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Processing, Properties and Potential Applications Edited by Carl C. Koch North Carolina State University Raleigh, North Carolina NOYES PUBLICATIONS WILLIAM ANDREW PUBLISHING Norwich, New York, U.S.A. NANOSTRUCTURED MATERIALS Copyright © 2002 by Noyes Publications No part of this book may be reproduced or utilized in any form or by any means, elec- tronic or mechanical, including photocopying, recording or by any information storage and retrieval system, without permission in writing from the Publisher. Library of Congress Catalog Card Number: 2001096788 ISBN: 0-8155-1451-4 Printed in the United States Published in the United States of America by Noyes Publications / William Andrew Publishing 13 Eaton Avenue Norwich, NY 13815 1-800-932-7045 www.williamandrew.com www.knovel.com 10 9 8 7 6 5 4 3 2 1 NOTICE To the best of our knowledge the information in this publication is accurate; however the Publisher does not assume any responsibility or liability for the accuracy or completeness of, or consequences arising from, such information. This book is intended for informational purposes only. Mention of trade names or commercial products does not constitute endorsement or recommendation for use by the Publisher. Final determination of the suitability of any information or product for use contemplated by any user, and the manner of that use, is the sole responsibility of the user. We recommend that anyone intending to rely on any recommendation of materials or procedures mentioned in this publication should satisfy himself as to such suitability, and that he can meet all applicable safety and health standards. v MATERIALS SCIENCE AND PROCESS TECHNOLOGY SERIES Series Editors Gary E. McGuire, Microelectronics Center of North Carolina Stephen M. Rossnagel, IBM Thomas J. Watson Research Center Rointan F. Bunshah, University of California, Los Angeles (1927–1999), founding editor Electronic Materials and Process Technology CHARACTERIZATION OF SEMICONDUCTOR MATERIALS, Volume 1: edited by Gary E. McGuire CHEMICAL VAPOR DEPOSITION FOR MICROELECTRONICS: by Arthur Sherman CHEMICAL VAPOR DEPOSITION OF TUNGSTEN AND TUNGSTEN SILICIDES: by John E. J. Schmitz CHEMISTRY OF SUPERCONDUCTOR MATERIALS: edited by Terrell A. Vanderah CONTACTS TO SEMICONDUCTORS: edited by Leonard J. Brillson DIAMOND CHEMICAL VAPOR DEPOSITION: by Huimin Liu and David S. Dandy DIAMOND FILMS AND COATINGS: edited by Robert F. Davis DIFFUSION PHENOMENA IN THIN FILMS AND MICROELECTRONIC MATERIALS: edited by Devendra Gupta and Paul S. Ho ELECTROCHEMISTRY OF SEMICONDUCTORS AND ELECTRONICS: edited by John McHardy and Frank Ludwig ELECTRODEPOSITION: by Jack W. Dini HANDBOOK OF CARBON, GRAPHITE, DIAMONDS AND FULLERENES: by Hugh O. Pierson HANDBOOK OF CHEMICAL VAPOR DEPOSITION, Second Edition: by Hugh O. Pierson HANDBOOK OF COMPOUND SEMICONDUCTORS: edited by Paul H. Holloway and Gary E. McGuire HANDBOOK OF CONTAMINATION CONTROL IN MICROELECTRONICS: edited by Donald L. Tolliver HANDBOOK OF DEPOSITION TECHNOLOGIES FOR FILMS AND COATINGS, Second Edition: edited by Rointan F. Bunshah HANDBOOK OF HARD COATINGS: edited by Rointan F. Bunshah HANDBOOK OF ION BEAM PROCESSING TECHNOLOGY: edited by Jerome J. Cuomo, Stephen M. Rossnagel, and Harold R. Kaufman HANDBOOK OF MAGNETO-OPTICAL DATA RECORDING: edited by Terry McDaniel and Randall H. Victora HANDBOOK OF MULTILEVEL METALLIZATION FOR INTEGRATED CIRCUITS: edited by Syd R. Wilson, Clarence J. Tracy, and John L. Freeman, Jr. HANDBOOK OF PLASMA PROCESSING TECHNOLOGY: edited by Stephen M. Rossnagel, Jerome J. Cuomo, and William D. Westwood HANDBOOK OF POLYMER COATINGS FOR ELECTRONICS, Second Edition: by James Licari and Laura A. Hughes HANDBOOK OF REFRACTORY CARBIDES AND NITRIDES: by Hugh O. Pierson HANDBOOK OF SEMICONDUCTOR SILICON TECHNOLOGY: edited by William C. O’Mara, Robert B. Herring, and Lee P. Hunt HANDBOOK OF SEMICONDUCTOR WAFER CLEANING TECHNOLOGY: edited by Werner Kern vi Series HANDBOOK OF SPUTTER DEPOSITION TECHNOLOGY: by Kiyotaka Wasa and Shigeru Hayakawa HANDBOOK OF THIN FILM DEPOSITION PROCESSES AND TECHNIQUES, Second Edition: edited by Krishna Seshan HANDBOOK OF VACUUM ARC SCIENCE AND TECHNOLOGY: edited by Raymond L. Boxman, Philip J. Martin, and David M. Sanders HANDBOOK OF VLSI MICROLITHOGRAPHY, Second Edition: edited by John