Scanning Electron Microscopy, X-Ray Microanalysis, and Analytical Electron Microscopy: A Laboratory Workbook

414 Pages·1990·28.09 MB·English

by  Charles E. Lyman

Scanning Electron Microscopy,
X-Ray Microanalysis, and
Analytical Electron Microscopy
A Laboratory Workbook
Scanning Electron Microscopy,
X-Ray Microanalysis, and
Analytical Electron Microscopy
A Laboratory Workbook
Charles E. Lyman Dale E. Newbury
Lehigh University National Institute oj Standards and Technology
Bethlehem, Pennsylvania Gaithersburg, Maryland
Joseph I. Goldstein David B. Williams
Lehigh University Lehigh University
Bethlehem, Pennsylvania Bethlehem, Pennsylvania
Aiton D. Romig, Jr. John T. Armstrong
Sandia National Laboratories California Institute oj Technology
Albuquerque, New Mexico Pasadena, California
Patrick Echlin Charles E. Fiori
University oj Cambridge National Institute oj Standards and Technology
Cambridge, England Gaithersburg, Maryland
David C. Joy Eric Lifshin
University oj Tennessee GE.Corporate Research and Development
Knoxville, Tennessee Schenectady, New York
Klaus-Ruediger Peters
The University oj Connecticut Health Center
Farmington, Connecticut
Plenum Press • New York and London
Library of Congress Cataloglng-In-Publlcatlon Data
Scanning electron microscopy. X-ray microanalysis. and analytical
electron microscopy: a laboratory workbook / Charles E. Lyman .,.
[et a1.1.
p. CIII.
Includes bibliographical references.
ISBN-13: 978-0-306-43591-1 e-ISBN-13: 978-1-4613-0635-1
DOl: 10.1007/978-1-4613-0635-1
I. Scanning electron IIIlcroscopes--Laboratory manuals. 2. X-ray
mlcroanalysls--Laboratory manuals. 3. Electron mlcroscopy
-Laboratory manuals. I. Lyman. Charles E.
QH212.S3S33 1990
502'.S'25--dc20 90-3380S
CIP
10987654
© 1990 Plenum Press, New York
Softcover reprint of the hardcover 1s t edition 1990
A Division of Plenum Publishing Corporation
233 Spring Street, New York, N.Y. 10013
All rights reserved
No part of this book may be reproduced, stored in a retrieval system, or transmitted
in any form or by any means, electronic, mechanical, photocopying, microfiiIning,
recording, or otherwise, without written permission from the Publisher
Foreword
During the last four decades remarkable developments have taken place in instrumentation and
techniques for characterizing the microstructure and microcomposition of materials. Some of
the most important of these instruments involve the use of electron beams because of the wealth
of information that can be obtained from the interaction of electron beams with matter. The
principal instruments include the scanning electron microscope, electron probe x-ray
microanalyzer, and the analytical transmission electron microscope. The training of students to
use these instruments and to apply the new techniques that are possible with them is an
important function, which.has been carried out by formal classes in universities and colleges
and by special summer courses such as the ones offered for the past 19 years at Lehigh
University.
Laboratory work, which should be an integral part of such courses, is often hindered by
the lack of a suitable laboratory workbook. While laboratory workbooks for transmission
electron microscopy have-been in existence for many years, the broad range of topics that must
be dealt with in scanning electron microscopy and microanalysis has made it difficult for
instructors to devise meaningful experiments. The present workbook provides a series of
fundamental experiments to aid in "hands-on" learning of the use of the instrumentation and the
techniques. It is written by a group of eminently qualified scientists and educators.
The importance of hands-on learning cannot be overemphasized. It is only by experience
that one acquires familiarity and only by familiarity that one acquires the confidence to attack
problems using the manifold techniques now available to the researcher. This workbook
provides the only comprehensive series of experiments devoted to a wide range of imaging and
analytical experiments. I was particularly pleased to see a number of experiments devoted to
some of the important but less frequently used techniques, such as channeling contrast,
magnetic contrast, low-voltage SEM, and stereo microscopy. I was also pleased to see
experiments on wavelength-dispersive spectrometry. Although the majority of students may
not have an opportunity to use this technique in their later work, they should be familiar with it
now in order to evaluate, in proper perspective, the work that they may do with energy
dispersive spectrometry.
