Advances in Materials Characterization II

411 Pages·1985·12.963 MB·English

by  P. J. Bray, S. J. Gravina (auth.), R. L. Snyder, R. A. Condrate Sr., P. F. Johnson (eds.)

MATERIALS SCIENCE RESEARCH
Volume 19
ADVANCES
IN MATERIALS
CHARACTERIZATION II
MATERIALS SCIENCE RESEARCH
Recent volumes in the series:
Volume 9 MASS TRANSPORT PHENOMENA IN CERAMICS
Edited by A. R. Cooper and A. H. Heuer
Volume 10 SINTERING AND CATALYSIS
Edited by G. C. Kuczynski
Volume 11 PROCESSING OF CRYSTALLINE CERAMICS
Edited by Hayne Palmour III, R. F. Davis, T. M. Hare
Volume 12 BORATE GLASSES: Structure, Properties, Applications
Edited by L. D. Pye, V. D. Frechette and N. J. Kreidl
Volume 13 SINTERING PROCESSES
Edited by G. C. Kuczynski
Volume 14 SURFACES AND INTERFACES IN CERAMIC AND
CERAMIC-METAL SYSTEMS
Edited by Joseph Pask and Anthony Evans
Volume 15 ADVANCES IN MATERIALS CHARACTERIZATION
Edited by David R. Rossington, Robert A. Condrate,
and Robert L. Snyder
Volume 16 SINTERING AND HETEROGENEOUS CATALYSIS
Edited by G. C. Kuczynski, Albert E. Miller, and Gordon A. Sargent
Volume 17 EMERGENT PROCESS METHODS FOR HIGH-TECHNOLOGY
CERAMICS
Edited by Robert F. Davis, Hayne Palmour III,
and Richard L. Porter
Volume 18 DEFORMATION OF CERAMIC MATERIALS II
Edited by Richard E. Tressler and Richard C. Bradt
Volume 19 ADVANCES IN MATERIALS CHARACTERIZATION II
Edited by R. L. Snyder, R. A. Condrate, Sr., and P. F. Johnson
A Continuation Order Plan is available for this series. A continuation order will bring delivery of each
new volume immediately upon publication. Volumes are billed only upon actual shipment. For further in
formation please contact the publisher.
Library of Congress Cataloging in Publication Data
Symposium on Advances in Materials Characterization (1984: Alfred, N.Y.)
Advances in materials characterization II.
(Materials science research; v. 19)
"Proceedings of a Symposium on Advances in Materials Characterization, held July
30-August 3, 1984, in Alfred, New York"-T.p. verso.
Includes bibliographical references and index.
1. Materials - Testing - Congresses. 2. Materials - Surfaces - Congresses. I. Snyder,
Robert L., 1935- . Condrate, Robert A., 1938- . III. Johnson, P. F. IV. Title.
V. Series.
TA41O.S93 1984 620.1'1 85-12300
ISBN-13: 978-1-4615-9441-3 e-ISBN-13: 978-1-4615-9439-0
DOl: 10.1007/978-1-4615-9439-0
Proceedings of a symposium on Advances in Materials Characterization,
held July 30-August 3, 1984, in Alfred, New York
© 1985 Plenum Press, New York
Softcover reprint of the hardcover 1s t edition 1985
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, microfilming,
recording, or otherwise, without written permission from the Publisher
MATERIALS SCIENCE RESEARCH • Volume 19
ADVANCES IN
MATERIALS
CHARACTERIZATION II
Edited by
R. L. Snyder
R. A. Condrate, Sr.
and
P. F. Johnson
New York State College of Ceramics
Alfred University
Alfred, New York
PLENUM PRESS • NEW YORK AND LONDON
PREFACE
This book represents the proceedings of the second inter
disciplinary conference on materials characterization held from July
30 through August 3, 1984 at the New York State College of Ceramics
at Alfred University. The conference was the 20th in the University
Series on Ceramic Science, instituted in 1964 by Alfred University,
the University of California at Berkeley, North Carolina State
University and Notre Dame University. Volume I of the proceedings
of the first conference using this interdisciplinary approach to
materials characterization was published as "Advances in Materials
Characterization", edited by D. R. Rossington, R. A. Condrate and
R. L. Snyder, and was listed as volume 15 of the Materials Science
Research series of Plenum Press (New York, 1983).
The purpose of bringing together scientists from a wide range
of disciplines to present and discuss the latest developments in
their fields is to promote cross fertilization. The first
conference of this type and its resulting volume of proceedings
stimulated a significant dialogue between disciplines concerning the
characterization of materials, therefore indicating a need for a
continuing series of such conferences.
Characterization lies at the core of materials science.