N. Helbert HIGH DENSITY PLASMA SOURCES: edited by Oleg A. Popov HYBRID MICROCIRCUIT TECHNOLOGY HANDBOOK, Second Edition: by James J. Licari and Leonard R. Enlow IONIZED-CLUSTER BEAM DEPOSITION AND EPITAXY: by Toshinori Takagi MOLECULAR BEAM EPITAXY: edited by Robin F. C. Farrow NANOSTRUCTURED MATERIALS: edited by Carl. C. Koch SEMICONDUCTOR MATERIALS AND PROCESS TECHNOLOGY HANDBOOK: edited by Gary E. McGuire ULTRA-FINE PARTICLES: edited by Chikara Hayashi, R. Ueda and A. Tasaki WIDE BANDGAP SEMICONDUCTORS: edited by Stephen J. Pearton Related Titles ADVANCED CERAMIC PROCESSING AND TECHNOLOGY, Volume 1: edited by Jon G. P. Binner CEMENTED TUNGSTEN CARBIDES: by Gopal S. Upadhyaya CERAMIC CUTTING TOOLS: edited by E. Dow Whitney CERAMIC FILMS AND COATINGS: edited by John B. Wachtman and Richard A. Haber CORROSION OF GLASS, CERAMICS AND CERAMIC SUPERCONDUCTORS: edited by David E. Clark and Bruce K. Zoitos FIBER REINFORCED CERAMIC COMPOSITES: edited by K. S. Mazdiyasni FRICTION AND WEAR TRANSITIONS OF MATERIALS: by Peter J. Blau HANDBOOK OF CERAMIC GRINDING AND POLISHING: edited by Ioan D. Marinescu, Hans K. Tonshoff, and Ichiro Inasaki HANDBOOK OF HYDROTHERMAL TECHNOLOGY: edited by K. Byrappa and Masahiro Yoshimura HANDBOOK OF INDUSTRIAL REFRACTORIES TECHNOLOGY: by Stephen C. Carniglia and Gordon L. Barna MECHANICAL ALLOYING FOR FABRICATION OF ADVANCED ENGINEERING MATERIALS: by M. Sherif El-Eskandarany SHOCK WAVES FOR INDUSTRIAL APPLICATIONS: edited by Lawrence E. Murr SOL-GEL TECHNOLOGY FOR THIN FILMS, FIBERS, PREFORMS, ELECTRONICS AND SPECIALTY SHAPES: edited by Lisa C. Klein SOL-GEL SILICA: by Larry L. Hench SPECIAL MELTING AND PROCESSING TECHNOLOGIES: edited by G. K. Bhat SUPERCRITICAL FLUID CLEANING: edited by John McHardy and Samuel P. Sawan vii Contributors Karl T. Aust Department of Metallurgy and Materials Science University of Toronto Toronto, Ontario Canada Ulrich Brossmann Institut für Technische Physik Technische Universität Graz A-8010 Graz, Austria Gan-Moog Chow Department of Materials Science National University of Singapore Kent Ridge, Singapore Philip Clapp Institute of Materials Science University of Connecticut Storrs, CT Uwe Erb Department of Metallurgy and Materials Science University of Toronto Toronto, Ontario Canada Jürgen Eckert IFW Dresden Institute of Metallic Materials Dresden, Germany Hans J. Fecht Center for Energy Technology Universitat Ulm Ulm, Germany Joanna Groza Department of Chemical Engineering and Materials Science University of California Davis, CA viii Contributors Akihisa Inoue Institute for Materials Research Tohoku University Sendai, Japan Carl C. Koch Materials Science and Engineering Department North Carolina State University Raleigh, NC Lynn K. Kurihara Naval Research Laboratory Washington, D.C. Maggy L. Lau Department of Chemical and Biochemical Engineering and Materials Science University of California Irvine, CA Enrique J. Lavernia Department of Chemical and Biochemical Engineering and Materials Science University of California Irvine, CA Akihiro Makino Central Research Laboratory Alps Electric Co. Ltd. Nagaoka, Japan Gino Palumbo Integran Technologies, Inc. Toronto, Ontario Canada Hans-Eckhardt Schaefer Institut für Theoretische und Angewandte Physik Universität Stuttgart D-70569 Stuttgart, Germany Michel Trudeau Hydro-Quebec Research Institute Varennes, Quebec Canada Raphael Tsu Department of Electrical and Computer Engineering University of North Carolina Charlotte, NC Julia R. Weertman Department of Materials Science and Engineering Northwestern University Evanston, IL Roland Würschum Institut für Technische Physik Technische Universität Graz A-8010 Graz, Austria Qi Zhang Department of Electrical and Computer Engineering University of North Carolina Charlotte, NC ix Preface INTRODUCTION Nanostructure science and technology has become an identifiable, if very broad and multidisciplinary, field of research and emerging applications in recent years. It is one of the most visible and growing research areas in materials science in its broadest sense. Nanostructured materials include atomic clusters, layered (lamellar) films, filamentary structures, and bulk nanostructured materials. The common thread to these various material forms is the nanoscale dimensionality, i.e., at least one dimension less than 100 nm, more typically less than 50 