Professional Documents
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Transmission Electron
Microscopy
A Practical Guide to
Transmission Electron
Microscopy
Fundamentals
Zhiping Luo
A Practical Guide to Transmission Electron Microscopy: Fundamentals
Copyright © Momentum Press®, LLC, 2016
DOI: 10.5643/9781606507049
10 9 8 7 6 5 4 3 2 1
Keywords
Analytical Electron Microscopy; Ceramics; Chemical Analysis; Chemis-
try; Composites; Crystallography; Electron Diffraction; Electron Energy-
Loss Spectroscopy (EELS); Forensic Science; Geosciences; Imaging;
Industry; Life Sciences; Materials Science and Engineering; Metals and
viii KEYWORDS
Appendices
Appendix I. SAED Indexing Table of Primitive Cubic Structure ...139
Appendix II. SAED Indexing Table of Body-Centered Cubic
Structure ..................................................................141
Appendix III. SAED Indexing Table of Face-Centered Cubic
Structure ..................................................................143
Appendix IV. SAED Indexing Table of Close-Packed Hexagonal
Structure ..................................................................145
Illustration Credits .............................................................................147
Index ...............................................................................................149
Preface
To study material structure, we need to use microscopes. With the
naked eyes, we can barely see objects beyond 0.1 mm, while by using a
light microscope composed of optical lenses, the resolution is improved
beyond 1 μm to several hundred nanometers. However, to further im-
prove the resolution, electron microscopy should be applied. Scanning
electron microscopy (SEM) extends the resolution to several nanome-
ters, and it can also provide elemental analyses, but it is hard to see
objects below the several nanometer range. The transmission electron
microscopy (TEM) has great advantages over other microscopy tech-
niques, in that its ultrahigh imaging resolution can routinely reach sev-
eral angstroms on a modern microscope, and it also has ability to study
the structure using electron diffraction, and auxiliary capabilities to
identify chemical compositions. Nowadays, TEM is a standard charac-
terization approach in scientific research, academic education, industrial
development, and governmental forensic investigations.
For over a decade at Texas A&M University, I held a TEM instru-
mental scientist position, where I taught TEM courses and trained many
TEM users. During the user training, I realized that step-by-step in-
structions were always very helpful so that the user could work in the
right way immediately, instead of learning from many trials. The users
should learn the instructions first and then practice on the instrument to
improve the working efficiency, rather than practice with minimum
instructions.
This book provides a practical guide to the TEM user as a quick ref-
erence on how to utilize the various TEM techniques more efficiently to
get meaningful results. It starts at the beginner level and introduces the
TEM skills concisely, including practical instructions on how to operate
the instrument correctly, how to avoid possible problems, how to under-
stand the results, and how to interpret and compute the data. It is sepa-
rated into two volumes with different levels. Volume 1 is on Fundamen-
tals of TEM, including TEM sample preparation, instrumentation and
operation procedures, electron diffraction I (selected-area electron dif-
fraction), and imaging I (mass-thickness imaging and diffraction contrast
xiv PREFACE
Zhiping Luo
Fayetteville, North Carolina
June 2015
Acknowledgments
First of all, I acknowledge my many collaborators who provided me
with wonderful samples for the TEM investigations and made fruitful
discussions on what we learned from the TEM. It is really hard to list all
of their names on this page, while the following major contributors are
apparently among them, alphabetically, Drs. M. Akbulut, S. Bashir,
J. Batteas, L. Carson, C.C. Chen, W. Chen, D. Fang, J. Fang, B. Guo,
Z. Guo, K.T. Hartwig, A. Holzenburg, X. Hong, X. Jiang, H.E. Karaca,
I. Karaman, B. Kockar, J.H. Koo, A. Kronenberg, S. Kundu, D. Lagou-
das, G. Liang, Y. Li, J. Liu, J. Ma, A.-J. Miao, D.J. Miller, J.F. Mitchell,
O. Ochoa, A. Oki, V. Paredes-García, Z. Quan, P.H. Santschi,
R.E. Schaak, L. Shao, D.H. Son, C. Song, Y. Song, L. Sun, X.S. Sun,
Y. Tang, Y. Vasquez, H. Wang, W. Wu, J. Zhang, S. Zhang, X. Zhang,
Q. Zhai, D. Zhao, H. Zheng, H.-C. Zhou, D. Zhu, J. Zhu, and
M. Zhu.
I also thank my previous colleagues (Dr. A. Holzenburg, Mr. R. Lit-
tleton, Ms. A. Ellis, Dr. C. Savva, Dr. J. Sun, Dr. S. Vitha, Dr. H. Kim,
etc.) at the Microscopy and Imaging Center, Texas A&M University for
technical assistance and stimulating discussions on biological samples;
Dr. D.J. Miller at the Electron Microscopy Center, Argonne National
Laboratory, for advanced TEM skills; and Profs. H. Hashimoto and
E. Sukedai at Okayama University of Science, Japan, for HREM.
Grateful appreciations should also be given to those professors who
introduced me to the field of electron microscopy in my early career in
China, alphabetically, Drs. K.H. Kuo, F.H. Li, and S. Zhang.
Finally, I am grateful to the book Collection Editor Dr. C. Richard
Brundle for technical assistance to edit this book, and to those publish-
ers for their permissions to reuse the materials presented in this book as
specifically referenced.
