Chapter 3 - SEM

Intensive SEM/TEM training: SEM Acha Hessler-Wyser 1 April 2010
3. Scanning Electron Microscopy

Dr Acha Hessler-Wyser
Bat. MXC 134, Station 12, EPFL+41.21.693.48.30.
Centre Interdisciplinaire de Microscopie Electronique
CIME
Outline
a. SEM principle
b. Detectors
c. Electron probe and resolution
d. Depth of field
e. Stereoscopy
f. Electron-matter interaction volume
g. Secondary and back-scattered electrons
h. Contrasts
i. Examples
j. Charging effects
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.
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
a. SEM principle
Response to incident
electrons:
! Secondary electrons SE
topography, low energy "0-30 eV
! Backscattered electrons BSE
atomic number Z, energy " eV
0
! 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)
a. SEM principle
Energy spectrum of electrons leaving the
sample
Auger (secondary)electrons
Back scatered electrons
BSE
Secondary electrons
SE
a detector (eye,
photographic
plate, video
camera...
an illumination
section (lenses,
apertures...)
a magnification
section
(lenses, apertures...)
A "light"
source
b. Detectors
a sample
(+ a "goniometer")
b. Detectors
Everhardt-Thornley detector: for SE and BSE
SE: 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.
BSE: 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).
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
a detector (eye,
photographic
plate, video
camera...
an illumination
section (lenses,
apertures...)
a magnification
section
(lenses, apertures...)
a sample
(+ a "goniometer")
A "light"
source
Resolution in probe mode (SEM, STEM)
! Spherical aberration
! Chromatic aberration
! Diffraction (Airy, Rayleigh)
! Brilliance ! conservation
! Combinaison
3
sph s
d C ! = "
d
d
= 0.61
!
n" sin#
d
ch
= C
ch
!E
E
+ 2
!I
I
"
#
$
%
&
' (
d
g
=
4I
!
2
"
#
1
$
d
i
a
m
t
r
e

(
n
m
)
A/cm
2
sr
Probe with coherent source: see Mory C, Cowley J M,
Ultramicroscopy 21 1987 171
Incoherent source
d
ech
= d
g
2
+ d
sph
2
+ d
ch
2
+ d
d
2
Resolving power ("resolution"): Rayleigh
criterium
probe size and resolution (no noise)
particles 100 nm diam.,
probe dia 2 nm
probe dia 2 nm
probe dia 2 nm
model 100 nm diam.
particles
Probe size and resolution (with noise)
(with noise)
model 100 nm diam.
particles
Particles100 nm
diam.,
probe diam 2 nm
probe diam 2 nm
probe diam 2 nm
How to increase resolving power?
Reduce the probe current at
constant dose
Increase exposure time t
Reduce volume interaction Reduce accelerating voltage
Reduce C
sph
Short focus lenses:
in-lens, semi in-lens, Snorkel
Increase brillance Field emission gun:
Cold emission, thermal assisted,
Schottky effect
Reduce C
sph
and increase
brillance
Dedicated columns: Gemini, XL30,

SEM: Effet of current, probe diameter and
image acquisition time
good resolution, but
statistical noise
smal loss of
resolution, still less
statistical noise
very few statistical
noise, but high
resolution loss!
Good resolution, less
statistical noise
SEM: Limiting parameters on resolving power "
with SE
1.High magnification
The probe size (generation of SE1)
rd
probe
2.The volume of interaction (generation of SE2+SE3 from BSE): energy
and atomic number influence
3.Low magnification
The screen (or recording media) pixel size d
screen
rd
screen
/magnification
Current/probe diameter
Thermionique source: spherical
aberration is the most important
Field emission source:
gun aberrations and chromatic
aberration are more important
I
max
=
3!
2
16
"C
sph
#2 3
d
8 3
I
max
= cd
2 3
Tir de L.Reimer, SEM
Thermionic SEM : low voltage?
Modern SEM short focus length: C
sph
=17 mm, C
ch
=9 mm, DE=1.5 eV, b=1.10
5
A/cm
2
sr
Short focus length or FEG?
Snorkel Regular focus length FEG
C
sph
=1.7 mm, C
ch
=1.9 mm C
sph
=17 mm, C
ch
=9 mm C
sph
=17 mm, C
ch
=9 mm
b=1.10
5
A/cm
2
sr, DE=1.5 eV b=1.10
5
A/cm
2
sr, DE=1.5 eV b=1.10
7
A/cm
2
sr, DE=0.4 eV
Resolution loss at low voltage
100
50
10
5
1
0.5 1 2 5 10 20 30
FE
LaB
6
W
Tension d'acclration (kV)
R
s
o
l
u
t
i
o
n

(
n
m
)