I expect this workbook to be highly successful and widely adopted. But I would like to
add one caution to the reader: do not be misled into thinking that, because you have done an
experiment on a technique, you fully understand it In fact, many of the experiments in this
book could have been expanded into several more experiments. I hope that this workbook is
only the beginning and that it will be followed by additional experiments in the not too distant
future.
David B. Wittry
Professor of Materials Science and Electrical Engineering
University of Southern California
Los Angeles, CA 90089-0241
v
Preface to the Student
These laboratory exercises were developed over several years at the short courses on scanning
electron microscopy, x-ray microanalysis, and analytical electron microscopy held annually at
Lehigh University. Laboratories 1-7 cover basic techniques that should be mastered before
attempting the more advanced SEM and x-ray microanalysis techniques of Laboratories 8-23.
Laboratories 24-27 cover techniques used in analytical electron microscopy in the transmission
electron microscope. The specimens required for Laboratories 1-27 can be prepared using step
by-step guidelines given in Laboratories 28-30. Often the recommended specimens may be
substituted with others that are more relevant to the work at individual companies or
institutions.
This laboratory workbook is a companion volume to three textbooks on electron
microscopy published by Plenum:
Scanning Electron Microscopy and X-Ray Microanalysis by 1. I. Goldstein, D. E. Newbury,
P. Echlin, D. C. Joy, C. E. Fiori, and E. Lifshin, Plenum Press, New York, 1981 (designated
SEMXM throughout this workbook),
Advanced Scanning Electron Microscopy and X-Ray Microanalysis by D. E. Newbury, D. C.
Joy, P. Echlin, C. E. Fiori, and J. I. Goldstein, Plenum Press, New York, 1986 (ASEMXM),
Principles ofA nalytical Electron Microscopy, edited by D. C. Joy, D. Romig, Jr., and 1. I.
Goldstein, Plenum Press, New York, 1986 (PAEM).
Each laboratory exercise illustrates one or more of the principles and techniques
discuss sed in these textbooks. For state-of-the-art techniques such as environmental SEM,
additional explanatory material has been given within the narrative of the laboratory. To obtain
the most benefit from these laboratories, the student is encouraged to read the recommended
sections of the appropriate textbook and the narrative of the laboratory before sitting down to
the instrument There is an important learning experience to be derived from performing all
parts of these labs on an instrument in your own laboratory rather than simply examining the
worked examples in the solutions section. It should be possible to complete each laboratory in
less than half a workday after suitable preparation of the specimens and alignment of the
instrument.
The publication of this book would not have been possible without the instrumentation
and technical assistance provided by the following manufacturers of electron microscopes and
x-ray detection equipment: Amray, Cambridge Instruments, CamS can USA, EDAX
International, ElectroScan, Gatan, NSA Hitachi Scientific Instruments, International Scientific
Instruments, mOL (USA), Kevex Corp., Link Analytical, Microspec, Philips Electronic
Instruments, Princeton Gamma-Tech, Tracor Northern, VG Microscopes, and Carl Zeiss.
The authors wish to thank the many students and colleagues who have contributed to
these laboratories including V. P. Dravid, D. R. Liu, S. M. Merchant, 1. R. Michael,
C. Robino, H. E. G. Rominal, C. Russo, J. Sutliff, K. S. Vecchio, and M. Zemyan. We also
appreciate the efforts of our reviewers for various sections of the book: R. M. Anderson,
E. L. Hall, and D. B. Wittry. Thanks also go to our technical staff, D. W. Ackland, D. C.
vii
Calvert, J. Kerner, and K. Repa, who prepared most of the specimens used in these labs.
Finally, special thanks go to our short course coordinator, Sharon Coe, for her devotion to the
production of this workbook.
