Applications of Analytical Techniques to the Characterization of Materials

Applications of Analytical Techniques to the Characterization of Materials

Applications of Analytical Techniques to the Characterization of Materials Edited by Lawrence Berkeley Laboratory University of California Berkeley, California Springer Science+Business Media, LLC

Library of Congress Catalog1ng-1n-PublIcatIon Data Applications of analytical techniques to the characterization of materials / edited by, p. cm. Proceedings of an American Chemical Society Division of Industrial and Engineering Chemistry symposium on Applications of Analytical Techniques to the Characterization of Materials, held August 29-30, 1990, in Washington, D.C." Includes bibliographical references and index. 1. Materials Analysis Congresses. I. Perry, Dale L. QD131.A66 1992 620. 1 ' 1299~dc20 92-70 CIP Proceedings of an American Chemical Society Division of Industrial and Engineering Chemistry symposium on Applications of Analytical Techniques to the Characterization of Materials, held August 29-30, 1990, in Washington, D.C. ISBN 978-1-4757-9228-7 DOI 10.1007/978-1-4757-9226-3 ISBN 978-1-4757-9226-3 (ebook) Springer Science+Business Media New York 1991 Originally published by Plenum Press, New York in 1991 Softcover reprint of the hardcover 1st edition 1991 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, microfilming, recording, or otherwise, without written permission from the Publisher

Contributors Frank J. Berry Department of Chemistry, The Open University Milton Keynes MK7 6AA, United Kingdom John G. Dillard Department of Chemistry Virginia Polytechnic Institute and State University Blacksburg, VA 24061-0212 Eric Faulques and Richard E. Russo Applied Science Division, Lawrence Berkeley Laboratory University of California, Berkeley, CA 94720, USA GaryJ. Long Department of Chemistry, University of Missouri-Rolla Rolla, MO 65401 and Fernande Grandjean Institut de Physique, B5, Universite de Liege B-4000 Sart-Tilman, Belgium Lisa C. Klein, Shu-Fang Ho, Sung-Ping Szu and Martha Greenblatt Rutgers - The State University of New Jersey Ceramics Department P.O.Box 909, Piscataway, NJ 08855-0909 Lawrence Berkeley Laboratory University of California, Berkeley, CA 94720 Walter H. Waddell PPG Industries, Chemicals Group Technical Center 440 College Park Drive, Monroeville, PA 15146 Mark G. White School of Chemical Engineering Georgia Institute of Technology Atlanta, CA 30332-0100 v

Preface Over the last several years, the field of materials science has witnessed an explosion of new, advanced materials. They encompass many uses and include superconductors, alloys, glasses, and catalysts. Not only are there quite a number of new enhies into these generic classes of materials, but the materials themselves represent a wide array of physical forms as well. Bulk materials, for example, are being synthesized and applications found for them, while still other materials are being synthesized as thin films for yet still more new (and in some cases, as yet unknown) applications. The field continues to expand with (thankfully!) no end in sight as to the number of new possibilities. As work progresses in this area, there is an ever increasing demand for knowing not only what material is formed as an end product but also details of the route by which it is made. The knowledge of reaction mechanisms in their synthesis many times allows a researcher to tailor a preparative scheme to either arrive at the final product in a purer state or with a better yield. Also, a good fundamental experimental knowledge of impurities present in the final material helps the investigator get more insight into making it. In addition to the generic types of materials (insulators, composites, etc.) that are of interest, there is also a wide diversity of chemical and electronic states involved in the various materials. Some are paramagnetic, while some are diamagnetic. Some are composed of metal centers, while others are based on nonmetallic systems. There are substantial repercussions of this, the chief one being that there must be judicious choices of analytical and instrumentative approaches for studying a system with its own peculiar chemical/electronic properties. In the examples mentioned above, a paramagnetic material could be studied quite well using magnetochernical and electron paramagnetic resonance (EPR) approaches but not in most cases with nuclear magnetic resonance. The opposite is true, however, for systems involving diamagnetic species that are carbon, tin, or other nuclear magnetic resonance (NMR) - amenable centers. Too, some other diamagnetic centers may be studied by other techniques such as nuclear quadrupole resonance (NQR) in which the central atom under study has nuclear properties that preclude NMR observation. Still other techniques such as x-ray photoelectron and Auger spectroscopies can be used to study both diamagnetic and paramagnetic materials with equal ease. It is easy to see then that in many instances, a broad, multiple technique approach is necessary to obtain a total understanding of a new material. The work contained in this volume represents a partial and supplemented proceedings of the Symposium on the Applications of Analytical Techniques to the Characterization of Materials which was held at the 200th National Meeting of the American Chemical Society, Washington, D.C., August 26-31, 1990, under the auspices of the Division of Industrial and Engineering Chemistry. The symposium was balanced between the types of materials that can be studied and the techniques that can be used. Obviously not all materials, techniques, and their various permutations can be addressed during such a symposium, regardless of its length. However, an attempt has been made to stlike a balance among several diverse analytical approaches and materials. Types of materials vii

included are inorganic salts and materials, superconductors, composites, rubbers, catalysts, ceramics, and oxides. Analytical approaches included Mossbauer, Raman, and infrared spectroscopy. In any endeavor of the scope and size of a research symposium, there are always people whose help is absolutely essential, and the one represented by these proceedings was no different. This help was deeply appreciated by me, with many thanks being extended to several people. First, I wish to thank the speakers, without whose help the symposium would have been impossible. Second, I wish to thank the Division of Industrial and Engineering Chemistry and its associated staff for being both supportive of the symposium and for helping to bring it to actual fruition. I especially wish to single out Kathleen and Wallace Schulz, James McEvoy, Melanie J. Cravey, Neil Ivory, and Costi A. Audeh for thanks. Berkeley, California November, 1991 viii

Contents Chapter 1. Application of Combined X-Ray Photoelectron/Auger Spectroscopy to Studies of Inorganic Materials... 1 Chapter 2. X-Ray Photoelectron and Ion Scattering Spectroscopic Studies of Composites... 25 John G. Dillard Chapter 3. Diffraction and Mossbauer Spectroscopic Characterization of Mixed Metal Oxides... 41 Frank J. Berry Chapter 4. Characterization of High Temperature Superconductors with Raman Spectroscopy... 59 Eric Faulques and Richard E. Russo Chapter 5. Applications of AC Complex Impedance Spectroscopy to Fast Ion Conducting Lithium Silicate Gels... 101 Lisa C. Klein, Shu-Fang Bo, Sung-Ping Szu and Martha Greenblatt Chapter 6. Applications of the Mossbauer Effect to the Characterization of Materials... 119 Gary J. Long and Femande Grandjean Chapter 7. Laser Mass Spectral Analysis of Rubber Surfaces... 153 Walter H. Waddell Chapter 8. The Uses of Thermogravimetric Analysis and Infrared Spectroscopy for Characterizating Supported Catalysts... 169 Mark G. White Index... 191 ix