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New Structures of Preceramic Polysilazanes Synthesized by Transition Metal Catalysis

  • Yigal D. Blum (a1), Kenneth B. Schwartz, Edward J. Crawford and Richard D. Hamlin

Abstract

Further capability of silazane dehydrocoupling polymerization catalyzed by ruthenium carbonyl (20–200 ppm) is demonstrated in a series of reactions. Ammonia and monomethylamine are used as reactants to bridge oligomers and polymers containing Si-H bonds to provide higher molecular weight polymers with higher latent reactivity and to increase the ceramic yields and the nitrogen-to-carbon ratio in the final ceramic compositions. New types of tractable polymers containing cyclomers having [MeSiHNH] units with molecular weights over 2000 d are formed. Various polymeric properties (e.g., viscosities, softening and melting points) and ceramic yields up to 80–85 wt% are obtained by controlling the catalytic reaction conditions.

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1. Laine, R. M., Blum, Y. D., Tse, D., and Glaser, R., in Inorganic and Organometallic Polymers, ACS Symposium Series 360, edited by Zeldin, M., Wynne, K. J., and Allcock, H. R. (ACS, Washington, DC, 1988), p. 124.
2. (a) Blum, Y. D. and Laine, R. M., Organomet. 5, 2081 (1986);
(b) Laine, R. M. and Blum, Y. D., U.S. Patent No. 4, 383 (Sept. 1986);
(c) Blum, Y. D., Laine, R. M., Schwartz, Y. D., Rowcliffe, D. J., Bening, R. C., and Cotts, D. C., in Better Ceramics Through Chemistry II, Mat. Res. Soc. Symp. Proc, Vol. 73, edited by Brinker, C. J., Clark, D. E., and Ulrich, D. R. (Materials Research Society, 1986), p. 389;
(d) Schwartz, K. B., Rowcliffe, D. J., Blum, Y. D., and Laine, R. M., in Better Ceramics Through Chemistry II, Mat. Res. Soc. Symp. Proc, Vol. 73, edited by Brinker, C. J., Clark, D. E., and Ulrich, D. R. (Materials Research Society, 1986), p. 389; p. 407;
(e) Chow, A. W., Hamlin, R. D., Blum, Y. D., and Laine, R. M., J. Pol. Sci.: Part C: Pol. Lett., 26, 103 (1988).
3. (a) Laine, R. M., Blum, Y. D., Hamlin, R. D., and Chow, A., in Ultrastructure Processing of Glass, Ceramics and Composites III, edited by Mackenzie, D. D. and Ulrich, D. R., (J.Wiley and Sons Inc., (in press);
(b) Biran, C., Blum, Y. D., Glaser, R., Tse, D., Youngdahl, K. A., and Laine, R. M., submitted to J. Mol. Catal. (1988).
4. (a) Schwartz, K. B., Rowcliffe, D. J., and Blum, Y. D., Comm. Am. Cer. Soc, in press;
(b) Lenhart, S. J., Blum, Y. D., and Laine, R. M., submitted to J. Corrosion.
5. Seyferth, D. and Wiseman, G. H., Am. Chem. Soc, Polymer Div. Polym. Prprt. 25 (1984), p. 10.
6. Blum, Y. D., Schwartz, K. B., and Laine, R. M., submitted to J. Mat. Sci.
7. Arai, M., Isoda, T., and Funayama, O., U.S Patent No. 4, 659, 850 (21 April 1987).
8. Matsutomo, M., Niwada, K., and Tanaka, S., Japan Patent No. 61 72, 607 (14 April 1986).
9. (a) Seyferth, D. and Wiseman, G. H., U.S. Patent No. 4,482,669
(b) Seyferth, D., Wiseman, G. H., Schwark, J. M., Yu, Y. F., and Charles, C. A., U.S. Patent No. 4,482,669 [1], p. 143.

New Structures of Preceramic Polysilazanes Synthesized by Transition Metal Catalysis

  • Yigal D. Blum (a1), Kenneth B. Schwartz, Edward J. Crawford and Richard D. Hamlin

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