Académique Documents
Professionnel Documents
Culture Documents
267-306~1996
Pergamon
Copyright 1996ElsevierScienceLtd
Printedin Great Britain.All rightsreserved
0360-1285/96$29.00
PII: S0360-1285(96)00008-1
CONTENTS
I. Introduction
1.1. Purpose and Description
1.2. Literature Overview
1.3. Importance of Particle-size Measurements
1.4. Extent of paper
1.4.1. Excluded techniques
1.4.2. Included techniques
2. Important Elements in Particle-size Measurement
2.1. Description of Particle Diameter and Shape
2.2. Particle Size Distribution Functions
2.3. The Gaussian Nature of Laser Beams
2.4. Spherical Versus Nonspherical Particles
2.5. Nonintrusive Versus Intrusive Methods
2.6. Other Optical Particle Sizing Concerns
2.6.1. Refractive index
2.6.2. Velocity measurements
2.6.3. Particle number density
2.6.4. Window access
3. Theories Used in Laser-based Particle Sizing
3.1. Lorenz-Mie
3.2. Generalized Lorenz-Mie
3.3. Fraunhofer Diffraction
3.4. Geometrical Optics
4. Single-Particle Counters (SPC)
4.1. Overview
4.2. Amplitude-dependent Methods
4.2.1. Absolute intensity
4.2.2. Intensity-ratio technique
4.2.3. Dual-beam sizing systems
4.2.4. Top-hat beam technique
4.3. Amplitude-independent Methods
4.3.1. Phase-Doppler analyzers
4.3,2. Projected grids
4.3.3. Displacement
4.3.4. Visibility
4.3.5. Miscellaneous particle analyzers
5. Ensemble Methods of Size Analysis
5.1. Fraunhofer Diffraction Based
5.2. Transmission Based
5.3. Comparisons Between Different Size Analyzers
267
268
268
269
270
270
271
272
273
273
275
276
276
277
277
278
278
279
279
280
280
281
281
282
283
283
283
284
285
286
287
288
288
291
292
292
294
296
296
297
298
268
Roman
b
d
dlo
d20
d21
d30
d31
d32
d43
dd
da
ds
dst
dF
dM
Dr
e
f
f(d)
fa
fd
F
I
I(0)
I0
I(s)
/max
Imin
JI
m
m'
n
N
N
r
R
R
Letters
measure of spread in particle sizes
equivalent spherical particle diameter
arithmetic mean diameter
surface mean diameter
surface diameter
volume mean diameter
volume diameter
Sauter mean diameter
weight mean diameter
drag diameter
projected area diameter
sieve diameter
Stokes' diameter
Feret's diameter
Martin's diameter
radial distance of the particle in the focal
plane from the optical axis
base of the natural log
focal length of the receiving lens
particle size distribution function
aniosotropic scatter frequency
LDA scatter frequency
function used in PDPA response to describe
system geometry
intensity of the scattered light
scattering intensity at a zero angle
laser beam intensity at a reference point
laser beam intensity at a distance s from a
reference point
maximum scatter intensity
minimum scatter intensity
first-order spherical Bessel function
refractive index of the particle
refractive index of the medium
characteristic of the particle material
relative refractive index (m/m')
number of particles in a sample
particle radius
percentage undersized
radial distance in focal plane
1. INTRODUCTION
1.1. Purpose and Description
Laser-based techniques for particle-size measurement are important in a variety of industries and to
researchers in many different fields. Examples include
combustion of pulverized coal and liquid fuels, spray
characterizations, analysis and control of particulate
299
299
300
300
301
301
301
301
s
distance along the path of the laser
S(d)
separation of refracted and reflected pulses
vp
particle velocity
vg
gas phase velocity
V
particle visibility
We
Weber number
x, y, z Cartesian coordinates
X
dimensionless radius used in Fraunhofer
diffrraction scattering
Greek letters
i5
fringe spacing of crossed LDV beams
0
half angle between the two cylindrical waves
00
beam convergence/divergence angle
Oi
incident angle
Ot
transmitted angle
~
optical thickness or opacity
laser wavelength
#
mean particle size
Ps
gas phase density
~r
standard deviation of size distribution
%
surface tension of a droplet
rR
refraction angle
rL
reflection angle
269
270
Applications in area
Combustion
Sprays
Medicine/pharmaceuticals
Paints
Metallic powders
Agriculture
Pollution control
Foods and consumer products
Particle-size measurements are important to researchers, scientists and engineers in both the research-anddevelopment and industrial communities working in
a broad range of disciplines. Table 1 describes some
of the many fields in which particle-size analysis is
essential and lists some of the primary uses of particlesizing methods in these areas. For example, particle
size and number density are critical parameters in
two-phase combustion experiments and modelling,
since the particles or droplets represent the energy
source in reacting two-phase flows. Thus, knowledge
of the particle size distribution is a key parameter
in modelling radiative heat transfer, as well as in
characterizing other properties, such as droplet
evaporation rates and total droplet/particle burnout.
