M. Verdenelli et al / Journal of the European Ceramic Society 23(2003)1207-1213 Table 3 and SrZrO3 coatings on SiC and C-fibers. J. Mater. Sci., 1999, 34 Tensile tests the coated SiC fibres for systems I and 2 after 4031-4037 nnealing at 600 and 1200C 6. Parola, S. Verdenelli, M.. Sigala. C. Scharff, J. P. Velez. K. Veytizou, C, and Quinson, J F. Sol-gel coatings on non-oxide SIC Hi-Nicalon Coated Hi-Nicalon Hi- Nicalon treated at1200° C treated at1200° planar substrates and fibers: a protection barrier against oxida- In aIr tion and corrosion. J. Sol-Gel Sci. Tech (in press). 7. Hashishin, T, Murashita, J, Joyama, A and Kaneko, Y Tensile strength(MPa) 3000 2170 dation-resistant coating of carbon fibers with TiO, b ethod Weibull modulus 8. Aparicio, M. and Duran, A, Yttrium silicate coatings for oxida- tion protection of carbon-silicon carbide compo 9. Gundel, D. B, Taylor, P J and Wawner, F. E, Fabrication of The original mechanical properties were preserved thin oxide coatings on ceramic fibres by a sol-gel technique. J. after the deposition of the oxide. Moreover, at high arer.Sci,1994,29,1795-1800. temperatures in an oxidative atmosphere, the mechan 10. Karlin, S and Colomban, Ph, Micro-Raman study of Sic fibre. ical behaviours were much better with a coated fibre 11. Colomban, Ph. Bruneton, E, Lagrange, J. L and Mouchon, E than with the uncoated ones Sol-gel mullite matrixSiC and-mullite 2D woven fabric compo- sites interphase: elaboration and properties. Eur. Ceram. Soc., 4. Conclusion 12. Brinker. C. J and Scherer. G. W.. Sol-Gel Science: The Physics ad Chemistry of Sol-Gel Processing. Academic Press, San Diego, Thin films of mixed silicon/aluminium oxides on SiC 13. Turova, N Ya, Turevskaya, E. P, Kessler, V.G. and Yanovs- Hi-Nicalon fibres were successfully elaborated using the kaya, M. I, The Chemistry of Metal Alkoxides. Kluwer Academic Publishers. Norwell MA. 2001 oI-gel process. The coated fibres were stable in an oxi- 14. Bradley, D. C, Mehrotra, R C and Gaur, D. P, Metal alk- lative environment even at high temperatures(1200C) oxides. Academic Press. London. 1978 The protective role of the oxides was thus demon 15. Sanchez, C, Livage, J, Henry, M. and Babonneau, F, Chemical strated, as well as the good mechanical behavior of the odification of alkoxide precursors. J. Non-Cryst. Solids, 1988, fibre/coating system. These porous coatings are there 100,65-76 fore potential interphases for applications in Ceramic Matrix Composites and micro-composites SiC/Oxide/ S, Tin dioxide thin films from Sn(Iv) modified alkoxides- synthesis and structural characterization of Sn(OEt)2(acac)2 and Sic which are currently under investigation Sn(O)(oEt)o(acac)2. Polyhedron, 2000, 10, 2069-2075. 17. Velez, K, Quinson, J. F and Fenet, B, Modification study of Acknowledgements 18. Nass, R and Schmidt, H, Synthesis of an alumina coating from chelated aluminium alkoxide Non-Cryst. Solids, 1990, 12 The authors wish to thank the cnrs for fina support 19. Patankar, S.N., Weibull distribution as applied to ceramic fibres J. Mater.Sci.Let,1991,10,1176-1 20. Kresge, C.T., Leonowicz, M. E, Roth, w.J., Vartuli, J. C and Beck, J.S. Ordered mesoporous molecular sieves by a liquid- Referen crystal template mechanism. Nature, 1992, 359, 710-712. 