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Innovative Processing and Synthesis of Ceramics, Glasses, and Composites VII Proceedings of the Ceramic Matrix Composites Symposium at the 105th Annual Meeting ofThe American Ceramic Society, April 21-30, 2003, in Nashville, Tennessee.

Edited by

J.R Singh Argonne National Laboratory

Narottam P. Bansal National Aeronautics and Space Administration Glenn Research Center

Published by The American Ceramic Society 735 Ceramic Place Westerville, Ohio 43081 www.ceramics.org

Proceedings of the Ceramic Matrix Composites Symposium at the 105th Annual Meeting ofThe American Ceramic Society, April 27-30, 2003, in Nashvillejennessee.

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tents Preface ix

Solution Method and Nanocrystalline Powders Use of Complexed Ammonia Precursors in Synthesizing Layered Nitride Compounds 3

K. Scott Weil and Prashant N. Kumta

Preparation of Nanocrystalline Silicon Carbide Powders by Carbothermal Reduction

Zhe Cheng, Michael D. Sacks, Chang-An Wang, and Zhaohui Yang

Preparation of Nanocrystalline Hafnium Carbide Powders by Carbothermal Reduction

Chang-An Wang, Michael D. Sacks, and Zhaohui Yang

Preparation of Nanocrystalline Zirconium Carbide Powders by Carbothermal Reduction

Anubhav Jain, Michael D. Sacks, and Chang-An Wang

Polymer Precursor and Sol-Gel Technology Polymer-Derived Ceramic foams with a Zeolitic Surface by Supported Crystallization . , 49

M. Scheffler, J. Zeschky, A. Zampieri, R. Herrmann, W Schwiegen F. Scheffler, and P Greil

Boron Nitride Fibers from Borylborazine Precursors 61 B.Toury, S. Duperrier, D. Cornu, S. Bernard, F. Chassagneux, S. Parola, and R Miele

Effect of Oxygen Atmosphere on the Morphology of LiTa03 Thin Films Prepared from Polymeric Precursor Method 69

A.H.M. Gonzalez, A.Z. Simöes, M.A. Zaghete, and JAVerela

Characterization of SiC Fiber Derived from Polycarbosilane... 77 Doh Hyung Riu, Young Hee Kim, Dong Geun Shin, and Hyung Rae Kim

v

15

27

37

Formation of Porous Articles with Ordered Capillary Structure by Alginate Sol-Gel Technique 87

Berthold Liebig and Jan. A. Puszynski

Microwave Processing Lower Dielectric Constant Ni-Zn Ferrites Obtained by Systematic Use of Microwave Sintering 101

Purushotham Yadoji, Ramesh Peelamedu, Dinesh Agrawal, and Rustum Roy

Novel Processing Methods Strain-Induced Forming of Ceramics Without the Application of External Pressure 115

Stephen J. Lombarde Rajesh V Shende, Chang Soo Kim, and Robert A. Winholtz

Alternatives to Hot-Pressing Silicon Nitride/Boron Nitride Fibrous Monolith Composites 123

Emily Pickens and Rodney Trice

Improving Binder Distribution in Extruded Ceramic Paste . . . 135 Justin Clark Tammy McCoy, Kevin Hurysz, and Joe Cochran

Supercritical Extraction of Binder from Green Ceramic Components 145

Stephen J, Lombardo, Rajesh V. Shende, and Trent R. Redfeam

Effects of Die Geometry and Paste Rheology on Extrusion Pressure 153

Raymond Oh, Joe Cochran, and Kevin Hurysz

Bulk Shear Stress Modeling of Pastes made from Low Maximum Solids Content Raw Materials 165

K.M. Hurysz and J.K. Cochran

Functionally Graded Materials Laminated WC-Co Composites for Tribological Applications.. 179

Kevin M. Fox, J.R. Hellmann, M.R Amateau, H. Izui.W. Fu, and RH. Cohen

Laminated Object Manufacturing Solid Freeform Fabrication of PZT Ceramics via an Automated Tape Laminated Object Manufacturing System 193

Barry A. Bender Roy Rayne, Carl Wu, Chulho Kim, and R.W Bruce

VI

Thin Films and Coatings Optical Properties of Mg Doped LiNb03 Thin Films Grown by Polymeric Precursor Method 207

A.Z. Sirnoes , A.H.M. Gonzalez, M. Cilense, M.A. Zaghete, F. Moura, A. Ries, JAVarela, and B.D. Stojanovic

Combustion Chemical Vapor Deposition of Alumina and Alumina-Chromia Coatings on Silica 217

S.N. Dunham, J.M. Hampikan, M.S. Mclntosh

Mechanical Behavior of Si3N4 Substrates with Environmental Barrier Coatings 225

K. Sharma, RS. Shankan and J.R Singh

Synthesis and Characterization Sol-Gel Synthesis and Electrical Properties of YCo03^ 235

O.S. Buassi-Monroy, C.C. Luhrs, A. Châvez-Châvez, and C.R. Michel

Synthesis and Electrical Properties of Super Ionic Conductor of Sr-Doped or Ba-Doped Laln03 245

