Scanning Electron Microscope (SEM)

Introduction

The first electron microscope was built in 1931 by Ernst Ruska and Max Knoll. It
was greatly developed through the 1950s and has allowed great advances in the natural
sciences. The small wavelength of the electrons allow a much higher resolution than
light microscopes (ca. 0.1 nm for Transmission Electron Microscope (TEM), 1-20nm for
Scanning Electron Microscope (SEM) compared to >200 nm for light microscopes). In
both types of electron microscopes high voltage electron beams from a cathode are
focused by magnetic lenses on to the specimen. They are then magnified by a series of
magnetic lenses until they hit light sensitive sensors which transfer the image to a
computer screen. The image produced is called an electron micrograph (EM). While a
Transmission electron microscope (TEM) produces images by detecting electrons that
are transmitted through the sample, the Scanning electron microscope (SEM) produces
images by detecting secondary electrons which are emitted from the surface due to
excitation by the primary electron beam.
The SEM image relies on surface processes rather than transmission it is able to image
bulk samples and has a much greater depth of view, and so can produce images that are a
good representation of the 3D structure of the sample. SEM has revolutionized the
microstructure characterization of various materials, when combined with a range of
elemental analytical techniques, such as energy dispersive spectroscopy (EDS or EDX)
and wavelength dispersive x-ray spectroscopy (WDS or WDX). It is routinely used in
'materials research and characterization laboratories.
As shown in Fig. 1 various phenomena (emissions) occur when a beam of
electrons strikes the surface of a solid material. These include the secondary electrons,
backscattered electrons, characteristic X-radiation, Auger electrons, cathode-
luminescence, in addition to the absorbed electron current and transmitted electrons, etc
(substantial transmission occurs only when the specimen plate is thin enough). All these
emissions can be used to explore the topography, surface structure, atomic number,
elemental composition and distribution, and crystallinity of the material, when they are
properly collected and analyzed.

Fig. 1 Interactions of an electron beam of high energy with

a solid material

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Fig. 2 Basic set-up of a conven-
tional SEM consists of:
(i) Electrons are produced with an
electron gun (tungsten filament
or field emission type gun) in
principle similar to the one in a
classic CRT monitor or TV;
(ii) The electrons are then accele-
rated through the anode plate
and focused with a magnetic
lens system;
(iii)Scanning coils force the
focused electron beam to
rapidly scan over an area of
the specimen in
(iv) the specimen chamber/stage.
(v) An image of the specimen can
be viewed on a monitor (and
recorded) in the backscattered
or secondary electron mode.
(vi) A vacuum system is required
to maintain the vacuum along
the path of the electron beam.

The basic working principle of SEM is schematically illustrated in Fig. 2 above. A

very fine probe (beam) of electrons with energies up to 30 to 40 keV is focused at the
specimen surface in a vacuum chamber and scanned across it in a 'raster' or pattern of
parallel lines. Of the several phenomena occurring at the specimen surface under electron
impact (cf. Fig. 1), the emission of secondary electrons with energies of a few tens of eV
and reemission or reflection of the backscattered electrons of high energy from the
primary electron beam are important. The intensity of emission of both secondary and
backscattered electrons is very sensitive to the angle (why?) at which the electron beam
strikes the surface, i.e. to topographical features of the specimen. Both types of emitted
electron current can be collected and amplified. The variation in the resulting signal
strength, as the electron probe is scanned across the specimen surface, is then used to vary
the brightness of trace of a cathode ray tube being scanned in synchronism with the
electron probe. There is thus a direct positional correspondence between the electron beam
scanning across the specimen surface and the fluorescent image on the cathode ray tube.

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The following operation modes are commonly
found in a conventional SEM:

