Name: Jie He UTA ID#: 1000568567 Experiment: SEM

1. Introduction
The Scanning Electron Microscope (SEM) is a microscope that uses electrons
rather than light to form an image. There are many advantages to using the SEM
instead of a light microscope.
The SEM has a large depth of field, which allows a large amount of the sample
to be in focus at one time. The SEM also produces images of high resolution, which
means that closely spaced features can be examined at a high magnification.
Preparation of the samples is relatively easy since most SEMs ony require the sample
to be conductive. The combination of higher magnification, larger depth of focus,
greater resolution, and ease of sample observation makes the SEM one of the most
popularly used instruments in research areas today.
A SEM may be equipped with an EDX (Energy Dispersive X-ray analysis)
system to enable it to perform compositional analysis on specimens. EDX analysis is
useful in identifying materials and contaminants, as well as estimating their relative
concentrations on the surface of the specimen.
In this lab session, we should have a basic understanding how SEM works and it
is used. And then we are required to practice image acquisition using two basic
imaging modes of SEM, SEI and BEI modes, respectively.
2. Background
(1) SEM Setup
The basic SEM setup is shown in Fig. 1. A beam of electrons is generated in the
electron gun, located at the top of the column, where a filament is located. The most
common used filament is Tungsten hairpin gun. This filament is a loop of tungsten
which functions as the cathode. A voltage is applied to the loop, causing it to heat up.
The anode, which is positive with respect to the filament, forms powerful attractive
forces for electrons. This causes electrons to accelerate toward the anode.
This beam is attracted through the anode, condensed by one or two condenser
lens, and focused as a very fine point on the sample by the objective lens. The beam
passes through pairs of scanning coils or pairs of deflector plates in the electron
optical column. The scan coils are energized (by varying the voltage produced by the
scan generator) and create a magnetic field which deflect the beam horizontally and
vertically so that it scans in a raster fashion over a rectangular area of the sample
surface. When the primary electron beam interacts with the sample, the electrons lose
energy by repeated scattering and absorption within a teardrop-shaped volume of the
specimen known as the interaction volume, which extends from less than 100 nm to
around 5 µm into the surface. The size of the interaction volume depends on the
electrons' landing energy, the atomic number of the specimen and the specimen's
density. The energy exchange between the electron beam and the sample results in the
emission of electrons and electromagnetic radiation, which can be detected to produce
an image, as described below.

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Name: Jie He UTA ID#: 1000568567 Experiment: SEM

(a) (b)
Fig. 1 (a) Basic SEM Setup and (b) SEM Optics

(2) Electron/Specimen Interactions

When the electron beam strikes the sample, a large number of signals (shown in
Fig. 2(a)) are generated. We can divide the signals into two broad categories: a)
electron signals, b) photon signals. While all these signals are present in the SEM, not
all of them are detected and used for information. The signals most commonly used
by SEM are the Secondary Electrons, the Backscattered Electrons and X-rays.
The specimen interaction volume (shown in Fig. 2(b)) is the volume inside the
specimen in which interactions occur while interacting with an electron beam.
Therefore we can know SEM is a kind of surface characterization.

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Name: Jie He UTA ID#: 1000568567 Experiment: SEM

(a)

(b)
Fig.2 (a) The signals generated when electron beam strikes the sample, and (b) Specimen
interaction volume.

Secondary electrons are low energy electrons and when produced deeper within
the interaction volume, will be absorbed by the sample. Only secondary electrons
close to the surface will be able to escape the specimen. The weakly negative
secondary electrons will be deflected by a positive pull exerted by the Faraday cage
surrounding the secondary electron detector and therefore will contribute to the image
formation, secondary electrons image (SEI).
Different numbers of secondary electrons produced at different areas of the
sample will provide image contrast. If at a certain spot on the sample more secondary
electrons are produced, a bright spot will appear on the image. Often many secondary
electrons are produced along raised areas of the sample; therefore many electrons will
be detected, producing a bright spot on the image. This effect is called the edge effect.
Some secondary electrons are produced in a valley of the sample and are difficult to
deflect by the Faraday Cage. In this case only few electrons will be detected

