Abstract
The conversion to ceramic of a commercial polycarbosilane (PCS) under various pyrolysis conditions has been investigated. The products of pyrolysis have been characterised by solid state 29Si and 13C NMR spectroscopy and X-ray diffraction (XRD). Some of the phases identified in the present study were found to differ from those reported previously, particularly in the earlier literature. Oxidation-cured PCS, when pyrolyzed up to 1400 °C in argon, generally produced silicon oxycarbide (SiO x C y ) as the second major phase with β-SiC as the major phase, and smaller amounts of free carbon. With increasing temperature above 1200 °C, the silicon oxycarbide phase decomposed to give β-SiC. Silica (SiO2) was also found to evolve from this silicon oxycarbide phase. Loss of some of the silica, probably by reaction with carbon, was found at 1400 °C, possibly yielding SiO, CO and SiC. At 1500 °C, crystalline α-cristobalite was found as a minor phase with β-SiC as the major phase and a lower amount of free carbon. Pyrolysis in vacuum leads to production and crystallization of β-SiC at a lower temperature than required if pyrolyzed in argon flow. After pyrolysis at 1600 ° in vacuum, the cured PCS converted to almost stoichiometric β-SiC.
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H. Q. Ly, R. Taylor, R. J. Day and F. Heatley, J.Mater.Sci. 36 (2001) 4037.
Y. Hasegawa and K. Okamura, J.Mater.Sci. 18 (1983) 3633.
Y. Hasegawa, ibid. 24 (1989) 1177.
M. Taki, K. Inui, K. Okamura and M. Sato, J.Mater. Sci.Lett. 8 (1989) 918.
G. Soraru, F. Babonneau and J. D. Mackenzie, J.Non-Cryst.Solids 106 (1988) 256.
Idem., J.Mater.Sci. 25 (1990) 3886.
E. Bouillon, F. Langlais, R. Pailler, R. Naslain, F. Cruege, P. V. Huong, J. C. Sarthou, A. Delpuech, C. Laffon, P. Lagarde, M. Monthioux and A. Oberlin, J.Mat.Sci. 26 (1991) 1333.
S. J. Ting, C. J. Chu and J. D. Mackenzie, J.Mater. Res. 7 (1992) 164.
M. Monthioux and O. Delverdier, J.Eur.Ceram.Soc. 16 (1996) 721.
K. Okamura, M. Sato, T. Matsuzawa and Y. Hasegawa, in “3rd Int. Conf. on Ultrastructure Processing of Ceramics, Glasses and Composites” (1987) pp. 501–518.
E. Bouillon, D. Mocaer, J. F. Villeneuve, R. Pailler, R. Naslain, M. Monthioux, A. Oberlin, C. Guimon and G. Pfister, J.Mater.Sci. 26 (1991) 1517.
Y. Sasaki, Y. Nishina, M. Sato and K. Okamura, J.Mater.Sci. 22 (1987) 443.
J. Lipowitz and G. L. Turner, Abstracts of Papers of the American Chemical Society 195 (1988) 74.
K. R. Carduner, G. R. Hatfield, W. A. Ellingson and S. L. Dieckman, in “Handbook of Ceramics and Composites,” Vol. 2, Mechanical Properties and Speciality Applications, edited by N. P. Cheremisinoff (Marcel Dekker, 1992) p. 465.
K. Okamura, M. Sato and Y. Hasegawa, J.Mater.Sci. Lett. 2 (1983) 769.
B. A. Bender, R. W. Rice and J. R. Spann, J.Amer. Ceram.Soc. 70 (1987) C-58.
R. J. Day, V. Piddock, R. Taylor, R. J. Young and M. Zakikhani, J.Mater.Sci. 24 (1989) 2898.
G. R. Hatfield and K. R. Carduner, ibid. 24 (1989) 4209.
T. Ishikawa, Comp.Sci.Technol. 51 (1994) 135.
Y. Maniette and A. Oberlin, J.Mater.Sci. 24 (1989) 3361.
Y. Xu, A. Zangvil, J. Lipowitz, J. A. Rabe and G. A. Zank, J.Amer.Ceram.Soc. 76 (1993) 3034.
L. C. Sawyer, M. Jamiesonz, D. Brikowski, M. Ishaq Haider and R. T. Chen, J.Amer.Ceram.Soc. 70 (1987) 798.
L. C. Sawyer, R. Arons, F. Haimbach, M. Jaffe and K. D. Rappaport, Ceram.Eng.Sci.Proc. 6 (1985) 567.
S. Yajima, K. Okamura, T. Matsuzawa, Y. Hasegawa and T. Shishido, Nature 279 (1979) 706.
A. R. Bunsell and M. H. Berger, Comp.Sci.Technol. 51 (1994) 127.
L. Porte and A. Sartre, J.Mater.Sci. 24 (1989) 271.
C. Laffon, A. M. Flank, P. Lagarde, M. Laridjani, R. Hagege, P. Olry, J. Cotteret, J. Dixmier, J. L. Miquel, H. Hommel and A. P. Legrand, ibid. 24 (1989) 1503.