The particles and the associated heat release also have
a large impact on the flow field in the combustion
region. Smoot and Hill 154list particle dynamics as one
of nine critical areas in fundamental combustion
research and consider it one of the most critical areas
needing research. Holve et al) present an overview
of measurement techniques suitable for particle-size
measurements in fossil fuel systems and discuss the
requirements of optical sizing methods for application
in high temperature environments. Specific issues
discussed by the authors as they apply to sizing
systems suitable for use in reacting environments
include number density requirements, size range, shape
insensitivity, velocity and refractive index effects.
Chigier, 3s in Combustion Measurements, discusses
recent advances in particle-sizing instrumentation and
the importance of particle size and velocity measurements. Issues addressed in this book include the
interactions of particles with the flow field, measurements in large-scale combustion environments, and
detailed characterizations of single or groups of
reacting particles. In a recent paper, Bachalo l reviews
several techniques suitable for measurements in
multiphase flows. This paper specifically addresses
the measurement of the turbulence parameters in
two phase flows and discusses several types of
instrumentation suitable for work with these types
of environments. Bachalo II has also addressed the
topic of the combustion of liquid fuels and reviews
271
ill
I m'n l
I
SPC
I
Sieving
Sedimentation
lmpactors
Electrical
Photography
Microscopy
Holography
PIV
Absolute Intensity
Intensity Ratio
Diffraction
Dual Beam
PCS
Transmission
Visibility
Phase Doppler
DLS
DCW
Projected Grids
Shadow Doppler
Pulse Displacement
Polarization
272
Amplitude independent
Absolute intensity
Intensity ratio
Top-hat
Dual beam
Phase-Doppler
Projected grids
Pulse displacement
Visibility
Dual-cylindrical wave
USED
Industrial
Lab
Developmental
PARTICLE
Opaque
Transparent
Nonspherical
Reacting
FEATURES
Velocity
Accuracy
Size range
Concentration
Refractive
index
dependent
PhaseDoppler
DCW
Some
Yes
No
No
No
Yes
Yes
Yes
No
Yes
Yes
High
Large
High
Yes-trans.
