25th Annual
`Conference on
`Composites,
`Advanced
`Ceramics,
`Materials, and
`Structures: A
`
`Edited by Mrityunjay Singh
`and Todd Jessen
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`GE-1026.001
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`TA 418.9 C6 C645 2001 PT.A ENGIN
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`THE UNIVERSITY OF TEXAS AT AUSTIN
`THE GENERAL LIBRARIES
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`GE-1026.003
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`w;11.1931w11m4;1u1~1T:1t§"iiWk·M·''"B·
`
`W. Paul Holbrook, Executive Director
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`GE-1026.004
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`I
`
`Ceramic Engineering & Science Proceedings ~~([~~fr...i~Lssue 3~
`
`25th Annual
`Conference on
`Composites,
`Advanced
`Ceramics,
`Materials, and
`Structures: A
`
`Mrityunjay Singh
`Todd Jessen
`Editors
`
`January 21-27, 200 I
`Cocoa Beach, Florida
`
`Published by
`The Arflerican Ceramic Society
`735 Ceramic Place
`Westerville, OH 43081
`
`© 200 I The American Ceramic Society
`ISSN 0 196-6219
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`GE-1026.005
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`Copyright 200 I ,The American Ceramic Society.All rights reserved
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`Statements of fact and opinion are the responsibility of the authors alone and do not imply
`an opinion on the part of the officers, staff, or members ofThe American Ceramic Society.
`The American Ceramic Society assumes no responsibility for the statements and opinions
`advanced by the contributors to its publications or by the speakers at its programs.
`Registered names and trademarks, etc., used in this publication, even without specific indica(cid:173)
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`
`Cover photo, "(A) The cross-section and (B) fracture surface of SA-Tyrannohex" is cour(cid:173)
`tesy ofT. Ishikawa, M. Sato, S. Kajii, YTanaka, and M. Suzuki and appears as figure 6b in their
`paper "A Thermally Conductive SiC-Polycrystalline Fiber and Its Fiber-Bonded Ceramic,''
`which begins on page 471.
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`GE-1026.006
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`Contents
`25th Annual Conference on Composites, Advanced
`Ceramics, Materials, and Structures: A
`
`Preface .......................................................... xiv
`
`Product Development and Commercialization
`
`Commercial Applications for Advanced Ceramics
`in Diesel Engines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
`WF. Mandler; Jr: and T.M.Yonushonis
`
`Ceramic Matrix Composites from Space to Earth:
`The Move from Prototype to Serial Production .....•..... I I
`R. Kochendorfer
`
`Application of Tyranno TM Fiber/Si-Ti-C-0 Matrix
`Composite to the Thermal Protection System of
`the Japanese Hope-X Space Vehicle . . . . . . . . . . . . . . . . . . . 23
`T. Ogasawara andT. Ishikawa
`
`Will Pigs Fly before Ceramics. Do? . . . . . . . . . . . . . . . . . . . . 3 I
`L.C.Veitch and WS. Hong
`
`Structural Ceramics with Complex Shape-Forming Methods
`G.H. Wroblewska
`
`. .43
`
`RBAO: From Materials Development to
`Commercial Components . . . . . . . . . . . . . . . . . . . . . . . . . . 5 I
`R. Janssen, N. Claussen, S. Scheppokat, and M. Roeger
`
`Molybdenum Disilicide Materials for Glass
`Melting Se~sor Sheaths . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
`j.J. Petrovic, R.G. Castro, RU.Vaidya, M.I. Peters, D. Mendoza, R.C. Hoover;
`and D.E. Gallegos
`
`Silicon Nitride Ceramics for Valve-Train Applications
`in Advanced Diesel Engines . . . . . . . . . . . . . . . . . . . . . . . . . 65
`S.K. Lee, P.H. McCluskey, M.J. Readey. H.-T. Lin, and A.A.Wereszczak
`
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`Ceramic Coatings for Cylinder Liners in Advanced
`Combustion Engines, Manufacturing Process,
