Microscope
(Compiled by Richard Tarrant, 2009, 2010)
Ruska and Knoll build the first electron microscope in Berlin in 1932 [5]
1 Introduction
In this experiment you are to read and complete the exercises and problems in this text,
and then undertake two 4 hour practical sessions in the Electron Microscope Unit (EMU)
in the Madsen Building.
It is strongly recommended that you read this text and complete the exercises BEFORE
you attend the practical EMU sessions. You will have a much better appreciation of the
practical sessions if you understand the physics behind them.
At various points in the text, checkpoints are indicated. Checkpoints 3 and 4 will
be awarded by EMU staff to indicate your participation in each of the practical sessions.
Checkpoints 1 and 2 will be awarded by Physics Lab staff ONLY. Please do not ask the
EMU staff to award checkpoints 1 or 2.
Please write/draw/attach all of your work into your 3rd yr lab. logbook.
Please bring your lab logbook to the EMU sessions and put your own notes and
comments into your logbook during the sessions.
1.1 Aims
To introduce the Scanning Electron Microscope, its basic physics and operational principles,
and, through a structured series of exercises, develop in students elementary operational
skills on an SEM .
1
2. Calculate electron wavelengths and velocities in electron microscopes, and backscatter
coefficients and penetration depths of the electron beam in a sample under investiga-
tion.
4. Present an analysis of an SEM image indicating the relative effects of secondary elec-
trons, backscattered electrons, operating voltage and sample topography and compo-
sition to the appearance of the image.
h
λ= eV
(2)
[2m0 eV (1 + 2m0 c2
)]0.5
Where m0 is the rest mass of the electron, e is the charge on the electron, V is the
accelerating voltage and c is the speed of light (all in SI units).
eV m0 v
[2m0 eV (1 + )]0.5 = p = 2 . (3)
2m0 c2 (1 − vc2 )0.5
Rearranging, this becomes
p2 c2
v=( )0.5 . (4)
m20 c2 + p2
Question 1: Calculate the velocities and wavelengths for electrons accelerated (from rest)
by the following potentials:
• 5 kV
2
• 25 kV
• 300 kV.
Express the electron velocities in both m/s and as fractions of c. Hint: A spreadsheet
programme (Origin, Excel, OO-Calc, Numbers) is more convenient for this question than a
calculator, and a maths. package (Matlab, Mathematica) is even better.
Question 2: Is the electron “beam” really what we imagine a beam to be, for example
like a beam of light? If we assume a negligible beam diameter, what is the average linear
separation of electrons along the axis of the electron beam of
• a 10 nA beam current at 5 kV (SEM)?
• TEM?
2. A system of electromagnetic lenses and apertures to focus and control the electron
beam.
3. A means of visualising the products of the high-energy electron impacts with the
sample.
Electron microscopes may be divided into two basic types:
1. Scanning electron microscopes (SEMs). These record electrons emitted from the sur-
face of the sample. The electron beam is scanned (rastered) across the sample, in
the same manner that the electron beam is rastered across the phosphor screen in a
cathode ray tube (CRT) television or computer monitor. Accelerating voltages in the
range 1 kV - 30 kV are used. Sample thickness is largely irrelevant.
3
Figure 1: When a high-energy electron beam strikes a sample, the interaction is complex!
[5]
Electron microscopes have been expanded to include a wide variety of add-ons and
detectors. Examples include sample mounts (stages) that may be heated to > 1000◦ C,
cooled to a few Kelvin or placed under mechanical stress. Detectors include x-ray, optical
and Raman spectrometers.
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Higher performance electron emitters have been developed, either from single crystals
of lanthanum hexaboride (LaB 6 ) or from field emission guns with an ultrafine tungsten tip.
These high performance emitters produce up to 1000x the emission of a tungsten filament,
with a much smaller electron energy spread, but are much more expensive and require much
higher vacuum conditions. Field emission guns (FEGs) are especially suited to the highest
resolution SEMs, but require ultra-high vacuum conditions. The Electron Microscope Unit
at the University of Sydney has microscopes with all three types of electron gun.
Figure 3: Cross sections of a generic electron lens. a) Note the rotation of the beam as it
passes through the lens. b) The electron path through the lens is helical. Electrons further
from the optic axis undergo greater deflection. Individual lenses vary widely in shape and
power. [2,1]
The lens works by applying a Lorentz force, F = e(v⊥ × B), to any electron with a net
velocity component v⊥ perpendicular to the B field. The electrons spiral through the lens
in a helical trajectory, the frequency of which is the electron cyclotron frequency, ω:
eB
ω= . (5)
m
The higher the magnetic field in the lens, the faster the electrons spiral; their trajectory
is described by:
dθ ηB
= , (6)
dz 2(V 0.5 )
5
where z is the distance travelled within the magnetic field along the axis of the lens, θ is the
angle of rotation, B is the magnetic field, V is the accelerating voltage and η is (e/2m0 c2 )0.5 .
