October 2003 Porous Oxide Matrix Composite Reinforced with Oxide Fibers 1739 National Materials Advisory Board, Committee on Advanced Fibers for Higl Temperature Ceramic Composites, Publication NMAB-494. National Academy Press, 00∞080 dvanced Hot Gas Filter Development, "Ceram. Eng. Sci. Proc., 0p tme 21(314757(20 R. Warren(Ed ) Comprehensive Composite Materials. Elsevier, Amsterdam, M. van Roode, w. D. Brentnall, K. O Smith, B D, Edwards, J. McClain, and J.R. 忍 Price, "Ceramic Stationary Gas Turbine D nent Program--Fourth Annual 720.1200°c/100h WOF= 1819/n Iz, S. Wittig, and G. Andrees, "Experimental Assessment of Fiber Reinforced Ceramics for Combustor Walls. m. Soc. Mech. WO K. Nishio, K-, Igashira, K. Take, and T. Suemitsu, "Development of a Combustor Liner Composed of Ceramic Matrix Composite( CMC),"Am Soc. Mech. Pa198GT:104(199 A. G. Razzell, M. Holmquist, L. Molliex, and O. Sudre, "Oxide/Oxide Ceramic Matrix Composites in Gas Turbine Combustors, Am. Soc. Mech. Eng,/Pap/ 98GT-30(1998) loW. H. Glime and J. D ""Stress Concentration Due to Fiber-Matrix Fusion in Ceramic-MatrIx s,J.Am. Ceram. Soc., 81[10] 2597-604 (1998) R. H. Jones, C. H. Henger Jr, C. A. Lewinsohn, and C. F. Windisch Jr. ig. 9. Load versus displacement plots for notched composites reinforced racking of Silicon Carbide Fiber/Silicon Carbide Composi with N720 or N610 fibers, in as-processed condition and after aging J. Am. Ce Recent Developments in Fibers and Interphases for High Matrix Composites, "Composites, Part A, 30, 429-37(1999) D. B. Marshall, J. B. Davis, P. E. D. Morgan, and J.R. Porter,"Interface Materials for Damage-Tolerant Oxide Composites, Key Eng. Mater, 127-13 been reached and, consequently, the area under the curve can be used as a measure of the work of fracture(WOF). WOF was Butler, and L. Al-Dawery, "Development of Interfaces measured to-16-2.0 kJ/m? for the N720 composite. Correspond. in spide Matrix. ” Key Eng Mater.,l64-165,351-56(1999) ing values for the N610 composite were -2.5-3.6 kJ/m". A slight Fiber Coatings fo Oxide CFCC, Ceram. Eng. Sci. Proc., 18 [3] 279-86 decrease in WoF could be seen after heat treatment at 1200%C fo (1997) 100 h. as shown in Table Ill. IbM. K. Cinibulk, "Hexaluminates as a Cleavable Fiber-Matrix Interphase: Syn- Development, and Phase Compatibility, "J. Eur. Ceram. Soc., 20, 17M. Holmquist, R Lundberg, O. Sudre, A. G.Razzell, L. Molliex,J.Benoit, IV. Conclusions J. Adlerborn,Alumina/Alumina Composite with a Porous Zirconia Interphak& ocessing, Properties and Component Testing, J. Eur. Ceram Soc., 20, 599-606 a process to manufacture porous oxide matrix/po oxide fiber composites was developed and evaluated. Th O Sudre, A. G. Razzell, L. Molliex, and M. Holmquist, "Alumina Single-Crystal Fibre Reinforced Alumina Matrix for Combustor Tiles. Ceran Eng. Sci. Proc. 19 uses a preconsolidated slurry with a very high volume f powder to infiltrate fiber cloths. These infiltrated fiber "M. J. O'Brien and B. W. Sheldon, "Porous Alumina Coating with Tailored be frozen and used latter to fabricate engineering shapes. Mechan- Fracture Resistance for Alumina Composites,J. Am. Ceram Soc., 82[12]3567-74 ical property measurements suggest that the processing method (299). used here was comparable to porous oxide matrix composites 20K. A. Keller, T-I. Mah, T. A. Parthasarathy and C. M. Cooke, F Interfacial Carbon Coatings for Oxide/Oxide Composites,J. Am. Ceram Soc., 832) manufactured by other processes using the same fibers. and mullite/alumina N20 fibers showed nonbrittle fracture behav- Ceramic Compos叫Em,℃m以Dm,m