Why use electrons for microscopy?

• Assuming g scattering
gggives yyou contrast,, the
shorter the wavelength of the radiation, the
better your resolution
0.61λ
∂=
μ sin β

• If wavelength = 500nm (visible light),

resolution = 300nm
• If we use electrons with E = 30keV (typical for
SEM), wavelength = ?nm
 Electron (e-) --> specimen
interactions
• Very important for studying how to get the
most from your samples in the SEM and TEM
• Defines where contrast comes from
• Allows us to determine our samples’
elemental composition quantitatively

• Things to remember!
– e-
e have mass - can transfer momentum
momentum, behave
relativistically at high energies
– e- are waves - can constructively and destructively
interfere
 Electron scattering

• 2p
primary
y classes of electron scattering:
g
– elastic scattering - incident electron will change
direction, but not kinetic energy, scales with Z2
– inelastic scattering - incident electron will change
direction, but also give up some kinetic energy to
the sample,
p , scales with Bethe expression
p
• will allow for elemental analysis
• Ultimately,
y scattering
g will lead to the image
g
contrast
 Electron scattering probability

• Scattering
g cross section:
N 1
σ= ∝ 2
nincident nt argg ets E
• Mean free path:
MW
λ=
N A ρσ
• Total mean free path:
1 1 1
= + + ....
λtotall λa λb
 Interaction Volumes
• From the mean free path, we can calculate
the “interaction
interaction volume”
volume of electrons and the
samples
– dependent upon incident electron energy, the
sample atomic mass, the sample density, and the
angle of incidence of the incoming electrons
 Interaction Volumes - accelerating
voltage dependence (SEM samples)

2kV

10kV

30kV
 Interaction Volumes - atomic mass
dependence

Al

Fe

W
 Interaction Volumes - sample density
dependence

Au 100% dense

A 50% dense
Au

Au 25% dense
 Interaction Volumes - incident
electron beam angle dependence

0 deg
g
(normal)

45 deg

60 deg
 Elastic Scattering - SEM signals
• Most elastic scattering signals in the SEM are evident as
“Backscattered” electrons - comparable to reflection microscopy
• No energy
energ loss,
loss just
j st change in direction d
due
e to scattering and diffraction
- large dependence on surface topography and atomic number

Al

W
 Elastic Scattering - TEM signals

• In TEM,, elastic scattering

g is evident as atomic
number or density contrast or as diffraction

Al

100keV, 50nm thick W

 Inelastic Scattering - secondary
electron emission
• Secondaryy electrons
– Main signal used in the SEM for imaging
– Due to interactions between the e- beam and weakly
bound conduction band e e- (metals) or valence band e
e-
(semiconductors or dielectrics)
• Secondary e- energies are typically 2-10eV, but can range
up to
t 50eV
50 V
• Since the scattering cross section increases with
decreasingg e- energy,
gy lower acceleratingg voltages
g g generally
y
give more SE signal
 Inelastic Scattering - X-ray emission