Note that as the operating voltage of the microscope is changed (and hence the electron
velocity!), the magnetic field in the lens must be changed to compensate. This is very
different from an optical microscope where the speed of light in a given medium is constant.
In the final or objective lens, the SEM contains extra sets of coils that allow it to scan
(raster) the electron beam back and forth across the sample.
Figure 4: Scanning coils in the objective (final) lens of an SEM enable the electron beam to
be rastered across the sample. [3]
6
Figure 5: Spectrum of emitted electrons produced by a 10 keV electron beam. The cut-off
at 50 eV is a somewhat arbitrary convention. The majority of SEs are ≤ 10 eV, whilst the
majority of BSEs are close to the beam energy. [6]
where nBSE is the number of BSEs and nB is the number of beam electrons impacting the
sample.
Any regions of lower atomic number (e.g. Al, C, Si) in a sample will appear darker than
areas of higher atomic number (e.g. Fe, Cu, W), which will appear brighter (high Z = more
BSE) . This phenomenon is referred to as “Z contrast”.
We can fit the curve of η versus Z with the following (empirically derived) expression
η = αZ 3 + βZ 2 + γZ + δ (9)
Note that Z is the only dependent variable in Equation 8, i.e. η is dependent only on Z,
and is independent of beam energy or intensity.
• Cu
• U
If your sample contains all three elements, which element will appear brightest and which
darkest?
The type of detector that we use to “see” the electrons is dependent on the electron
energy (i.e. SEs or BSEs).
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that acts like an electron “vacuum cleaner”, drawing into it any low-energy electrons in the
chamber. The E - T also collects any BSEs that happen to be travelling toward it. Above
10 keV beam energy, this BSE component increases significantly. The signal produced by
the E - T is the sum of all the electrons (SE and BSE) it receives.
BSEs are emitted from the surface of the sample with high energies, ≥1 keV, and, in
consequence they are little affected by electric fields in the chamber. BSE detectors are made
to subtend as large as possible a solid angle to the sample in order to maximise collection.
Two most common types of detector are a combined scintillator and light guide (Robinson
detector), and solid state diode detectors, which operate on the principle of electron-hole
pair production induced in a semiconductor by energetic electrons. Below 10 keV, efficiency
in both detector types drops rapidly, so effectively, only the signal from BSEs are detected.
Figure 7: BSE detectors subtend a large solid angle with the sample in order to maximise
the collection area. Common types are scintillators (Robinson), left, and solid state diode,
right. [3]
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Figure 8: Cross section of a generic SEM. Individual designs vary widely. [1]
4 Electron-sample interactions
Electrons impacting a solid are slowed down largely through “inelastic” collisions with outer
shell electrons in the atoms of the solid. These inelastic interactions are of three main types:
3. phonons, which are vibrations of the crystal lattice and result in heating of the sample
(mostly ≤2 eV)
Many of these interactions, as individual events, entail relatively small energy losses, and
we may make a reasonable approximation that the beam electron decelerates as a function
of the distance travelled (in a sample of constant composition).
Figure 9 shows Monte Carlo simulations of electron penetration into an iron sample , at a
range of voltages commonly used in SEM. A number of empirically derived equations for
determining the average stopping distance of the form:
E0β
zD = α , (10)
ρ
E01.68
zDA = 0.064 , (11)
ρ
where zDA is the (Anderson) stopping distance in µm, E0 is the beam energy in keV
and ρ is the density of the material (in g/cm3 ).
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Figure 9: Monte Carlo simulations of electron trajectories. Note the large increase in both
the depth and the width of the electron trajectories with beam energy, giving an indication
of the interaction volume. [1]
Anderson’s approximation is in very common use for biological (carbon based) samples,
however, for higher atomic weight samples, Kanaya and Okayama (1972) proposed a better
approximation:
AE01.67
zDKO = 0.0276 , (12)
Z 0.89 ρ
where zDKO is the K & O stopping distance in µm, A is the (average) atomic weight, and
Z is the (average) atomic number.
1. The boundary of the stopping distance is diffuse, i.e. there is a boundary zone without
clear edges.