`and Characterization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 5
`M. Buchmann and R. Gadow
`
`Porous Ceramic Preforms for Local Reinforcement
`of Light Metal Engine Components . . . . . . . . . . . . . . . . . . . 87
`l.T Lenke
`Cermet Tool and Die Materials from Metal
`Coated Powders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9 5
`A. Sherman, G. Smith, D. Baker, and R.Toth
`
`Novel Real-Time Method for Measuring the
`Densification Rate of Carbon-Carbon Fiber-Matrix
`Composites and Other Articles . . . . . . . . . . . . . . . . . . . . . I 03
`I. Golecki and D. Narasimhan
`
`Optimizations of Ceramic Core Manufacture Using
`Real-Time Monitoring and Process Design . . . . . . . . . . . . . . I I 5
`B.A. McCalla, S.O. Matthews, and M.J. Bevis
`
`Thermomechanical Property Characterization
`
`Mechanical Properties of Silicon Carbide Ceramics
`Densified with Rare-Earth Oxide and Alumina Additions ... . 127
`Y. Zhou, K. Hirao, M.Toriyama,Y.Yamauchi, and S. Kanzaki
`
`Creep-Resistant Biomorphic Silicon-Carbide
`Based Ceram.ics
`. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . I 3 5
`J. Martinez-Fernandez, F.M.Varela-Feria, S. L6pez-Pombero,
`A.R. de Arellano-Lopez, and M. Singh
`Creep Mechanisms of Alumina/Si( Nanocomposites ....... . 145
`M. Sternitzke and H. Hubner
`Mechanical Behavior of Er20 3 Single Crystals ........... . 151
`J.J. Petrovic, A.A. Sharif, A.M. Kukla, R.S. Romero,
`D. Mendoza, and F.M. Pitek
`
`Long-Term Tensile Creep Behavior of Highly
`Heat-Resistant Silicon Nitride for Ceramic Gas Turbines .... I 59
`T. Ohji
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`Tensile Creep in the Next-Generation Silicon Nitride ...... . 167
`F. Lofaj, S.M. Wiederhorn, G.G. Long, and P.R. Jemian
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`VI
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`Evaluation of Creep Property of AS800 Silicon Nitride
`from As-Processed Surface Regions . . . . . . . . . . . . . . . . . . . 17 5
`H.T Lin, S.B. Waters, K.L. More, J. Wimmer; and C.W. Li
`
`On the Mechanism of High-Temperature Strength
`Degradation of Low-Doped HIPed Silicon Nitride
`by ln-Deptfl TEM-SEM Investigation . . . . . . . . . . . . . . . . . . 183
`R. Pompe, M. Halvarsson, K. Kishi, and R. Lundberg
`Nondiamond Finishing of Silicon Nitride for
`Low-Friction against Steel . . . . . . . . . . . . . . . . . . . . . . . . . 191
`G.M. Crosbie, R.L. Allor; A. Gangopadhyay, D.G. McWatt, and P.A. Willermet
`
`Influence of Microstructure and Grain Boundary
`Phase on Tribological Properties of Si3N4 Ceramics ....... . 197
`H. Hyuga, S. Sakaguchi, K. Hirao,Y.Yamauchi, and S. Kanzaki
`
`Effect of Microstructure on Wear Behavior
`of Silicon Nitride . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 203
`M. Nakamura, K. Hirao, S. Sakaguchi,Y.Yamauchi, and S. Kanzaki
`
`Production and Characterization of Hexagonal
`Ceramic Packing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 209
`RT Hernandez Lopez, E. Rocha Rangel. and M. Rodriguez Cruz
`Mechanical Properties of Boron Carbide Ceramics ....... . 2 I 5
`S.Yamada, S. Sakaguchi, K. Hirao,Y.Yamauchi, and S. Kanzaki
`Oxidation of ZrB2-SiC . . . . . . . . . . . . . . . . . . . . . . . . . . . . 221
`E.J. Opila and M.C. Halbig
`
`Indentation Damage of Silicon Carbide Deposited
`on Different Substrates . . . . . . . . . . . . . . . . . . . . . . . . . . . 229
`J.Y. Park,W.-J Kim, M.Y. Lee,J.1. Kim, and G.W Hong
`
`Behavioral Modeling and Life Prediction
`
`Thermal Imaging Detection and Characterization
`of Normal Cracks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 237
`J.G. Sun, C. Deemer; S. Erdman, and W.A. Ellingson
`
`An Analysis of Crack-Growth Resistance of
`Microcracking Brittle Solids and Composites ........ . .. . 245
`S.B. Biner
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`VII
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`Modeling of Fracture Resistance of a Ceramic
`Composite at Elevated Temperatures ..... .