In-plane flexural tests of composites based on alumina N610 and strengths of >280 and >170 MPa, respectively, and moderate notch sensitivity. Interlaminar shear strength, which is F F. Lange, C G. Levi, and F. w. Zok, "Processing Fiber Reinforced Ceramics dominated by the porous matrix, ranged between 7 and 12 MPa for s,2000 matrix porosity ranging from 38% to 43%, respectively roth, and F. F. Lange, "Processing and Properties of an The composites possessed good thermal stability; the micro- All-Oxide Composite with a Porous Matrix,J. Eur. Cera. Soc., 20, 607 structure was stable after aging at 1200 C for 100 h, showing no C. G. Levi, F. W. Zok, J-Y. Yang, M. Mattoni, and J. P. A. Lofvander visible signs of densification. This heat treatment was found to Microstructural Design of Stable Porous Matrices for All-Oxide Ceramic Compos- slightly increase the interlaminar shear strength, which was ites” Z Metalled,90121037-47(1999) attributed to a strengthening of the matrix network, and was F. F. Lange, w. C. Tu, and A. G. Evans, U.S. Pat. No. 5856 252 accompanied by a reduction in composite toughness. However, Several the 1200 C/(100 h) treatment did not significantly change the Ceram. Eng. Sci. Proc., 19 [3]327-39(1 composite strength or strain to failure. Heat treatment at 1300C J.99GT-190(1999) for 100 h reduced the strength for the N610 and N720C G Levi, J-Y. Yang, B J Dalgleish, F. W Zok, and A G. Evans,"Processin composites by 35% and 20%, respectively, and increased their 2M. Mattoni, J -Y. Yang, C. G. Levi, and F. W. Zok, "Effects of a Precursor ived Alumina on the Mechanical Properties of a Porous-Matrix, All-Oxide Ceramic Composite,JAm, Ceram Soc., in review Acknowledgments In-Plane Mechanical Properties of an Al-Oxide Ceramic Composite, "J.Am. Ceram We thank R. Harrysson for SEM work and Professor F, w. Zok, Dr. J.-Y. Yang Soc,82]2721-301999 nd M. Mattoni for useful discussion E.A. V.Carelli, H Fujita, J. Y. Yang, and F. w. Zok,"Effects of Thermal Aging on the Mechanical Properties of a Porous-Matrix Ceramic Composite,"in revie 32G. W. Franks and F. F. Lange, "Plastic Clay-like Flow Stress of Saturated Advanced Ceramic Powder Compacts,".. Eur. Cera. Soc., in press References 3M. Holmquist, T C. Radsick, O. Sudre, FF. Lange, and F. W. Zok, "Fabrication esting of All-Oxide CFCC IC. P. Beesley, "The Application of CMC's in High Integrity Gas Turbine ange, T. C. Radsick, Engines, Key Eng Mater, 127-131, 165-74(1997 Control of Microstructure and Properties", Pp. 587-99 in Proceedings of the 4th H. Knabe, and F, Strobel, "Development and Testing of C/SiC omponents for Liquid Rocket Propulsion Applications, ALAA Pap, 99-2896 Edited by W. Krenkel, R. Naslain, and H, Schne eramic Matrix Composites International Conference on High Temperature Wiley-VCH, New Yorbeen reached and, consequently, the area under the curve can be used as a measure of the work of fracture (WOF). WOF was measured to
1.6–2.0 kJ/m2 for the N720 composite. Correspond￾ing values for the N610 composite were
2.5–3.6 kJ/m2 . A slight decrease in WOF could be seen after heat treatment at 1200°C for 100 h, as shown in Table III. IV. Conclusions A process to manufacture porous oxide matrix/polycrystalline oxide fiber composites was developed and evaluated. The method uses a preconsolidated slurry with a very high volume fraction of powder to infiltrate fiber cloths. These infiltrated fiber cloths can be frozen and used latter to fabricate engineering shapes. Mechan￾ical property measurements suggest that the processing method used here was