic
at mass of 18 cannot be detected at elec- mass unit); see in this context the sche-
tron energy of less than 43.5 eV and can matic drawing in Fig. 4.10.
therefore not falsify the detection of H2O+
at mass 18 in the sputter processes using
argon as the working gas – processes
which are of great importance in industry.

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+
100% log i

Regulation

+ Exact measurement
i range

Automatic shut-down:
≈ 5 · 10 –4

15%
1 amu
7,5%

M M+1 Atomic number


10–8 10–7 10–6 10–5 10–4 10–3 log P
∆M

Fig. 4.10 Line width – 15 % valley Fig. 4.11 Detection of Argon36 Fig. 4.12 Qualitative linearity curve

4.5.2 Mass range 4 ⋅ 10 – 14A which are to be specified (± 10 % for par-


pmin(FC) = = 4 ⋅10 – 10 mbar tial pressure measurement devices).
The mass range is characterized by the 1⋅10 – 4A / mbar
atomic numbers for the lightest and hea- In the range below 1 · 10-6 mbar the rela-
viest ions with a single charge which are tionship between the ion flow and partial
detected with the unit. pressure is strictly linear. Between 1 · 10-6
4.5.5 Smallest detectable
mbar and 1 · 10-4 mbar there are minor
partial pressure ratio deviations from linear characteristics.
4.5.3 Sensitivity (concentration) Above 1 · 10-4 mbar these deviations grow
The definition is: until, ultimately, in a range above 10-2
Sensitivity E is the quotient of the measu- mbar the ions for the dense gas atmos-
red ion flow and the associated partial SDPPR = pmin / pΣ (ppm) phere will no longer be able to reach the
pressure; it is normally specified for argon ion trap. The emergency shut-down for the
This definition, which is somewhat “clum-
or nitrogen: cathode (at excessive pressure) is almost
sy” for practical use, is to be explained
using the detection of argon36 in the air as always set for 5 · 10-4 mbar. Depending on
i+  A 
E=   (4.1) the example: Air contains 0.93 % argon by the information required, there will be dif-
pG  mbar fering upper limits for use.
volume; the relative isotope frequency of
Typical values are: Ar40 to Ar36 is 99.6 % to 0.337 %. Thus In analytical applications, 1 · 10-6 mbar
the share of Ar36 in the air can be calcula- should not be exceeded if at all possible.
Faraday cup: E = 1⋅10 – 4
A ted as follows: The range from 1 · 10-6 mbar to 1 · 10-4
mbar mbar is still suitable for clear depictions of
0.93 · 10–2 · 0.337 · 10–2 = 3.13 · 10–5 =
31.3 ppm the gas composition and partial pressure
A regulation (see Fig. 4.12).
SEM: E = 1⋅10 +2 Figure 4.11 shows the screen print-out for
mbar
the measurement. The peak height for Ar36
in the illustration is determined to be
1.5 · 10-13 A and noise amplitude ∆ · i+ to
R
be 4 · 10-14 A. The minimum detectable 4.5.7 Information on surfaces
4.5.4 Smallest detectable concentration is that concentration at which and amenability to
partial pressure the height of the peak is equal to the noise bake-out
amplitude. This results in the smallest mea-
The smallest detectable partial pressure is surable peak height being Additional information required to evaluate
defined as a ratio of noise amplitude to 1.5 · 10-13 A/2.4 · 10-14 A = 1.875. The a sensor includes specifications on the
sensitivity: smallest detectable concentration is then bake-out temperature (during measure-
derived from this by calculation to arrive at: ment or with the cathode or SEMP swit-
∆ ⋅iR+
Pmin = (mbar) ched off), materials used and surface
E 31.3 · 10–6 / 1.875 = 16.69 · 10–6
areas of the metal, glass and ceramic com-
= 16.69 ppm.
ponents and the material and dimensions
Æ á i+ = Noise amplitude for the cathode; data is also needed on the
R
Example (from Fig. 4.11): electron impact energy at the ion source
(and on whether it is adjustable). These
Sensitivity E = 1⋅ 10– 4
A
mbar
4.5.6 Linearity range
The linearity range is that pressure range
values are critical to uninterrupted operati-
on and to any influence on the gas compo-
D00
for the reference gas (N2, Ar) in which sen- sition by the sensor itself.
Noise amplitude Æ á i+ = 4 · 10–14 A sitivity remains constant within limits
R

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4.6 Evaluating spectra Element Ordinal- Atomic Relative Element Ordinal- Atomic Relative
number number frequency number number frequency
H 1 1 99.985 S 16 32 95.06
4.6.1 Ionization and fundamen- 2 0.015 33 0.74
tal problems in gas ana- He 2 3 0.00013 34 4.18
lysis 4 ≈ 100.0 36 0.016
B 5 10 19.78 Cl 17 35 75.4
Continuous change in the voltages applied
11 80.22 37 24.6
to the electrodes in the separation system
C 6 12 98.892 Ar 18 36 0.337
(“scanning”) gives rise to a relationship
13 1.108 38 0.063
between the ion flow I+ and the “atomic N 7 14 99.63 40 99.60
number” which is proportional to the m/e 15 0.37 Kr 36 78 0.354
ratio and expressed as: O 8 16 99.759 80 2.27
Mr 17 0.0374 82 11.56
M= (4.2)
ne 18 0.2039 83 11.55
F 9 19 100.0 84 56.90
(Mr = relative molar mass, Ne 10 20 90.92 86 17.37
ne = number of elementary charges e) 21 0.257 Xe 54 124 0.096
22 8.82 126 0.090
Na 11 23 100.0 128 1.919
This is the so-called mass spectrum,
Al 13 27 100.0 129 26.44
i+ = i+(M). The spectrum thus shows the
Si 14 28 92.27 130 4.08
peaks i+ as ordinates, plotted against the
29 4.68 131 21.18
atomic number M along the abscissa. One
30 3.05 132 26.89
of the difficulties in interpreting a mass
P 15 31 100.0 134 10.44
spectrum such as this is due to the fact
136 8.87
that one and the same mass as per the
equation (4.2) may be associated with Table 4.2 Relative frequency of isotopes Table 4.2 Relative frequency of isotopes
various ions. Typical examples, among
many others, are: The atomic number yield is greatest at an electron energy level 4) Finally, gas molecules are often broken
M = 16 corresponds to CH+4 and O2++; between about 80 and 110 eV; see Fig. down into fragments by ionization. The
M = 28 for CO+, N+2 and C2H+! Particular 4.14. fragment distribution patterns thus crea-
attention must therefore be paid to the fol- ted are the so-called characteristic spectra
lowing points when evaluating spectra: In practice the differing ionization rates for
(fingerprint, cracking pattern).
the individual gases will be taken into
1) In the case of isotopes we are dealing account by standardization against nitro- Important: In the tables the individual frag-
with differing positron counts in the nucle- gen; relative ionization probabilities ments specified are standardized either
us (mass) of the ion at identical nuclear (RIP) in relationship to nitrogen will be against the maximum peak (in % or ‰ of
charge numbers (gas type). Some values indicated (Table 4.3). the highest peak) or against the total of all
for relative isotope frequency are compiled peaks (see the examples in Table 4.4).
in Table 4.2.
2) Depending on the energy of the impac- 12
ting electrons (equalling the potential diffe-
rential, cathode – anode), ions may be eit- 10
+
her singly or multiply ionized. For example, Ar
Ions formed per cm · mbar

one finds Ar+ at mass of 40, Ar++ at mass 8


of 20 and Ar+++ at mass of 13.3. At mass
of 20 one will, however, also find neon, 6
Ne+. There are threshold energy levels for
the impacting electrons for all ionization 4
states for every type of gas, i.e., each type
of ion can be formed only above the asso- 2
ciated energy threshold. This is shown for
Ar in Fig. 4.13. 0 100 200 300 400 500
3) Specific ionization of the various Electron energy (eV)
gases Sgas, this being the number of ions Threshold
formed, per cm and mbar, by collisions energy Ar+ 15,7 eV Ar++ 43,5 eV Ar3+ 85,0 eV Ar4+ 200 eV
for argon ions
with electrons; this will vary from one type
of gas to the next. For most gases the ion Fig. 4.13 Number of the various Ar ions produced, as a factor of electron energy level

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quarter of the share of N+2 with its mass of


28. If, on the other hand, no oxygen is
detected in the spectrum, then the peak at
atomic number 28 would indicate carbon
monoxide. In so far as the peak at atomic
number 28 reflects the CO+ fragment of
Ions formed per cm · mbar

CO2 (atomic number 44), this share is


11 % of the value measured for atomic
number 44 (Table 4.5). On the other hand,
in all cases where nitrogen is present, ato-
mic number 14 (N2++) will always be found
in the spectrum in addition to the atomic
number 28 (N+2); in the case of carbon
monoxide, on the other hand, there will
always appear – in addition to CO+ – the
fragmentary masses of 12 (C+) and
++
16 (O2 )).
Figure 4.15 uses a simplified example of a
Electron energy (eV) “model spectrum” with superimpositions
of hydrogen, nitrogen, oxygen, water
Fig. 4.14 Specific ionization S for various gases by electrons exhibiting energy level E vapor, carbon monoxide, carbon dioxide,
neon and argon to demonstrate the diffi-
Both the nature of the fragments created obtained using devices made by different culties involved in evaluating spectra.
and the possibility for multiple ionization manufacturers.
will depend on the geometry (differing ion
Often the probable partial pressure for one
number, depending on the length of the
of the masses involved will be estimated
ionization path) and on the energy of the
through critical analysis of the spectrum.
impacting electrons (threshold energy for
Thus the presence of air in the vacuum
certain types of ions). Table values are
vessel (which may indicate a leak) is mani-
always referenced to a certain ion source +
fested by the detection of a quantity of O2
with a certain electron energy level. This is
(with mass of 32) which is about one-
why it is difficult to compare the results

CO+
O+

O+
H2+ Ar++ CO+
H 2 O+ O2 + Ar+ CO2+

H2+
O+
N+
H+ OH+ Ne+ N2+
C+ O+
13C+ H3O+ 22Ne +
13CO+

H+ Ne++ C+ 16O18O+ 36Ar+ 13C16O +


2
14N15N+

0 5 10 15 20 25 30 35 40 45 50
Hydrogen Oxygen Carbon dioxide Argon
Nitrogen Water Neon Carbon monoxide

Evaluation problems: The peak at atomic number 16 may, for example, be due to oxygen fragments resulting from O2, H2O, CO2 and CO; the peak at ato-
mic number 28 from contributions by N2 as well as by CO and CO as a fragment of CO2; the peak at atomic number 20 could result from singly ionized
Ne and double-ionized Ar D00
Fig. 4.15 Model spectrum

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Fundamentals of Vacuum Technology Mass Spectrometry

Type of gas Symbol RIP Type of gas Symbol RIP


Acetone (Propanone) (CH3)2CO 3.6 Hydrogen chloride HCl 1.6
Air 1.0 Hydrogen fluoride HF 1.4
Ammonia NH3 1.3 Hydrogen iodide HI 3.1
Argon Ar 1.2 Hydrogen sulfide H2S 2.2
Benzene C6H6 5.9 Iodine I2
Benzoic acid C6H5COOH 5.5 Krypton Kr 1.7
Bromine Br 3.8 Lithium Li 1.9
Butane C4H10 4.9 Methane CH4 1.6
Carbon dioxide CO2 1.4 Methanol CH3OH 1.8
Carbon disulfide CS2 4.8 Neon Ne 0.23
Carbon monoxide CO 1.05 Nitrogen N2 1.0
Carbon tetrachloride CCl4 6.0 Nitrogen oxide NO 1.2
Chlorobenzene C6H4Cl 7.0 Nitrogen dioxide N2O 1.7
Chloroethane C2H3Cl 4.0 Oxygen O2 1.0
Chloroform CHCl3 4.8 n-pentane C5H17 6.0
Chlormethane CH3Cl 3.1 Phenol C6H5OH 6.2
Cyclohexene C6H12 6.4 Phosphine PH3 2.6
Deuterium D2 0.35 Propane C3H8 3.7
Dichlorodifluoromethane CCl2F2 2.7 Silver perchlorate AgClO4 3.6
Dichloromethane CH2Cl2 7.8 Tin iodide Snl4 6.7
Dinitrobenzene C6H4(NO2)2 7.8 Sulfur dioxide SO2 2.1
Ethane C2H6 2.6 Sulfur hexafluoride SF6 2.3
Ethanol C2H5OH 3.6 Toluene C6H5CH3 6.8
Ethylene oxide (CH2)2O 2.5 Trinitrobenzene C6H3(NO2)3 9.0
Helium He 0.14 Water vapor H2O 11.0
Hexane C6H14 6.6 Xenon Xe 3.0
Hydrogen H2 0.44 Xylols C6H4(CH3)2 7.8
Table 4.3 Relative ionization probabilities (RIP) vis à vis nitrogen, electron energy 102 eV

Electron energy : 75 eV (PGA 100) 102 eV (Transpector)


Gas Symbol Mass Σ = 100 % Greatest peak = 100 % Σ = 100 % Greatest peak = 100 %
Argon Ar 40 74.9 100 90.9 100
20 24.7 33.1 9.1 10
36 0.3
Carbon dioxide CO2 45 0.95 1.3 0.8 1
44 72.7 100 84 100
28 8.3 11.5 9.2 11
16 11.7 16.1 7.6 9
12 6.15 8.4 5 6
Carbon monoxide CO 29 1.89 2.0 0.9 1
28 91.3 100 92.6 100
16 1.1 1.2 1.9 2
14 1.7 1.9 0.8
12 3.5 3.8 4.6 5
Neon Ne 22 9.2 10.2 0.9 11
20 89.6 100 90.1 100
10 0.84 0.93 9 4
Oxygen O2 34 0.45 0.53
32 84.2 100 90.1 100
16 15.0 17.8 9.9 11
Nitrogen N2 29 0.7 0.8 0.9 1
28 86.3 100 92.6 100
14 12.8 15 6.5 12
Water vapor H2O 19 1.4 2.3
18 60 100 74.1 100
17 16.1 27 18.5 25
16 1.9 3.2 1.5 2
2 5.0 8.4 1.5 2
1 15.5 20 4.4 6
Table 4.4 Fragment distribution for certain gases at 75 eV and 102 eV

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No Gas Symbol 1 = 100 2 3 4 5 6


1 Acetone (CH3)2CO 43/100 15/42 58/20 14/10 27/19 42/8
2 Air 28/100 32/27 14/6 16/3 40/1 -
3 Ammonia NH3 17/100 16/80 15/8 14/2 - -
4 Argon Ar 40/100 20/10 - - - -
5 Benzene C6H6 78/100 77/22 51/18 50/17 52/15 39/10
6 Carbon dioxide CO2 44/100 28/11 16/9 12/6 45/1 22/1
7 Carbon monoxide CO 28/100 12/5 16/2 29/1 - -
8 Carbon tetrachloride CCl4 117/100 119/91 47/51 82/42 35/39 121/29
9 Carbon tetrafluoride CF4 69/100 50/12 31/5 19/4 - -
10 Diff. pump oil, DC 705 78/100 76/83 39/73 43/59 91/32 -
11 Diff. pump oil, Fomblin 69/100 20/28 16/16 31/9 97/8 47/8
12 Diff. pump oil, PPE 50/100 77/89 63/29 62/27 64/21 38/7
13 Ethanol CH3CH2OH 31/100 45/34 27/24 29/23 46/17 26/8
14 Halocarbon 11 CCl3F 101/100 103/60 35/16 66/15 47/12 31/10
15 Halocarbon 12 CCl2F2 85/100 87/32 50/16 35/12 - -
16 Halocarbon 13 CClF3 69/100 85/15 50/14 31/9 35/7 87/5
17 Halocarbon 14 CF4 69/100 12/7 19/6 31/5 50/8 -
18 Halocarbon 23 CHF3 51/100 31/58 69/40 50/19 52/1 21/1
19 Halocarbon 113 C2C13F3 101/100 103/62 85/55 31/50 151/41 153/25
20 Helium He 4/100 - - - - -
21 Heptane C7H16 43/100 41/62 29/49 27/40 57/34 71/28
22 Hexane C6H14 41/100 43/92 57/85 29/84 27/65 56/50
23 Hydrogen H2 2/100 1/5 - - - -
24 Hydrogen sulfide H2S 34/100 32/44 33/42 36/4 35/2 -
25 Isopropyl alcohol C3H8O 45/100 43/16 27/16 29/10 41/7 39/6
26 Krypton Kr 84/100 86/31 83/20 82/20 80/4 -
27 Methane CH4 16/100 15/85 14/16 13/8 1/4 12/2
28 Mehtyl alcohol CH3OH 31/100 29/74 32/67 15/50 28/16 2/16
29 Methyl ethyl ketone C4H8O 43/100 29/25 72/16 27/16 57/6 42/5
30 Mechanical pump oil 43/100 41/91 57/73 55/64 71/20 39/19
31 Neon Ne 20/100 22/10 10/1 - - -
32 Nitrogen N2 28/100 14/7 29/1 - - -
33 Oxygen O2 32/100 16/11 - - - -
34 Perfluorokerosene 69/100 119/17 51/12 131/11 100/5 31/4
35 Perfluor-tributylamine C12F27N 69/100 131/18 31/6 51/5 50/3 114/2
36 Silane SiH4 30/100 31/80 29/31 28/28 32/8 33/2
37 Silicon tetrafluoride SiF4 85/100 87/12 28/12 33/10 86/5 47/5
38 Toluene C6H5CH3 91/100 92/62 39/12 65/6 45.5/4 51/4
39 Trichloroethane C2H3Cl3 97/100 61/87 99/61 26/43 27/31 63/27
40 Trichloroethylene C2HCl3 95/100 130/90 132/85 97/64 60/57 35/31
41 Trifluoromethane CHF3 69/100 51/91 31/49 50/42 12/4 -
42 Turbomolecular pump oil 43/100 57/88 41/76 55/73 71/52 69/49
43 Water vapor H2O 18/100 17/25 1/6 16/2 2/2 -
44 Xenon Xe 132/100 129/98 131/79 134/39 136/33 130/15

Table 4.5 Spectrum library of the 6 highest peaks for the TRANSPECTOR
D00

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4.6.2 Partial pressure + only after the spectrum has been standar-
pgas = igas , m 2 (measured ) ⋅
measurement dized, by setting the height of the highest
1 1 line equal to 100 or 1000 (see Table 4.5 as
The number of ions i+gas produced from a ⋅
E N2 BFgas , m2 ⋅ RIPgas ⋅TF (m) (4.3) an example).
gas in the ion source is proportional to the
emission current i–, to the specific ioni- The comparison can be made manually on
The partial pressure is calculated from the the basis of collections of tables (for
zation Sgas, to a geometry factor f repre-
ion flow measured for a certain fragment example, A. Cornu & R. Massot: Compil-
senting the ionization path inside the
by multiplication with two factors. The first ation of Mass Spectral Data) or may be
ionization source, to the relative ionization
factor will depend only on the nitrogen effected with computer assistance; large
probability RIPgas, and to the partial pres-
sensitivity of the detector and thus is a databases can be used (e.g. Mass Spectral
sure pgas. This number of ions produced
constant for the device. The second will Data Base, Royal Society of Chemistry,
is, by definition, made equal to the sensi-
depend only on the specific ion properties. Cambridge).
tivity Egas times the partial pressure pgas:
These factors will have to be entered sepa- When making comparisons with library
i+gas (produced) = i- · Sgas · f · RIPgas · pgas rately for units with direct partial pressure information, it is necessary to pay attenti-
= Egas · pgas indication (at least for less common types on to whether identical ion sources or at
of ions). least identical electron impact energies
due to RIPN2 = 1
were used.
EN2 is equal to i– · SN2 · f All these capabilities are, however, gene-
and Egas is equal to EN2 · RIPgas rally too elaborate for the problems
4.6.3 Qualitative gas analysis encountered in vacuum technology. Many
Almost all gases form fragments during commercial mass spectrometers can show
ionization. To achieve quantitative evalu- The analysis of spectra assumes certain a number of library spectra in the screen
ation one must either add the ion flows at working hypotheses: so that the user can see immediately
the appropriate peaks or measure (with a whether the “library substance” might be
1. Every type of molecule produces a cer-
known fragment factor [FF]) one peak and contained in the substance measured.
tain, constant mass spectrum or frag-
calculate the overall ion flow on that basis: Usually the measured spectrum was the
ment spectrum which is characteristic
result of a mix of gases and it is particu-
+
igas for this type of molecule (fingerprint,
+ + + ,m1 larly convenient if the screen offers the
igas (produced )= igas ,m 1 + igas ,m2 +.... = cracking pattern).
+
BFgas,m 1 capacity for subtracting (by way of trial)
igas,m2
= =.... = Egas ⋅ pgas 2. The spectrum of every mixture of gases the spectra of individual (or several) gases
BFgas,m2 is the same as would be found through from the measured spectrum. The gas can
linear superimposition of the spectra of be present only when the subtraction does
In order to maintain the number of ions the individual gases. The height of the not yield any negative values for the major
arriving at the ion trap, it is necessary to peaks will depend on the gas pressure. peaks. Figure 4.16 shows such a step-by-
multiply the number above with the trans- step subtraction procedure using the
mission factor TF(m), which will be depen- 3. The ion flow for each peak is proportio-
Transpector-Ware software.
dent on mass, in order to take into account nal to the partial pressure of each com-
the permeability of the separation system ponent responsible for the peak. Since Regardless of how the qualitative analysis
for atomic number m (analogous to this, the ion flow is proportional to the parti- is prepared, the result is always just a
there is the detection factor for the SEMP; al pressure, the constant of proportio- “suggestion”, i.e. an assumption as to
it, however, is often already contained in nality (sensitivity) varies from one gas which gases the mixture might contain.
TF). The transmission factor (also: ion- to the next. This suggestion will have still to be exami-
optical transmission) is thus the quotient ned, e.g. by considering the likelihood that
Although these assumptions are not
of the ions measured and the ions produ- a certain substance would be contained in
always correct (see Robertson: Mass
ced. the spectrum. In addition, recording a new
Spectrometry) they do represent a useful
spectrum for this substance can help to
Thus working hypothesis.
achieve clarity.
In qualitative analysis, the unknown spec-
, m2(produced)
+
igas
pgas = trum is compared with a known spectrum
BFgas , m2 ⋅ Egas in a library. Each gas is “definitively deter-
+
igas , m (measured ) mined” by its spectrum. The comparison
⇒ pgas = 2
with library data is a simple pattern reco-
BFgas , m ⋅ E gas ⋅TF (m)
2 gnition process. Depending on the availa-
bility, the comparison may be made using
and with any of a number ancillary aids. So, for
Egas = EN2 · RIPgas example, in accordance with the position,
size and sequence of the five or ten highest
the ultimate result is: peaks. Naturally, comparison is possible

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4.6.4 Quantitative gas analysis


Particular difficulties are encountered
when interpreting the spectrum of an
Parent spectrum unknown mixture of gases. The proporti-
ons of ion flow from various sources can
be offset one against the other only after
all the sources have been identified. In
many applications in vacuum technology
one will be dealing with mixtures of a few
A A = Parent simple gases of known identity, with ato-
range mic numbers less of than 50 (whereby the
process-related gases can represent
exceptions). In the normal, more compli-
cated case there will be a spectrum with a
multitude of superimpositions in a com-
Parent spectrum Assumption: pletely unknown mixture of many gas
Groups components; here a qualitative analysis
2 1
1 = Kr ypton + will have to be made before attempting
2 = Krypton ++ quantitative analysis. The degree of diffi-
culty encountered will depend on the num-
ber of superimpositions (individual/a few/
Library spectrum: many).
Krypton In the case of individual superimpositions,
mutual, balancing of the ion flows during
measurement of one and the same type of
gas for several atomic numbers can often
Parent spectrum without krypton Assumption: be productive.
3 Argon + Where there is a larger number of super-
4 3 4 Argon ++ impositions and a limited number of gases
overall, tabular evaluation using correction
factors vis à vis the spectrum of a calibra-
tion gas of known composition can often
Library spectrum: be helpful.
Argon
In the most general case a plurality of
gases will make a greater or lesser contri-
bution to the ion flow for all the masses.
The share of a gas g in each case for the
Parent spectrum without argon Assumption: atomic number m will be expressed by the
5 Neon + fragment factor Ffm,g. In order to simplify
5 calculation, the fragment factor Ffm,g will
also contain the transmission factor TF
and the detection factor DF. Then the ion
current to mass m, as a function of the
Library spectrum: overall ion currents of all the gases invol-
Neon ved, in matrix notation, is:

i j+   BF j, k ⋅ ⋅ ⋅ ⋅ ⋅ BF j,o   I k+ 
    
⋅ ⋅ ⋅ ⋅ ⋅ ⋅ ⋅  ⋅
⋅    
⋅  ⋅ ⋅ ⋅ ⋅ ⋅ ⋅ ⋅  ⋅
Parent spectrum after detection i +   ⋅ ⋅ ⋅ FFm, g ⋅ ⋅ ⋅  ·  I g+ 
=
of krypton, argon and neon  m    
⋅  ⋅ ⋅ ⋅ ⋅ ⋅ ⋅ ⋅  ⋅
⋅  ⋅ ⋅ ⋅ ⋅ ⋅ ⋅ ⋅  ⋅
 +    
iu   BFu, k ⋅ ⋅ ⋅ ⋅ ⋅ BFu,o  I o+ 

The ion current vector for the atomic num-


D00
Fig. 4.16 Subtracting spectra contained in libraries bers m (resulting from the contributions
by the fragments of the individual gases) is
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equal to the fragment matrix times the vec- 4.7 Software in particular to analyze interesting process
tor of the sum of the flows for the indivi- sections exactly, both during the process
dual gases. and retroactively, once the process has run
to completion, without having to interrupt
0 4.7.1 Standard SQX software
or: im+ = ∑ BFm, g · I g+ (DOS) for stand-alone
the measurement operations which are
g=k running in the background. Where
operation (1 MS plus ongoing monitoring of identical processes
(in simplified notation: i = FF · I) 1 PC, RS 232) is undertaken the program can generate
+
where im = ion flow vector for the atomic statistics (calculating mean values and
The conventional software package (SQX) standard deviations) from which a band-
numbers, resulting from contributions of
contains the standard routines for the width for “favorable process operation”
fragments of various individual gases
operation of the mass spectrometer can be derived. Error reports are issued
0
(MS)– various spectra depictions, queries where limit values are exceeded.
∑ BFm, g = fragment matrix of individual channels with the correspon-
g=k ding screen displays as tables or bar
charts, partial pressure conversion, trend
I+g = Vector of the sum of the flows for the displays, comparison with spectra libra-
individual gases or: ries (with the capability for trial subtrac-
4.7.4 Development software –
tion of library spectra), leak testing mode
Ff m, g etc. – and for sensor balancing, as well. TranspectorView
6444474448
Using PCs as the computer and display This software used to for develop custom
im+ = ∑ pg ⋅ E N2 ⋅ RIPg ⋅ FFm ⋅ TFm unit naturally makes available all the usual software versions for special situations. It
Transmission factor functions including storing and retrieving is based on the LabView development
for the mass m
Fragment factor
data, printing, etc. Characteristic of the package and includes the drivers required
for the gas to mass m conventional software package is that spe- to operate the Transpector.
Relative ionization probability
for the gas cific individual spectra will be measured,
Nitrogen sensitivity (equipment constant) even though the measurement is fully
Partial pressure of the gas automated and takes place at a point in
Ion current for atomic number m
time which is specified in advance. A
spectrum of this type can thus be only a
One sees that the ion flow caused by a gas
“snapshot” of a process in progress.
4.8 Partial pressure
is proportional to the partial pressure. The
linear equation system can be solved only regulation
for the special instance where m = g
Some processes, such as reactive sputter
(square matrix); it is over-identified for
processes, require the most constant pos-
m > g. Due to unavoidable measurement
4.7.2 Multiplex/DOS software sible incidence rates for the reacting gas
error (noise, etc.) there is no set of overall
molecules on the substrate being coated.
ion flow I+g (partial pressures or concentra- MQX (1 to 8 MS plus
tions) which satisfies the equation system 1 PC, RS 485) The “incidence rate” is the same as the
“impingement rate” discussed in Chapter
exactly. Among all the conceivable soluti- The first step toward process-oriented 1; it is directly proportional to the partial
ons it is now necessary to identify set Ig+* software by INFICON is the MQX. It makes pressure. The simplest attempt to keep the
which after inverse calculation to the parti- possible simultaneous monitoring of a partial pressure for a gas component con-
al ion flows Im +
* will exhibit the smallest maximum of eight sensors and you can stant is throughput by regulating with a
apply all the SQX functions at each sensor. flow controller; it does have the disadvan-
squared deviation from the partial ion cur-
+
rents im actually measured. Thus: tage that the regulator cannot determine
whether, when and where the gas con-
sumption or the composition of the gas in
∑(im − im*) = min
+ + 2
the vacuum chamber changes. The far
4.7.3 Process-oriented soft- superior and more effective option is parti-
This minimization problem is mathematic- ware –Transpector-Ware al pressure control using a mass spectro-
ally identical to the solution of another meter via gas inlet valves. Here the signifi-
equation system
for Windows
cant peaks of the gases being considered
FFT · i = FFT · FF · I Transpector-Ware is based on an entirely are assigned to channels in the mass spec-
new philosophy. During the course of the trometer. Suitable regulators compare the
which can be evaluated direct by the com- process (and using settings – the “recipe” analog output signals for these channels
puter. The ion current vector for the indivi- – determined beforehand) data will be with set-point values and derive from the
dual gases is then: recorded continuously – like the individual difference between the target and actual
–1 frames in a video. These data can be sto-
[FF T ⋅ i] ⋅ [FF T ⋅ BF ] values for each channel the appropriate
I= red or otherwise evaluated. It is possible
det[FF T ⋅ BF ] actuation signal for the gas inlet valve for

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Mass Spectrometry Fundamentals of Vacuum Technology

the channel. A configuration of this kind


has been realized to control six channels in t4
t5
the QUADREX PPC. Gas inlet valves mat- Mass spectrometer
ching the unit can also be delivered.
The gas used to measure the impingement
rate (partial pressure) must naturally be Pressure stage
Regulation valve t1 ^
ef
drawn from a representative point in the _
Sensor
t6 t2 t3
vacuum chamber. When evaluating the e Vacuum vessel ef

e
time constant for a regulation circuit of this
type it is important to take into account all TMP50CF
the time aspects and not just the electrical
signal propagation and the processing in
the mass spectrometer, but also the vacu-
um-technology time constants and flow
velocities, as illustrated in Figure 4.17.
Pressure converters or unfavorably instal- Fig. 4.17 Partial shares for overall time constants
led gas inlet lines joining the control valve
and the vacuum vessel will make particu- Sensor balancing at the mass axis (often grime, then the adjustment of the rods
larly large contributions to the overall time erroneously referred to as calibration) is which will be required afterwards will have
constant. It is generally better to establish done today in a very easy fashion with the to be carried out at the factory.
a favorable S/N ratio with a large signal (i.e. software (e.g. SQX, Transpector-Ware)
through an inlet diaphragm with a large and can be observed directly in the screen.
opening) rather than with long integration Naturally, not only the arrangement along
periods at the individual channels. Contra- the mass axis will be determined here, but
sted in Figure 4.18 are the effects of boo- also the shape of the lines, i.e. resolution
sting pressure and lengthening the integra- and sensitivity (see Section 4.5).
tion time on signal detectability. In depic-
tions a, b and c only the integration period It will be necessary to clean the sensor
was raised, from 0.1 to 1.0 and 10 seconds only in exceptional cases where it is heavi-
(thus by an overall factor of 100), respec- ly soiled. It is usually entirely sufficient to
tively. By comparison, in the sequence a-d- clean the ion source, which can be easily
e-f, at constant integration time, the total dismantled and cleaned. The rod system
pressure was raised in three steps, from can be cleaned in an ultrasonic bath once
7.2 · 10-6 mbar to 7.2 · 10-5 mbar (or by a it has been removed from the config-
factor of just 10 overall). uration. If dismantling the system is una-
voidable due to particularly stubborn

a b c
4.9 Maintenance
(Cathode service life, sensor balancing,
cleaning the ion source and rod system)
The service life of the cathode will depend
greatly on the nature of the loading. Expe-
rience has shown that the product of ope-
rating period multiplied by the operating
pressure can serve as a measure for the d e f
loading. Higher operating pressures (in a
range of 1 · 10-4 to 1 · 10-3 mbar) have a
particularly deleterious effect on service
life, as do certain chemical influences such
as refrigerants, for example. Changing out
the cathode is quite easy, thanks to the
simple design of the sensor. It is advisab-
le, however, to take this opportunity to D00
change out or at least clean the entire ion
source. Fig. 4.18 Improving the signal-to-noise ratio by increasing the pressure or extending the integration time

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Fundamentals of Vacuum Technology Leak Detection

• Indirect leaks: leaking supply lines in


5. Leaks and their vacuum systems or furnaces (water,
where R = 83.14 mbar · l/mol · K, T = tem-
perature in K; M = molar mass in g/mole;
∆m for the mass in g; ∆t is the time period
detection compressed air, brine)
in seconds. Equation 5.1 is then used
• “Serial leaks”: this is the leak at the end
a) to determine the mass flow ∆m / ∆t at a
Apart from the vacuum systems them- of several “spaces connected in series”,
known pV gas flow of ∆p · V/∆t (see in
selves and the individual components used e.g. a leak in the oil-filled section of the
this context the example at 5.4.1) or
in their construction (vacuum chambers, oil pan in a rotary vane pump
piping, valves, detachable [flange] connec- b) to determine the pV leak gas flow where
• “One-way leaks”: these will allow gas to
tions, measurement instruments, etc.), the mass flow is known (see the follo-
there are large numbers of other systems pass in one direction but are tight in the wing example).
and products found in industry and rese- other direction (very seldom)
Example for case b) above:
arch which must meet stringent require- An area which is not gas-tight but which is
ments in regard to leaks or creating a so- not leaky in the sense that a defect is pre- A refrigeration system using Freon (R 12)
called “hermetic” seal. Among these are sent would be the exhibits refrigerant loss of 1 g of Freon per
many assemblies and processes in the year (at 25 °C). How large is the leak gas
automotive and refrigeration industries in • Permeation (naturally permeability) of flow QL? According to equation 5.1 for
particular but also in many other branches gas through materials such as rubber M(R12) = 121 g/mole:
of industry. Working pressure in this case hoses, elastomer seals, etc. (unless
these parts have become brittle and ∆( p ⋅V ) . mbar ⋅ `⋅ 298K ⋅ 1g
8314
is often above ambient pressure. Here QL = =
thus “leaky”). ∆t mol ⋅ K ⋅ 121g ⋅ mol –1⋅ 1year
“hermetically sealed” is defined only as a
relative “absence of leaks”. Generalized . ⋅ 2.98 ⋅102⋅ 1 mbar ⋅ `
8314
statements often made, such as “no detec- = ⋅
121⋅1 . ⋅107s
315
table leaks” or “leak rate zero”, do not
represent an adequate basis for accep- . ⋅ 2.98⋅102 –7 mbar ⋅ `
8314
= ⋅ 10 ⋅
tance testing. Every experienced engineer 5.2 Leak rate, leak 1.21⋅102⋅ 315
. s
knows that properly formulated accep-
tance specifications will indicate a certain size, mass flow = 65 ⋅10–7⋅
mbar ⋅ `
s
leak rate (see Section 5.2) under defined No vacuum device or system can ever be
conditions. Which leak rate is acceptable is absolutely vacuum-tight and it does not Thus the Freon loss comes to
also determined by the application itself. actually need to be. The simple essential is QL = 6.5 · 10–6 mbar·l·s-1. According to the
that the leak rate be low enough that the “rule of thumb” for high vacuum systems
required operating pressure, gas balance given below, the refrigeration system men-
and ultimate pressure in the vacuum con- tioned in this example may be deemed to
tainer are not influenced. It follows that the be very tight. Additional conversions for
5.1 Types of leaks requirements in regard to the gas-tightn- QL are shown in Tables VIIa and VIIb in
ess of an apparatus are the more stringent Chapter 9.
Differentiation is made among the follo- the lower the required pressure level is. In
wing leaks, depending on the nature of the order to be able to register leaks quantita- The following rule of thumb for quantita-
material or joining fault: tively, the concept of the “leak rate” with tive characterization of high vacuum
the symbol QL was introduced; it is mea- equipment may be applied:
• Leaks in detachable connections: Flan-
sured with mbar·l·s-1 or cm3/s (STP) as Total leak rate < 10-6 mbar·l·s-1:
ges, ground mating surfaces, covers
the unit of measure. A leak rate of Equipment is very tight
• Leaks in permanent connections:Solder QL = 1 mbar·l·s-1 is present when in an
and welding seams, glued joints enclosed, evacuated vessel with a volume Total leak rate 10-5 mbar·l·s-1:
of 1 l the pressure rises by 1 mbar per Equipment is sufficiently tight
• Leaks due to porosity: particularly follo-
second or, where there is positive pressu- Total leak rate > 10-4 mbar·l·s-1:
wing mechanical deformation (ben- re in the container, pressure drops by 1 Equipment is leaky
ding!) or thermal processing of poly- mbar. The leak rate QL defined as a mea-
crystalline materials and cast compo- sure of leakiness is normally specified in A leak can in fact be “overcome” by a
nents the unit of measure mbar·l·s-1. With the pump of sufficient capacity because it is
true that (for example at ultimate pressure
• Thermal leaks (reversible): opening up assistance of the status equation (1.7) one
can calculate QL when giving the tempera- pend and disregarding the gas liberated
at extreme temperature loading (heat/
ture T and the type of gas M, registering from the interior surfaces):
cold), above all at solder joints
this quantitatively as mass flow, e.g. in the QL
• Apparent (virtual) leaks: quantities of g/s unit of measure. The appropriate p = (5.2)
end S
gas will be liberated from hollows and relationship is then: eff
cavities inside cast parts, blind holes
and joints (also due to the evaporation ∆(p ⋅ V ) R ⋅ T ∆m (QL Leak rate, Seff the effective pumping
QL = = ⋅ (5.1) speed at the pressure vessel)
of liquids) ∆t M ∆t

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Leak Detection Fundamentals of Vacuum Technology

Where Seff is sufficiently great it is possi-


ble – regardless of the value for the leak ∆p = 1013 mbar, Hole diameter d = 1 cm
rate QL – always to achieve a pre-determi- m
Gas speed = Speed of sound = 330 s
ned ultimate pressure of pend. In practice,
however, an infinite increase of Seff will run
12 · π · cm2 = 25.95 · 10+3 cm= 25.95 `
3

up against economic and engineering limi- Volume/second: 330 m


s · s s
4
tations (such as the space required by the
system). Quantity/second: 1013 mbar · 25.95 ` s = 2.63 · 10 P 10
+4 +4 mbar · `
s
Whenever it is not possible to achieve the mbar · `
desired ultimate pressure in an apparatus Diameter cm Leak rate s
there are usually two causes which can be 10–2 m= 1.0 cm 10+4
cited: The presence of leaks and/or gas 10–3 m= 1.0 mm 10+2
being liberated from the container walls 10–4 m= 0.1 mm 100 (= 1)
and sealants. 10–5 m= 0.01 mm 10–2
10–6 m= 1.0 µm 10–4
Partial pressure analysis using a mass 10–7 m= 0.1 µm 10–6
spectrometer or the pressure rise method 10–8 m= 0.01 µm 10–8
may be used to differentiate between these 10–9 m= 1.0 nm 10–10
two causes. Since the pressure rise 10–10 m= 1.0 Angstrom 10–12 (Detection limit, He leak detector)
method will only prove the presence of a
leak without indicating its location in the Fig. 5.1 Correlation between leak rate and hole size
apparatus, it is advisable to use a helium
leak detector with which leaks can, in
general, also be located much more quick- table shows that when the hole diameter is led to the development of calibrated refe-
ly. reduced to 1 µm (= 0.001 mm) the leak rate rence leaks with very small leak rates (see
will come to 10-4 mbar·l·s-1, a value which Section 5.5.2.3). This is a measurable “lack
In order to achieve an overview of the cor- in vacuum technology already represents a of tightness” but not a “leak” in the sense
relation between the geometric size of the major leak (see the rule of thumb above). A of being a defect in the material or joint.
hole and the associated leak rate it is pos- leak rate of 10-12 mbar·l·s-1 corresponds to Estimates or measurements of the sizes of
sible to operate on the basis of the follo- hole diameter of 1 Å; this is the lower atoms, molecules, viruses, bacteria, etc.
wing, rough estimate: A circular hole 1 cm detection limit for modern helium leak have often given rise to everyday terms
in diameter in the wall of a vacuum vessel detectors. Since the grid constants for such as “watertight” or “bacteria-tight”;
is closed with a gate valve. Atmospheric many solids amount to several Å and the see Table 5.1.
pressure prevails outside, a vacuum insi- diameter of smaller molecules and atoms
de. When the valve is suddenly opened all Compiled in Figure 5.2 are the nature and
(H2, He) are about 1 Å, inherent permeati-
the air molecules in a cylinder 1 cm in dia- detection limits of frequently used leak
on by solids can be registered metrologi-
meter and 330 m high would within a detection methods.
cally using helium leak detectors. This has
1-second period of time “fall into” the hole
at the speed of sound (330 m/s). The Concept / criterion Comment QL [mbar · l/s] Relevant particle size
quantity flowing into the vessel each
Water-tight *) Droplets QL < 10–2
second will be 1013 mbar times the cylin-
der volume (see Fig. 5.1). The result is that Vapor-tight “Sweating” QL < 10–3
for a hole 1 cm in diameter QL (air) will be Bacteria-tight *)
2.6 · 104 mbar·l·s-1. If all other conditions
(cocci) QL < 10–4 Avg. ≈ 1 µm
are kept identical and helium is allowed to
flow into the hole at its speed of sound of (rod-shaped) Avg. ≈ 0.5-1 µm, 2–10 µm long
970 m/s, then in analogous fashion the QL Oil-tight QL < 10–5
(helium) will come to 7.7 · 10+4 mbar·l·s-1,
Virus-tight *)
or a pV leaking gas current which is larger
by a factor of 970 / 330 = 2.94. This grea- (vaccines such as pox) QL < 10–6 Ø≈ 3 · 10–7 m
ter “sensitivity” for helium is used in leak (smallest viruses,
detection practice and has resulted in the bacteriophages) QL < 10–8 Ø 3 · 10–8 m
development and mass production of hig-
(viroids, RNA) QL < 10–10 Ø ª≈ 1 · 10–9 m (thread-like)
hly sensitive helium-based leak detectors
(see Section 5.5.2). Gas-tight QL < 10–7
“Absolutely tight” Technical QL < 10–10
Shown in Figure 5.1 is the correlation bet-
ween the leak rate and hole size for air, with *) As opposed to vapor, it is necessary to differentiate between hydrophilic and hydrophobic solids. This
also applies to bacteria and viruses since they are transported primarily in solutions.
D00
the approximation value of QL (air) of
10+4 mbar·l·s-1 for the “1 cm hole”. The Table 5.1 Estimating borderline leak rates

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Fundamentals of Vacuum Technology Leak Detection

Leak <----> Hole Substance quantity trhough hole per unit of time Helium standard leak rate:
Helium leak detector ULTRATEST UL 200 dry/UL 500 p1 = 1 bar, p2 < 1 mbar (∆p = 1 bar)
Q ... Leak rate, ∆ (p · V)

Vacuum method
In short: Leak Definition: Q = Test gas = Helium
∆t
Contura Z


Helium leak detector ULTRATEST UL 200/UL 500 dry/Modul 200/LDS 1000 Familiar leaks: Quantity escaping: Standard He leak rate:

mbar · ø mbar · ø
Pressure rise Dripping water faucet
mg
34 s Water 1 = 6.45 s Air 2 0.17 s He Std
4 mm diam., 1 Hz, ∆p = 4 bar

103................100 10-1 10-2 10-3 10-4 10-5 10-6 10-7 10-8 10-9 10-10 10-11 10-12 mbar · l · s-1 mbar · ø mbar · ø
Hair on a gasket 10 –2 s Air 0.9 · 10 –2 s He Std

Ecotec II / Protec Bicycle tube in water

Overpressure method
(bubble test) 3
mbar · ø mbar · ø
2 mm diam., 1 Hz, ∆p = 0.1 bar 4.19 · 10
–3 Ncm
s 1 = 4.24 · 10 –3
s Air 2 1.88 · 10 –2 s He Std
ULTRATEST with helium sniffer

Car tire loses air mbar · ø


Halogen sniffer HLD4000A mbar · ø 4.3 · 10 –5 s He Std
25 l, 6 Mo: 1.8 --> 1.6 bar 3.18 · 10 –4 s Air

Bubble test Small refrigerant cylinder


mbar · ø mbar · ø
empties in 1 year
g
1
430 a Frigen = 2.8 · 10 –3 s F12 2 4.33 · 10 –5 s He Std
Pressure drop test 430 g refrigerant R12, 25°C

