Advances in Materials Characterization

665 Pages·1983·23.731 MB·English

by  C. G. Pantano, J. F. Kelso, M. J. Suscavage (auth.), David R. Rossington, Robert A. Condrate, Robert L. Snyder (eds.)

MATERIALS SCIENCE RESEARCH
Volume 15
ADVANCES IN
MATERIALS
CHARACTERIZATION
MATERIALS SCIENCE RESEARCH
Recent volumes in the series:
Volume 5 CERAMICS IN SEVERE ENVIRONMENTS
Edited by W. Wurth Kriegel and Hayne Palmour III
Volume 6 SINTERING AND RELATED PHENOMENA
Edited by G. C. Kuczynski
Volume 7 SURFACES AND INTERFACES OF GLASS AND CERAMICS
Edited by V. D. Frechette, W. C. LaCourse, and V. L. Burdick
Volume 8 CERAMIC ENGINEERING AND SCIENCE: Emerging Priorities
Edited by V. D. Frechette, L. D. Pye, and J. S. Reed
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
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.
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MATERIALS SCIENCE RESEARCH • Volume 15
ADVANCES IN
MATERIALS
CHARACTERIZATION
Edited by
DavidR. Rossington
Robert A. Condrate
and
Robert L. Snyder
New York State College of Ceramics
Alfred University
Alfred, New York
PLENUM PRESS • NEW YORK AND LONDON
Library of Congress Cataloging in Publication Data
Conference on Advances in Materials Characterization (1982: New York State College of
Ceramics at Alfred University)
Advances in materials characterization.
(Materials science research; v. 15)
"Proceedings of a Conference on Advances in Materials Characterization, held August 15-
18, 1982, at the New York State College of Ceramics at Alfred University, Alfred, New
York"-P.
Includes bibliographical references and index.
1. Materials - Testing - Congresses. 2. Materials -Surfaces - Congresses. I. Rossington,
David R., 1932- . II. Condrate, Robert A., 1938- . III. Snyder, Robert L., 1941-
IV. Title. V. Series.
TA41O.C56 1982 620.1'1 83-4186
ISBN-13: 978-1-4615-8341-7 e-ISBN-13: 978-1-4615-8339-4
DOl: 10.1 007/978-1-4615-8339-4
Proceedings of a Conference on
Advances in Materials Characterization,
held August 15-18, 1982,
at the New York State College of Ceramics
at Alfred University, Alfred, New York
© 1983 Plenum Press, New York
Softcove reprint of the hardcover 1s t edition 1983
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
PREFACE
The characterization of materials and phenomena has
historically been the principal limitation to the development in
each area of science. Once what we are observing is well
defined, a theoretical analysis rapidly follows. Modern
theories of chemical bonding did not evolve until the methods of
analytical chemistry had progressed to a point where the bulk
stoichiometry of chemical compounds was firmly established. The
great progress made during this century in understanding chemistry
has followed directly from the development of an analytical
chemistry based on the Dalton assumption of multiple proportions.
It has only become apparent in recent years that the
extension of our understanding of materials hinges on their
non-stoichiometric nature. The world of non-Daltonian chemistry
is very poorly understood at present because of our lack of
ability to precisely characterize it. The emergence of materials
science has only just occurred with our recognition of effects,
which have been thought previously to be minor variations from
ideality, as the principal phenomena controlling properties. The
next step in the historical evolution of materials science must be
the development of tools to characterize the often subtle
phenomena which determine properties of materials.
The various discussions of instrumental techniques presented
in this book are excellent summaries for the state-of-the-art of
materials characterization at this rather critical 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.
This volume constitutes the proceedings of the August 15-18,
1982 Conference on Advances in Materials Characterization, held at
the New York State College of Ceramics at Alfred University. The
conference was the 18th in the University Series on Ceramic
Science, instituted in 1964 by Alfred University, the University
of California at Berkeley, North Carolina State Uni versi ty and
Notre Dame University.
v
vi PREFACE
The 49 papers included in these Proceedings cover all aspects
of surface and bulk characterization and they have been divided
into general areas according to different experimental techniques.