comparable to porous oxide matrix composites manufactured by other processes using the same fibers. In-plane flexural tests of composites based on alumina N610 and mullite/alumina N720 fibers showed nonbrittle fracture behav￾ior and strengths of 280 and 170 MPa, respectively, and moderate notch sensitivity. Interlaminar shear strength, which is dominated by the porous matrix, ranged between 7 and 12 MPa for matrix porosity ranging from 38% to 43%, respectively. The composites possessed good thermal stability; the micro￾structure was stable after aging at 1200°C for 100 h, showing no visible signs of densification. This heat treatment was found to slightly increase the interlaminar shear strength, which was attributed to a strengthening of the matrix network, and was accompanied by a reduction in composite toughness. However, the 1200°C/(100 h) treatment did not significantly change the composite strength or strain to failure. Heat treatment at 1300°C for 100 h reduced the strength for the N610 and N720 composites by 35% and 20%, respectively, and increased their brittle nature. Acknowledgments We thank R. Harrysson for SEM work and Professor F. W. Zok, Dr. J.-Y. Yang, and M. Mattoni for useful discussions. References 1 C. P. Beesley, “The Application of CMC’s in High Integrity Gas Turbine Engines,” Key Eng. Mater., 127-131, 165–74 (1997). 2 S. Beyer, H. Knabe, and F. Strobel, “Development and Testing of C/SiC Components for Liquid Rocket Propulsion Applications,” AIAA Pap., 99-2896 (1999). 3 National Materials Advisory Board, Committee on Advanced Fibers for High Temperature Ceramic Composites, Publication NMAB-494. National Academy Press, Washington, DC, 1998. 4 T. J. McMahon, “Advanced Hot Gas Filter Development,” Ceram. Eng. Sci. Proc., 21 [3] 47–57 (2000). 5 R. Warren (Ed.), Comprehensive Composite Materials. Elsevier, Amsterdam, Netherlands, 2000. 6 M. van Roode, W. D. Brentnall, K. O. Smith, B. D. Edwards, J. McClain, and J. R. Price, “Ceramic Stationary Gas Turbine Development Program—Fourth Annual Summary,” Am. Soc. Mech. Eng., [Pap.], 97-GT-317 (1997). 7 D. Filsinger, S. Mu¨nz, A. Schulz, S. Wittig, and G. Andrees, “Experimental Assessment of Fiber Reinforced Ceramics for Combustor Walls,” Am. Soc. Mech. Eng., [Pap.], 97-GT-154 (1997). 8 K. Nishio, K.-I. Igashira, K. Take, and T. Suemitsu, “Development of a Combustor Liner Composed of Ceramic Matrix Composite (CMC),” Am. Soc. Mech. Eng., [Pap.], 98-GT-104 (1998). 9 A. G. Razzell, M. Holmquist, L. Molliex, and O. Sudre, “Oxide/Oxide Ceramic Matrix Composites in Gas Turbine Combustors,” Am. Soc. Mech. Eng., [Pap.], 98-GT-30 (1998). 10W. H. Glime and J. D. Cawley, “Stress Concentration Due to Fiber–Matrix Fusion in Ceramic–Matrix Composites,” J. Am. Ceram. Soc., 81 [10] 2597–604 (1998). 11R. H. Jones, C. H. Henager Jr., C. A. Lewinsohn, and C. F. Windisch Jr., “Stress-Corrosion Cracking of Silicon Carbide Fiber/Silicon Carbide Composite,” J. Am. Ceram. Soc., 83 [8] 1999–2005 (2000). 12R. E. Tressler, “Recent Developments in Fibers and Interphases for High Temperature Ceramic Matrix Composites,” Composites, Part A, 30, 429–37 (1999). 13D. B. Marshall, J. B. Davis, P. E. D. Morgan, and J. R. Porter, “Interface Materials for Damage-Tolerant Oxide Composites,” Key Eng. Mater., 127–131, 27–36 (1997). 14M. H. Lewis, A. Tye, E. Butler, and I. Al-Dawery, “Development of Interfaces in Oxide Matrix Composites,” Key Eng. Mater., 164–165, 351–56 (1999). 15R. W. Goettler, S. Sambasivan, and V. P. Dravid, “Isotropic Complex Oxides as Fiber Coatings for Oxide–Oxide CFCC,” Ceram. Eng. Sci. Proc., 18 [3] 279–86 (1997). 