Basse tension/haute rsolution:
- observation de la surface relle
- chantillons non-mtalliss
- faible endommagement d au
faisceau
Haute tension/haute rsolution:
- effets de bord
- dtails fins non-rsolus
- fort endommagement d au
faisceau
1985
2000
Shorter objective
lens focal length
and C
s
d. Depth of field
Depth of field as a function of d
probe
h
prof .champ
= max
2
pixel
"image "
G
1
!
2d
sonde
1
!
"
#
$
%
$

h

h
2d
A
2#
d
A
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
d. Depth of field
Effect of working
distance (WD) and
aperture on depth of
field
d. Depth of field
Light bulb filament
d. Depth of field
Other examples
d. Depth of field
Effect of the objective aperture diameter
30 !m
50 !m
100 !m
d. Depth of field
Measuring depth of field: stereoscopy
e. Stereoscopy
The 3
rd
dimension: stereoscopic vision,
anaglyphs
e. Stereoscopy
3
-
D

r
e
c
o
n
s
t
r
u
c
t
i
o
n

(
a
n
a
g
l
y
p
h
)
e. Stereoscopy
3-D reconstruction
(pseudo-perspective)
e. Stereoscopy
3
-
D

r
e
c
o
n
s
t
r
u
c
t
i
o
n

(
g
r
e
y

l
e
v
e
l
s
)
e. Stereoscopy
3
-
D

r
e
c
o
n
s
t
r
u
c
t
i
o
n

(
f
a
l
s
e

c
o
l
o
r
s
)
e. Stereoscopy
e. Stereoscopy
Elastic interaction
Total kinetic energy and momentum are constant E
el
+ E
at
= cte
The light electron interacts with the electrical field in the heavy
atom: Rutherford scattering.
Only little energy is transferred, the electron speed does not
change significantly in amplitude but only in direction (elastic
scattering).
Elastic interaction:
Energy transfer
from the electron
to the target
100 kV
1000 kV
angle de
diffusion
C Au C Au
0.5 0.5 meV 0.03 meV 9 meV 0.5 meV
10 0.15 eV 9 meV 2.7 eV 0.17 eV
90 10 eV 0.6 eV 179 eV 11 eV
180 20 eV 1.2 eV 359 eV 22 eV

