29 Jan.
2010
Scanning electron
microscopy (SEM)
D.S. Su
(SEM: Sächsisches Eisenbahnmuseum)
Principle of SEM
SEM: electron beam/specimen interactions
Inelastic scattering of electrons
Secondary Electron Emission
Secondary electrons are electrons in the specimen that are
ejected by the beam electron
• If the electrons are in the conduction or valence bands then it doesn´t
take much energy to eject them. They are called slow SEs with energies
typically below about 50 eV.
• If the electrons are strongly bound inner-shell electrons they are less readily
ejected, but when they are thrown out of their shells they can have a
significant fraction of the beam energy (fast SEs)
• If the electrons are ejected from an inner shell by the energy released
when an ionized atom returns to the ground state, then these secondary
electrons are called Auger electrons.
Inelastic scattering of electrons: Secondary
electrons
Slow Secondary Electrons Fast Secondary Electrons
ejected from the conduction or High-energy electrons which are
valence bands of the specimen generated in the specimen.
(usually has energy < 50 eV)
SEs can only escape if they are In a TEM, fast SEs can have
near the specimen surface. energies of ~ 50 – 200 keV
Used to form images of the
specimen surface.
FSEs are generally both unavoidable
and undesirable. They are not used to
form images or give spectroscopic
data. And they may low the
quality of the latter.
Inelastic scattering of electrons: Secondary
electrons
Auger SE
Auger Electrons electron
Vacuum
The energy of Auger electrons is given Conduction band
by the difference between the original Valence band
excitation energy and the binding energy
of the outer shell from which electron
was ejected.
L3
L2
Typical Auger electron energies are L1
in the range of a few hundred eV to Incoming
a few keV and are strongly absorbed electron
within the specimen
K
An alternative to X-ray emission as an Energy-loss
Ionized atom returns to ground state. electron
X-ray emission of atomic electrons
Characteristic X-rays • Ionization
• Filling in the missing
electron with one from
Vacuum
the outer shells.
• Emission of X-rays or Auger e-
Conduction band Incoming electrons
Valence band
L3
L2
Characteristic X-rays
L1
Nucleus
Inelastic scattering of electrons
Electron-hole pairs and Cathodoluminescence (CL)
Incoming electron
A semiconductor creates electron-hole pairs
when hit by high-energy electron
C-band
} bandgap
If the electrons and holes recombine, V-band
light will be emitted (cathodoluminescence)
If a bias is applied (or if it happens
to be a p-n junction), the electrons and
holes can be separated.
The current detected is called the Energy-loss electron
electron beam induced current or EBIC signal
Charge-collection microscopy (CCM) hν
Inelastic scattering of electrons
Cross sections for the various
inelastic scattering processes in
Al as function of the incident
electron energy, assuming a small
angle of scatter; plasmon (P), K
and L-Shell ionization (K,L), fast
and slow secondary electron
generation (FSE, SE). For
comparison purposes the elastic
cross section (E) is also included.
Scheme of Scanning Electron Microscope
Electron gun
Wehnelt cap
Anode
CRT
Electron beam
Condenser lens
Figure
Variation of
magnification
Scanning coils Scan
generator
Objective lens
Signal
amplifier
Sample
Detector
SEM: electron optical column
TEM is more complicated
Electron Sources
An FEG tip, showing the extraordinarily
An LaB6 crystal fine W needle
LaB6 Gun
Probe diameter > 5 nm
Brightness 109 A/m2ster
Vacuum required 10-4 Pa
Field Emission Gun
Cathode
V1
ext volt
V0
acc volt
Probe diameter 1-2 nm
Brightness 1013 A/m2ster
Focusing Anodes Vacuum required 10-8 Pa
Electron Beam
SEM: General Information
Accelerating voltage 100 V – 30000 V
Resolution 0.7 nm – 5 nm (depends on the kind of electron gun)
Samples should be electrically conductive and
also be mounted electrically conductive on the holder
Size of sample is limited by the specimen chamber
Kind of Information
Topography
Morphology
Composition
Crystallographic structure
SEM: sample preparation
1) Remove all water, solvents, or other
materials that could vaporize while in the
vacuum.
2) Firmly mountall the samples.
3) Non-metallic samples, such as plants,
fingernails, and ceramics, should be coated so
they are electrically conductive.
An insect coated in gold, prepared for viewing with
a scanning electron microscope.
Secondary Electron Imaging (SEI)
• Secondary electrons are detected
• The mostly used operation mode of a SEM
SEM: Magnification
In a SEM, magnification results from
the ratio of the dimensions of the
raster on the specimen and the
raster on the display device.