C. E. Lyman
Bethlehem, Pennsylvania
vIII Preface to the Student
Contents
Part I
SCANNING ELECTRON MICROSCOPY
AND X-RAY MICROANALYSIS
Laboratory 1 Basic SEM Imaging ......................... 3
Laboratory 2 Electron Beam Parameters ..................... 8
Laboratory 3 Image Contrast and Quality . . . . . . . . . . . . . . . . . . . .. 16
Laboratory 4 Stereo Microscopy .......................... 22
Laboratory 5 Energy-Dispersive X-Ray Spectrometry . . . . . . . . . . . . .. 27
Laboratory 6 Energy-Dispersive X-Ray Microanalysis ............. 33
Laboratory 7 Wavelength-Dispersive X-Ray Spectrometry
and Microanalysis ........................ 42
Part II
ADVANCED SCANNING ELECTRON MICROSCOPY
Laboratory 8 Backscattered Electron Imaging .................. 51
Laboratory 9 Scanning Transmission Imaging in the SEM ........... 55
Laboratory 10 Low-Voltage SEM ."......................... 57
Laboratory 11 High-Resolution SEM Imaging .................. 61
Laboratory 12 SE Signal Components ....................... 67
Laboratory 13 Electron Channeling Contrast ................... 73
Laboratory 14 Magnetic Contrast .......................... 78.
Laboratory 15 Voltage Contrast and EBIC ..................... 81
Laboratory 16 Environmental SEM ......................... 86
Laboratory 17 Computer-Aided Imaging ...................... 90
ix
Part III
ADVANCED X-RAY MICROANALYSIS
Laboratory 18 Quantitative Wavelength-Dispersive X-Ray Microanalysis 99
Laboratory 19 Quantitative Energy-Dispersive X-Ray Microanalysis ...... 108
Laboratory 20 Light Element Microanalysis 117
Laboratory 21 Trace Element Microanalysis .................. - 122
Laboratory 22 Particle and Rough Surface Microanalysis ............ 127
Laboratory 23 X-Ray Images . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 132
Part IV
ANALYTICAL ELECTRON MICROSCOPY
Laboratory 24 Scanning Transmission Imaging in the AEM ........... 139
Laboratory 25 X-Ray Microanalysis in the AEM ................. 143
Laboratory 26 Electron Energy Loss Spectrometry .. . . . . . . . . . . . . . . 148
Laboratory 27 Convergent Beam Electron Diffraction .............. 153
Part V
GUIDE TO SPECIMEN PREPARATION
Laboratory 28 Bulk Specimens for SEM and X-Ray Microanalysis ....... 159
Laboratory 29 Thin Specimens for TEM and AEM . . . . . . . . . . . . . . . . 172
Laboratory 30 Coating Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . 180
SOLUTIONS TO LABORATORY EXERCISES
Laboratory 2 Electron Beam Parameters ..................... 189
Laboratory 3 Image Contrast and Quality . . . . . . . . . . . . . . . . . . . . . 197
Laboratory 4 Stereo Microscopy .......................... 204
Laboratory 5 Energy-Dispersive X-Ray Spectrometry .............. 207
Laboratory 6 Energy-Dispersive X-Ray Microanalysis ............. 213
Laboratory 7 Wavelength-Dispersive X-Ray Spectrometry
and Microanalysis ........................ 219
x Contents
Laboratory 8 Backscattered Electron Imaging ..•............... 227
Laboratory 9 Scanning Transmission Imaging in the SEM ........... 232
Laboratory 10 Low-Voltage SEM ......................... 234
Laboratory 11 High-Resolution SEM Imaging .................. 242
Laboratory 12 SE Signal Components ....................... 251
Laboratory 13 Electron Channeling Contrast ................... 263
Laboratory 14 Magnetic Contrast ......................... 275
Laboratory 15 Voltage Contrast and EBIC .................... 279
Laboratory 16 Environmental SEM ........................ 287
Laboratory 17 Computer-Aided Imaging ..................... 296
Laboratory 18 Quantitative Wavelength-Dispersive X-Ray Microanalysis . .. 309
Laboratory 19 Quantitative Energy-Dispersive X-Ray Microanalysis 316
Laboratory 20 Ught Element Microanalysis ................ 330
Laboratory 21 Trace Element Microanalysis ................... 335
Laboratory 22 Particle and Rough Surface Microanalysis ............ 343
Laboratory 23 X-Ray Images . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 352
Laboratory 24 Scanning Transmission Imaging in the AEM ........... 365
Laboratory 25 X-Ray Microanalysis in the AEM ................. 373
Laboratory 26 Electron Energy Loss Spectrometry .. . . . . . . . . . . . . .. 381
Laboratory 27 Convergent Beam Electron Diffraction .. . . . . . . . . . . .. 389
Index ........................................... 401
Contents xi
Part I
SCANNING ELECTRON MICROSCOPY
AND X-RAY MICROANALYSIS