2. It assumes that the electron beam is orthogonal to the (smooth) surface of the sample.
Question 4: You are examining a silicon based semiconductor with thick copper and
gold interconnects in an SEM. Using both the Anderson and the K & O approximations,
find the electron stopping distances for electron beams of 5 keV and 25 keV for different
areas of the semiconductor:
• Cu
• Au
• Si
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Question 5: If one of the interconnects was covered with a layer of graphite (ρ =
2.2g/cm3 ), 0.6 µm in thickness, would you be able to see the interconnect through the
graphite at either 5 keV or 25 keV? Carefully read Section 5 of these notes. Does it affect
your answer?
In Figure 10 we can see the origin in the sample of these electrons. Recall that we saw in
Figure 6 that SEs could come from anywhere in the chamber. These SEs derive from BSE
impacts with the chamber walls, the bottom of the objective lens or any other object in the
chamber. In Figures 6 and 10 these are labelled SE3. SE1 and SE2 electrons derive directly
from interactions of the beam electrons or BSEs (shown as BEs in the diagram) with the
sample. As we saw in Figure 5, SEs have low energies (a few eV), so the average distance
they are able to travel within the sample (their mean free path) is also very small. This
means that the SE1s and SE2s that reach the detector must have come from very close to
the surface of the sample. The probability of SE escape decreases exponentially with depth
in the sample:
z
p ≈ exp(− ) (13)
λ
where p is the probability of escape, z is the depth below the surface where the SE is
generated, and λ is the mean free path of the SE. As a generalisation, the limit of SE escape
depth is about 5λ. In turn, λ increases with SE energy, and has a strong inverse dependence
on the the density of free or loosely bound electrons in the sample. The inelastic scatter-
ing and attenuation of SEs takes place predominantly by interaction with conduction band
electrons in the sample, which are abundant in metals but rare in insulators.
11
Examination of Figures 9 and 10 shows that it is possible for BSEs to penetrate a
significant depth into the sample before changing direction sufficiently to exit the sample
and be directly captured by the detector or indirectly via SE3s. For a 20 keV beam,
orthogonal to the sample, the depth above which 95% of the BSEs emitted from the sample
originate may be fitted to the following curve:
where α = 2.47 × 10−5 , β = −3.74 × 10−3 , γ = 0.333, Z is the atomic number and zD is the
average stopping distance given in Equation (11) or (12).
The relative maximum BSE escape depth decreases with atomic number of the atoms
in the sample, so for carbon 95% of the BSEs come from the upper 33% of zD , whilst for
gold 95% of BSEs come from the upper 20% of zD .
Also, examination of Figures 9 and 10 shows that it is possible for BSEs to penetrate a
significant width in the sample before changing direction sufficiently to exit the sample to
be captured. Remember, any electron that escapes the surface of the sample is liable to be
captured and contribute to the signal.
The source of electrons from which we derive the image is thus a complex mixture of
SEs from very near the surface (SE1 and SE2) plus electrons from up to (very roughly) 25%
of the total electron penetration depth (BSEs and SE3s). The relative proportions of (SE1s
+ SE2s) to (BSEs + SE3s) will depend on the beam energy and atomic number(s) of the
sample.
SEM EXERCISE 1: The effect of different signals (secondary and backscattered elec-
trons) and detectors on the SEM image.
Aim: To show the differences in image contrast between Secondary Electron Im-
ages (SEI) and Backscattered Electron Images (BEI) - using large area backscattered
electron detectors.
EM Tutor’s initials:
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Aim: To demonstrate that magnification factor (M), on the viewing screen of an
SEM only is approximately correct, and that to make accurate measurements on SEM
images, it is necessary to calibrate the microscope.
EM Tutor’s initials:
7 References
[1] Goldstein, Joseph et al, Scanning electron microscopy and x-ray microanalysis, 3rd Ed.,
Springer, N.Y. 2003, Scitech Reserve, 502.825 5 B. The standard ref. work on SEM.
[2] http://www.microscopy.ethz.ch/lens.htm
[3] Reed, S.J.B., Electron microprobe analysis and scanning electron microscopy in geology,
Cambridge UP, Cambridge, 2005, Scitech 552.8 15.
[4] Lawes, Graham, Scanning electron microscopy and x-ray microanalysis, Wiley, N.Y.
1987, Scitech 543.0812 2
[5] The following is on transmission electron microscopy, but is exceptionally well written
and contains a lot of relevant material. Williams, David B and Carter, C. Barry,
Transmission electron microscopy : a textbook for materials science, Plenum Press,
N.Y., 1996. Scitech 502.825 44 v.1
[6] The EMU produces excellent training manuals on the operation of the SEM and electron
microanalysis.
[7] The EMU has a useful library in its tea room. Well worth a browse.
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