Fig. 5.2 Leak rate ranges for various leak detection processes and devices Fig. 5.3 Examples for conversion into helium standard leak rates

5.2.1 The standard helium range the manufacturer (who is liable red to as the “inside-out leak”), where
leak rate under the guarantee terms) must assume the fluid passes from inside the test
values on the safe side. The equations are specimen outward (pressure inside the
Required for unequivocal definition of a listed in Table 5.2. specimen being greater than ambient
leak are, first, specifications for the Here indices “I” and “II” refer to the one or pressure).
pressures prevailing on either side of the the other pressure ratio and indices “1” The specimens should wherever possible
partition and, secondly, the nature of the and “2” reference the inside and outside of be examined in a configuration corre-
medium passing through that partition the leak point, respectively. sponding to their later application – com-
(viscosity) or its molar mass. The designa-
ponents for vacuum applications using the
tion “helium standard leak” (He Std) has
vacuum method and using the positive
become customary to designate a situati-
pressure method for parts which will be
on frequently found in practice, where
pressurized on the inside.
testing is carried out using helium at 1 bar
differential between (external) atmosphe- 5.3 Terms and When measuring leak rates we differentia-
ric pressure and the vacuum inside a definitions te between registering
system (internal, p < 1 mbar), the designa-
a. individual leaks (local measurement) –
tion “helium standard leak rate” has beco- When searching for leaks one will general-
sketches b and d in Figure 5.4, and regi-
me customary. In order to indicate the ly have to distinguish between two tasks:
stering
rejection rate for a test using helium under
1. Locating leaks and
standard helium conditions it is necessary b. the total of all leaks in the test specimen
2. Measuring the leak rate.
first to convert the real conditions of use to (integral measurement) – sketches a
helium standard conditions (see Section In addition, we distinguish, based on the and c in Figure 5.4.
5.2.2). Some examples of such conversi- direction of flow for the fluid, between the
The leak rate which is no longer tolerable
ons are shown in Figure 5.3.
a. vacuum method (sometimes known as in accordance with the acceptance specifi-
an “outside-in leak”), where the direc- cations is known as the rejection rate. Its
tion of flow is into the test specimen calculation is based on the condition that
(pressure inside the specimen being the test specimen may not fail during its
5.2.2 Conversion equations less than ambient pressure), and the planned utilization period due to faults
When calculating pressure relationships caused by leaks, and this to a certain
b. positive pressure method (often refer-
and types of gas (viscosity) it is necessary
to keep in mind that different equations are
applicable to laminar and molecular flow; Range Laminar Molecular
the boundary between these areas is very
QI ⋅ (p12 − p22)II = Q II ⋅ (p12 − p22)I QI ⋅ (p1 − p2)II = QII ⋅ (p1 − p2)I
difficult to ascertain. As a guideline one Pressure
may assume that laminar flow is present at
Qgas A á ηgas A = Qgas B á ηgas B Qgas A ⋅ Mgas A = Qgas B ⋅ Mgas B
leak rates where QL > 10-5 mbar · l/s and Gas
molecular flow at leak rates where
Table 5.2 Conversion formulae for changes of pressure and gas type
QL < 10-7 mbar · l/s. In the intermediate

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Leak Detection Fundamentals of Vacuum Technology

5.4 Leak detection


methods without a
Helium
leak detector unit
The most sensible differentiation between
the test methods used is differentiation as
to whether or not special leak detection
equipment is used.
In the simplest case a leak can be determi-
ned qualitatively and, when using certain
test techniques, quantitatively as well (this
a: Integral leak detection; vacuum inside c: Integral leak detection (test gas enrichment being the leak rate) without the assistance
specimen inside the enclosure); pressurized test gas inside of a special leak detector. Thus the quanti-
specimen
ty of water dripping from a leaking water
faucet can be determined, through a cer-
tain period of time, using a graduated
cylinder but one would hardly refer to this
as a leak detector unit. In those cases
Helium where the leak rate can be determined
during the course of the search for the leak
without using a leak detector (see, for
example, Sect. 5.4.1), this will often be
converted to the helium standard leak rate
(Sect. 5.2.1). This standard leak rate value
is frequently needed when issuing accept-
Helium
ance certificates but can also be of service
when comparing leak rate values deter-
b: Local leak detection; vacuum inside specimen d: Local leak detection; pressurized test gas mined by helium leak detector devices.
inside the specimen
In spite of careful inspection of the indivi-
Fig. 5.4 Leak test techniques and terminology dual engineering components, leaks may
also be present in an apparatus following
in parallel to the system’s pumps, then one its assembly – be it due to poorly seated
degree of certainty. Often it is not the leak
refers to partial-flow mode. One also seals or damaged sealing surfaces. The
rate for the test specimen under normal
refers to partial stream mode when a sepa- processes used to examine an apparatus
operating conditions which is determined,
rate auxiliary pump is used parallel to the will depend on the size of the leaks and on
but rather the throughput rate of a test gas
leak detector. the degree of tightness being targeted and
– primarily helium – under test conditions.
also on whether the apparatus is made of
The values thus found will have to be con-
When using the positive pressure method metal or glass or other materials. Some
verted to correspond to the actual applica-
it is sometimes either impractical or in fact leak detection techniques are sketched out
tion situation in regard to the pressures
impossible to measure the leakage rate below. They will be selected for use in
inside and outside the test specimen and
directly while it could certainly be sensed accordance with the particular application
the type of gas (or liquid) being handled.
in an envelope which encloses the test situations; economic factors may play an
Where a vacuum is present inside the test specimen. The measurement can be made important part here.
specimen (p < 1 mbar), atmospheric pres- by connecting that envelope to the leak
sure outside, and helium is used at the test detector or by accumulation (increasing
gas, one refers to standard helium condi- the concentration) of the test gas inside
tions. Standard helium conditions are the envelope. The “bombing test” is a
always present during helium leak detec- special version of the accumulation test 5.4.1 Pressure rise test
tion for a high vacuum system when the (see Section 5.7.4). In the so-called sniffer
system is connected to a leak detector and technique, another variation of the of the This leak testing method capitalizes on the
is sprayed with helium (spray technique). positive pressure technique, the (test) gas fact that a leak will allow a quantity of gas
If the specimen is evacuated solely by the issuing from leaks is collected (extracted) – remaining uniform through a period of
leak detector, then one would say that the by a special apparatus and fed to the leak time – to enter a sufficiently evacuated
leak detector is operating in the direct-
flow mode. If the specimen is itself a com-
detector. This procedure can be carried out
using either helium or refrigerants or SF6
device (impeded gas flow, see Fig. 1.1). In
contrast, the quantity of gas liberated from D00
plete vacuum system with its own vacuum as the test gas. container walls and from the materials
pump and if the leak detector is operated used for sealing (if these are not suffi-

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Fundamentals of Vacuum Technology Leak Detection

ally in Figure 5.5. Once it has become clear tus) the test gas which has passed through
that the rise in pressure is due solely to a leaks and into the apparatus. Another opti-
real leak, then the leak rate can be deter- on is to use the positive-pressure leak test.
mined quantitatively from the pressure A test gas (helium) is used to fill the appa-
rise, plotted against time, in accordance ratus being inspected and to build up a
slight positive pressure; the test gas will
Pressure

with the following equation:


pass to the outside through the leaks and
∆p ⋅ V
QL = (5.3) will be detected outside the device. The
∆t
leaks are located with leak sprays (or soap
Example: Once the vacuum vessel with a suds, 5.4.5) or – when using He or H2 as
volume of 20 l has been isolated from the the test gas – with a leak detector and snif-
pump, the pressure in the apparatus rises fer unit (5.7.2).
Time
from 1·10-4 mbar to 1·10-3 mbar in 300 s.
1 Leak Thus, in accordance with equation 5.2, the
2 Gas evolved from the container walls leak rate will be
3 Leak + gas evolution
  5.4.2 Pressure drop test
1 ⋅10 – 3 − 1 ⋅ 10 – 4  ⋅ 20
Fig. 5.5 Pressure rise within a vessel after the pump is  
QL = The thinking here is analogous to that for
switched off 300
the pressure rise method (Section 5.4.1).
9 ⋅10 – 4 ⋅ 20 mbar ⋅ ` The method is, however, used only rarely
ciently free of outgassing) will decline = = 6 ⋅ 10 – 5
300 s to check for leaks in vacuum systems. If
through time since these will practically
this is nonetheless done, then gauge pres-
always be condensable vapors for which
The leak rate, expressed as mass flow sure should not exceed 1 bar since the
an equilibrium pressure is reached at
∆m / ∆t, is derived from equation 5.1 at flange connectors used in vacuum techno-
some time (see Fig. 5.5). The valve at the
QL = 6 · 10-5 mbar · l/s, T = 20 °C and the logy will as a rule not tolerate higher pres-
pump end of the evacuated vacuum vessel
molar mass for air (M = 29 g/mole) at sures. Positive pressure testing is, on the
will be closed in preparation for pressure
other hand, a technique commonly
rise measurements. Then the time is mea- ∆m mbar ⋅ ` g
QL = = 6 ⋅10–5⋅ ⋅ 29 ⋅ employed in tank engineering. When dea-
sured during which the pressure rises by a ∆t s mol
ling with large containers and the long test
certain amount (by one power of ten, for mol ⋅ K g
⋅ = 7 ⋅10 – 8 periods they require for the pressure drop
example). The valve is opened again and . mbar ⋅ `⋅ 293 ⋅102 K
8314 s there it may under certain circumstances
the pump is run again for some time, fol-
be necessary to consider the effects of
lowing which the process will be repeated.
If the container is evacuated with a temperature changes. As a consequence it
If the time noted for this same amount of
TURBOVAC 50 turbomolecular pump, for may happen, for example, that the system
pressure rise remains constant, then a leak
example (S = 50 l/s), which is attached to cools to below the saturation pressure for
is present, assuming that the waiting peri-
the vacuum vessel by way of a shut-off water vapor, causing water to condense;
od between the two pressure rise trials
valve, then one may expect an effective this will have to be taken into account
was long enough. The length of an appro-
pumping speed of about Seff = 30 l/s. Thus when assessing the pressure decline.
priate waiting period will depend on the
the ultimate pressure will be
nature and size of the device. If the pres-
sure rise is more moderate during the Q 6 ⋅ 10 – 5 mbar ⋅ ` ⋅ s – 1
pend = L =
second phase, then the rise may be assu- Seff 30 ` ⋅ s – 1
med to result from gases liberated from
the inner surfaces of the vessel. One may
5.4.3 Leak test using
= 2 ⋅10 – 6 mbar
also attempt to differentiate between leaks vacuum gauges which
and contamination by interpreting the Naturally it is possible to improve this ulti-
are sensitive to the type
curve depicting the rise in pressure. Plot- mate pressure, should it be insufficient, by of gas
ted on a graph with linear scales, the curve using a larger-capacity pump (e.g. the
for the rise in pressure must be a straight The fact that the pressure reading at vacu-
TURBOVAC 151) and at the same time to um gauges (see Section 3.3) is sensitive to
line where a leak is present, even at higher reduce the pump-down time required to
pressures. If the pressure rise is due to the type of gas involved can, to a certain
reach ultimate pressure. extent, be utilized for leak detection purpo-
gas being liberated from the walls (owing
ultimately to contamination), then the Today leak tests for vacuum systems are ses. Thus it is possible to brush or spray
pressure rise will gradually taper off and usually carried out with helium leak detec- suspected leaks with alcohol. The alcohol
will approach a final and stable value. In tors and the vacuum method (see Section vapors which flow into the device – the
most cases both phenomena will occur 5.7.1). The apparatus is evacuated and a thermal conductivity and ionizablity of
simultaneously so that separating the two test gas is sprayed around the outside. In which will vary greatly from the same pro-
causes is often difficult if not impossible. this case it must be possible to detect (on perties for air – will affect and change
These relationships are shown schematic- the basis of samplings inside the appara- pressure indication to a greater or lesser

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Leak Detection Fundamentals of Vacuum Technology

extent. The availability of more precise, Here, again, the detection of smaller leaks krypton 85, a gaseous, radioactive isotope,
easy-to-use helium leak detectors has, is time-consuming and will depend greatly can first be forced into the device by app-
however, rendered this method almost on the attentiveness of the inspector. The lying pressure from the outside. Once an
completely obsolete. hydrogen gas cooling systems used in exactly measured holding period has elap-
power plant generators represent a special sed the pressure will be relieved, the com-
case. These are indeed sometimes tested ponent flushed and the activity of the “gas
in the fashion described above but they charge” will be measured. In the same way
can be examined much better and at much it is also possible to use helium as the test
5.4.4 Bubble immersion test higher sensitivity by “sniffing” the hydro- gas (see Section 5.7.4, bombing test).
gen escaping at leaks using a helium leak
The pressurized test specimen is sub- detector which has been adjusted to res-
merged in a liquid bath. Rising gas bub- pond to H2 (see Section 5.7.2).
bles indicate the leak. Leak detection will
depend greatly on the attentiveness of the
5.4.8 High-frequency vacuum
person conducting the test and involves
the temptation to increase the “sensitivity” test
by using ever higher temperatures, wher- The so-called high-frequency vacuum
ein the applicable safety regulations are 5.4.6 Vacuum box check
tester can be used not only to check the
sometimes disregarded. This method is bubble pressure in glass equipment but also to
very time-consuming for smaller leaks, as locate porous areas in plastic or paint coa-
As a variation on the spray technique men-
Table 5.3 shows. It references leak testing tings on metals. This comprises a hand-
tioned above, in which the escaping gas
on a refrigeration system using type R12 held unit with a brush-like high-frequency
causes the bubbles, it is possible to place
refrigerant. Here the leak rate is specified electrode and a power pack. The shape
a so-called “vacuum box” with a seal
in grams of refrigerant loss per year (g/a). and color of the electrical gas discharge
(something like a diver’s goggles) on the
Water is used as a test liquid (which may can serve as a rough indicator for the pres-
surface being examined once it has been
be heated or to which a surfactant may be sure prevailing inside glass equipment. In
sprayed with a soap solution. This box is
added) or petroleum-based oils. The surfa- the case of the vacuum tester – which
then evacuated with a vacuum pump. Air
ce tension should not exceed 75 dyn/cm comprises primarily a tesla transformer
entering from the outside through leaks
(1 dyn = 10-5 N). (which delivers a high-voltage, high-fre-
will cause bubbles inside the box, which
can be observed through a glass window quency AC current) – the corona electrode
in the box. In this way it is also possible, approaching the apparatus will trigger an
for example, to examine flat sheet metal electrode-free discharge inside the appara-
plates for leaks. Vacuum boxes are availa- tus. The intensity and color of this dischar-
5.4.5 Foam-spray test ge will depend on the pressure and the
ble for a variety of applications, made to
In many cases pressurized containers or suit a wide range of surface contours. type of gas. The luminous discharge phe-
gas lines (including the gas supply lines nomenon allows us to draw conclusions
for vacuum systems) can be checked quite regarding the approximate value for the
conveniently for leaks by brushing or pressure prevailing inside the apparatus.
spraying a surfactant solution on them. The discharge luminosity will disappear at
Corresponding leak detection sprays are 5.4.7 Krypton 85 test high and low pressures.
also available commercially. Escaping gas When searching for leaks in glass equip-
forms “soap bubbles” at the leak points. When dealing with small, hermetically sea-
ment the suspect sections will be scanned
led parts where the enclosure is leaky,
or traced with the high-frequency vacuum
tester electrode. Where there is a leak an
Freon F12 loss Time taken to form Equivalent Detection time using arc will strike through to the pore in the
per year a gas bubble leak rate helium leak detector glass wall, tracing a brightly lit discharge
(g/a) (s) (cm3[STP]/s) (s) trail. Small pores can be enlarged by these
280 13.3 1.8 · 10–3 a few seconds sparks! The corona discharge of the vacu-
um tester can also penetrate thin areas in
84 40 5.4 · 10–4 a few seconds the glass particularly at weld points and
28 145 1.8 · 10–4 a few seconds transitional areas between intermediate
components. Equipment which was ori-
14 290 9.0· 10–5 a few seconds ginally leak-free can become leaky in this
2.8 24 min 1.8 · 10–5 a few seconds fashion! In contrast to the actual leak
detector units, the high-frequency vacuum
0.28 * 6h 1.8 · 10–6
*) This leak rate represents the detection limit for good halogen leak detectors (≈ 0,1 g/a).
a few seconds
tester is highly limited in its functioning. D00
Table 5.3 Comparison of bubble test method (immersion technique) wit helium leak detector

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Fundamentals of Vacuum Technology Leak Detection

5.4.9 Test with chemical lity of the surface of the solid and the capil- The function of most leak detectors is
reactions and dye lary action; see also Table 5.1. Some wide- based on the fact that testing is conducted
ly used leak detection methods are shown – with a special test gas, i.e. with a medium
penetration together with the test gas, application range other than the one used in normal operati-
Occasionally leaks can also be located or and their particular features – in Table 5.4. on. The leak test may, for example, be car-
detected by means of chemical reactions ried out using helium, which is detected
which result in a discoloration or by pene- using a mass spectrometer, even though
tration of a dye solution into fine openings. the component being tested might, for
The discoloration of a flame due to halo- example, be a cardiac pacemaker whose
gen gas escaping through leaks was used 5.5 Leak detectors and interior components are to be protected
against the ingress of bodily fluids during
earlier to locate leaks in solder joints for
refrigeration units. how they work normal operation. This example alone
makes it clear that the varying flow pro-
A less frequently employed example of a Most leak testing today is carried out using perties of the test and the working media
chemical effect would be that of escaping special leak detection devices. These can need to be taken into consideration.
ammonia when it makes contact with oza- detect far smaller leak rates than techni-
lid paper (blueprint paper) or with other ques which do not use special equipment.
materials suitably prepared and wrapped These methods are all based on using spe-
around the outside of the specimen. Leaks cific gases for testing purposes. The diffe-
are then detected based on the discolorati- rences in the physical properties of these
on of the paper.
5.5.1 Halogen leak detectors
test gases and the gases used in real-life
applications or those surrounding the test (HLD4000, D-Tek)
An example of a dye penetration test is the
inspection of the tightness of rubber plugs configuration will be measured by the leak Gaseous chemical compounds whose
or plungers in glass tubes, used for exam- detectors. This could, for example, be the molecules contain chlorine and/or fluorine
ple in testing materials suitability for dis- differing thermal conductivity of the test – such as refrigerants R12, R22 and
posable syringes or pharmaceutical packa- gas and surrounding air. The most widely R134a – will influence the emissions of
ges. When evaluating tiny leaks for liquids used method today, however, is the detec- alkali ions from a surface impregnated
it will be necessary to consider the wetabi- tion of helium used as the test gas. with a mixture of KOH and Iron(III)hydro-
xide and maintained at 800 °C to 900 °C by
an external Pt heater. The released ions
Method Test gas Smallest detectable Pressure range Quantitative flow to a cathode where the ion current is
leak rate measurement
measured and then amplified (halogen
mbar `/s g/a R 134 a
–4 –1
diode principle). This effect is so great that
Foaming Air and others 10 7 · 10 Positive pressure No partial pressures for halogens can be mea-
liquids
sured down to 10-7 mbar.
–2
Ultrasonic Air and others 10 70 Positive pressure No
microphone Whereas such devices were used in the
past for leak testing in accordance with the
–3 –5 –1
Thermal conducti- Gases other 10 – 10 10 – 7 Positive pressure No vacuum method, today – because of the
vity leak detector than air and vacuum
problems associated with the CFCs – more
sniffer units are being built. The attainable
–6 –3
Halogen Substances 10
–5
7 · 10
–1
Positive pressure With detection limit is about 1 · 10-6 mbar · l/s
leak detection containing (10 ) (10 ) (vacuum) limitations
halogens
for all the devisces. Equipment operating in
accordance with the halogen diode princi-
–5 –3
Universal Refrigerants, 10 7 · 10 Positive pressure Yes ple can also detect SF6. Consequently these
sniffer helium and sniffer units are used to determine whether
leak detector other gases
refrigerants are escaping from a refrigera-
–12 –9
Helium Helium 10
–7
7 · 10
–4
Vacuum, Yes tion unit or from an SF6 type switch box (fil-
leak detection 10 7 · 10 positive pressure led with arc suppression gas).
–3
Bubble test Air and other 10 7 Positive pressure No
gases
–2
Water pressure Water 10 70 Positive pressure No
test
5.5.2 Leak detectors with mass
–4 –1
Pressure Air and other 10 7 · 10 Positive pressure Yes spectrometers (MSLD)
drop test gases
–4 –1
The detection of a test gas using mass
Pressure Air 10 7 · 10 Vacuum Yes
rise test
spectrometers is far and away the most
sensitive leak detection method and the one
Table 5.4 Comparison of leak detection methods most widely used in industry. The MS leak

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detectors developed for this purpose make 5.5.2.1 The operating principle for a In this case the gas quantity per unit of
possible quantitative measurement of leak MSLD time is the leak rate being sought; the total
rates in a range extending across many pressure may not be used, but only the
The basic function of a leak detector and
powers of ten (see Section 5.2) whereby share for helium or the partial pressure for
the difference between a leak detector and
the lower limit ≈ 10-12 mbar · l/s, thus helium. This signal is delivered by the
mass spectrometer can be explained using
making it possible to demonstrate the inhe- mass spectrometer when it is set for ato-
Figure 5.6. This sketch shows the most
rent gas permeability of solids where heli- mic number 4 (helium). The value for Seff
commonly found configuration for leak
um is used as the test gas. It is actually is a constant for every series of leak detec-
detection using the helium spray method
possible in principle to detect all gases tors, making it possible to use a micropro-
(see Section 5.7.1) at a vacuum compo-
using mass spectrometry. Of all the availa- cessor to multiply the signal arriving from
nent. When the sprayed helium is drawn
ble options, the use of helium as a tracer the mass spectrometer by a numerical
into the component through a leak it is
gas has proved to be especially practical. constant and to have the leak rate dis-
pumped thorough the interior of the leak
The detection of helium using the mass played direct.
detector to the exhaust, where it again lea-
spectrometer is absolutely (!) unequivocal.
ves the detector. Assuming that the detec-
Helium is chemically inert, non-explosive,
tor itself is free of leaks, the amount of gas 5.5.2.2 Detection limit, background,
non-toxic, is present in normal air in a con-
flowing through each pipe section (at any gas storage in oil (gas
centration of only 5 ppm and is quite eco-
desired point) per unit of time will remain ballast), floating zero-point
nomical. Two types of mass spectrometer
constant regardless of the cross section suppression
are used in commercially available MSLD’s:
and the routing of the piping. The follo-
a) The quadrupole mass spectrometer, alt- wing applies for the entry into the pumping The smallest detectable leak rate is dicta-
hough this is used less frequently due port at the vacuum pump: ted by the natural background level for the
to the more elaborate and complex gas to be detected. Even with the test
design (above all due to the electrical Q=p·S (5.4) connector at the leak detector closed,
supply for the sensor), or At all other points every gas will pass – counter to the pum-
ping direction – through the exhaust and
b) the 180° magnetic sector field mass Q = p · Seff (5.4a) through the pumps (but will be reduced
spectrometer, primarily due to the rela-
accordingly by their compression) through
tively simple design. applies, taking the line losses into account.
to the spectrometer and will be detected
Regardless of the functional principle The equation applies to all gases which are there if the electronic means are adequate
employed, every mass spectrometer com- pumped through the piping and thus also to do so. The signal generated represents
prises three physically important sub- for helium. the detection limit. The high vacuum
systems: the ion source, separation system used to evacuate the mass spec-
QHe = pHe · Seff, He (5.4b)
system and ion trap. The ions must be able
to travel along the path from the ion sour-
ce and through the separation system to Test gas
the ion trap, to the greatest possible extent e.g. He
without colliding with gas molecules. This
path amounts to about 15 cm for all types
of spectrometers and thus requires a
medium free path length of at least 60 cm, Test specimen
corresponding to pressure of about
1 · 10-4 mbar; in other words, a mass Test connection
spectrometer will operate only in a vacu-
um. Due to the minimum vacuum level of
1 · 10-4 mbar, a high vacuum will be requi-
red. Turbomolecular pumps and suitable
roughing pumps are used in modern leak
detectors. Associated with the individual
component groups are the required electri-
Leak detector
cal- and electronic supply systems and
software which, via a microprocessor,
allow for the greatest possible degree of
automation in the operating sequence, QHe = pHe · SeffHe
including all adjustment and calibration
routines and measured value display.
Exhaust
D00
Fig. 5.6 Basic operating principle for a leak detector

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Fundamentals of Vacuum Technology Leak Detection

Test connection
tinued until all the oil from the pump’s oil
pan has been recirculated several times.
This period of time will usually be 20 to 30
minutes.
Mass spectrometer In order to spare the user the trouble of
always having to keep an eye on the back-
ground level, what has been dubbed floa-
Turbomolecular pump ting zero-point suppression has been inte-
grated into the automatic operating con-
Venting cepts of all INFICON leak detectors (Sec-
valve tion 5.5.2.5). Here the background level
measured after the inlet valve has been
Gas ballast closed is placed in storage; when the valve
valve is then opened again this value will auto-
Roughing pump
matically be deducted from subsequent
measurements. Only at a relatively high
Exhaust threshold level will the display panel show
a warning indicating that the background
noise level is too high. Figure 5.8 is provi-
Fig. 5.7 Correct set-up for a MSLD ded to illustrate the process followed in
zero point suppression. Chart on the left.
The signal is clearly larger than the back-
trometer will normally comprise a turbo- detector, to increase the helium level in the
ground. Center chart: the background has
molecular pump and an oil-sealed rotary oil and the elastomer seals there and thus
risen considerably; the signal can hardly
vane pump. (Diffusion pumps were used to induce a background signal in the mass
be discerned. Chart on the right: the back-
earlier instead of the turbomolecular spectrometer which is well above the nor-
ground is suppressed electrically; the sig-
pumps.) Like every liquid, the sealing oil in mal detection limit. When the device is
nal can again be clearly identified.
the rotary vane pump has the capability of properly installed (see Fig. 5.7) the gas
dissolving gases until equilibrium is rea- ballast valve and the airing valve will be Independent of this floating zero-point
ched between the gas dissolved in the oil connected to fresh air and the discharge suppression, all the leak detectors offer
and the gas outside the oil. When the line (oil filter!) should at least be routed to the capability for manual zero point shif-
pump is warm (operating temperature) outside the room where the leak test takes ting. Here the display for the leak detector
this equilibrium state represents the detec- place. at the particular moment will be “reset to
tion limit for the leak detector. The helium zero” so that only rises in the leak rate
An increased test gas (helium) background
stored in the oil thus influences the detec- from that point on will be shown. This ser-
level can be lowered by opening the gas
tion limit for the leak detector. It is possi- ves only to facilitate the evaluation of a dis-
ballast valve and introducing gas which is
ble for test gas to enter not only through play but can, of course, not influence its
free of the test gas (helium-free gas, fresh
the test connection and into the leak detec- accuracy.
air). The dissolved helium will be flushed
tor; improper installation or inept handling
out, so to speak. Since the effect always Modern leak detectors are being more fre-
of the test gas can allow test gas to enter
affects only the part of the oil present in quently equipped with oil-free vacuum
through the exhaust and the airing or gas
the pump body at the particular moment, systems, the so-called “dry leak detectors”
ballast valve and into the interior of the
the flushing procedure will have to be con- (UL 200 dry, UL 500 dry). Here the pro-
blem of gas being dissolved in oil does not
occur but similar purging techniques will
nonetheless be employed.
10–6
caution
10–7
5.5.2.3 Calibrating leak detectors;
10–8 test leaks
fine
10–9 Calibrating a leak detector is to be under-
prec
10–10 stood as matching the display at a leak
detector unit, to which a test leak is atta-
10–11
ched, with the value shown on the “label”
or calibration certificate. The prerequisite
Equipment background level: < 2 · 10–10 1 · 10–8 1 · 10–10 (suppressed)
Leak: 2 · 10–8 2 · 10–8 2 · 10–8
for this is correct adjustment of the ion
Display: 2 · 10–8 3 · 10–8 2 · 10–8 paths in the spectrometer, also known as
tuning. Often the distinction is not made
Fig. 5.8 Example of zero-point suppression quite so carefully and both procedures

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Leak Detection Fundamentals of Vacuum Technology

together are referred to as calibration. Test leaks (also known as standard leaks 5.5.2.4 Leak detectors with
or reference leaks) normally comprise a quadrupole mass
In the calibration process proper the
gas supply, a choke with a defined con- spectrometer (Ecotec II)
straight-line curve representing the nume-
ductance value, and a valve. The configu-
rically correct, linear correlation between INFICON builds leak detectors with qua-
ration will be in accordance with the test
the gas flow per unit of time and the leak drupole mass spectrometers to register
leak rate required. Figure 5.9 shows
rate is defined by two points: the zero point masses greater than helium. Apart from
various test leaks. Permeation leaks are
(no display where no emissions are detec- special cases, these will be refrigerants.
usually used for leak rates of
ted) and the value shown with the test leak These devices thus serve to examine the
10-10 < QL < 10-7, capillaries, between
(correct display for a known leak). tightness of refrigeration units, particular-
10-8 and 10-4 and, for very large leak rates
ly those for refrigerators and air conditio-
In vacuum operations (spray technique, in a range from 10 to 1000 mbar · l/s, pipe
ning equipment.
see Section 5.7.1) one must differentiate sections or orifice plates with exactly
between two types of calibration: with an defined conductance values (dimensions). Figure 4.2 shows a functional diagram for
internal or external test leak. When using a Test leaks used with a refrigerant charge a quadrupole mass spectrometer. Of the
test leak built into the leak detector the unit represent a special situation since the ref- four rods in the separation system, the two
can itself be calibrated but it can only cali- rigerants are liquid at room temperature. pairs of opposing rods will have identical
brate itself. When using an external test Such test leaks have a supply space for potential and excite the ions passing
leak not just the device but also a comple- liquid from which, through a shut-off through along the center line so that they
te configuration, such as a partial flow valve, the space filled only with the refrige- oscillate transversely. Only when the
arrangement, can be included. Internal test rant vapor (saturation vapor pressure) can amplitude of these oscillations remains
leaks are permanently installed and cannot be reached, ahead of the capillary leak. smaller than the distance between the rods
be misplaced. At present all the leak detec- One technological problem which is diffi- can the appropriate ion pass through the
tors being distributed by INFICON are fit- cult to solve is posed by the fact that all system of rods and ultimately reach the
ted with an automatic calibration routine. refrigerants are also very good solvents for ion trap, where it will discharge and thus
oil and grease and thus are often seriously be counted. The flow of electrons thus
Sniffer units or configurations will as a rule
contaminated so that it is difficult to fill the created in the line forms the measurement
have to be calibrated with special, external
test leaks with pure refrigerant. Decisive signal proper. The other ions come into
test leaks in which there is a guarantee that
here is not only the chemical composition contact with one of the rods and will be
on the one hand all the test gas issuing
but above all dissolved particles which can neutralized there.
from the test leak reaches the tip of the
probe and on the other hand that the gas repeatedly clog the fine capillaries. Figure 5.10 shows the vacuum schematic
flow in the sniffer unit is not hindered by for an Ecotec II. The mass spectrometer
calibration. When making measurements
using the sniffer technique (see Section
1 Diaphragm pump
5.7.2) it is also necessary to take into 5 2 Piezo-resistive
account the distance from the probe tip to pressure sensor
the surface of the specimen and the scan- external flow internal 3 Turbomolecular
ning speed; these must be included as a particle limiter 1 particle pump
filter filter 4 Quadrupole mass
part of the calibration. In the special case
spectrometer
where helium concentration is being mea- 5 Sniffer line
sured, calibration can be made using the 6 Gas flow limiter
6 7 Gas flow limiter
helium content in the air, which is a uni-
8 Gas flow meter
form 5 ppm world-wide. QMA 200 flow divider 1
flow
limiter 2
4
5 flow divider 2
flow
7 limiter 3
3
flow meter

pv

a b c d e 1 8
2

a Reference leak without gas supply, TL4, TL6


b Reference leak for sniffer and vacuum 1 2
applications, TL4-6
c (Internal) capillary test leak TL7
d Permeation (diffusion) reference leak, TL8
e Refrigerant calibrated leak
D00
Fig. 5.9 Examples for the construction of test leaks Fig. 5.10 Vacuum schematic for the Ecotec II

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Fundamentals of Vacuum Technology Leak Detection

(4) only operates under high vacuum con- is possible to switch directly from one gas 1. the mass spectrometer
ditions, i.e. the pressure here must always to another.
2. the high vacuum pump and
remain below 10-4 mbar. This vacuum is
generated by the turbomolecular pump (3) 3. the auxiliary roughing pump system in
with the support of the diaphragm pump 5.5.2.5 Helium leak detectors with stationary units.
(1). The pressure PV between the two 180° sector mass
spectrometer (UL 200, UL 500) The mass spectrometer (see Fig. 5.11)
pumps is measured with a piezo resistive
comprises the ion source (1–4) and the
measuring system (2) and this pressure These units are the most sensitive and also deflection system (5–9). The ion beam is
lies in the range between 1 to 4 mbar while provide the greatest degree of certainty. extracted through the orifice plate (5) and
in the measurement mode. This pressure Here “certain” is intended to mean that enters the magnetic field (8) at a certain
must not exceed a value of 10 mbar as there is no other method with which one energy level. Inside the magnetic field the
otherwise the turbomolecular pump will can, with greater reliability and better sta- ions move along circular paths whereby
not be capable of maintaining the vacuum bility, locate leaks and measure them the radius for a low mass is smaller than
in the mass spectrometer. The unit can quantitatively. For this reason helium leak that for higher masses. With the correct
easily be switched over at the control unit detectors, even though the purchase price setting of the acceleration voltage during
from helium to any of various refrigerants, is relatively high, are often far more eco- tuning one can achieve a situation in which
some of which may be selected as desired. nomical in the long run since much less the ions describe a circular arc with a defi-
Naturally the unit must be calibrated sepa- time is required for the leak detection pro- ned curvature radius. Where mass 4 (heli-
rately for each of these masses. Once set, cedure itself. um) is involved, they pass thorough the
however, the values remain available in
A helium leak detector comprises basically aperture (9) to the ion trap (13). In some
storage so that after calibration has been
two sub-systems in portable units and devices the discharge current for the ions
effected for all the gases (and a separate
three in stationary units. These are: impinging upon the total pressure electro-
reference leak is required for each gas!) it
des will be measured and evaluated as a
total pressure signal. Ions with masses
which are too small or too great should not
be allowed to reach the ion trap (13) at all,
but some of these ions will do so in spite
of this, either because they are deflected
by collisions with neutral gas particles or
because their initial energy deviates too far
14 1 from the required energy level. These ions
are then sorted out by the suppressor (11)
so that only ions exhibiting a mass of 4
13 (helium) can reach the ion detector (13).
2 The electron energy at the ion source is 80
12 3 eV. It is kept this low so that components
with a specific mass of 4 and higher –
4 such as multi-ionized carbon or quadruply
11 5 ionized oxygen – cannot be created. The
ion sources for the mass spectrometer are
simple, rugged and easy to replace. They
6 are heated continuously during operation
and are thus sensitive to contamination.
The two selectable yttrium oxide coated iri-
dium cathodes have a long service life.
10 These cathodes are largely insensitive to
7 air ingress, i.e. the quick-acting safety cut-
out will keep them from burning out even
if air enters. However, prolonged use of the
9 8 ion source may eventually lead to cathode
1 Ion source flange 5 Extractor 10 Magnetic field
embrittlement and can cause the cathode
2 Cathode 6 Ion traces for M > 4 11 Suppressor to splinter if exposed to vibrations or
(2 cathodes, Ir + Y2O3) 7 Total pressure electrode 12 Shielding of the ion trap shock.
3 Anode 8 Ion traces for M = 4 13 Ion trap
4 Shielding of the ion 9 Intermediate orifice 14 Flange for ion trap with Depending on the way in which the inlet is
source with discharge plate preamplifier connected to the mass spectrometer, one
orifice can differentiate between two types of
MSLD.
Fig. 5.11 Configuration of the 180° sector mass spectrometer

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5.5.2.6 Direct-flow and counter-flow for helium is QHe = pHe · Seff · K (5.5b)
leak detectors pmin,He = 1 · 10-12 mbar. The pumping
Seff = effective pumping speed at the
speed for helium would be SHe = 10 l/s.
Figure 5.12 shows the vacuum schematic rotary vane pump at the
Then the smallest detectable leak rate is
for the two leak detector types. In both branching point
Qmin = 1 · 10-12 mbar · 10 l/s
cases the mass spectrometer is evacuated K = Helium compression factor at
= 1 · 10-11 mbar · l/s. If the pumping speed
by the high vacuum pumping system com- the turbomolecular pump
is now reduced to 1/s, then one will achie-
prising a turbomolecular pump and a
ve the smallest detectable leak rate of The counter-flow leak detector is a particu-
rotary vane pump. The diagram on the left
1 · 10-12 mbar · l/s. One must keep in lar benefit for automatic vacuum units
shows a direct-flow leak detector. Gas
mind, however, that with the increase in since there is a clearly measurable pressu-
from the inlet port is admitted to the spec-
the sensitivity the time constant for achie- re at which the valve can be opened, name-
trometer via a cold trap. It is actually equi-
ving a stable test gas pressure in the test ly the roughing vacuum pressure at the
valent to a cryopump in which all the
specimen will be correspondingly larger turbomolecular pump. Since the turbo-
vapors and other contaminants condense.
(see Section 5.5.2.9). molecular pump has a very large compres-
(The cold trap in the past also provided
sion capacity for high masses, heavy mo-
effective protection against the oil vapors In Figure 5.12 the right hand diagram
lecules in comparison to the light test gas,
of the diffusion pumps used at that time). shows the schematic for the counter-flow
helium (M = 4), can in practice not reach
The auxiliary roughing pump system ser- leak detector. The mass spectrometer, the
the mass spectrometer. The turbomolecu-
ves to pre-evacuate the components to be high vacuum system and also the auxiliary
lar pump thus provides ideal protection for
tested or the connector line between the roughing pump system correspond exact-
the mass spectrometer and thus elimina-
leak detector and the system to be tested. ly to the configuration for the direct-flow
tes the need for an LN2 cold tap, which is
Once the relatively low inlet pressure arrangement. The feed of the gas to be
certainly the greatest advantage for the
(pumping time!) has been reached, the examined is however connected between
user. Historically, counter-flow leak detec-
valve between the auxiliary pumping the roughing pump and the turbomolecu-
tors were developed later. This was due in
system and the cold trap will be opened for lar pump. Helium which reaches this
part to inadequate pumping speed stabili-
the measurement. The Seff used in equati- branch point after the valve is opened will
ty, which for a long time was not sufficient
on 5.4b is the pumping speed of the tur- cause an increase in the helium pressure
with the rotary vane pumps used here. For
bomolecular pump at the ion source loca- in the turbomolecular pump and in the
both types of leak detector, stationary
tion: mass spectrometer. The pumping speed
units use a built-in auxiliary pump to assist
Seff inserted in equation 5.4b is the pum-
QHe = pHe · Seff,turbomolecular pump ion source in the evacuation of the test port. With por-
ping speed for the rotary vane pump at the
(5.5a) table leak detectors, it may be necessary to
branch point. The partial helium pressure
provide a separate, external pump, this
In the case of direct-flow leak detectors, an established there, reduced by the helium
being for weight reasons.
increase in the sensitivity can be achieved compression factor for the turbomolecular
by reducing the pumping speed, for exam- pump, is measured at the mass spectro-
ple by installing a throttle between the tur- meter. The speed of the turbomolecular 5.5.2.7 Partial flow operation
bomolecular pump and the cold trap. This pump in the counter-flow leak detectors is
regulated so that pump compression also Where the size of the vacuum vessel or the
is also employed to achieve maximum
remains constant. Equation 5.5b is derived leak makes it impossible to evacuate the
sensitivity. To take an example:
from equation 5.5a: test specimen to the necessary inlet pres-
The smallest detectable partial pressure sure, or where this would simply take too
long, then supplementary pumps will have
to be used. In this case the helium leak
Solution 1: Direct-flow leak detector Solution 2: Counter-flow leak detector detector is operated in accordance with the
so-called “partial flow” concept. This
means that usually the larger part of the
Test specimen Test specimen
gas extracted from the test object will be
Test gas stream Test gas stream
removed by an additional, suitably dimen-
sioned pump system, so that only a part of
p TOT < 10–4 mbar the gas stream reaches the helium leak
LN 2 pHe pHe
detector (see Fig. 5.13). The splitting of
MS MS the gas flow is effected in accordance with
p TOT < 10–4 mbar High vacuum pump the pumping speed prevailing at the bran-
High vacuum pump ching point. The following then applies:
Auxiliary pump Roughing pump Auxiliary pump Roughing pump
QVacuum vessel = γ · DisplayLeak detector (5.6)

D00
Cold trap:
2
S = 6.1 `/s · cm
Fl ≈ 1000 cm
2
where g is characterized as the partial flow
S = 6,100 `/s
ratio, i.e. that fraction of the overall leak
current which is displayed at the detector.
Fig. 5.12 Full-flow and counter-flow leak detector

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Fundamentals of Vacuum Technology Leak Detection

Where the partial flow ratio is unknown, g the partial flow ratio to be expected vis à valve. In order to avoid this valve being
can be determined with a reference leak vis a diffusion pump with pumping speed opened inadvertently, it should be sealed
attached at the vacuum vessel: of 12000 l/s, for example – which leak off with a blank flange during normal vacu-
rates can be detected at all. In systems um system operation.
Display at the leak detector
γ = ——————————— (5.7) with high vacuum- and Roots pumps, the
A second method for coupling to larger
QL for the reference leak surest option is to connect the leak detec-
systems, for example, those used for
tor between the rotary vane pump and the
removing the air from the turbines in po-
roots pump or between the roots pump
wer generating stations, is to couple at the
5.5.2.8 Connection to vacuum systems and the high vacuum pump. If the pressu-
discharge. A sniffer unit is inserted in the
re there is greater than the permissible
The partial flow concept is usually used in system where it discharges to atmosphe-
inlet pressure for the leak detector, then
making the connection of a helium leak re. One then sniffs the increase in the heli-
the leak detector will have to be connected
detector to vacuum systems with multi- um concentration in the exhaust. Without
by way of a metering (variable leak) valve.
stage vacuum pump sets. When conside- a tight coupling to the exhaust, however,
Naturally one will have to have a suitable
ring where to best make the connection, it the detection limit for this application will
connector flange available. It is also advis-
must be kept in mind that these are usual- be limited to 5 ppm, the natural helium
able to install a valve at this point from the
ly small, portable units which have only a content in the air. In power plants it is suf-
outset so that, when needed, the leak
low pumping speed at the connection flan- ficient to insert the tip of the probe at an
detector can quickly be coupled (with the
ge (often less than 1 l/s). This makes it all angle of about 45° from the top into the
system running) and leak detection can
the more important to estimate – based on discharge line (usually pointing upward) of
commence immediately after opening the
the (water ring) pump.

Partial flow principle (example) 5.5.2.9 Time constants

· ` (Leak rate) The time constant for a vacuum system is


QHe = 3 · 10 mbar
–5

V = 150 ` s set by
V
τ= (5.8)
Seff
Seff = SPFP + SLD → SLD = 8 ` Leak detector (LD)
s
τ = Time constant
m3 ` V = Volume of the container
SPFP = 60 s = 16.66 s Partial flow pump (PFP)
Seff = Effective pumping speed, at the
A) Signal amplitude:
Splitting of the gas flow (also of the test test object
gas!) in accordance with the effective pumping Figure 5.14 shows the course of the signal
speed at the partial flow branch point after spraying a leak in a test specimen
Overal pumping speed: Seff = SLD + SPFP = 8 + 16.66 = 24.66 `
s
attached to a leak detector, for three diffe-
rent configurations:
γ ... Partial flow ratio 1. Center: The specimen with volume of V
is joined directly with the leak detector
H

` LD (effective pumping speed of S).


