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Nanomaterials: Synthesis, Properties and Applications
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Page iii
Nanomaterials
Synthesis, Properties and Applications
Edited by
A S Edelstein
Naval Research Laboratory
Washington, DC
and
R C Cammarata
Department of Materials Science and Engineering
Johns Hopkins University
Baltimore, MD
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Copyright © 1996 by IOP Publishing Ltd and individual contributors. 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 written permission of
the publisher, except as stated below. Single photocopies of single articles may be made for private
study or research. Illustrations and short extracts from the text of individual contributions may be
copied provided that the source is acknowledged, the permission of the authors is obtained and IOP
Publishing Ltd is notified. Multiple copying is permitted in accordance with the terms of the licences
issued by the Copyright Licensing Agency under the terms of its agreement with the Committee of
Vice-Chancellors and Principals.
British Library Cataloguing in Publication Data
A catalogue record for this book is available from the British Library.
ISBN 0 7503 0358 1 (hbk)
ISBN 0 7503 0578 9 (pbk)
Library of Congress Cataloging-in-Publication Data are available
First published 1996
Paperback edition 1998
Published by Institute of Physics Publishing, wholly owned by The Institute of Physics, London
Institute of Physics Publishing, Dirac House, Temple Back, Bristol BS1 6BE, UK
US Office: Institute of Physics Publishing, The Public Ledger Building, Suite 1035, 150 South
Independence Mall West, Philadelphia, PA 19106, USA
Printed in the UK by J W Arrowsmith Ltd, Bristol
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CONTENTS
Preface xv
Authors' Addresses xvii
Acknowledgments xxi
Part 1
Introduction
1
1
Introduction
3
Part 2
Synthesis
11
2
Formation of Clusters and Nanoparticles from a Supersaturated Vapor and
Selected Properties
13
2.1 Introduction 13
2.2 Clusters 14
2.2.1 Classical Nucleation Theory for Cluster Formation 14
2.2.2 Techniques for Cluster Formation 16
2.2.3 Cluster Assembled Materials 24
2.2.4 Physical and Chemical Properties of Clusters 26
2.3 Nanoparticles Produced by Sputtering and Thermal Evaporation and
Laser Methods
35
2.3.1 Background 35
2.3.2 Achieving Supersaturation 38
2.3.3 Particle Nucleation and Growth 40
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2.3.4 Coalescence, Coagulation and Size Distributions 41
2.3.5 Particle Transport 43
2.3.6 Particle Collection 45
2.3.7 Crystal Structure and Crystal Habit 45
3
Particle Synthesis by Chemical Routes
55
3.1 Introduction 55
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3.2 Nucleation and Growth from Solutions 57
3.3 Stabilization of Fine Particles against Agglomeration 57
3.4 Materials 59
3.4.1 Metals and Intermetallics 59
3.4.2 Ceramics 62
3.4.3 Composites 63
3.4.4 Nanoparticles via Organized Membranes 65
3.4.5 Clusters 67
3.5 Conclusions 68
4
Synthesis of Semiconductor Nanoclusters
73
4.1 Characterization Methods and Potential Pitfalls in the Synthesis 74
4.2 Colloids/Micelles/Vesicles 76
4.3 Polymers 78
4.4 Glasses 79
4.5 Crystalline and Zeolite Hosts 80
4.6 Towards Single-size Clusters 82
4.6.1 Controlled Cluster Fusion in Solution 83
4.6.2 Controlled Thermolysis in the Solid State 84
5
Formation of Nanostructures by Mechanical Attrition
89
5.1 Introduction and Background 89
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5.2 High-energy Ball Milling and Mechanical Attrition 90
5.3 Phenomenology of Nanostructure Formation 92
5.3.1 Elements and Intermetallics 92
5.3.2 Nonequilibrium Solid Solutions 95
5.3.3 Nanocomposites by Mechano-chemistry 97
5.4 Mechanism of Grain-size Reduction 99
5.5 Property–microstructure Relationships 103
5.6 Related Topics 108
Part 3
Artificially Multilayered Materials
111
6
Artificially Multilayered Materials
113
6.1 Introduction 113
6.2 Structure and Characterization 114
6.2.1 Microstructure 114
6.2.2 Dislocation Filters 117
6.2.3 Characterization 117
6.3 Processing 120
6.3.1 Thin-film Deposition Methods 120
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6.3.2 Mechanical Processing Methods 126
6.4 Thermodynamics and Kinetics 126
6.4.1 Thermodynamics 126
6.4.2 Kinetics 127
6.5 Electrical and Optical Properties 128
6.5.1 Semiconductor Superlattices 128
6.5.2 Microelectronics Applications 130
6.5.3 Optoelectronics Applications 131
6.5.4 Electronic Transport in Metallic Multilayers 132
6.5.5 Bragg Reflectors 133
6.6 Superconducting Properties 134
6.6.1 Low-temperature Superconductors 134
6.6.2 High-temperature Superconductors 134
6.7 Magnetic Properties 135
6.7.1 Magnetic Superlattices 135
6.7.2 Giant Magnetoresistance 136
6.8 Mechanical Properties 137
6.8.1 Elastic Properties 137
6.8.2 Damping Capacity 138
6.8.3 Plastic Properties 138
6.8.4 Wear and Friction 140
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6.8.5 Fracture 140
Part 4
Processing of Nanomaterials
145
7
Processing of Nanostructured Sol–gel Materials
147
7.1 Introduction 147
7.2 Synthesis of Oxides by the Sol–gel Process 149