No-opaque
Pulse
displacement
Projected
grids
Visibility
GVG
No
No
Yes
No
Yes
Yes
No
Yes
No
No
No
Yes
Yes
Yes
No
Yes
No
Yes
No
Yes
Yes
No
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
No
Yes
Yes
Unknown
Large
High
Yes
Yes
Moderate
Large
Moderate
Yes
Yes
Low
Moderate
Low
No
Yes
Moderate
Moderate
Low
No
Yes
Unknown
Small
High
Yes
273
USED
Industrial
Lab
Developmental
PARTICLE
Opaque
Transparent
Nonspherical
Reacting
FEATURES
Velocity
Accuracy
Size range
Concentration
Refractive
index
dependent
Absolute
intensity
Intensity
ratio
Top-hat
Dual b e a m
Diffraction
Transmission
Yes
No
Yes
Yes
No
Yes
Yes
No
Yes
No
Yes
Yes
No
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
No
Yes
Yes
Yes
Moderate
Moderate
High
Yes
No
Moderate
Moderate
High
Yes
Yes
Moderate
Moderate
Moderate
Yes
Yes
Moderate
Moderate
Moderate
Yes
No
High
Large
High
No
No
Low
Large
High
No
Yes
Yes
'Yes
Yes
Yes
High
Low
Large
Small
Moderate
Accuracy
Concentration (#/cc)
better than 5%
less than 15%
NA
NA
5-15 %
NA
NA
0.5- I0 000
0.5-100
0.5-1000
NA
103-106
needle-shaped
sharp-edged
freely developed geometric shape
a branched crystalline shape
thread-like
plate-like
equidimensional irregular shape
lacking any symmetry
rounded, irregular shape
global in shape
D. L. Black et al.
274
Name
Definition
dd
Drag diameter
dst
Stoke's diameter
da
Projected area
dF
Feret's diameter
dM
ds
Martin's diameter
Sieve diameter
j.k.
Name
dl0
1,0
d20
2,0
d3o
3,0
d21
2,1
Arithmetic mean
diameter
Surfacemean
diameter
Volume mean
diameter
Surfacediameter
d31
3,1
Volume diameter
d32
3,2
d43
4,3
Sauter mean
diameter
Weight mean
Description
Normal average particle diameter of the size distribution
Diameter of a sphere with the average surface area of
the particles in the size distribution
Diameter of a sphere with the average volume of the
particles in the size distribution
Diameter of a sphere having the surface area of
the average particle size in the distribution
Diameter of a sphere having the volume of the average
particle size in the distribution
Diameter of a sphere with the equivalent surface to
volume ratio as all the particles in the size distribution
Diameter of a sphere having the average weight of all
the particles in the size distribution
275
mean diameter
standard deviation
Normal
(d-ju)2
f ( d ) = -~2 exp[- - ~ - -
#=~S'
0.2
Log-normal
f(d) = J
41nd-lnu)"l
~2T~exp[21-Zi~----.J
#=X
if2
Rosin-Rammler
R = 100exp(-bd")
b
d
f(d)
n
1
l +
~ = zTgP(~
= ~(dl-u)
N-I
1)
N number of samples.
R percentage undersized,
# mean of the distribution.
o- standard deviation of the distribution.
'~(d,-u) 2
(1)
276
277
278
Beam
Laser
SpLtter
/f
X~,Co~r
Sig~
Processing
Jln/terference ~
(samplevolume)
Fringes
Fig. 2. General optical arrangement for generating interference fringes in a small sample volume using
crossed laser beams.
2.6.1. Refractive index
1(s) = I~ e x p ( - ~ s )
(2)
279
280
I0 -,t.
plane wav.~.
~.Top-hat
. / ~ ] J(",,,b,~,
L0 -~l
I. t
~010 -'~.
0
J-
I0 -l*.
beam
7i:
I~ Gausllian
beam
10 -is.
,
. . . . . .
10
Particle
100
diameter
0zm)
Fig. 4. Effect of beam shape on the collected intensity. Solid line: plane wave, stars: top-hat beam, dashed
line: Gaussian beam.59
the window where the laser beam passes through.
This could have a significant impact on the optical
configuration at the sample volume, disturbing the
measurement at that location. It is essential in systems
sensitive to the intensity of the illuminating laser to
use stable detectors and lasers. Instability from this
source could have a significant impact on the measured
results.
3. THEORIES USED IN LASER-BASED PARTICLE SIZING
x=
~rmd
(3)
281
z(o)
(4)
282
0.8
0.6
0.4-
0.2"
A ~ ~ A A A A A A A A a A - - A A ~
0
0.00
2.00
~ ~
4.00
6.00
. . . . . . . .
