Quantitative X-Ray Diffractometry PDF
Preview Quantitative X-Ray Diffractometry
Quantitative X-Ray Diffractometry Springer New York Berlin Heidelberg Barcelona Budapest Hong Kong London Milan Paris Santa Clara Singapore Tokyo Lev S. Zevin Giora Kimmel Quantitative X-Ray Diffractometry Edited by Inez Mureinik With 70 Illustrations , Springer Lev S. Zevin (deceased) Giora Kimmel The Institutes for Applied Research and Department of Materials Engineering Department of Materials Engineering Ben-Gurion University of the Negev Ben-Gurion University of the Negev Beer-Sheva 84105, Israel Beer-Sheva 84105, Israel Edited by Inez Mureinik The Institutes for Applied Research Ben-Gurion University of the Negev Beer-Sheva 84105, Israel Library of Congress Cataloging-in-Publication Data Zevin, Lev S. Quantitative X-ray diffractometry / Lev S. Zevin, Giora Kimmel; edited by Inez Mureinik. p. cm. Includes bibliographical references and index. ISBN-13:978-1-4613-9537-9 e-ISBN-13:978-1-4613-9535-5 DOl: 10.1007/978-1-4613-9535-5 1. X-rays-Diffraction. 2. X-rays-Diffraction-Industrial applications. -I. Kimmel, Giora. II. Mureinik, Inez. III. Title. QC482.D5Z48 1995 545'.81-dc20 95-19428 Printed on acid-free paper. © 1995 Springer-Verlag New York, Inc. Softcover reprint of the hardcover 1st edition 1995 All rights reserved. This work may not be translated or copied in whole or in part without the written permission of the publisher (Springer-Verlag New York, Inc., 175 Fifth Avenue, New York, NY 10010, USA), except for brief excerpts in connection with reviews or scholarly analysis. Use in connection with any form of information storage and retrieval, electronic adaptation, computer software, or by similar or dissimilar methodology now known or hereaf ter developed is forbidden. The use of general descriptive names, trade names, trademarks, etc., in this publication, even if the former are not especially identified, is not to be taken as a sign that such names, as understood by the Trade Marks and Merchandise Marks Act, may accordingly be used freely by anyone. Production managed by Hal Henglein; manufacturing supervised by Jeffrey Taub. Camera-ready copy prepared from the editor's Microsoft Word files. 987654321 ISBN-13 :978-1-4613-9537-9 Preface The first book dealing with quantitative analysis in powder mixtures (if only in one chapter) was that of Klug and Alexander, X-ray Diffraction Procedures, which was published in 1954. The only work dedicated entirely to quantitative X-ray powder diffraction (QXRD) that has appeared since that time is the 200-page monograph of Davis, Reference Intensity Method of QXRD Analysis. However, this publica tion, which appeared in 1988, was devoted only to a single aspect of QXRD, as reflected in its title. On the other hand, most books on the characterization of materials by X-ray powder diffraction do include a section or a chapter on QXRD. In contrast to structure determination, in which single crystal methods are favored, quantitative analysis of phases is specific to the powder method, and the lack of a special book dealing with QXRD analysis is inexplicable. The aim of the present book is to fill this void. Since the terminology pertaining to QXRD is not always standard ized in the literature, the reader should pay special attention to descriptions of the particular methodology and to the formulation of each method in order to compare similar procedures described under different names by other workers. The book is divided into six chapters. The first chapter is introduc tory, giving the history of X-ray powder diffraction and comparing QXRD to other analytical methods. The second chapter deals with the physical background of X-ray powder diffraction in general and with its application to QXRD, with special emphasis on the attenuation of X-rays and microabsorption. The third chapter is devoted to instrumen tation, with particular reference to the Bragg-Brentano diffractometer. Other powder facilities are also reviewed in detail. The methodology of QXRD is given in the fourth chapter, which constitutes the core of the book. A variety of problems and solutions in the field of quantitative phase analysis are given. The chapter starts with the general case, in which all absorption coefficients are known, and then continues with the internal standard method (including the addition methods of doping and dilution); full-phase analysis (external standard); the reference intensity ratio method; the full diffraction pattern approach; standardl ess methods; combination of v vi Preface X-ray diffraction with chemical analysis; crystallinity of polymers; and analysis of low-mass samples. The fifth chapter is devoted to practical aspects of QXRD: optimal data collection; hints for sample preparation; intensity measurement; absorption; analytical standards; pattern treatment and simulation; correction of preferred orientation; and errors and limitations. The section on preferred orientation was kindly edited by Prof. Matti Jarvinen. The final ~hapter addresses some applications, most of them industrial. The unique quality of this book lies in the fact that it brings together between one set of covers all the aspects of the multifaceted discipline of QXRD, and we thus trust that it will make a major contribution to promoting QXRD in a wide spectrum of applications. Giora Kimmel Editor's preface It might seem strange to dedicate a book to the author himself, but this book is dedicated to the memory of Lev Zevin, who sadly did not live to