`E.T Park and R.N. Singh
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`... 253
`
`Design Issues for Variable Mixed Mode I/II Testing ........ 261
`C.B. Milz, J. Chapa-Cabrera, and I.E. Reiman is
`Influence of Crack Path on Crack Resistance
`of Brittle Matrix Composites . . . . . . . . . . . . . . . . . . . . . . . 269
`S. Wu, B.R Patterson, E.R. Fuller Jr., and M.K. Ferber
`
`Compliance and Crack-Bridging Analysis for
`Alumina Ceramics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 277
`M.E. Ebrahimi, J. Chevalier, and G. Fantozzi
`
`Slow Crack Growth of Sapphire . . . . . . . . . . . . . . . . . . . . . 289
`J. Salem, A. Calomino, R. Allen, and L. Powers
`Microscopic Simulation of Microcrack Propagation
`in Al 20 3-Zr02 Ceramic Composites . . . . . . . . . . . . . . . . . . . 299
`J. Cao,Y. Sakaida, and M. Matsui
`
`Crack-Growth Observations in a Graded
`Composite Using PSMI . . . . . . . . . . . . . . . . . . . . . . . . . . . 307
`E. D. Steffler; J.K. Wright, and W .E. Windes
`
`Impact and Erosion Testing
`
`Digital Signal Processing Algorithms Applied to
`Acoustic Impact Testing of Advanced Ceramics ........... 315
`S.R. Short and S. Chen
`
`Damage Evolution and Mechanical Properties of
`Woven Glass Fiber/Polymer Composites under
`Low-Velocity Impact . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 323
`T.-W Kim and S.-S Hwang
`
`Processing Aluminum Oxide/Titanium Diboride
`Composites for Penetration Resistance . . . . . . . . . . . . . . . . 331
`G. Gilde, J.WAdams, M. Burkins, M. Sutaria, M.J. Rigali, and L. Prokurat Franks
`
`Sand Erosion of Alumina and Silicon Nitride Ceramics
`at Elevated Temperatures . . . . . . . . . . . . . . . . . . . . . . . . . 343
`T Senda, K.Arai,Y. Sasaki, A. Matsubara, and M.Ajima
`
`VIII
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`Ceramic Matrix Composites
`
`Fibers and lnterphases
`
`A Statistical Upper Limit Strength for Ceramic
`fiber Bundles . . . . . . . . . . . . . . . . . . . . . . . . . • . . . . . . . 355
`T. Morimoto
`The Effect of Diameter Variation along a Fiber on
`the Determination of Fiber Strengths and the
`Parameters of Their Distribution . . . . . . . . . . . . . . . . . . . . 363
`E. Lara-Curzio and D. Garcia Jr:
`
`Design of Fiber/Coating Systems for High Strength
`in Ceramic Matrix Composites . . . . . . . . . . . . . . . . . . . . . . 371
`z. Xia and WA Curtin
`Process-Induced Carbon Sub-Layer in SiC/BN/SiC
`Composites: Characterization and Consequences ......... 379
`L.U.J.T. Ogbuji, D.R. Wheeler; and TR. McCue
`
`Progress on BN and Doped-BN Coatings on
`Woven Fabrics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 389
`F.I. Hurwitz, P.V. Chayka, and J.M. Scott
`
`Development of Si-M-C-(0) Tyranno Fiber Containing
`a Small Amount of Sol-Gel-Derived Oxide .............. 399
`K. Kumagawa, H.Yamaoka, M. Shibuya, and TYamamura
`
`Structural Properties and Thermomechanical
`Behavior of New CVD-SiC Monofilaments .........•..... 407
`G. Chollon and R. Naslain
`
`Effect of Microstructure on the Creep Behavior of
`a Directionally Solidified YAG/Alumina Eutectic Fiber ...... 415
`J.E. Pitchford, F. Deleglise, M.H. Berger; AR. Bunsell, and W.J. Clegg
`Creep of Directionally Solidified Al 20/Er3Al 50 12 Fibers
`with Hypo-Eutectic Composition . . . . . . . . . . . . . . . . . . . . 42 I
`J. Martinez Fernandez and A Sayir
`
`Exploration of Reliable Oxide Fiber Testing Procedures
`and Development of a Multicontinuum Based
`Creep Analysis Module . . . . . . . . . . . . . . . . . . . . . . . . . . . 429
`D. Pai, Y Acharya, S. Yarmolenko, J. Sankar; J. Lua, and L. Zawada
`
`IX
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`Fiber-Reinforced Composites: C and SiC Fibers
`
`Composite Processing
`
`Cost Effective Processing of CMC Composites by
`Melt Infiltration (LSI-Process) . . . . . . . . . . . . . . . . . . . . . . 443