(1) Secondary electron image

Secondary electrons are low energy electrons
that originate from the specimen atoms by
collision with high energy electrons. The latter
may be primary electrons entering the specimen
or backscattered electrons on their way out of it.
Fig. 3a: Secondary Electron Image re-
(2) Reflected or backscattered electron image vealing the broken surface of a piece of
Reflected or backscattered electrons are those metal. Secondary electron images
electrons from the primary electron beam which produce a depth of field that reveals the
have interacted with nuclei in the specimen and surface topography.
have been turned back out of the specimen
again. Depending on their individual collision
histories, they may have energies ranging from
the full primary beam energy down to the level
of secondary electrons. In many cases, the
origins of emitted electrons cannot be
determined precisely, since it is not possible to
identify individual electrons except in terms of
their energy levels. As illustrated in the plot
below, one of the most important features of
reflected or backscattered electrons is their
dependence of intensity on the atomic number of
Fig. 3b: Backscattered Electron
scattering atoms. This is utilized in Imaging reveals information about the
differentiating the phases or grains of differing material compositional differences. In
composition in various materials. this example the lighter areas are
mostly aluminum and the dark areas
(3) X-ray photons for elemental analysis: are mostly copper.
X-ray photons with the wavelength and energy
characteristic of the elements in a specimen are
emitted under electron bombardment. The spectrum
can thus be used in elemental identification.
When an atom is bombarded by electrons of high
energy, energy is transferred to the atom as a result
of the inelastic collisions. When an electron, e.g. a
K electron, is given enough energy, it will overcome
the nuclear attraction and escape from the atom.
The energy required for the escape is defined as the
binding energy, which is also called the absorption
energy of the K electron. It is a quantity
characteristic of the atom species and increases with
atomic number of the element. Removal of a K
electron in this way leaves a vacancy in the K shell,
Fig. 4: Dependence of backscattered
which can be filled by an electron from one of the
electron intensity on atomic number
higher energy shells, i.e. L, M, etc. The excess
energy of the electron, i.e. the difference between
energy states in the two shells, is radiated during the transition as a photon of x-ray

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radiation. Thus, the energy of Kα X-ray radiation equals EL-EK, if the transition is
between L and K shells. A similar situation is created for the electrons in L shell (and M
for atoms of sufficiently high atomic number). Every atom species, therefore, exhibits a
characteristic X-ray emission spectrum, which can be excited by supplying a level of
energy equal to or in excess of the appropriate binding energy by electron bombardment.
In energy dispersive spectroscopy (EDS or EDX), a semiconductor detector is employed
to classify the x-radiation spectrum according to energy level. On the basis of this, a
number of analytical functions can be carried out, including point, line and area analyses,
and X-ray mapping.
The interaction of the beam with the
specimen is known as the interaction
volume, and is the volume below the
surface of the material, in which,
primary electrons interact with electrons
orbiting around atoms of the incident
material. The (low-energy) secondary
electrons are detected from a near-
surface region of this volume. As
mentioned above the surface topography
has a high influence on whether a
secondary electron may reach the
detector. Backscattered electrons can be
detected from this and much deeper
parts of the specimen. Many electrons escaping from this region are absorbed into the
material or not detected at all, as is the case with a small number of x-rays. The range of
detected electrons and x-rays is said therefore to have come from the sampling volume.
The sampling volume for x-rays is similar in size to the interaction volume as x-rays are
less easily absorbed by the material. The diagram below is a simple illustration of the
interaction volume and particle detection zones-

Magnification and Resolution

The magnification produced by a SEM is the ratio between the dimensions of final image
displayed on the screen and the field scanned by electron beam on the specimen surface.
For example, if the electron probe is scanned across an area of 1 mm square on the
specimen surface and the output is displayed on a screen of 100 mm square, then the linear
magnification is 100 times. Changes in magnification are brought about by altering the
extent of scan on the specimen surface whilst keeping the size of display constant. In
practice, the magnification switch or button in SEM actually varies the angle through
which the beam is deflected, and therefore the linear extent of scan depends on the
distance (working distance) between the specimen surface and the final lens. In a typical
SEM, the magnification covers the range of x 20 to x 100,000 at a working distance of
11mm. It can be extended to the range of x 10 to x 200,000, when the working distance is
varied between zero and 35 mm.
The resolving power of SEM is therefore directly influenced by the smallest area which
can be scanned by the probe. This is in turn controlled by the diameter of the electron
beam (or effectively the sampling volume). Minimizing the probe diameter calls for a lens
system with small aberrations and high electrical stability. In reality, the smallest probe
that can be formed with enough electrons in it is dependent on the focal length or working

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distance of the final probe-forming lens and the brightness of electron gun. For
conventional tungsten filament gun and a working distance of about 10 mm, the size is
about 4 nm. Therefore, the secondary electron resolving power is somewhere between 4
to 7 rim. Better resolving power is only attainable by employing a stronger lens or a
brighter electron source. However, the practical resolutions in secondary and
backscattered electron images are generally poorer than the probe diameter would suggest,
because an electron beam of high energy penetrates and diffuses sideways in the
specimen, releasing electrons from a wider area than that actually illuminated by the
focused probe.

