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EXPERIMENT 31 — The Scanning Electron

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 Intended Learning Objectives


At the conclusion of this experiment you should be able to:
1. Explain the basic physics of the SEM.

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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.

3. Explain the operational principles of the SEM.

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.

5. Undertake some simple operations with an SEM.

2 Why use Electrons?


The resolution of “ordinary” light microscopes is limited by the wavelength of light. The
middle range of the visible spectrum is about 500-550 nm, limiting the resolution of an
optical microscope to about 300 nm.
In 1925, de Broglie theorised that all particles, including the electron, had wave-like
properties, and that the momentum p of a particle could be related to its wavelength λ via
Planck’s constant, h,
h
λ= (1)
p
A couple of years later, Davisson and Germer and Thompson and Reid experimentally
demonstrated electron diffraction, and hence, the wave nature of electrons. In 1932, Knoll
and Ruska built a practical electron lens, coined the term “electron microscope” and con-
structed the instrument shown above, for which Ruska received the Nobel Prize (in 1986!!).

2.1 Electron Velocities


In electron microscopes, we accelerate the electrons by anywhere from 1 keV to >1MeV.
Over most of this range, the electrons attain velocities that are a significant percentage of
the speed of light, so we must treat them relativistically, i.e.

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).

To determine the (relativistic) electron velocity v, we may put

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

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• 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.

2.2 The Electron Beam


In the literature, you will notice many references to the “electron beam”. The (electron)
beam current in an electron microscope most commonly varies between approximately 10
nA and 10 pA. Usually, SEMs use currents in the nA range, whereas Transmission Electron
Microscopes (TEMs) have beam currents in the pA range, especially the higher energy (300
keV+) TEMs.

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)?

• a 10 pA beam current at 300 kV (TEM)?


If our 5 kV SEM has a column length of 0.5 m, and our 300 kV TEM has a column length
of 1.2 m, how many electrons are there in the electron beam at any instant of the
• SEM?

• TEM?

Physics Tutor’s initials:

3 The Electron Microscope


All electron microscopes are built around three basic components:
1. A source of electrons and a means of accelerating them to keV energies (the “electron
gun”).

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.

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Figure 1: When a high-energy electron beam strikes a sample, the interaction is complex!
[5]

2. Transmission electron microscopes (TEMs). These usually concentrate on electrons


that have passed through the sample. TEMs operate on thin samples (≤150 nm) and
at much higher voltages (≥100 kV).

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.

3.1 The Electron Gun


The purpose of the electron gun is to provide an adequate supply of electrons of the required
energy. Your answers to Question 2 should have shown you the the term electron “gun”
is an apt one! Until fairly recently, the most common type was made from a bent piece of
tungsten wire approximately 100 µm in diameter (a “hairpin”). These sources are simple
and inexpensive, and well suited to low resolution microscopy. Electrons from the heated
filament tip are accelerated towards the positively charged anode; the negatively charged
cap over the filament assists focusing the emitted electrons towards the anode aperture.

Figure 2: Tungsten filament electron gun. [1,5]

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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.

3.2 Electron Lenses


Analogous to the lenses in an optical microscope, an electron microscope has a series of
electromagnetic lenses and apertures to produce a focused electron beam at the sample.
Essentially these lenses (see Figure 3) consist of a cylindrical iron case with a bore down
its axis, enclosing a coil of copper wire, through which current is applied to generate the
magnetic field in the gap between the pole pieces.
The magnetic field is rotationally symmetric but radially inhomogeneous across the bore,
so that it is weak in the center of the gap and becomes stronger close to the edges. Electrons
close to the center are less strongly deflected than those passing through the lens far from
the axis. The overall effect is that a beam of parallel electrons is focused into a spot at some
distance beyond the gap (the “cross-over”).

