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Transmission Electron Microscopy A Textbook for Materials Science Transmission Electron Microscopy A Textbook for Materials Science David B. Williams Lehigh University Bethlehem, Pennsylvania and C. Barry Carter University of Minnesota Minneapolis, Minnesota Springer Science+Business Media, LLC Library of Congress Cataloging in Publication Data Williams, David B. (David Bemard), 1949- 1i'ansmission electron microscopy: a textbook for materials science I David B. WIiliams and C. Barry Carter. p. cm. Includes bibliographica1 references and index. ISBN 978-0-306-45324-3 ISBN 978-1-4757-2519-3 (eBook) DOI 10.1007/978-1-4757-2519-3 1. Materials-Microscopy. 2. 1i'ansmission electron microscopy. 1. Carter, C. Barry. II. Ti­ tie. TA417.23.W56 1996 96-28435 502'.8'25~c20 CIP ISBN 978-0-306-45324-3 © 1996 Springer Science+Business Media New York Originally published by Plenum Press, New York in 1996 Softcover reprint of the hardcover 1st edition 1996 109876543 AII rights reserved No part 01 this book may be reproduced, stored in a retrieval system, or transmitted in any lorm or by any means, electronic, mechanical, photocopying, microlilming, recording, or otherwise, without written permission Irom the Publisher To our parents, Walter Dennis and Mary Isabel Carter, and Joseph and Catherine Williams, who made everything possible Foreword Electron microscopy has revolutionized our understanding the extraordinary intellectual demands required of the mi­ of materials by completing the processing-structure-prop­ croscopist in order to do the job properly: crystallography, erties links down to atomistic levels. It now is even possible diffraction, image contrast, inelastic scattering events, and to tailor the microstructure (and meso structure ) of materials spectroscopy. Remember, these used to be fields in them­ to achieve specific sets of properties; the extraordinary abili­ selves. Today, one has to understand the fundamentals ties of modem transmission electron microscopy-TEM­ of all of these areas before one can hope to tackle signifi­ instruments to provide almost all of the structural, phase, cant problems in materials science. TEM is a technique of and crystallographic data allow us to accomplish this feat. characterizing materials down to the atomic limits. It must Therefore, it is obvious that any curriculum in modem mate­ be used with care and attention, in many cases involving rials education must include suitable courses in electron mi­ teams of experts from different venues. The fundamentals croscopy. It is also essential that suitable texts be available are, of course, based in physics, so aspiring materials sci­ for the preparation of the students and researchers who must entists would be well advised to have prior exposure to, for carry out electron microscopy properly and quantitatively. example, solid-state physics, crystallography, and crystal The 40 chapters of this new text by Barry Carter defects, as well as a basic understanding of materials sci­ and David Williams (like many of us, well schooled in mi­ ence, for without the latter how can a person see where croscopy at Cambridge and Oxford) do just that. If you TEM can (or may) be put to best use? want to learn about electron microscopy from specimen So much for the philosophy. This fine new book preparation (the ultimate limitation); or via the instrument; definitely fills a gap. It provides a sound basis for research or how to use TEM correctly to perform imaging, diffrac­ workers and graduate students interested in exploring tion, and spectroscopy-it's all there! This is, to my those aspects of structure, especially defects, that control knowledge, the only complete text now available that in­ properties. Even undergraduates are now expected (and cludes all the remarkable advances made in the field of rightly) to know the basis for electron microscopy, and this TEM in the past 30 to 40 years. The timing for this book is book, or appropriate parts of it, can also be utilized for un­ just right and, personally, it is exciting to have been part of dergraduate curricula in science and engineering. the developments it covers-developments that have im­ The authors can be proud of an enormous task, very pacted so heavily on materials science. well done. In case there are people out there who still think TEM is just taking pretty pictures to fill up one's bibliogra­ G. Thomas phy, please stop, pause, take a look at this book, and digest Berkeley; California vii Preface How is this book any different from the many other books than annular dark-field imaging-or even secondary-elec­ that deal with TEM? It has several unique features, but the tron or STEM Z-contrast modes. Similarly, convergent­ most distinguishing one, we believe, is that it can really be beam and scanning-beam diffraction are integral parts of described as a "textbook"-that is, one designed to be used electron diffraction, and are complementary to