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A TERM PAPER
BY
MARK, UDOCHUKWU
20044449298
SUBMITTED TO
AUGUST 2005
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PREFACE
This term paper surveys the applications of electron microscopy in the field
research and writing skills since my undergraduate days. This is the third
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TABLE OF CONTENTS
Title Page i
Preface ii
1.0 Introduction 1
1.2.3 Microscopy 8
2.3.1 General 17
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5.1 Introduction 48
6.0 Conclusion 63
References 65-67
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CHAPTER ONE
2.0 INTRODUCTION
The title of this paper indicates an interest in the field of materials and
and ceramics, polymers and many other natural and man-made materials.
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metallic materials. Hence, materials engineering was born in the early 1970s.
and the recognition of the fact that the same principles of science and
This term paper therefore, may have been better titled, ‘Applications of
science and engineering includes both the basic knowledge (the science) and
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ceramics and glass, polymers, and composites. By this definition, liquids and
gases are ruled out. Again, solid-state physics and chemistry are implied in
the term materials science, so that the biological sciences are not
nanotechnology, etc.
techniques are employed. The microscope ranks top among such analytical
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the physical aid used are a measure of the level of the observation. The
higher is the magnification, the finer is the level. The details that are
details disclosed at some other level1, 15. Depending on the level, we can
about 1500 times linear, without loss of resolution of details of the structure.
The limit of resolution of the human eye is about 0.3mm, that is, the eye can
distinguish two lines as separate lines, only when their distance of separation
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is more than 0.3mm. The optical microscope can resolve details up to a limit
minute scale. NB: The term ‘microstructure’ is used quite often in technical
arrangement of a few atoms within what is called a unit cell. The crystal
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patterns in space i.e. three dimensions. The main technique employed for
ELUCIDATION
The science of materials uses diverse methods for the testing and analysis of
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the role of the traditional analytical laboratory has now been expanded to
reasons for looking at these materials have also multiplied. The demand for
materials with unique properties grows on daily basis, and so also does the
them.
The numerous methods, which may differ substantially from one another,
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1.2.3 MICROSCOPY
any other electromagnetic radiation that may result from the interaction of
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A. OPTICAL MICROSCOPY
the study of metals, and their alloys. It enables opaque objects to be seen
glass lenses and prisms. The useful magnification, however, cannot exceed
detect elements of a structure not less than 0.2µm in size, which is in most
alloy.
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B. ELECTRON MICROSCOPY
follows that the lower the wavelength, the better the resolving power
achievable.
The resolving power feasible in an electron microscope is 100 000 times that
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than that of optical microscopes. Thus, the maximum magnification that can
electrons passes through the object, the image formed being the result
the SEM and the TEM, i.e. it is a hybrid of the two basic types of
electron microscopes.
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CHAPTER TWO
occurs when the moving electron losses some of its kinetic energy as a result
The different signals are used in different microscopes and for different
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of thin crystalline films or foils. The conventional or standard mode uses the
must be very small so that electron waves can pass through. They are usually
made in form of thin metallic films (100 - 2000Ǻ thick) or replicas (moulds)
electron beam strikes the specimen, part of the beam is diffracted by the
crystal planes in the material, and the remainder will pass directly through
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either the image formed by the direct or transmitted beam or the image
formed by the diffracted beam. The TEM is so constructed that either of the
When the diffracted beam is intercepted [by a diaphragm in the optical path
of the TEM], while the transmitted beam is allowed to pass through the
the matrix crystal and therefore visible in the image as a result of loss in
intensity of the beam where it passes through the more opaque particles. Of
more general interest, however, is the case where imperfections are faults in
the crystal lattice itself, e.g. dislocations. Because these imperfections cause
diffraction of the beam, they are visible in the image formed by a direct or
dark lines.
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pass, while the transmitted beam is cut off. The image of the specimen
zone that has its axis parallel to the electron beam. The diffraction patterns
can yield information both about the nature of the crystal structure (bcc, fcc,
Furthermore, the TEM has a diaphragm in its optical path that controls the
microscope is operated to form images by bright field (BF), dark field (DF),
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formed by the interference of at least two beams in the image plane of the
objective lens. In the scanning mode, the TEM is used as a SEM i.e.
2.3.1 GENERAL
In most cases the TEM can be used to derive information of several different
kinds which extend right across the sciences concerned with elucidating
Materials of interest here are fibres and small particles in which the natural
surface has a direct bearing on the properties and uses of the material.
studying a prepared surface. The TEM may be used to cast a shadow of the
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One of the first applications of the TEM was to study the size, shape and
and fibres show the shape of the object and, if the specimen preparation is
applications in this area are the study of particle shape and size distribution
from
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are of an effective size greater than the resolving power of the TEM can, in
electron scattering power between the defect and the surrounding perfect
lattice of atoms.
study of line and planer defects. Information can be obtained about partial
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condensation of point defects. The nature of these loops i.e. whether they are
the crystal or foil thickness is known so that a true volume count can be
obtained. Slip planes or twinning planes can be characterized and the nature
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material and is often at the size level too small to allow an examination by
precipitates and second phase particles. This could comprise, for example,
materials are often non-crystalline e.g. glass and carbon fiber material and
polymers.
