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Dr Acha Hessler-Wyser
Bat. MXC 134, Station 12, EPFL+41.21.693.48.30.
Acha Hessler-Wyser
CiMe
Outline
a. b. c. d. e. f. g. h. i. j. SEM principle Detectors Electron probe and resolution Depth of field Stereoscopy Electron-matter interaction volume Secondary and back-scattered electrons Contrasts Examples Charging effects
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Acha Hessler-Wyser
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Outline
This chapter will describe the principle of a scanning electron microscope (SEM). We will start with a description of the detectors allowing signal detection, the formation of an electron probe and its influence on the spatial resolution. Then we will will define the depth of field and see how to control it, how to do stereoscopy. In order to understand the image formation and the contrasts observed on a picture, there will be considerations about the electron-matter interaction volume, and then an explanation of the origin of the secondary and back-scattered electrons (SE and BSE). This will allow us to analyse the different possible contrasts of a SEM picture, including artefacts. We will end with application examples.
Acha Hessler-Wyser
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a. SEM principle
Image formed step by step by the sequential scanning of the sample with the electron probe Image acquisition as numerical data Bulk sample Imaging the sample !surface! (from 1 nm to "1 #m depth depending on the analysed signal Contrast is due to secondary electrons (SE) emission or back scattered elctrons (or sometimes to photons, RX, absorbed current) Resolution: 1 nm to 10 nm
Acha Hessler-Wyser
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a. SEM principle
Response to incident electrons:
! Secondary electrons SE topography, low energy "0-30 eV ! Backscattered electrons BSE atomic number Z, energy " eV0 ! Auger Electrons : not detected in conventional SEM, surface analysis ! Cathodoluminescence: photons UV, IR, vis ! Absorbed current, electron-holes pairs creation, EBIC ! plasmons ! Sample heating (phonons) ! Radiation damages: chemical bounding break, atomic displacement out of site (knock-on)
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a. SEM principle
Energy spectrum of electrons leaving the sample
Secondary electrons SE Back scatered electrons BSE
Auger (secondary)electrons
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b. Detectors
a detector (eye, photographic plate, video camera... a magnification section (lenses, apertures...)
A "light" source
a sample (+ a "goniometer")
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b. Detectors
Everhardt-Thornley detector: for SE and BSE
SE: BSE:
the positive collector voltage (" +200 +400V) attracts the SE toward the detector, the 10kV post acceleration give them enough energy to create a bunch of photons for each SE. a negative collector polarisation ("-100V) repels the SE and the only BSE emitted in the narrow cone to the scintillator are detected (low collection efficiency = poor S/ N ratio).
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b. Detectors
BSE detectors
BSE Robinson detector: a large scintillator collects the BSE and guides more or less efficiently the light to a photomultiplicator !large collection angle !works at TV frequency
BSE semiconductor detector: a silicon diode with a p-n junction close to its surface collects the BSE (3.8eV/e--hole pair) !large collection angle !slow (poor at TV frequency) !some diodes are split in 2 or 4 quadrants to bring spatial BSE distribution info
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A "light" source
a sample (+ a "goniometer")
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courte focale
Spherical aberration
microscope photonique
d sph = Cs " ! 3
100
100pA 10pA
1pA 10 dd
! d d = 0.61 n"sin #
!
dg =
!
1 # ! 2" $
4I
dc h dsph 0.01
0.001
Ouverture (mrad)
Probe with coherent source: see Mory C, Cowley J M, Ultramicroscopy 21 1987 171
Intensive SEM/TEM training: SEM 11
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3. Low magnification The screen (or recording media) pixel size dscreen r#dscreen/magnification
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500nm
10 pA/10 s
good resolution, but statistical noise
10 pA/160 s
Good resolution, less statistical noise
100 pA/160 s
smal loss of resolution, still less statistical noise
1 nA/160 s
very few statistical noise, but high resolution loss!