nm. In some cases, the physics of such nanoscale materials can be very different from the macroscale properties of the same substance. The different, often superior, properties that can then occur are the driving force behind the explosion in research interest in these materials. While the use of nanoscale dimensions to optimize properties is not new, as will be outlined below, the present high visibility and definition of the field is mainly attributable to the pioneering work of Gleiter and coworkers in the early 1980s. [1] They synthesized nanoscale grain size materials by the in situ consolidation of atomic clusters. The studies of clusters preceded the work by researchers such as Uyeda. [2] The International Technology Re- search Institute, World Technology Division (WTEC), supported a panel x Preface study of research and development status and trends in nanoparticles, nanostructured materials, and nanodevices during 1996–1998. The main results of this study have been published. [3] This report attempted to cover the very broad field of nanostructure science and technology and included assessments of the areas of synthesis and assembly, dispersions and coatings, high surface area materials, functional nanoscale devices, bulk nanostruc- tured materials, and biologically related aspects of nanoparticles, nanostruc- tured materials, and nanodevices. A conclusion of the report is that while many aspects of the field existed well before it was identified as a field in the last decade, three related scientific/technological advances have made it a coherent area of research. These are: 1. New and improved synthesis methods that allow control of the size and manipulation of the nanoscale “building blocks.” 2. New and improved characterization tools for study at the nanoscale (e.g., spatial resolution, chemical sensitivity). 3. Better understanding of the relationships between nano- structure and properties and how these can be engineered. With the recent intense interest in the broad field of nanostructure science and technology, a number of books, articles, and conference proceedings have been published. A partial listing of these publications is given in the bibliography, starting with the review of Gleiter in 1989. The justification for yet another book in this expanding field is two-fold. Since many areas of the field are moving rapidly with increased understanding from both experiment and simulation studies, it would appear useful to record another “snapshot” of the field. It will be assumed that by the time of publication certain information may become obsolete, but at least most of the background will still be useful to researchers and students. Second, since the field is so broad, spanning the study of atomic clusters to bulk, and materials from biological to metallic structures, the book has been designed to focus mainly on those areas of synthesis, characterization, and properties relevant to applications that require bulk, and mainly inorganic materials. An excep- tion is the article by Tsu on electronic and optoelectronic materials. Before a brief description of the chapters and organization of the book is presented, a historical perspective will be given to suggest how the field has developed and what new information has been provided by reaching the limit of the nanoscale. Preface xi HISTORICAL PERSPECTIVE Nanoscale microstructural features are not new, either in the natural world or in materials engineering. There are examples of nanoscale ferromagnetic particles found in microorganisms, e.g., 50 nm Fe 3 O 4 in the organism A. magnetotactum. [4] A number of examples exist of improve- ment in mechanical properties of structural materials when a fine micro- structure was developed. Early in the last century, when “microstructures” were revealed primarily with the optical microscope, it was recognized that refined microstructures, for example, small grain sizes, often provide attractive properties such as increased strength and toughness in structural materials. A classic example of property enhancement due to a refined microstructure—with features too small to resolve with the optical micro- scope—was age-hardening of aluminum alloys. The phenomenon, discov- ered by Alfred Wilm in 1906, was essentially explained by Merica, Waltenberg, and Scott in 1919, [5] and the