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Scanning Electron Microscopy

David Muller 2008


Electron Energy Loss Spectrum of SiO2

Most likely energy transfer is ionization of valence electrons


8
10

Incident Beam
7
10
Valence Excitations
Intensity (arb. units)

6
10

Si L edge
5
10
O-K edge

4
10

0 100 200 300 400 500 600 700


Energy Loss (eV)
David Muller 2008
Path of the Electron Beam

BS2 SE2 SE1

David Muller 2008


Kanaya-Okayama Depth Penetration
Formula

1.67
0.0276 A E
R= ______________ μm
0.89
(Z ρ)

R= Depth Penetration
A= Atomic Weight (g/mole)
E= Beam Energy (KV)
Z= Atomic number
ρ = density (g/cm )2

David Muller 2008


The Affect of Accelerating Voltage

Primary Beam
30KV 15KV 5KV 1KV .5KV

.01 μm 35 A
.16 μm (100A)
.99 μm

3.1 μm
Depth Penetration in Iron

(predictions from the KO formula)


David Muller 2008
Interaction Volume vs Accelerating Voltage

5 kV
15 kV

25 kV

Better control of where SE, BSE and x-rays are produced at lower beam voltages

David Muller 2008


Interaction Volume –Sample Composition
(20 kV incident beam in all 3 cases)

Silver
Iron

Pear to apple-shaped
Carbon

David Muller 2008


Secondary Electrons

final lens

SE3

SE1 BSE
SE2

specimen

David Muller 2008


Electron Interactions (Between Primary Beam and Sample)

• SE1- at point of primary interaction


• SE2- away from initial interaction point
• SE3- by BSE outside of sample
• BSE1- at point of primary interaction
• BSE2- away from initial interaction point

David Muller 2008


Lateral Distribution of SE

SE1

SE Escape Depth
SE2A

SE1 > 100KX Total Beam Penetration Volume


SE2A- 50KX
SE2B< 15KX SE2B

David Muller 2008


Lateral Distribution of BSE

BS1

BS2A Escape Depth


BS2A BS2B Escape Depth

BS2B

David Muller 2008


One Primary Electron In Can Create Several
SEs Out at Low Accelerating Voltages

100
Angstroms

SE out
Secondary Electron
Yield Coefficient
δ=
PE in
David Muller 2008
Energy Distribution of Emitted Electrons

SE BSE
# of electrons
collected

Auger
0 50 eV 2 kV EPE
electron energy

SE out
Secondary Electron
Yield Coefficient
δ=
David Muller 2008 PE in
Secondary Electron Yields
Carbon-contaminated Cleaned in-situ

As-received samples are all coated with a carbon contamination layer


Overall scaling factor is from the different backscattering responses of the substrate
David Muller 2008
Charge Neutralization
Electron Yield δ= # SE out / # Inc e- in

Sample charges +ve


1.4 (increases landing energy
1.2
Of incident electrons)
δ

0.8

0.6
Sample charges –ve
(reduces landing energy
0.4 Of incident electrons)
0.2

0
0 EC EC KV
KV 1 2

Incident Beam Voltage

David Muller 2008 Q: If sample charges, does it get brighter?


Voltage Contrast with SE
(SE have low energies so are easily deflected by small voltages)

The floating end of the via chain is bright


because of trapped negative charge causes
secondary electrons to be repelled.

The remainder of the chain is neutral, and thus


darker.

(http://www.acceleratedanalysis.com/hepvc.html)
David Muller 2008
High Vacuum E.T. Secondary
Electron Detector

Light guide Faraday cage


(-150 - +300 V)

Phosphorous
screen (Al-coated)
(10 kV)
glass target

Scintillator
Photomultiplier
David Muller 2008
Secondary Electron Detectors

TLD

PMT

Internal
E.T. SED
Lens

Specimen

David Muller 2008


Lens Modes of a Modern SEM

Field-Free Operation Immersion Lens

Large area, lower resolution Small area, high resolution

David Muller 2008


TLD in BSE Mode

• Within-the-lens
detector is
part of the final
lens
SE3
• Bias voltage
down to -150V SE BSE

Specimen

David Muller 2008


Topography Affects Secondary Electron Emission
(Angle of Incidence)

David Muller 2008


Scanning Action of the
Electron Beam in a 3-D
Specimen

David Muller 2008


Location of Detector Leads to Shadowing

+300 V

SE-detector

B
A C

Increasing the detector bias will wash out the shadows


David Muller 2008
What Is “Reality” in the SEM ?

David Muller 2008


What Is “Reality” in the SEM ?

Previous image turned upside down.