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 )

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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]

3.3 Visualising Electrons


In SEMs, we collect electrons that have been emitted from the surface the sample. As shown
in Figure 1, there is a large range of entities emitted from the surface, but for “seeing” the
surface of the sample we rely on two types of electron emission (Figure 5).
1. Secondary Electrons (SE): These are electrons that have been ejected from the
outer electron shell of an atom as a result of impact from a high energy electron. SEs
have relatively low energies (up to about 50 eV, compared to the 3 - 30 keV of the
beam electrons) and highlight the surface features (topography) of the sample.
2. Backscattered Electrons (BE, or BSE): These electrons are beam electrons that
have undergone sufficient elastic “collisions” (read: Coulomb interactions) with atomic
nuclei and consequent changes in direction to exit the surface of the sample. BSEs
retain a significant percentage of the beam energy, i.e. are in the keV range.
When a (negatively charged) electron passes close to a (positively charged and much
heavier) nucleus, it is deflected, without much energy loss, by an angle θ, so that:
Z
tan(θ/2) = , (7)
(1.4pE)
where p is the minimum distance (in nm) of the undeflected electron path from the nucleus,
Z is the atomic number, and E is the electron energy. Deflection will be greatest for low
electron energies and high atomic number nuclei. High Z elements are more efficient electron
backscatterers, i.e they have a higher backscatter coefficient, η, which is defined as
nBSE
η= , (8)
nB

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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)

where α = 8.3 × 10−7 , β = −1.86 × 10−4 , γ = 0.016 and δ = −0.0254.

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.

Question 3: Calculate the backscatter coefficients for the following elements:


• C

• 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).

3.3.1 Detecting secondary electrons


As you may see from Figure 6, SEs may come from anywhere in the SEM chamber! More
than half the total SEs may originate from the chamber walls. However, all these SEs are
derived from BSEs originating from the sample, impacting the chamber walls and releasing
SEs. The Everhart-Thornley (E - T) SE detector has a grid, positively charged to ≤ 400 V,

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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.

Figure 6: SEs may come from anywhere in the chamber! [1]

3.3.2 Detecting backscattered electrons

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]

3.4 The Scanning Electron Microscope


We may now assemble the components of our microscope into an operational SEM. In
addition to the basic components listed above, the most important is the scan generator,
which synchronizes the rastering of the electron beam over the surface of the sample with the
rastering on the display screen. Additionally, there are a lot of other components; vacuum
pumps, computers, detectors, etc.

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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:

1. with bound orbital electrons, such as ionisation or band transitions,

2. plasmons, which are collective oscillations in weakly bound or delocalised electrons.


These plasmons may be transverse surface waves (a few eV) or volume plasmons, (10
- 30 eV),

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

have been used as approximations of the depth of penetration, (e.g. Andersen),

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.

Three caveats apply to both these approximations:

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.

3. The sample is of uniform composition

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

Compare the results obtained with the two approximations.

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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?

Physics Tutor’s initials:

5 Origin of imaging electrons


The image of the sample we see on the monitor screen, depending on the electron detector
used, will be either a mix of SEs and BSEs or BSEs alone.

Figure 10: Sources of electrons used to produce the image. [6]

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.

For SEs of a few eV, λ ≈ 1 nm in metals and up to ≈ 10 nm in insulators.

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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:

D95% = zD (αZ 2 + βZ + γ) (14)

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.

6 Summary of SEM exercises in EMU sessions


In your two sessions in the EMU you will undertake six exercises on an SEM. A separate
hand-out will be supplied by the EMU containing the exercises in detail. Here is a brief
summary:

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.

SEM EXERCISE 2: Depth of field in the SEM.


Aim: To demonstrate how the depth of field can be varied by changing the working
distance.

SEM EXERCISE 3: Accelerating voltage and beam penetration.


Aim: To show that as the accelerating voltage is reduced, so is the depth of penetra-
tion of electrons into the sample.

EM Tutor’s initials:

SEM EXERCISE 4: Magnification in the SEM.

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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.

SEM EXERCISE 5: High resolution performance of the SEM.


Aim: This exercise aims to take the student through the various parameters that
affect the resolution obtainable in the SEM in order to give them an understanding of
the different factors that need to be considered to obtain optimum performance from
the microscope.

SEM EXERCISE 6: Electron Penetration Depth.


Aim: To compare electron penetration depths, zD derived from empirical formulae,
with penetration depths generated by Monte Carlo modelling.

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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