• After the incoming e- beam excites

inner shell e
e- in the sample
sample, the
excited e- decay back to a ground
state
• In order to obey energy and mass
conservation, they emit a X-ray
– The X-ray energy is dependent
upon the elements present
within the sample
– Can quantify composition by
measuring these energies
(EDX)
• Most X-rays generated are re-
absorbed by the sample
 Inelastic scattering - other processes
• Auger e- emission
– 2e- pprocess similar to the X-rayy
scenario, but instead of emitting an
X-ray, a weakly bound outer shell
e- is emitted (typically from the first
2nm of the surface)
– outer shell e- can give bonding
information about the samples!! -
very useful in surface science
• Cathodoluminescence
– again similar to X-ray
X ray and Auger
Auger,
but energy is conserved by the
emission of a photon in the IR /
g
Visible / UV range
 Inelastic Scattering - more other
processes
• Plasmons
– incident e
e- introduce electrostatic potential waves
in the solid which forms oscillations of e- (low
energy)
• Phonons
– incident e- introduce lattice vibrations within the
solid
lid which
hi h causes sample l hheating
ti
• Bremsstrahlung X-ray emission
– as the
th incident
i id t e- interact
i t t with
ith the
th electrostatic
l t t ti
potential of the sample, they decrease kinetic
energy and emit an X-ray to obey conservation of
energy
– does NOT excite an inner shell e- in the sample
 Inelastic Scattering - e- beam
damage
• Inelastic events can p
produce “radiation
damage”
• 2 types of damage:
– radiolysis - inelastic scattering produces sample
heating and breaks the chemical bonds (polymers
and some biological samples)
• reduced at high e- energies, increased at lower
– knock
knock-onon - direct displacement of atoms due to the
incoming electron beam creates point defects
(insulators and semiconductors)
• increased
i d att hi
high
h e- energies,
i reduced
d d att llower
 How the Scanning Electron
Microscope works!
• Electron source
• Condenser and
Objective Lenses
• Faraday
F d C Cup
• Steering lens
• Ray traces
• Detectors
• Electronics
• Imaging
 Scanning and Image Formation
• Scanning - moving beam across sample, sampling
specimen
p at different locations with different detectors
– Analog - beam scanned continuously, but at different rates
– Digital - beam placed at (x,y) coordinates, intensity recorded
at each point
• Dwell time: amount of time an area is sampled (digital:
length of time beam stays in one spot)
 Scanning and Magnification
• Older systems (JEOL 5800) - CRT is
scanned at same rate as beam on specimen
using
g same scan g generator
– Need special CRT able to scan at
different rates (TV, slow, photo, etc)
– Also needs to be able to do line scans
(no yy-coordinates,
coordinates just x)

• Magnification
– M = Lcrt / Lspecimen
– Magnification depends on the size of
your monitor and the resolution you have
it set
– If monitor
it size
i andd resolution
l ti are fifixed,
d
can only change mag by changing
Lspecimen (decreasing the length of
beam scan on the sample)
• ONLY dependent upon the scan
coils, NOT the OL strength
 More Magnification
• e- travel down electron column in helical path, should result in
image rotation when WD or focal length is changed
– Does not occur due to compensation by the scan coils
• Magnification calibration
– Completed using ASTM standards
– Also adjusts scan coils for squareness and roundness
• Digital Image Acquisition
– Pixel definition
definition, size
– Sampling: Pixel is not necessarily a fundamental unit of the specimen
being sampled - depends on spot size, interaction volume
 Imaging - Depth of Field
• Depth of Field - biggest advantage of SEM
– Defined as the distance (D) between where the
crossover occurs and the beam broadening is
large enough that the broadening (r) is noticeable
((+ and -))
r 2r
tan α = D≈
D /2 α

– For CRTs, r = 1pixel ~ 0.1mm

– r = 0.1mm
0 1mm / Mag
– D = 0.2mm / (α * Mag)
α = Raperture / WD
Depth of Field
 How the Scanning Electron
Microscope works!
• Electron source
• Condenser and
Objective Lenses
• Faraday
F d C Cup
• Steering lens
• Ray traces
• Detectors
• Electronics
• Imaging
 Electron Emitters Specifics

• Electrons ejected from

the emitter tip
tip, current
due to gun bias
• Electrons are then
accelerated past the
Wehnelt cap (anode)
and into the column
• First
Fi t crossover occurs
before the anode
• Brightness
g can be
affected by filament to
Wehnelt distance (in
addition to Vo))
Electron Beam Sources - Thermionic
Emission ((type
yp 1))
• Heat the emitter so that e-
can escape the work
function of the material into
the vacuum
• Materials:
– W (Ewf = 4.8eV), high Jc at T
< Tmelting
– LaB6 (Ewf = 2.5eV), higher
Jc but
b t need d llower vacuum
for stability
• Smaller tip radius, higher Jc
due to electric field
enhancement
– Schottky effect,
– especially important to LaB6
– Can reduce Ew by >0.1eV
Jc = 120A/cm2K2 (T2) exp(-Ew/kT)
 Electron Beam Sources - Field
Emission ((type
yp 2))
• Small tip radius, extremely high
fields allow electron emission
without
ith t h
heating,
ti e- “tunnels”
“t l ” directly
di tl
into vacuum
• Ewf is reduced due to Schottky
effects
• Bias tip 3-5kV negative relative to
first anode
• 107V/cm
Field strengths >10
• Fowler-Nordheim tunneling from tip
into vacuum
• Advantages:
g
– High brightness
– Narrow e- energy distribution
– High resolution
 More FEG