Chen-Feng Kao and Chieng-Teh Wu

Synthesis and Characterization byTEM and HRTEM of Nanocrystalline CuO and Cu20 Obtained by Precipitation Method 259

C.R. Michel, C.H. Rios-Reyes, and C.C. Luhrs

Synthesis of Cordierite Ceramics with a Mixture of Kyanite andTalc 269

Ivan Vemet-Patifio, Herberto Balmori-Ramfrez, Carlos Gomez-Yanez, and Richard C. Bradt

Diamond Films Effect of Pulsed Methane Flow on Nanostructured Diamond Films Synthesized by Microwave Plasma CVD 283

V. Shanov, R Ramamurti, and R N. Singh

Electrophoresis Preparation of SrBi2Ta209 Ferroelectric Thick Films by Electrophoretic Deposition Using Aqueous Suspensions 297

S.M. Zanetti, JAVarela, ER. Leite, and E. Longo

vii

Processing-Microstructure-Property Relationships Sintering,Grain Growth, and Phase Composition of Gd203-Stabilized Z r0 2 Powders 311

J.R. Gross, M.N. Rahaman, and &E. Dutton

Influence of the Addition of Sm on the Microstructure and Magnetic Properties of Ni05Zn05Fe2xSmxO4 Ferrites 321

A.C.F.M. Costa , M.R. Morelli, and R.H.G.À. Kiminami

Index 333

viu

face This volume contains papers presented at the symposium on Innovative Processing and Synthesis of Ceramics, Glasses, and Composites held during the 105th Annual Meeting and Exposition of The American Ceramic Society (ACerS), April 27-30,2003 in Nashville,Tennessee.This symposium provided an international forum for scientists and engineers to discuss all aspects of processing and synthesis of ceramics, glasses, and composites. A total of 98 papers, including invited talks, oral presentations, and posters, were presented from 18 countries (the United States, Belgium, Brazil, Canada, China, France, Germany, Iran, Israel, Italy, Japan, Korea, Mexico, Spain, Sweden, Switzerland, Taiwan, and the United Kingdom). The speakers rep-resented universities, industry, and research laboratories.

This volume contains 29 invited and contributed papers, all peer-reviewed according to ACerS procedures.The latest developments in processing and characterization are covered including solution method and nanocrystalline powders, polymer precursor and sol-gel technology, microwave processing, novel processing methods, functionally graded materials, laminated object manufacturing, thin films and coatings, synthesis and characterization, dia-mond films, electrophoresis, and processing-microstructure-property rela-tionships. All of the most important aspects necessary for understanding and further development of ceramic processing and characterization are discussed.

The organizers are grateful to all participants and session chairs for their time and effort, to authors for their timely submissions and revisions of their manuscripts, and to reviewers for their valuable comments and sug-gestions. Without the contributions of all involved, this volume would not have been possible. Financial support from ACerS is gratefully acknowl-edged. Thanks are due to the staff of the Meetings and Publications Departments of ACerS for their tireless efforts. Especially, we greatly appre-ciate the helpful assistance and cooperation of Greg Geiger throughout the production process of this volume.

We hope that this volume will serve as a useful reference for professionals working in the field of synthesis and processing of ceramics, glasses, and composites.

J.R Singh

Narottam R Bansal

IX

Solution Method and Nanociystalline Powders

USE OF COMPLEXED AMMONIA PRECURSORS IN SYNTHESIZING LAYERED NITRIDE COMPOUNDS

K. Scott Weil Prashant N. Kumta Department of Materials Science Department of Materials Science and Pacific Northwest National Laboratory Engineering Richland, WA 99352, U.S.A. Carnegie Mellon University

Pittsburgh, PA 99352, U.S.A.

ABSTRACT Ammonia-complexed precursors have been used by the authors to synthesize

a number of new layered transition metal nitride compounds, including &WN2, CoWN2, (Ni0.8Moo.2)MoN2, and FeZrN2. The precursors are first prepared by complexing a stoichiometric mixture of metal chlorides dissolved in acetonitrile with ammonia and are then heated at moderate temperature in flowing ammonia to form the layered nitride of interest. As will be discussed, the key reactions responsible for this transformation have been identified by tracking the thermolysis of the precursor as a function of temperature using a series of analytical techniques.

INTRODUCTION Ternary nitrides are a relatively unexplored class of materials. One of the

primary reasons for this is the difficulty in synthesizing these compounds by the standard high temperature solid state approach of mechanically mixing the requisite binary nitride powders, heating at elevated temperature, and grinding the product in repeated fashion until a single phase material is obtained. The optimal synthetic conditions of ternary nitrides are often bounded by the low diffusion rate of nitrogen at low temperatures and by the inherent instability of these compounds at high temperatures. Studies by Wintenberger et al. [I], Bern et al. [2], and Elder et al. [3] however have demonstrated the feasibility of using multicomponent oxides and metalloorganics as precursors to form ternary nitride compounds at much lower temperatures than can be achieved with solid state synthesis.

Recently, we have developed an alternative solution-based synthesis approach that offers the compositional flexibility necessary to explore a given region of compositional space in at least one particular layered nitride system, CrWN2 [4].

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