The 3D appearance of secondary electron images is closely related to the highlighting of

edges due to the fact that at the edges a larger region of the interaction volume is close
enough to the surface that secondary electrons can escape:

Fig. 5: Schematic
representation showing the
influence of the surface
topography on the number of
escaping (i.e. detectable)
secondary electrons.

2. Experiment

Student has to read through

the experiment’s risk
assessment prior to
beginning their
experiments.

There are 2 parts to this.

Part 1, you will be provided with two specimens that differ in composition and
microstructure features. They are paper and BSE reference. A Philips XL30 will be used
to characterize the two specimens. Demonstrator will assist you in learning and acquiring
the basic skill of operating the SEM.

Part 2, prepare a solid specimen you obtain from your surroundings. Use the SEM to study
and understand the “inner workings” of this solid specimen.

You should NEVER try to operate it by yourself until you have reached a certain standard
as judged by your demonstrator. If there are any questions, please consult the lab officer
in-charge. It is also very important to remember if you are not sure what you are doing,
STOP and ASK.

(1) XL30 is fully computerized with almost all the switches and buttons being controlled
by keyboard and mouse. To start with, you will be given a brief by the technician on the
major components of XL30, such as the vacuum column, specimen chamber, specimen
stage, various detectors in the chamber, control unit (computer) and the image recording
system.

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(2) The lab officer will assist you in loading the first one of the two specimens provided
into a specimen holder and then to the specimen stage in the SEM chamber. You are
required to wear gloves when handling the specimen and specimen holder, in order to
avoid contamination to the specimen stage and SEM chamber.

(3) With the help of the lab officer, you then learn how to obtain an image formed by
secondary electrons for the specimen. You will find out how to optimize the quality of the
image by adjusting a number of operation parameters (switches and buttons in old types of
SEM) such as stigmator, spot-size, contrast, brightness, magnification and focus controls.
By doing this, you will experience how these parameters can affect the image generated by
secondary electrons. You may also alter the parameters such as working distance and
accelerating voltage, under close supervision of the demonstrator.

(4) Having repeated (3) for obtaining an image formed by backscattered electrons, you
should record (print) images (micrographs) formed by secondary and backscattered
electrons, respectively, for a selected area in the specimen.

(6) Perform both point and area EDX analyses in an area that you are interested in.
Record (print) both the image and x-ray spectrum and then correlated them together.

(7) Repeat the above procedures for the other specimen provided in the second unit.

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3. Homework and Questions

(a) Describe the micrographs taken in both secondary and backscattered electron modes
for each specimen. Explain their differences. In the case of the insulating specimen, what
are the additional procedures/steps taken. Why?

(b) On the basis of EDX spectra, you should be able to tell the main composition for each
of the specimen provided.

(c) You are given a material consisting of grains of Al2O3 and HfO2. What image mode
will you use for differentiating the two types of grain?

(d) Many materials, such as ceramics and polymers, are not electrically conductive
(enough). What will be the consequence of directly imaging a non-conductive material in
SEM? Suggest how the problem can be solved.

(e) As you may have realized, SEM compresses information from what is a three
dimensional object into a two dimensional image. Suggest how you can take a
stereoscopic pair of micrographs by SEM and then superimpose them together in order to
obtain a 3-D image.

(f) Two of the main advantages offered by SEM over conventional optical microscope are
high magnification and large field depth. Explain the reason behind these.

(g) What is astigmatism? Explain in detail. Is astigmatism present in the SEM imaging
and if yes, how it is corrected? Justify your answers.

(h) In Part 2 of the experiments, justify why this sample was chosen and write a paragraph
on your observations when this sample was viewed at high resolution.

4. Reference Books
1. S.L. Flegler, Scanning and transmission electron microscope: An introduction.
W.H. Freeman, NY (1 993), QH212 ScaF.
2. J.W. Edington, Practical electron microscopy in materials science. Vol.1-4, Macmillan
Press Ltd, 502.8 Ed44.

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