Ceramic Engineering & Science Proceedings issue 4, 1996 Proceedings of the 20th Annual Conference on Composites, Advanced Ceramics, Materials, and Structures-B January 7-1 1, 19 96 Cocoa Beach, FL Victor Greenhut Program Chair Published by The American Ceramic Society 735 Ceramic Place Westerville, OH 43081-61 36 Copyright 0 1996 The American Ceramic Society ISSN 019 6-621 9 W. Paul Holbrook, Executive Director John B. Wachtman Jr., Editor Mark Mecklenborg, Director of Publications Lori A. Kozey, Product Manager Sarah Godby, Production Assistant Committee on Publications: Marina R. Pascucci, chair; ; Man F. Yan; Richard Haber; Terrence E. Mitchell; Steven Freiman, ex officio; Prabhat Gupta, ex officio; Richard M. Spriggs, ex officio; Timothy M. Robinson, ex officio; John B. Wachtman Jr., ex officio; W. Paul Holbrook, ex officio; Mark Mecklenborg, ex officio. Editorial and Subscription Offices: P.0 Box 6136, Westerville, 43086-6136. 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These articles are of practical value for the ceramic industries and the general public. The issues are based on the proceedings of a conference. Both American Ceramic Society and non-Society conferences provide these technical articles. Each issue is organized by an editor who selects and edits material from the conference proceedings. The opinions expressed are entirely those of the presentors. There is no other review prior to publication. Table of Contents 20th Annual Conference on Composites, Advanced - Ceramics, Materials, and Structures B Introduction CMCs: Research in Europe and the Future Potential of CMCs ................................................. inIndustry 3 Marcel H. Van de Voorde and Martin R. Nedele Fibers and Tows .................... Stability of Polycrystalline Nextel 720 Fiber .25 Gopal Das Mechanical and Structural Analysis of Silicon Carbide Fiber ........................................... Hi-NicalonTypes 35 M. Takeda, J. Sakamoto, A. Saeki, and H. Ichikawa ........... Fiber Strength with Coatings from Sols and Solutions .43 Randall S. Hay, Dennis Petry, and Emmanuel Boakye Porous Aluminum Oxide and Lanthanum Phosphate Fiber .................................................. Coatings 53 E. Boakye, M.D. Petry, and Hay R.S. Thermomechanical Behavior of Advanced Sic Fiber ........................................ Multifilament Tows .61 Hee Mann Yun and James A. DiCarlo Characterization of Fiber Materials Using Metallographic and .................................. Image Analysis Techniques .68 Matthias Hoffmann and David J. Diaz Processing Impregnation Molding of Particle-Filled Preceramic Polymers ........................................ into Fiber Preforms .79 Merve Erdal Selpk Giiqeri and ... 111 Method for Reinforcing Threads in Multilayer Composite lhbes .................................. and Cylindrical Structures .90 G.R. Romanoski and T.D. Burchell Influence of Fiber Lay-Up Sequence on Mechanical Properties ................................... of SiC(f)/SiC Composites. .98 Dileep Singh, Jitendra P. Singh, and Manish Sutaria Processing, Properties, and Microstructure of HVR Nicalon ...... Fiber Cloth-Reinforced Zirconium Phosphate Composites. ,110 Barry A. Bender, Roy J. Rayne, Todd L. Jessen, and Scott Browning Fabrication and Properties of Dense Silicon Carbide Matrix .............................................. Composites .118 S. Suyama, Kameda, and N. Amiji T. Microstructure and Interface Characteristics of Alumina- ...................................... Zirconia Composites .125 R.F. Yttergren, Z.-K. Liu, and D.J. Rowcliffe Fabrication and Mechanical Properties of Si3Nq-Based ........................... Composites with Layer Structure. .131 Yasuhiro Shigegaki, Manuel E. Brito, Kiyoshi Hirao, and Motohiro Toriyama . The Multi-Fracture Response of Cross-Ply Ceramic Composites. ,139 Erdman andY.J. Weitsman D.L. Modeling of Flexural Behavior of Continuous-Fiber Ceramic Composites ...............................................147 S. Raghuraman, E. Lara-Curzio, and M.K. Ferber ... Low-Cycle Tensile Fatigue Behavior of an SiC/SiC Composite. .157 0.O nd ....... Laminated Matrix Composites: A New Class of Materials .166 Jack Lackey, Sundar Vaidyaraman, and Karren L. More W. Low-Cost, Near-Net-Shape Ceramic Composites Using Resin ..................... Transfer Molding and Pyrolysis (RTMP) .174 W.J. Sherwood, C.K. Whitmarsh, J.M. Jacobs, and L.V. Interrante Improvement of Si-Ti(Zr)-C-0 Fiber and a Precursor Polymer ............................... for High-Temperature CMC. .184 T. Yamamura, S. Masaki, T. Ishikawa, M. Sato, M. Shibuya, and