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Inorganic Polymers,
Second Edition

James E. Mark
Harry R. Allcock
Robert West

OXFORD UNIVERSITY PRESS

INORGANIC POLYMERS
This page intentionally left blank
INORGANIC POLYMERS
Second Edition

James E. Mark
Harry R. Allcock
Robert West

1
2005
3
Oxford University Press, Inc., publishes works that further
Oxford University’s objective of excellence
in research, scholarship, and education.
Oxford New York
Auckland Cape Town Dar es Salaam Hong Kong Karachi
Kuala Lumpur Madrid Melbourne Mexico City Nairobi
New Delhi Shanghai Taipei Toronto
With offices in
Argentina Austria Brazil Chile Czech Republic France Greece
Guatemala Hungary Italy Japan Poland Portugal Singapore
South Korea Switzerland Thailand Turkey Ukraine Vietnam

Copyright © 2005 by Oxford University Press, Inc.

Published by Oxford University Press, Inc.

198 Madison Avenue, New York, New York, 10016
www.oup.com
This volume is a revised edition of Inorganic Polymers
published in 1992 by Prentice Hall.
Oxford is a registered trademark of Oxford University Press
All rights reserved. No part of this publication may be reproduced,
stored in a retrieval system, or transmitted, in any form or by any means,
electronic, mechanical, photocopying, recording, or otherwise,
without the prior permission of Oxford University Press.

Library of Congress Cataloging-in-Publication Data

Mark, James E., 1934–
Inorganic polymers/James E. Mark, Harry R. Allcock, Robert West.—2nd ed.
p. cm.
Includes bibliographical references and index.
ISBN-13 978-0-19-513119-2
ISBN-0-19-513119-3
1. Inorganic polymers. I. Allcock, H. R. II. West, Robert, 1928– III. Title.
QD196.M37 2004
546—dc22 2004043395

9 8 7 6 5 4 3 2 1
Printed in the United States of America
on acid-free paper
 Preface to the Second Edition

As was the case with the first edition, the goal was to provide a broad overview of
inorganic polymers in a way that will be useful to both the uninitiated and to those
already working in this field. The coverage has been updated and expanded significantly
to cover advances and interesting trends since the first edition appeared. The most
obvious changes are the three new chapters, “Ferrocene-Based Polymers, and
Additional Phosphorus- and Boron-Containing Polymers,” “Inorganic-Organic Hybrid
Composites,” and “Preceramic Inorganic Polymers.”
The authors once again hope that readers will be inspired to enter and contribute to
this fascinating area of inorganic polymeric materials.
This page intentionally left blank
 Preface to the First Edition

Most polymers being synthesized, characterized, and utilized in today’s world are
organic in nature. That is, their chain backbones consist primarily of carbon atoms,
frequently along with some heteroatoms such as oxygen and nitrogen. Their attractive
properties, such as easy processibility, high strength, and low density, have been
exploited in all industrialized societies to the extent that it is now difficult to imagine
life without them.
In spite of their many successes, organic polymers have a number of deficiencies.
For one, the monomers from which they are prepared are frequently subject to the
vagaries of the petroleum industry. The polymers themselves frequently have low soft-
ening temperatures or low degradation temperatures. Many are also vulnerable to
degradation from oxygen, ozone, or high-energy radiation. Some are subject to disso-
lution or swelling when in contact with solvents or fluids in commercial applications.
Finally, many present environmental problems by resisting incorporation into the
biosphere, or by forming highly toxic products upon combustion.
Inorganic polymers, with backbones typically of silicon, phosphorus, oxygen, or
nitrogen atoms, are now being more and more intensively studied. One obvious reason
is the quest to find materials not suffering from some of the limitations mentioned
above. No single polymer, of course, can be expected to meet all of the desired proper-
ties for an application, particularly in the high-technology area. Nonetheless, the very
different chemical nature of inorganic materials suggests they could well be superior to
their organic counterparts in a variety of ways. The polysiloxanes, with their superb
thermal stability, are a good example in this regard. The controlled degradability and
the innocuous degradation products of polyphosphazenes in controlled drug-delivery
systems is another.
There are numerous other reasons for being interested in inorganic polymers. One is
the simple need to know how structure affects the properties of a polymer, particularly
viii PREFACE TO THE FIRST EDITION