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Name: Jie He UTA ID#: 1000568567 Experiment: SEM

producing a dark spot on the image. Therefore, Image formation of surface structures
using the SEM mainly depends on the production of secondary electrons.
Backscattered electrons are also produced deep within the sample but have a
much higher energy and because of this, are able to escape from deeper within the
interaction volume. Because of their high energy, backscattered electrons will not be
deflected by the Faraday Cage and therefore not contribute to the image formation.
Backscattered electrons may be used to detect contrast between areas with different
chemical compositions, especially when the average atomic number of the various
regions is different, since the brightness of the backscattered electrons image (BEI)
tends to increase with the atomic number.
Backscattered electrons can also be used to form an electron backscatter
diffraction image. This image can be used to determine the crystallographic structure
of the specimen.
There are fewer backscattered electrons emitted from a sample than secondary
electrons. The number of backscattered electrons leaving the sample surface upward
might be significantly lower than those that follow trajectories toward the sides.
Additionally, in contrast with the case with secondary electrons, the collection
efficiency of backscattered electrons cannot be significantly improved by a positive
bias common on Everhart-Thornley detectors. This detector positioned on one side of
the sample has low collection efficiency for backscattered electrons due to small
acceptance angles. The use of a dedicated backscattered electron detector above the
sample in a "doughnut" type arrangement, with the electron beam passing through the
hole of the doughnut, greatly increases the solid angle of collection and allows for the
detection of more backscattered electrons.
Therefore, the quality of SEM image is affected greatly by the size of probing electrons and
method of detecting electron emission. In case of SEI, the detector has a fast response and can
work under TV rate. On the other hand, BEI detector works slow and thus cannot be used under
TV rate. Therefore, it is customary to adjust all imaging conditions under SEI mode (using TV
monitor), and create BEI image using slow scan rate imaging method.

(3) Using a Vacuum

When a SEM is used, the column must always be at a vacuum. There are many
reasons for this. If the sample is in a gas filled environment, an electron beam cannot
be generated or maintained because of a high instability in the beam. Gases could
react with the electron source, causing it to burn out, or cause electrons in the beam to
ionize, which produces random discharges and leads to instability in the beam. The
transmission of the beam through the electron optic column would also be hindered
by the presence of other molecules. Those other molecules, which could come from
the sample or the microscope itself, could form compounds and condense on the
sample. This would lower the contrast and obscure detail in the image.

(4) Application of SEM

SEM could be used to characterize the information of sample below:
(a) Topography

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Name: Jie He UTA ID#: 1000568567 Experiment: SEM

The surface features of an object or "how it looks", its texture; detectable features limited
to a few manometers
(b) Morphology
The shape, size and arrangement of the particles making up the object that are lying on
the surface of the sample or have been exposed by grinding or chemical etching;
detectable features limited to a few manometers
(c) Composition
The elements and compounds the sample is composed of and their relative ratios, in areas
~ 1 micrometer in diameter.
(d) Crystallographic Information
The arrangement of atoms in the specimen and their degree of order; only useful on
single-crystal particles >20 micrometers

3. Experiment
The samples inside SEM are penny and nickel. Find the joint area and
magnification this part, and take pictures under SEI mode and BEI mode. Besides,
BEI mode has two different modes: COMP and TOPO mode. Present all the images in
the report and compare them. Record the SEM setting of every image.
4. Results and Discussion
(1) Joint area between Penny and Nickel
The SEM setting of images (shown in Fig. 3) taken in joint area is:
Magnification: ×100
Working distance: 15mm
HT: 19.0kV
Probe current: 3×10-9A

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Name: Jie He UTA ID#: 1000568567 Experiment: SEM

(a) SEI of joint area between Penny and Nickel

(b) COMP mode image of joint area between Penny and Nickel

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Name: Jie He UTA ID#: 1000568567 Experiment: SEM

(c) TOPO mode image of joint area between Penny and Nickel
Fig. 3 Different SEM mode images of joint area between Penny and Nickel.
(2) Magnification area on Penny
The SEM setting of images (shown in Fig. 4) taken on Penny is:
Magnification: ×2000
Working distance: 15mm
HT: 19.0kV
Probe current: 1×10-9A

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Name: Jie He UTA ID#: 1000568567 Experiment: SEM

(a) SEI of some area on Penny

(b) COMP mode image of some area on Penny

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Name: Jie He UTA ID#: 1000568567 Experiment: SEM