Assuming that the display screen has
a fixed size, higher magnification
results from reducing the size of the
raster on the specimen, and vice
versa. Magnification is therefore
controlled by the current supplied to
the x, y scanning coils,, and not by
objective lens power.
SEM: Resolution
• The spatial resolution of the SEM depends on
the size of the electron spot, which in turn
depends on both the wavelength of the electrons
and the electron-optical system which produces
the scanning beam.
• The resolution is also limited by the size of the
interaction volume, or the extent to which the
material interacts with the electron beam.
• The spot size and the interaction volume are
both large compared to the distances between
atoms, so the resolution of the SEM is not high
enough to image individual atoms
Resolution of a TEM
Information SEM: Information depth Penetration depth of PE
of and
surface PE size of X-ray resolution
depend on
and BSE detector
accelarating voltage
Characteristic BSE
bulk
X- rays Cathodoluminescence and
X-ray detector
density of material
SE detector
SE R=100.E1.43/ρ
Auger e-
SE
(1-10 nm depth)
l e
p
a m
S
BSE
(ca. 0.5 of PE depth
Sample
Pentration depth of PE
Characteristic X-rays
(nearly PE depth) X-ray resolution
Secondary Electron Imaging (SEI)
• Resolution
Secondary Electron Imaging (SEI)
• Why 3 D appearance ?
Due to the very
narrow electron
beam, SEM
micrographs have a
large depth of field
yielding a
characteristic three-
dimensional
appearance useful
for understanding
the surface structure
of a sample.
Pollen grains taken on an SEM show the characteristic depth of field of SEM micrographs
Depth of field
A macro graph with very shallow
depth of field.
Imaging using Back Scattered Electrons (BSE)
σ(θ) ~ Z2
BSE image of BMW catalyst, bright particle being Pd.
SE image – BSE image
Mineral
020823 SE HV15kV 020824 BSE HV15kV
• SBA-15
1 kV 15 kV
Changing the high voltage of the SEM....
SE, HV 30 kV SE, HV 2 kV
Influence of acc voltage
SEM: Contrast Mechnisms
SE
PE Detector
Effect of topography
Effect of position relative to the detetector
spikes and edges are brighter than plane surfaces
a surface turned towards the detector is brighter
than one turned away from it
Effect of electrical charge Effect of chemical composition
negatively charged points are brighter regions of heavy elements are brighter
than positively charged ones than those of light ones
SEM: Effect of topography
La0.8Sr0.2Ga0.85Mg0.15O2.825
020293 <0° HV 10kV 020294 <45° HV 10kV
Tilting
New SEM: scanning and transmission
New SEM: scanning and transmission
• Ni/CNTs
Chemical Composition
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Chemical Composition: EDX
X-ray emission of atomic electrons
Characteristic X-rays • Ionization
• Filling in the missing
electron with one from
Vacuum
the outer shells.
• Emission of X-rays or Auger e-
Conduction band Incoming electrons
Valence band
L3
L2
Characteristic X-rays
L1
Nucleus
Inelastic scattering of electrons
Bremsstrahlung
Inelastic scattering of electrons: X-ray emission
Bremsstrahlung X-rays
If an electron is decelerated by the
Coulomb field of the nucleus while
penetrating completely through the
electron shell, it emit an X-ray.
KZ(E0 – E)
N(E) =
E
The bremsstrahlung X-ray intensity as a function of energy.
N(E): number of bremsstrahlung The generated intensity increases rapidly at low energies but
Very low energy bresstrahlung is absorbed in the specimen
photon of energy E, produced by And the detector, so the observed intensity drops to zero.
electrons of Energy E0. E0 is the energy of the electrons that cause the X-ray emission.
The EDX Spectrum
Characteristic X-ray peaks
Continuous background (Bremsstrahlung)
Localization of the element distribution
Bi Cd
Sn Pb
Wood Alloy - Mapping
Brief introduction of ESEM
N2 CO
C2H4 O2
NH3
imaging
gas H2
FEI Quanta 200 FEG
Jan. 17-20, 2010 emcat2010
Brief introduction of image detector
Vout
out
A
Electrons
SE Detector +
Positive Ions
V
Gas Molecules
Schematic diagram of SE Detector
Schematic diagram of Gas Ionization Detector
SEM and TEM results
1bar 1mbar
Jan. 17-20, 2010 emcat2010
Scheme of Scanning Electron Microscope
Electron gun
Wehnelt cap
Anode
CRT
Electron beam
Condenser lens
Figure
Variation of
magnification
Scanning coils Scan
generator
Objective lens
Signal
amplifier
Sample
Detector