microstructural features respon- sible were first inferred by the x-ray studies of Guinier and Preston in 1938. With the advent of transmission electron microscopy (TEM) and sophisti- cated x-ray diffraction methods, it is now known that the fine precipitates responsible for age-hardening, in Al-4%Cu alloys, for example, are clusters of Cu atoms—Guinier-Preston (GP) Zones—and the metastable partially coherent θ´ precipitate. [6][7] Maximum hardness is observed with a mixture of GPII (or θ´´ , coarsened GP zones) and θ´, with the dimensions of the θ´ plates, typically about 10 nm in thickness by 100 nm in diameter. Therefore, the important microstructural feature of age-hardened aluminum alloys is nanoscale. Critical length scales often determine optimum properties which are structure sensitive. Mechanical properties such as strength and hardness are typical and as above, microstructural features such as precipitates or dispersoids are most effective when their dimensions are nanoscale. In ferromagnetic materials, the coercive force has been found to be a maximum if spherical particles (e.g., Fe 3 C in Fe) which act as domain wall pinners have a diameter about equal to the domain wall thickness, i.e., about 50 nm. [8] Similarly, in type II superconductors, it has been found that fluxoid pinning, which determines the magnitude of the critical current density, is most effective when the pinning centers typically have dimensions of the order of the superconducting coherence length for a given material. For the high field superconductors, the coherence length is usually about 10–20 nm and indeed the commercial superconductors have pinning centers that approximate xii Preface these dimensions. In Nb 3 Sn, the grain boundaries are the major pinning sites and optimum critical current densities are obtained when the grain sizes are about 50 nm. [9] Many other examples could be given of the long term use of nanoscale materials in fields such as catalysis. ORGANIZATION The scientific/technological advances that have focused the field into a broad but coherent field were given above. In this book, the new or improved synthesis methods that are one of the cornerstones of the field will be reviewed in Part I. In Part II, selected properties of nanostructured materials will be covered. Potential applications of nanostructured materials will be described as appropriate throughout the book. In Ch. 1, Chow and Kurihara present an overview of the chemical synthesis and processing of nanostructured particles, films, and coatings. This includes particles from all materials classes, that is metals, ceramics, organic materials, etc. The chemical methods described include aqueous, non-aqueous, sonochemical, precursor, organometallic, hydrolysis, hydro- thermal, and sol-gel methods. Other methods discussed are host-derived hybrid materials, surfactant membrane mediated synthesis, and a variety of films and coatings. Lau and Lavernia describe the thermal spray processing of nanostruc- tured materials. This method has the potential for early commercialization of coatings with nanocrystalline microstructures and superior properties. The chapter provides an overview of thermal sprayed coatings produced from nanocrystalline feedstock powders. The various routes for producing the nanocrystalline feedstock powders are discussed. The structure and prop- erties of the nanocrystalline coatings are considered in the light of retention of a nanoscale microstructure during processing. A review of theoretical models to predict and optimize the thermal spraying parameters for opti- mized coatings is presented. Fecht considers in his chapter the preparation of nanostructured materials and composites by solid-state processing methods which involve plastic mechanical deformation. The use of ball-milling of powders has become a popular method of producing nanocrystalline materials because of the simplicity of the equipment and the possibility to scale-up from laboratory to tonnage quantities of material. Fecht describes the use of mechanical attrition for production of nanocrystalline materials in a wide variety of [...]