`W. Krenkel
`
`Fabrication of SiC/SiC Composites by Modified
`Reaction Sintering Process . . . . . . . . . . . . . . . . . . . . . . . . 455
`S.P. Lee,Y. Katoh, J.S. Park, S. Dong, and A Kohyama
`
`Manufacturing of 3-D Woven SiC/SiC Composite
`Combustor Liner . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 463
`Y. Matsuda, N. Akikawa, and T. Satoh
`
`A Thermally Conductive SiC-Polycrystalline Fiber and
`Its Fiber-Bonded Ceramic . . . . . . . . . . . . . . . . . . . . . . . . . 471
`T. Ishikawa, M . Sato, S. Kajii,Y.Tanaka, and M. Suzuki
`
`CVI Tyranno-SA/SiC Composites with Various PyC
`and SiC lnterlayers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 481
`WYang,Y. Katoh, A Kohyama, H. Araki,T. Noda, and J.Yu
`
`Mechanical Properties
`
`Optimized Performance in Unidirectional CFCMCs:
`Evolution from Experimental Observations
`to Desktop Design
`. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .49 I
`T.L. Jessen
`
`Elasti~ Modulus and Proportional Limit Stress in
`Ceramic Matrix Composites: Comparison of
`Methods and Results . . . . . . . . . . . . . . . . . . . . . . . . . . • . 503
`M.G. Jenkins and L.P. Zawada
`
`CMC Constitutive Law Based on Continuum Damage
`Mechanics and Its First Order Implementation
`into ABAQUS ......... . . . . . . . . . . . . . . . . . . . . . . . . . 51, 3
`J. Shi
`Tensile Behavior of SiC/SiC Composites Reinforced
`by Treated Sylramic SiC Fibers . . . . . . . . . . . . . . . . . . . . . . 521
`H.M.Yun,J.Z. Gyekenyesi,Y.L. Chen, D.R.Wheeler, and J.A. DiCarlo
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`Mechanical and Thermal Properties of Dense SiC/SiC
`Composite Fabricated by Reaction-Bonding Process ....... 533
`TTaguchi, N. lgawa, R.Yamada, M. Futakawa, and S.Jitsukawa
`
`Stress Rupture and Stress Relaxation of SiC/SiC
`Composites at Intermediate Temperature •............. 539
`G.N. Morscher and J. Hurst
`
`Room Temperature Creep of SiC/SiC Composites ........•. 547
`G.N. Morscher and A. Gyekenyesi
`
`Effect of Frequency on Fatigue Behavior in Tyranno
`Fiber-Reinforced SiC Composites . . . . . . . . . . . . . . . . . . . . 553
`Y. Kaneko, S. Zhu,Y Ochi,T Ogasawara, andT Ishikawa
`
`Tensile Stress Rupture of SiC/SiC Minicomposites
`in Vacuum. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 561
`J. Martinez Fernandez and G.N. Morscher
`
`Analysis of CMC C-Coupon Specimens for
`Structural Evaluation . . . . . . . . . . . . . . . . . . . . . . . . . . . . 569
`A.M. Calomino, F.I. Hurwitz, and A. Abdul-Aziz
`
`C-Coupon Studies of CMCs: Fracture Behavior and
`Microstructural Characterization . . . . . . . . . . . . . . . . . . . . 577
`F.I. Hurwitz, AM. Calomino, A. Abdul-Aziz, and TR. McCue
`
`lnterlaminar Shear Strength of a Unidirectional
`Fiber-Reinforced Celsian Composite by Short-Beam
`and Double-Notched Shear Tests . . . . . . . . . . . . . . . . . . . . 585
`0. Unal and N.P Bansal
`
`Effect of Load Rate on Tensile Strength of Various
`CFCCs at E1evated Temperatures-An Approach to
`Life-Prediction Testing . . . . . . . . . . . . . . . . . . . . . . . . . . . 597
`S.R. Choi and J.P Gyekenyesi
`
`Oxidation Effects
`
`Strength of 3-D SiC/SiC Composite after Long-Term
`Exposure to Elevated Temperature . . . . . . . . . . . . . . . . . . . 609
`T Satoh, Y Matsuda, and N . A kikawa
`
`XI
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`Crack Growth Behavior and TEM Analysis of lnterphase
`Oxidation in Boron-Enhanced SiC/SiC Composites ......... 617
`L.A. Giannuzzi and C.A. Lewinsohn
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`Stressed Oxidation and Modeling of C/SiC in
`Oxidizing Environments . . . . . . . . . . . . . . . . . . . . . . . . . . 625
`M.C. Halbig
`
`Fiber-Reinforced Composites: Oxide Fibers
`
`Optical and Mechanical Properties of Fiber-Reinforced
`Ceramic Matrix Optically Transparent Composites ........ 635