outside the well-plowed area of organic materials. Another is the bridge that inorganic
polymers provide between polymer science and ceramics. More and more chemistry is
being used in the preparation of ceramics of carefully controlled structure, and inor-
ganic polymers are increasingly important precursor materials in such approaches.
The present book was prepared to provide an introduction to the field of inorganic
polymers. There has long been a need for such a book, as opposed to the ready avail-
ability of numerous other books, that are highly specialized and written for scientists
already working in this area. The only background required for its comprehension are
the basic concepts presented in a typical undergraduate course in chemistry. Some famil-
iarty with the fundamentals of polymer science would be helpful, but not necessary,
since many of these are covered in an introductory chapter on polymer characterization.
It is hoped that the book will be useful to a variety of readers, including polymer
chemists, inorganic chemists, chemical engineers, and materials scientists. The highly
tutorial nature of the presentation should also make it useful as a textbook, for a one-
term course.
One of the advantages of writing a book is the uncovering of an almost endless series
of interesting research ideas. We hope our readers benefit in the same way and will
explore more deeply this fascinating new area of polymer science and engineering.
 Contents

About the Authors xiii

1 Introduction 3
1.1 What Is a Polymer? 3
1.2 How Polymers Are Depicted 3
1.3 Reasons for Interest in Inorganic Polymers 5
1.4 Types of Inorganic Polymers 6
1.5 Special Characteristics of Polymers 7

2 Characterization of Inorganic Polymers 8

2.1 Molecular Weights 8
2.2 Molecular Weight Distributions 18
2.3 Other Structural Features 22
2.4 Chain Statistics 26
2.5 Solubility Considerations 28
2.6 Crystallinity 34
2.7 Transitions 40
2.8 Spectroscopy 49
2.9 Mechanical Properties 50
References 58

3 Polyphosphazenes 62
3.1 Introduction 62
3.2 History 65
3.3 Alternative Synthesis Routes to Linear Polymers 70
3.4 Surface Reactions of Polyphosphazenes 83
x CONTENTS

3.5 Hybrid Systems through Block, Comb, or Ring-Linked Copolymers 84

3.6 Hybrid Systems through Composites 93
3.7 Organometallic Polyphosphazenes 93
3.8 Small-Molecule Models 99
3.9 Molecular Structure of Linear Polyphosphazenes 100
3.10 Structure–Property Relationships 107
3.11 Applications of Polyphosphazenes 111
3.12 Optical and Photonic Polymers 137
3.13 Polymers Related to Polyphosphazenes 141
3.14 Conclusions 143
References 146

4 Polysiloxanes and Related Polymers 154

4.1 Introduction 154
4.2 History 155
4.3 Nomenclature 155
4.4 Preparation and Analysis 156
4.5 General Properties 162
4.6 Reactive Homopolymers 176
4.7 Elastomeric Networks 177
4.8 Some New Characterization Techniques Useful for Polysiloxanes 181
4.9 Copolymers and Interpenetrating Networks 183
4.10 Applications 184
References 189

5 Polysilanes and Related Polymers 200

5.1 Introduction 200
5.2 History 201
5.3 Synthesis 204
5.4 Chemical Modification of Polysilanes 212
5.5 Physical Properties of Polysilanes 213
5.6 Electronic Properties of Polysilanes 215
5.7 Chromotropism of Polysilanes 220
5.8 Electrical Conductivity and Photoconductivity 230
5.9 Luminescence of Polysilanes 232
5.10 Photodegradation of Polysilanes 233
5.11 Cross-Linking 234
5.12 Structural Arrangements in Polysilanes 236
5.13 Technology of Polysilanes 244
5.14 Additional Readings 250
References 250
 CONTENTS xi

6 Ferrocene-Based Polymers, and Additional Phosphorus- and

Boron-Containing Polymers 254
6.1 Ferrocene-Based Polymers 254
6.2 Other Phosphorus-Containing Polymers 266
6.3 Boron-Containing Polymers 269
References 270

7 Miscellaneous Inorganic Polymers 273

7.1 Introduction 273
7.2 Other Silicon-Containing Polymers 273
7.3 Polygermanes 275
7.4 Polymeric Sulfur and Selenium 276
7.5 Other Sulfur-Containing Polymers 279
7.6 Aluminum-Containing Polymers 284
7.7 Tin-Containing Polymers 284
7.8 Arsenic-Containing Polymers 286
7.9 Metal Coordination Polymers 286
7.10 Other Organometallic Species for Sol-Gel Processes 289
References 290

8 Inorganic-Organic Hybrid Composites 294

8.1 Sol-Gel Ceramics 294
8.2 Fillers in Elastomers 295
8.3 Polymer-Modified Ceramics 305
References 307

9 Preceramic Inorganic Polymers 312

9.1 Overview of Ceramic Aspects 312
9.2 The Sol-Gel Process to Oxide Ceramics 313
9.3 Carbon Fiber 319
9.4 Silicon Carbide (SiC) 320
9.5 Silicon Nitride (Si3N4) 324
9.6 Boron Nitride (BN) 327
9.7 Boron Carbide (B4C) 329
9.8 Aluminum Nitride (AlN) 330
9.9 Phosphorus Nitride (P3N5) 330
9.10 Poly(ferrocenylsilanes) as Ceramic Precursors 331
References 332