P. Schreck, C. Vix-Guterl, P. Ehrburger and J. Lahaye, ibid. 27 (1992) 4243.
S. M. Bleay, A. R. Chapman, G. Love and V. D. Scott, ibid. 27 (1992) 5389.
P. Le Coustumer, M. Monthioux and A. Oberlin, J.Eur.Ceram.Soc. 11 (1993) 95.
B. Hahn, R. Weissmann and P. Greil, J.Mater.Sci.Lett. 15 (1996) 1243.
J. Lipowitz, H. A. Freeman, R. T. Chen and E. R. Prack, Adv.Ceram.Mater. 2 (1987) 121.
H. Zhang and C. G. Pantano, J.Amer.Ceram.Soc. 73 (1990) 958.
R. Pampuch, W. Ptak, S. Jonas and J. Stoch, Mater. Sci.Monographs 6 (1980) 435.
G. M. Renlund, S. Prochazka and R. H. Doremus, J.Mater.Res. 6 (1991) 2716.
F. Babonneau, G. D. Soraru, G. D'andrea, S. Dire and L. Bois, Mater.Res.Soc.Symp.Proc. 271 (1992) 789.
G. M. Renlund, S. Prochazka and R. H. Doremus, J.Mater.Res. 6 (1991) 2723.
R. J. P. Corriu, D. Leclercq, P. H. Mutin and A. Vioux, J.Mater.Sci. 30 (1995) 2313.
O. Delverdier, M. Monthioux, D. Mocaer and R. Pailler, J.Eur.Ceram.Soc. 12 (1993) 27.
H. Yao, S. Kovenklioglu and D. M. Kalyon, Chem. Eng.Comm. 96 (1990) 155.
M. Narisawa, S. Oda, S. Kitano and K. Okamura, J.Appl.Polym.Sci. 65 (1997) 261.
R. M. Silverstein, G. Clayton Bassler and T. C. Morrill, “Spectrometric Identification of Organic Compounds,” 5th edn. (Wiley, New York, 1991).
N. Hochet, M. H. Berger and A. R. Bunsell, J.Microsc.Oxford 185 (1997) 243.
H. P. Martin, G. Irmer, G. Schuster and E. Muller, Fresenius J.Anal.Chem. 349 (1994) 160.
Z. F. Zhang, F. Babonneau, R. M. Laine, Y. Mu, J. F. Harrod and J. A. Rahn, J.Amer.Ceram.Soc. 74 (1991) 670.
E. Lippmaa, M. Magi, A. Samoson, G. Engelhardt and A. R. Grimmer, J.Amer. Chem.Soc. 102 (1980) 4889.
G. D. Soraru, G. D'andrea, R. Campostrini, F. Babonneau and G. Mariotto, J.Amer.Ceram.Soc. 78 (1995) 379.
A. T. Hemida, R. Pailler and R. Naslain, J.Mater. Sci. 32 (1997) 2359.
S. Yajima, Ceram.Bull. 62 (1983) 893.
R. Bodet, N. Jia and R. E. Tressler, J.Eur.Ceram.Soc. 16 (1996) 653.
T. F. Cooke, J.Amer.Ceram.Soc. 74 (1991) 2959.
M. Monthioux, D. Cojean, O. Delverdier, P. Lecoustumer and V. Madigou, Microsc.Microanal. Microstruct. 2 (1991) 47.
W. D. Kingery, “Introduction to Ceramics,” 2nd edn. (Wiley-Interscience, 1976), p. 87.
V. G. Gerlivanov, R. A. Rabinovitch, N. M. Balagurova and N. N. Korneev, “Residual Stresses, II: Science and Technology,” Vol. 1 (Elsevier Science, UK, 1992), p. 567.
C. H. Andersson and R. Warren, Composites 15 (1984) 16.
V. D. Krstic, J.Amer.Ceram.Soc. 75 (1992) 170.
R. Bodet, N. Jia and R. E. Tressler, J.Eur.Ceram.Soc. 15 (1995) 997.
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Ly, H.Q., Taylor, R., Day, R.J. et al. Conversion of polycarbosilane (PCS) to SiC-based ceramic Part II Pyrolysis and characterisation. Journal of Materials Science 36, 4045–4057 (2001). https://doi.org/10.1023/A:1017994810727
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DOI: https://doi.org/10.1023/A:1017994810727