8.00
10.00
Lens
I
Laser
t
~X
|l
Single Particle
Difl~efion t
Pa~rn
X = -~7-.
(5)
283
l Reflected
,~0~/
OJ
DirectlyTransmitted
(Refracted,
Internal
Reflection
Fig. 7. Ray-tracing diagram for a single light ray interacting with a spherical particle.
sin Ot = N.
sin Ot
Single-Particle Counters (SPC) are a broad classification of particle-sizing methods. These methods
typically incorporate small sample volumes into
the instrumentation to measure one particle at a
time. The sample volume size determines the largest
measurable particle size and number density of the
technique. Methods that fall in the SPC category can
be divided into two types: amplitude dependent and
amplitude independent.
(6)
4. SINGLE-PARTICLECOUNTERS(SPC)
4.1. Overview
284
Measurement Volume
Block
285
I00(~
0
a.
U
III
~
t_
1C~)
0.01
0.0001
.00
10.00
100.00
1000.00
nd
286
Laser
Dispersion MirrorExpander
Prism
Beam
Expander^
Polarization!
Rotator
Focusing
Lens^
Sample
Volume
PMT
Fig. 10. Optical configuration of the PIR technique.6
x~/~~mple
\
Volume
~R~eFocalPlane
SizingBeam
Fig. 11. Optical setup of the sample volume using a two-color method.
high as 40% for latex particles in air and approach
20% for latex in water. Due to the possibility of large
errors and the need to measure the intensity at two
separate locations, this method is not widely used for
particle analysis.
In a related method, called the Polarized Intensity
Ratio (PIR) technique, the ratio of the polarized light
intensity scattered from two different coaxial beams
illuminating a particle is measured and used to
determine the particle size. Azzazy and Hess 6 used
two coaxial beams of different wavelengths, polarized
in different directions. The measured light-scattering
signal of the two beams at 30 degrees from the
forward axis contained the information necessary to
determine the particle size. This is possible since
Lorenz-Mie theory contains information on both the
parallel and perpendicular polarization states of the
scattered light. The ratio of these two parameters
gives a unique curve that is only a function of particle
size. A schematic showing the implementation of this
optical system using an argon-ion laser is shown in
Fig. 10. Azzazy and Hess 6 compared measurements
taken using this technique with data from a pointerbeam instrument similar to one discussed in the
following section. From their data, they concluded
that the same type of oscillatory error is present in
the PIR technique as in the standard intensity-ratio
implementation previously discussed. They also found
SizingBeam
Particle
287
~ / L
DopplerSignal
A
)V Beams
Scatter Sianal
Sizing Beam
From
Fig. 12. Top-hat beam sample volume cross-section and light scattering signals. 63
288
Measurement Volume
!
Transmitter
,
Laser Beam
Beaia S p l i t t e r
~ e c e i v e r
DIET 1
4;
OET2
DET @
^ ^.A.AA .AA
vvVVVVV
AAAAAAA,,^
- vvv_VVV
,
fi A A A A A
"vVVVVv
289
3;50300"
250"
200'
I
a.
150
100'
50
0
d min
d max
Diameter (d)
Fig. 15. Representative response function for a PDPA system using three detectors.
interference patterns in other directions in the sample
volume can be established using different wavelengths.
This configuration allows particle-sizing systems that
measure one, two, or three velocity components.
Regardless of the velocity components measured,
only a single set of crossed beams is needed for
particle sizing.
To size particles, the PDA relies on the measurement of the spatial frequency of the interference
fringe pattern produced by the scattered light from
the particle. The interference fringe pattern produced
by the reflected and refracted rays from the particle is
a function of the optical parameters of the system, the
refractive index of the particle and the particle
diameter. The far-field interference pattern from the
light scattered from the particle at any particular
angle can be characterized by an amplitude and a
phase. In practice, the phase difference between the
light-scattering signal at two or more spatial locations
in the receiving optics is determined by finding the
time difference between the zero-crossings in the
Doppler signal between two detectors and dividing by
the measured Doppler period. The measured phase
difference, illustrated in Fig. 14, of the light-scattering
signal between the detectors can be linearly related to
the particle diameter based on geometrical optics.