Signal to Leak detector: 3 · 10–5 mbars · ` · 8 s
= 9.73 · 10–6 mbar · `
s
(8 + 16.66) `s
` 2. Left: In addition to 1, a partial flow
Signal to partial flow pump: 3 · 10–5 mbars · ` · 16,668s
= 2.02 · 10–5 mbar · `
s pump with the same effective pumping
(8 + 16.66) `s
speed, S’ = S, is attached to the test
Check: Overall signal QHe = QLD + QPFP = 3.00 · 10–5 mbars · ` specimen.
3. Right: As at 1, but S is throttled down to
Partial flow ratio = Fraction of the overall flow to the leak detector 0.5 · S.

or
Q
γ = LD =

γ=
QLD

SLD
=

= 1
1
QHe QLD + QPFP 1 + nnn

S
Q
Q
PFP

LD
H
QLD = γ · QHe
Display Leak rate
The signals can be interpreted as follow:
1: Following a “dead period” (or “delay
time”) up to a discernible signal level, the
SLD + SPFP 1 + nnn PFP
signal, which is proportional to the partial
S LD
pressure for helium, will rise to its full
B) Response time: t95% = 3 · SV = 3 · 24.66
150 ` value of pHe = Q/Seff in accordance with
` = 18.25 s
m
eff s
equation 5.9:
Estimate: Value for S, V and γ are uncertain → certain: calibrate with reference leak Q  –t

pHe = ⋅ 1 − e τ  (5.9 )
Seff  
Fig. 5.13 Partial flow principle

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Leak Detection Fundamentals of Vacuum Technology

5.7 Leak detection


2 Q 1 Q 3 Q techniques using
S
V
S’ S
V
S/2
V
helium leak
MS MS MS
detectors

}
Q Throttle
Signal S
LD LD LD

amplitude
Faster, less sensitive normal Slower, more sensitive 5.7.1 Spray technique
Q = 2p 2,0
100% (local leak test)
S/2
95% The test specimen, connected to the heli-
3 um leak detector, is slowly traced with a
very fine stream of helium from the spray
Signal rise
pistol, aimed at likely leakage points (wel-
Q =p 100%
S
1,0 ding seams, flange connectors, fused
95%
1 joints), bearing in mind the time constant
Q = P/ 100% of the system as per Equation 5.8 (see Fig.
2 0,5 Compensation period, e.g. t95% = 3 · τ = 3 V
·
S + S’ 95% S 5.14). The volume sprayed must be adju-
2 (τ = V ... Time constant)
S sted to suit the leak rate to be detected and
Time the size and accessibility of the object
0
to 3 · V = 1 (3 · V) 3· V 3 · SV = 2 (3 · V ) being tested. Although helium is lighter
Dead time S + S’ 2 S S /2 S
than air and therefore will collect beneath
the ceiling of the room, it will be so well
Fig. 5.14 Signal responses and pumping speed
distributed by drafts and turbulence indu-
ced by movements within the room that
one need not assume that helium will be
The signal will attain a prortion of its ulti- 5.6 Limit values / found primarily (or only) at the top of the
mate value after room during search for leaks. In spite of
t = 1 τ . . 63.3 % t = 2 τ . . 86.5 %
Specifications for this, it is advisable, particularly when dea-
ling with larger components, to start the
t = 3 τ . . 95.0 % t = 4 τ . . 98.2 % the leak detector search for leaks at the top.
t = 5 τ . . 99.3 % t = 6 τ . . 99.8 %
1. The smallest detectable leak rate. In order to avoid a surge of helium when
The period required to reach 95 % of the
2. The effective pumping speed at the the spray valve is opened (as this would
ultimate value is normally referred to as
test connection. “contaminate” the entire environment) it is
the response time.
advisable to install a choke valve to adjust
2: With the installation of the partial flow 3. The maximum permissible pressure the helium quantity, directly before or after
pump both the time constant and the sig- inside the test specimen (also the the spray pistol (see Fig. 5.15). The correct
nal amplitude will be reduced by a factor of maximum permissible inlet pressure). quantity can be determined easiest by sub-
2; that means a quicker rise but a signal This pressure pmax will be about 10-1 merging the outlet opening in a container
which is only half as great. A small time for LDs with classical PFPs and about 2 of water and setting the valve on the basis
constant means quick changes and thus to 10 mbar for LDs with compound of the rising bubbles. Variable-area flow-
quick display and, in turn, short leak detec- PFPs. The product of this maximum meters are indeed available for the requi-
tion times. permissible operating pressure and the red small flow quantities but are actually
pumping speed S of the pump system too expensive. In addition, it is easy to use
3: The throttling of the pumping speed to at the detector’s test connection is the the water-filled container at any time to
0.5 S, increases both the time constant maximum permissible throughput: determine whether helium is still flowing.
and the signal amplitude by a factor of 2. A
Qmax = pmax · Seff, connector (5.10)
large value for t thus increases the time The helium content of the air can also be
required appropriately. Great sensitivity, This equation shows that it is by no means detected with helium leak detectors where
achieved by reducing the pumping speed, advantageous to attain high sensitivity by large leaks allow so much air to enter the
is always associated with greater time throttling down the pumping speed. The vessel that the 5 ppm share of helium in
requirements and thus by no means is maximum permissible throughput would the air is sufficient for detection purposes.
always of advantage. otherwise be too small. The unit is not fun- The leak rate is then:
An estimate of the overall time constants ctional when – either due to one large leak Display (pure He) Display (atmosph. He)
or several smaller leaks – more gas flows ———————– = ——————————
for several volumes connected one behind
to another and to the associated pumps into the unit than the maximum permissi-
ble throughput rate for the leak detector.
1

QL = Display (pure He)


5 · 10-6

(5.11)
D00
can be made in an initial approximation by
adding the individual time constants. = 2 · 10+5 · Display (atmospheric He)

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Fundamentals of Vacuum Technology Leak Detection

5.7.3.1 Envelope test – test specimen


pressurized with helium

a) Envelope test with concentration


measurement and subsequent leak
rate calculation
To determine overall leakiness of a test
object pressurized with helium the object
shall be enclosed in an envelope which is
either rigid or deformable (plastic). The
test gas leaving the leaks accumulates so
that the helium concentration in the enve-
lope rises. Following an enrichment period
to be determined (operating period) the
change in concentration inside the envelo-
pe will be measured with a sniffer connec-
ted to the helium detection unit. The over-
all leak rate (integral leak rate) can be cal-
culated following calibration of the test
Avoiding the “helium surge” when the pistol valve is opened configuration with a reference concen-
a) Throttle hose or tration, e.g. atmospheric air. This method
b) Adjustable throttle valve ahead of the spray pistol makes it possible to detect even the smal-
Minimum helium quantity for correct display: Changing the setting for the throttle shall not affect
indication.
lest overall leakiness and is suitable in par-
The minimum quantity is always much smaller than one would set without a flowmeter (e.g. by ticular for automated industrial leak
listening for flow or letting the helium flow across moistened lips). The simplest check without a testing. Due to gas accumulation, the
flowmeter: Letting gas bubble through water. limits for normal sniffer techniques are
shifted toward lower leak rates and the
Fig. 5.15 Helium spray equipment
ambient conditions such as temperature,
air flow and sniffer tracing speed lose
5.7.2 Sniffer technology detector and sniffer unit will have to be influence. When using plastic envelopes it
(local leak test using the calibrated together. Here the distance from is necessary to take into account helium
the specimen and the tracing speed will permeation through the plastic envelope
positive pressure have to be included in calibration, too. during long enrichment periods.
method)
Here the points suspected of leaking at the b) Direct measurement of the leak rate
pressurized test specimen (see Fig. 5.4, d) with the leak detector (rigid envelope)
are carefully traced with a test gas probe When the test specimen, pressurized with
which is connected with the leak detector 5.7.3 Vacuum envelope test helium, is placed in a rigid vacuum cham-
by way of a hose. Either helium or hydro- (integral leak test) ber, connected to a helium leak detector,
gen can be detected with the INFICON heli- the integral leak rate can be read directly at
Vacuum envelope tests are integral leak
um leak detectors. The sensitivity of the the leak detector.
tests using helium as the test gas, in which
method and the accuracy of locating leaky
the test specimen is enclosed either in a
points will depend on the nature of the
rigid (usually metal) enclosure or in a light
sniffer used and the response time for the 5.7.3.2 Envelope test with test
plastic envelope. The helium which enters
leak detector to which it is connected. In specimen evacuated
or leaves (depending on the nature of the
addition, it will depend on the speed at
test) the test specimen is passed to a heli- a) Envelope = “plastic tent”
which the probe is passed by the leak
um leak detector, where it is measured. The evacuated test specimen is surroun-
points and the distance between the tip of
Envelope tests are made either with the ded by a light-weight (plastic) enclosure
the probe and the surface of the test spe-
test specimen pressurized with helium and this is then filled with helium once the
cimen. The many parameters which play a
(Fig. 5.4c) or with the test specimen eva- atmospheric air has been removed. When
part here make it more difficult to determi-
cuated (Fig. 5.4a). In both cases it may be using a plastic bag as the envelope, the
ne the leak rates quantitatively. Using snif-
necessary to convert the helium enrich- bag should be pressed against the test
fer processes it is possible, virtually inde-
ment figure (accumulation) to the helium specimen before filling it with helium in
pendent of the type of gas, to detect leak
standard leak rate. order to expel as much air as possible and
rates of about 10-7 mbar · l/s. The limitati-
to make the measurement with the purest
on of sensitivity in the detection of helium
helium charge possible. The entire outside
is due primarily to the helium in the atmos-
surface of the test object is in contact with
phere (see Chapter 9, Table VIII). In regard
the test gas. If test gas passes through
to quantitative measurements, the leak
leaks and into the test specimen, then the
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Leak Detection Fundamentals of Vacuum Technology

integral leak rate will be indicated, regard- 5.8 Industrial leak


less of the number of leaks. In addition, it
is necessary to observe when repeating testing
testing in enclosed areas that the helium
content of the room will rise quite rapidly Industrial leak testing using helium as the
when the envelope is removed. Using pla- test gas is characterized above all by the fact
stic bags is thus more advisable for “one- that the leak detection equipment is fully
off” testing of large plants. The plastic integrated into the manufacturing line. The
envelope used here is often referred to as design and construction of such test units
a “tent”. will naturally take into account the task to be
carried out in each case (e.g. leak testing
b) Rigid envelope vehicle rims made of aluminum or leak
The use of a solid vacuum vessel as the testing for metal drums). Mass-produced,
rigid envelope, on the other hand, is better standardized component modules will be
for repetitive testing where an integral test used wherever possible. The parts to be
is to be made. When solid envelopes are examined are fed to the leak testing system
used it is also possible to recover the heli- (envelope test with rigid envelope and positi-
um once the test has been completed. ve pressure [5.7.3.1b] or vacuum [5.7.3.2b]
inside the specimen) by way of a conveyor
system. There they will be examined indivi-
dually using the integral methods and auto-
matically moved on. Specimens found to be
leaking will be shunted to the side.
5.7.4 “Bombing” test,
“Storage under pressure” The advantages of the helium test method,
seen from the industrial point of view, may
The “bombing” test is use to check the be summarized as follows:
tightness of components which are alrea-
dy hermetically sealed and which exhibit a • The leak rates which can be detected
gas-filled, internal cavity. The components with this process go far beyond all prac-
to be examined (e.g. transistors, IC hou- tical requirements.
sings, dry-reed relays, reed contact swit- • The integral leak test, i.e. the total leak
ches, quartz oscillators, laser diodes and rate for all individual leaks, facilitates
the like) are placed in a pressure vessel the detection of microscopic and spon-
which is filled with helium. Operating with ge-like distributed leaks which alto-
the test gas at relatively high pressure (5 gether result in leakage losses similar
to 10 bar) and leaving the system standing to those for a larger individual leak.
over several hours the test gas (helium)
will collect inside the leaking specimens. • The testing procedure and sequence
This procedure is the actual “bombing”. To can be fully automated.
make the leak test, then, the specimens are • The cyclical, automatic test system
placed in a vacuum chamber following
check (self-monitoring) of the device
“bombing”, in the same way as described
ensures great testing reliability.
for the vacuum envelope test. The overall
leak rate is then determined. Specimens • Helium is non-toxic and non-hazardous
with large leaks will, however, lose their (no maximum allowable concentrations
test gas concentration even as the vacuum need be observed).
chamber is being evacuated, so that they
• Testing can be easily documented, indi-
will not be recognized as leaky during the
cating the parameters and results, on a
actual leak test using the detector. It is for
printer.
this reason that another test to register
very large leaks will have to be made prior Use of the helium test method will result in
to the leak test in the vacuum chamber. considerable increases in efficiency (cyc-
ling times being only a matter of seconds
in length) and lead to a considerable
increase in testing reliability. As a result of
this and due to the EN/ISO 9000 require-
ments, traditional industrial test methods D00
(water bath, soap bubble test, etc.) will
now largely be abandoned.

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Fundamentals of Vacuum Technology Thin Film Controllers / Control Units

6 Thin film oscillates reliably) despite refined techno-


logy, a number of approaches have been
of less than one atomic layer can be detec-
ted.
controllers and developed to expand this capacity:
In the late 1950s Sauerbrey and Lostis dis-
1. The use of several crystals, one behind covered that the frequency shift connected
control units the other, in a multiple crystal holder with the coating of the quartz crystal is a
with automatic change and data upda- function of the change in mass due to the
with quartz ting in the event of imminent failure of a coating material in the following way:
quartz: CrystalSix.
Mf ∆F ∆F
oscillators 2. The RateWatcher function, in which the
=
Mq Fq
or Mf = Mq ·
Fq
with (6.1)
quartz is alternately exposed to the coa-
ting beam for a short time until all mea- Mf mass of the coating
6.1 Introduction surements and regulation have been
carried out and then remains covered
Mq mass of the quartz prior to coating
Fq frequency prior to coating
It took a long time to go from the coating by a shutter for a longer period of time. Fc frequency after coating
of quartz crystals for frequency fine ∆F = Ff – Fc ... frequency shift due to coa-
tuning, which has long been in practice, to The selection of the “right” crystal holder
ting
utilization of frequency change to determi- thus plays an important role in all measu-
rements with quartz oscillators. Various If the following are now applied:
ne the mass per unit area as a microbalan- Mf = (Mc – Mq) = Df · ρf · A and
ce with the present-day degree of precisi- crystal holder designs are recommended
on. In 1880 two brothers, J. and P. Curie, for the different applications: with or with-
Mq = Dq · rq · A, where T = the coating
out shutter, bakeable for UHV, double
discovered the piezoelectric effect. Under thickness, ρ = density and A stands for
mechanical loads on certain quartz crystal crystal holder or crystal six as well as spe-
area while the index q stands for the state
surfaces, electrical charges occur that are cial versions for sputter applications. In
of the “uncoated quartz” and c for the state
caused by the asymmetrical crystalline addition to these important and more
after “frequency shift due to coating”, the
structure of SiO2. Conversely, in a piezo- “mechanical” aspects, the advances in
following results are obtained for the coa-
crystal deformations appear in an electri- measuring and control technology and
ting thickness:
cal field and mechanical oscillations occur equipment features will be discussed in
in an alternating field. A distinction is the following. Fq ∆F ∆F
Df = · Dq · ρ q · =K·
made between bending oscillations, thick- Fq Fq · ρ f ρ f with
ness shear mode and thickness shear
oscillations. Depending on the orientation
Dq · Fq · ρq NAT · ρq
of the cut plane to the crystal lattice, a K= = where
number of different cuts are distinguished, 6.2 Basic principles of 2
Fq
2
Fq
of which only the so-called AT cut with a
cut angle of 35°10" is used in thin film con- coating thickness N = Fq · Dq is the frequency constant (for
trollers because the frequency has a very measurement with the AT cut NAT = 166100 Hz · cm) and
low temperature dependence in the range ρq = 2.649 g/cm3 is the density of the
between 0 and 50 °C with this cut. Accor- quartz oscillators quartz. The coating thickness is thus pro-
dingly, an attempt must be made not to portional to the frequency shift ∆F and
exceed this temperature range during coa- The quartz oscillator coating thickness
gauge (thin film controller) utilizes the pie- inversely proportional to the density ρf of
ting (water cooling of crystal holder). the coating material. The equation
zoelectric sensitivity of a quartz oscillator
Since there is still a problem with “quartz (monitor crystal) to the supplied mass. ∆F
capacity” (i.e. the maximum possible coa- Df = K ·
This property is utilized to monitor the ρf
ting thickness of the quartz at which it still coating rate and final thickness during
vacuum coating. for the coating thickness was used in the
A very sharp electromechanical resonance first coating thickness measuring units
occurs at certain discrete frequencies of with “frequency measurement” ever used.
rel. frequency change (ppm)

the voltage applied. If mass is added to the According to this equation, a crystal with a
surface of the quartz crystal oscillating in starting frequency of 6.0 MHz displays a
resonance, this resonance frequency is decline in frequency of 2.27 Hz after coa-
diminished. This frequency shift is very ting with 1Å of aluminum
reproducible and is now understood preci- (de = 2.77 g/cm3). In this way the growth
sely for various oscillation modes of of a fixed coating due to evaporation or
quartz. Today this phenomenon, which is sputtering can be monitored through pre-
Temperature (°C) easy to understand in heuristic terms, is cise measurement of the frequency shift of
an indispensable measuring and process the crystal. It was only when knowledge of
Fig. 6.1 Natural frequency as a function of temperature
control tool, with which a coating increase the quantitative interrelationship of this
in an AT cut quartz crystal

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Thin Film Controllers / Control Units Fundamentals of Vacuum Technology

E

Node

Fig. 6.2 Thickness shear oscillations Fig. 6.3 Shape of INFICON quartz crystals

effect was acquired that it became possible The characteristic motions of the thickness The two together ensure that the acoustic
to determine precisely the quantity of shear oscillation are parallel to the main energy is recorded. Reducing the electrode
material that is deposited on a substrate in crystal boundary surfaces. In other words: diameter limits the excitation to the midd-
a vacuum. Previously this had been prac- the surfaces are shift antinodes, see Fig. le area. The surface contour consumes the
tically impossible. 6.2. The resonance frequencies slightly energy of the moving acoustic waves befo-
above the basic frequency are called re they reach the crystal edge. It is not
“anharmonic” and are a combination of reflected into the center where it could
thickness shear and thickness rotation interfere with new incoming waves.
oscillation forms. The resonance frequen-
Such a small crystal behaves like an infini-
6.3 The shape of cy at around three times the value for the
tely expanded crystal. However, if the
fundamental wave is called “quasi-harmo-
quartz oscillator nic”. Near the quasi-harmonic there are
crystal vibrations remain restricted to the
center, one can clamp the outer edge to a
crystals also a number of anharmonics with a
crystal holder, without engendering unde-
slightly higher frequency.
sired side effects. Moreover, contouring
Regardless of how sophisticated the elec-
The design of the monitor crystals used reduces the resonance intensity of undesi-
tronic environment is, the main compo-
nowadays (see Fig. 6.3) displays a number red anharmonics. This limits the capacity
nent for coating measurement remains the
of significant improvements over the origi- of the resonator to maintain these oscilla-
monitor quartz crystal. Originally monitor
nal square crystals. The first improvement tions considerably.
quartzes had a square shape. Fig. 6.4
was the use of round crystals. The enlar-
shows the resonance spectrum of a quartz Use of an adhesive coating has enhanced
ged symmetry greatly reduced the number
resonator with the design used today (Fig. the adhesion of the quartz electrode. Even
of possible oscillation modes. A second
6.3). The lowest resonance frequency is the rate spikes occurring with increasing
group of improvements involved providing
initially given by a thickness shear oscilla- film stress (strain) and caused by micro-
one of the surfaces with a contour and
tion, which is called the fundamental wave. tears in the coating were reduced. Coating
making the excitation electrode smaller.
material remains at these micro-tears
without adhesion and therefore cannot
oscillate. These open areas are not registe-
red and thus an incorrect thickness is indi-
cated.
Fig. 6.4 shows the frequency behavior of a
quartz crystal shaped as in Fig. 6.3. The
log Relative intensy

ordinate represents the amplitude of the


oscillation or also the current flowing
through the crystal as a function of the fre-
quency on the abscissa.
Usually an AT cut is chosen for the coating
thickness measurement because through
the selection of the cut angle the frequen-
cy has a very small temperature coefficient
at room temperature.
D00
Frequency (MHz)
Fig. 6.4 Frequency resonance spectrum Since one cannot distinguish between

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Fundamentals of Vacuum Technology Thin Film Controllers / Control Units

• coating: frequency reduction = negati- multaneously with the first and counts the 6.5 The Z match
ve influence oscillations of the reference crystal during
• temperature change:
m oscillations of the monitor crystal. technique
Because the reference frequency Fr is
negative or positive influence Miller and Bolef (1968) treated the quartz
known and stable, the time for m monitor
• temperature gradients on the crystal, oscillations can be determined accurately oscillator and coating system as a single-
positive or negative to ± 2/Fr. The monitor oscillation period is dimensional, coherent acoustic resonator.
then Lu and Lewis (1972) developed the simpli-
• stresses caused by the coating fied Z match equation on that basis. Simul-
n
taneous advances in electronics, particu-
it is important to minimize the temperatu- Fr · m larly the microprocessor, made it possible
re influence. This is the only way to mea-
to solve the Z match equation in real time.
sure small differences in mass. where n is the reading of the reference Most coating process control units sold
counter. The accuracy of the measurement today use this sophisticated equation,
is determined by the frequency of the refe- which takes into account the acoustic pro-
rence oscillator and the length of the coun- perties of the quartz oscillator/coating
ting time that is specified through the size system:
6.4 Period of m.
 NAT ⋅ dq   (
 π ⋅ Fq − Fc
 ⋅ arctg Z ⋅ tg 
)
measurement For low coating rates, small densities of Tf = 
π ⋅ d ⋅ F
f c ⋅ Z 
  Fq  (6.4)
the coating material and fast measure-
Although the instruments that functioned ments (that require short counting times),
according to equation 6.2 were very use- it is important to have a reference oscilla-
ful, it soon became obvious that for the tor with a high frequency. All of this requi- dq ⋅ Uq acoustic impedance ratio
desired accuracy their area of application Z=
res great time precision so that the small df ⋅ U f
was typically limited to ∆F < 0.02 Fq. Even coating-related frequency shifts can be
at a relative frequency change of Uq = shear module, quartz
resolved. If the frequency shift of the mo-
(Fq – Fc) / Fq < 2 %, errors of around 2 % Uf = shear module, film
nitor crystal decreases between two mea-
occurred in the coating thickness measu- surements on the order of magnitude of This led to basic understanding of the con-
rement so that the "usable service life" of the frequency measurement accuracy, version of frequency shift into thickness
the coating in the case of a 6-MHz monitor good rate regulation becomes impossible which enabled correct results in a practical
crystal was about 120 kHz. (rate regulation: regulation of the energy time frame for process control. To achieve
In 1961 Behrndt discovered that: supply to the coating source so that a spe- this high degree of accuracy, the user
Mf (Tc − Tq) ∆F cified coating thickness growth per time must only enter an additional material
= = with (6.3) unit is maintained). The great measure- parameter Zf for the coating material. The
Mq Tq Fc
ment uncertainty then causes more noise validity of the equation was confirmed for
Tc = 1 / Fc ... oscillation period, coated in the closed loop, which can only be many materials and it applies to frequency
Tq = 1 / Fq ... oscillation period, uncoated countered with longer time constants. This shifts up to ∆F < 0.4 Fq! Note that equati-
in turn makes the corrections due to on 6.2 was only valid up to ∆F < 0.02 Fq.
The period measurement (measurement of system deviation slow so that relatively And equation 6.3 only up to ∆F < 0.05 Fq.
the oscillation duration) was the result of long deviations from the desired rate
the introduction of digital time measure- result. This may not be important for sim-
ment and the discovery of the proportiona- ple coatings, but for critical coatings, as in
lity of crystal thickness Dq and oscillation the case of optical filters or very thin,
duration Tq. The necessary precision of slowly growing single-crystal coatings,
thickness measurement permits applicati- errors may result. In many cases, the desi-
6.6 The active
on of equation 6.3 up to about red properties of such coatings are lost if oscillator
∆F < 0.05 Fq. the rate deviations are more than one or
two percent. Finally, frequency and stabili- All units developed up to now are based on
In period measurement a second crystal use of an active oscillator, as shown sche-
oscillator is essentially used as a reference ty of the reference oscillator determine the
precision of the measurement. matically in Fig. 6.5. This circuit keeps the
oscillator that is not coated and usually crystal actively in resonance so that any
oscillates at a much higher frequency than type of oscillation duration or frequency
the monitor crystal. The reference oscilla- measurement can be carried out. In this
tor generates small precision time inter- type of circuit the oscillation is maintained
vals, with which the oscillation duration of as long as sufficient energy is provided by
the monitor crystal is determined. This is the amplifier to compensate for losses in
done by means of two pulse counters: the the crystal oscillation circuit and the
first counts a fixed number of monitor crystal can effect the necessary phase
oscillations m. The second is started si- shift. The basic stability of the crystal

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output phase
amplifier

phase (degrees)
| impedance |

log .Z. (Ohm)


series resonance

crystal Frequency (MHz)

Fig. 6.5 Circuit of the active oscillator Fig. 6.6 Crystal frequencies near the series resonance point

oscillator is created through the sudden noise in the oscillator circuit leads to a lar- cantly smaller, i.e. by the amount of the
phase change that takes place near the ger frequency shift than would be the case frequency difference between the funda-
series resonance point even with a small with a new crystal. In extreme cases, the mental wave and the anharmonic adopted
change in crystal frequency, see Fig. 6.6. original phase/frequency curve shape is by the oscillation.
not retained; the crystal is not able to carry
Normally an oscillator circuit is designed
out a full 90° phase shift.
such that the crystal requires a phase shift
of 0 degrees to permit work at the series The impedance “Z” can increase to very
resonance point. Long- and short-term high values. If this happens, the oscillator
frequency stability are properties of crystal prefers to oscillate in resonance with an 6.7 The mode-lock
oscillators because very small frequency anharmonic frequency. Sometimes this
differences are needed to maintain the condition is met for only a short time and
oscillator
phase shift necessary for the oscillation. the oscillator oscillation jumps back and INFICON has developed a new technology
The frequency stability is ensured through forth between a basic and an anharmonic for overcoming these constraints on the
the quartz crystal, even if there are long- oscillation or it remains as an anharmonic active oscillator. The new system con-
term shifts in the electrical values that are oscillation. This phenomenon is well stantly analyzes the response of the crystal
caused by “phase jitter” due to temperatu- known as “mode hopping”. In addition to to an applied frequency: not only to deter-
re, ageing or short-term noise. If mass is the noise of the rate signal created, this mine the (series) resonance frequency, but
added to the crystal, its electrical pro- may also lead to incorrect termination of a also to ensure that the quartz oscillates in
perties change. coating because of the phase jump. It is the desired mode. The new system is
important here that, nevertheless, the con- insensitive to mode hopping and the resul-
Fig. 6.7 shows the same graph as Fig 6.6,
troller frequently continues to work under tant inaccuracy. It is fast and precise. The
but for a thickly coated crystal. It has lost
these conditions. Whether this has occur- crystal frequency is determined 10 times a
the steep slope displayed in Fig. 6.6.
red can only be ascertained by noting that second with an accuracy to less than
Because the phase rise is less steep, any
the coating thickness is suddenly signifi- 0.0005 Hz.
The ability of the system to initially identify
and then measure a certain mode opens
up new opportunities thanks to the advan-
tages of the additional information content
of these modes. This new, “intelligent”
measuring device makes use of the
phase (degress)
log .Z. (Ohm)

phase phase/frequency properties of the quartz


crystal to determine the resonance fre-
| impedance | quency. It works by applying a synthesized
sinus wave of a certain frequency to the
crystal and measuring the phase differen-
series resonance
ce between the applied signal voltage and
the current flowing through the crystal. In
the case of series resonance, this differen-

Frequency (MHz)
ce is exactly zero degrees; then the crystal
behaves like an ohmic resistance. By dis-
D00
connecting the applied voltage and the
Fig. 6.7 Oscillations of a thickly coated crystal
current that returns from the crystal, one

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Fundamentals of Vacuum Technology Thin Film Controllers / Control Units

can determine with a phase comparator 1) The Z values of the solid material often cut on the position of the anharmonic in
whether the applied frequency is higher or deviate from those of a coating. Thin relation to the fundamental oscillation.
lower than the crystal resonance point. coatings are very sensitive to process
If one side of the quartz is coated with
parameters, especially in a sputter envi-
The crystal impedance is capacitive at fre- material, the spectrum of the resonances
ronment. As a result, the existing values
quencies below the fundamental wave and is shifted to lower frequencies. It has been
for solid material are not adequate.
inductive at frequencies above the reso- observed that the three above mentioned
nance. This information is useful if the 2) For many exotic substances, including modes have a somewhat differing mass
resonance frequency of a crystal is unkno- alloys, the Z value is not known and not sensitivity and thus experience somewhat
wn. A brief frequency sweep is carried out easy to determine. different frequency shifts. This difference
until the phase comparator changes over is utilized to determine the Z value of the
3) It is repeatedly necessary to carry out a
and thus marks the resonance. For AT material. By using the equations for the
precise coating thickness measurement
quartzes we know that the lowest usable individual modes and observing the fre-
for multiple coating with the same
frequency is the fundamental wave. The quencies for the (100) and the (102)
crystal sensor. This applies in particular
anharmonics are slightly above that. This mode, one can calculate the ratio of the
to optical multiple and semi-conductor
information is not only important for the two elastic constants C60 and C55. These
coatings with a high temperature coeffi-
beginning, but also in the rare case that the two elastic constants are based on the
cient TC. However, the effective Z value
instrument loses “track” of the fundamen- shear motion. The key element in Wajid’s
of the mixture of multiple coatings is
tal wave. Once the frequency spectrum of theory is the following equation:
unknown.
the crystal is determined, the instrument
must track the shift in resonance frequen- In such a case, therefore, the only effective (C55 / C66 )coated 1
≈ (6.5)
cy, constantly carry out frequency measu- method is to assume a Z value of 1, i.e. to (C55 / C66 )uncoated (1 + M ⋅ Z )
rements and then convert them into ignore reality with respect to wave propa-
thickness. gation in multi-substance systems. This with
incorrect assumption causes errors in the M ... area mass/density ratio (ratio of coa-
Use of the “intelligent” measuring system prediction of thickness and rate. The
has a number of obvious advantages over ting mass to quartz mass per area
magnitude of the error depends on the unit)
the earlier generation of active oscillators, coating thickness and the amount of devia-
primarily insensitivity to mode hopping as Z ... Z value
tion from the actual Z value.
well as speed and accuracy of measure- It is a fortunate coincidence that the pro-
ment. This technique also enables the In 1989 A. Wajid invented the mode-lock duct M π Z also appears in the Lu-Lewis
introduction of sophisticated properties oscillator. He presumed that a connection equation (equation 6.4). It can be used to
which were not even conceivable with an existed between the fundamental wave and assess the effective Z value from the follo-
active oscillator setup. The same device one of the anharmonics, similar to that wing equations:
that permits the new technology to identify ascertained by Benes between the funda-
the fundamental wave with one sweep can mental oscillation and the third quasi-har-  F  F 
tg M ⋅ Z ⋅ π ⋅ c + Z ⋅ tg  π ⋅ c  = 0 (6.6)
also be used to identify other oscillation monic oscillation. The frequencies of the  Fq  Fq 
modes, such as the anharmonics or quasi- fundamental and the anharmonic oscillati-
harmonics. The unit not only has a device ons are very similar and they solve the or
for constantly tracking the fundamental problem of the capacity of long cables. He  Fc 
found the necessary considerations for tg  M ⋅ Z ⋅ π ⋅ 
wave, but can also be employed to jump  Fq 
back and forth between two or more establishing this connection in works by Z=−
Wilson (1954) as well as Tiersten and  Fc 
modes. This query of different modes can tg  π ⋅ 
take place for two modes with 10 Hz on the Smythe (1979).  Fq 
same crystal. The contour of the crystal, i.e. the spheri-
cal shape of one side, has the effect of Here Fq and Fc are the frequencies of the
separating the individual modes further non-coated or coated quartz in the (100)
from each other and preventing energy mode of the fundamental wave. Because of
transfer from one mode to another. The the ambiguity of the mathematical func-
tions used, the Z value calculated in this
6.8 Auto Z match usual method of identification is to desig-
way is not always a positively defined
nate the fundamental oscillation as (100),
technique the lowest anharmonic frequency as (102) variable. This has no consequences of any
and the next higher anharmonic as (120). significance because M is determined in
The only catch in the use of equation 6.4 is another way by assessing Z and measuring
These three indices of the mode nomen-
that the acoustic impedance must be the frequency shift. Therefore, the thickn-
clature are based on the number of phase
known. There are a number of cases where ess and rate of the coating are calculated
reversals in the wave motion along the
a compromise has to be made with accu- one after the other from the known M.
three crystal axes. The above mentioned
racy due to incomplete or restricted know-
works by Wilson, Tiersten and Smythe One must be aware of the limits of this
ledge of the material constants of the coa-
examine the properties of the modes by technique. Since the assessment of Z
ting material:
studying the influence of the radius of the depends on frequency shifts of two mo-

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des, any minimal shift leads to errors due The most widespread type of controller is used for the setting, a distinction is made
to substantial mechanical or thermal stres- the PID controller. Here P stands for pro- between the closed loop, open loop and
ses. It is not necessary to mention that portional, I for integral and D for differen- resonance response method.
under such circumstances the Z match tial control function. In the following some
Due to the simplicity with which the expe-
technique, too, leads to similar errors. of the properties of this controller are
rimental data can be obtained, we prefer-
Nevertheless, the automatic Z value deter- described in detail. Information on the
red the open loop method. Moreover,
mination of the Z match technique is system behavior is gained through a step
application of this technique permits
somewhat more reliable regarding occur- response to a control fault in certain con-
extensive elimination of the trial and error
rence of errors because the amplitude dis- troller settings.
method.
tribution of the (102) mode is asymmetric
This response is recorded, and then
over the active crystal surface and that of The Auto Control Tune function developed
improved control parameters for a new
the (100) mode is symmetric. by Inficon characterizes a process on the
test are estimated. This procedure is con-
basis of its step responses. After a step-by-
According to our experience, coating-rela- tinued until a satisfactory result is achie-
step change in the power the resulting
ted stresses have the most unfavorable ved. At the end the controller is optimized
changes in the rate as a function of time are
effect on the crystal. This effect is particu- so that its parameters exactly match the
smoothed and stored. The important step
larly pronounced in the presence of gas, characteristics of the evaporator source.
responses are determined, see Fig. 6.8.
e.g. in sputter processes or reactive vacu-
It is a long and frustrating process to
um coating or sputter processes. If the Z In general, it is not possible to characteri-
adjust a controller to an evaporation sour-
value for solid material is known, it is bet- ze all processes exactly, so several appro-
ce, requiring several minutes for stabiliza-
ter to use it than to carry out automatic ximations have to be made. Normally one
tion and hours to obtain satisfactory
determination of the “auto Z ratio”. In assumes that the dynamic characteristic
results. Often the parameters selected for
cases of parallel coating and coating can be reproduced by a process of the first
a certain rate are not suitable for an altered
sequences, however, automatic Z determi- order plus dead time. The Laplace trans-
rate. Thus, a controller should ideally
nation is significantly better. formation for this assumption (transfer to
adjust itself, as the new controllers in
the s plane) is approximated:
INFICON coating measuring units do. At
the beginning of installation and connec- −L

tion the user has the unit measure the cha- Output K p ⋅ 10 s
= with (6.8)
racteristics of the evaporation source. Input τ ⋅ s+1
6.9 Coating thickness Either a PID controller is used as the basis
for slow sources or another type of con- Kp = amplification in stationary state
regulation troller for fast sources without significant L = dead time
The last point to be treated here is the dead time. τ = time constant
theory of the closed loop for coating In relevant literature a distinction is made These three parameters are determined
thickness measuring units to effect coating between three different ways of setting through the response curve of the pro-
growth at a controlled (constant) growth controllers. Depending on which data are cess. An attempt has been made by means
rate. The measuring advantages of the
instruments, such as speed, precision and
reliability, would not be completely exploi-
ted if this information were not inputted
into an improved process monitoring 1.00 K p
system. For a coating process this means
the coating rate should be kept as close
and stable as possible to a setpoint. The
purpose of the closed loop is to make use 0.0632 K p
of the information flow of the measuring point of
maximum
system in order to regulate the capacity for rise
a special evaporation source in an appro-
priately adapted way. When the system
functions correctly, the controller transla-
tes small deviations of the controlled para- 0 t (0.632) Time t
meter (the rate) from the setpoint into cor- L
rection values of the re-adjusted evaporati-
on capacity parameter. The ability of the
controller to measure quickly and precise- T1 = t(0.632) – L
ly keeps the process from deviating signi-
ficantly from the setpoint.
Kp = (change in output signal)/(change in control signal) D00
Fig. 6.8 Process response to a step change with t = 0 (open loop, control signal amplified)

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Fundamentals of Vacuum Technology Thin Film Controllers / Control Units

amplification Kp, time constant T1 and


setpoint deviation precipitation rate dead time L) are used to generate the most
–L
R(s) + E(s) K p · eaaa
s C(s)
s appropriate PID control parameters.
(Σ) Kc (1 + + Td * s) T1s + 1
– Ti
The best results in evaluating coating con-
trol units are achieved with ITAE. There are
[process] [controller] overshoots, but the reaction is fast and the
ripple time short. Controller setting condi-
Fig. 6.9 Block diagram of the PID controller tions have been worked up for all integral
evaluation criteria just mentioned so as to
of several methods to calculate the requi- setpoint minus measured rate. ISE is rela- minimize the related deviations. With a
red parameters of the system response tively insensitive to small deviations, but manual input as well as with experimental
from curves, as shown in Fig. 6.8. This large deviations contribute substantially to determination of the process response
results in a 1-point accordance at 63.2 % the value of the integral. The result is small coefficients, the ideal PID coefficients for
of the transition (a time constant), an “overshoots”, but long ripple times becau- the ITAE evaluation can easily be calcula-
exponential accordance at two points and se deviations occurring late contribute litt- ted from equations 6.13, 6.14 and 6.15:
an exponential accordance weighted le to the integral.
– 0947
.
according to the method of the smallest .   L
 136
The integral of the absolute value of the Kc =   ⋅   (6.13)
squares. A process is sufficiently characte-
deviation IAE (Integral Absolute Error)  p   T1
K
rized by this information so that the con-
was also proposed as a measure for con-
troller algorithm can be applied. Equation 0.738
trol quality:  119
.   L
6.9 shows the Laplace transformation for Ti =   ⋅  (6.14)
 T1   T1
the very often used PID controller: IAE = ∫ e(t) ⋅ dt (6.11)
 S  0995
.
M(s) = Kc · 1 + + Td · S · E (s) (6.9)  L
 Ti  This is more sensitive for small deviations, Td = (0.381⋅ T1) ⋅   (6.15)
 T1
but less sensitive for large deviations than
with ISE.
For slow systems the time interval bet-
M(s)= controlled variable or power Graham and Lanthrop introduced the inte- ween the forced changes in control voltage
Kc = Control amplification gral over time, multiplied by the absolute is extended to avoid “hanging” the control-
(the proportional term) error ITAE (Integral Time Absolute Error), ler (hanging = rapid growth of the control
Ti = integration time as a measure for control quality: signal without the system being able to
Td = differentiation time respond to the altered signal). This makes
ITAE = ∫ t ⋅ e(t) ⋅ dt (6.12) a response to the previous change in the
E(s) = process deviation
controller setting and “powerful” control-
Fig. 6.9 shows the control algorithm and a The ITAE is sensitive to initial and, to a ler settings possible. Another advantage is
process with a phase shift of the first order certain extent, unavoidable deviations. the greater insensitivity to process noise
and a dead time. The dynamics of the mea- Optimum control responses defined because the data used for control do not
suring device and the control elements (in through ITAE consequently have short come from merely one measurement, but
our case the evaporator and the power response times and larger “overshoots” from several, so that the mass-integrating
supply) are implicitly contained in the pro- than in the case of the other two criteria. nature of the quartz crystal is utilized.
cess block. R(s) represents the rate set- However, ITAE has proven to be very use-
In processes with short response times
point. The return mechanism is the devia- ful for evaluating the regulation of coating
(short time constants) and small to
tion created between the measured preci- processes.
unmeasurable dead times, the PID control-
pitation rate C(s) and the rate setpoint
INFICON’S Auto Control Tune is based on ler often has difficulties with the noise of
R(s).
measurements of the system response the coating process (beam deflection,
The key to use of any control system is to with an open loop. The characteristic of rapid thermal short-circuits between melt
select the correct values for Kc, Td and Ti. the system response is calculated on the and evaporator, etc.). In these cases a con-
The “optimum control” is a somewhat basis of a step change in the control sig- trol algorithm of the integral reset type is
subjective term that is made clear by the nal. It is determined experimentally used with success. This controller always
presence of different mathematical defini- through two kinds of curve accordance at integrates the deviation and presses the
tions: two points. This can be done either quick- system towards zero deviation. This tech-
Usually the smallest square error ISE ly with a random rate or more precisely nique works well with small or completely
(Integral Square Error) is used as a mea- with a rate close to the desired setpoint. imperceptible dead times. However, if it is
sure of the quality of the control: Since the process response depends on used with a noticeable phase shift or dead
the position of the system (in our case the time, the controller tends to generate
ISE = ∫ e2(t) ⋅ dt (6.10) coating growth rate), it is best measured oscillations because it overcompensates
near the desired work point. The process the controller signal before the system has
Here e is the error (the deviation): e = rate information measured in this way (process a chance to respond. Auto Control Tune

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recognizes the properties of these fast


systems during the measurement of a step
response and utilizes the information to
calculate the control amplification for a
non-PID control algorithm.

6.10 INFICON
instrument variants
The instrument models available differ
both in hardware and software equipment:
the simplest unit, the XTM/2, is purely a
measuring or display device that cannot
control vacuum coating.
The XTC/2 and XTC/C group can control
vacuum coating sources and up to three
different coatings of a process (not to be
confused with nine different coating pro-
grams). In the case of XTM/2, XTC/2 and
XTC/C units, the AutoZero and AutoTune
functions are not available, and measure-
ment with several sensors simultaneously
as well as simultaneous control of two
vacuum coating sources are not possible.
However, the IC/5 offers all comfort func-
tions available today: measurement with
up to eight sensors with AutoZero and
AutoTune as well as capability of simulta-
neous control of two evaporator sources.
Moreover, it offers 24 material programs,
with which 250 coatings in 50 processes
can be programmed. To simplify operation
and avoid errors, the unit also has a dis-
kette drive. All types of crystal holders can
be connected here. The thickness resoluti-
on is around 1 Å, the rate resolution for
rates between 0 and 99.9 Å/s around 0.1
Å/s and for rates between 100 and 999 Å/s
around 1 Å/s. A particularly attractive opti-
on offered by the IC/5 is a microbalance
board with a highly stable reference
quartz. This oscillator is 50 times more
stable than the standard oscillator; long-
term stability and accuracy are then 2 ppm
over the entire temperature range. This
option is specially designed for coatings of
material with low density and at low coa-
ting rates. This is important for space con-
tamination and sorption studies, for exam-
ple.