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operation of the conventional TEM that yield useful information but have, a
The fringes observed in the images of stacking faults are often termed
into the electron micrograph image and the origin of the fringe pattern
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such fringes.
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e.g. the presence of bubble signifies unity and its absence zero.
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CHAPTER THREE
instrument that greatly extends the usefulness of the optical microscope for
field than can be attained optically. The SEM is capable of greatly extending
A SEM has a lower resolution than a TEM, but its advantage is that the
with many new data and extended our knowledge of peculiarities of the fine
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surfaces. The depth of field of the SEM can be as great as 300 times that of
the optical microscope. This feature makes the SEM especially valuable for
analyzing fractures.11, 17
On the other hand, at low magnifications, that is, below 300 to 400x, the
raster. The interaction of this sharply pointed beam with the specimen
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furnish useful information about the nature of the specimen at the spot under
the beam. In the standard mode of the SEM, one normally uses the
secondary electrons to develop an image. The reason for this is that the
secondary electron signal comes primarily from the area directly under the
beam and thus furnishes an image with a very high resolution or one in
The typical SEM uses 1000 line scans to form a 10 x 10cm image. A CRT
(cathode ray tube) screen with a long persistence phosphor is used so that the
image will last long enough for the eye to be able to see a complete picture
photographic record of the image, on the other hand, a cathode ray tube with
requirements for suitable specimens are much less stringent than for
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transmission microscopy. With the SEM, virtually anything that does not
examined using emissive effects. The SEM may utilize any of a number of
These modes are closely related. The reflective mode uses reflected or
discussed below.
required.
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science that is concerned with surfaces is likely to benefit from the emissive
more difficult. The types of problem associated with textile research include
the determination of the size distribution of constituent fibres and the study
fabrics. An added bonus of the SEM is that the large specimen chamber
studies.
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Important contrast effects in the emissive mode arise from the presence of
cases the trajectories of the secondary electrons are altered by the electric
magnetic domains.
This is another contrast effect observable in the emissive mode and one
accelerating voltage for the microscope. The lower the voltage at a particular
specimen area the brighter will be the corresponding area in the CRT image.
semiconducting materials and devices e.g. the p-n junction. If a p-n junction
with reverse bias is mounted in the microscope the p and n type material will
be at different voltages and thus the junction region is revealed. The location
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provide information about the device under actual operating conditions and
Although the reflective mode is often used to detect channeling patterns they
photographic film suitably placed in the vicinity of the specimen will record
a ‘channeling type’ pattern if the scan generator is switched off. The term
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Channeling patterns have very useful properties relating to the fact that they
depend upon the crystallography of the specimen. The angular width of any
band is 2θ and so depends not only on crystal properties i.e. interplanar or‘d’
spacings but also upon the accelerating voltage which controls the electron
spacings and hence the lattice constants. Lateral movement of the specimen
causes no change in the ECP but a tilt or rotation will produce change, a
property shared with Kikuchi patterns seen in the conventional TEM. Hence,
Apart from instrumental factors, the quality of ECP’s depends upon the
perfection of the crystalline sample and this property has been exploited in
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difference between the primary current (incident electron beam) and the sum
not be confused with the widely used conductive mode which exploits
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with voltage contrast obtained in the emissive mode. The basis of the
thereby leave the holes. The process of charge separation with its resulting
Two types of problem can be tackled with the conductive mode of scanning
semiconductor devices such as diodes and field effect transistors (FETs) can
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escaping radiation;
The dwell time of the probe at any point on the sample is greater than
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The link between impurities and luminescent centres has been widely
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applications.
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homogenous composition.
number elements for which the x – rays have low energies and long
energy.
electrons: the electron knocked out of an inner shell, the outer – shell
electron that jumps into the inner – shell hole, and the ejected outer
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than three electrons because three electrons are needed for an Auger
energy per unit energy interval (ε) versus the energy of the electrons
(E).
elements above He. It also has a spatial resolution > 100nm, which
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problem. 12, 17
(iii) crystallographic,
range of materials. Moreover the method has certain advantages over more
traditional techniques e.g. it can reveal the internal domain structure. Apart
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from the domain patterns themselves the probe may be used to investigate
the field distributions from recording tapes and heads. As far as electrical
Success in the use of all the modes of the SEM came as a result of
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CHAPTER FOUR
The attraction of marrying the resolution of the TEM with the versatility and
signal processing of the SEM is obvious and this explains the growing
on to the specimen which is them scanned in the usual way. Unlike the
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Since its early development in the late 1960’s by a group in Chicago, the
the STEM for the structural analysis of crystalline objects. They pointed out
the specimen. 7
materials have also been analyzed by the EELS technique]. When equipped
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constitutes an extremely powerful tool for microanalysis and its impact into
the microelectronic age has been noted. All aspects of its performance rely
on the “nanoprobe”.7
The future trend of the STEM is that of eclipsing the conventional TEM and
goal of designing a high resolution STEM, i.e. a device which will match the
analyzer, this instrument and technique has been used to observe single
crystallographic defects.12
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present time work at voltages up to 1MV, and some are designed to use
where it is clear that many defects structures and dynamic processes in very
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(100kV) microscopy. Also, the term ‘environmental cells’ implies that the
physics and chemistry abound in the use of environment cells for high
cells the life sciences will also benefit. The design of successful and
facilities into the SEM. Similar techniques can also be combined with the
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data on a very fine scale. For this reason it is ideally suited to a whole range
fitted to the new STEM class of microscopes. Energy analyzers have also
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CHAPTER FIVE
ANALYSIS
5.1 INTRODUCTION
Instruments capable of analyzing the chemical nature and the electronic state
of surface atoms have been developed at a rapid rate in the last few years,
utilizing all kinds of interaction with incident photons, electrons and ions.