Inelastic interaction
part of the total kinetic energy is dissipated (energy loss)
!vibration in molecules or crystals (phonons "meV-100meV)
! collective oscillations of electrons (plasmons "10 eV)
! intra- et interband transitions ("mev-"1 eV)
! inner shell atom ionisation ("50 to150 keV < eV
0
)
! bond breaking " eV, atom displacement " 10-30eV (requires
V
acc
100kV...1MV, no longer SEM!)
Mean free path
Elastic cross-sections $
el
and mean free path %
el
,
total (elastic+inelastic)
mean free path %
t
and
electron range R
The mean free path is
the average path that
an electron does before
having interaction with
an atom
Monte-Carlo simulations
Electron Flight Simulator ($$$ Small World / D. Joy)
old DOS !!!!
http://www.small-world.net
Single Scattering Monte Carlo Simulation (Freeware)
"Monte Carlo Simulation" Mc_w95.zip
by Kimio KANDA
http://www.nsknet.or.jp/~kana/soft/sfmenu.html
CASINO (Freeware)
" monte CArlo SImulation of electroN trajectory in sOlids "
by P. Hovongton and D. Drouin
http://www.gel.usherbrooke.ca/casino/What.html
Number/Energy of backscattered electrons by
Monte-Carlo simulations
30 kV 3 kV 1 kV
BSE 5% BSE 8% BSE 10%
C
BSE 52% BSE 43% BSE 41%
W
Penetration and back-
scattering vs elements (Z)
V
acc
= 20kV = cte
Depth of electron
penetration vs Z and yield of
electron backscattering BSE
(Monte-Carlo simulation):
1
C 20 keV
BSE=6%
BSE=33%
1
U 20 keV
BSE=50%
Cu 20 keV
1
BSE=33%
10 nm
C 1keV
U 1keV 10 nm
Cu 1keV
10 nm
BSE=14%
BSE=34%
BSE=44%
V
acc
= 1 kV = cte
Depth of electron
V
acc
= 5 kV = cte
Depth of electron
200 nm
C 5 keV
Cu 5 keV
200nm
U 5 keV
200 nm
BSE=8%
BSE=33%
BSE=47%
Penetration and backscat-
tering vs energy(E)
Z = cte
Depth of electron
penetration in Cu vs
energy E
0
and yield of
electron backscattering
BSE (Monte-Carlo
simulation):
BSE=33%
Cu 20 keV
1#m
Cu 5 keV
1#m
Cu 1 keV
Cu 1keV
1#m
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
x
0
,y
0
intensity and delocalisation of SE
stemming from the probe at x
0
,y
0
(leading
to the X
0
,Y
0
pixel intensity on the image)
g. SE and BSE
"true" secondary electrons SE1 and "converted
BSE" secondaries SE2+SE3
x
0
,y
0
intensity and delocalisation of SE
stemming from the probe at x
0
,y
0
(leading
to the X
0
,Y
0
pixel intensity on the image)
The SE signal always contain a high resolution part (SE1
from the probe) and an average (low resolution) part
from SE2+SE3!
g. SE and BSE
Relative contribution of SE1 and SE2 (+SE3) vs
primary energy
The total intensity (green and brown) is
attributed to the (x,y) pixel, here at 0
nm on this 1-D model
(adapted from D.C. Joy
Hitachi News 16 1989)
total
total
total
SE1
SE2
g. SE and BSE
Yield for SE and BSE emission per incident
electron vs atomic number Z
&
:
': SE: low or no chemical contrast but for
light elements
the topographical contrast will
dominate on rough surfaces
I
SE
=I
pe
$' +I
SE3
=I
pe
('
pe
+'
pe
$&+'
sur
$&)
with ' the total SE yield, '
pe
the yield for SE1
and '
sur
the SE3 yield for materials surrounding
the sample (pole-pieces...)
SE1 SE2 SE3
Al Ni
0.11
0.28
(SE1)
BSE: chemical contrast for all the
elements
(sensitivity (DZ=0.5)
A fast way to phase mapping
I
BSE
=I
pe
$& with I
pe
the intensity of
the primary beam, & the BSE
yield
sample surface polished (no topography) and
perpendicular to the incident beam direction
(intermediate energy E
0
( 15 keV)
g. SE and BSE
Yield for SE and BSE emission per incident
electron vs tilt
BSE yield ! SE yield " ~1/cos#
Cu
Al
'
SE
~1/cos)
'
SE
(40)/'
SE
(0)(1.30
Monte-Carlo:
for Al:
&
BSE
(0)(0.15
&
BSE
(40)(0.24
&
BSE
(40)/&
BSE
(0)(1.60
for Cu:
&
BSE
(0)(0.31
&
BSE
(40)(0.40
&
BSE
(40)/&
BSE
(0)(1.30
(adapted from L. Reimer,
Scanning electron
microscopy)
g. SE and BSE
Dust on WC (different Z materials)
SE 25 kV BSE
low Z material flat material rough material low Z material
thin low Z material
g. SE and BSE
Contaminated area around a soldering spot
g. SE and BSE
Toner particle (penetration in light material)
SE 28 kV BSE
g. SE and BSE
Topographical contrast
in SE mode
Effet de l'inclinaison de la surface
)
I
0
I())
(1-10nm
penetration depth ("range") >>SE escape length
(adapted from D.C. Joy Hitachi News 16 1989)
Relative yield of SE vs angle of
incidence on the sample
surface
!
I " ( ) = I
0
# " ( ) $
I 0 ( )
cos"
)
h. Contrast
Topographical contrast at low energy
Effect of the incidence angle
(adapted from D.C. Joy Hitachi News 16 1989)
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!!!
intensity profile on image intensity profile on image
h. Contrast
h. Contrast
(From L. Reimer, Image Formation in
Low-Voltage Scanning Electron
Microscopy, (1993))
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
contrast = 2(I
1
-I
2
)/(I
1
+I
2
)
I
SE
(0)=I
PE
'=I
PE
10% I
SE
(40) = I
PE
'1/cos40=I
PE
13% SE1 contrast = 26%
I
BSE
(0)=I
PE
&=I
PE
31% I
BSE
(40)=I
PE
37% BSE contrast = 18%
I
SE2+3
= I
BSE
'= I
PE
&'
I
SE2+3
(0) = I
PE
37%10%= I
PE
3.1% out of 10%
I
SE2+3
(40) = I
PE
37%10%=I
PE
3.7% out of 13%