16M. K. Cinibulk, “Hexaluminates as a Cleavable Fiber-Matrix Interphase: Syn￾thesis, Texture Development, and Phase Compatibility,” J. Eur. Ceram. Soc., 20, 569–82 (2000). 17M. Holmquist, R. Lundberg, O. Sudre, A. G. Razzell, L. Molliex, J. Benoit, and J. Adlerborn, “Alumina/Alumina Composite with a Porous Zirconia Interphase— Processing, Properties and Component Testing,” J. Eur. Ceram. Soc., 20, 599–606 (2000). 18O. Sudre, A. G. Razzell, L. Molliex, and M. Holmquist, “Alumina Single-Crystal Fibre Reinforced Alumina Matrix for Combustor Tiles,” Ceram. Eng. Sci. Proc., 19 [4] 273–80 (1998). 19M. J. O’Brien and B. W. Sheldon, “Porous Alumina Coating with Tailored Fracture Resistance for Alumina Composites,” J. Am. Ceram. Soc., 82 [12] 3567–74 (1999). 20K. A. Keller, T.-I. Mah, T. A. Parthasarathy, and C. M. Cooke, “Fugitive Interfacial Carbon Coatings for Oxide/Oxide Composites,” J. Am. Ceram. Soc., 83 [2] 329–36 (2000). 21W.-C. Tu, F. F. Lange, and A. G. Evans, “Concept for a Damage Tolerant Ceramic Composite with ”Strong“ Interfaces,” J. Am. Ceram. Soc., 79 [2] 417–24 (1996). 22F. F. Lange, C. G. Levi, and F. W. Zok, “Processing Fiber Reinforced Ceramics with Porous Matrices”; Ch. 14 in Comprehensive Composite Materials. Edited by R. Warren. Elsevier, Amsterdam, Netherlands, 2000. 23J. J. Haslam, K. E. Berroth, and F. F. Lange, “Processing and Properties of an All-Oxide Composite with a Porous Matrix,” J. Eur. Ceram. Soc., 20, 607–18 (2000). 24C. G. Levi, F. W. Zok, J.-Y. Yang, M. Mattoni, and J. P. A. Lo¨fvander, “Microstructural Design of Stable Porous Matrices for All-Oxide Ceramic Compos￾ites,” Z. Metallkd., 90 [12] 1037–47 (1999). 25F. F. Lange, W. C. Tu, and A. G. Evans, U.S. Pat. No. 5 856 252, 1999. 26L. P. Zawada, “Longitudinal and Transthickness Tensile Behavior of Several Oxide/Oxide Composites,” Ceram. Eng. Sci. Proc., 19 [3] 327–39 (1998). 27R. A. Jurf and S. C. Butner, “Advances in Oxide–Oxide CMC,” Am. Soc. Mech. Eng., [Pap.], 99-GT-190 (1999). 28C. G. Levi, J.-Y. Yang, B. J. Dalgleish, F. W. Zok, and A. G. Evans, “Processing and Performance of an All-Oxide Ceramic Composite,” J. Am. Ceram. Soc., 81 [8] 2077–86 (1998). 29M. Mattoni, J.-Y. Yang, C. G. Levi, and F. W. Zok, “Effects of a Precursor Derived Alumina on the Mechanical Properties of a Porous-Matrix, All-Oxide Ceramic Composite,” J. Am. Ceram. Soc., in review. 30J. A. Heathcote, X.-Y. Gong, J.-Y. Yang, U. Ramamurty, and F. W. Zok, “In-Plane Mechanical Properties of an All-Oxide Ceramic Composite,” J. Am. Ceram. Soc., 82 [10] 2721–30 (1999). 31E. A. V. Carelli, H. Fujita, J. Y. Yang, and F. W. Zok, “Effects of Thermal Aging on the Mechanical Properties of a Porous-Matrix Ceramic Composite,” in review. 32G. W. Franks and F. F. Lange, “Plastic Clay-like Flow Stress of Saturated Advanced Ceramic Powder Compacts,” J. Eur. Ceram. Soc., in press. 33M. Holmquist, T. C. Radsick, O. Sudre, F. F. Lange, and F. W. Zok, “Fabrication and Testing of All-Oxide CFCC Tubes,” to be submitted. 34F. F. Lange, T. C. Radsick, and M. Holmquist, “Oxide/Oxide Composites: Control of Microstructure and Properties”; pp. 587–99 in Proceedings of the 4th International Conference on High Temperature Ceramic Matrix Composites. Edited by W. Krenkel, R. Naslain, and H. Schneider. Wiley-VCH, New York, 2001. Fig. 9. Load versus displacement plots for notched composites reinforced with N720 or N610 fibers, in as-processed condition and after aging. October 2003 Porous Oxide Matrix Composite Reinforced with Oxide Fibers 1739