Advancements in this science proceed rapidly after breakthroughs in
characterization techniques. This series of conferences has as
their goal the stimulation of the development of new ways of
"seeing" into the nature of materials phenomena. It is the nature
of modern science for researchers to become specialists. We become
expert at the use of a particular set of physical principles and
their applications to a limited set of problems. This usually
implies the devotion of such a large portion of our time and
energies to our own particular limited areas that we cannot follow
developments in other fields at the depth required to stimulate new
ideas in our own.
If we have learned anything in recent years it is that
characterization of a material or a phenomena is seldom accomplished
v
by the application of a single tool but results from a broad attack
using the full arsenal of modern techniques. Thus an interdiscipli
nary approach to characterization has two benefits: the increasing
of our awareness of the potential of other techniques and the condi
tions under which they are applied, and even more significantly, the
application of ideas born in another discipline to our own.
The various discussions of instrumental techniques presented in
both of these volumes are excellent summaries of the state-of-the
art of materials characterization at this still rather early stage
of materials science. The application of the tools described here,
and those yet to be developed, holds the key to the development of
this infant into a mature science. It seems clear that conferences
as presented in this series, and the resulting volumes of their
proceedings should help catalyze such growth. However one rather
myopic reviewer of volume I tried to view it as a text book!
The 32 papers included in these Proceedings cover a broad
array of established and new characterization techniques. They
have been broadly divided into categories determined by the type of
characterization being sought. These categories are: Molecular
Structure, Lattice Structure, Phase, Surface and Interfaces and
Microstructure. However, as would be expected for such a broad
survey there is often considerable overlap among techniques and
goals of the studies.
The three day conference was preceeded by a series of hands on
work shops which proved invaluable to preparing researchers, in
fields outside their own, for full participation in the conference
to follow. The editors would like to express their special
appreciation to the following people for their efforts in preparing
and conducting these workshops:
1. W. A.Lanford for "Nuclear Reaction Analysis and
Rutherford Backscattering Spectrometry".
2. W. E. Votava for "Analytical Scanning Electron
Microscopy" •
3. R. A. Condrate and J. R. Ferraro for "Optical Spectral
Techniques for Elemental, Phase and Structural Analysis".
4. R. L. Snyder for "Quantitative Phase Analysis by
Automated X-ray Diffraction".
5. P. F. Johnson for "Techniques of Surface Analysis, XPS,
SIMS and AES".
The editors wish to thank all speakers and contributors to
the conference, and especially to those who were invited to
present overview papers in their field of expertise (specifically,
Dr. P. J. Bray, Dr. R. M. Barnes and Dr. B. O. Mysen).
The editors also gratefully acknowledge the conference sponsors
listed below. Their financial support and commitments were
invaluable constituents to the success of the conference.
vi
u.s.
Dept. of the Interior - Bureau of Mines
Brockway, Inc.
Horiba Instruments, Inc.
Instruments SA, Inc
Joel
Leybold-Heraeus Vacuum Products
Perkin-Elmer Corporation
Shott Optical Glass Co.
Siemens Corporation
The success of any conference depends not only upon the quality
of papers presented and its sponsorship, but also on the many people
involved in the planning and preparation stages. It is impossible
to list all the people at the New York State College of Ceramics who
were responsible for the efficient running of the conference, but
special thanks are due to Mrs. Coral Link and Ms. Faith Orth for
registration, organizational and secretarial services. Mr. William
Emrick did an outstanding job of setting up most of the local
arrangements, including housing, food and many details of the
program for those accompanying the participants. Special thanks
must go to our wives Sheila Snyder, Judy Condrate and Karen Johnson
for the endless details that they kept organized, and for their
planning and conducting of the program involving those accompanying
conference participants. To all these people, and the many graduate
students who performed the many last minute tasks that inevitably
arise, the editors express their deep gratitude.
It is our sincere hope that this volume will prove to be of
benefit to all people involved in materials characterization.