Using this approach, the response function of a
PDPA instrument can be given by the following linear
relationship. 2
d = A__~__~
2zrF "
(7)
(8)
290
291
Laser Sheet
[~
i S(d)
X-.~-
)J
Reflected Ray
Refracted Ray
Fig. 16. Particle scattering refracted and reflected light in an angle O.s
292
d?
I '~
ii I ~1
$1 ,s ~S
Laser Diodes
Lens 1
Mask
'0
,~,
Detector
iI
01
,.,,-~ o2
Lens 2
%
Fig. 17. Diagram of the LMFV optical configuration.TM
method, the LDA laser beams pass through the
receiving optics where they are not blocked, but are
imaged with a photo diode array placed in the focal
plane of the collection optics. Size information is
found by analyzing the temporal signal of the diode
array to define the shadow of the particle passing
through the sample volume and therefore its shape.
This technique is useful for sizing nonspherical
particles and is insensitive to complications from the
index of refraction. The accuracy of the shadow
Doppler technique has been addressed by Hardalupas
et al. 73 They show that the sizing accuracy for both
transparent and opaque particles between 30 and
140#m is better than 10% of the measured particle
size for particles passing through the focal plane of
the transmitting lens. Additional error is encountered
from particles being imaged that are passing outside
the focal plane of the sample volume. This technique
has also been applied to a pulverized coal, laboratoryscale furnace to measure simultaneous size and
velocity information by Maeda et aL 11s.
4.3.3. Displacement
The pulse displacement technique uses a laser sheet
to measure particle size and velocity. The method is
capable of measuring particles from as small as a few
microns to as large as several millimeters in diameter.
The details of the technique were first described in
papers by Hess and Wood ys and Lading and Hansen. m
Additional details are given in two subsequent papers
by Hess and Wood. 79's Particle size is determined by
measuring the time between the reflected and refracted
rays scattered by the particle as it passes through a
laser sheet. With this information and knowledge of
the particle velocity, found by either traditional LDV
techniques or by measuring the transit time of the
particle, the separation distance between the refracted
and reflected pulses, S(d), can be calculated. S(d) is
then related to the particle diameter by
d =
2S(d)
cos rR + cos r L
(9)
angles, respectively. A schematic of the light scattering based on geometrical optics for sizing a sphere
using the pulse displacement technique is shown in
Fig. 16. This method of particle analysis depends on
the measurement of the correct particle speed to
determine the correct separation between the pulses.
For particles with unknown or varying trajectories,
this presents a problem in that particles not moving
perpendicular to the laser sheet will be inaccurately
sized. The change in the particle's refractive index
also represents a potential source of error, since the
method depends on measuring the refracted and
reflected light from the particle. The sizing limits
for this technique range from 0.2 to 1.5 times the
thickness of the laser sheet up to several hundred
times the sheet thickness, depending on the specific
optical configuration used to implement the technique.
In a technique that can also be described in terms of
displacements. Nakatani et a1.124 developed what they
call a laser three-focus velocimeter. A schematic of
this device is shown in Fig. 17. This device uses an
array of three laser diodes focused at the same
location to measure the particle size and velocity.
This is done by focusing the parallel beams to a set of
three parallel focal points. Since the spacing of the
focal points is known, the particle velocity can be
calculated from the time between the light-scattering
pulses measured as the particle passes through these
points. With this information, the particle size is
found by using two detectors and measuring the
refracted light from the particle. The delay time
between these two detectors can then be related to
particle size. This method has the same potential
problems with particle trajectories and refractive
index as the technique previously discussed.