D00

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Fundamentals of Vacuum Technology Applications of Vacuum Technology

7. Application of produce conductive coatings for film capa-


citors. Polymer layers on metals enhance
7.2 Coating sources
vacuum the corrosion resistance of the substrate. In all vacuum coating methods layers are
formed by deposition of material from the
Through the use of vacuum it is possible
technology for to create coatings with a high degree of gas phase. The coating material may be
formed by physical processes such as eva-
uniform thickness ranging from several
coating nanometers to more than 100 mm while poration and sputtering, or by chemical
reaction. Therefore, a distinction is made
still achieving very good reproducibility of
techniques the coating properties. Flat substrates, between physical and chemical vapor
deposition:
web and strip, as well as complex molded-
plastic parts can be coated with virtually • physical vapor deposition = PVD
no restrictions as to the substrate materi-
7.1 Vacuum coating al. For example, metals, alloys, glass, cera- • chemical vapor deposition = CVD.
mics, plastics and paper can be coated.
technique The variety of coating materials is also
Vacuum technology has been increasingly very large. In addition to metal and alloy
used in industrial production processes coatings, layers may be produced from
during the last two decades. Some of various chemical compounds or layers of 7.2.1 Thermal evaporators
these processes and their typical working different materials applied in sandwich (boats, wires etc.)
pressure ranges are shown in Fig. 7.1. form. A significant advantage of vacuum
In the evaporation process the material to
coating over other methods is that many
Since a discussion of all processes is be deposited is heated to a temperature
special coating properties desired, such as
beyond the scope of this brochure, this high enough to reach a sufficiently high
structure, hardness, electrical conductivity
section will be restricted to a discussion of vapor pressure and the desired evaporati-
or refractive index, are obtained merely by
several examples of applications in the on or condensation rate is set. The sim-
selecting a specific coating method and
important field of coating technology. plest sources used in evaporation consist
the process paramaters for a certain coa-
of wire filaments, boats of sheet metal or
Deposition of thin films is used to change ting material.
electrically conductive ceramics that are
the surface properties of the base material, heated by passing an electrical current
the substrate. For example, optical pro- through them (Fig. 7.2). However, there
perties such as transmission or reflection are restrictions regarding the type of mate-
of lenses and other glass products, can be rial to be heated. In some cases it is not
adjusted by applying suitable coating layer possible to achieve the necessary evapora-
systems. Metal coatings on plastic web

Ultrahigh vacuum High vacuum Medium vacuum Rough vacuum

Annealing of metals

Degassing of melts

Electron beam melting

Electron beam welding

Evaporation

Sputtering of metals

Casting of resins and lacquers

Drying of plastics

Drying of insulating papers

Freeze-drying of bulk goods

Freeze-drying of pharmaceutical products

10–10 10–7 10–3 100 103

Pressure [mbar]

Fig. 7.1 Pressure ranges for various industrial processes

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Applications of Vacuum Technology Fundamentals of Vacuum Technology

Hairpin-shaped
evaporator made of Evaporator made of
twisted tungsten wire electrically conductive 6
ceramics
5 7
4
Spiral evaporator
made of twisted tung- Boat-shaped
sten wire evaporator 8
3

Trough-shaped
Evaporator 1 9
evaporator
with ceramic
insert

1 Substrates 6 Cathode
2 Sputtered 7 Magnetic
atoms field lines
3 Anode 8 Argon ions
Trough-shaped
4 Electrons 9 Substrate
evaporator with Basket-shaped 5 Target
ceramic coating evaporator

Fig. 7.2 Various thermal evaporators Fig. 7.3 Schematic diagram of a high-performance cathode sputter arrangement

tor temperatures without significantly eva- 7.2.3 Cathode sputtering 7.2.4 Chemical vapor
porating the source holder and thus con- deposition
taminating the coating. Furthermore che- In the cathode sputtering process, the tar-
mical reactions between the holder and the get, a solid, is bombarded with high ener- In contrast to PVD methods, where the
material to be evaporated can occur resul- gy ions in a gas discharge (Fig. 7.3). The substance to be deposited is either solid or
ting in either a reduction of the lifetime of impinging ions transfer their momentum liquid, in chemical vapor deposition the
the evaporator or contamination of the to the atoms in the target material, substance is already in the vapor phase
coating. knocking them off. These displaced atoms when admitted to the vacuum system. To
– the sputtered particles – condense on deposit it, the substance must be thermal-
the substrate facing the target. Compared ly excited, i.e. by means of appropriate
to evaporated particles, sputtered particles high temperatures or with a plasma. Gene-
have considerably higher kinetic energy. rally, in this type of process, a large num-
7.2.2 Electron beam
Therefore, the conditions for condensation ber of chemical reactions take place, some
evaporators and layer growth are very different in the of which are taken advantage of to control
(electron guns) two processes. Sputtered layers usually the desired composition and properties of
have higher adhesive strength and a den- the coating. For example, using silicon-
To evaporate coating material using an
ser coating structure than evaporated hydrogen monomers, soft Si-H polymer
electron beam gun, the material, which is
ones. Sputter cathodes are available in coatings, hard silicon coatings or – by
kept in a water-cooled crucible, is bombar-
many different geometric shapes and sizes addition of oxygen – quartz coatings can
ded by a focused electron beam and there-
as well as electrical circuits configurations. be created by controlling process parame-
by heated. Since the crucible remains cold,
What all sputter cathodes have in common ters.
in principle, contamination of the coating
is a large particle source area compared to
by crucible material is avoided and a high
evaporators and the capability to coat large
degree of coating purity is achieved. With
substrates with a high degree of uniformi-
the focused electron beam, very high tem-
ty. In this type of process metals, alloys of
peratures of the material to be evaporated
any composition as well as oxides can be
can be obtained and thus very high evapo-
used as coating materials.
ration rates. Consequently, high-melting
point compounds such as oxides can be
evaporated in addition to metals and
alloys. By changing the power of the elec-
D00
tron beam the evaporation rate is easily
and rapidly controlled.

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Fundamentals of Vacuum Technology Applications of Vacuum Technology

7.3 Vacuum coating in the plasma and deposits on the substra-


tes as a polymer coating. In this type of
turbomolecular pumps and backing pump
sets consisting of Roots and rotary vane
technology/ system there may be plastic substrates pumps.
with a surface area of several 10 m2 on the
coating systems cage, causing a correspondingly high
desorption gas flow. The vacuum system
must be able to attain the required pressu- 7.3.2 Web coating
7.3.1 Coating of parts res reliably despite these high gas loads.
In the example shown, the system is eva- Metal-coated plastic webs and papers play
For molded-plastic parts, vacuum coating an important role in food packaging. They
cuated with a combination of a backing
techniques are increasingly replacing con- preserve food longer according to storage
and Roots pump. A diffusion pump along
ventional coating methods, such as elec- and transport logistics requirements and
with a cold surface forms the high vacuum
troplating. For example, using vacuum give packaging an attractive appearence.
pump system. The cold surfaces pump a
coating methods, automobile reflectors Another important area of application of
large portion of the vapor and volatile sub-
obtain a mirror-like surface, plastic articles metal-coated web is the production of film
stances emitted by the plastic parts while
in the furniture, decoration, clock and capacitors for electrical and electronics
the diffusion pump basically removes the
watch as well as electronics industry are applications. Metal-coating is carried out
non-condensable gases as well as the
metal-coated and optical effects are crea- in vacuum web coating systems. Fig. 7.6
noble gas required for the sputter process.
ted on articles in the decoration industry. shows a typical scheme. The unit consists
A completely different concept for the
Fig. 7.4 shows a type of vacuum system in of two chambers, the winding chamber
same process steps is shown in Fig. 7.5.
which large batches of molded-plastic with the roll of web to be coated and the
The system consists of four separate stati-
parts can be coated simultaneously. The winding system, as well as the coating
ons made up of a drum rotating around the
substrates are placed on a cage that rota- chamber, where the evaporators are loca-
vertical axis with four substrate chambers
tes past the coating source, a sputter ted. The two chambers are sealed from
and process stations mounted in the vacu-
cathode in this example. In some applica- each other, except for two slits through
um chamber. During rotation, a substrate
tions, by using a glow discharge treat- which the web runs. This makes it possible
chamber moves from the loading and
ment, the substrates are cleaned and the to pump high gas loads from the web roll
unloading station to the pretreatment sta-
surface is activated prior to the coating using a relatively small pumping set. The
tion, to the metallization station, to the
process. This enhances the adhesive pressure in the winding chamber may be
protective coating station and then back to
strength and reproducibility of the coating more than a factor of 100 higher than the
the initial position. Since each station has
properties. A corrosion protection coating pressure simultaneously established in the
its own pumping system, all four proces-
can be applied after sputtering. In this coating chamber. The pump set for the
ses can run simultaneously with entirely
case, a monomer vapor is admitted into winding chamber usually consists of a
independent adjustable process parame-
the system and a high-frequency plasma combination of Roots and rotary vane
ters. The vacuum system comprises of
discharge ignited. The monomer is actived pumps.

1 Vacuum chamber 7 Rotary piston pump


2 High-performance cathode 8 Cold trap
3 Substrate holder 9 High vacuum valve
4 Substrates 10 Valve for bypass line
5 Diffusion pump 11 Foreline valve
6 Roots pump 12 Venting valve
Fig. 7.5 Multi-chamber parts-coating unit (rotationally symmetric in-line system
Fig. 7.4 Diagramm of a batch system for coating parts DynaMet 4V)

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Applications of Vacuum Technology Fundamentals of Vacuum Technology

With strongly degassing rolls of paper, it 7.3.3 Optical coatings periods of time. This requires to produce
may be necessary to install a cold surface the densest coatings possible, into which
in the winding chamber to act as a water Vacuum coatings have a broad range of neither oxygen nor water can penetrate.
vapor pump. The rolls of the plastic web or applications in production of ophthalmic Using glass lenses, this is achieved by
paper typically have diameters between optics, lenses for cameras and other opti- keeping the substrates at temperatures up
400 and 1000 mm and a width of 400 to cal instruments as well as a wide variety of to 300 °C during coating by means of
3000 mm. A precise, electronically con- optical filters and special mirrors. To radiation heaters. However, plastic lenses,
trolled winding system is required for win- obtain the desired transmission or reflec- as those used in eyeglass optics, are not
ding and unwinding as well as web gui- tion properties, at least three, but someti- allowed to be heated above 80 °C. To
dance. mes up to 50 coatings are applied to the obtain dense, stable coatings these sub-
glass or plastic substrates. The coating strates are bombarded with Ar ions from
During the coating process the web, at a properties, such as thickness and refrac- an ion source during coating. Through the
speed of more than 10 m/s, passes a group tive index of the individual coatings, must ion bombardement the right amount of
of evaporators consisting of ceramic boats, be controlled very precisely and matched energy is applied to the growing layer so
from which aluminium is evaporated. To to each other. Most of these coatings are that the coated particles are arranged on
achieve the necessary Al-coating thickness produced using electron beam evapora- the energetically most favorable lattice
at these high web speeds, very high evapo- tors in single-chamber units (Fig. 7.7). The sites, without the substrate temperature
ration rates are required. The evaporators evaporators are installed at the bottom of reaching unacceptably high values. At the
must be run at temperatures in excess of the chamber, usually with automatically same time oxygen can be added to the
1400 °C. The thermal radiation of the eva- operated crucibles, in which there are argon. The resulting oxygen ions are very
porators, together with the heat of conden- several different materials. The substrates reactive and ensure that the oxygen is
sation of the growing layer, yields a consi- are mounted on a rotating calotte above included in the growing layer as desired.
derable thermal load for the web. With the the evaporators. Application of suitable
help of cooled rollers, the foil is cooled shieldings combined with relative move- The vacuum system of such a coating unit
during and after coating so that it is not ment between evaporators and substrates, usually consists of a backing pump set
damaged during coating and has cooled results in a very high degree of coating comprising a rotary vane pump and Roots
down sufficiently prior to winding. uniformity. With the help of quartz coating pump as well as a high vacuum pumping
thickness monitors (see Section 6) and system. Depending on the requirements,
During the entire coating process the coa-
direct measurement of the attained optical diffusion pumps, cryo pumps or turbo-
ting thickness is continuously monitored
properties of the coating system during molecular pumps are used here, in most
with an optical measuring system or by
coating, the coating process is fully con- cases in connection with large refrigerator-
means of electrical resistance measure-
trolled automatically. cooled cold surfaces. The pumps must be
ment devices. The measured values are
installed and protected by shieldings in a
compared with the coating thickness set- One of the key requirements of coatings is way that no coating material can enter the
points in the system and the evaporator that they retain their properties under pumps and the heaters in the system do
power is thus automatically controlled. usual ambient conditions over long

High-perfor-
mance
plasma
source
Electron
beam
evaporator

1 Unwinder
2 Coating source
3 Coating roller
4 Drawing roller
5 Take-up reel
Monomer

Ar
O2
D00
Fig. 7.6 Schematic diagram of a vacuum web coating system Fig. 7.7 Coating unit for optical coating systems

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Fundamentals of Vacuum Technology Applications of Vacuum Technology

not thermally overload them. Since shiel- with oxygen, the individual process stati- required. It is provided by combinations of
ding always reduces the effective pumping ons have to be vacuum-isolated from each rotary vane pumps and Roots pumps. For
speed, the system manufacturer must find other and from the transfer stations. Uti- particularly short cycle times gas cooled
a suitable compromise between shielding lization of valves for separating process Roots pumps are also used.
effect and reduction of pumping speed. chambers is unsatisfactory because it
All major functions of a plant, such as
increases plant dimensions. To avoid fre-
glass transport, control of the sputter pro-
quent and undesirable starting and stop-
cesses and pump control, are carried out
ping of the glass panes, the process cham-
fully automatically. This is the only way to
bers are vacuum-separated through so-
ensure high productivity along with high
7.3.4 Glass coating called “slit locks”, i.e. constantly open slits
product quality.
combined with an intermediate chamber
Coated glass plays a major role in a num- with its own vacuum pump (Fig. 7.9). The
ber of applications: window panes in gaps in the slits are kept as small as tech-
moderate and cold climate zones are pro- nically possible to minimize clearance and
vided with heat-reflecting coating systems therefore conductance as the glass panes
to lower heating costs; in countries with are transported through them. The pum- 7.3.5 Systems for producing
high intensity solar radiation, solar protec- ping speed at the intermediate chamber is data storage disks
tion coatings are used that reduce air kept as high as possible in order to achie-
conditioning costs; coated car windows Coatings for magnetic- or magneto-optic
ve a considerably lower pressure in the data storage media usually consist of
reduce the heating-up of the interior and intermediate chamber than in the process
mirrors are used both in the furniture and several functional coatings that are applied
chambers. This lower pressure greatly to mechanically finished disks. If several
the automobile industry. Most of these reduces the gas flow from a process
coatings are produced in large in-line plates are placed on one common carrier,
chamber via the intermediate chamber to the coating processes can be carried out in
vacuum systems. Fig. 7.8 shows a typical the adjacent process chamber. For very
system. The individual glass panes are a system using a similar principle to that
stringent separation requirements it may used for glass coating. However, most
transported into a entrance chamber at be necessary to place several intermediate
atmospheric pressure. After the entrance disks must be coated on both sides and
chambers between two process chambers. there are substantially greater low particle
valve is closed, the chamber is evacuated
with a forepump set. As soon as the pres- The glass coating process requires high contamination requirements as compared
sure is low enough, the valve to the eva- gas flows for the sputter processes as well to glass coating. Therefore, in-line
cuated transfer chamber can be opened. as low hydrocarbon concentration. The systems for data memories use a vertical
The glass pane is moved into the transfer only vacuum pump which satisfies these carrier that runs through the system (Fig.
chamber and from there at constant speed requirements as well as high pumping 7.10). The sputter cathodes in the process
to the process chambers, where coating is speed stability over time are turbo-mole- stations are mounted on both sides of the
carried out by means of sputter cathodes. cular pumps which are used almost exclu- carrier so that the front and back side of
On the exit side there is, in analogy to the sively. the disk can be coated simultaneously.
entrance side, a transfer chamber in which While the transfer and process chambers An entirely different concept is applied for
the pane is parked until it can be transfer- are constantly evacuated, the entrance and coating of single disks. In this case the dif-
red out through the exit chamber. exit chambers must be periodically vented ferent process stations are arranged in a
Most of the coatings consist of a stack of and then evacuated again. Due to the large circle in a vacuum chamber (Fig. 7.11).
alternative layers of metal and oxide. Since volumes of these chambers and the short The disks are transferred individually from
the metal layers may not be contaminated cycle times, a high pumping speed is a magazine to a star-shaped transport arm.

Process chamber Intermediate chamber Process chamber


1 2
L1Z LZ2
← Slits →
to backing pumps

S1 SZ S2
Entrance chamber Transfer chamber 2 Exit chamber
Transfer chamber 1
Sputter chambers

L1Z, LZ2 = conductance between intermediate chamber and


process chamber 1 or 2
SZ = pumping speed at intermediate chamber
S1, S2 = pumping speed at process chamber 1 or 2
Fig. 7.8 Plant for coating glass panes – 3-chamber in-line system, throughput up to
3,600,000 m2 / year Fig. 7.9 Principle of chamber separation through pressure stages

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Applications of Vacuum Technology Fundamentals of Vacuum Technology

The transport arm cycles one station furt- rated from each other by closing seals. dual processes can be achieved. However,
her after each process step and in this way Each station is pumped by means of its since the slowest process step determines
transports the substrates from one pro- own turbomolecular pump and the indivi- the cycle interval, two process stations
cess station to the next. During cycling all dual processes are started. As many pro- may have to be dedicated for particularly
processes are switched off and the stati- cess stations as there are in the system as timeconsuming processes.
ons are vacuum-linked to each other. As many processes can be performed in par-
soon as the arm has reached the process allel. By sealing off the process stations,
position, the individual stations are sepe- excellent vacuum separation of the indivi-

Fig. 7.10 Plant for coating data storage disks with carrier transport system

Fig. 7.11 Plant for individual coating of data storage disks

D00

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Fundamentals of Vacuum Technology Instruction for Equipment Operation

8. Instructions for 8.2 Contamination of unsuitable in all cases) will have to be used
for cleaning. Maximum cleanliness can be
vacuum equip- vacuum vessels achieved with vapor baths such as those
commonly found in industry. If one desires
and eliminating
ment operation contamination
to get down to extremely low pressure ran-
ges (< 10-7 mbar), then – after cleaning –
the metal components will have to be baked
In addition to the pressure rise method out at temperatures of up to 200 °C.
(Section 6.1) there is a further method for
8.1 Causes of faults detecting contamination, based on the fact
Seriously contaminated metal components
will first have to be cleaned by cutting away
where the desired that condensable vapors will generally or sandblasting the top surface. These
account for the major share of the gas mix methods suffer the disadvantage that the
ultimate pressure in dirty vessels: here the pressure reading surface area for the surface thus treated
is not achieved or at a compression vacuum gauge (partial will be increased through roughening and
pressure for the non-condensable gases) is active centers may potentially be formed
is achieved too compared with that at an electrical vacuum which would readily adsorb vapor molecu-
gauge, e.g. a thermal conductivity or
slowly ionization vacuum gauge (measuring total
les. Supplementary cleaning in the vapor
bath (see above) is advisable. In some
If the desired ultimate pressure is not rea- pressure). These two vacuum gauges cases electrolytic pickling of the surface
ched at all in vacuum equipment or if it is must, however, be clean themselves. may be beneficial. In the case of high vacu-
attained only after an excessively long Where vapors are present the compression um components it is necessary to pay
pumping period, then the following pro- vacuum gauge will indicate much better attention to ensuring that the pickling does
blems may be the reason: pressure than the electrical vacuum gauge. not turn into etching, which would serious-
If the desired ultimate pressure is not reached, This is a sure sign that the vessel walls are ly increase the surface area. Polishing sur-
then contaminated, usually with oil. Another faces which have been sandblasted is not
commonly used procedure is to compare necessary when working in the rough and
• the apparatus may be leaky or dirty, the pressure indication of one and the medium vacuum ranges since the surface
same vacuum gauge (not a compression plays only a subordinate role in these pres-
• the pump may dirty or damaged,
vacuum gauge) with and without a cold sure regimes.
• the vacuum gauge may be defective. trap inserted in the line: Filling the cold trap
with liquid nitrogen will cause the pressure
If the desired ultimate pressure is reached to drop abruptly, by one power of ten or
only after a very long running time, then more, if the container is contaminated 8.3 General operating
• the apparatus may be dirty, since the vapors will freeze out in the trap.
information for
• the pumping line may be restricted, Eliminating contamination for glass
vacuum pumps
• the pump may be dirty or of too small a equipment
capacity, If the contaminants exhibit a high vapor If no defects are found in the vacuum ves-
pressure, then they can be pumped out sels and at the measurement tubes or if
• the pumping speed may be restricted relatively quickly. If this is not successful, the apparatus still does not operate satis-
due to other causes. then the apparatus will have to be cleaned. factorily after the faults have been rec-
In order to locate the fault, one normally Contaminated glass components will first tified, then one should first check the flan-
proceeds by separating the evacuated ves- be cleaned with chromic-sulfuric acid mix- ge seals at the pump end of the system
sel from the pump system (where this is ture or – if this is necessary – with dilute and possibly the shut-off valve. Flange
possible) and checking the vessel alone for hydrofluoric acid (1:30). They are then rin- seals are known to be places at which
leaks and contamination using the pressu- sed with distilled water. If this does not leaks can appear the most easily, resulting
re rise method, for example. If it has been bring about the desired results, then an from slight scratches and mechanical
found that the vessel is free of defects in organic solvent can be tried. Then the damage which initially appears insignifi-
this regard, then the measurement system glass components will again have to be cant. If no defect can be discerned here,
will be checked for cleanliness (see Sec- rinsed with methanol and distilled water. either, then it is advisable to check to see
tion 8.38) and ultimately – if required – the (Do not use denatured alcohol!) whether the pumps have been maintained
pump or the pumping system itself will be in accordance with the operating instruc-
examined. Eliminating contamination at metallic tions.
equipment
Metal components will usually exhibit Given initially in this section are general
traces of contamination by oil and greases. instructions on pump maintenance, to be
If these cannot be readily removed by pum- followed in order to avoid such defects
ping down the vessel, then an appropriate from the very outset. In addition, potential
organic solvent (denatured alcohol is errors and their causes are discussed.

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Instruction for Equipment Operation Fundamentals of Vacuum Technology

8.3.1 Oil-sealed rotary vacuum the minimum level. During a pumping pro- extent of which will depend on the size of
pumps cess oil-sealed rotary pumps will emit oil the pump and the nature of the operations.
vapors from the discharge port, this being In the worst case this can amount to about
(Rotary vane pumps and due to the high operating temperature. 2 cm3 for every cubic meter of air pumped
rotary piston pumps) This leads to oil loss to an extent which (at STP and including the gas ballast also
will depend on the quantity of gas or vapor drawn in). Figure 8.1 makes it possible to
which is drawn into the pump. Larger oil predict the amount of oil loss to be expec-
8.3.1.1 Oil consumption, oil droplets can be retained by installing a ted in practical situations. The example
contamination, oil change coarse separator in the discharge line. This demonstrates that greater oil losses must
The oil serves to: will reduce oil loss considerably. The fine be expected when operating the pump with
• lubricate moving parts, oil mist filter installed in some pumps will gas ballast. This situation, which is gene-
• seal moving parts against atmospheric also retain the finest oil droplets (fine rally valid, is always to be taken into
pressure, separation) so that no oil at all will leave account in practice.
• seal the valve, the outlet of the pump and oil loss is redu- If the pump oil has become unusabledue
• fill the dead space below the valve, ced practically to zero since – as in coarse to exposure to the vapors or contaminants
separation – the oil which is separated out
• to seal the various operational spaces which are encountered in the process,
is returned to the pump. With pumps with- then the oil will have to be replaced. It is
one from another.
out an integral fine separator this device is impossible to formulate any hard-and-fast
In all pumps it is possible to check the oil offered as an optional extra. rules as to when an oil change will be
charge during operation using the built-in required since the nature of the operations
If an oil-filled rotary pump is operated
oil level sight glass. During continuous will determine how long the oil will remain
without an oil separation and return devi-
operation in particular it is necessary to good. Under clean conditions (e.g. backing
ce, then it will be necessary to expect a
ensure that the oil charge never falls below pumps for diffusion pumps in electro-
certain amount of oil consumption, the
nuclear accelerators) rotary vacuum
pumps can run for years without an oil
change. Under extremely “dirty” conditi-
ons (e.g. during impregnation) it may be
necessary to change the oil daily. The oil
will have to be replaced when its original
light brown color, has turned dark brown
or black due to ageing or has become
cloudy because liquid (such as water) has
entered the pump. An oil change is also
necessary when flakes form in corrosion
Pumping speed [m3 · h–1]∏

protection oil, indicating that the corrosion


protection agent is exhausted.

Changing the oil


The oil change should always be carried
out with the pump switched off but at ope-
rating temperature. The oil drain (or fill)
opening provided for each pump is to be
used for this purpose. Where the pump is
more seriously contaminated, then it
should be cleaned. The applicable opera-
ting instructions are to be observed in this
case.

Intake pressure [mbar]


8.3.1.2 Selection of the pump oil
Example: Oil losses for a TRIVAC S 16 A at pressure of 1 mbar: when handling aggressive
a) Without gas ballast: in accordance with the pumping speed curve S = 15 m3 / h; according to diagram: vapors
oil loss = 0.03 cm3 / h (line a)
b) With gas ballast: S = 9 m3/h at 1 mbar; oil loss = 0.018 cm3 / h (line b1), plus additional loss due to If corrosive vapors (e.g. the vapors formed
gas ballast quantity (0.1 times the 1.6 m3 / h rated pumping speed); that is: Chart on the horizontal by acids) are to be pumped, then a
line b2 up to atmospheric pressure: additional loss: 3 cm3 / h (diagonal line). Overall loss during gas PROTELEN® corrosion protection oil
ballast operation 0.018 + 3 = 3.018 cm3 / h
should be used in place of the normal
pump oil (N 62). These types of vapors will
D00
Fig. 8.1 Oil loss for oil-sealed pumps (referenced to an approximate maximum value of 2 cm3 oil loss per cubic meter
then react with the basic (alkaline) corrosi-
of air drawn in [STP])
on protection agent in the oil. The conti-
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Fundamentals of Vacuum Technology Instruction for Equipment Operation

nuous neutralization reactions will exhaust Protection against condensation cing agent. When CO is being pumped it is
the corrosion protection agent at a rate LEYBOLD pumps offer three options for therefore important that air not be used as
depending on the quantity and acidity of keeping vapors from condensing in the the gas ballast but rather that inert gases
the vapors. The oil will have to be changed pumps: be used at the very outside (e.g. Ar or N2).
more frequently, in accordance with these Inert gas ballast should also be used when
• The gas ballast principle (See Fig. 2.14).
factors. Corrosion protection oils are eit- pumping SO2, SO3, and H2S. A corrosion
This increases considerably the amount
her very hygroscopic or they easily form inhibiting oil is also to be used when hand-
of vapor which the pump can tolerate.
emulsions with water. Consequently a ling these three anhydrides. Carbon dioxi-
• Increased pump temperature. The rug-
pump which is filled with corrosion pro- de (CO2) can be pumped without making
ged design of our pumps makes it pos-
tection oil will absorb moisture from the any special arrangements.
sible to run them at temperatures of up
air if it is out of service for an extended
to 120 °C. Thus the tolerance for pure c) Alkaline solutions
period of time. In no case should one ever
water vapor, for example, will rise by a Normal N 62 pump oil is to be used to
use a pump filled with corrosion protection
factor of five when compared with nor- pump basic (alkaline) solutions. Sodium
oil in order to pump water vapor since the
mal gas ballast operation. hydroxide and caustic potash solutions
lubricating and corrosion inhibition pro-
• Using vacuum condensers (see Section should not be pumped in their concen-
perties of the oil would be adversely affec-
ted. Once the oil has absorbed water it will 2.15). These act as selective pumps and trated form. Ammonia is highly amenable
no longer be possible for such pumps to should be sized so that the downstream to pumping with the gas ballast valve clo-
achieve the ultimate pressures which gas ballast pump will not receive more sed. Alkaline organic media such as
would be the case with fresh corrosion vapor than the amount corresponding methylamine and dimethylamine can also
protection oil or standard pump oil (N 62). to the appropriate vapor tolerance. be pumped satisfactorily, but with the gas
Oil-filled pumps should, under normal ballast valve open.
Corrosion protection
operating con-ditions, not be filled with
Oil-sealed pumps are already quite satis- d) Elementary gases
corrosion protection oil. N 62 oil is prefer-
factorily protected against corrosion due Pumping nitrogen and inert gases requires
red when pumping air, water vapor and
to the oil film which will be present on all no special measures.
non-corrosive organic vapors in so far as
the component surfaces. Corrosion is defi-
there is positive protection against the When handling hydrogen it is necessary to
ned here as the electrochemical dis-
vapors condensing inside the pump. make note of the hazard of creating an
solution of metals, i.e. the release of elec-
trons by the metal atom and their accep- explosive mixture. The gas ballast valve
tance by the oxidation agent (corrosive may in no case be opened when dealing
8.3.1.3 Measures when pumping
gas). A metal atom which is susceptible to with hydrogen. The motors driving the
various chemical substances
corrosion must therefore be exposed to an pumps must be of explosion-proof design.
This discussion cannot provide exhaustive active atom of the oxidation agent. Oxygen: Particular caution is required
coverage of the many and varied applicati-
This makes clear how the oil-sealed pump when pumping pure oxygen! Specially
on fields for oil-filled vacuum pumps in the
is protected against corrosion; the concen- formulated pump oils must be used for
chemicals industry. Our many years of
tration of the oxidation agent in the oil is this purpose. We can supply these,
experience with the most difficult of che-
negligible and thus the opportunity for the accompanied by an approval certificate
micals applications can be used to solve
metal to release electrons is equally small. issued by the German Federal Materials
your particular problems. Three aspects
This also makes it clear that the use of so- Testing Authority (BAM), following consul-
should, however, be mentioned briefly:
called “non-rusting” or “stainless” steels tation.
pumping explosive gas mixes, condensab-
le vapors, and corrosive vapors and gases. does not make sense since oxidation is
necessary for the passivation of these e) Alkanes
steels, in order to reach the so-called pas- The low molecular weight alkanes such as
Explosion protection methane and butane can be pumped with
Applicable safety and environmental pro- sive region for these steel compounds.
The critical passivation current density will the gas ballast valve closed or using inert
tection regulations shall be observed when gas as the gas ballast and/or at increased
planning and engineering vacuum normally not appear in oil-sealed pumps.
temperature of the pump. But important –
systems. The operator must be familiar Increased explosion hazard!
with the substances which the system will a) Acids
be pumping and take into account not only Our pumps are fundamentally suited to
f) Alcohols
normal operating conditions but also pumping acids. In special situations
Once operating temperature has been rea-
abnormal situations, operating outside problems with the oil and with auxiliary
ched, methanol and ethanol can be extrac-
normal parameters. The most important equipment attached at the intake and/or
ted without using gas ballast (N 62 pump
aids to avoiding explosive mixtures are – discharge end may occur. Our engineers in
oil). To pump higher molecular weight
in addition to inertization by adding pro- Cologne are available to assist in solving
alcohols (e.g. butanol) the gas ballast
tective gases – maintaining the explosion such problems.
valve will have to be opened or other pro-
limit values with the aid of condensers, tective measures will have to be imple-
adsorption traps and gas scrubbers. b) Anhydrides
mented to prevent condensation.
CO (carbon monoxide) is a strong redu-

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g) Solvents c) The measurement instrument is soiled vacuum vessel down to the cut-in pressu-
Acetone: Can be extracted without difficul- (see Section 8.4.2). re.
ty; wait until normal operating temperatu-
Permissible cut-in pressure PE will depend
re is reached. Potential sources of error when the pump
on the reduction ratios of the roots pump
no longer turns
Benzene: Caution – vapors are highly as against the roughing pump and is cal-
• Check the pump electrical supply.
flammable. Ultimate pressure is degraded culated by dividing the permissible pressu-
• The pump has stood for a long time
by dilution of the pump oil. Mixtures of air re differential ∆pmax by the compression
containing contaminated or resinous
and benzene are explosive and flammable. ratio, reduced by the value of 1:
oil.
Work without a gas ballast! Inert gases
• The pump is colder than 10°C and the ∆pmax
may possibly be used as ballast gas. p = where
oil is stiff. Heat the pump. E k th – 1
Carbon tetrachloride and trichlorethy- • There is a mechanical error. Please con-
lene: Amenable to pumping; non-flam- tact our customer service department. Theoretical pumping speed for the roots pump
k th =
mable and non-explosive but will be dis- Nominal pumping speed for the roughing pump
solved in oil and thus increase the ultima- Oil exits at the shaft
te pressure; wait until normal operating If oil is discharged at the shaft, then the If the pump is protected using a dia-
temperature is achieved. Keep the gas bal- Seeger rotary shaft circlip in the drive bea- phragm-type pressure switch, then the
last open when pumping carbon tet and ring will have to be inspected and possibly pump will be switched on automatically. If
other non-flammable solvents. Use N 62 replaced. The design of the pumps makes a combination of roots pump and roughing
pump oil. it possible to replace this ring easily, follo- pump is to convey highly volatile sub-
wing the operating instructions provided stances such as liquids with a low boiling
Toluene: Pump through the low-temper- point, then it is advisable to use a roots
ature baffle and without gas ballast. Use with the unit.
pump which is equipped with an integral
inert gas, not air, as the gas ballast. bypass line and a valve which will respond
to a pre-set pressure. Example: Roots
vacuum pumps RUVAC WAU/WSU.
8.3.1.4 Operating defects while
pumping with gas ballast – 8.3.2 Roots pumps Roots pumps from the RUVAC WAU/WSU
Potential sources of error series, being equipped with bypass lines,
where the required ultimate 8.3.2.1 General operating instruc- can generally be switched on together with
pressure is not achieved tions, installation and com- the forepump. The bypass protects these
missioning roots pumps against overloading.
a) The pump oil is contaminated (parti-
cularly with dissolved vapors). Check Roots pumps must be exactly level. When
the color and properties. Remedy: attaching the pump it is necessary to ensu-
8.3.2.2 Oil change, maintenance work
Allow the pump to run for an extended re that the pump is not under any tension
period of time with the vacuum vessel or strain whatsoever. Any strains in the Under clean operating conditions the oil in
isolated and the gas ballast valve open. pump casing caused by the connection the roots pump will be loaded only as a
In case of heavy contamination an oil lines shall be avoided. Any strain to which result of the natural wear in the bearings
change is advisable. The pump should the pump is subjected will endanger the and in the gearing. We nevertheless
never be allowed to stand for a longer pump since the clearances inside the roots recommend making the first oil change
period of time when it contains conta- pump are very small. after about 500 hours in service in order to
minated oil. remove any metal particles which might
Roots pumps are connected to the line
have been created by abrasion during the
b) The sliding components in the pump power supply via the motor terminal strip;
run-in period. Otherwise it will be suffi-
are worn or damaged. Under clean con- a motor protection switch (overload/
cient to change the oil every 3000 hours in
ditions our pumps can run for many overheating) shall be provided as required
operation. When extracting gases contai-
years without any particular mainte- by local codes.
ning dust or where other contaminants are
nance effort. Where the pump has been The direction of motor rotation shall be present, it will be necessary to change the
allowed to run for a longer period of checked with the intake and outlet ports oil more frequently. If the pumps have to
time with dirty oil, however, the bea- open prior to installing the pump. The run at high ambient temperatures, then the
rings and the gate valves may exhibit drive shaft, seen from the motor end, must oil in the sealing ring chamber shall also
mechanical damage. This must always rotate counter-clockwise. Note the arrow be replaced at each oil change.
be assumed when the pump no longer on the motor indicating the direction of
achieves the ultimate pressure specified We recommend using our specially formu-
rotation! If the roots pump runs in the
in the catalog even though the oil has lated N 62 oil.
wrong direction, then it is reversed by
been changed. In this case the pump
should be sent in for repair or our
customer service department should be
interchanging two of the phases at the
motor connection cord.
Under “dirty” operating conditions it is
possible for dust deposits to form a D00
“crust” in the pump chamber. These conta-
contacted. The roots pump may be switched on only
minants will deposit in part in the pumping
after the roughing pump has evacuated the

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chamber and in part on the pump’s impel- 2. Excessive power consumption: All the The turbomolecular pump may, for exam-
lers. They may be removed, once the two factors which can lead to elevated tem- ple, be used unprotected inside magnetic
connection lines have been detached, eit- peratures can also cause excessisve fields if the magnetic induction at the sur-
her by blowing out the system with dry amounts of power to be drawn. The face of the pump casing does not exceed
compressed air or by rinsing with a suita- motor is defective if excessive power B = 3 · 10-3 T when radially impinging and
ble cleaning agent, such as petroleum requirements are not accompanied by a B = 15 · 10-3 T at axial impingement.
ether (naphtha). rise in the temperature at the pump.
In a radioactive environment standard tur-
The oil in the roots pump will then have to 3. Oiling at the pump chamber: bomolecular pumps can be used without
be changed. The rotor may be turned only hazard at dose rates of from 104 to 105
by hand during cleaning since, due to the Possible causes: rad. If higher dose rates are encountered,
high speed when the motor is running, the • Oil level too high: Oil is subjected to then certain materials in the pump can be
deposits could damage the pump as they modified in order to withstand the greater
excessive thermal loading. Oil foam is
dislodge from the surfaces. loading. The electronic frequency conver-
swept along.
ters in such cases are to be set up outside
Grime which cannot be eliminated by • Oil mixed with the product: Azeotropic
the radioactive areas since the semicon-
washing can be removed mechanically degasification of the oil.
ductors used inside them can tolerate a
using a wire brush, metallic scrubber or • Pump leaking: Air ingress through the
dose rate of only about 103 rad. The use of
scraper. oil drain or filler screw will cause a large
motor-driven frequency converters which
stream of air and conveyance of oil into
can withstand up to 108 rad represents
Important! the pumping chamber.
another option.
The dislodged residues may not remain in
the pump chamber. After cleaning is com- 4. Abnormal running noises: Roughing (backing) pumps are required
pleted check the pump for operability by Possible causes: for the operation of turbomolecular
slowly turning the impellers by hand. pumps. Depending on the size of the ves-
There may be no resistance to rotation. It • Grime at the impeller sel to be evacuated, the turbomolecular
is generally not necessary to dismantle the • Bearing or gearing damage pumps and forepumps may be switched
roots pump. If this should nevertheless be • Impellers are touching the housing on simultaneously. If the time required to
required due to heavy soiling, then it is pump the vessel down to about 1 mbar
In the case of bearing or gearing damage
highly advisable to have this done by the using the particular fore-pump is longer
or where the impeller scrapes the housing
manufacturer. than the run-up time for the pump (see
the pump should be repaired only by the
operating instructions), then it is advisab-
manufacturer.
le to delay switching on the turbomolecu-
8.3.2.3 Actions in case of operational lar pump. Bypass lines are advisable when
disturbances using turbomolecular pumps in systems
set up for batch (cyclical) operations in
1. Pump becomes too warm: (maximum
order to save the run-up time for the
operating temperature 100 to 115 °C) 8.3.3 Turbomolecular pumps pump. Opening the high vacuum valve is
Possible causes: not dangerous at pressures of about
8.3.3.1 General operating instructions 10-1 mbar.
• Overloading: Excessive heat of com-
pression due to an excessively high In spite of the relatively large gap between
pressure ratio. Check the pressure the pump rotor and the stator, the turbo-
8.3.3.2 Maintenance
value adjustments and the tightness of molecular pumps should be protected
the vacuum chamber! against foreign objects entering through Turbomolecular pumps and frequency
• Incorrect clearances: The distances the intake port. It is for this reason that the converters are nearly maintenance-free. In
between the rotors and the housings pump should never be operated without the case of oil-lubricated pumps it is
have been narrowed due to dirt or the supplied wire-mesh splinter guard. In necessary to replace the bearing lubricant
mechanical strain. addition, sharp shock to the pump when at certain intervals (between 1500 and
• Soiled bearings: Excessive friction in running and sudden changes in attitude 2500 hours in operation, depending on the
the bearings are to be avoided. type). This is not required in the case of
• Improper oil level: If the oil level is too grease-lubricated pumps (lifetime lubri-
Over and above this, and particularly for
high, the gears will touch the oil, cation). If it should become necessary to
the larger types with long rotor blades,
causing friction resistance. Where the clean the pump’s turbine unit, then this
airing the pump to atmospheric pressure
oil level is too low the system will not be can easily be done by the customer, obser-
while the impellers are rotating may be
lubricated. ving the procedures described in the ope-
done only when observing exactly the
• Incorrect oil type: An SAE 30 grade oil rating instructions.
rules given in the operating instructions.
must be used for the pump. Under certain circumstances it is possible
to operate turbomolecular pumps under
exceptional conditions.