Alfred, New York
Robert L. Snyder
Robert A. Condrate
Paul F. Johnson
CONTENTS
STRUCTURAL AND ELEMENTAL CHARACTERIZATION
NMR Characterization of Glasses................................ 1
P. J. Bray and S. J. Gravina
Application of Inductively Coupled Plasma Spectrometry
for the Analysis of Ceramics and Glasses ••••••••••••• 31
Ramon M. Barnes
Raman Spectra and Structure of Fluorine- and Water-bearing
Silicate Glasses and Melts ••••••••••••••••••••••••••• 43
B. 0. Mysen and D. Virgo
Simultaneous Crystallite Size, Strain and Structure
Analysis from X-ray powder Diffraction Pattern ••••••• 57
Scott A. Howard and Robert L. Snyder
The Infrared and Raman Spectra of Phosphorosilicate
Phases With 1: 1 Si0zlP 205 Molar Ratios.......... • • •• 73
I. N. Chakraborty and R. A. Condrate Sr.
Measurement of Nonstoichiometry in BaTi03 Using Raman
Spectroscopy ••••••••••••••••••••••••••••••••••••••••• 89
M. W. Urban and Bahne C. Cornilsen
Reststrahlen Effects in DRIFT Experiments for NaCl in
the Far-Infrared Region •••••••••.•••••••••••••••••••. 97
John R. Ferraro
PHASE CHARACTERIZATION
Newer Techniques in Optical Microscopy ••••••••••••••••••••••••• 103
V. D. Frechette
ix
Laser Raman Microprobe Study of the Identification and
Thermal Transformations of Some Carbonate and
Aluminosilicate Minerals ••••••••••••••••••••••••••••• 113
R. G. Herman, C. E. Bogdan and A. J. Sommer
Sample Characteristics Affecting Quantitative Analysis
by X-ray Powder Diffraction •••••••••••••••••••••••••• 131
James P. Cline and Robert L. Snyder
Laser Raman Microprobe Characterization of Fly Ash ••••••••••••• 145
Barry E. Scheetz, William B. White and F. Adar
Raman and Luminescence Spectroscopy of Zirconium Oxide
with the use of the Mole Microprobe •••••••••••••••••• 155
T. E. Doyle and J. L. Alvarez
SURFACE AND INTERFACE CHARACTERIZATION
High Resolution Electron Microscopic Characterization
of Interfaces in Ceramics •••••••••••••••••••••••••••• 167
Mehmet Sarikaya, Ilhan A. Aksay and Gareth Thomas
Characterization of Grain Boundaries in Alumina •••••••••••••••• 179
Karen J. Morrissey and C. B. Carter
Surface Reactivity of Silica and Alumina Ceramic Powders ••••••• 189
Wayne C. Hasz and Alan Bleier
Diffusion of Water in Si02 at Low Temperature •••••••••••••••••• 203
W. A. Lanford, C. Burman and R. H. Doremus
Spectroscopic Analysis of Molecular Surfaces by Ion,
Photoelectron and Vibrational Spectroscopy ••••••••••• 209
Joseph A. Gardella, Jr., Robert L. Schmitt,
Joseph H. Wandass and R. L. Chin
Thermal lvave Imaging of Defects in Opaque Solids ••••••••••••• 221
D. N. Rose, D. C. Bryk, D. J. Thomas, R. L. Thomas,
L. D. Favro, P. K. Kuo, L. J. Ingelhart, M. J. Lin,
and K. o. Legg
Studies of Adhesion Failure Mechanisms at Metal-HgCdTe and
ZnS-Ge Interfaces by SEM/SAM/EDX ••••••••••••••••••••• 241
Gerald A. Garwood, Jr. and Michael Ray
Electron Microscopic Studies of Plasma-Sprayed Coatings •••••••• 265
Christopher C. Berndt and Reginald McPherson
x
MICROSTRUCTURE CHARACTERIZATION
Experimental and Theoretical Aspects of Frequency-Domain
Photopyroelectric Spectroscopy of Condensed
Phases (PPES), A New, Simple and Powerful
Spectroscopic Technique
Andres Mandelis and John Zuccon •••••••••••••••••••••••••••••••• 279
Ultrasonic Flaw Detection in Model Ceramic Systems ••••••••••••• 291
Arthur J. Stockman and Patrick S. Nicholson
The Hygroscopic Behavior of SiO and Si 0 Cl Thin Films
on Si using ATR FTIR Spectra.~.~ •• ~ •••••••••••••••••• 301
R. Koba, J. R. Monkowski and R. E. Tressler
A New FT-IR Technique for the in situ Study of the Mechanism
of Solid State Materials Preparations •••••••••••••••• 315
William R. Moser, John C. Chiang and Jack E. Cnossen
Mercury Porosimetry of Dry Silica Gels ••••••••••••••••••••••••• 329
E. M. Rabinovich, and S. D. Poulsen
Characterization of Microstructural Evolution by Mercury
Porosimetry ....••••.••••..••.••.••••••••••••••••.••.• 339
C. Han, I. A. Aksay and O. J. Whittemore
Electrical Characterization of Ceramics and Polymers ••••••••••• 349
Larry C. Burton
Thermal Analysis of Organic Binders for Ceramic Processing ••••• 359
J. P. Pollinger and G. L. Messing
The Thermal Diffusivity of Simulated Nuclear Waste Glass
Below the Glass Transition Temperature ••••••••••••••• 371
Marco Y. Liem, L. D. Pye and D. Bickford
Characterization of Matrix-Dispersoid Reactions in
Si1N4-TiC Composites ••••••••••••••••••••••••••••••••• 389
Galina Zilberstein and S. Thomas Buljan
Kirlian Photography Material Science, Testing and Ichnology •••• 403
Daniel B. Sass and David C. Meissner
Index •••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••• ~ ••• 411
xi