Hostname: page-component-77c89778f8-vpsfw Total loading time: 0 Render date: 2024-07-19T20:39:57.971Z Has data issue: false hasContentIssue false

Fabrication of Sic Matrix Composites by Liquid Phase Infiltration with a Polymeric Precursor

Published online by Cambridge University Press:  15 February 2011

Leonard V. Interrante
Affiliation:
Department of Chemistry, Rensselaer Polytechnic Institute, Troy, NY 12180-3590
C.W. Whitmarsh
Affiliation:
Starfire Systems, Inc, 877 25th Street, Watervliet, NY 12189
W. Sherwood
Affiliation:
Starfire Systems, Inc, 877 25th Street, Watervliet, NY 12189
Get access

Abstract

A process for the fabrication of SiC matrix composites has been developed which employs aliquid, highly branched, polycarbosilane (AHPCS). This polymer thermosets on heating at 200-400 °C (or at 100 °C with catalyst) and yields an amorphous SiC with low excess C and O content in 60-80% yield on pyrolysis to 1000 °C. Preforms consisting of C-coated Nicalon SiC fiber cloth, unidirectional Textron SiC SCS-6 fiber layups, or Mo boats packed with SiC whiskers, were infiltrated with the polymer, cured in an autoclave, and pyrolyzed to 1000 °C. Five to eight infiltration cycles gave net shape composites with final densities at 85-94 % of theoretical. The results of 4-point flexure tests on the as-prepared Nicalon composites indicate flexure strengths (aver. 378 MPa) that are comparable to or better than similarly reinforced CVI-SiC matrix composites. The whisker and SCS-6 composites showed a small weight loss (10-20%) on heating to 1500 °C in Ar and little or no weight change or obvious embrittlement in air at 1000 °C.

Type
Research Article
Copyright
Copyright © Materials Research Society 1995

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

[1] Naslain, R. and Langlais, F., MRS Sympos. Proc. 20, 145 (1985); P.J. Lamicq, G.Q. Bernhart, M.M. Dauchier, and J.C. Mace, Am. Ceram. Soc. Bull. 65[2], 336 (1986); A.J. Caputo, D.P. Stinton, R.A. Lowden, and T.M. Bessman, Am. Ceram. Soc. Bull. 66[2], 368 (1987); T.M. Bessman, R.A. Lowden, D.P. Stinton, T.L. Starr, J. de Physique, Colloque C5, 229 (1989).Google Scholar
[2] Yajima, S., Okamura, K., Hayashi, J., and Imura, M., J. Amer. Ceram. Soc. 59[7-8] 324 (1976); S. Yajima, Y. Hasegwa, J. Hayashi, and M. Omori, J. Mater. Sci. 13[12] 2569 (1978); S. Yajima, “Silicon Carbide Fibers”, pp. 201-37, in Handbook of Composites, edited by W. Watt and B.V. Perov, North-Holland, Amsterdam, Netherlands, (1985).Google Scholar
[3] K. Okamura, “Ceramic Fiber and Whisker Requirements to Advanced Structural Inorganic Composite”, pp. 1934 in Advanced Structural Composites, edited by Vicenzini, P., Elsevier Science Publ. B.V., Amsterdam (1991); J. Lipowitz, Am. Ceram. Soc. Bull. 70[12], 1888 (1991); T.F. Cooke, J. Amer. Ceram. Soc.,74[12] 2959 (1991).Google Scholar
[4] Hurwitz, F.I., Hyatt, L., Gorecki, J., and D'Amore, L., Ceram. Eng. Sci. Proc. 8, 732 (1987); F.I. Hurwitz, J.Z. Gyekenyesi, and P.J. Conroy, Ceram. Eng. Sci. Proc. 10, 750 (1989); H. Zhang, C.G. Pantano, pp. 223-, in Ultrastructure Processing of Advanced Materials, D.R. Uhlmann and D.R. Ulrich, Eds., John Wiley &Sons (1992).Google Scholar
[5] Sato, K., Suzuki, T., Funayama, O., and Isoda, T., J. Ceram. Soc. Japan 100[4] 444 (1992).Google Scholar
[6] Fohey, W., Battison, M., Halada, J., and Nielson, T., U.S. Government Report No. WL-TR-92-4019, July 1992.Google Scholar
[7] Strife, J.R., Wesson, J.P., and Streckert, H.H., “A Study of the Critical Factors Controlling the Synthesis of Ceramic Matrix Composites from Preceramic Polymers”, US Government Report No. AD-A23 686, December 1990; B.C. Mutsuddy, Ceramics International 13, 41 (1987); R.P. Boisvert, “Ceramic Matrix Composites via Organometallic Precursors”, M.S. Thesis, Rensselaer Polytechnic Institute, 214 pages (1988).Google Scholar
[8] Wu, H-J. and Interrante, L.V., Macromolecules 25, 1840 (1992); H.-J. Wu and L.V. Interrante, Polymer Preprints 33[2], 210 (1992).Google Scholar
[9] Interrante, L.V., Whitmarsh, C.W., Sherwood, W., Wu, H-J., Lewis, R. and Maciel, G., MRS Sympos. Proc. 346, 593 (1994).Google Scholar
[10] Whitmarsh, C.W., Interrante, L.V., Organometallics 10, 1336 (1991); C.W. Whitmarsh, L.V. Interrante, “Carbosilane Polymer Precursors to Silicon Carbide Ceramics”, U.S. Patent No. 5 153 295 (6 October 1992);.Google Scholar
[11] Yang, C-Y. and Interrante, L.V., Polymer Preprints 33 [2], 152 (1992).Google Scholar
[12] Recent (proprietary) process improvements have resulted in a polymer whose composition is very close to the expected SiH2CH2 formula. These same process improvements provide a higher yield of the polymer per reactor run and reduce the overall time required for the polymerization reaction to 1 day (from ca. 5 days).Google Scholar
[13] The polymer has been prepared in our own laboratory many times on a 12L reactor scale (yielding ca. 250 mL of product) and has been scaled up to the 100 gallon reactor level at a chemical company under contract to Rensselaer.Google Scholar
[14] Wu, H-J. and Interrante, L.V., to be published.Google Scholar
[15] Interrante, L.V., Whitmarsh, C.W., Yang, C-Y., Sherwood, W., Schmidt, W., Marchetti, P.S. and Maciel, G.E., Ceramic Trans. 42, 57 (1994).Google Scholar
[16] Harrod, J., Laine, R. et al. , J. Amer. Ceram. Soc. 74, 670 (1991).Google Scholar
[17] Elemental analysis of the 1000°C 5%-AHPCS-SiC gave the following results: %C, 27.7; %0, 5.5; Si (by difference) 66.8; [(SiC)2.2(SiO2)0.17(C) 0.10].Google Scholar
[18] The % theoretical density was calculated from the rule of mixtures, using the relative weights and the published density values for the Nicalon fiber cloth. A value of 2.35g/cm3 was used for the density of the AHPCS-SiC matrix material. This was obtained by direct measurement on a densified pellet of 1000 oC AHPCS-SiC. The pellet was prepared by VPIP (8 cycles) starting from a preform derived by hot-pressing (200°C; 360 kg/cm2) a mixture of finely-ground 1000°C AHPCS-SiC powder and HPCS as a binder in a pellet press.Google Scholar
[19] duPont de Nemours & Co., Wilmington, DE, Product Data Sheet.Google Scholar