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8.3.4 Diffusion and vapor-jet the contaminated pump fluid poured out. should not exceed 10-2 mbar when
vacuum pumps The interior section and the pump body are DIFFELEN is being used.
then cleaned with pure petroleum ether • Measurement system old or soiled (see
8.3.4.1 Changing the pump fluid and (naphtha). The interior section and pump Section 8.4.2).
cleaning the pump body of mercury pumps should have been
cleaned beforehand with a clean brush; Potential sources of error where there is
Changing the pump fluid is always ne- use a bottle brush for the nozzle bores. insufficient pumping speed:
cessary whenever the pump no longer Ensure that all the nozzle orifices are pro- • Forevacuum pressure is too high:
achieves the required ultimate vacuum or perly cleaned. It is advantageous to evapo- Check the forevacuum; allow the gas
when its pumping speed falls off. The ser- rate all solvent residues in a drying kiln. ballast pump to run for a longer period
vice life of the pump fluid will as a rule Then the inside section is inserted once of time with the gas ballast valve open.
come to several weeks or months – or again and the fresh pump fluid is installed It may be necessary to change the oil in
even years – and will depend largely on the through the forevacuum port. It is neces- the forepump.
operating conditions for the pump. It is sary to ensure that the upper nozzle cover • The pump fluid in the diffusion pump
reduced by frequent pumping at high pres- is not moistened with pump fluid! Do not has become unserviceable: Driving
sures, by exposure to aggressive vapors install too much pump fluid! medium will have to be replaced.
and by air ingress of longer duration (this • Nozzles at the diffusion pump are clog-
does not apply to silicone oil and mer- ged: Clean the diffusion pump.
cury). 8.3.4.2 Operating errors with diffusion • Heating is too weak: Check heating out-
In the case of oil diffusion and vapor-jet and vapor-jet pumps put; examine heating plate for good
pumps the danger presented to the pump Potential sources of defects when the thermal contact with the bottom of the
fluid where there is air ingress with the desired ultimate pressure is not reached boiler chamber.
pump hot is often overestimated. Where • Coolant temperature is too high; inade- • Substances are present in the vacuum
air ingress (up to atmospheric pressure) is quate water throughput. The coolant vessel which have a higher vapor pres-
encountered only occasionally and for flow should always be monitored by a sure than the driving medium being
short periods of time then silicone oil will water flowmeter in order to protect the used: among these are, for example,
not be attacked at all and the DIFFELEN pump from damage. Remedy: Measure mercury, which is particularly hazard-
pump fluid will only barely be affected. The the exit temperature of the coolant ous because the mercury vapors will
products with considerably higher vapor water (it should not exceed 30 °C). form amalgams with the nonferrous
pressures which can be created through Increase the coolant flow-through rate. metals in the oil diffusion pump and
oxidation are removed again in a short The cooling coils at the pump may have thus make it impossible to achieve per-
period of time by the fractionation and to be decalcified. fect vacuums.
degassing equipment in the pump (see • Forevacuum pressure too high: This is
Section 2.1.6.1). Even though the pump possible particularly where vapors
fluid which was originally light in color has which are either evacuated from the
been turned brown by air ingress, this vessel or are created as cracking pro-
need not necessarily mean that the medi- ducts from the driving medium (e.g. 8.3.5 Adsorption pumps
um has become unusable. If, on the other following air ingress) get into the roug-
hand, the pump fluid has turned cloudy hing pump. Check the forevacuum 8.3.5.1 Reduction of adsorption
and has become more viscous, as well pressure with the oil diffusion pump capacity
(which may be the case following periods disconnected. Remedy: Run the fore-
of air ingress lasting for several minutes) A considerable reduction in pumping
vacuum pump for an extended period of
then the medium will have to be replaced. speed and failure to reach the ultimate
time with gas ballast. If this is not suffi-
It is possible that under certain circum- pressure which is normally attainable in
cient, then the oil in the forepump will
stances cracking products from the pump spite of thermal regeneration having been
have to be changed.
carried out indicates that the zeolite being
fluid may make the oil in the forepump • Pump fluid at the diffusion pump spent
unserviceable so that here, too, an oil used has become contaminated by outside
or unserviceable: Replace the driving
change will have to be made. substances. It does not make good sense
medium.
to attempt to rejuvenate the contaminated
Mercury diffusion and vapor-jet pumps are • Heating is incorrect: Check the heating
zeolite with special thermal processes. The
less sensitive to air ingress than oil diffusi- output and check for good thermal
zeolite should simply be replaced.
on pumps. The oxidation of the hot mer- contact between the heating plate and
cury caused by the air ingress is negligible the bottom of the boiler section. Repla-
in regard to the operating characteristics ce the heating unit if necessary.
8.3.5.2 Changing the molecular sieve
of the pump when compared with the mer- • Leaks, contamination: Remedy: if the
pump has been contaminated by vapors It will be necessary to rinse the adsorption
cury loss in the forepump line.
Changing the pump fluid: The interior sec-
it may help to use a metering valve to
pass air through the apparatus for
pump thoroughly with solvents before
installing the new zeolite charge. Before
D00
tion will be extracted from the pump and some period of time; here the pressure putting the adsorption pump which has

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been charged with fresh zeolite into servi- 8.3.7 Sputter-ion pumps pump itself will have to be baked out for a
ce it is also necessary to bake out the new few hours at 250 to 300 °C (but not higher
zeolite charge, under vacuum and using Sputter-ion pumps use high-voltage cur- than 350 °C!). The pump should without
the heating element associated with the rent. Installation and connection should be fail remain in operation throughout this
pump, for a period of several hours so that carried out only under the supervision of a period! If the pressure rises above
contaminants which might have collected qualified specialist. The operating instruc- 5 · 10-5 mbar it will be necessary either to
during the storage period can dissipate. tions shall be observed! heat more slowly or to connect an auxiliary
The service life of sputter-ion pumps pump. Before airing one should allow the
depends linearly on the pump’s operating hot sputter-ion pump enough time to cool
pressure. In the case of pumps manufac- down at least to 150 °C.
tured by LEYBOLD, the following applies:
8.3.6 Titanium sublimation
p · T = 45 · 10-3 mbar · h
pumps
(p = operating pressure, T = service life)
Each of the turns in the titanium sublimati-
This means that for operating pressure of 8.4 Information on
on pump contains approximately 1.2 g of
useable titanium supply. At a heating cur- 10-3 mbar working with
rent of 50 A the surface temperature comes the service life is 45 hours
to about 1850 K, the sublimation rate 10-6 mbar vacuum gauges
approximately 0.12 g/h, i.e. a turn can be the service life is 45,000 hours
operated continuously for about 10 hours. -9
10 mbar 8.4.1 Information on installing
Since at pressures below 1 · 10-6 mbar sub- the service life is 45,000,000 hours vacuum sensors
limation is not continuous but rather only at
If a triode pump is not needed over an Here both the external situation in the
intervals which – at low pressures (below
extended period of time it can either be immediate vicinity of the vacuum appara-
5 · 10-8 mbar) and low gas volumes – are
operated continuously at low pressure – tus and the operating conditions within the
already more than ten times the actual sub-
with practically no influence on the service apparatus (e.g. working pressure, compo-
limation period, one may assume a pum-
life – or it can be aired, removed from the sition of the gas content) will be important.
ping period of almost one month at a wor-
pump and packed in a dust-tight container. It is initially necessary to ascertain whether
king pressure of 10-10 mbar per turn.
The starting properties of the sputter-ion the measurement system being installed is
The effective pumping speed of a titanium (triode) pumps manufactured by sensitive in regard to its physical attitude.
sublimation pump will depend on the get- LEYBOLD are so good that no problems Sensors should only be installed vertically
ter screen surface and the geometry of the will be encountered when returning the with the vacuum flange at the bottom to
suction opening. The pumping speed, refe- units to service, even after a longer period keep condensates, metal flakes and filings
renced to the surface area of the getter in storage. from collecting in the sensor or even small
surface, will be dependent on the type of components such as tiny screws and the
When the sputter-ion pumps are installed
gas and the getter screen temperature. like from falling into the sensorand the
one should ensure that the magnetic fields
Since inert gases, for example, cannot be measurement system. The hot incandes-
will not interfere with the operation of
pumped at all, titanium sublimation pumps cent filaments could also bend and deform
other devices (ionization vacuum gauges,
should always be used only with an auxili- improperly and cause electrical shorts
partial pressure measurement units, etc.).
ary pump (sputter-ion pump, turbomole- inside the measurement system. This is
Mounting devices for the sputter-ion
cular pump) used to pump these gas com- the reason behind the following general
pumps may not short circuit the induc-
ponents. The supplementary pump can be rule: If at all possible, install sensors
tance flow and thus weaken the air gap
much smaller than the titanium sublimati- vertically and open to the bottom. It is
inductance and pumping speed.
on pump. Only in a few special cases can also very important to install measurement
one do without the additional pump. If the ultimate pressure which can be attai- systems if at all possible at those points in
ned is not satisfactory even though the the vacuum system which will remain free
The selection of the coolant is dictated by
apparatus is properly sealed, then it will of vibration during operation.
the working conditions and the require-
usually be sufficient to bake out the atta-
ments in terms of ultimate pressure. At The outside temperature must be taken
ched equipment at about 200 to 250 °C. If
high pressures, above 1 · 10-6 mbar, more into account and above all it is necessary
the pressure here rises to about
thermal energy is applied to the getter to avoid hot kilns, furnaces or stoves or
1 · 10-5 mbar when this is done, then the
screen by frequent sublimation cycles. It is other sources of intense radiation which
sputter ion pump will become so hot after
for this reason that cooling with liquid generate an ambient temperature around
evacuating the gases for two hours that it
nitrogen is more favorable. At low pressu- the measurement system which lies above
will not be necessary to heat it any further
res water cooling may be sufficient. The the specific acceptable value. Excessive
in addition. It is also possible to heat the
getter screen should if at all possible be ambient temperatures will result in false
pump by allowing air to enter for 2 hours
heated to room temperature before airing pressure indications in thermal conductivi-
at 10-5 mbar before the other apparatus is
the pump as otherwise the humidity in the ty vacuum sensors.
then subsequently baked out. If the ultima-
air would condense out on the surface.
te pressure is still not satisfactory, then the

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8.4.2 Contamination at the des, electrodes and the tube walls can be used the pressure indication, depending
measurement system and soiled which, under certain circumstances, on the cleanliness of the measurement
will result in a reduction of dielectric sensors and the connector line, may be
its removal strengths. Here, however, the measure- either too high or too low. Here measure-
ment systems can usually be baked out ment errors by more than one complete
The vacuum gauges used in vacuum tech- and degassed by passing a current order of magnitude are possible! Where
nology for pressure measurement will cer- through or by electron bombardment, systems can be baked out it is necessary
tainly work under “dirty” conditions. This quite aside from the fact that ionization to ensure that the connector line can also
is quite understandable since a vacuum vacuum gauges are often used in the ultra- be heated.
device or system does not serve simply to high vacuum range where it is necessary
produce low pressures but rather and pri- to ensure clean operating conditions for
marily have to run processes in chemistry, other reasons.
metallurgy or nuclear physics at low pres-
sures. Here, depending on the nature of 8.4.4 Connectors, power pack,
the process, considerable quantities of
measurement systems
gases or vapors will be liberated either
continuously or intermittently; these can 8.4.3 The influence of The measurement cables (connector
pass into the measurement systems provi- cables between the sensor and the vacuum
magnetic and electrical
ded for pressure measurement and instal- gauge control unit) are normally 2 m long.
led in the vacuum system and – due to fields If longer measurement cables must be
surface reactions or through simple depo- In all those measurement instruments used – for installation in control panels, for
sits – can falsify the pressure measure- which use the ionization of gas molecules example – then it will be necessary to
ments considerably. This is true for all as the measurement principle (cold-catho- examine the situation to determine
types of vacuum gauges whereby, of cour- de and hot-cathode ionization vacuum whether the pressure reading might be fal-
se, high-sensitivity, high-accuracy measu- gauges), strong magnetic leakage fields or sified. Information on the options for using
rement systems are particularly suscep- electrical potentials can have a major influ- over-length cables can be obtained from
tible to soiling resulting from the causes ence on the pressure indication. At low our technical consulting department.
named. One can attempt to protect the pressures it is also possible for wall poten-
measurement systems against contam- tials which deviate from the cathode
ination by providing suitable shielding. potential to influence the ion trap current.
This, however, will often lead to the pres-
sure registered by the measurement In vacuum measurement systems used in
system – which is indeed clean – deviating the high and ultrahigh regimes it is neces-
considerably from the pressure actually sary to ensure in particular that the requi-
prevailing in the system. red high insulation values for the high-vol-
tage electrodes and ion traps also be main-
It is not fundamentally possible to keep the tained during operation and sometimes
measurement system in a vacuum gauge even during bake-out procedures. Insulati-
from becoming soiled. Thus it is necessary on defects may occur both in the external
to ensure that feed line and inside the measurement
• the influence of the contamination on system itself. Insufficient insulation at the
pressure measurement remains as trap (detector) lead may allow creep cur-
small as possible and that rents – at low pressures – to stimulate
overly high pressure value readings. The
• the measurement system can readily be very low ion trap currents make it neces-
cleaned. sary for this lead to be particularly well
These two conditions are not easy to satis- insulated. Inside the measurement sen-
fy by most vacuum gauges in practice. sors, too, creep currents can occur if the
trap is not effectively shielded against the
Dirt in a compression vacuum gauge will other electrodes.
cause an incorrect and uncontrollable
pressure indication. Dirty THERMOVAC An error frequently made when connecting
sensors will show a pressure which is too measurement sensors to the vacuum
high in the lower measurement range system is the use of connector piping
since the surface of the hot wire has chan- which is unacceptably long and narrow.
ged. In Penning vacuum gauges contami- The conductance value must in all cases
nation will induce pressure readings which
are far too low since the discharge cur-
be kept as large as possible. The most
favorable solution is to use integrated
D00
rents will become smaller. In the case of measurement systems. Whenever connec-
ionization vacuum gauges with hot catho- tor lines of lower conductance values are

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Fundamentals of Vacuum Technology Tables, Formulas, Diagrams

9. Tables, formulas, nomograms and symbols

Unit N · m–2, Pa 2) mbar bar Torr Abbrev. Gas C* = λ · p


[cm · mbar]
1 N · m–2 (= 1 Pa) 1 1 · 10–2 1 · 10–5 7.5 · 10–3
1 mbar 100 1 1 · 10–3 0.75 H2 Hydrogen 12.00 · 10–3
1 bar 1 · 105 1 · 103 1 750 He Helium 18.00 · 10–3
Ne Neon 12.30 · 10–3
1 Torr 3) 133 1.33 1.33 · 10–3 1
Ar Argon 6.40 · 10–3
1) The torr is included in the table only to facilitate the transition from Kr Krypton 4.80 · 10–3
this familiar unit to the statutory units N · m-2, mbar and bar. In futu- Xe Xenon 3.60 · 10–3
re the pressure units torr, mm water column, mm mercury column
(mm Hg), % vacuum, technical atmosphere (at), physicalatmosphe- Hg Mercury 3.05 · 10–3
re (atm), atmosphere absolute (ata), pressure above atmospheric O2 Oxygen 6.50 · 10–3
and pressure below atmospheric may no longer be used. Reference N2 Nitrogen 6.10 · 10–3
is made to DIN 1314 in this context. HCl Hydrochloric acid 4.35 · 10–3
2) The unit Newton divided by square meters (N · m-2) is also
designated as CO2 Carbon dioxide 3.95 · 10–3
Pascal (Pa): 1 N · m-2= 1 Pa. H2O Water vapor 3.95 · 10–3
Newton divided by square meters or Pascal is the SI unit for the pres- NH3 Ammonia 4.60 · 10–3
sure of fluids. C2H5OH Ethanol 2.10 · 10–3
3) 1 torr = 4/3 mbar; fl torr = 1 mbar.
Cl2 Chlorine 3.05 · 10–3
Air Air 6.67 · 10–3

Table III: Mean free path l


Values of the product c* of the mean free path λ ( and pressure p for various
Table I: Permissible pressure units including the torr 1) and its conversion gases at 20 °C (see also Fig. 9.1)

1↓= → mbar Pa dyn · cm–2 atm Torr inch Micron cm kp · cm–2 lb · in–2 lb · ft–2
(N/m3) (µbar) (phys.) (mm Hg) Hg (µ) H2O (at tech.) (psi)
mbar 1 102 103 9.87 · 10–4 0.75 2.953 · 10–2 7.5 · 102 1.02 1.02 · 10–3 1.45 · 10–2 2.089
Pa 10–2 1 10 9.87 · 10–6 7.5 · 10–3 2.953 · 10–4 7.5 1.02 · 10–2 1.02 · 10–5 1.45 · 10–4 2.089 · 10–2
µbar 10–3 0.1 1 9.87 · 10–7 7.5 · 10–4 2.953 · 10–5 7.5 · 10–1 1.02 · 10–3 1.02 · 10–6 1.45 · 10–5 2.089 · 10–3
atm 1013 1.01 · 105 1.01 · 106 1 760 29.92 7.6 · 105 1.03 · 103 1.033 14.697 2116.4
Torr 1.33 1.33 · 102 1.33 · 103 1.316 · 10–3 1 3.937 · 10–2 103 1.3595 1.36 · 10–3 1.934 · 10–2 2.7847
in Hg 33.86 33.9 · 102 33.9 · 103 3.342 · 10–2 25.4 1 2.54 · 104 34.53 3.453 · 10–2 0.48115 70.731
µ 1.33 · 10–3 1.33 · 10–1 1.333 1.316 · 10–6 10–3 3.937 · 10–5 1 1.36 · 10–3 1.36 · 10–6 1.934 · 10–5 2.785 · 10–3
cm H2O 0.9807 98.07 980.7 9.678 · 10–4 0.7356 2.896 · 10–2 7.36 · 102 1 10–3 1.422 · 10–2 2.0483
at 9.81 · 102 9.81 · 104 9.81 · 105 0.968 7.36 · 102 28.96 7.36 · 105 103 1 14.22 2048.3
psi 68.95 68.95 · 102 68.95 · 103 6.804 · 10–2 51.71 2.036 51.71 · 103 70.31 7.03 · 10–2 1 1.44 · 102
lb · ft–2 0.4788 47.88 478.8 4.725 · 10–4 0. 3591 1.414 · 10–2 359.1 0.488 4.88 · 10–4 6.94 · 10–3 1

Normal conditions: 0 °C and sea level, i.e. p = 1013 mbar = 760 mm Hg = 760 torr = 1 atm
in Hg = inches of mercury; 1 mtorr (millitorr) = 10-3 torr = 1 µ (micron … µm Hg column)
Pounds per square inch = lb · in-2 = lb / sqin = psi (psig = psi gauge … pressure above atmospheric, pressure gauge reading; psia = psi absolute … absolute
pressure)
Pounds per square foot = lb / sqft = lb / ft2; kgf/sqcm2 = kg force per square cm = kp / cm2 = at; analogously also: lbf / squin = psi
1 dyn · cm-2 (cgs) = 1 µbar (microbar) = 1 barye; 1 bar = 0.1 Mpa; 1 cm water column (cm water column = g / cm2 at 4 °C) = 1 Ger (Geryk)
atm … physical atmosphere – at … technical atmosphere; 100 - (x mbar / 10.13) = y % vacuum

Table II: Conversion of pressure units

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Tables, Formulas, Diagrams Fundamentals of Vacuum Technology

VARIABLE General formula For easy calculation Value for air at 20 °C


Most probable speed
of particles cw
cw = ABBB2 M⋅ RB ⋅ T cw = 1.29 ⋅ 104AB [ ]T
M
cm
s
cw = 410 [m/s]

AB8πBBB
⋅R⋅T –c = 1.46 ⋅ 10 AB
M [ s ]
Mean velocity –c = 4 T cm –c = 464 [m/s]
⋅M
of particles c–
–2 3 ⋅ R ⋅ T 2
cm2
Mean square of velocity

of particles c2
c =
M
–2 T
c = 2.49 ⋅ 108 M [ cms ]
2
–2
c = 25.16 ⋅ 104 2[s ]
p=n⋅k⋅T p = 13.80 ⋅ 10–20 ⋅ n ⋅ T [mbar] p = 4.04 ⋅ 10–17 ⋅ n [mbar] (applies to all gases)
Gas pressure p of particles 1 –
p = ⋅ n ⋅ mT ⋅ c2
3
1 –
p = ⋅ % ⋅ c2
3

Number density of particles n p


n = 7.25 ⋅ 1018 ⋅ [cm–3] p = 2.5 ⋅ 1016 ⋅ p [cm–3] (applies to all gases)
n = p/kT
T

1
Area-related impingement ZA ZA = · n · –c ZA = 2.63 · 1022 ·
p
· p [cm–2 s–1] ZA = 2.85 ⋅ 1020 ⋅ p [cm–2 s–1] (see Fig. 78.2)
4 ABB
M BB
·T
ZA = ABBBB
N
·p
2⋅π⋅M⋅k⋅T
A

1 n ⋅ –c p2 ZV = 8.6 ⋅ 1022 ⋅ p2 [cm–3 s–1] (see Fig. 78.2)


Volume collision rate ZV ZV = ⋅ ZV = 5.27 · 1022 · [cm–3 s–1]
2 λ c* · ABB
BBBB
M ·T
ZA =
1
c* ABBBB
2⋅N
π⋅M⋅k⋅T
⋅p A 2

Equation of state of ideal gas p⋅V=ν⋅R⋅T p ⋅ V = 83.14 ⋅ ν ⋅ T [mbar ⋅ `] p ⋅ V = 2.44 ⋅ 104 ν [mbar ⋅ `] (for all gases)

Area-related mass flow rate qm, A qm, A = ZA ⋅ mT = ABBBB


M
2⋅π⋅k⋅T⋅N
⋅p
A
Qm, A = 4.377 ⋅ 10–2 ABMT ⋅ p [g cm –2 s–1] qm, A = 1.38 ⋅ 10–2 ⋅ p g [cm–2 s–1]

c* = λ · p in cm · mbar (see Tab. III) mT particle mass in g p gas pressure in mbar


k Boltzmann constant in mbar · l · K–1 NA Avogadro constant in mol–1 R molar gas constant in mbar · l · mol–1 K–1
λ mean free path in cm n number density of particles in cm–3 T thermodynamic temperature in K
M molar mass in g · mol–1 υ amount of substance in mol V volume in l

Table IV: Compilation of important formulas pertaining to the kinetic theory of gases

Designation, Symbol Value and Remarks


alphabetically unit

Atomic mass unit mu 1.6605 · 10–27 kg


Avogadro constant NA 6.0225 · 1023 mol–1 Number of particles per mol,
formerly: Loschmidt number
Boltzmann constant k 1.3805 · 10–23 J · K–1
mbar · l
13.805 · 10–23
K
Electron rest mass me 9.1091 · 10–31 kg
Elementary charge e 1.6021 · 10–19 A · s
Molar gas constant R 8.314 J · mol–1 K–1
mbar · l
= 83.14 R = NA · k
mol · K
Molar volume of 22.414 m3 kmol–1 DIN 1343; formerly: molar volume
the ideal gas Vo 22.414 l · mol–1 at 0 °C and 1013 mbar
Standard acceleration of free fall gn 9.8066 m · s–2
Planck constant h 6.6256 · 10–34 J · s
W
Stefan-Boltzmann constant s 5.669 · 10–8 2 4 also: unit conductance, radiation constant
m K
–e A·s
Specific electron charge – 1.7588 · 1011
me kg
Speed of light in vacuum c 2.9979 · 108 m · s–1
Standard reference density ln kg · m–3 Density at ϑ = 0 °C and pn = 1013 mbar
of a gas
Standard reference pressure
Standard reference temperature
pn
Tn
101.325 Pa = 1013 mbar
Tn = 273.15 K, J = 0 °C
DIN 1343 (Nov. 75)
DIN 1343 (Nov. 75)
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Table V: Important values

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Fundamentals of Vacuum Technology Tables, Formulas, Diagrams

Unit l · s–1 m3 · h–1 cm3 · s–1 cuft · min–1


1 l · s–1 1 3.6 1000 2.12
1 m3 · h–1 0.2778 1 277.8 0.589
1 cm3 · s–1 10–3 3.6 · 10–3 1 2.1 · 10–3
1 cuft · min–1 0.4719 1.699 471.95 1
Table VI: Conversion of pumping speed (volume flow rate) units

1↓ = ... → mbar · l/s kg · h–1 (20°C) kg · h–1 (0°C) cm3/h (NTP) cm3/s (NTP) Torr · l/s g/a (F12. 20 °C) g/a (F12. 25 °C) µ · cfm lusec Pa · l/s slpm
mbar · l/s 1 4.28 · 10–3 4.59 · 10–3 3554 0.987 0.75 1.56 · 105 1.54 · 105 1593 7.52 · 102 100 59.2 · 10–3
kg · h–1 (20 °C) 234 1 1.073 8.31 · 105 231 175 – – 37.2 · 104 1.75 · 105 23.4 · 103 13.86
kg · h–1 (0 °C) 218 0.932 1 7.74 · 105 215 163 – – 34.6 · 104 1.63 · 105 21.8 · 103 12.91
cm3/h (NTP) 2.81 · 10–4 1.20 · 10–6 1.29 · 10–6 1 2.78 · 10–4 2.11 · 10–4 44 – 44.7 · 10–2 2.11 · 10–1 2.81 · 10–2 1.66 · 10–5
cm3/s (NTP) 1.013 4.33 · 10–3 4.65 · 10–3 3600 1 0.760 1.58 · 105 – 1611 760 101 6 · 10–2
Torr · l/s 1.33 5.70 · 10–3 6.12 · 10–3 4727 1.32 1 2.08 · 105 2.05 · 105 2119 1 · 103 133 78.8 · 10–3
g/a (F12. 20 °C) 6.39 · 10–6 – – 2.27 · 10–2 6.31 · 10–6 4.80 · 10–6 1 – 10.2 · 10–3 4.8 · 10–3 6.39 · 10–4 37.9 · 10–8
g/a (F12. 25 °C) 6.50 · 10–6 – – – – 4.88 · 10–6 – 1 10.4 · 10–3 4.89 · 10–3 6.5 · 10–4 38.5 · 10–8
µ · cfm 6.28 · 10–4 2.69 · 10–6 2.89 · 10–6 2.24 6.21 · 10–4 4.72 · 10 –4 98.16 96.58 1 0.472 6.28 · 10–2 37.2 · 10–6
lusec 1.33 · 10–3 5.70 · 10–6 6.12 · 10–6 4.737 1.32 · 10–3 1 · 10–3 208 205 2.12 1 13.3 · 10–2 78.8 · 10–6
Pa · l/s 1 · 10–2 4.28 · 10–5 4.59 · 10–5 35.54 9.87 · 10–3 7.5 · 10–3 1.56 · 103 1.54 · 103 15.93 7.50 1 59.2 · 10–5
slpm 16.88 72.15 · 10–3 77.45 · 10–3 60.08 · 103 16.67 12.69 2.64 · 106 2.60 · 106 26.9 · 103 12.7 · 103 16.9 · 102 1

1 cm3 (NTP) = 1 cm3 under normal conditions (T = 273.15 K; p = 1013.25 mbar) NTP = normal temperature and pressure (1 atm; 0 °C) R = 83.14 mbar · l · mol–1 · K–1
1 cm3 (NTP) · h–1 = 1 atm · cm3 · h–1 = 1 Ncm3 · h–1 = 1 std cch 1 sccm = 10–3 slpm = 10–3 N · l · min–1 = 60 sccs
SI coherent: 1 Pa · m3 · s–1 = 10 mbar · l · s–1; R = 8.314 Pa · m3 · mol–1 · K–1; M in kg / mol
1 cm3 (NTP) · s–1 = 1 sccs = 60 cm3 (NTP) · min–1 60 sccm = 60 std ccm = 60 Ncm3 · min–1
1 lusec = 1 l · µ · s–1 1 · µ = 1 micron = 10–3 Torr 1 lusec = 10–3 Torr · l · s–1
Freon F 12 (CCl2F2) M = 120.92 g · mol–1; air M = 28.96 g · mol–1
Note: Anglo-American units are not abbreviated nonuniformly! Example: Standard cubic centimeter per minute → sccm = sccpm = std ccm = std ccpm

Table VIIa: Conversion of throughput (QpV) units; (leak rate) units

1↓= ... → mbar · l/s cm3/s **) Torr · l/s Pa · m3/s g/a *) oz/yr *) lb/yr *) atm · ft3/min µ · l/s µ · ft3/h µ · ft3/min
mbar · l/s 1 0.987 0.75 10–1 1.56 · 105 5.5 · 103 3.4 · 102 2.10 · 10–3 7.52 · 102 9.56 · 104 1593
cm3/s **) 1.013 1 0.76 1.01 · 10–1 1.58 · 105 5.6 · 103 3.44 · 102 2.12 · 10–3 760 96.6 · 103 1614
Torr · l/s 1.33 1.32 1 1.33 · 10–1 2.08 · 105 7.3 · 103 4.52 · 102 2.79 · 10–3 103 1.27 · 105 2119
Pa · m3/s 10 9.9 7.5 1 1.56 · 106 5.51 · 104 3.4 · 103 2.09 · 10–2 7.5 · 103 9.54 · 105 15.9 · 103
g/a *) 6.39 · 10–6 6.31 · 10–6 4.80 · 10–6 6.41 · 10–7 1 3.5 · 10 –2 2.17 · 10–3 1.34 · 10–8 4.8 · 10–3 0.612 10.2 · 10–3
oz/yr *) 1.82 · 10–4 1.79 · 10–4 1.36 · 10–4 1.82 · 10–5 28.33 1 6.18 ·· 10–2 3.80 · 10–7 0.136 17.34 0.289
lb/yr *) 2.94 · 10–3 2.86 · 10–3 2.17 · 10–3 2.94 · 10–4 4.57 · 102 16 1 6.17 · 10–6 2.18 280 4.68
atm · ft3/min 4.77 · 102 4.72 · 102 3.58 · 102 47.7 7.46 · 107 2.63 · 106 1.62 · 105 1 3.58 · 105 4.55 · 107 7.60 · 105
µ · l/s 1.33 · 10–3 1.32 · 10–3 10–3 1.33 · 10–4 208 7.34 4.52 · 10–1 2.79 · 10–6 1 127 2.12
µ · ft3/h 1.05 · 10–5 1.04 · 10–5 7.87 · 10–6 1.05 · 10–6 1.63 5.77 · 10–2 3.57 · 10–3 2.20 · 10–8 7.86 · 10–3 1 1.67 · 10–2
µ · ft3/min 6.28 · 10–4 6.20 · 10–4 4.72 · 10–4 6.28 · 10–5 98 3.46 2.14 · 10–1 1.32 · 10–6 0.472 60 1

1 · µ · ft3 · h–1 = 1.04 · 10–5 stsd cc per second 1 micron cubic foot per hour = 0.0079 micron liter per second 1 kg = 2.2046 pounds (lb)
1 cm3 · s–1 (NTP) = 1 atm · cm3 · s–1 = 1 scc · s–1 = 1 sccss 1 micron liter per second = 0.0013 std cc per second = 1 lusec 1 cubic foot (cfut. cf) =
28.3168 dm3
1 atm · ft3 · min–1 = 1 cfm (NTP) 1 micron cubic foot per minute = 1 µ · ft3 · min–1 = 1 µ · cuft · min–1 = 1 µ · cfm
1 lb = 16 ounces (oz)
1 Pa · m3/s = 1 Pa · m3/s (anglo-am.) = 103 Pa · l/s 1 standard cc per second = 96.600 micron cubic feet per hour 1 lusec = 1 µ · l · s–1
1 µ · l · s–1 = 127 µ · ft3 · h–1 = 0.0013 std cc per second = 1 lusec 1 std cc/sec = 760 µ · l · s–1

*) F12 (20 °C) C.Cl2F2 M = 120.92 h/mol **) (NTP) normal temperature and pressure 1 atm und 0 °C

Table VII b: Conversion of throughput (QpV) units; (leak rate) units

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Tables, Formulas, Diagrams Fundamentals of Vacuum Technology

% by weight % by volume Partial pressure mbar


N2 75.51 78.1 792
O2 23.01 20.93 212
Ar 1.29 0.93 9.47
CO2 0.04 0.03 0.31
Ne 1.2 · 10–3 1.8 · 10–3 1.9 · 10–2
He 7 · 10–5 7 · 10–5 5.3 · 10–3
CH4 2 · 10–4 2 · 10–4 2 · 10–3
Kr 3 · 10–4 1.1 · 10–4 1.1 · 10–3
N2O 6 · 10–5 5 · 10–5 5 · 10–4
H2 5 · 10–6 5 · 10–5 5 · 10–4
Xe 4 · 10–5 8.7 · 10–6 9 · 10–5
O3 9 · 10–6 7 · 10–6 7 · 10–5
Σ 100 % Σ 100 % Σ 1013
50 % RH at 20 °C 1.6 1.15 11.7

Note: In the composition of atmospheric air the relative humidity (RH) is indicated separately along
with the temperature.
At the given relative humidity, therefore, the air pressure read on the barometer is 1024 mbar
Table VIII: Composition of atmospheric air

Rough vacuum Medium vacuum High vacuum Ultrahigh vacuum


Pressure p [mbar] 1013 – 1 1 – 10–3 10–3 – 10–7 < 10–7
Particle number density n [cm–3] 1019 – 1016 1016 – 1013 1013 – 109 < 109
Mean free path λ [cm] < 10–2 10–2 – 10 10 – 105 > 105
Impingement rate Za [cm–2 · s–1] 1023 – 1020 1020 – 1017 1017 – 1013 < 1013
Vol.-related collision rate ZV [cm–3 · s–1] 1029 – 1023 1023 – 1017 1017 – 109 < 109
Monolayer time τ [s] < 10–5 10–5 – 10–2 10–2 – 100 > 100
Type of gas flow Viscous flow Knudsen flow Molecular flow Molecular flow

Other special features Convection dependent Significant change in Significant reduction- Particles on the
on pressure thermal conductivity in volume surfaces dominate
of a gas related collision rate to a great extend in
relation to particles in
gaseous space

Table IX: Pressure ranges used in vacuum technology and their characteristics (numbers rounded off to whole power of ten)

At room temperature
Standard values1 Metals Nonmetals
(mbar · l · s–1 · cm–2) 10–9 ... · 10–7 10–7 ... · 10–5
Outgassing rates (standard values) as a function of time
Examples: 1/2 hr. 1 hr. 3 hr. 5 hr. Examples: 1/2 hr. 1 hr. 3 hr. 5 hr.
Ag 1.5 · 10–8 1.1 · 10–8 2 · 10–9 Silicone 1.5 · 10–5 8 · 10–6 3.5 · 10–6 1.5 · 10–6
Al 2 · 10–8 6 · 10–9 NBR 4 · 10–6 3 · 10–6 1.5 · 10–6 1 · 10–6
Cu 4 · 10–8 2 · 10–8 6 · 10–9 3.5 · 10–9 Acrylic glass 1.5 · 10–6 1.2 · 10–6 8 · 10–7 5 · 10–7
Stainless steel 9 · 10–8 3.5 · 10–8 2.5 · 10–8 FPM, FKM 7 · 10–7 4 · 10–7 2 · 10–7 1.5 · 10–7
1 All values depend largely on pretreatment!

Table X: Outgassing rate of materials in mbar · l · s–1 · cm–2

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Fundamentals of Vacuum Technology Tables, Formulas, Diagrams

Nominal width (DN) Internal diam. (mm)


Series R5 R10
10 10
16 16
20 21
25 24
32 34
40 41
50 51
63 70
80 83
100 102
125 127
160 153
200 213
250 261
320 318
400 400
500 501
630 651
800 800
1000 1000

The nominal internal diameters correspond approximately to the


internal diameters of the pipeline components” (DIN 2402 - Feb.
1976). The left-hand column of the nominal internal diameter series
is preferred in practice.

Table XI: Nominal internal diameters (DN) and internal diameters of tubes, pipes and
apertures with circular cross-section (according to PNEUROP)

Solvent Relative Density Melting Boiling Maximum admissible


molecular g / cm3 point point concentration (MAC)
mass (20 °C) °C °C cm3 / m3

Acetone 58 0.798 56
Benzene (solution) 78 0.8788 5.49 80.2 25
Petrol (light) 0.68 ... 0.72 > 100
Carbon tetrachloride 153.8 1.592 – 22.9 76.7 25
Chloroform 119.4 1.48 – 63.5 61 50
Diethyl ether 46 0.7967 –114.5 78 1000
Ethyl alcohol 74 0.713 – 116.4 34.6 400
Hexane 86 0.66 – 93.5 71 500
Isopropanol 60.1 0.785 – 89.5 82.4 400
Methanol 32 0.795 – 97.9 64.7 200 (toxic!)
Methylene chloride 85 1.328 41
Nitromethane 61 1.138 – 29.2 101.75 100
Petroleum ether mixture 0.64 – 40 ... 60
Trichlorethylene (“Tri”) 131.4 1.47 55
Water 18.02 0.998 0.00 100.0 –

Table XII: Important data (characteristic figures) for common solvents

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Tables, Formulas, Diagrams Fundamentals of Vacuum Technology

t ps %D t ps %D t ps %D t ps %D
°C mbar g/m3 °C mbar g/m3 °C mbar g/m3 °C mbar g/m3
– 100 1.403 · 10–5 1.756 · 10–5 – 35 0.2233 0.2032 30 42.43 30.38 95 845.3 504.5
– 99 1.719 2.139 – 34 0.2488 0.2254 31 44.93 32.07 96 876.9 522.1
– 98 2.101 2.599 – 33 0.2769 0.2498 32 47.55 33.83 97 909.4 540.3
– 97 2.561 3.150 – 32 0.3079 0.2767 33 50.31 35.68 98 943.0 558.9
– 96 3.117 3.812 – 31 0.3421 0.3061 34 53.20 37.61 99 977.6 578.1
– 95 3.784 · 10–5 4.602 · 10–5 – 30 0.3798 0.3385 35 56.24 39.63 100 1013.2 597.8
– 94 4.584 5.544 – 29 0.4213 0.3739 36 59.42 41.75 101 1050 618.0
– 93 5.542 6.665 – 28 0.4669 0.4127 37 62.76 43.96 102 1088 638.8
– 92 6.685 7.996 – 27 0.5170 0.4551 38 66.26 46.26 103 1127 660.2
– 91 8.049 9.574 – 26 0.5720 0.5015 39 69.93 48.67 104 1167 682.2
– 90 9.672 · 10–5 11.44 · 10–5 – 25 0.6323 0.5521 40 73.78 51.19 105 1208 704.7
– 89 11.60 13.65 – 24 0.6985 0.6075 41 77.80 53.82 106 1250 727.8
– 88 13.88 16.24 – 23 0.7709 0.6678 42 82.02 56.56 107 1294 751.6
– 87 16.58 19.30 – 22 0.8502 0.7336 43 86.42 59.41 108 1339 776.0
– 86 19.77 22.89 – 21 0.9370 0.8053 44 91.03 62.39 109 1385 801.0
– 85 23.53 · 10–5 27.10 · 10–5 – 20 1.032 0.8835 45 95.86 65.50 110 1433 826.7
– 84 27.96 32.03 – 19 1.135 0.9678 46 100.9 68.73 111 1481 853.0
– 83 33.16 37.78 – 18 1.248 1.060 47 106.2 72.10 112 1532 880.0
– 82 39.25 44.49 – 17 1.371 1.160 48 111.7 75.61 113 1583 907.7
– 81 46.38 52.30 – 16 1.506 1.269 49 117.4 79.26 114 1636 936.1
– 80 0.5473 · 10–3 0.6138 · 10–3 – 15 1.652 1.387 50 123.4 83.06 115 1691 965.2
– 79 0.6444 0.7191 – 14 1.811 1.515 51 129.7 87.01 116 1746 995.0
– 78 0.7577 0.8413 – 13 1.984 1.653 52 136.2 91.12 117 1804 1026
– 77 0.8894 0.9824 – 12 2.172 1.803 53 143.0 95.39 118 1863 1057
– 76 1.042 1.145 – 11 2.376 1.964 54 150.1 99.83 119 1923 1089
– 75 1.220 · 10–3 1.334 · 10–3 – 10 2.597 2.139 55 157.5 104.4 120 1985 1122
– 74 1.425 1.550 – 9 2.837 2.328 56 165.2 109.2 121 2049 1156
– 73 1.662 1.799 – 8 3.097 2.532 57 173.2 114.2 122 2114 1190
– 72 1.936 2.085 – 7 3.379 2.752 58 181.5 119.4 123 2182 1225
– 71 2.252 2.414 – 6 3.685 2.990 59 190.2 124.7 124 2250 1262
– 70 2.615 · 10–3 2.789 · 10–3 – 5 4.015 3.246 60 199.2 130.2 125 2321 1299
– 69 3.032 3.218 – 4 4.372 3.521 61 208.6 135.9 126 2393 1337
– 68 3.511 3.708 – 3 4.757 3.817 62 218.4 141.9 127 2467 1375
– 67 4.060 4.267 – 2 5.173 4.136 63 228.5 148.1 128 2543 1415
– 66 4.688 4.903 – 1 5.623 4.479 64 293.1 154.5 129 2621 1456
– 65 5.406 · 10–3 5.627 · 10–3 0 6.108 4.847 65 250.1 161.2 130 2701 1497
– 64 6.225 6.449 1 6.566 5.192 66 261.5 168.1 131 2783 1540
– 63 7.159 7.381 2 7.055 5.559 67 273.3 175.2 132 2867 1583
– 62 8.223 8.438 3 7.575 5.947 68 285.6 182.6 133 2953 1627
– 61 9.432 9.633 4 8.129 6.360 69 298.4 190.2 134 3041 1673
– 60 10.80 · 10–3 10.98 · 10–3 5 8.719 6.797 70 311.6 198.1 135 3131 1719
– 59 12.36 12.51 6 9.347 7.260 71 325.3 206.3 136 3223 1767
– 58 14.13 14.23 7 10.01 7.750 72 339.6 214.7 137 3317 1815
– 57 16.12 16.16 8 10.72 8.270 73 354.3 223.5 138 3414 1865
– 56 18.38 18.34 9 11.47 8.819 74 369.6 232.5 139 3512 1915
– 55 20.92 · 10–3 20.78 · 10–3 10 12.27 9.399 75 385.5 241.8 140 3614 1967
– 54 23.80 23.53 11 13.12 10.01 76 401.9 251.5
– 53 27.03 26.60 12 14.02 10.66 77 418.9 261.4
– 52 30.67 30.05 13 14.97 11.35 78 436.5 271.7
– 51 34.76 33.90 14 15.98 12.07 79 454.7 282.3
– 50 39.35 · 10–3 38.21 · 10–3 15 17.04 12.83 80 473.6 293.3
– 49 44.49 43.01 16 18.17 13.63 81 493.1 304.6
– 48 50.26 48.37 17 19.37 14.48 82 513.3 316.3
– 47 56.71 54.33 18 20.63 15.37 83 534.2 328.3
– 46 63.93 60.98 19 21.96 16.31 84 555.7 340.7
– 45 71.98 · 10–3 68.36 · 10–3 20 23.37 17.30 85 578.0 353.5
– 44 80.97 76.56 21 24.86 18.34 86 601.0 366.6
– 43 90.98 85.65 22 26.43 19.43 87 624.9 380.2
– 42 102.1 95.70 23 28.09 20.58 88 649.5 394.2
– 41 114.5 · 10–3 106.9 · 10–3 24 29.83 21.78 89 674.9 408.6
– 40 0.1283 0.1192 25 31.67 23.05 90 701.1 423.5
– 39 0.1436 0.1329 26 33.61 24.38 91 728.2 438.8
– 38 0.1606 0.1480 27 35.65 25.78 92 756.1 454.5
– 37 0.1794 0.1646 28 37.80 27.24 93 784.9 470.7
– 36 0.2002 0.1829 29 40.06 28.78 94 814.6 487.4

Sources: Smithsonian Meteorological Tables 6th. ed. (1971) and VDI vapor tables 6th ed (1963).
D00
Table XIII: Saturation pressure ps and vapor density % D of water in a temperature range from –100 °C to +140 °C

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Fundamentals of Vacuum Technology Tables, Formulas, Diagrams

Group A 3) Group B 3) Group C 3)

Methane c Ethylene c Hydrogen c

Ethane c Buta-1,3-diene c Acetylene (ethyne) c

Propane c Acrylonitrile c Carbon bisulfide c

Butane c hydrogen cyanide a

Pentane c Dethyl ether (s) c

Hexane c Ethylene oxide (oxiran) c

Heptane c 1.4 Dioxan a

Octane a Tetrahydrofuran a

Cyclohexane c Tetrafluoroethylene a

Propylene (propene) a

Styrene (s) b

Benzene (s) c

Toluene (s) –

Xylene a Legend Group A Group B Group C

Naphthalene – MESG 1) > 0.9 mm 0.5 ... 0.9 mm < 0.5 mm

Methanol (s) c MIC 2) ratio > 0.8 mm 0.45 ... 0.8 mm < 0.45 mm
Ethanol (s) c
1) Minimum Electrical Spark Gap
Propyl alcohol (propanol) c 2) Minimum Ignition Current
The ratio is based on the MIC value for laboratory methane
Butyl alcohol (butanol) a 3) Group allocation:

Phenol – a – according to MESG value


b – according to MIC ratio
Acetaldehyde (ethanal) a c – according to both MESG value and MIC ratio
(s) – solvent
Acetone (s) (propanone) c

Methyl ethyl ketone (s) (propan-2-one) c

Ethyl acetate (s) a

Butyl acetate (s) c

Amyl acetate (s) –

Ethyl methacrylate –

Acetic acid (ethanoic acid) b

Methyl chloride (s) a

Methylene chloride (s) (dichlormethane) –

Ammonia a

acetonitrile a

Aniline –

Pyridine –

Table XIV: Hazard classification of fluids according to their MESG1 and/or MIC2 values. (Extract from European Standard EN 50.014)

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Tables, Formulas, Diagrams Fundamentals of Vacuum Technology

Nitrile-butadiene rubber (NBR) Perbunan

Nitrile-butadiene rubber (NBR) Perbunan


Chloroprene rubber (CR) Neoprene

Chloroprene rubber (CR) Neoprene


Medium Medium

Fluoro rubber (FPM, FKM) Viton

Fluoro rubber (FPM, FKM) Viton


x = resistant x = resistant
– = conditionally resistant – = conditionally resistant
o = not resistant o = not resistant

Silicone rubber

Silicone rubber

Teflon (PTFE)
Teflon (PTFE)

EPDM
EPDM
Acetaldehyde o o o o x x Carbon dioxide, dry x x x x x
Acetic acid (crystalline), pure – o – o x – Carbon dioxide, wet x x x x
Acetic acid, industrial x x Carbon tetrachloride o o o x x o
Acetic acid vapors x x – x Chloracetic acid o o o x x
Acetic acid, 20 % x x x Chlorinated solvents o x

Acetic acid, 50 % o x x x Clorine, dry x x


Acetic acid, 80 % o o x Chlorine water – x o x x
Acetic anhydride – x x x Chlorine, wet o o x x x
Aceto-acetic ester o x – Chlorobromomethane o x –
Acetone o – o x x Chlorobenzene o o o x o

Acetophenone o x x Chloroform o o x x o
Acetylene x – x x Chloromethyl o – x x o
Acrylnitrile – o x Citrus oils o o x
Air, clean x x x x x x Coke furnace gas o o x o
Air, oily x x x x x o Copra oil acid – o – x

Ammonia liquid x x – – x x Cottonseed oil x – x x –


Ammonia gas x x o x Cresol x x o
Amyl acetate o o o x x Crude petroleum – x x o
Amyl alcohol – – o o x x Cyclohexane x x x o
Aniline o o x x x Cyclohexanone o o o x o

Anthracene oil o o x x Cyclohexylamine x o


ASTM oil No. 1 x x x x x o Decahydronaphtalene x x o
ASTM oil No. 2 x x x x x o Desmodur T o o x o
ASTM oil No. 3 – – – o x o Desmophene 2000 x x
Benzaldehyde 100 % x x Dibutylphthalate o o x o x x

Benzene o o x x o Dichlorethylene x
Benzene bromide o o x o Dichlorethane x x x o
Benzoic acid x x Diethylamine – o x x
Bitumen x Diethylene glycol x x x x
Blast furnace gas x x x x – Diethyl ether o – o x o

Boron trifluoride x x x Diethyl ether o o x –


Bromine o o x x Diethyl sebazate o o x –
Butadiene x o Dichlorbenzene o o x o
Butane x – x x o Dichlorbutylene x x o
Butyl acetate o o o x – Diesel oil o – x x o

Butyl alcohol – x – o x x Di-isopropyl ketone o x x


Butyl glykol x x x Dimethyl ether o x x
Butyraldehyde o o x x – Dimethylaniline o o x
Carbolineum o o x x x o Dimethyl formamide o o o x –
Carbon bisulfide o o – x x o Dioctylphthalate o o x x –
D00
Table XV: Chemical resistance of commonly used elastomer gaskets and sealing Table XV: Chemical resistance of commonly used elastomer gaskets and sealing
materials materials

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Fundamentals of Vacuum Technology Tables, Formulas, Diagrams

Nitrile-butadiene rubber (NBR) Perbunan

Nitrile-butadiene rubber (NBR) Perbunan


Chloroprene rubber (CR) Neoprene

Chloroprene rubber (CR) Neoprene


Medium Medium

Fluoro rubber (FPM, FKM) Viton

Fluoro rubber (FPM, FKM) Viton


x = resistant x = resistant
– = conditionally resistant – = conditionally resistant
o = not resistant o = not resistant

Silicone rubber

Silicone rubber
Teflon (PTFE)

Teflon (PTFE)
EPDM

EPDM
Dioxan o o x – Heating fuel oil (coal base) o o x x
Diphenyl o o – x x o Heating fuel oil (petroleum crude base) x – x x o
Diphenyloxyd o x x Heptane x – o x x o
Edenol 888 x x Hexaldehyde o o x x
Essential oils o o – x o Hexane x – o x x o

Ethyl acetate (acetic ether) o o x x Hydraulic fluids


Ethane x – o x x o Hydraulic oils DIN 51524 x – – x x o
Ethyl acetate o o o o x o Phosphoric ester HFD o o o x
Ethyl acrylate o x Polyglycol water HFC x – x x x x
Ethyl alcohol, denatured – – – x Hydrobromic acid o o x x

Ethyl alcohol, pure – – – x x Hydrobromic crystalline acid x x


Ethyl cloride x – o x – Hydrocyanic acid – – x x
Ethylene bromide o o x Hydrogen bromide x
Ethylene chloride x – Hydrogen gas 20 x x – x
Ethylene dichloride o o – x Hydrogen sulfide x x x x

Ethylene glycol x x o x x x Isobutyl alcohol – x x x


Ethyl ether o o o x – Isopropyl acetate o o x –
Ethyl silicate x x x Isopropyl alcohol – x x x
Ethyl acrylate x Isopropyl chloride o o x o
Fatty acids – – x Isopropyl ether o x

Fatty alcohol x x x x – Kerosene – – x x


Fir leaf oil x o x Kerosine x – x x o
Fluorbenzene x o x o Lighting gas – – x x o
Hydrofluoric acid, cold, 5 % x x x Maleic anhydride x
Hydrofluoric acid, cold, pure – x Mercury x x x x