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particles 25 nm diam., probe dia 2 nm model 100 nm diam. particles particles 100 nm diam., probe dia 2 nm
Intensive SEM/TEM training: SEM 16
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Field emission source: gun aberrations and chromatic aberration are more important
I max = cd 2 3
Tir de L.Reimer, SEM Intensive SEM/TEM training: SEM 18
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100
diamtre (nm)
100
diamtre (nm)
10
dd dch dsph 5 kV
dsph
20 KV
1 0.001
1 0.001
dsph
1 kV
0.001
Modern SEM short focus length: Csph=17 mm, Cch=9 mm, $E=1.5 eV, !=1.105 A/cm2sr
Intensive SEM/TEM training: SEM 20
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SEM: rsolution
Interaction volume versus E0
1 Penetration depth in Cu as a function of incident energy E0 and proportion of BSE (Monte-Carlo simulation)
Cu 5keV
Cu 20keV
Z = cte
1
Cu 1keV
Cu 1keV
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or
100pA
FEG?
microscope photonique 100
diamtre (nm)
microscope photonique
100
diamtre (nm)
100
10pA 1pA 10 dd dc h
10 dd
1 0.001
dch
dsph
dsph
20 KV
0.001
!=1.105A/cm2sr, $E=1.5 eV
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FE 10 5
1985
W LaB 6
Haute tension/haute rsolution: - effets de bord - dtails fins non-rsolus - fort endommagement d au faisceau
2000
0.5
10
20 30
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Short questions
1. What is a condensor lens for?
a) b) a) b) c) d) e) f) a) b) c) d) a) b) To create the image of the sample To reduce the size of the electron source The size of the probe The electron current The electron energy The aquisition device The wave length The lens aberration By reducing the electron energy By reducing the apperture size By increasing the Working Distance By removing the spherical aberration By reducing the electron current By reducing the electron energy
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d. Depth of field
Depth of field as a function of dprobe
The depth of field is the depth for which the image is focussed The depth of field increases when % decreases. Increase the working distance Reduce objective aperture size
2%& 2dA h dA
h prof .champ
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d. Depth of field
Effect of working distance (WD) and aperture on depth of field
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d. Depth of field
Light bulb filament
Rsolution "
10m 10mm 1m
1m 0. d ra
100nm
10nm
1nm
1mm
1m
Profondeur de champ h
d ra
100m
10 m d ra
10m LM !=500 nm
SEM
1m
0.1m 10
102
103
104
105
Grandissement (grossissement) G
Intensive SEM/TEM training: SEM 29
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d. Depth of field
Other examples
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d. Depth of field
Effect of the objective aperture diameter
100 !m 50 !m 30 !m
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d. Depth of field
Measuring depth of field: stereoscopy
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e. Stereoscopy
The 3rd dimension: stereoscopic vision, anaglyphs
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e. Stereoscopy
3-D reconstruction (anaglyph)
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e. Stereoscopy
3-D reconstruction
(pseudo-perspective)
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e. Stereoscopy
3-D reconstruction (grey levels)
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e. Stereoscopy
3-D reconstruction (false colors)
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e. Stereoscopy
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e. Stereoscopy
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1 kV C
BSE 10%
3 kV
30 kV
BSE 8%
BSE 5%
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C 20 keV
BSE=50%
BSE=33%
1&
U 20 keV
1&
Cu 20 keV
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10 nm
BSE=14%
BSE=34%
10 nm
10 nm U 1keV
BSE=44%
Cu 1keV
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BSE=8%
BSE=33%
200nm
200 nm
BSE=47%
Cu 5 keV
U 5 keV
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Cu 20 keV
1#m
1#m
Cu 5 keV
Cu 1 keV
Cu 1keV
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g. SE and BSE
"true" secondary electrons SE1 and "converted BSE" secondaries SE2+SE3
Various SE types from SE1: incident probe SE2: BSE leaving the sample SE3: BSE hitting the surroundings
although this signal is gathered around the probe, its intensity is only attributed to the pixel corresponding to the actual probe position
x0,y0
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g. SE and BSE
"true" secondary electrons SE1 and "converted BSE" secondaries SE2+SE3
The SE signal always contain a high resolution part (SE1 from the probe) and an average (low resolution) part from SE2+SE3!