• Types:
– C
Cold
ld cathode
th d (b
(best,
t needd
high vacuum)
– Thermal (bigger energy
spread))
– Schottky (thermal, but good
energy spread like cold
cathode, small current)
• Vacuum considerations:
– At 10-5 Pa, one monolayer
of gas is formed per second
– Run vacuum at 10-9 Pa to
avoid changes in Ew
– “flash” heat the tip to bake
off gas
– Use Schottk
Schottky FE
 FEG Tip Materials

• Single
g crystal
y W sharpened
p to ~100nm radius
– W good due to high mechanical strength
• Needed due to high strains put on materials
under high fields
• How to increase e- current?
– W crystal
t l direction
di ti <310>310 tto give
i llowestt work k
function direction the best look at the first anode
– Coat W crystal with ZrO (Ew = 2.8eV)
 Electron Lenses
• How direct electrons into a point? – Electromagnets

B = magnetic
ti flflux d
density,
it f(I)
B = H in vacuum
F = -e (B x v) using right hand rule
Iron core wrapped N times with a
conductor, pass I (current) through
the conductors
B is
i hhomogeneous b
between
t th
the
gaps
Produces “Fringing
Fringing Fields”
Fields near
the optic axis - steer the e-
 Lenses - General

e- interact with Br to produce a

rotational force and velocity
Rotational e- interact with Bz to
produce a radial force - causes e-e
to bend toward optic axis
Also causes axial ppath within the
column - relates as image
rotations while changing focal
length or spot size
 How the SEM works!

• Electron source
• Condenser and
Objective Lenses
• Faraday
F d C Cup
• Steering lens
• Ray traces
• Detectors
• Electronics
• Imaging
 Control of Lenses

• Effects of objective lens

apertures
– Optimizes convergence
angle
g
– Controls depth of focus
– Controls probe current
 Control of Lenses

• Effects of working
di t
distance (WD)
– Longer WD, larger beam
diameter
 Control of Lenses

• Effects of Condenser
lens strength
– Stronger CL, smaller spot
size
 Lens Aberrations

• Aberrations are the biggest

gg ultimate
resolution limiters in SEM and TEMs
• Types:
– Spherical – strength of lens on e- at the outside of
the lens is stronger than on those at the center
– Chromatic
Ch ti – e- off different
diff t energies
i focus
f att
different places
• Directly dependent upon focal length and e- e
energy spread (FEG has smaller Cc)
– Aperture diffraction – produces beam divergence
 Lens Aberrations

Aperture Diffraction

Astigmatism

Spherical aberration

Chromatic aberration
Astigmatism
 Imaging Defects
• Tilt distortion
– Mag is lower
perpendicular to tilt
axis (more specimen
is mapped) than
parallel to the tilt axis
– Tilt correction
– Dynamic
D i ffocus
correction
• Moire effects
• Scan distortion
– Misaligned scan coils
give rise to distortions
at the edges of the
scan
 Imaging Detectors - SE
• Everhart - Thornley
Detector
– Converts e- into
light, then back into
electrical signals
– Positively biased
Faraday cage
attracts low E SEs
– Also collect BSEs
present within line
of sight
More SE Imaging

Placement of E E-TT detector

is important for image
interpretation
 Imaging Detectors - TTL
• Through the lens
detectors
– Snorkel OL guides
SEs back up the
b
beam path
th tto a
scintilltor detector with
high
g bias
– Eliminates SEs
formed via the
chamber walls,
walls
minimizes BSEs
formed off-axis (nearly
pure SE detector)
 Elastic Scattering – Backscattered
electrons in the SEM
• Most elastic scattering signals in the SEM are evident as
“Backscattered” electrons - comparable to reflection microscopy
• No energy
energ loss,
loss just
j st change in direction d
due
e to scattering and diffraction
- large dependence on surface topography and atomic number
• Angular dependence of BSE – follows a cos distribution
 Backscattered electrons - atomic
mass dependence

Al

Fe

W
 Backscattered electrons - atomic
mass dependence
for pure
p
compounds

For mixed compositions, backscatter coefficient is the sum of th

BSE for each atomic composition within the material
 Interaction Volumes - accelerating
voltage dependence (SEM samples)