Formaldehyde x – x x x Methane x – x –
Formalin, 55 % x x x x Methane (pit gas) x x x x –
Formic acid – – x – Methylene chloride o o o x o
Formic acid methyl ester o – – x Methyl acrylate o x o
Freon 11 x x o x Methyl alcohol (methanol) – – x o x x

Freon 12 x x – x – Methyl ethyl ketone o o o x –


Freon 22 o x o x x Methyl isobutyl ketone o o x –
Freon 113 x x x x Methyl methacrylate o o o x o
Furane o o x o Methyl salicylate o o x –
Furfurol o o o o x Naphtalene o o x o

Gas oill x – x x o Natural gas – x – x x –


Generator gas x – x x Nitrobenzene o o o x o
Glycerine x x x x x x Nitrous oxide x x x
Glycol x x x x x x Oleic acid x x x o
Halowax oil o o x Orange oil o o x x
Table XV: Chemical resistance of commonly used elastomer gaskets and sealing Table XV: Chemical resistance of commonly used elastomer gaskets and sealing
materials materials

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Tables, Formulas, Diagrams Fundamentals of Vacuum Technology

Nitrile-butadiene rubber (NBR) Perbunan

Nitrile-butadiene rubber (NBR) Perbunan


Chloroprene rubber (CR) Neoprene

Chloroprene rubber (CR) Neoprene


Medium Medium

Fluoro rubber (FPM, FKM) Viton

Fluoro rubber (FPM, FKM) Viton


x = resistant x = resistant
– = conditionally resistant – = conditionally resistant
o = not resistant o = not resistant

Silicone rubber

Silicone rubber

Teflon (PTFE)
Teflon (PTFE)

EPDM
EPDM
Oxygen x x x x Tar oil o x o
Ozone o – x x x x Tetrachlorethylene x x o
Palmitic acid x x x o Tetrahydrofurane o o x o
Palm oil acid – o x x Tetraline o o o x o
Paraffin x x x x o Toluene o o o x x o

Paraffin oil x x x o Transformer oil x x x x o


Pentachlordiphenyl o x x o Train oil o x x –
Pentane x x o x x o Triethanolamine o o x –
Perchloroethylene o o x x o Tributoxyethyl phosphate o o x o
Petrol x – o x o Tributyl phosphate o o o x o

Petrol alcohol 3:1 – o x x Trichloroethane o o x x


Petrol benzene 4:1 x o o x x o Trichloroethylene o o x x o
Petrol benzene 7:3 o o o x x o Trichloroethyl phosphate 20 – x x
Petrol benzene 3:2 o o o x x o Trichloroethyl phosphate 80 o x x
Petrol benzene 1:1 o o o x x o Trichloracetic acid 60 x x –

Petrol benzene 3:7 o o o x x Tricresyl phosphate o x x x –


Petrol benzene spirit 5:3:2 o o o x o Turpentine – – x x o
Phenol o o x x x o Turpentine oil, pure x x x o
Phenyl ethyl ether o o x o Vinyl acetate o o x
Phenylic acid (phenol) o o – – x – Vinylaceto-acetic acid 3:2 o – o o x

Phosphorous chloride o – x x Vinyl chloride, liquid x x x


Phthalic anhydride x x x x Water 50 x x x x x
Piperidine o o x Water 100 x – x x x
Polyglycol x x Wood oil – x
Propane, gas x x x x x Xylamon o o x x o

Propylene oxyde o x – Xylene o o o x x o


Propyl alcohol x x x x
Pydraul F-9 o o x x x
Pydraul AC o x x x
Pydraul A 150 o x x

Pydraul A 200 o x x x
Pyridine o x –
Salicylic acid x x x x
Skydrol 500 x o x x
Skydrol 7000 x x x

Stearic acid – x x
Styrene o o x x o
Sulfur – x x x x x
Sulfur dioxide
Sulfur trioxide, dry
o
o
o

x
x
x
x
x

D00
Table XV: Chemical resistance of commonly used elastomer gaskets and sealing Table XV: Chemical resistance of commonly used elastomer gaskets and sealing
materials materials

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Fundamentals of Vacuum Technology Tables, Formulas, Diagrams

Vacuum symbols Ejector vacuum pump *)


Vacuum chambers
All symbols with the exception of those
marked with *) do not depend on the posi-
Diffusion pump *) Vacuum chamber
tion.
*) These symbols may only be used in the
position shown here (tip of the angle Adsorption pump *) Vacuum bell jar
pointing down)
The symbols for vacuum pumps should Getter pump
always be arranged such that the side with
the constriction is allocated to the higher
Shut-off devices
pressure Sputter-ion pump

Shut-off device, general


Vacuum pumps Cryopump
Shut-off valve, straight-
through valve
Scroll pump *)
Vacuum pump, general
Right-angle valve
Evaporation pump
Piston vacuum pump
Stop cock

Diaphragm vacuum pump


Accessories Three-way stop cock
Rotary positive
Condensate trap, general
displacement pump *)
Right-angle stop cock

Rotary plunger Condensate trap with heat


vacuum pump *) exchanger (e.g. cooled)
Gate valve
Sliding vane rotary
Gas filter, general
vacuum pump *)
Butterfly valve

Rotary piston vacuum pump *) Filtering apparatus, general


Nonreturn valve

Liquid ring vacuum pump *) Baffle, general


Safety shut-off valve

Roots vacuum pump *) Cooled baffle

Turbine vacuum pump, general Cold trap, general Modes of operation


Radial flow vacuum pump Cold trap with coolant reservoir Manual operation

Axial flow vacuum pump Sorption trap Variable leak valve

Turbomolecular pump Throttling Electromagnetic operation

Table XVI: Symbols used in vacuum technology (extract from DIN 28401)

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Tables, Formulas, Diagrams Fundamentals of Vacuum Technology

Hydraulic or pneumatic Linear-motion leadthrough,


operation flange-mounted

Electric motor drive Linear-motion leadthrough,


without flange

Leadthrough for transmission


Weight-operated
of rotary and linear motion

Rotary transmission
leadthrough

Electric current leadthrough


Connections and
piping

Flange connection, general


Measurement and
gauges
Bolted flange connection

General symbol for


Small flange connection vacuum *)

Vacuum measurement, vacu-


Clamped flange connection um gauge head *

Vacuum gauge, operating and


display unit for vacuum gauge
Threaded tube connection
head *)

Ball-and-socket joint Vacuum gauge, recording *)

Vacuum gauge with analog


Spigot-and-socket joint measured-value display *)

Vacuum gauge with digital


Taper ground joint connection measured-value display *)

Intersection of two lines with Measurement of throughput


connection

Intersection of two lines


without connection

Branch-off point

Combination of ducts

Flexible connection
(e.g. bellows, flexible tubing) D00
Table XVI: Symbols used in vacuum technology (extract from DIN 28401)

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Fundamentals of Vacuum Technology Tables, Formulas, Diagrams

Kelvin Celsius Réaumur Fahrenheit Rankine


Boiling point H2O 373 100 80 212 672
Body temperature 37 °C 310 37 30 99 559
Room temperature 293 20 16 68 527
Freezing point H2O 273 0 0 32 492
NaCl/H2O 50:50 255 –18 –14 0 460
Freezing point Hg 34 –39 –31 –39 422
CO2 (dry ice) 195 –78 –63 –109 352
Boiling point LN2 77 –196 –157 –321 170
Absolute zero point 0 –273 –219 –460 0

Conversion in
K °C °R °F °R
Kelvin Celsius Réaumur Fahrenheit Rankine
K 4 9 9
1 K – 273 (K – 273) (K – 273) + 32 K = 1,8 K
Kelvin 5 5 5

°C 4 9 9
°C + 273 1 · °C · °C + 32 (°C + 273)
Celsius 5 5 5

°C
Réaumur
5
4
· °R + 273
5
4
· °R 1
9
4
· °R + 32
5
9 [ 54 (°R + 273)]
°F 5 (°F – 32) + 273 5 (°F – 32) 4 (°F – 32) 1 °F + 460
Fahrenheit 9 9 9

°R
Rankine
5 (°R)
9
5 (°R – 273)
9 [
4 5 (°R – 273)
5 9 ] °R – 460 1

Table XVII: Temperature comparison and conversion table (rounded off to whole degrees)
– p2
V

2
Z

p

ZA
Mean free path λ [cm]

λ∼
1
p

Pressure p [mbar]
Pressure p [mbar]
λ : mean free path in cm (λ ~ 1/p)
n : particle number density in cm–3 (n ~ p)
ZA : area-related impingement rate in cm–3 · s–1 (ZA ~ p2)
ZV : volume-related collision rate in cm–3 · s–1 (ZV ~ p2)

Fig. 9.1: Variation of mean free path λ (cm) with pressure for various gases Fig. 9.2: Diagram of kinetics of gases for air at 20 °C

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Tables, Formulas, Diagrams Fundamentals of Vacuum Technology

106

105
Pressure [mbar]

104

Temperature (K)

conductance [l · cm–1]
103

102

1018
Altitude [km] 6
4

2
Fig. 9.3: Decrease in air pressure (1) and change in temperature (2) as a function of
altitude 100 1 2 4 6 8
10 102 103 104
Pipe length l [cm]

Fig. 9.5: Conductance values for piping of commonly used nominal width with circu-
lar cross-section for laminar flow (p = 1 mbar) according to equation 53a.
(Thick lines refer to preferred DN) Flow medium: air (d, l in cm!)
conductance [l · s–1]
Altitude (km)

Molecules/atoms [cm–3]
Pipe length l [cm]

Fig. 9.6: Conductance values for piping of commonly used nominal width with cir-
D00
cular cross-section for molecular flow according to equation 53b. (Thick
Fig. 9.4: Change in gas composition of the atmosphere as a function of altitude lines refer to preferred DN) Flow medium: air (d, l in cm!)

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Fundamentals of Vacuum Technology Tables, Formulas, Diagrams

pSTART – pend, P
R= pEND – pend, p
pEND – pend, P
mbar
pSTART < 1013 mbar
pSTART = 1013 mbar

Column ➀: Vessel volume V in liters Example 1 with regard to nomogram 9.7: Example 2 with regard to nomogram 9.7:
Column ➁: Maximum effective pumping speed Seff,max A clean and dry vacuum system (qpV,in = 0) with
at the vessel in (left) liters per second or A vessel with the volume V = 2000 l is to be pumped V = 2000 l (as in example 1) is to be pumped down
(right) cubic meters per hour. down from a pressure of pSTART = 1000 mbar to a pressure of pEND = 10-2 mbar. Since this pres-
Column ➂: Pump-down time tp in (top right) seconds (atmospheric pressure) to a pressure of pEND = 10-2 sure is smaller than the ultimate pressure of the
or (center left) minutes or (bottom right) mbar by means of a rotary plunger pump with an rotary piston pump (Seff,max = 60 m3/h = 16.7 l
hours. effective pumping speed at the vessel of ( s-1 = 3 · 10-2 mbar), a Roots pump must be used
Seff,max = 60 m3/h = 16.7 l · s-1. The pump-down time in connection with a rotary piston pump. The former
Column ➃: Right: can be obtained from the nomogram in two steps: has a starting pressure of p1 = 20 mbar, a pumping
Pressure pEND in millibar at the END of the
speed of Seff,max = 200 m3/h – 55 l · s-1 as well as
pump-down time if the atmospheric 1) Determination of τ: A straight line is drawn pult,p – 4 · 10-3 mbar. From pstart = 1000 mbar to p =
pressure pSTART ( pn = 1013 prevailed at the through V = 2000 l (column ➀) and Seff = 60 m3/h-1 20 mbar one works with the rotary piston pump and
START of the pump-down time. The desired = 16.7 l · s-1 (column ➁) and the value t = 120 s then connects the Roots pump from p1 = 20 mbar to
pressure pEND is to be reduced by the = 2 min is read off at the intersection of these straight pEND = 10-2 mbar, where the rotary piston pump acts
ultimate pressure of the pump pult,p and the lines with column ➂ (note that the uncertainty of this as a backing pump. For the first pumping step one
differential value is to be used in the co- procedure is around ∆τ = ± 10 s so that the relative obtains the time constant τ = 120 s = 2 min from the
lumns. If there is inflow qpV,in, the value uncertainty is about 10 %). nomogram as in example 1 (straight line through
pend – pult,p – qpV,in / Seff,max is to be used
V = 2000 l, Seff = 16.7 l · s-1). If this point in
in the columns. 2) Determination of tp: The ultimate pressure of the column ➂ is connected with the point
Left: rotary pump is pult,p = 3 · 10-2 mbar, the apparatus is p1 - pult,p = 20 mbar – 3 · 10-2 mbar = 20 mbar (pult,p
Pressure reduction ratio R = (pSTART – pult,p clean and leakage negligible (set qpV,in = 0); this is is ignored here, i.e. the rotary piston pump has a
– qpV,in / Seff,max)/(pend – pult,p – qpV,in / pSTART – pult,p = 10-1 mbar – 3 · 10-2 mbar = 7 · 10-2 constant pumping speed over the entire range from
Seff,max), if the pressure pSTART prevails at mbar. Now a straight line is drawn through the point 1000 mbar to 20 mbar) in column 5, one obtains tp,1
the beginning of the pumping operation found under 1) t = 120 s (column ➂) and the point = 7.7 min. The Roots pump must reduce the
and the pressure is to be lowered to pEND pEND – pult,p = 7 · 10-2 mbar (column ➄) and the pressure from p1 = 20 mbar to pEND = 10-2 mbar, i.e.
by pumping down. intersection of these straight lines with column ➃ the pressure reduction ratio R = (20 mbar – 4 · 10-3
The pressure dependence of the pumping tp = 1100 s = 18.5 min is read off. (Again the relative mbar) / (10-2 mbar-4 · 10-3) = 20/6 · 10-3 mbar =
speed is taken into account in the nomo- uncertainty of the procedure is around 10 % so that 3300.
gram and is expressed in column ➄ by the relative uncertainty of tp is about 15 %.) Taking The time constant is obtained (straight line V = 2000
pult,p. If the pump pressure pult,p is small in into account an additional safety factor of 20 %, l in column ➀, Seff = 55 l · s–1 in column ➁) at = 37
relation to the pressure pend which is one can assume a pump-down time of s (in column ➂). If this point in column ➂ is
desired at the end of the pump-down tp = 18.5 min · (1 + 15 % + 20 %) connected to R = 3300 in column ➄, then one
operation, this corresponds to a constant = 18.5 min · 1.35 = 25 min. obtains in column ➃ tp, 2 = 290 s = 4.8 min. If one
pumping speed S or Seff during the entire takes into account tu = 1 minfor the changeover
pumping process. time, this results in a pump-down time of
tp = tp1 + tu + tp2 = 7.7 min + 1 min + 4.8 min = 13.5 min.
Fig. 9.7: Nomogram for determination of pump-down time tp of a vessel in the rough vacuum pressure range

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Tables, Formulas, Diagrams Fundamentals of Vacuum Technology

Conductance for molecular flow


Correction factor for short tubes
Tube length

Tube diameter

Example: What diameter d must a 1.5-m-long pipe have so tubes, is taken into account by means of a correction factor
that it has a conductance of about C = 1000 l / sec in the α. For d / l < 0.1, α can be set equal to 1. In our example
region of molecular flow? The points l = 1.5 m and C = 1000 d/l = 0.16 and α = 0.83 (intersection point of the straight line
l/sec are joined by a straight line which is extended to inters- with the a scale). Hence, the effective conductance of the
ect the scale for the diameter d. The value d = 24 cm is obtai- pipeline is reduced to C · α = 1000 · 0.83 = 830 l/sec. If d
ned. The input conductance of the tube, which depends on is increased to 25 cm, one obtains a conductance of
the ratio d / l and must not be neglected in the case of short 1200 · 0.82 = 985 l / sec (dashed straight line).

D00
Fig. 9.8: Nomogram for determination of the conductance of tubes with a circular cross-section for air at 20 °C in the region of molecular flow (according to J. DELAFOSSE and
G. MONGODIN: Les calculs de la Technique du Vide, special issue “Le Vide”, 1961)

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Fundamentals of Vacuum Technology Tables, Formulas, Diagrams

C
Air 20 °C

Correction factor for higher pressures


Pressure [mbar]

Pressure [mbar]

Uncorrected conductance for mol. flow [m3 · h–1]


conductance [ l · s–1]
Laminar flow

Tube internal diameter [cm]


Tube length [meters]

Clausing factor
Knudsen flow
Mol. flow

Procedure: For a given length (l) and internal dia- Example: A tube with a length of 1 m and an internal In a tube with a length of 1 m and an internal dia-
meter (d), the conductance Cm, which is indepen- diameter of 5 cm has an (uncorrected) conductance meter of 5 cm a molecular flow prevails if the mean
dent of pressure, must be determined in the mole- C of around 17 l/s in the molecular flow region, as pressure p in the tube is < 2.7 · 10-3 mbar.
cular flow region. To find the conductance C* in determined using the appropriate connecting lines To determine the conductance C* at higher
the laminar flow or Knudsen flow region with a between the “l” scale and the “d” scale. The conduc- pressures than 2.7 · 10-3 mbar, at 8 · 10-2 mbar
given mean pressure of p in the tube, the conduc- tance C found in this manner must be multiplied (= 6 · 10-2 torr), for example, the corresponding
tance value previously calculated for Cm has to be by the clausing factor γ = 0.963 (intersection of point on the p scale is connected with the point
multiplied by the correction factor a determined in connecting line with the γ scale) to obtain the true d = 5 cm on the “d” scale. This connecting line
the nomogram: C* = Cm · α. conductance Cm in the molecular flow region: intersects the “a“ scale at the point α = 5.5.
Cm · γ = 17 · 0.963 = 16.37 l/s. The conductance C* at p = 8 · 10-2 mbar is:
C* = Cm · α = 16.37 · 5.5 = 90 l/s.

Fig. 9.9: Nomogram for determination of conductance of tubes (air, 20 °C) in the entire pressure range

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Tables, Formulas, Diagrams Fundamentals of Vacuum Technology

[m3 · h–1] Pumping speed


Volume V [min3]
Pump-down time t [min]

2
Example

ple 1
Exam
Gas evolution [mbar · l · s–1 · m–2]

weak

normal

strong

Area F [m2]

The nomogram indicates the relationship between the surface area concerned of 100 m2 and a gas evo- 70 m3 (C) on the volume scale: the extension results
the nominal pumping speed of the pump, the cham- lution of 2 · 10-3 mbar · l · s-1 · m-2 result in an inters- in the intersection point at 30 min (E) on the time
ber volume, size and nature of the inner surface as ection point A, which is joined to point B by an scale.
well as the time required to reduce the pressure upward sloping line and then connected via a vertical
from 10 mbar to 10-3 mbar. line to the curve that is based on the pumping speed In example 2 one has to determine what
of the pump of 1300 m3/h (D). If the projection to the pumping speed the pump must have if the vessel
Example 1: A given chamber has a volume of 70 m3 curve is within the marked curve area (F), the pum- (volume = approx. 3 m3) with a surface area
and an inner surface area of 100 m2; a substantial ping speed of the pump is adequate for gas evoluti- of 16 m2 and a low gas evolution of
gas evolution of 2 · 10-3 mbar · l · s-1 · m-2 is assu- on. The relevant pump-down time (reduction of pres- 8 · 10-5 mbar · l · s-1 · m-2 is to be evacuated from
med. The first question is to decide whether a pump sure from 10 mbar to 10-3 mbar) is then given as 10 mbar to 10-3 mbar within a time of 10 min. The
with a nominal pumping speed of 1300 m3/h is 30 min on the basis of the line connecting the point nomogram shows that in this case a pump with a
generally suitable in this case. The coordinates for 1300 m3/h on the pumping speed scale to the point nominal pumping speed of 150 m3/h is appropriate.

D00
Fig. 9.10: Determination of pump-down time in the medium vacuum range taking into account the outgasing from the walls

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Fundamentals of Vacuum Technology Tables, Formulas, Diagrams

1000
1,00E+03

Mercury
100
1,00E+02

Halocarbon 11 10
1,00E+01

Halocarbon 12
Vapor pressure [mbar]

1
Halocarbon 13 1,00E+00
Santovac 5
(similar to Ultralen)
Halocarbon 22 10-1
1,00E-01
Aziepon 201

Vapor pressure (mbar)


10-2
1,00E-02

Trichorethylene
Acetone 10-3
1,00E-03
DC 704 Diffelen ultr a

10-4
1,00E-04

10-5
1,00E-05

1,00E-06 -6
10 DC 705

1,00E-07-7
10
Diffelen
light
Temperature [°C]
1,00E-08-8
10
Diffelen
normal
Fig. 9.11: Saturation vapor pressure of various substances 1,00E-09-9
10

10 -10
1,00E-10

10-11
1,00E-11

10-12
1,00E-12

0 25 50 75 100 150 200 250


Temperature (°C)

Fig. 9.12: Saturation vapor pressure of pump fluids for oil and mercury fluid
entrainment pumps
Temperature [°C]
Temperature [K]

Vapor pressure
Fig. 9.13: Saturation vapor pressure of major metals used in vacuum technology

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Tables, Formulas, Diagrams Fundamentals of Vacuum Technology


Vapor pressure [mbar]

p critical point
P melting point

Temperature [°C]
1 NBR (Perbunan) 2 Silicone rubber 3 Teflon

Fig. 9.14: Vapor pressure of nonmetallic sealing materials (the vapor pressure curve Fig. 9.15: Saturation vapor pressure ps of various substances relevant for
for fluoro rubber lies between the curves for silicone rubber and Teflon) cryogenic technology in a temperaturerange of T = 2 – 80 K

Ultrahigh vacuum High vacuum Medium vacuum Rough vacuum


<10–7 mbar 10–7 to 10–3 mbar 10–3 to 1 mbar 1 to approx. 103 mbar
<10–5 Pa 10–5 to 10–1 Pa 10–1 to 102 Pa 102 to approx. 105 Pa

Piston vacuum pump

Diaphragm vacuum pump

Liquid-ring vacuum pump

Sliding-vane rotary vacuum pump

Multiple-vane rotary vacuum pump

Trochoide vacuum pump

Rotary plunger vacuum pump

Roots vacuum pump

Turbine vacuum pump

Gaseous-ring vacuum pump

Turbomolecular pump
Liquid jet vacuum pump

Vapor jet vacuum pump

Diffusion pump

Diffusion ejector pump

Adsorption pump

Submilation pump

Sputter-ion pump

Cryopump

10–14 10–13 10–12 10–11 10–10 10–9 10–8 10–7 10–6 10–5 10–4 10–3 10–2 10–1 100 101 102 103

Working range for special model or special operating data


p in mbar →
Normal working range
D00
Fig. 9.16: Common working ranges of vacuum pumps

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Fundamentals of Vacuum Technology Tables, Formulas, Diagrams

Ultrahigh vacuum High vacuum Medium vacuum Rough vacuum


<10–7 mbar 10–7 to 10–3 mbar 10–3 to 1 mbar 1 to approx. 103 mbar
<10–5 Pa 10–5 to 10–1 Pa 10–1 to 102 Pa 102 to approx. 105 Pa

Pressure balance

Spring element vacuum gauge

Bourdon vacuum gauge

Diaphragm vacuum gauge

Capacitance diaphragm vacuum gauge

Piezoelectric vacuum gauge

Liquid level vacuum gauge

U-tube vacuum gauge

Compression vacuum gauge

(McLeod vacuum gauge)

Decrement vacuum gauge

Thermal conductivity vacuum gauge

Pirani vacuum gauge

Thermocouple vacuum gauge

Bimetallic vacuum gauge

Thermistor vacuum gauge

Cold-cathode ionization vacuum gauge

Penning ionization vacuum gauge

Magnetron gauge

Hot-cathode ionization vacuum gauge

Triode ionization vacuum gauge for medium vacuum

Triode ionization vacuum gauge for high vacuum

Bayard-Alpert ionization vacuum gauge

Bayard-Alpert ionization vacuum gauge with modulator

Extractor vacuum gauge

Partial pressure vacuum gauge

10–14 10–13 10–12 10–11 10–10 10–9 10–8 10–7 10–6 10–5 10–4 10–3 10–2 10–1 100 101 102 103
p in mbar →
The customary limits are indicated in the diagram.

Working range for special models or special operating data

Fig. 9.16a: Measurement ranges of common vacuum gauges

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Tables, Formulas, Diagrams Fundamentals of Vacuum Technology

Saturated vapor

Fig. 9.17: Specific volume Vsp of saturated water vapor in m3/kg within a range of 0.013 to 133 mbar

D00
Fig. 9.18: Breakdown voltage U between parallel electrodes in a homogeneous electrical field as a function of gas
pressure p distance between electrodes d (in mm) (Paschen curve), for air

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Fundamentals of Vacuum Technology Tables, Formulas, Diagrams

SOLID liquid

Evaporation

Melting

Triple point
(0.01°C, 6.09 mbar)
Water vapor pressure [mbar]

Sublimation

GASEOUS

Temperature [°C]

Fig. 9.19: Phase diagram of water

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Statutory Units Fundamentals of Vacuum Technology

10. The statutory the units now to be used, including the SI


units (see below) and legally permissible
Detailed descriptions are provided in publi-
cations by W. Haeder and E. Gärtner (DIN),
units used in units derived from them. The list is follo-
wed by a number of remarks in Section
by IUPAP 1987 and by S. German, P. Draht
(PTB). These should always be referred to
vacuum 10.3. The purpose of the remarks is, on the
one hand, to establish a connection with
if the present summary tailored to vacuum
technology leaves any questions open.
technology previous practice wherever this is neces-
sary and, on the other hand, to provide
explanations on practical use of the con-
10.1 Introduction tent of the alphabetical list.
The statutory units for measurements are
Two federal German laws and the related
implementing provisions stipulate which
based on the seven basic SI units of the 10.2 Alphabetical list 1)
Système International (SI).
units must be used for measurements of variables,
today (generally since January 1, 1978) in Statutory units are:
business and official documents and com- symbols and units
a) the basic SI units (Table 10.4.1)
munications. The provisions resulted in a
b) units derived from the basic SI units, in
frequently used in
number of fundamental changes that also
have to be taken into account in vacuum some cases with special names and unit vacuum technology
technology. Many of the units commonly symbols (Tables 10.4.2 and 10.4.4)
used in the past, such as torr, gauss, stan-
and its
c) units used in atomic physics (Table
dard cubic meter, atmosphere, poise, kilo- 10.4.3) applications (see
calorie, kilogram-force, etc., are no longer
permissible. Instead, other units are to be d) decimal multiples and decimal parts of also DIN 28 402)
used, some of which are new while others units, some with special names
1)
were previously used in other fields. The Examples: 105 N ( m-2 = 1 bar)
The list is based on work done by Prof. Dr. I.
alphabetical list in Section 10.2 contains Lückert, for which we would like to express our
1 dm3 = 1 l (liter) gratitude
the major variables relevant for vacuum 103 kg = 1 t (ton)
technology along with their symbols and

No. Variable Symbol SI- Preferred statutory No. of remark Notes


unit units in Section 10.3
1 Activity (of a radioactive substance) A s–1 (Bq) s–1 3/1
2 (General gas constant) – see no. 73
3 Work W J J, kJ, kWh, Ws
4 Atomic mass mu kg kg, mg see Table V in Sect. 9
5 Avogadro constant NA mol–1 mol–1
6 Acceleration a m · s–2 m · s–2, cm · s–2
7 Boltzmann constant k J · K–1 j · K–1, mbar · l · K–1 see Table V in Sect. 9
8 Celsius temperature ϑ (theta) – °C 3/2
9 Vapor pressure pv N · m–2, Pa mbar, bar 3/3 Pa = Pascal
10 Time t s s, min, h see Table 10.4.4
11 Density (gas density) ρ (ro) kg · m–3 kg · m–3, g · cm–3 3/6
12 Dielectric constant ε (epsilon) F · m–1 F · m–1, As · V–1 · m–1 F = Farad
13 Diffusion coefficient D m2 · s–1 m2 · s–1, cm2 · s–1
14 Moment of momentum L N·s·m N·s·m
15 Torque M N·m N · m, kN · m
16 Rotational speed,
rotational frequency n, f s–1 s–1, min–1
17 Pressure in fluids p N · m–2, Pa bar, mbar 3/3 Pa = Pascal
18 Pressure as mechanical stress p N · m–2, Pa N · mm–2 3/4
19 Diameter d m cm, mm
20 Dynamic viscosity η (eta) Pa · s mPa · s 3/5
21 Effective pressure pe N · m–2, Pa mbar 3/3 see also no. 126
22
23
Electric field strength
Electrical capacitance
E
C
V · m–1
F
V · m–1
F, µF, pF F = Farad
D00
24 Electrical conductivity σ (sigma) S · m–1 S · m–1

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Fundamentals of Vacuum Technology Statutory Units

No. Variable Symbol SI unit Preferred statutory No. of remark Notes


units in Section 10.3
25 Electrical conductance G S S S = Siemens
26 Electrical voltage U V V, mV, kV
27 Electric current density S A · m–2 a · m–2, A · cm–2
28 Electric current intensity I A A, mA, µA
29 Electrical resistance R Ω (ohm) Ω , kΩ , MΩ
30 Quantity of electricity (electric charge) Q C C, As C = Coulomb
31 Electron rest mass me kg kg, g see Table V in Sect. 9
32 Elementary charge e C C, As
33 Ultimate pressure pult N · m–2, Pa mbar
34 Energy E J J, kJ, kWh, eV J = Joule
35 Energy dose D J · k–1 3/5 a
36 Acceleration of free fall g m · s–2 m · s–2 see Table V in Sect. 9
37 Area A m2 m2, cm2
38 Area-related impingement rate ZA m–2 · s–1 m–2 · s–1; cm–2 · s–1
39 Frequency f Hz Hz, kHz, MHz
40 Gas permeability Qperm m3 (NTP) cm3 (NTP) 3/19 d =day (see Tab. 10.4.4
–––––––––– ––––––––––
m2 · s · Pa m2 · d · bar see no. 73 and no. 103)
41 Gas constant R
42 Velocity v m · s–1 m · s–1, mm · s–1, km · h–1
43 Weight (mass) m kg kg, g, mg 3/6
44 Weight (force) G N N, kN 3/7
45 Height h m m, cm, mm
46 Lift s m cm see also no. 139
47 Ion dose J C · kg–1 c · kg–1, C · g–1 3/8
48 Pulse ^p (b) N·s N·s
49 Inductance L H H, mH H = Henry
50 Isentropic exponent κ (kappa) – – κ = cp · cv–1
51 Isobaric molar heat capacity Cmp J · mol–1 · K–1 J · mol–1 · K–1
52 Isobaric specific heat capacity cp J · kg–1 · K–1 J · kg–1 · K–1
53 Isochore molar heat capacity Cmv J · mol–1 · K–1
54 Isochore specific heat capacity cv J · kg–1 · K–1 J · kg–1 · K–1
55 Kinematic viscosity ν (nü) m2 · s–1 mm2 · s–1, cm2 · s–1 3/9
56 Kinetic energy EK J J
57 Force F N N, kN, mN 3/10 N = Newton
58 Length l m m, cm, mm 3/11
59 Linear expansion coefficient α (alpha) m m
––––– –––––––– ; K–1
m·K m·K
60 Leak rate QL N · m · s–1 mbar · l ; cm3 3/12
––––––– –––– (NTP)
s s
61 Power P W W, kW, mW
62 Magnetic field strength H A · m–1 A · m–1 3/13
63 Magnetic flux density B T T 3/14 T = Tesla
64 Magnetic flux Φ (phi) Wb, V · s V·s 3/15 Wb = Weber
65 Magnetic induction B T T see no. 63
66 Mass m kg kg, g, mg 3/6
67 Mass flow rate qm kg · s–1 kg · s–1, kg · h–1, g · s–1
68 Mass content wi kg · kg–1 %, o/oo, ppm ppm = parts per million
69 Mass concentration ρi (ro-i) kg · m–3 kg · m–3, g · m–3, g · cm–3
70 Moment of inertia J kg · m2 kg · m2
71 Mean free path λ m m, cm
72 Molality bi mol · kg–1 mol · kg–1
73 Molar gas constant R J mbar · l see Table V in Sect. 9
–––––––––– ––––––––––
mol · K mol · K
74 Molar mass (quantity-related mass) M kg mol–1 kg · kmol–1, g · mol–1

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Statutory Units Fundamentals of Vacuum Technology

No. Variable Symbol SI unit Preferred statutory No. of remark Notes


units in Section 10.3
75 Molar volume Vm m3 · mol–1 m3 · mol–1, l · mol–1
76 Molar volume, standard Vmn m3 · mol–1 m3 · mol–1 (NTP) see Table V in Sect. 9
l · mol–1 (NTP)
77 Molecular mass m kg g
78 Normal stress (mech.) σ (sigma) N · m–2 N · mm–2
79 Standard density of a gas ρn (ro-en) kg · m–3 kg · m–3, g · cm–3
80 Standard pressure pn N · m–2, Pa mbar see Table V in Sect. 9
81 Standard volume Vn m3 m3 (NTP), cm3 (NTP) 3/16
82 Partial pressure pi N · m–2, Pa mbar 3/17
83 Period T s s, ms, µs
84 Permeation coefficient P m3 · m cm2 3/18
––––––––– ––––––––
s · m2 · bar s · mbar
85 Planck constant h J·s J·s see Table V in Sect. 9
86 pV throughput qpV N · m · s–1 mbar · l · s–1 3/19
87 pV value pV N·m mbar · l 3/19
88 Radius (also molecular radius) r m cm, mm, µm
89 Space charge density ρ (ro) C · m–3 C · m–3, As · m–3
90 Solid angle Ω (omega) sr sr sr = steradian
91 Relative atomic mass AT – – 3/20 nondimensional variab.
92 Relative molecular mass Mr – – 3/21 nondimensional variab.
93 Relative particle mass Mr – – nondimensional variab.
94 Residual vapor pressure prd N · m–2, Pa mbar
95 Residual gas pressure prg N · m–2, Pa mbar
96 Residual (total) pressure pr N · m–2, Pa mbar
97 Reynold number nondimensional Re – – nondimensional variab.
variable
98 Saturation vapor pressure ps N · m–2, Pa mbar
99 Throughput (of a pump) qpV, Q N · m · s–1 mbar · l · s–1
100 Pumping speed S m3 · s–1 m3 · h–1, l · s–1 see no. 132
101 Stress (mech.) ρ, σ, τ N · m–2 N · m–2, N · mm–2 3/4 see no. 18
(ro,
sigma, tau)
102 Specific electron charge –e · me–1 C · kg–1 C · kg–1, As · kg–1 see Table V in Sect. 9
103 Specific gas constant Ri J · kg–1 · K–1 mbar · l 3/22
––––––––
kg · K
104 Specific ion charge e · m–1 C · kg–1 C · kg–1, As · kg–1
105 Specific electrical resistance ρ (ro) Ω·m Ω · cm, Ω · mm2 · m–1
106 Specific volume v m3 · kg–1 m3 · kg–1; cm3 · g–1
107 Specific heat capacity c J · kg–1 · K–1 J · kg–1 · K–1, J · g–1 · K–1 3/23
108 Stefan-Boltzmann constant s (sigma) W W see Table V in Sect. 9
–––––– ––––––
m2 · K4 m2 · K4
109 Quantity of substance ν (nü) mol mol, kmol
110 Throughput of substance qv mol · s–1 mol · s–1
111 Concentration of substance ci mol · m–3 mol · m–3, mol · l–1 for substance “i”
112 Collision rate Z s–1 s–1
113 Conductance C, German: L m3 · s–1 m3 · s–1, l · s–1
114 Flow resistance R s · m–3 s · m–3, s · l–1
115 Number of particles N – – nondimensional variab.
116 Particle number density (volume-related) n m–3 cm–3
117 Particle number density (time-related) qN s–1 s–1 see no. 120
118
119
Particle throughput density
Particle mass
jN
m
m–2 · s–1
kg
m–2 · s–1, cm–2 · s–1
kg, g
see no. 121
D00
120 Particle flux qN s–1 s–1 see no. 117

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Fundamentals of Vacuum Technology Statutory Units

No. Variable Symbol SI unit Preferred statutory No. of remark Notes


units in Section 10.3
121 Particle flux density jN m–2 · s–1 m–2 · s–1, cm–2 · s–1 see no. 118
122 Thermodyn. temperature T K K, mK
123 Temperature difference ∆T, ∆ϑ K K, °C 3/24
124 Temperature conductivity a m2 · s–1 a = λ · ρ–1 · cp
125 Total pressure pt N · m–2, Pa mbar 3/3
126 Overpressure pe N · m–2, Pa mbar 3/3
127 Ambient pressure Pamb N · m–2, Pa mbar, bar 3/3
128 Speed of light in vacuum c m · s–1 m · s–1, km · s–1 see Table V in Sect. 9
129 Evaporation heat Ld J kJ
130 Viscosity, dynamic η (eta) Pa · s mPa · s see no. 20
131 Volume V m3 m3, l, cm3
132 Volume throughput (volumetric flow) qv m3 · s–1 m3 · h–1, l · s–1
133 Volume concentration σi m3 · m–3 l · l–1, %, o/oo, ppm ppm = parts per million
(sigma-i)
134 Volume-related collision rate Zv s–1 · m–3 s–1 · m–3, s–1 · cm–3
135 Quantity of heat Q J J, kJ, kWh, Ws 3/25
136 Heat capacity C J · K–1 J · K–1, kJ · K–1
137 Thermal conductivity λ W W
––––– ––––––
(lambda) K·m K·m
138 Heat transfer coefficient α (alpha) W
––––––
K · m2
139 Path length s m m, cm
140 Wave length λ (lambda) m nm 3/11
141 Angle (plane) α, β, γ rad rad rad, °, ‘, ‘’ 3/26 rad = radian
(alpha,
beta, gamma)
142 Angular acceleration α (alpha) rad · s–2 rad · s–2
143 Angular velocity ω (omega) rad · s–1 rad · s–1
144 Efficiency η (eta) – – nondimensional variab.
145 Time t s s, min, h, nn, mn see Table 10.44
146 Period of time t, ∆t s s, min, h see Table 10.44

10.3 Remarks on bar (1 bar = 0.1 MPA = 105 Pa) is stated gnated as overpressure pe: pe = p – pamb.
The overpressure can have positive or
in addition to the (derived) SI unit,
alphabetical list 1 Pa = 1 N · m-2, as a special name for one negative values.
in Section 10.2 tenth of a megapascal (Mpa). This is in
Conversions
accordance with ISO/1000 (11/92), p. 7.
3/1: Activity Accordingly the millibar (mbar), a very 1 kg · cm-2 = 980.665 mbar = 981 mbar
The unit previously used was curie (Ci). useful unit for vacuum technology, is also 1 at (technical atmosphere) =
permissible: 1 mbar = 102 Pa = 0.75 torr. 980.665 mbar = 981 mbar
1 Ci = 3.7 · 1010 · s-1 = 37 ns-1 The unit “torr” is no longer permissible.
1 atm (physical atmosphere) =
3/2: (°C) Celsius temperature Special note 1013.25 mbar = 1013 mbar
The term degrees Celsius is a special name Exclusively absolute pressures are measu- 1 atmosphere above atmospheric pressure
for the SI unit kelvin (K) [see no. 122] for red and used for calculations in vacuum (atmospheric overpressure) =
indicating Celsius temperatures. The term technology. 2026.50 mbar = 2 bar
degrees Celsius is legally approved.
In applications involving high pressures, 1 atm
3/3: Pressure frequently pressures are used that are 1 torr = 1 mm Hg = –––––– = 1
760
The revised version of DIN 1314 must based on the respective atmospheric pres-
be complied with. The specifications of sure (ambient pressure) pamb. According 33.322 Pa= 1.333 mbar
this standard primarily apply to fluids to DIN 1314, the difference between a
pressure p and the respective atmospheric 1 meter head of water = 9806.65 Pa =
(liquids, gases, vapors). In DIN 1314,
pressure (ambient pressure) pamb is desi- 98 mbar

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Statutory Units Fundamentals of Vacuum Technology

1 mm Hg = 133.332 Pa = 1.333 mbar = 3/10: Force 3/18: Gas permeability


4/3 mbar The dyne, the CGS unit for force, is no lon- The permeation coefficient is defined as
ger used. the gas flow m3 · s-1 (volumetric flow pV)
The pressure as mechanical stress
that goes through a fixed test unit of a
(strength) is generally given in pascal (Pa) 1 dyne = 10-5 N
given area (m2) and thickness (m) at a
and in N · nm–2. given pressure difference (bar).
3/11: Length/wavelength According to DIN 53.380 and DIN 7740,
Conversions: The unit Ångström (Å) (e.g. for wave- Sheet 1, supplement, the gas permeability
1 Pa = 1 N · m–2 = 10–6 N · mm–2 length) will no longer be used in future (see no. 40) is defined as “the volume of a
(see Table 4.6). gas, converted to 0 °C and 760 torr, which
1 kg · cm–2 = 98,100 Pa = 0.981 N · mm–2 goes through 1 m2 of the product to be
= 0,1 N mm–2 1 Å = 10-8 cm = 0.1 nm
tested at a certain temperature and a cer-
1 kg · mm–2 = 9,810,000 Pa = tain pressure differential during a day
9.81 N · mm–2 = 10 N · mm–2 3/12: Leak rate (= 24 hours)”.
In DIN 40.046 sheet 102 (draft of August
1973 issue), the unit mbar · dm3 · s-1
3/5: Dynamic viscosity (= mbar · l · s-1) is used for the leak rate. 3/19: pV throughput/pV value
The unit previously used was poise (P). Note that the leak rate corresponding DIN 28.400, Sheet 1 is to be taken into
to the unit 1 mbar · l · s-1 at 20 °C is account here. No. 86 and no. 87 have a
1 P = 0.1 Pa · s = 1 g · cm–1 · s–1 quantitative physical significance only if
practically the same as the leak rate
1 cm3 · s-1 (NTP). (See also 3/17) the temperature is indicated in each case.
3/5a: Energy dose
Rad (rd) is no longer permissible.
3/13: Magnetic field strength 3/20: Relative atomic mass
1 The previously used unit was the oersted Misleadingly called “atomic weight” in the
1 rd = –––– J · kg–1 (Oe). past!
100
1 Oe = 79.577 A · m-1
3/6: Weight
DIN 1305 is to be complied with in this 3/21: Relative molecular mass
context. Because of its previous ambiva- 3/14: Magnetic flux density Misleadingly called “molecular weight” in
lence, the word weight should only be The previously used unit was the gauss the past!
used to designate a variable of the nature (G).
of a mass as a weighing result for indica-
ting quantities of goods. 1 G = 10-4 Vs · m-2 = 10-4 T (T = Tesla) 3/22: Specific gas constant
As mass-related gas constant of the
The designations “specific weight” and
substance “i”. Ri = Rm ( Mi-1; Mi molar
“specific gravity” should no longer be 3/15: Magnetic flux mass (no. 74) of the substance “i”. See
used. Instead, one should say density. The previously used unit was the maxwell also DIN 1345.
(M).
1 M = 10-8 Wb (Weber)
3/7: Weight force 3/23: Specific heat capacity
See DIN 1305. The previous units pond (p) Also called specific heat:
and kilopond, i.e. kilogram-force, (kp) as 3/16: Standard volume
well as other decimal multiples of p are no Specific heat (capacity) at constant
DIN 1343 must be complied with. pressure: cp.
longer used.
The designation m3 (NTP) or m3 (pn, Tn) Specific heat (capacity) at constant
1 kp = 9.81 N is proposed, though the expression in volume: cV.
parentheses does not belong to the unit
symbol m3 but points out that it refers to
3/8: Ion dose the volume of a gas in its normal state
The previously used unit was the Röntgen 3/24: Temperature difference
(Tn = 273 K, pn = 1013 mbar). Temperature differences are given in K,
(R). 1 R = 2,58 · 10–4 C · kg–1
but can also be expressed in °C. The
designation degrees (deg) is no longer
3/17: Partial pressure permissible.
3/9: Kinematic viscosity
The index “i” indicates that it is the partial
The previously used unit was stokes (St).
pressure of the “i-th” gas that is contained
1 St = 1 cm2 · s–1; 1 cSt = 1 mm2 · s–1 in a gas mixture. D00

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Fundamentals of Vacuum Technology Statutory Units