`AF. Dericioglu and Y Kagawa
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`Effect of Notches, Specimen Size, and Fiber Orientation
`on the Monotonic Tensile Behavior of Composites
`at Ambient and Elevated Temperatures . . . . . . . . . . . . . . . . 643
`M-L. Antti and E. Lara-Curzio
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`Fatigue Behavior of a Nextel™ 610 Composite ........•. 651
`H.G. Halverson and S.W Case
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`Effect of Small Effusion Holes on Creep Rupture
`Behavior of Oxide/Oxide Nextel™ 720/AS Composite ...... 659
`D.j. Buchanan, VA. Kramb, R.John, and L.P. Zawada
`
`Evaluation of All-Oxide Composites Based on
`Coated Nextel™ 610 and 650 Fibers . . . . . . . . . . . . . . . . . 667
`K.A. Keller,T Mah,TA. Parthasarathy, E. E. Boakye, and M. Cinibulk
`
`Nextel TM 61 0 and 650 Fiber Reinforced Porous
`Alumina-YAG Matrix Composites . . . . . . . . . . . . . . . . . . . . 677
`M.K. Cinibulk, K.A. Keller,T-11 Mah, and TA. Parthasarathy
`
`Analytical and Experimental Characterization of
`Thermomechanical Properties of a Damaged
`Woven Oxide-Oxide Composite . . . . . . . . . . . . . . . . . . . . . 687
`G.P.Tandon, D.J. Buchanan, N.J. Pagano, and R. John
`
`Fatigue Behavior of a Nextel™ 720/Alumina (N720/A)
`Composite at Room and Elevated Temperature .......... 695
`S.G. Steel, L.P. Zawada, and S. Mall
`
`XII
`
`GE-1026.014
`
`

`
`r
`
`Processing, Microstructure, and Properties of
`Nextel™ 610, 650, and 720 Fiber/Porous Mullite
`Matrix Composites .· . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 703
`B.J. Kanka, J. Goring, M. Schmucker; and H. Schneider
`Analysis of Damage Evolution in Continuous
`fiber-Reinforced Oxide/Oxide Composites under
`Cyclic Loading, Using Infrared Thermography ............ 71 I
`M-L. Antti, E. Lara-Curzio, and M.K. Ferber
`Application of Dielectric Properties to Noncontact
`Damage Detection for Continuous Fiber-Ceramic
`Matrix Composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 717
`T Mamiya, S. Zhu, and Y. Kagawa
`Electrical and Microstructural Characterization
`of Insulating Matrix with Conducting Particles .......... 725
`S. Hussain and 0. Sbaizero
`
`XIII
`
`GE-1026.015
`
`

`
`r
`
`Processing, Microstructure, and Properties of
`Nextel™ 610, 650, and 720 Fiber/Porous Mullite
`Matrix Composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 703
`B.J. Kanka, J. Goring, M. Schmucker; and H . Schneider
`Analysis of Damage Evolution in Continuous
`fiber-Reinforced Oxide/Oxide Composites under
`Cyclic Loading, Using Infrared Thermography ............ 71 I
`M-L. Antti, E. Lara-Curzio, and M.K. Ferber
`Application of Dielectric Properties to Noncontact
`Damage Detection for Continuous Fiber-Ceramic
`Matrix Composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 17
`T Mamiya, S. Zhu, and Y. Kagawa
`Electrical and Microstructural Characterization
`of Insulating Matrix with Conducting Particles .......... 725
`5. Hussain and 0. Sbaizero
`
`XIII
`
`GE-1026.016
`
`

`
`-Pr
`
`Preface
`
`The 25th Annual Cocoa Beach Conference and Exposition, an international meeting on
`engineering ceramics and structures, was held Januc ry 21 -26, 200 I. The conference attract(cid:173)
`ed more than 525 attendees from 24 different countl"ies. D uring the meeting, more than
`350 technical papers covering a wide range of advanced ceramics topics were presented in
`eight topical rocused areas and three symposia. One symposium on piezocomposite
`devices: design and utilization was held in honor of Professor Robert E. Newnham. The
`200 I James Mueller Lecture, the highest award granted by the Engineering Ceramics
`Division of the American Ceramic Society, was presented by Professor R. Judd Diefendorf,
`McAlister Trustee Professor Emeritus of Clemson University, Clemson, SC.