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g. SE and BSE
Relative contribution of SE1 and SE2 (+SE3) vs primary energy
total total total
SE2 SE1
The total intensity (green and brown) is attributed to the (x,y) pixel, here at 0 nm on this 1-D model
Intensive SEM/TEM training: SEM 52
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g. SE and BSE
Yield for SE and BSE emission per incident electron vs atomic number Z
sample surface polished (no topography) and perpendicular to the incident beam direction (intermediate energy E0 # 15 keV)
):
BSE: chemical contrast for all the elements (sensitivity #DZ=0.5) A fast way to phase mapping
IBSE=Ipe$)
yield
*:&
0.28
SE: low or no chemical contrast but for light elements the topographical contrast will dominate on rough surfaces
ISE
0.11
(SE1)
Al
Ni
with * the total SE yield, *pe the yield for SE1 and *sur the SE3 yield for materials surrounding the sample (pole-pieces...)
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g. SE and BSE
Dust on WC (different Z materials)
flat material rough material low Z material low Z material
thin
low Z material
SE 25 kVBSE
Intensive SEM/TEM training: SEM 54
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g. SE and BSE
Contaminated area around a soldering spot
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g. SE and BSE
Toner particle (penetration in light material)
SE 28 kVBSE
Intensive SEM/TEM training: SEM 56
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g. SE and BSE
Topographical contrast in SE mode
Effet de l'inclinaison de la surface
penetration depth ("range") >>SE escape length
I0 +
I(+)
I (0) cos"
#1-10nm
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h. Contrast
SE and BSE topography contrast
For one position (x,y) of the electron probe: BSE escape from a "pear" volume around the probe position SE1 escape from a thin layer under the entrance surface of the probe SE2 escape from a thin layer under the escape surface of BSE
ISE(0)=IPE!*=IPE!10% IBSE(0)=IPE!)=IPE!31%
ISE2+3 = IBSE!*= IPE!)!* & ISE2+3(0) = IPE!37%!10%= IPE!3.1% out of 10% ISE2+3(40) = IPE!37%!10%=IPE!3.7% out of 13%
Acha Hessler-Wyser Intensive SEM/TEM contrast is not 58 BSE topographical training: SEM negligible! Chemical contrast is well observed only on polished samples
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h. Contrast
Topographical contrast at low energy
Effect of the incidence angle
(adapted from D.C. Joy Hitachi News 16 1989) Intensive SEM/TEM training: SEM 59
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h. Contrast
Size and edge effects
Do not forget, in SEM: The signal is displayed at the probe position, not at the actual SE production position!!!
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h. Contrast
Size and edge effects
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h. Contrast
Size and edge effects
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h. Contrast
Comparison of SE and BSE contrast modes
SE BSE
ET detector +200V
(0V)
backscattered and transmitted e- create SE, some of them are driven to the ET detector by the electric field BSE are absorbed The trajectories of BSE are not The observator looks down to the column and the strongly affected by the "light" seems to come from the Everhardt-Thornley electrical field, most BSE miss the detector. detector
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h. Contrast
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h. Contrast
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h. Contrast
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h. Contrast
Detector ? Detector ?
pyramid?
Intensive SEM/TEM training: SEM 67
etch-pit?