3/25: Quantity of heat 10.4.2 Derived coherent 1) SI 10.4.3 Atomic units


The units calorie (cal) and kilocalorie (kcal)
are no longer be used.
units with special names
Basic unit Symbol Vartiable
and symbols ————————————————
1 kcal = 4.2 kJ (alphabetical) Atomic Mass for
indication of
Name Symbol Variable Relationship mass mu particle mass;
3/26: Angle of unit
1 radian (rad) is equal to the plane angle ———————————————————— unit 1 mu = 1/12 mass
which, as the central angle of a circle, cuts coulomb C quantity of of 12C
out an arc having a length of 1 m from the electricity also amu
circle. See also DIN 1315 (8/82). or electric (atomic mass
charge 1C=1A·s
π unit).
farad F electrical
1° = ––––– rad: 1’ = 1°/60; 1’’ = 1’/60. Electron eV energy
180 capacitance 1 F = 1 A · s · V–1
volt
henry H inductance 1 H = 1 V · s · A–1
360° hertz Hz frequency 1 Hz = 1 · s–1
1 rad = ––––– · 60°
2π joule J energy, work, 1 J = 1 N · m
quantity = Ws
of heat
10.4.4 Derived noncoherent
lumen lm luminous flux 1 lm = cd · sr
SI units with special
lux lx illuminance 1 lx = 1 lm · m–2
names and symbols
newton N force 1 N = 1 kgm · s–2
10.4 Tables ohm Ω electrical 1 Ω = 1 V · A–1 Basic unit Symbol Definition
resistance ————————————————
pascal Pa pressure, 1 Pa = 1 N · m–2 Day d 1 d = 86.400 s
10.4.1 Basic SI units mechanical
stress
Hour h 1 h = 3.600 s
radian rad 2) angle, 1 rad = 1 m · m–1 Minute min 1 min = 60 s
Basic unit Symbol Variable plane angle
Round angle – 2 p rad
———————————————— siemens S electrical
meter m length conductance 1 S = 1 · Ω–1 π
kilogramm kg mass Degree (°) –––– rad
steradian sr 2) solid angle 1 sr = 1 m2 · m–2 180
second s time, period;
duration
tesla T magnetic 1 T = 1 Wb · m–2 π
flux density or Minute (‘) –––––– rad
ampere A electric current induction
10.800
kelvin K thermodyn. 1
volt V electrical 1 V = 1 W · A–1
temperature voltage (= ––– grad)
60
mole mol quantity of or potential
substance difference p
candela cd luminous Second (‘’) ––––––– rad
watt W power, 1W=1J· s–1 648.000
intensity energy flux,
heat 1
(= –––– minute)
flux 60
weber Wb magnetic 1 Wb = 1 V · s
flux 1 Wb = 1 V · s

1) Formed with numeric factor 1; e.g. 1 C


= 1 As, 1 Pa = 1 N · m–2
2) Additional SI unit

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Vacuum Technology Standards Fundamentals of Vacuum Technology

11. National and with German participation (also by


LEYBOLD), has been extensively incorpo-
DIN
1319
Title
Basic definitions for
Issue

international rated into DIN standards, as reflected in


designations such as DIN / ISO or DIN /
measurement technology
Part 1 – Basic definitions 1/95
Part 2 – Definitions for the
standards and EN. use of gauges
Part 3 – Definitions for
1/80
The most important standards to be com-
recommendati- plied with are listed in Table 11.1 below.
measurement
uncertainty and
evaluation of gauges
ons particular- Abbreviations used:
D = draft
and measuring
equipment 8/83

ly relevant to CD = Committee Draft Part 4 – Treatment of use


of measurements 12/85

vacuum
A) National agreements, Part 1: DIN
technology 11.1 National and (cont.)
international DIN Title Issue

For around 20 years now, numerous stan-


standards and 1343 Normal state, reference state 1/90

dards and recommendations have been recommendations 1345 Thermodynamics; basic


definitions
drawn up at national and international level
and revised, whenever necessary, in of special 12/93
1952 Flow measurement with
accordance with the state of the art. These relevance to screens, nozzles, etc. 7/82
standards and recommendations must be
observed whenever use is made of vacu- vacuum technology 2402 Pipelines; nominal internal
diameters, definitions,
um equipment (pumps, gauges, valves, classification 2/76
etc.) and vacuum apparatus, systems and A) National agreements, Part 1: DIN 3535 Seals for gas supply – Part 6 4/94
plants are assembled. They not only con-
DIN Title Issue
tain specifications applying specially to 8964 Circuit parts for refrigeration
vacuum technology, but also go beyond 1301-8 E Units systems with hermetic and
Part 1 – Names of units, semi-hermetic compressors
this specific field and involve, for example, Part 1: Tests 3/96
symbols 1993
physical units, formulas, noise protection Part 2 – Parts and multiples Part 2: Requirements 9/86
regulations, etc. generally used 2/78 (E 12/95)
Part 3 – Conversions for units 16005 Overpressure gauges with
National standards are primarily DIN stan- no longer used 6/79 elastic measuring element for
dards, particularly those relating to the general use Requirements
1304 General symbols
area of vacuum technology in the DIN Part 1 – General symbols 3/94 and testing 2/87
Standards Committee on Mechanical Part 2 – Symbols for 16006 Overpressure gauges with
Engineering (NAM). International stand- meteorology and Bourdon tube Safety-related
ards and recommendations are drawn up geophysics 9/89 requirements and testing 2/87
Part 3 – Symbols for electrical
and issued energy supply 3/89 19226 – 1 Control and
Part 5 – Symbols for flow instrumentation
a) by the International Standardization mechanics 9/89 technology;
Organization (ISO), in particular by ISO Part 6 – Symbols for electrical control and regulation
Committee TC 112 (vacuum technolo- communications technology; definitions –
gy) technology 5/92 general principles 2/94
Part 7 – Symbols for – 4 Control and
b) by the European Committee of Manu- meteorology and instrumentation
facturers of Compressors, vacuum geophysics technology;
Part 7 – Symbols for control and regulation
pumps and compressed air tools electric machines 1/91 technology;
(PNEUROP), in particular by PNEUROP definitions for control
1305 Mass; weighed value, force,
Subcommittee C5 (vacuum technology) weight force, weight
and regulation systems 2/94
– 5 Control and
c) by the European Committee for Stan- load, definitions 1/88 instrumentation
dardization (CEN), in particular by Tech- 1306 Density; definitions 6/84 technology; control and
regulation technology;
nical Committee TC 138 (nondestruc- 1313 Physical variables and functional definitions 2/94
tive testing) and Technical Committee equations, definitions, spelling 4/78
TC 318.
The content of the documents drawn up by
1314 Pressure; basic definitions,
units 2/77
25436 Integral leak rate test of safety
vessel with absolute pressure
method 7/80
D00
the international organizations in a) to c),

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Fundamentals of Vacuum Technology Vacuum Technology Standards

DIN Title Issue DIN Title Issue A) European/national agreements, EN,


28090 Static seals for flange 28426 Vacuum technology; DIN/EN, CEN
connections acceptance specifications or
DIN/EN Title Issue
Part 1 - Characteristic values frotary piston vacuum pumps
for seals and Part 1 – Rotary piston and EN 473 Training and certification of
testing methods 9/95 vane type rotary personnel for nondestructive
Part 2 - Seals made of vacuum pumps in testing (including leak test) 7/93
sealing plate; special rough and medium
testing methods for vacuum range 837-1 Pressure gauges, Part 1:
quality assurance 9/95 Part 2 – Roots vacuum pumps Pressure gauges with
in medium Bourdon tubes, dimensions,
28400 Vacuum technology; vacuum range measurement
designations and definitions technology, requirements
Part 1 - Basic definitions, units, 28427 Vacuum technology; and testing 2/97
ranges, characteristic acceptance specifications
variables and basic for diffusion pumps and 837-2 Pressure gauges, Part 2:
principles 5/90 ejector vacuum pumps for Selection and installation
Part 2 - Vacuum pumps 10/80 pump fluid vapor pressures of recommendations for
Part 3 - Vacuum plants; less than 1 mbar 2/83 pressure gauges 1/95
characteristic 837-3 Pressure gauges, Part 3:
variables and gauges 6/92 28428 Vacuum technology;
acceptance specifications Pressure gauges with
Part 4 - Vacuum coating plate and capsule elements,
technology 3/76 for turbo-molecular pumps 11/78
dimensions, measurement
Part 5 - Vacuum drying and 28429 Vacuum technology; technology, requirements
vacuum freeze-drying 3/81 acceptance specifications and testing 2/97
Part 6 - Analytical techniques for getter-ion pumps 8/85
for surface technology 10/80 1330-8 E Nondestructive testing -
Part 7 - Vacuum metallurgy 7/78 28430 Vacuum technology; definitions for leak test –
Part 8 - Vacuum systems, measuring specifications for terminology 6/94
components and ejector vacuum pumps and
accessories 10/80 ejector compressors. 1779 E Nondestructive
(E 7/91) Pump fluid: water vapor 11/84 testing – leak test. Instructions
for selection of a testing
28401 Vacuum technology; 28431 Acceptance specifications method 3/95
symbols – overview 11/76 for liquid ring vacuum pumps 1/87
1338-8 E Nondestructive
28402 Vacuum technology: variables, 28432 Acceptance specifications for testing – leak test.
symbols, units - overview 12/76 diaphragm vacuum pumps E 5/95 Terminology on leak test 1994
28403 Vacuum technology; quick 53380 Testing of plastic foils, 1518 E Nondestructive
connections, small flange determination of gas testing – determination of
connections 9/86 permeability 6/69 characteristic variables for
(E 10/83) mass spectrometer
28404 Vacuum technology: flanges, leak detectors
dimensions 10/86 45635 Noise measurement at
machines: measurement 1593 E Nondestructive
28410 Vacuum technology; mass of airborne noise, enveloping testing – bubble type
spectrometer partial pressure surface methods. testing method 12/94
gauges, definitions, Part 13 – Compressors,
characteristic variables, including vacuum NMP 826 Calibration of gaseous
operating conditions 11/86 pumps, positive reference leaks, CD 9/95
displacement, turbo Nr. 09–95
28411 Vacuum technology;
acceptance specifications and steam ejectors 2/77
for mass spectrometer leak 55350 Definitions of quality
detection devices, definitions 3/76 assurance and statistics B) International agreements, ISO, EN/ISO
Part 11 – Basic definitions of
28416 Vacuum technology; DIN Title Issue
quality assurance 8/95
calibration of vacuum gauges in
Part 18 – Definitions regarding 1000 SI units and recommendations
a range from 10-3 to 10-7 mbar.
certification of for the use of their multiples
General methods; pressure
results of quality and of certain other units 11/92
reduction through constant flow 3/76 tests/quality test
28417 Vacuum technology; measuring certificates 7/87 1607 / 1 Positive displacement vacuum
pV mass flow according to pumps. Measurement of
volumetric method at constant 66038 Torr – millibar; millibar – torr performance characteristics. 12/93
pressure 3/76 conversion tables 4/71 Part 1 - Measurement of
volume rate of flow
28418 Vacuum technology; standard – Thesaurus Vacui
(pumping speed)
method for calibrating vacuum (definition of terms) 1969
gauges through direct compa- 1607 / 2 Positive displacement vacuum
rison with a reference device pumps. Measurement of
Part 1 – General principles 5/76 performance characteristics. 11/89
Part 2 – Ionization vacuum Part 2 - Measurement of
gauges 9/78 ultimate pressure
Part 3 – Thermal conductivity
vacuum gauges 8/80

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Vacuum Technology Standards Fundamentals of Vacuum Technology

DIN Title Issue DIN Title Issue


1608 / 1 Vapor vacuum pumps. DIN/ISO Requirements placed on quality
Part 1 Measurement of volume 10012 assurance for measuring
rate of flow 12/93 equipment 8/92
Part 1 – Confirmation system
1608 / 2 Vapor vacuum pumps. for measuring
Part 2: Measurement of critical equipment
backing pressure 12/89
1609 Vacuum technology. Flange
dimensions 3/86 C) PNEUROP/C5 (6.93)
DIN/ISO Standard atmosphere 12/79
Number Title/remark identical Issue
2533
to DIN
2861 / 1 Quick release couplings.
5607 Vacuum pumps;
Dimensions 8/74
acceptance specifications 28427 1972
Part 1 - Clamped Type
Part II: (Fluid
2861 / 2 Quick release couplings. entrainment pumps)
Dimensions 8/80
5608 Vacuum pumps;
Part 2 - Screwed type
acceptance specifications 28428 1973
3529 / 1 Vacuum Technology Part III: (Turbomolecular
Vocabulary 12/81 pumps)
Part 1 - General terms
5615 Vacuum pumps;
3529 / 2 Vacuum Technology acceptance specifications 28429 1976
Vocabulary 12/81 Part IV: (Getter-ion
Part 2 - Vacuum pumps and pumps)
related terms
6601 Measurement of per
3529 / 3 Vacuum Technology formance of ejector
Vocabulary 12/81 vacuum pumps and
Part 3 - Vacuum gauges ejector compressors 28430 5/78

3556 / 1 Measurement of performance 6602 Vacuum pumps;


characteristics. 1992 acceptance specifications
Part 1 - Sputter ion pumps (E) Part I: (Oil-sealed rotary
pumps and
3567 Vacuum gauges. Calibration by Roots pumps) 28426 1979
direct comparison with a
reference gauge (CD) 2/91 6606 Vacuum flanges and
connections; 28403 1985
3568 Ionisation vacuum gauge. dimensions and
Calibration by direct 28404
comparison with a
reference gauge (CD) 2/91 PN5ASR Vacuum pumps,
CC/5 acceptance specifications
3570 / 1 Vacuum gauges – standard refrigerator cooled
methods for calibration 2/91 cryopumps 7/89
Part 1 - Pressure reduction
by continuous flow in
the pressure range
10–1 ... 10–5 Pa
3669 Vacuum Technology. Bakable
flanges, dimensions. 2/86
Part 1: Clamped Type
EN/ISO Rubber and plastic hoses and
4080 hose lines – determination of
gas permeability 4/95
5167 Measurement of fluid flow by
means of orifice
plates, nozzles etc. 1980
5300 Vacuum gauges of the thermal
conductivity type. 2/91
Calibration by direct
comparison with a
reference gauge (CD)
9803 Pipeline fittings-mounting,
dimensions (E) 2/93 D00

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Fundamentals of Vacuum Technology References

12. References C. M. van Atta


Vacuum Science and Engineering
L. Fabel
Physik in der 2. Hälfte des 19. Jahr
459 pages, 1965, McGraw-Hill hunderts und die vakuumtechnische
1. Overview, New York/San Francisco/Toronto/
London/Sydney
Entwicklung bis Gaede
Pages 128-138
definitions and J. M. Lafferty et. al. H.-B. Bürger:
Foundations of Vacuum Science and G. Ch. Lichtenberg und die Vakuum
history Technology technik
704 pages, 1998, Wiley 1998 Pages 124-127
K. Diels, R. Jaekel
Leybold Vacuum Handbook A. Schubert G. Reich:
Pergamon Press Normen und Empfehlungen für die Gaede und seine Zeit
1st Ed. 1966 Vakuum-Technik Pages 139-145
Vakuum in der Praxis,
W. Haeder, E. Gärtner Vol. 3, 1991, 211-217 H. Adam
Die gesetzlichen Einheiten in der Technik Vakuum-Technik in der Zeit nach
Beuth-Vertrieb GmbH, 5. Aufl. 1980, H. Scharmann Gaede (1945 to the present);
Berlin 30, Köln, Frankfurt (Main) Vakuum – Gestern und Heute Pages 146-147
Vakuum in der Praxis,
H. Ebert Vol. 2, 1990, 276-281 G. Reich
Vakuum-Chronik, A documentation on Die Entwicklung der Gasreibungspumpen
works concerning vacuum that were M. Auwärter von Gaede, über Holweck, Siegbahn bis
published before 1928 Das Vakuum und W. Gaede zu Pfleiderer und Becker (mit zahlreichen
PTB-Bericht ATWD-11, September 1977 Vakuum-Technik, Vol. 32, 1983, 234-247 Literaturangaben)
Vakuum-Technik in der Praxis, Vol. 4,
M. Dunkel J. F. O’Hanlon 1992, 206-213
„Gedenken an Wolfgang Gaede“ A User’s Guide to Vacuum Technology
Physikalische Blätter Nr. 34 (1978), 3nd Ed., 402 pages, Wiley 1989, G. Reich
Heft 5, Pages 228-232 as well as New York Carl Hoffman (1844-1910), der Erfinder
Vakuum-Technik, 27. Jahrgang, No. 4, der Drehschieberpumpe
Pages 99-101 G. Reich Vakuum in der Praxis, 1994, 205-208
Wolfgang Gaede – Einige Gedanken zu
IUPAP (SUNANCO Commission) seinem 50. Todestag aus heutiger Sicht Th. Mulder
Symbols, Units etc. Vakuum in der Praxis, Blaise Pascal und der Puy de Dôme –
Document 25, 1987 7th year, 1995, 136-140 Große Männer der Vakuum-Technik
Vakuum in der Praxis, 1994, 283-289
Leybold AG S. German, P. Draht
Vademekum, 93 pages, 1988 Handbuch SI Einheiten W. Pupp und H. K. Hartmann
Vieweg Braunschweig/Wiesbaden, Vakuum-Technik, Grundlagen und Anwen-
M. Wutz, H. Adam, W. Walcher 1979, 460 pages dungen
Theory and Practice of C. Hanser, München, 1991, Wien,
Vacuum Technology “Gesetz über Einheiten im Meßwesen”
5. Aufl., 696 pages, 1992, vom 2. Juli 1969
Friedrich Vieweg u. Sohn, “Gesetz zur Änderung des Gesetzes über
Braunschweig/ Wiesbaden Einheiten im Meßwesen” vom 6. Juli
1973
A. Guthrie and R. K. Wakerling “Ausführungsverordnungen” vom 26.
Vakuum Equipment and Techniques Juni 1970
2. Vacuum pumps
264 pages, 1949, McGraw-Hill,
New York/London/Toronto In Vakuum-Technik Vol. 35, 1986: 2.1 Positive displacement
Th. Mulder pumps, condensers
D. J. Hucknall Otto von Guericke
Vacuum Technology and Applications Pages 101-110 W. Gaede
1st Ed., 319 pages, 1991 Demonstration einer rotierenden
Butterworth-Heinemann, Oxford P. Schneider Quecksilberpumpe
Zur Entwicklung der Luftpumpen- Physikalische Zeitschrift, 6, 1905, 758-760
Initiationen und erste Reife
bis 1730 Pages 111-123

D00.174 LEYBOLD VACUUM PRODUCTS AND REFERENCE BOOK 2001/2002


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References Fundamentals of Vacuum Technology

W. Gaede H. Lang K. P. Müller


Gasballastpumpen Vakuumpumpen in der chemischen Indu- Trockenlaufende Drehschiebervakuum-
Zeitschrift für Naturforschung, strie – Wälzkolbenpumpen pumpen in einer Vielzweck-Produktions-
2a, 1947, 233-238 Vakuum-Technik, 1980, 72-82 anlage
Vakuum in der Praxis, 1994, 109-112
W. Armbruster und A. Lorenz H. F. Weber
Das maximale Kompressionsverhältnis Vakuumpumpen in der chemischen F. J. Eckle, W. Jorisch, R. Lachenmann
und der volumetrische Wirkungsgrad von Industrie – ölgedichtete Vakuum-Technik im Chemielabor
Vakuumpumpen nach dem Rootsprinzip Rotationsvakuumpumpen Vakuum in der Praxis, 1991, 126-133
Vakuum-Technik, 7, 1958, 81-85 Vakuum-Technik, 1980, 98-104
P. Bachmann und M. Kuhn
W. Armbruster und A. Lorenz D. Bartels Einsatz von Vorpumpen im Al-Ätzprozeß.
Die Kombination Rootspumpe-Wasser- Vakuumpumpen in der chemischen Erprobung trockenverdichtender Klauen-
ringpumpe Industrie pumpen und ölgedichteter Drehschieber-
Vakuum-Technik, 7, 1958, 85-88 Flüssigkeitsring-Vakuumpumpen – A Vakuumpumpen im Vergleich
Vakuum-Technik, 1980, 131-140 Vakuum in der Praxis, 1990, 15 – 21
H. Reylander
Über die Wasserdampfverträglichkeit von R. W. Adam und C. Dahmlos U. Gottschlich
Gasballastpumpen Flüssigkeitsring-Vakuumpumpen – B Vakuumpumpen im Chemielabor
Vakuum-Technik, 7, 1958, 78-81 Vakuum-Technik, 1980, 141-148 Vakuum in der Praxis, 1990, 257-260

F. Fauser U. Seegebrecht M. H. Hablanian


Charakteristik von Pumpsystemen für Förderung trockener Luft und von Aufbau und Eigenschaften verschiedener
größere Wasserdampfmengen unter gesättigtem Luft-Wasserdampfgemisch ölfreier Vakuumpumpen für den Grob-
Vakuum und unter Anwendung von Kon- mit Flüssigkeitsring-Vakuumpumpen und Feinvakuumbereich (wichtige
densation und Kompression des Vakuum-Technik, 1980, 246-252 Literaturangaben)
Wasserdampfes Vakuum in der Praxis, 1990, 96-102
1965 Transactions of the Third Internatio- H.-D. Bürger
nal Vacuum Congress, Stuttgart, Bd. 2/II, Fortschritte beim Betrieb von B. W. Wenkebach und J. A. Wickhold
393-395, Pergamon Press, Oxford 1966 Wälzkolbenpumpen Vakuumerzeugung mit Flüssigkeitsring-
Vakuum-Technik 1983, 140-147 Vakuumpumpen
M. Wutz Vakuum in der Praxis, 1989, 303-310
Das Abpumpen von Dämpfen mit gekühl- U. Seegebrecht
ten Kondensatoren Einfluß der Temperatur des Fördermittels U. Gottschlich und W. Jorisch
Vakuum-Technik, 16, 1967, 53-56 auf das Saugvermögen von Flüssigkeits- Mechanische Vakuumpumpen im
ring-Vakuumpumpen bei der Förderung Chemieeinsatz
H. Hamacher von trockener Luft Vakuum in Forschung und Praxis, 1989,
Kennfeldberechnung für Rootspumpen Vakuum-Technik, 1985, 10-14 113-116
DLR FB 69-88, 1969
P. Bachmann und H.-P. Berger W. Jorisch
H. Hamacher Sicherheitsaspekte beim Einsatz von Neue Wege bei der Vakuumerzeugung in
Beitrag zur Berechnung des ölgedichteten Drehschiebervakuumpum- der chemischen Verfahrenstechnik
Saugvermögens von Rootspumpen pen in CVD-Anwendungen Vakuum in der Praxis, 1995, 115-118
Vakuum-Technik, 19, 1970, 215-221 Vakuum-Technik, 1987, 41-47
D. Lamprecht
H. Hamacher U. Fussel Trockenlaufende Vakuumpumpen
Experimentelle Untersuchungen an Trockenlaufende Vakuumpumpen in der Vakuum in der Praxis, 1993, 255-259
Nachkühlern von Rootspumpen chemischen Industrie
Vakuum-Technik, 23, 1974, 129-135 Vakuum in der Praxis, 1994, 85-88 P. Deckert et al.
Die Membranvakuumpumpe – Entwick-
M. Rannow L. Ripper lung und technischer Stand
Ölgedichtete Vakuumpumpen in der Explosionsschutz-Maßnahmen an Vaku- Vakuum in der Praxis, 1993, 165-171
Chemie umpumpen (with numerous references to
Chemie-Technik, No. 7, 1978, 39-41 relevant literature) W. Jorisch und U. Gottschlich
Vakuum in der Praxis, 1994, 91-100 Frischölschmierung – Umlaufschmierung,
H. P. Berges et al.
TRIVAC-B, ein neues Vakuumpumpen-
Gegensätze oder Ergänzung?
Vakuum in der Praxis, 1992, 115-118 D00
Konzept für universelle Anwendungen
Vakuum-Technik, 31, 1982, 168-171

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Fundamentals of Vacuum Technology References

W. Jitschin et al. W. Armbruster J. Henning


Das Saugvermögen von Pumpen: Unter- Vakuumpumpenkombinationen für Labor, 30 Jahre Turbo-Molekularpumpe
suchung verschiedener Meßverfahren im Technikum und Produktion Vakuum-Technik, 1988, 134-141
Grobvakuumbereich Chemiker-Zeitung / Chemische Apparatur,
Vakuum in Forschung und Praxis, 7, 88, 1964, 895-899 P. Duval et. al.
(1995) 183 -193 Die Spiromolekularpumpe
W. Becker Vakuum-Technik, 1988, 142-148
H.P. Berges and M. Kuhn Die Turbo-Molekularpumpe
Handling of Particles in Forevacuum Vakuum-Technik, 15, 1966, 211-218 and G. Reich
pumps 254-260 Berechnung und Messung der Abhängig-
Vacuum, Vol. 41, 1990, 1828-1832 keit des Saugvermögens von Turbo-Mole-
R. Frank et al. kularpumpen von der Gasart
M. H. Hablanian Leistungsdaten von Turbo-Molekularpum- Vakuum-Technik, 1989, 3-8
The emerging technologies of oil-free pen des Typs TURBOVAC mit senkrecht
vacuum pumps angeordnetem Axialkompressor J. Henning
J. Vac. Sci. Technol. Vakuum-Technik, 24, 1975, 78 -85 Die Entwicklung der Turbo-Molekular-
A6 (3), 1988, 1177-1182 pumpe
W. Becker Vakuum in der Praxis, 1991, 28-30
E. Zakrzewski, P. L. May and B. S. Emslie Eine gegenüberstellende Betrachtung von
Developments in vacuum Pumping Diffusionspumpen und Molekularpumpen D. Urban
systems based on mechanical pumps Ergebnisse europäischer Ultrahochvaku- Moderne Bildröhrenfertigung mit
with an oil free swept volume umforschung Turbo-Molekularpumpen
Vacuum, 38, 968, 757-760 Leybold-Heraeus GmbH u. Co., in its own Vakuum in der Praxis, 1991, 196-198
publishing house, Cologne 1968, 41-48
H. Wycliffe O. Ganschow et al.
Mechanical high-vacuum pumps with an R. Frank, E. Usselmann Zuverlässigkeit von Turbo-Molekular-
oil-free swept volume Kohlenwasserstoffreier Betrieb mit Turbo- pumpen
J. Vac. Sci. Technol. Molekularpumpen des Typs TURBOVAC Vakuum in der Praxis, 1993, 90-96
A5 (4) 1987, 2608-2611 Vakuum-Technik, 25, 1976, 48-51
M. H. Hablanian
A. P. Troup and D. Turell R. Frank, E. Usselmann Konstruktion und Eigenschaften von
Dry pumps operating under harsh Magnetgelagerte Turbo-Molekularpumpen turbinenartigen Hochvakuumpumpen
condictions in the semiconductor industry des Typs TURBOVAC Vakuum in der Praxis, 1994, 20-26
J. Vac. Sci. Technol. A7 (3), Vakuum-Technik, 25, 1976, 141-145
1989, 2381-2386 J. H. Fremerey und H.-P. Kabelitz
H.-H. Henning und G. Knorr Turbo-Molekularpumpe mit einer
P. Bachmann and M. Kuhn Neue luftgekühlte, lageunabhängige neuartigen Magnetlagerung
Evaluation of dry pumps vs rotary vane Turbo-Molekularpumpen für Industrie und Vakuum-Technik, 1989, 18-22
pumps in aluminium etching Forschung
Vacuum 41, 1990, 1825-1827 Vakuum-Technik, 30, 1981, 98-101 H. P. Kabelitz and J.K. Fremerey
Turbomolecular vacuum pumps with a
H. P. Berges and D. Götz H.-H. Henning und H. P. Caspar new magnetic bearing concept
Oil-free vacuum pumps of compact Wälzlagerungen in Turbo-Molekularpum- Vacuum 38, 1988, 673-676
design pen
Vacuum, Vol. 38, 1988, 761-763 Vakuum-Technik, 1982, 109-113 E. Tazioukow et al.
Theoretical and experimental investigation
E. Kellner et al. of rarefied gas flow in molecular pumps
Einsatz von Turbo-Molekularpumpen bei Vakuum in Forschung und Praxis, 7,
Auspumpvorgängen im Grob- und 1995, 53-56
2.2 Turbomolecular pumps Feinvakuumbereich
Vakuum-Technik, 1983, 136-139
W. Gaede
Die Molekularluftpumpe D. E. Götz und H.-H. Henning
Annalen der Physik, 41, 1913, 337-380 Neue Turbo-Molekularpumpe für
überwiegend industrielle Anwendungen
W. Becker Vakuum-Technik, 1988, 130-135
Eine neue Molekularpumpe
Vakuum-Technik, 7, 1958, 149-152

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References Fundamentals of Vacuum Technology

2.3 Fluid entrainment pumps R. Gösling W. Bächler und H. Henning


Treibmittelpumpen Neuere Untersuchungen über den
W. Gaede Vakuum-Technik, 1980, 163-168 Edelgas-Pumpmechnismus von
Die Diffusion der Gase durch Quecksilber- Ionenzerstäuberpumpen des Diodentyps
dampf bei niederen Drücken und die Dif- M. Wutz Proc. of the Forth Intern. Vacuum
fusionspumpe Grundlagen zur Bestimmung der Congress 1968, I. 365-368,
Annalen der Physik, 46, 1915, 357-392 charakteristischen Daten von Inst. of Physics, Conference Series No. 5,
Dampfstrahl-Ejektorpumpen London
W. Gaede Vakuum-Technik, 1982, 146-153
Die Öldiffusionspumpe H. Henning
Z. techn. Physik, 13, 1932, 210-212 H. Bayer Der Erinnerungseffekt für Argon bei
R. Jaeckel, H. G. Nöller und H. Kutscher Dampfstrahlpumpen Trioden-Ionenzerstäuberpumpen
Die physikalischen Vorgänge in Diffusi- Vakuum-Technik, 1980, 169-178 Vakuum-Technik, 24, 1975, 37-43
ons- und Dampfstrahlpumpen
Vakuum-Technik, 3, 1954, 1-15 H. Bayer
Vakuumerzeugung durch
W. Bächler und H. G. Nöller Dampfstrahl-Vakuumpumpen
Fraktionierung und Entgasung in Vakuum in der Praxis, 1989, 127-135 2.5 Cryopumps and
Öl-Diffusionspumpen cryoengineering
Z. angew. Physik einschl. Nukleonik, 9, F. Hinrichs
1957, 612-616 Aufbau, Betriebsverhalten und R. A. Haefer
Regelbarkeit von Cryo-Pumping
H. G. Nöller Dampfstrahl-Vakuumpumpen 456 pages, 1989 Oxford University Press,
Weshalb sind systematische Fehler bei Vakuum in der Praxis, 1991, 102-108 Oxford
Saugvermögensmessungen besonders
groß für Hochvakuumpumpen großer H. Frey und R-A. Haefer
Leistung ? Tieftemperaturtechnologie, 560 pages,
Vakuum-Technik, 12, 1963, 291-293 VDI-Verlag, Düsseldorf, 1981
2.4 Sorption pumps
W. Bächler und H.-J. Forth G. Klipping und W. Mascher
Die wichtigsten Einflußgrößen bei der G. Kienel Vakuumerzeugung durch Kondensation
Entwicklung von Diffusionspumpen Zur Desorption von Gasen in Getter- an tiefgekühlten Flächen, I. Kryopumpen
Vakuum-Technik, 13, 1964, 71-75 Ionenpumpen in „Physik und Technik von Vakuum-Technik, 11, 1962, 81-85
Sorptions- und Desorptionsvorgängen bei
W. Reichelt niederen Drücken“ W. Bächler, G. Klipping und W. Mascher
Bemerkungen zur Arbeitsweise moderner Rudolf A. Lange Verlag, 1963, Esch/Tau- Cryopump System operating down to 2,5
Diffusionpumpen nus, 266-270 K, 1962 Trans. Ninth National Vacuum
Vakuum-Technik, 13, 1964, 148-152 Symposium, American Vacuum Society,
W. Bächler 216-219, The Macmillan Company,
H. G. Nöller Ionen-Zerstäuberpumen, ihre New York
Theory of Vacuum Diffusion Pumps Wirkungsweise und Anwendung
Handbook of Physics, Vol.1, Part 6, Leybold-Heraeus GmbH u. Co., in its own G. Klipping
(pp. 323...419) Ed. A. H. Beck, Pergamon publishing house, Cologne 1966 Kryotechnik – Experimentieren bei tiefen
Press Ltd., London, W.I. (1966) W. Espe Temperaturen
Zur Adsorption von Gasen und Dämpfen Chemie-Ingenieur-Technik, 36,
G. Herklotz an Molekularsieben 1964, 430-441
Enddruckversuche mit Diffusionspumpen Feinwerktechnik, 70, 1966, 269-273
hohen Saugvermögens und M. Schinkmann
Restgasspektren G. Kienel Messsen und Regeln tiefer Temperaturen,
Vakuum-Technik, 20, 1971, 11 – 14 Vakuumerzeugung durch Kondensation Teil I: Thermodynamische Verfahren
und durch Sorption Meßtechnik, 81, 1973, 175-181
H. G. Nöller Chemikerzeitung / Chem. Apparatur 91,
Die Bedeutung von Knudsenzahlen und 1967, 83-89 und 155-161 G. Schäfer, M. Schinkmann
Ähnlichkeitsgesetzen in Diffusions- und Messsen und Regeln tiefer Temperaturen,
Dampfstrahlpumpen H. Hoch Teil II: Elektrische Verfahren,
Vakuum-Technik, 26, 1977, 72-78 Erzeugung von kohlenwasserstoffreiem
Ultrahochvakuum
Meßtechnik, 82, 1974, 31-38 D00
Vakuum-Technik, 16, 1967, 156-158

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R. Frank et al. J. P. Deville, L. Holland and L. Laurenson M. H. Hablanian


Entwicklung von Refrigeratoren für den Measurement of the rate of evaporation of Backstreaming Measurements above
Einbau in Kryopumpen Pump oils using a crystal vibrator Liquid-Nitrogen Traps
Vakuum-Technik, 30, 1981, 134-137 3rd. Internat. Vac. Congr Stuttgart 153- Vac. Sci. Tech., Vol. 6, 265-268, 1969
160, Pergamon Press, Oxford, 1965
J. J. Scheer und J. Visser Z. Hulek, Z. Cespiro, R. Salomonovic,
Anwendungen von Kryopumpen in der L. Laurenson, S. Hickman and M. Setvak and J. Voltr
industriellen Vakuumtechnik R. G. Livesey Measurement of oil deposit resulting from
Vakuum-Technik, 31, 1982, 34-45 Rotary pump backstreaming: An backstreaming in a diffusion pump
analytical appriasal of practical results system by proton elastic scattering
P. Duval and the factors affecting them Vacuum, Vol. 41 (7-9), 1853-1855, 1990
Diffusionspumpen, Turbo-Molekularpum- J. Vac. Sci. Technol. A 6 (2),
pen oder Kryopumpen ? – Auswahlkriteri- 238-242, 1988 M. H. Hablanian
en für Hochvakuumpumpen Elimination of backstreaming from
Vakuum-Technik, 31, 1982, 99-105 B. D. Power, A. M. I. Mech, E. Crawley mechanical vacuum pumps
and D. J. Crawley J. Vac. Sci. Technol. A5 (4), 1987,
H. Henning und H.-H. Klein Sources, Measurement and Control of 2612-2615
Pumpen von Helium mit Backstreaming in Oil Vapour Vacuum
Refrigerator-Kryopumpen Pumps
Vakuum-Technik, 34, 1985, 181-184 Vacuum, Vol. 4 (4), 415-437, 1957

H.-H. Klein et al. M. A. Baker 3. Ultrahigh vacuum


Einsatz von Kryopumpen in A cooled quartz crystal microbalance
Produktionsanlagen methode for measuring diffusion pump technology
Vakuum-Technik, 34, 1986, 203-211 backstreaming
Journal of Scientific Instruments (Journal G. Kienel
D. Müller und M. Sydow of Physics E), Series 2, Volume 1, Probleme und neuere Entwicklungen auf
Kryopumpen im Vergleich mit anderen 774-776, 1968 dem Ultrahochvakuum-Gebiet
Hochvakuumpumpen VDI-Zeitschrift, 106, 1964, 777-786
Vakuum in der Praxis, 2, 1990, 270-274 N. S. Harris
Diffusion pump back-streaming G. Kienel und E. Wanetzky
G. Kiese und G. Voß Vacuum, Vol. 27 (9), 519-530, 1977 Eine mehrmals verwendbare
Kryopumpen mit neuartiger Metalldichtung für ausheizbare
Regenerationstechnik M. A. Baker Uktrahochvakuum-Ventile und
Vakuum in der Praxis, 4, 1992, 189-192 Vapour and Gas Measurements in Vacu- Flanschdichtungen
um with the Quartz Crystal Microbalance Vakuum-Technik, 15, 1966, 59-61
in Vol.1, Proceedings of the ninth Confe-
rence on Vacuum Microbalance Techni- H. G. Nöller
ques, „Progress in Vacuum Microbalance Physikalische und technische Vorausset-
2.6 Oil backstreaming Techniques“ zungen für die Herstellung und Anwen-
dung von UHV-Geräten.
G. Levin Th. Gast and E. Robens ed., “Ergebnisse europäischer Ultrahochvaku-
A quantitativ appraisal of the Heyden & Son Ldt., London, New York, um Forschung”
backstreaming of forepump oil vapor Rheine, 1970 LEYBOLD-HERAEUS GmbH u. Co., in its
J. Vac. Sci. Technol. A 3 (6), 1985, own publishing house,
2212-2213 M. A. Baker and L. Laurenson Cologne 1968, 49-58
The use of a quartz crystal microbalance
M. A. Baker and L. Laurenson for measuring vapour backstreaming W. Bächler
A quartz crystal microbalance holder for from mechanical pumps Probleme bei der Erzeugung von
low Temperature use in vacuum Vacuum, Volume 16 (11), 633-637, 1966 Ultrahochvakuum mit modernen
Vacuum Vol. 17, (12), 647-648, 1967 Vakuumpumpen. „Ergebnisse
(Letters to the Editor) R. D. Oswald and D. J. Crawley europäischer Ultrahochvakuum
A method of measuring back migration of Forschung“
M. A. Baker and W. Steckelmacher oil through a baffle
The Measurement of Contamination in Vacuum, Vol. 16 (11), 623-624, 1966 Leybold-Heraeus GmbH u. Co., in its own
Vacuum Systems publishing house, Cologne 1968, 139-148
Vuoto, scienza e technologia, Bd.3 ,
(1/2), 3-17, 1970

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References Fundamentals of Vacuum Technology

P. Readhead, J. P. Hobson und W. Röllinger 5. Measurement of


E. V. Kornelsen Die Verwendung von Klammerflanschen in
The Physical Basis of Ultrahigh Vacuum der Vakuumtechnik low pressures
Chapman and Hall, London, 1968 Vakuum-Technik, 13, 1964, 42-45
C. Meinke und G. Reich
E. Bergandt und H. Henning H. Hoch Vermeidung von Fehlmessungen mit dem
Methoden zur Erzeugung von Ausheizbare Verbindungen an Hoch- System McLeod-Kühlfalle
Ultrahochvakuum vakuum-Apparaturen Vakuum-Technik, 12, 1963, 79-82
Vakuum-Technik, 25,1970, 131-140 Vakuum-Technik, 10, 1961, 235-238
P. A. Readhead and J. P. Hobson
H. Wahl W. Bächler und I. Wikberg Total Pressure Measurem. below 10–10
Das Hochvakuumsystem der CERN am Dual Seal Bakable Section Valves of the Torr with Nonmagnetic Ionisation Gauge
450 GeV Supersynchrotron und CERN Intersection Storage Ring Brit. J. Appl. Phys., 16, 1965, 1555-1556
Speichering (SPS) Vacuum, 21, 1971, 457-459
Vakuum in der Praxis, 1989, 43-51 C. Meinke und G. Reich
K. Teutenberg Comparison of Static and Dymanic
F. Grotelüschen UHV-Ganzmetallventile großer Nennweite Calibration Methods for Ionisation Gauges
Das UHV-System bei DESY. 1. Teil Vakuum-Technik, 21, 1972, 169-174 J. Vac. Sci. Techn., 4, 1967, 356-359
Vakuum in der Praxis, 4, 1991, 266-273
H. Henning G. Reich und W. Schulz
D. Trines The approximate calculation of Probleme bei der Verwendung von
Das Strahlrohrvakuumsystem des Hera- transmission probabilities Ionisations-Vakuummetern im Druck-
Protonenringes Vacuum, 28, 1978, No. 3, Seite 151 bereich oberhalb 10–2 Torr
Vakuum in der Praxis, 2, 1992, 91-99 Proc. of the Fourth Intern. Vacuum
G. Kühn Congress, 1968,
G. Schröder et al. Gasströme durch Spalte im Grobvakuum II. Inst. of Physics Conference Series No.
COSV- eine neue Forschungsanlage mit Vakuum-Technik, 33, 1984, 171-175 6, London, 661-665
UHV-Technologie
Vakuum in der Praxis, 5, 1993, 229-235 G. Reich
Probleme bei der Messung sehr niedriger
W. Jacobi Total- und Partialdrücke
Das Vakuumsystem der GSI-Beschleuni- R. Haberland und B. Vogt „Ergebnisse europäischer Ultrahoch-
geranlage UHV-Ventil für extrem viele Schließzyklen vakuum Forschung“
Vakuum in der Praxis, 6, 1994, 273-281 Vakuum-Technik, 34, 1985, 184-185 Leybold-Heraeus GmbH u. Co., in its own
publishing house, Cologne 1968, 99-106
A. Sele
Vakuum-Ventile (VAT) A. Barz and P. Kocian
Vakuum in der Praxis, 1, 1989, 206-212 Extractor Gauge as a Nude System
4. Conductances, J. Vac. Sci Techn. 7, 1970, 1, 200-203
L. Fikes
flanges, valves, Berechnung von Auspumpkurven mit U. Beeck and G. Reich
Hilfe der Analogie von Gasstrom und Comparison of the Pressure Indication of a
etc. elektrischem Strom Bayard-Alpert and an Extractor Gauge
Vakuum in der Praxis, 4, 1992, 265-268 J. Vac. Sci. and Techn. 9, 1972, 1,126-128
M. Knudsen
Gesetze der Molekularströmung und der W. Herz U. Beeck
inneren Reibungsströmung der Gase Zuverlässige Flanschverbindung im Untersuchungen über die Druckmessun-
durch Röhren Anwendungsgebiet der Tieftemperatur- gen mit Glühkathoden-Inisations-Vakuum-
Annalen der Physik, 4th issue, 28, 1909, und Vakuumtechnik metern im Bereich größer als 10–3 Torr
75-130 Vakuum-Technik, 29, 1980, 67-68 Vakuum-Technik, 22, 1973, 16-20

P. Clausing G. Reich
Über die Strömung sehr verdünnter Gase Über die Möglichkeiten der Messung sehr
durch Röhren von beliebiger Länge niedriger Drücke
Annalen der Physik, 5th issue, 12, Meßtechnik, 2, 1973, 46-52
1932, 961-989
D00

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G. Reich Vakuum in der Praxis, 3, 1991, 290-296 H. Dohmen


Spinning rotor viscosity gauge; a transfer Vakuumdruckmessung und -Regelung in
standard for the laboratory or an accurate M. Ruschitzka and W. Jitschin der chemischen Verfahrenstechnik
gauge for vacuum process control Physikalische Grundlagen des Vakuum in der Praxis, 6,1994, 113-115
J. Vac. Sci. Technol., 20 (4), Wärmeleitungsvakuummeters
1982, 1148-1152 Vakuum in der Praxis, 4, 1992, 37-43 N. Pöchheim
Druckregelung in Vakuumsystemen
G. Reich T. Koopmann Vakuum in Forschung und Praxis, 7,
Das Gasreibungs-Vakuummeter Neue Trends in der Vakuum-Meßtechnik 1995, 39-46
VISCOVAC VM 210 Vakuum in der Praxis, 5, 1993, 249-254
Vakuum-Technik, 31, 1982, 172-178 R. Heinen und W. Schwarz
Chr. Edelmann Druckregelung bei Vakuumprozessen
G. Grosse and G. Messer Die Entwicklung der Totaldruckmessung durch umrichtergespeiste Rootspumpen
Calibration of Vacuum Gauges at im UHV- und Extremvakuumbereich Vakuum-Technik, 35, 1986, 231-236
Pressures below 10–9 mbar with a Vakuum in der Praxis, 6, 1994, 213-219
molecular beam method
Vakuum-Technik, 30, 1981, 226-231 W. Jitschin
Kalibrierung, Abnahme und Zertifizierung
Chr. Edelmann et al.: Möglichkeiten der (with numerous references to relevant li- 7. Mass spectrometer
Meßbereichserweiterung bei Glühkatho- terature)
den-Ionisationsmanometern (numerous Vakuum in der Praxis, 6, 1994, 193-204 gas analysis at low
references to relevant literature)
Vakuum-Technik, 31, 1982, 2-10 W. Jitschin
pressures
Obere Meßbereichsgrenze von Glühkato-
Chr. Edelmann den-Ionisationsvakuummetern H. Hoch
Stand und Entwicklungstendenzen der Vakuum in Forschung und Praxis, 7, Total- und Partialdruckmessungen bei
Totaldruckmessung in der Vakuum-Tech- 1995, 47-48 Drücken zwischen 2 · 10–10 und
nik 2 · 10–2 Torr
Vakuum-Technik, 16, 1967, 8-13
Vakuum-Technik, 33, 1984, 162-180 F. Mertens et al.
Einfluß von Gasadsorbaten auf die Eigen-
H. Junge
J. K. Fremerey schaften eines Glühkatoden-Ionisations-
Partialdruckmessung und Partialdruck-
Das Gasreibungsvakuummeter vakuummeters mit axialer Emission nach
meßgeräte
Vakuum-Technik, 36, 1987, 205-209 Chen und Suen
G-I-T May 1967, 389-394 and
Vakuum in der Praxis, 7, 1995, 145-149
June 1967, 533-538
G. Messer
Kalibrierung von Vakuummetern
A. Kluge
Vakuum-Technik, 36, 1987, 185-192
Ein neues Quadrupolmassenspektrometer
mit massenunabhängiger Empfindlichkeit
G. Messer und W. Grosse 6. Pressure Vakuum-Technik, 23, 1974, 168-171
Entwicklung der Vakuum-Metrologie in der
PTB (numerous references to relevant li- monitoring, control S. Burzynski
terature)
Vakuum-Technik, 36, 1987, 173-184
and regulation Microprocessor controlled quadrupole
mass spectrometer
K. G. Müller Vacuum, 32, 1982, 163-168
G. Reich
Industrielle Vakuummeßtechnik Betriebsüberwachung, Steuerung und
Automatisierung von Vakuumanlagen W. Große Bley
Vakuum-Technik, 36, 1987, 193-197
Chemie-Ingenieur-Technik, 35, Quantitative Gasanalyse mit dem
1963, 73-77 Quadrupol Massenspektrometer
L. Schmidt und E. Eichler
Vakuum-Technik, 38, 1989, 9-17
Die Praxis einer DKD-Kalibrierstelle
Vakuum-Technik, 36, 1987, 78-82 G. Kienel
Elektrische Schaltgeräte der Vakuumtech- A. J. B. Robertson
nik Mass Spectrometry
C. Kündig
Elektro-Technik, 50, 1968, 5-6 Methuen & Co, Ltd., London, 1954
Vakuummeßgeräte für Totaldruck
Vakuum in der Praxis, 2, 1990, 167-176
A. Bolz, H. Dohmen und H.-J. Schubert C. Brunee und H. Voshage
Prozeßdruckregelung in der Massenspektrometrie
Chr. Edelmann
Vakuumtechnik Karl Thiemig Verlag, München, 1964
Glühkahtoden-Ionisationsmanometer für
hohe Drücke im Vakuumbereich Leybold Firmendruckschrift 179.54.01