K. Kumagawa iv Interfaces and Coatings .................. B4C Coated Carbon Fiber Reinforced Si3N4. .195 P.M. Bronsveld, I. Gideonse, A. Van der Heide, Guder, J.Th.M. De Hosson, S. E. Sabouret, J.B. Veyret, and E. Bullock Damage Evolution Due to Thermal Shock in a 2-D Woven Fiber- ............................. Reinforced CVI SIC Composite .203 James E. Webb and Raj N. Singh ......................... Carbon-Carbon Composites Joining .211 Liang A. Xue Residual Stress and Poisson Expansion Effects on the Fiber- ..... Matrix Interfacial Properties Measured in Fiber Push Tests ,225 A.M. Daniel, M.R. Elizalde, J.M. Marthez-Esnaola, and J. Janczak Microstructure and Mechanical Response of Lanthanum Phosphate/Yttrium Aluminate and Yttrium PhosphateKttrium ....................................... Aluminate Systems. .233 Dong-Hau Kuo and Waltraud M. Kriven .................... Sol-Gel Coating of Nicalon Fiber Cloths.. .241 Michael K. Cinibulk ........ Rb P-Alumina an Interface Coating in Oxide CMCs.. .250 as Sambasivan, J.A. Morris, and Petuskey S. W.T. Interfacial Bonding of Carbon-Coated Glass Fiber Reinforced .................................................. Cement 258 Chao M. Huang, D. Zhu, C.X. Dong, W.M. Kriven, R. Loh, and J. Huang Investigation of Fibermatrix Interfacial Mechanical Behavior .. in Ceramic Matrix Composites by Cyclic Fiber Push-In Testing .266 J.I. Eldridge, R.T. Bhatt, N.P. Bansal, and F.A. Olmstead Interface Modification During Oxidation of a Glass-Ceramic ............................... MatridSiC Fiber Composite. .280 A.M. Daniel, A. Martfn Meizoso, K.P. Plucknett, and D.N. Braski V Mechanical and Elevated Temperature Properties Hi-Nicalon Sic Fiber Reinforced Glass and Glass-Ceramic ....................................... Matrix Composites. .291 William K. Tredway .... Mullite Fiber Reinforced Reaction Bonded Si3N4 Composites .299 Saleh, A. Lightfoot, J. Haggerty, and A. Sayir T. The Effect of Fiber Loading on the Mechanical Behavior of ................................... Unidirectional CFCMCs ,307 Todd L. Jessen, A. Bender, and Victor A. Greenhut Barry Tensile and Interlaminar Shear Evaluation of Du Pont Lanxide CMCs ...................................................... Michael R. Effnger, Dennis S. Tucker, and Terry R. Bamett Microstructures and Mechanical Properties of Hi-Nicalon Fiber ........................ Reinforced Si3N4 Matrix Composites. .324 K. Nakano, S. Kume, K. Sasaki, and H. Saka Mechanical Properties and Microstructure of Oxidized SiC/SiC .............................................. Com osites .333 0. pu'n al, A.J. Eckel, and F.C. Laabs Mechanisms of Hot Corrosion of a Silicon Carbide Fiber- ................................. Reinforced Glass-Ceramic. ,342 Atul Kumar, Alan G.F ox, and Shaio-Wen Wang Fracture Energy and Fiber Pullout Process of a Continuous Carbon Fiber Reinforced Silicon Nitride Matrix Composite at .................................... Elevated Temperatures ,349 T. Miyajima, D. Torikai, andY. Yamauchi Elevated Temperature Properties and Performance of Nicalon ................. Reinforced Enhanced Sic Matrix Composites .357 Mehran Elahi, Kenneth Reifsnider, Thomas Dunyak, and Kin Liao Time Dependence of Oxidation-Induced Microstructural ............... Changes in Nicalon- and Nextel-Reinforced Sic. ,366 Tortorelli and K.L. More P.F. vi ARPA's Low-Cost Ceramic Composites Program Process Simulation for RTM of Blackglas MatrixAVextel Fiber ...................................... Ceramic Composites .377 R. Leek, G. Carpenter, J. Madsen, and T.M. Donnellan ...... Curing and F'yrolysis of Blackglas Resins and Composites. .386 Roger Y. hung and Wallace D. Porter NMR Study of Redistribution Reactions in Blackglas and Their ............................... Influence on Oxidative Study .394 M.A.B. Meador, F.I. Hurwitz, and S.T. Gonczy .................. Pyrolysis Behavior of Blackglas Composites. ,401 J. Annamalai, W.N. Gill, A. Tobin, J. Madsen, and T.M. Donneilan Performance of Blackglas Composites in 4000-Hour Oxidation ................................................. Study.. .411 S. Campbell, S. Gonczy, M. McNallan, and A. Cox ........... Strength of Fabric-Reinforced Blackglas Composites .421 Charles Lei and Frank K. KO Abradability Testing of BN-Nextel/312/Blackglas3 -D Woven ............. Composites and the Effect on Retained Strength.. .431 Durell Wildman and Pramod Khandelwal NDE of Nextel 312 and Nicalon Fiber Reinforced Blackglas .............................................. Composites .441 Pramod Khandelwal, GeorgeY. Baaklini, Don 3. Roth, James R. Bodis, and Richard W. Rawer Processing and Performance of SiC/Blackglas CFCCs Using ........................................ Filament Winding. .449 M.N. Ghasemi Nejhad, M.V. Chandramouli, and A.A. Wereszczak vii Introduction Ceramic Engineering & Science Proceedings Victor Greenhut CouvriehtOl996 The American Ceramic Society CMC’s Research in Europe and the Future Potential of CMC’s in Industry Marcel H.Van de Voorde Martin R. Nedele European Union Deutsche Forschungsanstalt Luft- und Raumfahrt fiir JRC-Institute for Advanced Materials Institute of Structures and Design P.O. Box 2, ZG Petten Pfaffenwaldring 38-40, Stuttgart 1755 D-70569 The Netherlands Germany Abstract CMC’s ceramics Matrix Composites) have been developed for high temperature applications in aerospace and military industries. In general, the CMC’s should be capable of outperforming the best available superalloys. Great efforts are being given to pinpoint spin-off technologies i.e. applications in modern fossil fuel power plants, gas turbines, petrochemistry etc. In these applications, the CMC’s have to operate at temperatures up to 140O0C, in corrosive environments for long durations. These developments will provoke a breakthrough for this new group CMC- materials. The paper will: i) give an overview of the CMC’s research in Europe; processing, and characterization of physical, chemical and engineering properties at high temperatures; ii) pinpoint the R&D needs to achieve the potential growth; iii) review the industrial potentials. Introduction Many challenges for improvements and new developments in energy technology and industrial productivity are not met because of the unavailability of structural materials capable of assuring safe and reliable plant operation, at competitive costs. The advanced enerev technology requires materials with: i) improved erosion - and corrosion resistance, ii) better mechanical behaviour, iii) higher temperature capability. A new group of high temperature materials with engineering properties better than the best modem superalloys and metal matrix composites has to be invented. The transDort industry has an additional need for light weight materials; with high stiffness and wear resistance. New materials, complimenting the use of advanced polymers and carbon composites have to be realized, to meet the severe technical specifications. Monolithic ceramics offer combined properties of low weight, high temperature strength and 3 environmental stability. The problem with these ceramic materials is their lack of defect tolerance, leading to the possibility of catastrophic service failure in structural components. may result This in: i) air-trafic problems caused by for example; damaged aero engine components and ii) in important financial losses due to unforseen shutdowns in industrial plants. Improved ceramic processing techniques and toughening of ceramics through the incorporation of particulates, whisker and short result in ceramics with better fracture toughness, but the fibers brittle failure problem still persists. Long fiber and woven reinforced ceramic composites have the potential to combine chemical resistance, high temperature strength and toughness. CMC's may offer a challenge for the technology of the 211L century which the modem industry demands a combination of: in i) high temperature stability for thousands of hours, ii) hot and ash corrosion resistance, iii) reliable mechanical properties - in the 1200°C to 1600°C temperature range; and iv) cost competitivety, Figs. 1 and 2. .- -., A Ceramicmatrix 900 CFRP ~ Carbon fiber reinforced polymers Ceramics matrix bmZmic matfix 18: GGCMMC C --. GG llaassss -mceartarimx cico mmaptrobcs itcensm posites + plastic n CMMMCC - CMeertaaml mica mtriaxt rcixo mwpmopsoitessit es +P lcaesrtaicm micastr ix z66.. w C-C ~ Carbon-carbon composites $400 rom B 200 v) 100 0 Metal mairix Fktlc matrix 0 200 400 6w 800 loo0 1200 1400 1800 +plasUc +metal Temperature, *C Fig. 1 : Different forms of composites Fig.2: S-ht of stnrdural materials The ceramic matrix composites "C-Sic" and Sic-Sic" form the leitmotiv through the whole paper, because of the great interest in these materials by industry the extreme difficulties to introduce and them in innovative technologies. Much information available in the paper can easily be used for other ceramic- and carboncarbon composites. 2. MANUFACTURE OF TEMPERATURE CMC-MATERIALS HIGH A status is given on the development of: report i) high temperature ceramic f i br einforcements, ii) ceramic matrices and iii) manufacturing methods for industrial CMC's-materials. 4