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microscopy (SAM).
heat, and conductivity). This new technique, not only offers sensitive
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detecting the infra-red radiation emitted from the sample surface. The
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lie within 10 µm of the surface. However, owing to the fact that the
for other materials, e.g. for detection of planes and grains in alloys or
dynamic studies.
Very high gradients of electric fields at the surface of a metal cause emission
microscopy.
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current) depends on the voltage and the work of emission; the lattice
structure and local geometric structure of surfaces can be studied with high
boundary was located in the tip) the structure and the movement of grain
boundaries as well as changes of the tip material during heating have been
oxides) changes the image drastically, which has been used for studying the
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atomic dimensions (< 0.15 nm), are achieved in field ion microscopy (FIM).
Noble gas atoms (usually Helium) are ionized at the cooled surface of a
pointed metal tip. The ions are accelerated by a high voltage and hit a
resolution image of the tip is obtained showing individual atoms and their
arrangement.
Terrace steps ionize most strongly and, therefore, appear bright. Lattice
defects cut by the tip surface, such as dislocations, stacking faults, grain
taking photographs after certain time intervals. Moiré simulation can be used
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spectrometer, the chemical nature of atoms pulled off the tip surface by a
very large high voltage impulse can be identified. The atom passes a hole in
the screen and hits a detector, and from TOF the specific mass is calculated.
By positioning the tip with respect to the aperture hole, it is possible to focus
each individual atom (FIM atom-probe). The same physical principle allows
to analyze the chemical composition of the entire tip in the field desorption
the screen with a pulsed potential. Successive layers of the tip can be
microscopy can be carried out by field-ion microscopy and the atom probe.
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work, is used most widely in the study of metals. Here, a short account is
Soft x-ray microscopy was developed early but was then overshadowed by
investigations.
105/cm2) but owing to its high selectivity for different types of defects and
possible to magnify the image directly, owing to the lack of x-ray lenses.
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typical exposure times ranging from 10 min. to 2 hours with a 1kW x-ray
source. More recently, digital image storage and accumulation have become
longer wavelength which is typical for the substance. This effect is called
biology after suitable staining with fluorescent substances. Very few phases
in this way.
For chemical analysis, x-ray fluorescence has been widely used in the last
five decades and has become a standard technique in materials science and
the x-ray spectra excited by a high-intensity x-ray beam which has a wide
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atomic numbers (9- 92). Concentrations from some ppm to 100% can be
Electrons excited by photons are used for high-resolution imaging and for
Owing to the very small depth of information (10nm), the excellent phase
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oxidation products but also the electronic state of the metal atoms in the
beam used for surface microscopy can also create electron-hole pairs.
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abound. These phenomena are exploited in (i) x-ray mapping, (ii) Energy –
accelerating facilities were available; now this method has spread since
small accelerators are not much more expensive than other instruments
elements with atomic numbers higher than 14 can be achieved with very
high sensitivity. The main fields of application have been in air pollution
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backscattered electrons are most successfully used for surface imaging in the
signal intensity of the Auger electrons in the same way as in x-ray mapping.
analysis of thin layers, segregation in grain boundaries and oxide layers and
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Ions can leave the surface owing to excitation by photons, electrons, or ions,
ion mass spectroscopy (SSIMS and DSIMS), rate among the most powerful
surfaces with a sensitivity of better than 1ppm or 10-15g. SIMS and IMMA
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CHAPTER SIX
6.0 CONCLUSION
state physicist, and geophysical scientists all owe a lot of thanks to Henry
Sorby for opening up a new world to the microscopist. In the second half of
now more than just a research tool; it is used for quality control of
articles.5, 15
microscopist: nearly every object has a microstructure and this is what the
microscopist is looking for. The condition of this structure tells us all: why
the bolt failed, why the bridge collapsed, why the paint peeled off, etc.
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are required not just to observe the material grain structure but also the
demand upon the materials technologist to make the maximum use of all
types of analysis that would formerly have required the effort for a PhD
thesis.
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REFERENCES
Ohio.
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133 – 136
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pp. 1-7
India. p.407.
pp. 33 – 67.
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