`
`We wou ld like to thank t he sym posia and focused topical session organizers, session chairs,
`presenters, and conference attendees for their efforts and enthusiasm in planning and par(cid:173)
`ticipating In a vibrant and leading edge conference. Once again, "Cocoa Beach" has demon(cid:173)
`strated why it is the premier conference on advanced ceramics and composites in the
`world. A special thanks is extended to the ACerS staff for keeping things running smooth ly.
`
`The 156 technical presentations accepted for publication in the conference proceedings
`following a peer-review process are a tribute to this excellent meeting. These papers are
`included as issues 3 and 4 in Volume 22 of the Ceramic Engineering and Science
`Proceedings. Issue 3 includes papers under the broad topical headings of Product
`Development and Commercialization, Thermomechanical Property Characterization, and
`Ceramic Matrix Composites. Issue 4 covers Advanced Synthesis and Processing, Porous
`Materials, Wear Resistant and Protective Coatings, TBCs and EBCs, Piezocomposite
`Devices, Biomaterials and FGMs. Subtopics for each of the areas are included in the appro(cid:173)
`priate table of contents.
`
`We hope you find these papers technically stimulating and look forward to seeing you at
`"Cocoa Beach 2002".
`
`Todd Jessen
`Mrityunjay Singh
`
`GE-1026.017
`
`

`
`Product Development and Commercialization
`
`..
`
`on
`act(cid:173)
`han
`] in
`;ite
`-he
`llCS
`xf,
`
`rs,
`ir-
`
`5s
`
`~e
`
`:e
`:t
`d
`IS
`e
`
`t
`
`GE-1026.018
`
`

`
`IS
`r.
`
`. e
`!.
`
`MOLYBDENUM DISILICIDE MATERIALS FOR GLASS MELTING
`SENSOR SHEATHS
`
`J.J. Petrovic, R.G. Castro, R.U. Vaidya, M.I. Peters, D. Mendoza, R.C. Hoover,
`and D.E. Gallegos
`Materials Science and Technology Division
`Los Alamos National Laboratory
`Los Alamos, NM 87545
`
`ABSTRACT
`Sensors for measuring the properties of molten glass require protective sensor
`sheaths in order to shield them from the extremely corrosive molten glass
`environment. MoSiz has been shown to possess excellent corrosion resistance in
`molten glass, making it a candidate material for advanced sensor sheath
`applications. MoSiz-coated A}i03 tubes, MoSiz-Ah03 laminate composite tubes,
`and MoSh-Ah03 functionally graded composite tubes have been produced by
`plasma spray-forming techniques for such applications.
`
`INTRODUCTION
`The glass industry has a critical need for advanced sensors that can determine
`properties of molten glass such as temperature, viscosity, and chemistry. Because
`molten glass is a very corrosive high temperature environment, sensors placed in
`molten glass must be protected by sensor sheaths that are corrosion-resistant to
`molten glass. Materials that are presently used for direct exposure to molten glass
`are noble metals such as platinum, refractory metals such as molybdenum, and
`refractory ceramics such as AZCS (Alumina-Zirconia-Chromia-Silica).