7.2.1 Alkoxide Solution Routes 149
7.2.2 Colloidal Sols and Suspensions 151
7.2.3 Single-component Oxides 152
7.2.4 Multicomponent Oxides 152
7.3 Powder-free Processing of Gel Shapes 152
7.3.1 Thin Films 153
7.3.2 Fibers, Sheets and Thick Layers 154
7.3.3 Microporous Monoliths 155
7.4 Unconsolidated Gels: Aging and Syneresis 155
7.5 Consolidated Gels: Sintering 156
7.6 Matrices for Access to the Nanostructure 157
7.6.1 In situ composites 159
7.6.2 Volatile Host Method 159
7.6.3 Infiltrated Composites 161
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7.7 Prospects for the Sol–gel Processing of Nanostructured Materials 161
8
Consolidation of Nanocrystalline Materials by Compaction and Sintering
165
8.1 Introduction 165
8.2 Dry Compaction of Nanocrystalline Particles 166
8.3 Wet Compaction of Nanocrystalline Particles 169
8.4 Ideal Densification during Pressureless Sintering 170
8.5 Non-ideal Densification during Pressureless Sintering 177
8.5.1 Agglomeration Effects 177
8.5.2 Inhomogeneous Sintering/Differential Densification 179
8.6 Grain Growth during Pressureless Sintering 182
8.7 Grain Boundary Pinning by Pores during Pressureless Sintering 186
8.8 Minimizing Grain Growth and Maximizing Densification during
Pressureless Sintering
187
8.9 Pressure-assisted Sintering and Sinter Forging 189
8.10 Summary 194
Part 5
Characterization of Nanostructured Materials
199
9
Nanostructures of Metals and Ceramics
201
9.1 Introduction 201
9.2 Structures of Nanophase Materials 203
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9.2.1 Grains 203
9.2.2 Atomic Defects and Dislocations 204
9.2.3 Pores 207
9.2.4 Grain Boundaries 210
9.2.5 Stability 212
9.2.6 Strains 214
9.3 Conclusions 215
10
Characterization by Scattering Techniques and EXAFS
219
10.1 Introduction 219
10.2 Real-space Information from Experimental Reciprocal-space Data:
Atomic Distribution Function
222
10.2.1 Real-space-reciprocal-space Relations 222
10.2.2 Atomic Distribution and Interference Functions for Arrays of
Nanometer Particles
223
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10.2.3 Comparison of a Non-reconstructed Nanocrystalline Solid to
Isolated Particles
225
10.2.4 Nanocrystalline Solid with a Disordered Grain Boundary
Component
226
10.2.5 Particles with a Distribution of Sizes 227
10.3 Characterizing the Crystal Lattice 230
10.3.1 Crystallographic Phase and Lattice Constant 230
10.3.2 Grain-size Distribution 233
10.3.3 Grain Growth and Control of Grain Size 238
10.3.4 Lattice Strain 241
10.3.5 Stacking Faults and Twin Boundaries 245
10.3.6 Short- and Medium-range Correlated Displacements 246
10.4 Characterizing the Grain Boundaries 250
10.4.1 Relation Between Grain Boundary Short-range Order and
Grain Size
250
10.4.2 Grain Boundary Short-range Order in Nanocrystalline
Solids
251
10.4.3 Grain Boundary Short-range Order from EXAFS Studies 254
10.5 Distribution of Free Volume from Small-angle Scattering 257
10.6 Nanostructured Amorphous Solids 264
10.7 Magnetic Structure 266
10.8 Dynamics from Inelastic Neutron Scattering 269
10.9 Summary 270
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11
Interfacial Free Volumes and Atomic Diffusion in Nanostructured Solids
277
11.1 Introduction 277
11.2 Preparation and Characterization of Nanocrystalline Materials 278
11.3 Structural Free Volumes in Nanophase Materials as Probed by
Positrons
279
11.3.1 The Technique of Positron Lifetime Spectroscopy 279
11.3.2 Nanocrystalline Metals 280
11.3.3 Nanocrystalline Alloys 288
11.3.4 Nanocrystalline Silicon 290
11.3.5 Nanocrystalline Ceramics 291
11.4 Diffusion 294
11.5 Helium Desorption after Implantation 295
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Part 6
Properties of Nanostructured Materials
303
12
Chemical Properties
305
12.1 Introduction 305
12.2 Examples of Nanostructures in Chemistry 306
12.2.1 Colloids 306
12.2.2 Supported Nanoscale Catalysts 307
12.2.3 Nucleation Phenomena 308
12.3 The Effect of Nanoscale Materials on Chemical Reactivity 309
12.3.1 Chemical Reactivity: Metal Nanocrystallites Supported on
Oxides
309
12.3.2 Electrochemical Reactivity 310
12.3.3 Effect of Nanostructures on Mass Transport 314
12.4 The Effect of Chemistry on Nanostructures 316
12.5 Conclusions 318
13
Mechanical Properties
323
13.1 Low-temperature Properties: Yield Strength 323
13.1.1 Nanocrystalline Metals and Alloys 323
13.1.2 Nanocrystalline Ceramics 333
13.2 High-temperature Properties: Superplasticity 333
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13.2.1 Background of Superplasticity 334
13.2.2 Survey of Experimental Results 337
13.2.3 Sinter Forging 341
13.3 Future Directions 343
14
Magnetic and Electron Transport Properties of Granular Films
347
14.1 Introduction 347
14.2 Microstructure 348
14.3 Magnetic Properties 352
14.3.1 Overview 353
14.3.2 Superparamagnetic Properties 356
14.3.3 Ferromagnetic Properties 359
14.4 Electrical Transport Properties 360
14.4.1 Overview 361
14.4.2 Metallic Regime 363
14.4.3 Insulating Regime 365
14.5 Giant Magnetoresistance 367
14.6 Summary 371
15
Magnetic and Structural Properties of Nanoparticles
375
15.1 Introduction 375
15.2 Smoke Particles 377
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