selected­ primarily in the classroom rather than in the research labo­ area diffraction. Inelastic electron scattering is the source ratory. We have constructed the book as a series of rela­ of both Kikuchi lines and characteristic X-rays. So we tively small chapters (with a few notable exceptions!). The don't deliberately split off "conventional" microscopy contents of many chapters can be covered in a typical lec­ from "analytical" microscopy. ture of 50 to 75 minutes. The style is informal for easier Our approach is to thread two fundamental ques­ reading; it resembles an oral lecture rather than the formal tions throughout the text. writing you would encounter when reading research papers. Why should we use a particular technique? In our experience, the TEM books currently avail­ How do we put the idea into practice? able fall into three major categories. They may be too theo­ We attempt to establish a sound theoretical basis where retical for many materials science students; they attempt to necessary, although not always giving all the details. We cover all kinds of electron microscopy in one volume, then use this knowledge to build a solid understanding of which makes it difficult to include sufficient theory on any how we use the instrument. The text is illustrated with ex­ one technique; or they are limited in the TEM topics they amples from across the fields of materials science and en­ cover. The rapid development of the TEM field has meant gineering and, where possible, a sense of the history of the that many of the earlier books must automatically be placed technique is introduced. We keep references to a minimum in the third category. Although these books are often invalu­ and generally accepted concepts are not specifically cred­ able in teaching, we have not found them generally suitable ited, although numerous classical general references are as the course textbook in a senior-year undergraduate or included. first-year graduate course introducing TEM, so we have en­ We both have extensive teaching and research back­ deavored to fill this perceived gap. grounds in all aspects of TEM comprising diffraction, Since this text is an introduction to the whole sub­ imaging, and microanalysis. Our research in TEM of mate­ ject of TEM, we incorporate all aspects of a modem TEM rials spans metals, ceramics, composites, and semiconduc­ into an integrated whole. So, rather than separating out the tors. We each bring more than 25 years of TEM experience broad-beam and convergent-beam aspects of the subject to the book, and have contributed to the training of a gener­ (the traditional structural analysis or imaging versus the ation of (we hope) skilled electron microscopists. We found "chemical" analysis or "new" techniques), we treat these that writing the book broadened our own knowledge con­ two aspects as different sides of the same coin. Thus scan­ siderably and was actually fun on some occasions. We hope ning-beam (STEM) imaging is just another way to form an you experience the same reactions after reading it. image in a TEM. There is no reason to regard "conven­ Lastly, we encourage you to send us any comments tional" bright-field and "conventional" dark-field imaging (positive or negative). We can both be reached by email: as any more fundamental ways of imaging the specimen dbwl @lehigh.edu and [email protected] ix Acknowledgments We have spent the best part of a decade in the conception this support none of the research that underpins the con­ and gestation of this text and such an endeavor can't be ac­ tents of this book would have been accomplished. In par­ complished in isolation. Our first acknowledgments must ticular, DBW wishes to acknowledge the National Science be to our wives, Margie and Bryony, and our families, who Foundation (Division of Materials Research) for almost have borne the brunt of our absences from home (and occa­ 20 years of continuous funding, the National Aeronautics sionally the brunt of our presence, also!). and Space Administration, the Department of Energy (Ba­ We have both been fortunate to work with other mi­ sic Energy Sciences), Sandia National Laboratories, and croscopists, post-doctoral associates, and graduate students the Materials Research Center at Lehigh, which supports who have taught us much and contributed significantly to the microscopy laboratory. Portions of the text were writ­ the examples in the text. We would like to thank a few of ten while DBW was on sabbatical or during extended visits these colleagues directly: Dave Ackland, Ian Anderson, to Chalmers University, Goteborg, with Gordon Dunlop Charlie Betz, John Bruley, Dov Cohen, Ray Coles, Vinayak and Hans Norden; the Max Planck Institut fUr Metall­ Dravid, Joe Goldstein, Brian Hebert, Jason Heffelfinger, forschung, Stuttgart, with Manfred Ruhle; and Los Alamos John Hunt, Matt Johnson, Vicki Keast, Ron Liu, Charlie National Laboratory, with Terry Mitchell.

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