(c) TOPO mode image of some area on Penny

Fig. 4 Different SEM mode images of some area on Penny.
(3) Comparison between images taken at different modes
From the SEI images, we can tell the morphology of the sample’s surface, the
shape of the coins, the gap between them, the size of the gap and the coins, and the
arrangement of the coins, we can know which side is Penny and which side is Nickel.
And also we can see clearly the dust (bright spot in the SEI image) on the coin.
The COMP images can provide elemental composition variation in the sample.
Backscatter imaging can distinguish elements with atomic number differences of at
least 3, i.e., materials with atomic number differences of at least 3 would appear with
good contrast on the image. That is because the efficiency of production of
backscattered electrons is proportional to the sample material's mean atomic number,
which results in image contrast as a function of composition. The materials with
higher atomic number would be brighter than low atomic number materials in COMP
image. Therefore, we can tell that the bright area and dark area in our COMP images
have different elemental composition. Due to Penny and Nickel are made of copper
and nickel, and the atomic number of copper is bigger than that of nickel, so the areas
which contain copper is a little brighter than the areas which contain nickel in the
COMP image. Besides, there maybe some dust on the coin, and that will also cause
the different contrasts.
From the TOPO images, we can tell the surface topography of sample: the
surface features and its texture. Therefore, we can see clearly the texture on the joint
area and on the Penny.

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Name: Jie He UTA ID#: 1000568567 Experiment: SEM

5. Problems
a. The current of electron beam is the probe current. The current in the condenser
lens changes the spot size or diameter of the beam of electrons that scans the sample,
and therefore will affect the probe current. More detailed information will be
collected when the electron beam scans the same area with a smaller spot size. An
increased current or a higher number for the condenser lens setting, will produce a
smaller spot size and in general will result in a better resolution.
The disadvantage of obtaining a better resolution using a higher probe current is
the effect on the beam current or number of electrons available to interact with the
specimen. An increase in condenser lens current results in a lower beam current. The
effect of a lower beam current is that fewer electrons interact with the sample and
therefore fewer secondary and back scattered electrons become available to form an
image. Electronically this signal can be increased to compensate for the low beam
current but this will also result in an increase in electronic noise. Because of the
increased noise, it will be more difficult to focus the specimen and the final image
will start to look grainy as well.
Therefore, a correct balance between spot size and beam current needs to be found
for getting a good quality and high resolution image.

b. The working distance is the distance between the final condenser lens and the
specimen. Changing the working distance will have an effect on the spherical
aberration of the imaging system and therefore will effect the resolution of the final
image (Fig.5). Spherical aberration is the failure of the lens system to image central
and peripheral electrons at the same focal point. Electrons passing along the axis of
the electron beam refract less than electrons passing through the periphery of the
electron beam creating more than one focal point and therefore resulting in an
enlarged, unsharp spot. When the working distance decreases, this effect of spherical
aberration will become less, the spot striking the specimen will become smaller and
therefore will improve resolution.

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Name: Jie He UTA ID#: 1000568567 Experiment: SEM

Fig. 5 The effect of working distance. (A) If spherical aberration is present, the beam
will scan with an enlarged, unsharp spot. (B) If spherical aberration is absent, the
beam will scan with the sharpest spot possible.

The working distance also has an effect on the depth in the sample that appears
to be in focus or in other words, has an effect on the depth of field. At a short working
distance the sample will be scanned with a wide cone of electrons resulting in an
image with little depth of field. At a longer working distance the sample will be
scanned with a narrow cone of electrons resulting in an image with an increased depth
of field (Fig. 6). A longer working distance will not provide the optimal resolution. If
a sample with large topographical variation needs to be scanned it may be important
to use a longer working distance to bring as much of the image into focus as possible;
however, some of the resolution will be lost. If a relative flat sample is scanned it is
possible to benefit from a better resolution using a shorter working distance since
depth of field becomes less important. Depending on the sample and the contained
features, a correct balance between working distance and depth of field needs to be
found for a good quality and high resolution image.

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Name: Jie He UTA ID#: 1000568567 Experiment: SEM

Fig. 6 The shape of the cone of electrons depends partly on the working distance and
is important in determining the depth of field of a sample. (A) At a short working
distance little of the sample appears to be in focus. (B) At a long working distance,
more of the sample appears to be in focus because of a greater depth of field.

c. Specimens need to be conductive when examined using a SEM. When a specimen

is nonconductive a negative charge from the electron beam tends to accumulate, thus
effecting the final image. Some of the effects are abnormal contrast, appearing of
abnormal lines or shifts/breaks within the image. Biological samples are mainly
nonconductive and need to be coated with a thin layer of metal making the surface
conductive. Specimens like metals and most semiconductors are conductive and can
be examined without coating.