4.3.4. Visibility
The concept of visibility, given the symbol V, as
related to particle sizing was theoretically established
by Farmer 51 in 1972 and later verified experimentally
by Farmer s2 and Hong and Jones. 13 By determining
the maximum and minimum scattered intensity from
a particle in the fringe pattern of an LDA system, the
293
A_
0.6
0 . 4 . ~
0.2
0
0.00
'
'
'
I '
2.00
4.00
6.00
8.00
I0.00
nd
-'b-
Slotted Mirror
Laser
Cell
Smnple Volume
t
~
Forward-Scatter
CollectionLenses
Slit
iI
I
mm~.mm
Slit
Fig. 19. Optical system for back and forward-scatter visibility measurements) 42
(10)
294
D e t e c t o r 1'1
Laser
Rouchi
Grafinl
"" ~
.,
..........
I ~ X
D e t e c t o r 1'2
Loser
Beom-Exponder
Beom-Splitter
Mirror
295
Cytindn~colLens
Beom-Merger
Mirror
MovingPortiele
Loser Beoms
Detector
C y h n d r i c ~
Fnnges
Monosize Portictes
Fourier
Transform
Beam
i
Light
,~
De~tors
in Focal
Plane
m cos O
d
2X/2(1 +cos~b)[1 + m 2 - m v / 2 ( 1 +cos~b)] zz
(11)
where m is the index of refraction and 9, ~ and z
describe the physical geometry of the system, as
shown in Fig. 21. In the system described above, the
particle size in the dual-cylindrical wave method is
296
Traction
Volume
Fig. 23. Sample volune comparison between diffraction and SPC instruments. 39
297
298
D.L. Black et aL
80-
+
Powder manufacturer supplied
---o----Insitec ensemble diffraction (EPCS)
=
Impactormeasurements
=
~ / rv~
/ / /~"
20-
0.1
10
I00
Particle Diameter ~ m )
Fig. 25. Comparison between several types of particle-sizing instrumentation on measurements of silicon
dioxide powder.
100
---0- I.AStER-DIFF'RAClION~
p~s~-ooPpt~ srs suo
SMD J
80
~eo
t
~,
40
2o
r,,,
hi
I--
-5
- 14
- t3
/2
-1
t~
299
6. A P P L I C A T I O N S OF LASER-BASED SYSTEMS
300
'
'
'
'
'
'
'
'
'
'
'
'
'
'
'
'
Sieving medlam
particle diameter
300
---<>--Ensemble
scattering
angular light
median
250
a
,m
200
150
100
50
....
I ....
I * , * , l , , , , l l l l l l
J , , , I
....
Run number
Fig. 28. The volume distribution's mean particle diameter for sieving and ensemble angular light scattering
over eight test runs. 76
employing Fraunhofer diffraction, such as the
Microtrac, Coulter and Malvern particle analyzers,
have been used for some time in a large number of
industrial, lab-based environments. 123 These techniques have enjoyed wide acceptance for a number of
years because of their ability to measure powder and
droplet size distributions easily and consistently.
Traditional particle analyzers consisted primarily
of off-line instruments and have been used for quality
control and laboratory analysis. Through recent
development of SPC and ensemble diffraction
systems, laser-based instruments are also now
capable of providing real-rime, on-line information
suitable for process control in manufacturing processes. Wedd 175 illustrates the increasing focus
on particle measuring systems designed especially
for the industrial community. Poh1138 and Weiner and
Fairhurst 176 discuss the selection of instrumentation
suitable for use in a particular industrial application.
Issues such as size range, imaging vs. nonimaging
systems, diffraction vs. single-particle methods, informarion content of the measurement, time involved in
sampling and measuring, as well as use of nonoptical
techniques among other concerns, are discussed
specifically in relation to the application of sizing
instrumentation in industrial environments.
6.1.1. Manufacturing processes
301
7. CONCLUSIONS
Acknowledgements--This
REFERENCES
302
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5.
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303
304
106.
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