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h. Contrast
Change in SE contrast with the voltage
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h. Contrast
Contraste enhancement at low voltage: less delocalization by SE2. An example: a fracture in Ni-Cr alloy
SE, 5 kV
SE, 30 kV
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h. Contrast
SEM: Effect of the accelerating voltage on (from D.C. Joy penetration and SE signal Hitachi News 16 1989)
20 kV: strong penetration, SE3 is a much larger signal than SE1/SE2. It reveals the copper grid under the C film via the electron backscattering, but the structure of the film itself is hidden
Intensive SEM/TEM training: SEM
2 kV: low penetration, only a few electrons reach the copper grid and most of the SE3 are produced in the C film together with SE1/SE2. The C film and its defects become visible
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i. Examples
Physical limit to the imaging in secondary electron mode
Tin grains on a thin carbon film (TEM supporting grid) HRSEM 25 kV 1 nm nominal resolution left: SE right: scanning transmitted electrons (STEM)
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i. Examples
Physical limit to the imaging in secondary electron mode
(from B. Ocker, Scanning Microscopy 9 (1995) 63)
The average grain size looks larger in SE (12.3 nm) than in STEM (9.1 nm) "Delocalisation": the elastic scattering in STEM (Rutherford) occurs at a much closer distance from the atom nucleus than the inelastic coulombian e-/e-interaction required to eject a SE
Intensive SEM/TEM training: SEM 72
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i. Examples
AlxGa1-xAs/GaAs "quantum wire" quantum well)
GaAs
x=0.55
(2-D
x=0.20
SE mode image on a cleaved surface. The SE2 (BSE chemical) contrast dominates this image in absence of topographical contrast (SE1=cte)
(by courtesy of Dr. K. Leifer, IPEQ/EPFL)
QW
Intensive SEM/TEM training: SEM 73
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i. Examples
Contrast reversal in BSE mode at low accelerating voltage
Si
Cu
Ag
Au
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j. Charging effects
Fiberglass on epoxy
1 kV
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j. Charging effects
Improving SE contrast at low voltage
fiberglass on epoxy
Which polarity ??????
by courtesy B. Senior/CIME
Intensive SEM/TEM training: SEM 76
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j. Charging effects
Total yield for electron emission (SE + BSE) on insulators
E1 and E2 are critical energies where 1 electron leaves the surface for each incident electron: neutrality
1 taux !>>0 !>0 !0
when eVacc= E2 charging-up disappears! eVacc= E1 is unstable, eVacc= E2 is stable Caution: E1 and E2 are specific to the material, but also change with the incidence angle +!
Intensive SEM/TEM training: SEM
E1
1000
E2
2000
3000
nergie keV
Caution: this simple (simplist!) model is not quantitative for insulators because charge implantation and removal depends of the scanning speed and precise sample geometry
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j. Charging effects
Charging-up on a mask for microelectronic
(SiO2 substrate, photoresist, SE mode)
Vacc >> E2
Intensive SEM/TEM training: SEM 78
Vacc"E2
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j. Charging effects
Charging-up on spherical silica particles
TV scan slow scan
5 kV
at 1.5 kV, close to 1.5 kV the neutrality point, particles recover their sphere contrast
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j. Charging effects
Observation of insulating samples
Charging-up is reduced or even cancelled when working at E2 Charging-up may be cancelled under partial atmosphere in a "low vacuum" or "low pressure" SEM, ESEM
Caution the "skirt" (incident electrons from the probe are scattered out of it by the atmosphere reduced resolution and contrast delocalized microanalysis (may attain mm!)
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j. Charging effects
Contrast reversal in SE mode close to the neutrality point
SiO2-Cr mask for TEG-FET transistors production
SiO2
(E2~3.0keV)
Cr (E2~1.8keV)
3.0 kV
Intensive SEM/TEM training: SEM 81
1.8 kV
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j. Charging effects
Some values of the neutrality E2 energy
E2: upper neutrality energy Em: maximum emission energy *m: maximum yield at Em
adapted from: E. Plies, Advances in Optical and Electron Microscopy,13 (1994) p 226
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j. Charging effects
obj pole-piece
(adapted from L. Reimer Scanning Electron Microscopy)
Intensive SEM/TEM training: SEM 83
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0V
Negative charges left on the particle create an electric field that repells the SE toward the substrate around the dust
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j. Charging effects
Extreme charging-up: electrons are reflected by the sample and hit the microscope sample chamber!!!
- + -
ET
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j. Charging effects
Surface potential (voltage) contrast
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