However, as would be expected for such a broad topic as
characterization, there is often considerable overlap among
techniques.
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, namely:
Dr. R. Conzemius, Dr. E. Etz, Dr. J. Ferraro, Dr. B. T.
Khuri-Yakub, Dr. C. Pantano, Dr. R. L. Snyder, Dr. I.S.T. Tsong
and Dr. K. Wefers.
The editors also gratefully acknowledge the conference
sponsors listed below. Their financial support and commitment was
an invaluable constituent to the success of the conference.
U.S. Dept. of the Interior - Bureau of Mines
Corning Glass Works Foundation
IBM Corporation
General Motors Corporation - AC Spark Plug Division
Leybold-Heraeus Vacuum Products
Perkin-Elmer Corporation
Siemens Corporation
Spex Industries, Inc.
The success of any conference depends not only upon the
quality of papers presented and 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. Darlene Brewe.r,
Mrs. Josephine Schieder and Mrs. Doris Snowden for registration
and secretarial services, Mr. William Emrick for projection
facilities, Ms. Carol Binzer for accommodation facilities and
Mr. Michael Linehan for food service. 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 some area of materials
characterization.
Alfred, New York David R. Rossington
December, 1982 Robert A. Condrate
Robert L. Snyder
CONTENTS
SURFACE SPECTROSCOPY
Surface Studies of Multicomponent Silicate Glasses:
Quantitative Analysis, Sputtering Effects
and the Atomic Arrangement .• 1
C. G. Pantano, J. F. Kelso and M. J. Suscavage
Depth-Profiling Studies of Glasses and Ceramics
by Ion Beam Techniques. • . •.•. 39
I. S. T. Tsong
Analysis of Solids by Spark Source and Laser
Mass Spectroscopy • • • • • 59
Robert J. Conzemius and Harry J. Svec
Surface and Interface Studies of Metal
Oxide/Glass Systems • . 71
K. L. Smith
Atomic Structure at Electrode Surfaces • • • • • . 91
Gerald A. Garwood Jr., and Arthur T. Hubbard
SURFACE TECHNIQUES
Surface Characterization of Certain Metal
Oxides Determined by the Isothermal
Adsorption and Desorption of Argon • • • • • • • • • 109
Richard G. Herman, Philip Pendleton,
and John B. Bulko
Hysteresis in Mercury Porosimetry ••••••••••••••• 133
S. Lowell and J. E. Shields
Pore Structure Characterization by
Mercury Porosimetry •••.•••••••• 147
O. J. Whittemore and G. D. Halsey
viii CONTENTS
Surface Characteristics of Yttria Precursors
in Relation to Their Sintering
Behavior. . . . • . . • . . . . . • . • • • . • 159
Mufit Akinc and M. D. Rasmussen
VIBRATIONAL SPECTROSCOPIC TECHNIQUES
An Overview of Techniques Used in FT-IR
Spec troscopy. . . . . . . . . • . . . . . • . . • . . 171
John R. Ferraro
Raman Microprobe Spectroscopy of
Polyphase Ceramics.. •..••.•...•..•. 199
D. R. Clarke and F. Adar
Characterization of Anodically Grown Native
Oxide Films on HgO.7CdO.3Te ............. 215
Fran Adar, R. E. Kvaas and D. R. Rhiger
The Raman Spectra of Potassium Boro-
germanate Glasses . . . . . . . • 223
I. N. Chakraborty and R. A. Condrate, Sr.
Characterization of the Structure and
Nonstoichiometry of CaO-NiO
Solid Solutions . • . . . . . . • . . . . . . • . • 239
B. C. Cornilsen, E. F. Funkenbusch,
C. P. Clarke, P. Singh and
V. Lorprayoon
Vibrational Spectroscopies of Molecular
Monolayers in Thin Film Geometries. . ....•.. 249
J. R. Kirtley, J. C. Tsang, Ph. Avouris,
and Y. Thefaine
Characterization of Rare Earth Sulfides ••.......... 267
C. Lowe-Ma
ELECTRON OPTICAL METHODS
Applications of Analytical Microscopy
to Ceramic Research . . . . . . . . . . . . . . . . . 281
Paul F. Johnson
Analysis of Second-Phase Particles in A1203' .•....... 297
K. J. Morrissey and C. B. Carter
CONTENTS ix
Microstructural Characterization Abnormal
Grain Growth Development in Al203' • • . . .. 309
M. P. Harmer, S. J. Bennison and C. Narayan
Properties and Characterization of Surface
Oxides on Aluminum Alloys ..... 321
Karl Wefers
The Characterization of Microcracks
in Brittle Solids. 323
D. R. Clarke and D. J. Green
X-ray Energy Dispersive Spectroscopy of
Intergranular Phases in
S11 and S' Sialons .....• 339
T. R. Dinger and G. Thomas
EM Study of the Structure and Composition
of Grain Boundaries in (Mn, Zn) Fe204' 351
I-Nan Lin, R. K. Mishra and G. Thomas
Cross-Sectional Transmission Electron
Microscopy of Semiconductors 359
D. K. Sadana
Microstructural Characterization of Nuclear
Waste Ceramics • . . • . • 367
F. J. Ryerson and D. R. Clarke
Semiautomatic Image Analysis for Microstructure
and Powder Characterization. . . • . 387
D. W. Readey, E. Bright, S. S. Campbell,
J. H. Lee, R. S. Pan, T. Quadir, and
K. A. Williams
ACOUSTIC AND MECHANICAL PROPERTIES
Acoustic Characterization of Structural
Ceramics ... 401
B. T. Khuri-Yakub
Characterization of Ceramics by
Acoustic Microscopy 413
D. E. Yuhas and L. W. Kessler
Determination of Slow Crack Growth Using
an Automated Test Technique. . . 425
Helen H. Moeller and Robert L. Farmer
x CONTENTS
Biaxial Compression Testing of
Refractory Concretes. . . . . • . • . . . . • • • . • 437
Albert H. Bremser and Oral Buyukozturk
Mechanical Testing of Glass Hollow
Microspheres. • . . . . . . • . . . • . . . . . • . . 441
Paul W. Bratt, J. P. Cunnion and Bruce D. Spivack
GENERAL CRYSTALLOGRAPHIC TECHNIQUES
The Renaissance of X-ray Powder Diffraction. . • . . • . . . . 449
Robert L. Snyder
Characterization of Imperfections in Plasma-
Sprayed Titania . . . . . . . . • • . . 465
C. C. Berndt, R. Korlipara, R. A. Zatorski,
A. Jonca, T. Templeton and R. K. MacCrone
Characterization of the Mechanical Properties
of Plasma-Sprayed Coatings ........•..... 473
N. R. Shankar, C. C. Berndt and H. Herman
Analysis of Silicon Nitride. . . • .•.•... 491
Gary Czupryna and Samuel Natansohn
Acid-Base Properties of Ceramic Powders ..•..•...... 449
Alan Bleier
Recent Advances in Computerized High Temperature
Differential Thermal Analysis . . . . . . . 515
Charles M. Earnest, W. P. Brennan and
M. P. DiVito
Reflectance Technique for Measurement of
Bottom Surface Tin Concentration
on Clear Float Glass .••......•.•..•.• 531
Thomas O. LaFramboise
Characterization of Reinforcements for
Inorganic Composites • . . . • . . . . . . . 535
S. W. Bradstreet
GENERAL GLASS CHARACTERIZATION STUDIES
Nuclear Reaction Analysis of Glass Surfaces:
The Study of the Reaction Between
Water and Glass • . . . . . . • . . . • • 549
W. A. Lanford and C. Burman