BSE topographical contrast is not negligible! Chemical contrast is well observed only on polished samples
I
BSE
31%
I
BSE
37%
incidence normale )=0 incidence )=40
Ni Ni
h. Contrast
Comparison of SE and BSE contrast modes
SE BSE
ET detector ET detector
(0V)
+200V +200V
BSE BSE are are
absorbed
The observator looks down to the column and the
"light" seems to come from the Everhardt-Thornley
detector.
backscattered and
transmitted e
-
create
SE, some of them are
driven to the ET
detector by the
electric field
The trajectories of BSE are not
strongly affected by the
electrical field, most BSE miss the
detector
h. Contrast
What does it suggest?
Which objective information?
h. Contrast
h. Contrast
pyramid?
Detector ? Detector ?
etch-pit?
h. Contrast
(from L.Reimer, Image formation in the low-voltage SEM)
Change in SE contrast with the voltage
h. Contrast
h. Contrast
SE, 5 kV SE, 30 kV
An example: a fracture in Ni-Cr alloy
Contraste enhancement at low voltage: less
delocalization by SE2.
h. Contrast
SEM: Effect of the accelerating voltage on
penetration and SE signal
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
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
(from D.C. Joy
Hitachi News 16 1989)
i. Examples
Tin grains on a thin carbon
film (TEM supporting grid)
HRSEM 25 kV 1 nm nominal
resolution
left: SE
right: scanning transmitted
electrons (STEM)
(from B. Ocker, Scanning Microscopy 9
(1995) 63)
SE: e
-
/e
-
coulombian
STEM: Rutherford
(e-/electric field in atom)
Physical limit to the
imaging in
secondary electron
mode
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
(from B. Ocker,
Scanning
Microscopy 9 (1995)
63)
Physical limit to the
imaging in
secondary electron
mode
i. Examples
i. Examples
SE and BSE images of a geologic polished
sample
A B
A B
BSE COMPO
(A+B)
BSE TOPO
(A-B)
SE
i. Examples
Al
x
Ga
1-x
As/GaAs "quantum wire" (2-D
quantum well)
(by courtesy of Dr. K. Leifer, IPEQ/EPFL)
GaAs
x=0.55
x=0.20
SE mode image on a
cleaved surface. The
SE
2
(BSE chemical)
contrast dominates
this image in absence
of topographical
contrast (SE
1
=cte)
QW
i. Examples
Contrast reversal in BSE mode at low
accelerating voltage
Ag Au Cu Si
from L.Reimer, Image formation
in low-voltage SEM
j. Charging effects
Fiberglass on epoxy
1 kV 1 kV
5 kV, low 5 kV, low current
5 kV, high 5 kV, high current
(by courtesy of B. Senior CIME/EPFL)
j. Charging effects
by courtesy B. Senior/CIME
fiberglass on epoxy
Which polarity ??????
Improving SE contrast at low voltage
j. Charging effects
Total yield for electron emission (SE + BSE) on
insulators
E
1
and E
2
are critical energies
where 1 electron leaves the
surface for each incident
electron: neutrality
when eV
acc
= E
2
charging-up
disappears!
eV
acc
= E
1
is unstable,
eV
acc
= E
2
is stable
Caution: E
1
and E
2
are specific
to the material, but also
change with the incidence
angle )!
Caution: this simple (simplist!) model is not
quantitative for insulators because charge
implantation and removal depends of the
scanning speed and precise sample geometry
j. Charging effects
Charging-up on a mask for microelectronic
V
acc
>> E
2
V
acc
"E
2
(SiO
2
substrate, photoresist, SE mode)
j. Charging effects
Charging-up on spherical silica particles
5 kV
TV scan slow scan
1.5 kV at 1.5 kV, close to
the neutrality point,
particles recover
their sphere
contrast
charges at the
particle surface
lead to anomalous
contrast as a
flying saucer
j. Charging effects
Observation of insulating samples
Charging-up is reduced or even
cancelled when working at E
2
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!)
Clich Kontron (Kuschek)pour CIME
j. Charging effects
Contrast reversal in SE mode close to the
neutrality point
SiO
2
-Cr mask for TEG-FET transistors production
3.0 kV 3.0 kV 1.8 kV 1.8 kV
Cr (E
2
~1.8keV) SiO
2
(E
2
~3.0keV)
Clich Kontron (Kuschek)pour CIME
j. Charging effects
Some values of the neutrality E
2
energy
E
2
: upper neutrality
energy
E
m
: maximum emission
energy
d
m
: maximum yield at
E
m
adapted from:
E. Plies, Advances in
Optical and Electron
Microscopy,13 (1994)
p 226
j. Charging effects
Charging-up of an
insulating particle of
dust
Negative charges left on
the particle create an
electric field that repells the
SE toward the substrate
around the dust
0V
2
0
0
V
o
b
j

p
o
l
e
-
p
i
e
c
e
(adapted from L. Reimer Scanning Electron Microscopy)
j. Charging effects
Extreme charging-up: electrons are reflected
by the sample and hit the microscope sample
chamber!!!
+
-
-
- -
- -
- -
ET ET
(adapted from Philips Bulletin)
j. Charging effects
Surface potential (voltage) contrast
(from Golstein et al, Practical SEM (1975))

Chapter 3 - SEM

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Chapter 3 - SEM

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Intensive SEM/TEM training: SEM Acha Hessler-Wyser 1 April 2010

3. Scanning Electron Microscopy

Intensive SEM/TEM training: SEM Acha Hessler-Wyser 16 April 2010

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