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Engineering of Porosity in Amorphous Materials. Plasma Oxidationof Hydrocarbon Templates in Polysilsesquioxanes*

Published online by Cambridge University Press:  21 February 2011

Douglas A. Loy
Affiliation:
Sandia National Laboratories, Albuquerque, NM 87185
Richard J. Buss
Affiliation:
Sandia National Laboratories, Albuquerque, NM 87185
Roger A. Assink
Affiliation:
Sandia National Laboratories, Albuquerque, NM 87185
Kenneth J. Shea
Affiliation:
Department of Chemistry, University of California, Irvine, CA 92717.
Henry Oviatt
Affiliation:
Department of Chemistry, University of California, Irvine, CA 92717.
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Abstract

Arylene- and alkylene-bridged polysilsesquioxanes were prepared by sol-gelprocessing of bis(triethoxysilyl)-arylene monomers 1-4, and alkylenemonomers 5-9. The arylene polysilsesquioxanes were porous materials withsurface areas as high as 830 m2/g (BET). Treatment with aninductively coupled oxygen plasma resulted in the near quantitative removalof the arylene bridging groups and a coarsening of the pore structure. Solidstate 29Si NMR was used to confirm the conversion of thesesquioxane silicons (T) to silica (Q). The alkylene-bridgedpolysilsesquioxanes were non-porous. Oxygen plasma treatment afforded silicagels with mesoporosity. The porosity in the silica gels appears to ariseentirely from the oxidation of the alkylene spacers.

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Type
Research Article
Copyright
Copyright © Materials Research Society 1998

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References

REFERENCES

1 Brinker, C. J., Scherer, G. W., Sol-Gel Science (Academic Press: London, 1990).Google Scholar
2 Agaskar, P. A., J. Am. Chem. Soc. III, 6858 (1989).Google Scholar
3 Kaszynski, P., Michl, J., J. Am. Chem. Soc. 110, 5225 (1988).Google Scholar
4 Day, V. W., Klemperer, W. G., Mainz, V. V., Miller, D. M., J. Am. Chem.Soc. 107, 8262 (1985).Google Scholar
5 Dines, M. B., DiaGiacomo, P. M., Inorg. Chem. 20, 92 (1981).Google Scholar
6 Shea, K. J., Loy, D. A., Webster, O. W., Chem. Mater. 512 (1989).Google Scholar
7 Shea, K.J., Loy, D. A., Webster, O. W., J. Am. Chem. Soc. 114, 6700 (1992).Google Scholar
8 Chujo, Y., Ihara, E., Kure, S., Susuki, K., Saegusa, T., Makromol. Chem., Macromol. Symp., 42/43 (Int. Symp. Ring Opening Cyclopolym., 6th, 1990), pp 303-12.Google Scholar
9 Roger, C., Hampden-Smith, M. J., Brinker, C. J. in Better Ceramics Through Chemistry V edited by Hampden-Smith, M. J., Klemperer, W. G., and Brinker, C. J. (Mater. Res. Soc. Symp. Proc.271 Pittsburgh, PA 1992), p. 51.Google Scholar
10 Loy, D. A., Ph.D. Dissertation, University of California at Irvine, 1991.Google Scholar
11 Small, J. H., Shea, K. J., Loy, D. A., J. Non-Cryst. Solids 160, 234 (1993).Google Scholar
12 Oviatt, H., Shea, K. J., Small, J. H., Chem. Mater. 5, 943 (1993).Google Scholar
13 Loy, D. A., Russick, E., Shea, K. J. in Better Ceramics Through Chemistry V. edited by Hampden-Smith, M. J., Klemperer, W. G., and Brinker, C. J. (Mater. Res. Soc. Symp. 271 Proc. Pittsburgh, PA 1992), p. 699.Google Scholar
14 T resonances in the 29Si NMR spectra arise from silicon species with one substituent attached through a carbon-silicon bond and three substituents attached with silicon-oxygen bonds: RSi(OH)3 = T°, [RSiO1.5] n= T3.Google Scholar
15 Brunauer, S., Emmett, P. H., Teller, E., J. Am. Chem. Soc. 60, 309 (1938).Google Scholar