We need to know where the detector is to tell bumps from pits!
David Muller 2008
Why Edges Appear Brighter

David Muller 2008


Edge Effect at Lower Voltage

David Muller 2008


Edge Effects on a Sphere

A 250

200

2nd e- Intensity
150

100
B

50
0 200 400 600 800 1000
Distance (microns)

David Muller 2008


Example of Sample charging in a
Secondary Electron Image

Charging is worse
On this face
As more secondaries
escape

David Muller 2008


A Line Profile on a Semi-conductor
Line

One Micron SiO2 in Si

The E-Beam line profile of the specimen

Where do you measure “One Micron” ?


David Muller 2008
A Line Profile on a Semi-conductor
Line

.99 μm
One Micron SiO2 in Si

1KV

A 1 KV bean has minimal beam penetration and can give


an image that is closer to ‘reality’.

David Muller 2008


A Line Profile on a Semi-conductor
Line

.74uM
One Micron SiO2 in Si

5KV

A 5KV beam penetrates deep into the specimen


which gives the appearance of the peaks
being closer together

David Muller 2008


Line Profiles on the Same Sample Can
Change with Accelerating Voltages

.99 μm .92 μm

1KV 2KV

.85 μm .74 μm

3KV 5KV

This was a 1 μm line


David Muller 2008
Secondary Electrons

final lens

SE3

SE1 BSE
SE2

specimen

David Muller 2008


Angular Distribution of BSE

• Normal angle of
incidence

• Greater angle of
incidence

David Muller 2008


Angular Distribution of BSE

• Contrary to SE images, BSE images can have


dark edges

David Muller 2008


Electron Emission Coefficient Vs.
Atomic Number at 20 KV

1
Total

• Electron BSE
Emission
Coefficient
.2 SE

20 80
• Atomic Number

David Muller 2008


SE Electron Emission Coefficient Vs
Atomic Number at Various KV

2KV
1
• Secondary 5KV
Electron
10KV
Emission
Coefficient 15KV
.2 20KV

20 80
• Atomic Number

David Muller 2008


SE Emission Coefficient Vs. KV at
Various Atomic Numbers

• Secondary
Electron
Emission AU
Coefficient AL
.2
C

5 15 25
• Accelerating Voltage in KV

David Muller 2008


Z Dependence of BSE

David Muller 2008 From “Scanning Electron Microscopy and X-Ray Microanalysis”, Goldstein et al, 3rd ed. Chap 3
Tilt Dependence of BSE

David Muller 2008 From “Scanning Electron Microscopy and X-Ray Microanalysis”, Goldstein et al, 3rd ed. Chap 3
Reverse Biased S.E.D. Repulses
Secondary Electrons

-150 V

SE-detector

B
A C

David Muller 2008


Backscatter Electrons Ignore
the Bias

-150 V

SE-detector

BSE
B
A C

David Muller 2008


A Solid State BSD Can Image
Two Ways
• Elemental backscatter images are acquired by
adding detectors A+B.

• Topographical backscatter electron images


can be acquired by subtracting b from a (A-
B)

David Muller 2008


Solid State BSD

From http://www.jeol.com/sem_gde/bkscat.html

David Muller 2008


Grains in a Polished Fe-Si Alloy imaged by
Different SEM methods
-ve Biased E-T -ve Biased E-T
Noisy Backscattered Signal Secondary Electron Signal

Backscattered A+B “Composition” Signal Backscattered A-B “Topographic” Signal

David Muller 2008


Electron Channeling in a Crystal

Electron wave fields within a crystal for incident electron directions close to the Bragg angle qB. The vertical lines are the
position of the Bragg reflecting atomic planes. From H. Niedrig, “Electron backscattering from thin films”, Journal of
Applied Physics -- April 1982 -- Volume 53, Issue 4, pp. R15-R49

David Muller 2008


Electron Channeling in a Crystal

Electron Backscatter Diffraction Pattern of Germanium. Right –automatic indexing software


matches the high symmetry zone axes and spacing between them to identify the crystal type
and orientation. (University of Queensland, http://www.uq.edu.au/nanoworld/xl30_anl.html)

David Muller 2008


Electron Backscattering Diffraction Patterns
(EBSD or EBDP) for Orientational Imaging
Orientation Imaging Map (color shows grain orientation)

Boundary – Color shows angle of grain boundary

David Muller 2008 (From http://www.edax.com/technology/EBSD/OIM/intro6.html)


Sample Prep for EBSD

Damage layer must be much less than the range of the electrons

3 micron diamond polish No pattern visible 10 minutes colloidal silica Pattern IQ = 177

Pattern Image Quality


1 micron alpha alumina (IQ) = 25 30 minutes colloidal silica Pattern IQ = 224

David Muller 2008 http://www.edax.com/TSL/support/EBSD_Sample_Prep.html