2kV

10kV

No significant
accelerating voltage 30kV
dependence on BSE
 BSE – tilt angle dependence

0 deg
(normal)

Higher tilts,
tilts more BSE

45 deg Does not necessarily mean

more signal to the detector –
need to tilt toward detector

60 deg
 BSE detectors

Negatively biased E-T detector

-Photomultiplier
Photomultiplier tube
tube, same
as for SE
-Neg. bias repels low energy
SE, only detects BSE

Solid-state detector
-p-n junction like a solar
cell
-detect electronic signal to
determine contrast
 Solid State BSE detectors
• Flat, thin detectors placed directly
above sample, allows for high BSE
collection
ll ti efficiency
ffi i
• Signal is sent through an amplifier
to change the brightness and
contrast
t t off the
th image
i

• Can be formed in arrays – signals

from the different parts of the
arrays can either be combined,
subtracted, or viewed separately
– If A-B, gives topographic
contrast
– If A+B, gives compositional
contrast
BSE vs. SE Imaging

Imaging with SE and BSE on the

same areas will illustrate the
composition changes in the samp

Brighter areas - higher atomic

number
 Special Topics in SEM
• What else can we do with the SEM?
– HRSEM
– Low kV imaging
– STEM
– Stereomicroscopy
– Voltage contrast
– Magnetic field contrast
– Crystallographic contrast
– Electron channeling diffraction
 HRSEM
• “High Resolution” SEM
– Must overcome the contrast limits defined by the
threshold equation
– Dependent upon C (=ΔS/S), defined by IB, τ, DQE
– Also dependent upon interaction volume and
where the signals are generated

SE1 is the HR
signal - need to
minimize the
other signals for
HR imaging
 More HRSEM
• Signal to pixel ratios
– At low mag (<1,000x), pixels are generally smaller than the
interaction volume
– At medium mag (10,000x), overlap of pixels and interaction
volumes begins to occur
• For 1nm, 10kV probe into Si, interaction volume is 10,000x
larger than the probe size
– At high mag (100,000x), FOV is smaller than the interaction
volume, BSE and SE2 signals get averaged out in the noise
– Bright edges help with contrast
• HRSEM at low kV
– Interaction volume smaller
– Most of the emitted e e- have high spatial res
– Brightness falls off too, must balance
 Setting up HRSEM

1. Reduce contamination!!
2. Thin, fine grained metal coating (increase
SE1)
3. Small spot size
4. Low kV ((balance with spot
p size to maintain
contrast)
5. Short WD
6. Snorkel lens
7. TTL detector
8. STIGMATE!!!!
 HRSEM

Low-k / Ru surface
 Stereomicroscopy
• SEM has large depth of field compared to LM
• 3-D info is lost when displaying a 2-D image
– Can be recovered by stereomicroscopy
• Stereomicroscopy:
py
– Collect (2) 2-D images at different tilts (6° separation) -
sample must be at eucentric height!
– Displaying stereopairs:
• Blue / red 3-d glasses (Image J, instructions in text)
• Stereoviewer used with p printed imagesg
– Can also be done quantitatively using geometry to determine
3-D information about the samples
20 μm
10 μm
200 μm
 Voltage and Magnetic Contrast
• If high local fields are present, they
mayy be strong g enough
g to either
significantly repel e- or attract them
back into the surface
• Voltage Contrast
– Useful for failure analysis of
electronic devices - bias the device
in the SEM, look for bright and dark
areas to see where the device is
failing
• Which areas will appear bright
vs. dark?
– Also visible during “charging”
 Magnetic Contrast - Type 1

• Interactions of SE1
with leakage B
F = -ev x B
 Magnetic Contrast - Type 2

• Interactions of e- with B
inside the specimen
 Crystallographic Contrast and
Channeling
• e- can be Bragg diffracted by
individual crystals (grains)
– Directionality induced by
diffraction gives rise to light / dark
areas
– Contrast determination?
Threshold equation?
– Best to use large solid angle BSE
detector
• e- channeling can also give rise to
diffraction patterns
– Strongly affected by surface
topography
– Better to determine
crystallography with EBSD
(discussed later in the semester)