... Chemical Synthesis and Processing of Nanostructured Powders and Films Gan-Moog Chow* and Lynn K Kurihara** 1.0 INTRODUCTION The performance of materials depends on their properties The properties in turn depend on the atomic structure, composition, microstructure, defects, and interfaces, which are controlled by thermodynamics and kinetics of the synthesis A current paradigm of synthesizing and processing... as the structure and properties of the electrodeposited nanostructured materials Comparisons are presented for the structure and properties with those of nanostructured materials made by other methods Examples of industrial applications of electrodeposited nanostructured materials are given Clapp reviews the growing area of computer simulation of nanomaterials This comprises “virtual processing, so... repulsion and the attractive van der Waals forces The DLVO theory (Derjaguin, Landau, Verwey, and Overbeek) describes the effects of attraction and repulsion of particles as a function of separation distance.[18] On the DLVO plot of potential energy vs the separation distance of particles, there exists a positive potential energy peak, which separates the negative potential energy of primary minimum and. .. Carolina October, 2001 Contents Part I Processing 1 Chemical Synthesis and Processing of Nanostructured Powders and Films 3 Gan-Moog Chow and Lynn K Kurihara 1.0 INTRODUCTION 3 2.0 PARTICLES 5 2.1 Nucleation and Growth 5 2.2 Stable Dispersion and Agglomeration 6 2.3 Metals, Intermetallics, Alloys, and Composites 10 2.4 Ceramics 20 2.5 Host-Derived... 179 Uwe Erb, Karl T Aust, and Gino Palumbo 1.0 INTRODUCTION 179 2.0 SYNTHESIS OF NANOSTRUCTURED MATERIALS BY ELECTRODEPOSITION 179 3.0 STRUCTURE OF NANOCRYSTALLINE METAL ELECTRODEPOSITS 183 4.0 PROPERTIES 187 4.1 Mechanical Properties 187 4.2 Corrosion Properties 193 4.3 Hydrogen Transport and Activity 197 4.4 Magnetic Properties 200... Conventional Solidification and Devitrification of Bulk Samples 458 3.3 Mechanically Attrited Powders 468 4.0 MECHANICAL PROPERTIES AT ROOM AND ELEVATED TEMPERATURES 482 4.1 Al-Based Two-Phase Nanostructured Alloys 483 4.2 Mg-Based Amorphous and Nanostructured Alloys 488 4.3 Zr-Based Alloys 494 4.4 Mechanically Attrited Composites 502 5.0 SUMMARY AND OUTLOOK ... W., Hu, E., and Roco, M C., (eds.), Nanostructure Science and Technology, Kluwer Academic Publishers, Dordrecht, Netherlands (1999) 4 Kirschvink, J L., Koyayashi-Kirschvink, A., and Woodford, B J., Proc Nat’l Acad Sci., USA, 89:7683–7687 (1992) 5 Mehl, R F., and Cahn, R W., Historical Development, Physical Metallurgy, 3rd ed., pp 1–35, North Holland (1983) 6 Silcock, J M., Heal, T J., and Hardy, H... SynthesisProperties-Appplications, Kluwer Press, Dordrecht, Netherlands (1994) Siegel, R W., Nanophase Materials, in: Encyclopedia of Applied Physics, (G L Trigg, ed.), 11:1–27, VCH, Weinheim (1994) Gleiter, H., Nanostructured Materials: State of the Art and Perspectives, NanoStructured Materials, 6:3 (1995) Edelstein, A S., and Cammarata, R C., (eds.), Nanomaterials: Synthesis, Properties, and Appplications, Institute of Physics,... T., and Stoffers, R C., Trans ASM, 62:257 (1969) 9 Scanlan, R M., Fietz, W A., and Koch, E F., J Appl Phys., 46:2244 (1975) xvi Preface BIBLIOGRAPHY Gleiter, H., Nanocrystalline Materials, Progress in Materials Science, 33:223–315 (1989) Siegel, R W., Nanostructured Materials—Mind Over Matter, Nanostructured Materials, 3:1 (1993) Hadjipanayis, G C., and Siegel, R W., Nanophase Materials: SynthesisProperties-Appplications,... assembly of atoms and particles, from the atomic or molecular scale to the macroscopic scale Nanostructured materials, often characterized by a physical dimension of 1–100 nm (such as grain size) and a significant amount of surfaces and interfaces, have been attracting much interest because of their demonstrated or anticipated unique properties compared to conventional materials Nanostructured materials . R. W., Nanophase Materials: Synthesis- Properties- Appplications, Kluwer Press, Dordrecht, Netherlands (1994) Siegel, R. W., Nanophase Materials, in: Encyclopedia of Applied Physics, (G. L. Trigg,. Nanostructured Materials: State of the Art and Perspectives, NanoStructured Materials, 6:3 (1995) Edelstein, A. S., and Cammarata, R. C., (eds.), Nanomaterials: Synthesis, Properties, and Appplications,. theoretical models to predict and optimize the thermal spraying parameters for opti- mized coatings is presented. Fecht considers in his chapter the preparation of nanostructured materials and composites by