`For thermocouple protection sheaths, the glass industry currently uses either
`platinum tubes or platinum-coated alumina tubes for thermocouples that are
`inserted through the glass-air line. While platinum is a corrosion-resistant
`material above, at, and below the glass line, it is very expensive and its expense is
`a constraining factor on the extent of its use. Molybdenum sheaths can be
`employed fot thermocouples that are completely immersed in molten glass, but
`not for thermocouples that traverse the glass-air line, due to the poor oxidation
`resistance of molybdenum. While refractory ceramics such as AZCS possess
`good molten glass corrosion-resistance above, at, and below the glass line, these
`materials are difficult to fabricate into long and narrow thermocouple protection
`
`To the extent authorized under the laws of the United States of America, all copyright interests in this publication are the property
`of The American Ceramic Society. Any duplication, reproduction, or republication of this publication or any part thereof, without
`the express written consent of The American Ceramic Society or fee paid to the Copyright Clearance Center, is prohibited.
`
`59
`
`GE-1026.019
`
`

`
`sheath tubes. Additionally, AZCS has very low strength and can exhibit extensive
`plastic deformation at elevated temperatures.
`MoSirbased materials show excellent molten glass corrosion-resistance both
`above and below the glass line. Unlike platinum, MoSii materials are inexpensive
`and can be readily fabricated into protective sheath tubular geometries by
`industrial processes such as plasma spraying.
`In addition,
`the elevated
`temperature strength of MoSii materials is significantly higher than that of the
`refractory ceramics. MoSi2 is also electrically conductive, while the refractory
`ceramics are insulator materials.
`Because of their combination of properties, MoSirbased materials constitute
`an important new class of materials for glass industry sensor sheath applications.
`
`MOLTEN GLASS CORROSION RESISTANCE OF MoSii
`The molten glass corrosion-resistance of MoSi2 has been characterized in an
`alkali borosilicate glass (1). The corrosion behavior of MoSi 2 in comparison to
`the refractory ceramic AZCS is shown in Figure 1, for locations above, below,
`
`0.1
`
`AZCS
`
`0
`
`0.0 i~
`,
`MoSi
`
`0.0
`
`0
`
`-0.2
`
`I -0.4
`t
`]
`~
`
`--0.6
`
`-0.8
`
`AZCS
`Below glass-line
`
`0
`
`Above glass-line.
`
`--0.1
`
`I
`"
`~
`-'il
`.,
`~ --0.2
`~
`
`--0.3
`
`0.0
`
`-0.2
`
`-0.4
`
`-0.8
`
`I -0.6
`..,
`l -1.0
`"' "' .,
`-1.2
`~
`~ -1.4
`-1.6
`
`50
`
`150
`100
`Exposure time (hrs)
`
`200
`
`230
`
`-1.0
`
`50
`
`100
`150
`Exposure time {hrs)
`
`200
`
`250
`
`At glass-line
`
`AZCS
`
`and at the glass-air line. The corrosion(cid:173)
`resistance of MoSii is similar to that of
`AZCS both above and below the glass(cid:173)
`line, but at the glass-air line MoSii has
`a
`lower
`corrosion-resistance
`than
`AZCS by approximately a factor of
`five.
`
`0
`
`20
`
`40
`
`RO
`
`100
`
`Figure 1: Molten glass corrosion of MoSh above, below, and at the glass-air line
`(1).
`
`60
`
`imn
`whi
`Ho\
`Mo:
`gla~:
`che
`
`Fi:
`
`M
`
`fu
`fu
`bt
`cc
`
`si
`tt:
`tl
`n
`
`c
`1'
`1 .,
`
`<
`c
`
`GE-1026.020
`
`

`
`I
`
`• 1ve
`
`::>th
`LVe
`by
`:ed
`he
`>ry
`
`tte
`
`an
`to
`N,
`
`f
`
`s
`l
`f
`
`Figure 2 shows the corrosion mechanisms that occur for MoSiz when it is
`immersed in molten glass. Above the glass-line a protective Si02 layer forms,
`while below the glass-line a complex multiphase protective layer is formed.