21. Monnier, A, Schuth, F, Huo, Q, Kumar, D, Margolese, 1. Carpenter, H. W. and Bohlen, J. w, Fibers coatings for D, Maxwell, R. S, Stucky, G. D, Krishnamurty, M, Petr- matrix composites. Ceram. Eng. Sci. Proc., 1992. 13(7 ff, P, Firouzi, A, Janicke, M. and Chmelka, B. F, Coop- 6 H.W. Carpenter, J Bohlen and N.s. Steffier, Weak fr erative formation of inorganic-organic interfaces in the fiber coating with unfilled pores for toughening ceramic fiber synthesis of silicate mesostructures. Science, 1993, 261, 1299- matrix composites, US Patent No. 5.221. 578, 1992 1303. 2. Reig, P, Demazeau, G. and Naslain, R, KMg2AISi4O12 phyllo- 2. Murakata, T, Sato. S, Ohgawara, T, Watanabe, T and process using inorganic salts, surfactants as additives. J 3. Tressler, R. E, Recent developments in fibers and interphases for high temperature ceramic matrix composites Composites: Part A 23. Zhou, H.S. Kundu, D. and Honma, I, Synthesis of oriented 4. Cinibulk, M. K. and Hay, R.S., Ter magnetoplumbite 13 fiber-matrix interphase derived from sol-gel fiber coatings. J. Am. 24. Goucher, F.S. and Ward, H, A problem in viscosity: the thick- eram.Soc,1996.795),1233-1246 ness of liquid films formed on solid surfaces under dynami 5. Wurm. R, Dernovsek, O. and Greil, P. Sol-gel derived SrTiO ditions. Phil Mag. 6th Ser., 1922, 44, 1002-1014The original mechanical properties were preserved after the deposition of the oxide. Moreover,at high temperatures in an oxidative atmosphere,the mechan￾ical behaviours were much better with a coated fibre than with the uncoated ones. 4. Conclusion Thin films of mixed silicon/aluminium oxides on SiC Hi-Nicalon fibres were successfully elaborated using the sol-gel process. The coated fibres were stable in an oxi￾dative environment even at high temperatures (1200
C). The protective role of the oxides was thus demon￾strated,as well as the good mechanical behavior of the fibre/coating system. These porous coatings are there￾fore potential interphases for applications in Ceramic Matrix Composites and micro-composites SiC/Oxide/ SiC which are currently under investigation. Acknowledgements The authors wish to thank the CNRS for financial support. References 1. Carpenter,H. W. and Bohlen,J. W.,Fibers coatings for ceramic matrix composites. Ceram. Eng. Sci. Proc.,1992, 13(7–8),238– 256 H.W. Carpenter,J. Bohlen and N.S. Steffier,Weak frangible fiber coating with unfilled pores for toughening ceramic fiber￾matrix composites,US Patent No. 5.221.578,1992. 2. Reig,P.,Demazeau,G. and Naslain,R.,KMg2AlSi4O12 phyllo￾siloxide as potential interphase material for ceramic matrix com￾posites. J. Mater. Sci.,1997, 32,4195–4200. 3. Tressler,R. E.,Recent developments in fibers and interphases for high temperature ceramic matrix composites. Composites: Part A, 1999, 30,429–437. 4. Cinibulk,M. K. and Hay,R. S.,Textured magnetoplumbite fiber-matrix interphase derived from sol-gel fiber coatings. J. Am. Ceram. Soc.,1996, 79(5),1233–1246. 5. Wurm,R.,Dernovsek,O. and Greil,P.,Sol-gel derived SrTiO3 and SrZrO3 coatings on SiC and C-fibers,J. Mater. Sci.,1999, 34, 4031–4037. 6. Parola,S.,Verdenelli,M.,Sigala,C.,Scharff,J.P.,Velez,K. Veytizou,C.,and Quinson,J.F. Sol-gel coatings on non-oxide planar substrates and fibers: a protection barrier against oxida￾tion and corrosion. J. Sol-Gel Sci. Tech. (in press). 