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A. Cornu and R. Massot Chr. Falland 8.2 Leak detection with


Compilation of Mass Spectral Data Ein neuer Universal-Lecksucher mit halogen leak detectors
Heyden and Son Ltd., London, 1966 luftgekühlter Turbo-Molekularpumpe
Vakuum-Technik, 29, 1980, 205-208 H. Moesta und P. Schuff
P. Dawson Über den thermionischen Halogendetektor
Quadrupole Mass Spectroscopy W. Jansen Berichte der Bunsengesellschaft für
Elsevier, Amsterdam, 1976 Grundlagen der Dichtheitsprüfung mit physikaische Chemie,
Hilfe von technischen Gasen Bd. 69, 895-900, 1965
J. Backus Vakuum-Technik, 29, 1980, 105-113 Verlag Chemie, GmbH, Weinheim,
Chap. 11 in “Characteristics of Electrical Bergstraße
Discharges in Magnetic Fields” H. Mennenga
National Nuclear Energy Series, Div. I, Dichtheitsprüfung von Kleinteilen J. C. Leh and Chih-shun Lu
Vol. 5, McGraw-Hill Book Company Inc., Vakuum-Technik, 29, 1980, 195-200 US Patent Nr. 3,751,968
New York, 1949 Solid State Sensor
Chr. Falland
J. Backus Entwicklung von He-Lecksuchtechniken
University of California Radiation für UHV-Systeme großer Beschleuniger-
Laboratory Report, RL 20.6.36, und Speicherringe
Mar. 1945. Vakuum-Technik, 30, 1981, 41-44
9 Film thickness
W. Engelhardt et al. measurement and
Lecksuchanlagen in der Industrie
Vakuum-Technik, 33, 1984, 238-241 control
8. Leaks and Leak G. Sänger et al. G. Z. Sauerbrey
detection Über die Lecksuche bei Raumfahrzeugen Phys. Verhandl. 8, 113, 1957
Vakuum-Technik, 33, 1984, 42-47
8.1 Mass spectrometer leak G. Z. Sauerbrey
W. Jitschin et al. Verwendung von Schwingquarzen zur
detection He-Diffusionslecks als sekundäre Normale Wägung dünner Schichten und zur
für den Gasdurchfluß Mikrowägung
G. Kienel Vakuum-Technik, 36, 1987, 230-233
Lecksuche an Vakuumanlagen auf Zeitschrift für Physik 155, 206-222, 1959
elektrischem Wege L. Holland, L. Laurenson and J. P. Deville
W. Große Bley Use of a Quartz Crystal Vibrator in Vacu-
Elektrotechnik, 49, 1967, 592-594 Moderne He-Leckdetektoren um Destillation Invstigations
unterschiedlicher Prinzipien im prakti- Nature, 206 (4987), 883-885, 1965
U. Beeck schen Einsatz
Möglichkeiten und Grenzen der automati- Vakuum in der Praxis, 1, 1989, 201-205
schen Lecksuche im Bereich unter R. Bechmann
10–8 Torr. l/s Über die Temperaturabhängigkeit der
H. D. Bürger Frequenz von AT- und
Vakuum-Technik, 23, 1974, 77-80 Lecksucher (with references to relevant
Lecksuche an Chemieanlagen BT-Quarzresonatoren
literature) Archiv für Elektronik und Übertragungs-
Dechema Monographien (Ed. H. E. Bühler Vakuum in der Praxis, 2, 1990, 56-58
and K. Steiger), Vol. 89, Verlag Chemie, technik, Bd. 9, 513-518, 1955
Weinheim / New York W. Fuhrmann K. H. Behrndt and R. W. Love
W. Jansen Einführung in die industrielle Dichtheits- Automatic control of Film Deposition Rate
Grundlagen der Dichtheitsprüfung mit prüftechnik with the crystal oscillator for preparation
Hilfe von Testgasen Vakuum in der Praxis, 3, 1991, 188-195 of alloy films.
Vakuum-Technik, 29, 1980, 105-113 Vacuum 12 ,1-9, 1962
W. Fuhrmann
K. Paasche Industrielle Dichtheitsprüfung – ohne P. Lostis
Lecksuche an Chemieanlagen Testgas nach dem Massenspektrometrie- Automatic Control of Film Deposition Rate
Vakuum-Technik, 29, 1980, 227-231 verfahren with the Crystal Oscillator for Preparation
Vakuum in Forschung und Praxis, 7, fo Alloy Films.
H. B. Bürger 1995, 179 -182 Rev. Opt. 38, 1 (1959)
Lecksuche an Chemieanlagen mit He-
Massenspektrometer-Lecksuchern
D00
Vakuum-Technik, 29, 1980, 232-245

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Fundamentals of Vacuum Technology References

K. H. Behrndt H. F. Tiersten and R. C. Smythe C. Lu and A. W. Czanderna


Longterm operation of crystal oscillators An analysis of contowced crystal Application of Piezoelectric Quarz Crystal
in thin film deposition resonators operating in overtones of Microbalances (Vol.7 of: Methodes and
J. Vac. Sci. Technol. 8, 622 (1971) coupled thickness shear and thickness Phenomena, Their Applications in Sience
twist. and Technology)
L. Wimmer, S. Hertl, J. Hemetsberger and J. Acoustic Soc. Am. 65, (6) 1455, 1979 Elesvier, Amsterdam, Oxford, New York,
E. Benes Tokio, 1984
New method of measuring vibration R. E. Bennett, C. Rutkoeski and
amplitudes of quartz crystals. L. A. Taylor G. Simmons and H. Wang
Rev. Sci. Instruments 55 (4) , 608, 1984 Proceedings of the Thirteenth Annual Single Crystal Elastic Constants and
Symposium on Frequency Controll, Calculated Aggregate Properties –
P. J. Cumpson and M. P. Seah 479, 1959 A Handbook
Meas. Sci. Technol., 1, 548, 1990 The MIT Press, Cambridge, Massachu-
Chih-shun Lu setts, 1971
J. G. Miller and D. I. Bolef Improving the accuracy of Quartz csystal
Sensitivity Enhancement by the use of monitors C. D. Stockbridge
Acoustic Resonators in cw Ultrasonic Research/Development, Vol. 25, 45-50, in Vol. 5 “Vacuum Microbalance
Spectroscopy. 1974, Technical Publishing Company Techniques” K. Behrndt, editor, Plenum
J. Appl. Phys. 39, 4589, (1968) Press, Inc., New York, 1966
A. Wajid
J. G. Miller and D. I. Bolef Improving the accuracy of a quartz crystal S. Sotier
Acoustic Wave Analysis of the Operation microbalance with automatic determinati- Schwingquarz-Schichtdickenmessung
of Quartz Crystal Film Thickness Moni- on of acoustic impedance ratio. Vakuum in der Praxis 1992, 182-188
tors. Rev. Sci. Instruments, Vol. 62 (8), 2026-
J. Appl. Phys. 39, 5815, (1968) 2033, 1991

C. Lu and O. Lewis D. Graham and R. C. Lanthrop


Investigation of Film thickness The Synthesis fo Optimum Transient 10. Materials and
determination by oscillating quartz Response: Criteria and Standard Forms
resonators with large mass load. Transactions IEEE, Vol. 72 pt. II, material
J. Appl. Phys. 43, 4385 (1972) Nov. 1953
processing
C. Lu A. M. Lopez, J. A. Miller, C. L. Smith and
Mas determination with piezoelectric P. W. Murrill W. Espe
quartz crystal resonators. Tuning Controllers with Error-Integral Werkstoffkunde der Hochvakuumtechnik
J. Vac. Sci. Technol. Vol. 12 (1), Criteria Vol. 1 1959, Vol. 2 1960, Vol. 3 1961,
581-582, 1975 Instrumentation Technology, Nov. 1969 VEB Deutscher Verlag der Wissenschaf-
ten, Berlin
A. Wajid C. L. Smith and P. W. Murril
U.S. Patent No. 505,112,642 A More Precise Method for Tuning W. Espe
(May 12, 1992) Controllers Werkstoffe für trennbare metallische Ver-
ISA Journal, May 1966 bindungen der Ultrahochvakuumtechnik
C. Hurd Feinwerktechnik, 68, 1964, 131-140
U.S. Patent No. 5,117,192 (May 26, G. H. Cohen and G. A. Coon
1992) Theoretical considerations of Retarded W. Espe
Control Synthetische Zeolithe und ihre Verwen-
E. Benes Taylor Technical Data Sheet Taylor dung in der Hochvakuumtechnik
Improved Qartz Crystal Microbalance Instrument Companies, Rochester, Experimentelle Technik der Physik, XII,
Technique New York 1964, 293-308
J. Appl. Phys. 56, (3), 608-626 (1984)
J. G. Ziegler and N. B. Nichols H. Adam
C. J. Wilson Optimum Settings for Automatic Allgemeiner Überblick über die Werkstoffe
Vibration modes of AT-cut convex quartz Controllers der Vakuumtechnik und deren Auswahl
resonators. Taylor Technical Data Sheet No. TDS Haus der Technik Vortragsveröffentlichun-
J. Phys. d 7, 2449, (1974) 10A100, Taylor Instrument Companies, gen “Werkstoffe und Werkstoffverbindun-
Rochester, New York gen in der Vakuumtechnik” H. 172, Vul-
kan-Verlag, Dr. W. Classen, Essen, 1968,
4 – 13

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References Fundamentals of Vacuum Technology

K. Verfuß
Bessere Oberflächenvergütung durch
Elektropolieren – am Beispiel der Vaku-
um-Technik
VDI-Berichte, 183, 1972, 29-34

K. Verfuß
Schweißen und Hartlöten
Haus der Technik, Vortragsveröffentli-
chungen “Werkstoffe und Werkstoffver-
bindungen in der Vakuumtechnik”, H. 172
Vulkan-Verlag Dr. W. Classen, Essen,
1968, Seiten 39 -49

Chr. Edelmann
Gasabgabe von Festkörpern im Vakuum
Vakuum-Technik, 38, 1989, 223-243

R. Fritsch
Besonderheiten vakuumdichrter
Schweißverbindungen
Vakuum-Technik, 38, 1989, 94-102

H. Henning
Vakuumgerechte Werkstoffe und
Verbindungstechnik, Part 1
Vakuum in der Praxis, 2, 1990, 30-34

R. Fritsch
Vakuumgerechte Werkstoffe und
Verbindungstechnik, Part 2
Vakuum in der Praxis, 2, 1990, 104-112

M. Mühlloff
Vakuumgerechte Werkstoffe und
Verbindungstechnik, Part 3
Vakuum in der Praxis, 2, 1990, 179-184

11. Dictionaries
F. Weber
Elsevier’s Dictionary of High Vacuum
Science and Technology (German,
English, French, Spanish, Italian, Russian)
Elsevier Verlag 1968

Hurrle / Jablonski / Roth


Technical Dictionary of Vacuum Physics
and Vacuum Technology (German,
English, French, Russian)
Pergamon Press Verlag, Oxford, 1972

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Fundamentals of Vacuum Technology Index

13. Index Causes of faults if/when the desired


ultimate pressure
Cryocondensation . . . . . . . . . . . . . . .52
Cryopumps . . . . . . . . . . . . . . . .49, 177
is not achieved . . . . . . . . . . . . . . . . .134 Cryosorption . . . . . . . . . . . . . . . . . . .52
Absolute pressure . . . . . . . . . . . . . . . .7 Ceramic ball bearings (hybrid ball Cryotrapping . . . . . . . . . . . . . . . . . . .52
Absorption isotherms . . . . . . . . . . . . .45 bearings) . . . . . . . . . . . . . . . . . . . . . .42 Crystal Six . . . . . . . . . . . . . . . . . . .120
Absorption pumps . . . . . . . . . . .45, 139 CF-flange (conflathflange) . . . . . . . . .68 Cut in (start) pressure . . . . . .44, 54, 55
Absorption traps . . . . . . . . . . . . . . . .33 Changing the molecular sieve . . . . . .139 CVD (chemical vapor
Accessories for rotary Charles' law (Gay-Lussac's law) . . . . .11 deposition) . . . . . . . . . . . . . . . .128, 129
displacement pumps . . . . . . . . . . . . .33 Chemical resistance of elastomer Dalton's law . . . . . . . . . . . . . . . . . . . .11
Active oscillator . . . . . . . . . . . .122, 123 gaskets . . . . . . . . . . . . . . .149, 150, 151 Danger classes of fluids . . . . . . . . . .148
Adjustment and calibration of Chemical vapor deposition (CVD) . . .129 Data storage coating . . . . . . . . . . . .132
vacuum gauges . . . . . . . . . . . . . . . . .88 Choked flow, critical pressure DC 704, DC 705 (Silicone oils) . . . . . .39
Adsorption pumps, difference . . . . . . . . . . . . . . . . . . . . . .12 Degassing of the pump oil . . . . . . . . .37
Instructions for operation . . . . .139, 140 CIS (closed ion source) . . . . . . . . . . .93 Derived coherent and not coherent
Aggressive vapors . . . . . . . . . . . . . .135 Clamp flange . . . . . . . . . . . . . . . . . . .67 SI units with special
AGM (aggressive gas monitor) . . . . .94 Classification of vacuum pumps . . . . .16 names and symbols . . . . . . . . . . . . .170
Air, atmospheric . . . . . . . . . . . . . . . . .10 Clausius-Clapeyron equation . . . . . . .11 Detection limit (leak detectors) . . . . .111
ALL·ex pumps . . . . . . . . . . . . . . .28, 30 Claw pump . . . . . . . . . . . . . . . . . . . .27 Determination of a suitable
Ambient pressure . . . . . . . . . . . . . . . . .7 Closed ion source, (CIS) . . . . . . . . . . .93 backing pump . . . . . . . . . . . . . . . . . .64
Amonton's law . . . . . . . . . . . . . . . . . .11 Coating of parts . . . . . . . . . . . . . . . .130 Determination of pump down
Anticreep barrier . . . . . . . . . . . . . . . .40 Coating thickness regulation . . . . . . .125 time from Nomograms . . . . . . . . . . . .65
Anti-suckback valve . . . . . . . . . . . . . .19 Cold cap baffle . . . . . . . . . . . . . . . . . .39 Determination of pump sizes . . . . . . .62
APIEZON AP 201 . . . . . . . . . . . .39, 160 Cold cathode ionization vacuum DI series diffusion pumps . . . . . . . . .38
Atmospheric air . . . . . . . . . . . . . . . . .10 gauge . . . . . . . . . . . . . . . . . . . . . . . .77 Diaphragm contoller, examples
Atmospheric air, composition . . . . . .145 Cold head . . . . . . . . . . . . . . . . . . . . .50 of application . . . . . . . . . . . . . . . .86, 87
Atmospheric pressure . . . . . . . . . . . . .7 Cold surfaces, bonding of Diaphragm vacuum gauges . . . . . . . .72
Atomic units . . . . . . . . . . . . . . . . . .170 gases to . . . . . . . . . . . . . . . . . . . . . . .51 Diaphragm vacuum pumps . . . . . . . . .17
Autoc ontrol tune . . . . . . . . . .125, 126 Cold traps . . . . . . . . . . . . . . . . . . . . .39 DIAVAC diaphragm vacuum gauge . . .72
Automatic protection, monitoring Collision frequency . . . . . . . . . . . . . . .10 DIFFELEN, light, normal, ultra . . .39, 160
and control of vacuum systems . . . . .83 Collision rate . . . . . . . . . . . . . . . . . . .10 Diffusion / vapor-jet pumps,
Auto-Z match technique . . . . . . . . . .122 Common solvents . . . . . . . . . . . . . .146 Instructions for operation . . . . . . . . .139
Avogadro's law . . . . . . . . . . . . . . . . .11 Compression . . . . . . . . . . . . . . . . . . .43 Diffusion pumps . . . . . . . . . . . . . . . .36
Avogadro's number (Loschmidt Compression vacuum gauges . . . . . . .74 Diode-type sputter ion pumps . . . . . .46
number) . . . . . . . . . . . . . . . . . . .12, 143 Condensate traps . . . . . . . . . . . . . . . .33 Direct-flow leak detector . . . . . . . . . .115
Backing line vessel . . . . . . . . . . . . . . .64 Condensers . . . . . . . . . . . . . . . .33, 174 Discharge filters . . . . . . . . . . . . . . . . .33
Baffle . . . . . . . . . . . . . . . . . . . . . . . . .36 Conductance . . . . . . . . . . . . . . . . .9, 13 Displacement pumps . . . . . . . . .16, 174
Baffles (vapor barriers) . . . . . .36, 37, 39 Conductance of openings . . . . . . . . .179 DIVAC vacuum pump . . . . . . . . . . . . .17
Baking (degassing) . . . . . . . .61, 68, 141 Conductance of DKD (Deutscher Kalibrierdienst)
Barrier gas operation . . . . . . . . . . . . .44 piping . . . . . . . . . . . . .14, 155, 161, 179 German calibration service . . . . . . . . .81
Basis SI units . . . . . . . . . . . . . . . . . .170 Conductance, nomographic Dry compressing rotary
Bath cryostats . . . . . . . . . . . . . . . . . .49 determination . . . . . . . . . . . . . . . . . . .14 displacement pumps . . . . . . . . . . . . .24
Bayard-Alpert gauge . . . . . . . . . . . . . .80 Conductances, calculation of . . . . . . .13 Dry processes . . . . . . . . . . . . . . . . . .57
Boat (thermal evaporator) . . . . . . . . .128 Connection of leak detectors to Drying of paper . . . . . . . . . . . . . . . . .67
Boltzmann constant . . . . . . . . . .11, 143 vacuum systems . . . . . . . . . . . . . . .116 Drying processes . . . . . . . . . . . . . . . .60
Bombing-Test (storing under Contamination of vacuum sensors . .139 Drying processes, selection of
pressure) . . . . . . . . . . . . . . . . . . . . .119 Contamination of vacuum vessels . . .134 pumps for . . . . . . . . . . . . . . . . . . . . .66
Booster (oil-jet) pump . . . . . . . . .38, 46 Continous flow . . . . . . . . . . . . . . . . . .12 DRYVAC-Pumps . . . . . . . . . . . . . . . .28
Bourdon vacuum gauge . . . . . . . . . . .72 Continous flow cryopumps . . . . . . . . .49 D-Tek . . . . . . . . . . . . . . . . . . . . . . .110
Boyle-Mariotte law . . . . . . . . . . . . . . .11 Continuum theory . . . . . . . . . . . . . . .11 Duo seal (sealing passage) . . .17, 18, 19
Break down voltage Conversion of leak rate units . . . . . .106 Dust separator (dust filter) . . . . . . . . .33
(Paschen curve for air) . . . . . . . . . . .163 Conversion of leak rate units . . . . . .144 Dynamic expansion method . . . . . . . .82
Bubble (immersion) test . . . . . . . . .109 Conversion of pressure units . . . . . .142 Ecotec II . . . . . . . . . . . . . . . . . . . . .113
Calibration curves of Conversion of pV-throughput units . .144 Effective pumping speed . . . . . . . .33, 62
THERMOVAC gauges . . . . . . . . . . . . .77 Corrosion protection . . . . . . . . .135, 136 Elastomer gaskets . . . .69, 149, 150, 151
Calibration inspection . . . . . . . . . . . . .81 Counter-flow leak detector . . . . . . . .115 Electrical break down voltage
Coating sources . . . . . . . . . . . . . . . .128 Cracking pattern . . . . . . . . . . . . . . .136 (Paschen curve air) . . . . . . . . . . . . .163
Capacitance diaphragm gauges . . . . .73 Critical pressure difference Electron beam evaporators
Capsule vacuum gauge . . . . . . . . . . .772 (choked flow) . . . . . . . . . . . . . . . . . . .12 (electron guns) . . . . . . . . . . . . . . . .129
Crossover value . . . . . . . . . . . . . . . . .53 Envelope test . . . . . . . . . . . . . .118, 119

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Envelope test (concentration Hybrid ball bearings (Ceramic ball LN2 cold traps . . . . . . . . . . . . . . . . . .40
measurement) . . . . . . . . . . . . . . . . .118 bearings) . . . . . . . . . . . . . . . . . . . . .42 Local leak rate . . . . . . . . . . . . . . . . .106
Evacuation in the rough / medium / Hydrocarbon-free vacuum . . . . . .39, 60 Loschmidt's number
high vacuum region . . . . . . . .62, 63, 64 IC 5 . . . . . . . . . . . . . . . . . . . . . . . .127 (Avogadro constant) . . . . . . . . . .11, 143
Evacuation of gases / vapors . . . . . . .66 Ideal gas law . . . . . . . . . . . . . . . . . 7, 11 Magnetic suspension (bearings) . . . . .42
Evaluating spectra . . . . . . . . . . . . . . .96 Impingement rate . . . . . . . . . . . . . . . .10 Mass flow . . . . . . . . . . . . . . . . . .8, 104
Expansion method static / Industrial leak testing . . . . . . . . . . . .119 Mass flow (leak detection) . . . . . . . .104
dynamic . . . . . . . . . . . . . . . . . . . .81, 82 Influence of magnetic / Mass range . . . . . . . . . . . . . . . . . . .195
Extractor ionization vacuum electrical fields . . . . . . . . . . . . . . . . .141 Mass spectrometer, general,
gauge . . . . . . . . . . . . . . . . . . . . . . . .80 Internal compression (claw pumps) . .28 historical . . . . . . . . . . . . . . . . . .89, 180
Fast regeneration (partial Inside-out leak . . . . . . . . . . . . . . . . .107 Maximum backing pressure
regeneration) . . . . . . . . . . . . . . . . . . .54 Integral leak rate . . . . . . . . . . . . . . .107 (critical forevacuum pressure) . . . . . .37
Fingerprint . . . . . . . . . . . . . . . . . . . . .96 Internal reflow (roots pumps) . . . . . . .24 McLeod vacuum gauge . . . . . . . . . . .74
Flanges and their seals . . . . . . . .67, 179 Ion desorption effect . . . . . . . . . . . . .79 Mean free path . . . . . . . . . . .9, 142, 159
Floating zero-point suppression . . . .111 Ion sputter pumps . . . . . . . . . . . .45, 46 Measuring range of vacuum
Fluid entrainment pumps . . . . . .35, 177 Ionization vacuum gauge for gauges . . . . . . . . . . . . . . . . . . . . . . .161
Foam spray leak test . . . . . . . . . . . .109 higher pressures up to 1 mbar . . . . . .80 Measuring range, favorable . . . . . . . .70
Fractionation of pump fluids . . . . . . . .37 Ionization vacuum gauges . . . . . . . . .77 Measuring ranges of vacuum
Fragment distribution pattern . . . . . . .98 Ionization, specific (gas analysis) . . . .96 gauges . . . . . . . . . . . . . . . . . . . . . . .162
Fundamental pressure Isotopes . . . . . . . . . . . . . . . . . . . . . .96 Measuring vacuum, vacuum
measurement methods . . . . . . . . . . . .81 Kammerer compression vacuum gauges . . . . . . . . . . . . . . . . . . . .70, 179
Gas analysis . . . . . . . .89, 100, 101, 180 gauge . . . . . . . . . . . . . . . . . . . . . . . .74 Medium vacuum adsorption trap . . . .33
Gas ballast . . . . . . . . . . . . . .21, 22, 111 Kinetic gas theory . . . . . . . . . . . . . . .11 MEMBRANOVAC . . . . . . . . . . . . . . . .73
Gas composition as a function Kinetic of gases, diagram of . . . . . . .154 Mercury (pump fluid) . . . . . . .36, 39,160
of altitude . . . . . . . . . . . . . . . . . . . .155 Kinetic of gases, formulas . . . . . . . .143 Mode-lock oscillator . . . . . . . . . . . .123
Gas constant, general (molar) .7, 11, 143 Knudsen flow . . . . . . . . . . . . . . . . . . .13 Molar gas constant . . . . . . . . .7, 11, 143
Gas density . . . . . . . . . . . . . . . . . . . . .7 Krypton 85 test . . . . . . . . . . . . . . . .109 Molar mass
Gas dependent pressure reading, Laminar flow . . . . . . . . . . . . . . . . . . .12 (molecular weight) . . . . . . . . . .7, 10, 11
vacuum gauges with . . . . . . . . . . . . .75 Langmuir-Taylor-effect . . . . . . . . . .111 Molecular flow . . . . . . . . . . . . . . .12, 13
Gas discharge . . . . . . . . . . . . . . .46, 78 Laval nozzle . . . . . . . . . . . . . . . . . . . .38 Molecular sieve . . . . . . . . . . . . .45, 139
Gas independent pressure reading, Leak detection . . . . . . . . . . . . .104, 181 Monolayer . . . . . . . . . . . . . . . . . . . . .10
vacuum gauges with . . . . . . . . . . . . .72 Leak detection using Helium Monolayer formation time . . . .10, 13, 61
Gas laws . . . . . . . . . . . . . . . . . . . . . .11 leak detectors . . . . . . . . . . . . . . . . .117 National standards, resetting to . . . . .81
Gas locks . . . . . . . . . . . . . . . . . . . . . .69 Leak detection without leak detector .107 NEG pumps (non evaporable
Gas sorption (pumping) of Leak detection, leak test . . . . . . . . . .104 getter pumps) . . . . . . . . . . . . . . .45, 48
vacuum gauges . . . . . . . . . . . . . .78, 79 Leak detectors with 180° sector Neoprene . . . . . . . . . .68, 149, 150, 151
Gas storage in the oil of rotary mass spectrometer . . . . . . . . . . . . .114 Nitrogen equivalent . . . . . . . . . . .71, 78
vane pumps . . . . . . . . . . . . . . . . . . .111 Leak detectors with mass Nominal internal diameter and
Gaskets . . . . . . . . . . .68, 149, 150, 151 spectrometer . . . . . . . . . . . . . .110, 181 internal diameter of tubes . . . . . . . . .146
Gay-Lussac's law . . . . . . . . . . . . . . . .11 Leak detectors with quadrupole Nomogram . . . . . . . . . . . . . . . . . . . .65
General gas constant mass spectrometer . . . . . . . . . . . . .113 Nomogram: conductance of
(Molar gas constant) . . . . . . .7, 11, 143 Leak detectors, how they work . . . . .110 tubes / entire pressure range . . . . . .158
Getter pumps . . . . . . . . . . . . . . . . . . .45 Leak rate, hole size, Nomogram: conductance of
Glass coating . . . . . . . . . . . . . . . . . .132 conversion . . . . . . . . . .9, 104, 105, 106 tubes / laminar flow range . . . . . . . .155
Halogen leak detector . . . . . . . .110, 181 Leak test (chemical reactions, dye Nomogram: conductance of
Helium leak detectors with 180° penetration) . . . . . . . . . . . . . . . . . . .110 tubes / molecular flow range . . .155, 162
sector mass spectrometer . . . . . . . .114 Leak test, using vacuum gauges Nomogram: pump down time /
Helium spray equipment . . . . . . . . . .118 sensitive to the type of gas . . . . . . . .108 medium vacuum, taking in
Helium standard leak rate . . . . . . . .106 LEYBODIFF-Pumps . . . . . . . . . . . . . .37 account the outgasing from the
High frequency vacuum test . . . . . . .109 INFICON Quartz crystal walls . . . . . . . . . . . . . . . . . . . . . . . .159
High pressure ionization vacuum controllers . . . . . . . . . . . . . . . . . . . .127 Nomogram: pump down time /
gauge . . . . . . . . . . . . . . . . . . . . . . . .80 Line width . . . . . . . . . . . . . . . . . . . . .94 rough vacuum . . . . . . . . . . . . . . . . .156
High vacuum range . . . . . . . . . . .62, 63 Linearity range of quadrupole Non evaporable getter (NEG)
HLD 4000 . . . . . . . . . . . . . . . . . . . .110 gauges . . . . . . . . . . . . . . . . . . . . . . .102 pumps . . . . . . . . . . . . . . . . . . . . .45, 48
HO-factor (diffusion pumps) . . . . . . .37 Liquid ring pumps . . . . . . . . . . . . . . .17 Non gas-tight area . . . . . . . . . . . . .1104
Hot cathode ionization vacuum
gauge . . . . . . . . . . . . . . . . . . . . . . . .78
Liquid sealed rotary displacement
pumps . . . . . . . . . . . . . . . . . . . . . . . .17
Nude gauge (nude system) . . . . . . . . .72
Oil backstreaming . . . . . . . . . . . .39, 178 D00
HY.CONE pumps . . . . . . . . . . . . . . . .44 Liquid-filled vacuum gauges . . . . . . . .74 Oil change . . . . . . . . . . . . . . . . . . . .137
Literature references . . . . . . . .174 – 183 Oil consumption . . . .135, 136, 137, 138

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Fundamentals of Vacuum Technology Index

Oil contamination . . . . . . . . . . . . . . .135 Pressure ranges in vacuum Roots pumps . . . . . . . . . . . . . . . . . . .24


Oil diffusion pumps . . . . . . . . . . . . . .36 technology . . . . . . . . . . .12, 56, 57, 145 Roots pumps, Instructions for
Oil sealed rotary displacement Pressure regulation / control . . .84, 180 operation . . . . . . . . . . . . . . . . . . . . .137
pumps . . . . . . . . . . . . . . . . . . . . . . . .18 Pressure regulation / control rough Rotary displacement pumps . . . . . . . .18
Oil vapor ejector vacuum pumps . . . .36 and medium vacuum systems . . . . . .84 Rotary plunger pumps . . . . . . . . . . . .20
Oil-free (hydrocarbon-free) Pressure regulation in high and Rotary vane / piston pumps,
vacuum . . . . . . . . . . . . . . . . . . . .39, 60 ultra high vacuum systems . . . . . . . .87 Instructions for operation . . . . . . . . .135
Oils (pump fluids) . . . . . . . . . . . . . . .39 Pressure regulation, continuous / Rotary vane pumps . . . . . . . . . . . . . .18
Open (normal) ion source . . . . . . . . . .90 discontinuous . . . . . . . . . . . . . . .84, 86 Salt, drying of . . . . . . . . . . . . . . . . . .66
Optical coatings . . . . . . . . . . . . . . . .131 Pressure rise / drop (leak) test .107, 108 Saturation vapor pressure
Oscillation displacement pumps . . . . .17 Pressure units . . . . . . . . . . . . . . .7, 142 (nonmetallic gaskets) . . . . . . . . . . . .161
Oscillator, ( active, mode-lock) .122, 123 PTB (Federal physical-technical Saturation vapor pressure . . . . . . .7, 22
Outgasing of materials . . . . . . . . . . .145 institute) . . . . . . . . . . . . . . . . . . . . . .81 Saturation vapor pressure
Outgasing rate (referred to Pumpdown time . . . . . . . . . . . . .62 - 66 (cryogenic technology) . . . . . . . . . . .161
surface area) . . . . . . . . . . . . . . . . .9, 61 Pump fluid . . . . . . . . . . . . . . . . . . . . .39 Saturation vapor pressure (metals) . .160
Outside-in leak . . . . . . . . . . . . . . . . .107 Pump fluid backstreaming . . . . . . . . .39 Saturation vapor pressure
Overpressure . . . . . . . . . . . . . . . . . . . .7 Pump fluid change cleaning (pump fluids) . . . . . . . . . . . . . . . . . .160
Oxide-coated cathodes . . . . . . . . .78, 90 (diffusion pumps) . . . . . . . . . . . . . .139 Saturation vapor pressure
Partial final pressure . . . . . . . . . . . . .74 Pump oil, selection when handling (solvents) . . . . . . . . . . . . . . . . . . . .160
Partial flow opeartion . . . . . . . . . . . .115 aggressive vapors . . . . . . . . . . . . . .135 Saturation vapor pressure and
Partial flow ratio . . . . . . . . . . . . . . . .116 Pump throughput . . . . . . . . . . . . . . . . .9 vapor density of water . . . . . . .147, 164
Partial pressure . . . . . . . . . . . . . . . . . .7 Pumping (gas sorption) of Sealing passage . . . . . . . . . . . . . .18, 19
Partial pressure measurement . . . . .100 vacuum gauges . . . . . . . . . . . . . .77, 78 Seal-off fitting . . . . . . . . . . . . . . . . . .69
Partial pressure regulation . . . . . . . .101 Pumping chamber . . . . . . . . . . . . . . .16 Selection of pumps . . . . . . . . . . . . . .56
Particle number density . . . . . . . . . . . .7 Pumping of gases . . . . . . . . . . . . . . .57 Selection of pumps for drying
Paschen curve . . . . . . . . . . . . . . . . .163 Pumping of gases and processes . . . . . . . . . . . . . . . . . . . . .66
Penning vacuum gauges . . . . . . . . . .77 vapors . . . . .20, 21, 34, 52, 57, 58, 135 Sensitivity of quadrupole sensors . . . .95
Perbunan . . . . . . . . .68, 149 - 151, 161 Pumping speed . . . . . . . . . . . . . . . . . .8 Sensitivity of vacuum gauges . . . . . . .78
Period measurement . . . . . . . . . . . .122 Pumping speed units, Separating system of
Permissible pressure units . . . . . . . .142 conversion of . . . . . . . . . . . . . . . . . .144 mass spectrometers . . . . . . . . . . . . . .90
Phase diagram of water . . . . . . . . . .164 Pumping various chemical Shell baffle . . . . . . . . . . . . . . . . . . . . .39
Photons . . . . . . . . . . . . . . . . . . . . . . .79 substances . . . . . . . . . . . . . . . . . . .136 Silicone oils, DC 704, DC 705 . .39, 160
PIEZOVAC . . . . . . . . . . . . . . . . . . . . .73 Purge gas . . . . . . . . . . . . . . . . . . . . .29 Small flange . . . . . . . . . . . . . . . . . . . .67
Pirani vacuum gauge . . . . . . . . . . . . .76 PVD (physical vapor deposition) . . .128 Smallest detectable concentration . . . .95
Plastic tent (envelope) . . . . . . . . . . .118 pV-flow . . . . . . . . . . . . . . . . . . . . . . . .9 Smallest detectable partial pressure . .95
Plate baffle . . . . . . . . . . . . . . . . . . . . .39 pV-value . . . . . . . . . . . . . . . . . . . . . . .8 Smallest detectable partial
PNEUROP . . . . . . . . . . . . . . .165 – 168 Quadrupole mass spectrometer . . . . .89 pressure ratio . . . . . . . . . . . . . . . . . .95
PNEUROP flanges . . . . . . . . . . . . . . .68 Quadrupole, design of the sensor . . . .90 Sniffer technology . . . . . . . . . . . . . .118
Poiseuille flow . . . . . . . . . . . . . . . . . .12 Quadrupole, gas admission / Software for TRANSPECTOR . . . . . .102
Poisson's law . . . . . . . . . . . . . . . . . .11 pressure adaptation . . . . . . . . . . . . . .93 SOGEVAC pumps . . . . . . . . . . . . . . .18
Positive pressure methode Quadrupole, measurement system Solvents . . . . . . . . . . . . . . . . . . . . . .146
(leak detection) . . . . . . . . . . . . . . . .106 (detector) . . . . . . . . . . . . . . . . . . . . . .92 Sorption pumps . . . . . . . . . . . . .45, 177
Pre-admission cooling (roots Quadrupole, separating system . . . . .91 Specific volume of water vapor .147, 163
pumps) . . . . . . . . . . . . . . . . . . . . . . .27 Quadrupole, specifications . . . . . . . . .94 Spinning rotor gauge (SRG) . . . . . . .75
Precision diaphragm vacuum gauge . .72 Qualitative gas analysis . . . . . . . . . .100 Spray technique (Helium) . . . . . . . . .117
Pressure . . . . . . . . . . . . . . . . . . .7, 168 Quantitative gas analysis . . . . . . . . .101 Sputter ion pumps, Instructions
Pressure and temperature as Quantity of gas (pV value) . . . . . . . . . .8 for operation . . . . . . . . . . . . . . . . . .140
function of altitude . . . . . . . . . . . . . .155 Quartz crystals, shape of . . . . . . . . .121 Sputter pumps . . . . . . . . . . . . . . . . . .46
Pressure converter . . . . . . . . . . . . . . .92 Rate watcher . . . . . . . . . . . . . . . . . .120 Sputtering . . . . . . . . . . . . . . . . . . . .129
Pressure dependence of the Reduction of adsorption capacity . . .139 Sputtering (cathode sputtering) . . . .129
mean free path . . . . . . . . . . . . .145, 154 Reduction ratio . . . . . . . . . . .24, 25, 137 Sputter-ion pumps . . . . . . . . . . . .46, 47
Pressure difference oil supply . . . . . . .19 Refrigerator cryopump . . . . . . . . .49, 51 SRG (spinning rotor gauge),
Pressure lubrication by geared Regeneration time . . . . . . . . . . . . . . .53 VISCOVAC . . . . . . . . . . . . . . . . . . . . .75
oil pump . . . . . . . . . . . . . . . . . . . . . .19 Relative ionization probability (RIP) . .98 Stability for noble gases (sputter ion
Pressure measurement Residual gas composition pumps) . . . . . . . . . . . . . . . . .46, 47, 48
direct / indirect . . . . . . . . . .71, 179, 180 (spectrum) . . . . . . . . . . . . . . . . . .43, 44 Standard pressure . . . . . . . . . . . . . . . .7
Pressure measurement, depending on / Response time of leak detectors . . . .117 Standards in
independent of the type of gas . . . . . .71 Reynold's number . . . . . . . . . . . . . . .12 vacuum technology . . . . . . . .171 – 173
Rigid envelope . . . . . . . . . . . . .118, 119 Static expansion method . . . . . . .81, 82

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Steam ejector pumps . . . . . . . . . . . . .40 Vacumm meters, instructions on


Storage under pressure installing . . . . . . . . . . . . . . . . . . . . .140
(bombing test) . . . . . . . . . . . . . . . . .119 Vacuum coating techniques . . . . . . .128
Stray magnetic field . . . . . . . . . . . . . .47 Vacuum control . . . . . . . . . . . . . . . . .70
Stray magnetic field Vacuum equipment, Instructions for
(sputter ion pumps) . . . . . . . . . . . . . .47 operation . . . . . . . . . . . . . . . . . . . . .134
Sublimation pumps . . . . . . . . . . .46, 47 Vacuum gauge contant . . . . . . . . . . . .78
Symbols and units, Vacuum method (leak detection) . . .107
alphabetical list . . . . . . . . . . .165 – 170 Vacuum physics . . . . . . . . . . . . . . . . . .7
Symbols used in vacuum Vacuum pumps, literature
technology . . . . . . . . . . . . . . .1572, 153 references . . . . . . . . . . . . . . . . . . . .174
Temperature comparison and Vacuum pumps, survey,
conversion table . . . . . . . . . . . . . . . .154 classification . . . . . . . . . . . . . . . .16, 17
Temperature in the atmosphere . . . .155 Vacuum ranges (Pressure ranges)
Terms and definitions . . . . . . . . . . . .13, 56, 57, 145, 161, 162
(leak detection) . . . . . . . . . . . . . . . .106 Vacuum regulation . . . . . . . . . . . . . . .70
Test gas accumulation . . . . . . . . . . .119 Vacuum symbols . . . . . . . . . . .152, 153
Test leaks . . . . . . . . . . . . . . . . . . . . .113 Vacuum coating technology . . . . . . .128
Thermal conductivity vacuum gauge, Values of important physical
constant / variable resistance . . . . . . .76 constants . . . . . . . . . . . . . . . . . . . . .143
Thermal conductivity vacuum Valves . . . . . . . . . . . . . . . . . . . .67, 178
gauges . . . . . . . . . . . . . . . . . . . . . . . .76 Van der Waals' equation . . . . . . . . . . .11
Thermal evaporator (boat) . . . . . . . .128 Vapor density of water . . . . . . .147, 164
THERMOVAC . . . . . . . . . . . . . . . . . .75 Vapor pressure . . . .7, 39, 160, 161, 164
Thickness control with quartz Vapor-jet pumps . . . .38, 39, 40, 41, 139
oscillators . . . . . . . . . . . . . . . . . . . .120 Venturi nozzle . . . . . . . . . . . . . . . . . .38
Thickness measurement . . . . . . . . . .120 Viscous (continuum) flow . . . . . . . . .12
Thin film controllers . . . . .120, 127, 181 VISCOVAC vacuum gauge . . . . . . . .775
Throtteling of pumping speed Vitilan, Viton . . . . . . . . . . .68, 149, 161
when using condensers . . . . . . . .34, 35 Volume . . . . . . . . . . . . . . . . . . . . . . . .8
Time constant . . . . . . . . . . . . . .62, 116 Volumetric efficiency (roots pumps) . .24
Titanium sublimation pump . . . . . . . .46 Volumetric flow . . . . . . . . . . . . . . . . . .8
Titanium sublimation pumps, Water jet pumps . . . . . . . . . . . . . . . .40
Instructions for operation . . . . . . . . .140 Water ring pumps . . . . . . . . . . . . . . .18
Torr and its conversion . . . . . . . . . . .142 Water vapor tolerance . . . . . . . . . . . .23
Total pressure . . . . . . . . . . . . . . . . . . .7 Web coating . . . . . . . . . . . . . . . . . . .130
Transfer standard . . . . . . . . . . . . . . . .81 Wet processes . . . . . . . . . . . . . . . . . .58
Transmitter . . . . . . . . . . . . . . . . . . . .75 Working pressure . . . . . . . . . . . . . . . .7
TRANSPECTOR . . . . . . . . . . . . . . . . .89 Working ranges of vacuum pumps . .161
Triode sputter ion pumps . . . . . . . . . .47 X-ray effect . . . . . . . . . . . . . . . . . . . .78
TRIVAC pumps . . . . . . . . . . . . . . . . .19 XTC, XTM . . . . . . . . . . . . . . . . . . . .127
Trochoid pumps . . . . . . . . . . . . . . . .21 Zeolith . . . . . . . . . . . . . . . . . . . . . . .45
Tuning / adjustment and Z-Match technique . . . . . . . . . . . . .122
calibration of leak detectors . . . . . . .112
Turbomolecular pumps . . . . . . . .41, 176
Turbomolecular pumps,
Instructions for operation . . . . . . . . .138
TURBOVAC pumps . . . . . . . . . . . . . .43
Turbulent flow . . . . . . . . . . . . . . . . . .12
Types of leak . . . . . . . . . . . . . . . . . .104
Types pV flow . . . . . . . . . . . . . . . . . .12
UL 200, UL 500 . . . . . . . . . . . . . . .114
Ultimate pressure . . . . . . . . . . . . . . . . .7
Ultra high vacuum . .11, 13, 60, 61, 178
ULTRALEN . . . . . . . . . . . . . . . .39, 161
Units, symbols . . . . . . . . . . . .165 – 170
U-tube vacuum gauge . . . . . . . . . . . .74 D00

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