`flowever, at the glass-line no protective layer forms. Hence, the corrosion rate of
`l\tfoSiz is maximum at the glass-line. For any material that is immersed in molten
`glass, the m~~imum corrosio.n rate occu~s at the. glass-~ine due to the increased
`chemical activity and mechamcal convect10n at this locat10n.
`
`Glass+[)issolved SiO 1
`
`At
`
`figure 2: Corrosion mechanisms of MoSiz in molten alkali borosilicate glass (1) .
`
`MoSiz-COATED AJi03 TUBES
`Sensor sheaths for glass furnace temperature sensors and for other types of
`furnace sensors such as video monitoring systems operating inside the glass
`furnace require a tubular geometry for the sensor sheath. MoSiz-based tubes can
`be readily fabricated by plasma spray-forming (2).
`In this process, MoSiz or
`composites based on MoSiz are plasma sprayed onto graphite or alumina tubes.
`MoSiz and Ali03 constitute a good composite system for such applications,
`since these materials are thermodynamically stable with each other at elevated
`temperatures, and possess matching thermal expansion coefficients that minimize
`thermal stresses. MoSiz-Ali03 composites may exhibit improved thermal shock
`resistance, which is desirable for sensor sheath applications.
`Advanced plasma spray techniques were employed to place MoSiz coatings on
`commercial A}i03 tubes. A Miller thermal spraying system (SG 100 Gun and two
`Model 1264 programmable hoppers) coupled to a Fanuc robotic system (S-10), an
`in-flight particle analyzer (Technar DPV 2000), and an infrared camera (Mikron
`TH 5104) were employed to fabricate the MoSiz-coated A1i03 tubes.
`A photo of a MoSiz-coated A}i03 tube is shown in Figure 3. The Al20 3 was a
`commercially available closed-end tube (998 alumina from LSP Industrial
`Ceramics Inc.) with an OD of 12.7 mm and an ID of 9.53 mm. The tube was
`coated with a 2 mm thick coating of MoSiz, over a 450 mm length of the tube,
`
`61
`
`GE-1026.021
`
`

`
`including the closed end. A cross-section of the coated tube is also shown m
`Figure 3.
`
`Figure 3: MoSh-coated Ah03 closed-end tube. Tube cross-section is also shown .
`
`MoSii-Al20 3 LAMINATE COMPOSITE TUBES
`Figure 4 shows the cross-sections of laminate MoSh-Ah03 tubes that were
`fabricated by plasma spraying alternate layers of MoSi 2 and Ah03 onto a graphite
`tube mandrel (the graphite mandrel is subsequently removed by oxidation).
`
`JO mm
`
`IO mm
`
`IO mm
`
`Large layer thickness
`
`Medium layer thickness
`
`Fine layer thickness
`
`Figure 4: 50 vol.% MoSir50 vol.% Ah03 laminate composite tubes produced by
`plasma spray-forming. MoSh is the dark phase and Ah03 the light phase.
`
`Tubes with three different layer thicknesses of 0.8 mm, 0.2 mm, and 0.08 mm
`were fabricated. The fabricated tubes were approximately 300 mm in length.
`Because of the thermal expansion coefficient match between MoSh and Ah03 , no
`cracking due to thermal stresses has occurred in the tubes. MoSh-Ah03
`
`62
`
`la1
`ol:
`
`M
`
`F
`pl
`
`Cl
`
`F
`f1
`
`GE-1026.022
`
`

`
`i in
`
`inate composite bend strengths were in the range of 85-115 MPa and were
`Iatn
`·
`· h d
`.
`1
`h. k
`observed to mcrease wit
`ecreasmg ayer t ic ness.
`
`MoSiz-Alz03 FUNCTIONALLY GRADED COMPOSITE TUBES
`Figure 5 shows the cross-sections of functionally graded MoSh-Alz03 tubes
`f bricated by plasma spray-forming. Both continuously graded and layered
`~aded tubes were fabricated.
`The strengths of these FGM tubes were
`!pproximately 70 MPa.
`
`La ered and Graded
`
`rn.
`
`re
`te
`
`lO mm
`
`Figure 5: Continuously graded and layered graded MoSiz-Ah03 composite tubes
`produced by plasma spray-forming.
`
`The MoSh-Ah03 functionally graded materials exhibited interesting load(cid:173)
`displace