7. Hashishin,T.,Murashita,J.,Joyama,A. and Kaneko,Y.,Oxi￾dation-resistant coating of carbon fibers with TiO2 by sol-gel method. J. Ceram. Soc. Jap. Int. Ed.,1998, 106,4–8. 8. Aparicio,M. and Dura´n,A.,Yttrium silicate coatings for oxida￾tion protection of carbon-silicon carbide composites. J. Am. Ceram. Soc.,2000, 83(6),1351–1355. 9. Gundel,D. B.,Taylor,P. J. and Wawner,F. E.,Fabrication of thin oxide coatings on ceramic fibres by a sol-gel technique. J. Mater. Sci.,1994, 29,1795–1800. 10. Karlin,S. and Colomban,Ph.,Micro-Raman study of SiC fibre￾oxide matrix reaction. Composites Part B,1998, 29B,41–50. 11. Colomban,Ph.,Bruneton,E.,Lagrange,J. L. and Mouchon,E., Sol-gel mullite matrix-SiC and-mullite 2D woven fabric compo￾sites interphase: elaboration and properties. J. Eur. Ceram. Soc., 1996, 16,301–314. 12. Brinker,C. J. and Scherer,G. W., Sol-Gel Science: The Physics and Chemistry of Sol-Gel Processing. Academic Press,San Diego, 1990. 13. Turova,N.Ya.,Turevskaya,E. P.,Kessler,V. G. and Yanovs￾kaya,M. I., The Chemistry of Metal Alkoxides. Kluwer Academic Publishers,Norwell MA,2001. 14. Bradley,D. C.,Mehrotra,R. C. and Gaur,D. P., Metal Alk￾oxides. Academic Press,London,1978. 15. Sanchez,C.,Livage,J.,Henry,M. and Babonneau,F.,Chemical modification of alkoxide precursors. J. Non-Cryst. Solids,1988, 100,65–76. 16. Verdenelli,M.,Parola,S.,Hubert-Pfalzgraf,L. G. and Lecocq, S.,Tin dioxide thin films from Sn(IV) modified alkoxides— synthesis and structural characterization of Sn(OEt)2(acac)2 and Sn4(O)2(OEt)10(acac)2. Polyhedron,2000, 10,2069–2075. 17. Velez,K.,Quinson,J. F. and Fenet,B.,Modification study of aluminium sec-butoxide by acrylic acid. J. Sol-gel Sci. Technol, 1999, 16,201–208. 18. Nass,R. and Schmidt,H.,Synthesis of an alumina coating from chelated aluminium alkoxides. J. Non-Cryst. Solids,1990, 121, 329–333. 19. Patankar,S. N.,Weibull distribution as applied to ceramic fibres. J. Mater. Sci. Let.,1991, 10,1176–1181. 20. Kresge,C. T.,Leonowicz,M. E.,Roth,W. J.,Vartuli,J. C. and Beck,J. S.,Ordered mesoporous molecular sieves by a liquid￾crystal template mechanism. Nature,1992, 359,710–712. 21. Monnier,A.,Schu¨th,F.,Huo,Q.,Kumar,D.,Margolese, D.,Maxwell,R. S.,Stucky,G. D.,Krishnamurty,M.,Petr￾off,P.,Firouzi,A.,Janicke,M. and Chmelka,B. F.,Coop￾erative formation of inorganic-organic interfaces in the synthesis of silicate mesostructures. Science,1993, 261,1299– 1303. 22. Murakata,T.,Sato,S.,Ohgawara,T.,Watanabe,T. and Suzuki, T.,Control of pore size distribution of silica gel through sol-gel process using inorganic salts,surfactants as additives. J. Mater. Sci.,1992, 27,1567–1574. 23. Zhou,H. S.,Kundu,D. and Honma,I.,Synthesis of oriented meso-structure silica functional thin film. J. Eur. Ceram. Soc., 1999, 19,1361–1364. 24. Goucher,F. S. and Ward,H.,A problem in viscosity: the thick￾ness of liquid films formed on solid surfaces under dynamic con￾ditions. Phil. Mag. 6th Ser.,1922, 44,1002–1014. Table 3 Tensile tests on the coated SiC fibres for systems 1 and 2 after annealing at 600 and 1200
C SiC Hi-Nicalon Hi-Nicalon treated at 1200
C in air Coated Hi-Nicalon treated at 1200
C in air Tensile strength (MPa) 3000 2170 2970 Tensile modulus (GPa) 270 230 270 Weibull modulus 6.9 5.5 4.8 M. Verdenelli et al. / Journal of the European Ceramic Society 23 (2003) 1207–1213 1213