see its completion. Zevin, as he was known affectionately to those of us who worked with him at Ben-Gurion University of the Negev, was an outstanding diffractionist-the range of his knowledge and experience is reflected in the scope and depth of this work. Indeed, the concept of the book-of bringing together all the facets of quantitative X-ray analysis, both theoretical and applied-evolved during many years of teaching, research and analytical work, first in the former USSR and later in Israel. I sincerely hope that what stands on these pages will be a fitting tribute to a scientist of his caliber. Inez Mureinik vii Acknowledgments Prof. Lev Zevin dedicated his life to scientific research. He was a hard-working, active, and creative personality who never hesitated to share his knowledge and inexhaustible sources of original ideas with all who came into contact with him-researchers in different fields, colleagues, and especially the students who were so important to him. We hope that this book will contribute to progress in the field of quantitative X-ray diffractometry. The methods of QXRD analysis outlined in this book will be of use to researchers and scientists at universities and industrial laboratories who are investigating compounds with special technological properties; to chemists and physicists working on the synthesis and properties of new materials; to geologists studying natural deposits; and to specialists dealing with ore beneficiation. These methods also have important applications in the routine technological processes of the cement industry. If this book will serve as an everyday working manual for all these fields, it will be the best way to preserve the memory of Prof. Zevin. Prof. Zevin started working on this book a few years before his death. At the time he passed away, the book was almost completely written, except for the last few sections of Chapter 6. The final editing and completion of the book were accomplished after his death. Before he died, Prof. Zevin asked his colleague and friend, Prof. Giora Kimmel, to see the book through to completion. We thank him for his part. The publication of the book was made possible due to the efforts of the highly qualified and professional editor, Ms. Inez Mureinik. We would like to express our deepest gratitude to her. Special thanks are due to Prof. M. Jarvinen of Lappeenranta University of Technology, Finland, who read and edited the sections on crystallite orientation. We would also like to thank Ms. Shula Rabinovitz for her highly professional illustrations; Ms. Marion Milner for typing the manuscript; and Ms. Dorot Imber for her understanding and encouragement. Finally, we would like to thank Dr. Thomas von Foerster, Springer Verlag's Senior Editor for Physics and Mathematics, for his sympathetic attitude and patience, and the Production staff at ix x Acknowledgments Springer-Verlag, for their investment of time and effort in the production aspects of the book. If we-his wife and children-have inadvertently omitted any of Prof. Zevin's colleagues who were involved in the writing of this book, we apologize and thank them. Isabella, Shaul, and Miriam Zevin Contents Preface. ........................................................................................... v EdI' tor' s pre ace .......f..................................."............................... VII Acknowledgments ..................................................................... ix 1 Introduction .............................................................................. 1 1.1 Phase analysis-when and why ............................................. 1 1.2 Phase analysis as an analytical method ................................. 2 1.2.1 Direct methods of phase analysis ............................... 2 1.2.2 Indirect methods of phase analysis ............................. 3 1.2.3 General approach to phase quantification ................. .4 1.3 History of quantitative X-ray phase analysis ......................... 5 1.3.1 Quantification techniques .......................................... 5 1.3.2 Instrumentation .......................................................... 8 2 Physical basis .......................................................................... 10 2.1 Interaction of X-rays with materiaL .................................... 10 2.1.1 Scattering of X-rays ................................................. 11 2.1.2 Absorption of X-rays ................................................ 15 2.1.3 Various forms of absorption coefficients .................... 16 2.2 Intensity in powder diffraction ............................................. 18 2.2.1 General expression derived from the kinematic theory of diffraction ................................................ 19 2.2.2 Polarization factor in X-ray diffractometry .............. 21 2.2.3 Extinction of X-rays .................................................. 22 2.3 Background-angle variation and intensity .......................... 24 2.3.1 Introduction ............................................................. 24 2.3.2 Scattering of continuous radiation ............................. 25 2.3.3 Scattering of characteristic radiation ....................... 26 2.4 X-ray diffraction by nonhomogeneous polycrystalline materials ............................................................................. 29 2.4.1 Introduction ............................................................. 29 xi
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