d. SEM is often equipped with analytical tools such as EDX and WDX for elemental
characterization.
(1) EDX Analysis stands for Energy Dispersive X-ray analysis. It is sometimes
referred to also as EDS or EDAX analysis. It is a technique used for identifying the
elemental composition of the specimen. The EDX analysis system works as an
integrated feature of a scanning electron microscope (SEM), and can not operate on
its own.
During EDX Analysis, the specimen is striked by an electron beam inside the
scanning electron microscope. The electrons collide with the specimen atoms' own
electrons, knocking some of them off in the process. A position vacated by an ejected
inner shell electron is eventually occupied by a higher-energy electron from an outer
shell. To be able to do so, however, the transferring outer electron must give up some
of its energy by emitting an X-ray.
The amount of energy released by the transferring electron depends on which
shell it is transferring from, as well as which shell it is transferring to. Furthermore,
the atom of every element releases X-rays with unique amounts of energy during the

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Name: Jie He UTA ID#: 1000568567 Experiment: SEM

transferring process. Thus, by measuring the amounts of energy present in the X-rays
being released by a specimen during electron beam bombardment, the identity of the
atom from which the X-ray was emitted can be established (Fig. 7).
The output of an EDX analysis is an EDX spectrum. The EDX spectrum is just a
plot of how frequently an X-ray is received for each energy level. An EDX spectrum
normally displays peaks corresponding to the energy levels for which the most X-rays
had been received. Each of these peaks are unique to an atom, and therefore
corresponds to a single element. The higher a peak in a spectrum, the more
concentrated the element is in the specimen.
An EDX spectrum plot not only identifies the element corresponding to each of
its peaks, but the type of X-ray to which it corresponds as well (Fig. 7).
The pros of EDX is simple to operate and maintain, and it is cheap comparing
other elemental characterization equipment.
The cons of EDX is it has bigger noise and lower resolution (about 0.5 at%)
comparing WDX.

Fig. 7 Elements in an EDX spectrum are identified based on the energy content of the
X-rays emitted by their electrons as these electrons transfer from a higher-energy
shell to a lower-energy shell

(2) WDX Analysis stands for Wavelength Dispersive X-ray analysis. It is

sometimes referred to also as WDS analysis.
WDX analysis works in pretty much the same way as EDX analysis, except that
its detector classifies and counts the impinging X-rays in terms of its characteristic
wavelengths. The detector system uses an X-ray analyzing crystal that only allows
the diffraction of desired wavelengths into the X-ray detector for counting.
The pros of WDX is: 1) a much better energy resolution, preventing many peak
overlap errors frequently encountered in EDX analysis; and 2) lower background
noise allowing a more accurate quantitative analysis.
The cons of WDX is: 1) higher time consumption; 2) greater sample damage
and chamber contamination because of the high beam currents required; 3) high cost;
and 4) bulky..

e. When the electron beam strikes the sample, a large number of signals (shown in
Fig. 2(a)) are generated. Except secondary electrons and backscattered electrons, there

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Name: Jie He UTA ID#: 1000568567 Experiment: SEM

are some other signals could be detected, such as Auger electrons.

Auger Emission Spectroscopy (AES), or Auger Analysis, is a failure analysis
technique used in the identification of elements present on the surface of the sample.
Like EDX and WDX analysis, AES involves the bombardment of the sample with an
energetic primary beam of electrons. This process generates, among other things, a
certain class of electrons known as Auger electrons.
The energy content of the emitted Auger electron is unique to the atom where it
came from. Thus, AES works by quantifying the energy content of each of the Auger
electrons collected and matching it with the right element.
AES has the ability to provide excellent lateral resolution, allowing reliable
analysis of very small areas (less than 1 micron). It also offers satisfactory sensitivity,
detecting elements that are less than 1% of the atomic composition of the sample.
Coupled with ion-sputter milling capability and raster scanning, AES can even be
used to generate 3-dimensional maps of elemental distributions of a volume of the
sample. This analysis technique is known as scanning auger microscopy (SAM).
The output of AES is referred to as an Auger spectrum. This spectrum would
show peaks at Auger electron energy levels corresponding to the atoms from which
the auger electrons were released.
However, AES has the following limitations: 1) charging up of insulative
surfaces when struck by the primary electron beam; 2) damage to certain materials,
especially organic ones, when struck by the electron beam; 3) occurrence of matrix
effects, i.e., signal alterations when some elements are present in particular matrices.

Note: I should be in the Monday morning group, but this time I attended the Thursday
morning group, that is because that Monday morning I was out of town for research
with my instructor. So the experiment data is the same with the Thursday morning
group. Thanks.

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