About the Book
This book is a concise practical guide for the TEM users to
improve TEM skills in a short period of time.
It is also a textbook for a short course (semester-long TEM
undergraduate or graduate course, or intensive short-term
workshop).
It provides step-by-step instructions how to operate the
instrument, how to analyze, and how to compute the data.
It covers areas primarily for physical sciences (chemistry,
engineering, geosciences, materials science, and physics) and some
examples in life sciences (agriculture, biology, and medicine).
It applies to scientific research, academic education, industrial
developments, governmental forensic investigations, and
others.
Personnel Experiences
with TEM
1. Be aware of what you are doing with the microscope!
- Read sufficient literature to make clear what is new and
what has been done previously.
2. See both, the forest and the trees!
- Information in both high and low magnifications should be
known.
3. Good results are obtained out of the microscope room!
- Post-experiment analyses (data processing, computation,
and quantification) and documentation are very important.
4. A good habit is beneficial to your whole career!
- Organize your samples and data well.
CHAPTER 1
Introduction
To reveal small objects that are beyond the visual capacity of human eyes,
various microscopy techniques have been developed. Without the help of
any instrument, the resolution of naked eyes is only about 0.1 mm, or
100 μm. The early developed light microscope (LM) is used to magnify
objects by optical lenses using visible lights. The resolution of LM can be
improved to below 1 μm at several hundred nanometers. After the LM
technique, it was discovered that electrons could be used as the illumina-
tion source to improve the imaging resolution, and therefore various elec-
tron microscopy (EM) techniques have been developed to study different
types of samples. Among them, bulk samples can be analyzed by scanning
electron microscope (SEM), electron probe microanalyzer (EPMA) or
electron microprobe analyzer (EMPA), or scanning Auger microscope
(SAM) or scanning Auger microprobe (SAM). In these techniques, vari-
ous detected signals come from the electron–specimen interactions. If the
sample is thin enough, the electrons can penetrate right through the sam-
ples to form images using electromagnetic lenses. The instrument imaging
samples using transmitted electrons is named as transmission electron
microscope (TEM), and this technique is named as transmission electron
microscopy (TEM). Nowadays the terminology TEM can mean either the
microscope or the technique.
TEM is a very powerful tool to study the sample structures [1–6]. It
can provide not only a high imaging resolution down to angstroms or
even subangstrom level but also structural information through electron
diffraction, and chemical composition information through the interac-
tions of high-energy electrons with core electrons of the specimen. TEM
has been widely applied in multidisciplines, including physical sciences
(chemistry, engineering, geosciences, materials science, and physics) and
life sciences (agriculture, biology, and medicine), and for technical
development, product inspection, and forensic investigations.
2 A PRACTICAL GUIDE TO TRANSMISSION ELECTRON MICROSCOPY
Fig. 1.1 Image formation by a lens (a) and formation of Airy disks
from a single image spot by diffraction effect (b). Separation of two
image spots is shown in (c–g) with a series of different distances. The
microscope resolution is defined in (f) for Rayleigh criterion that the
minimum intensity of one spot coincides with maximum intensity of
another spot.
A better resolution means a shorter distance δ for identifying two
image points. From Eq. 1.1, it is possible to improve the resolution (or
decreasing δ ) through the following methods:
Fig. 1.4 Comparison of SEM and TEM images: SEM (a) and TEM
(b) image of carbon nanofibers in polymer, and SEM (c, d) images
and TEM image (e) of clay in polymer.
References
[1] P.B. Hirsch, A. Howie, R.B. Nicholson, D.W. Pashley, M.J.
Whelan. Electron Microscopy of Thin Crystals. Krieger, Florida, 1977.
[2] G. Thomas, M.J. Goringe. Transmission Electron Microscopy of
Materials. John Wiley & Sons, New York, 1979.
[3] J.W. Edington. Practical Electron Microscopy in Materials Science.
Techbooks, Herndon, Virginia, 1991.
[4] L. Reimer. Transmission Electron Microscopy: Physics of Image
Formation and Microanalysis. Springer, Heidelberg, Berlin, 1997.
[5] J.J. Bozzola, L.D. Russell. Electron Microscopy: Principles and
Techniques for Biologists. Jones and Bartlett Learning, Massachu-
setts, 1999.
[6] D.B. Williams, C.B. Carter. Transmission Electron Microscopy: A
Textbook for Materials Science. Springer, New York, 2009.
[7] J.I. Goldstein, A.D. Romig, Jr., D.E. Newbury, C.E. Lyman, P.
Echlin, C. Fiori, D.C. Joy, E. Lifshin. Scanning Electron Microscopy
and X-Ray Microanalysis: A Textbook for Biologists, Materials Scien-
tists, and Geologists. 2nd Edition. Plenum Press, New York, 1992.
12 A PRACTICAL GUIDE TO TRANSMISSION ELECTRON MICROSCOPY
• Secondary Ion Mass Spectrometry: Applications for Depth Profiling and Surface
Characterization by Fred Stevie
• Auger Electron Spectroscopy: Practical Application to Materials Analysis and
Characterization of Surfaces, Interfaces, and Thin Films by John Wolstenholme
• Spectroscopic Ellipsometry: Practical Application to Thin Film Characterization
by Harland G. Tompkins and James N. Hilfiker
• A Practical Guide to Transmission Electron Microscopy, Volume 2: Advanced Microscopy
by Zhiping Luo
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