Index 335
This page intentionally left blank
 About the Authors

James E. Mark received his B.S. degree in 1957 in Chemistry from Wilkes College
and his Ph.D. degree in 1962 in Physical Chemistry from the University of
Pennsylvania. After serving as a Postdoctoral Fellow at Stanford University under
Professor Paul J. Flory, he was Assistant Professor of Chemistry at the Polytechnic
Institute of Brooklyn before moving to the University of Michigan, where he became
a Full Professor in 1972. In 1977, he assumed the position of Professor of Chemistry
at the University of Cincinnati, and served as Chairman of the Physical Chemistry
Division and Director of the Polymer Research Center. In 1987, he was named the first
Distinguished Research Professor, a position he holds at the present time. In addition,
he has extensive research and consulting experience in industry and has served as a
Visiting Professor at several institutions. Dr. Mark’s research interests pertain to the
physical chemistry of polymers, including the elasticity of polymer networks, hybrid
organic-inorganic composites, liquid-crystalline polymers, and a variety of computer
simulations. Dr. Mark is an extensive lecturer in polymer chemistry, is an organizer and
participant in a number of short courses, and has published approximately 625 research
papers and coauthored or coedited twenty books. He is the founding editor of the journal
Computational and Theoretical Polymer Science, which was started in 1990, is an
editor for the journal Polymer, and serves on a number of journal Editorial Boards. He
is a Fellow of the New York Academy of Sciences, the American Physical Society, and
the American Association for the Advancement of Science. His awards include the
Dean’s Award for Distinguished Scholarship, the Rieveschl Research Award, and the
Jaffe Chemistry Faculty Excellence Award (all from the University of Cincinnati),
the Whitby Award and the Charles Goodyear Medal (Rubber Division of the American
Chemical Society), the ACS Applied Polymer Science Award, the Flory Polymer
Education Award (ACS Division of Polymer Chemistry), election to the Inaugural
Group of Fellows (ACS Division of Polymeric Materials Science and Engineering),

xiii
xiv ABOUT THE AUTHORS

the Turner Alfrey Visiting Professorship, the Edward W. Morley Award from the ACS
Cleveland Section, the ACS Kipping Award in Silicon Chemistry, the Reed Lectureship
at Rensselaer, and an Award for Outstanding Achievement in Polymer Science and
Technology from the Society of Polymer Science, Japan.

Harry Allcock has devoted most of his career to the field of inorganic polymers. He
was responsible for the design and synthesis of the first stable polyphosphazenes, and
he and his coworkers at The Pennsylvania State University have played a major role in
the development of this field through their 475 research publications. His research
focuses on fundamental synthetic chemistry and an understanding of structure–property
relationships, together with explorations of possible applications for the new polymers
in biomedicine, aerospace, energy storage and generation, and communications
technology. Allcock has also written three monographs on inorganic rings and macro-
molecules, has coauthored a widely used textbook on polymer chemistry and an
introductory text on inorganic polymers, and has coedited three books on inorganic
chemistry and inorganic materials. He is the recipient of three American Chemical
Society National Awards, is a Guggenheim Fellow, and has lectured widely on
polyphosphazenes and other inorganic polymer systems. Allcock was born and edu-
cated in the United Kingdom and received B.Sc. and Ph.D. degrees from the University
of London. His position as an Evan Pugh Professor of Chemistry at Penn State is the
highest academic honor bestowed by the University.

Robert West was born in New Jersey and educated at Cornell University (B.A.)
and Harvard University (A.M., Ph.D.). For the past 45 years he has been a
faculty member in the chemistry department at the University of Wisconsin, where he is
now E. G. Rochow Professor and Director of the Organosilicon Research Center. His
many awards include the Frederick Stanley Kipping Award, the Wacker silicone prize,
the Alexander von Humboldt Award, and the main group chemistry medal. He has
published more than 600 scientific papers, mostly in the area of silicon chemistry. Major
discoveries in his laboratories include the first soluble polysilanes (1978), the silicon-
silicon double bond (1981), the first stable silylenes (1994), and electrically conducting
organosilanes for high energy density batteries (2000). He is an airplane pilot and a
mountaineer, with numerous first ascents in Canada and Alaska.
INORGANIC POLYMERS
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