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Hydrocarbon-Bridged Polysiloxane and Polysilsesquioxane Network Materials. §

Published online by Cambridge University Press:  21 February 2011

Gregory M. Jamison
Affiliation:
Properties of Organic Materials Department, Sandia National Laboratories, Albuquerque, New Mexico 87185-0367
Douglas A. Loy
Affiliation:
Properties of Organic Materials Department, Sandia National Laboratories, Albuquerque, New Mexico 87185-0367
Roger A. Assinkt
Affiliation:
Properties of Organic Materials Department, Sandia National Laboratories, Albuquerque, New Mexico 87185-0367
Kenneth J. Shea
Affiliation:
Department of Chemistry, University of California Irvine, Irvine, California 92717
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Abstract

Hexylene-and phenylene-bridged polymethylsiloxane xerogels X-2 and X-4, respectively, were prepared by the sol-gel hydrolysis and condensation of 1, 6-bis(diethoxymethyl-silyl)hexane 1 and 1, 4-bis(diethoxymethysilyl)benzene 2 under acidic and basic conditions. These polymerizations afforded network polymers in the form of wet gels within several hours. The gels were processed to afford xerogels whose characteristics (determined by solid state 13C and 29Si CP MAS NMR spectroscopy and nitrogen sorption porosimetry) were compared and contrasted with those of their analogous polysilsesquioxanes. 29Si CP MAS NMR indicates a high, degree of hydrolysis and polycondensation; porosimetry measurements reveal that the materials have significant surface areas, save for the acid-catalyzed hexylene gels X-2.

Type
Research Article
Copyright
Copyright © Materials Research Society 1998

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Footnotes

§

This research was supported by the United States Department of Energy under contract No.DE-AC04-94AL85000.

§

This research was supported by the United States Department of Energy under contract No. DE-AC04-94AL85000.

References

1 (a) Shea, K. J., Loy, D. A. and Webster, O. W., J. Am. Chem. Soc. 114,6700 (1992). (b) K. J. Shea, D. A. Loy, D. A. and O. W. Webster, Chem. Mater. 1, 572 (1989). (c) K. J. Shea, O. W. Webster and D. A. Loy in Better Ceramics Through Chemistry IV edited by B. J. J. Zelinski, C. J. Brinker, D. E. Clark and D. R. Ulrich, (Mater. Res. Soc. Proc, 180, Pittsburgh, PA 1990), p. 975. (d) K. J. Shea, D. A. Loy, O. W. Webster, Proceedings of ACS Division of Polymeric Materials Science and Engineering 63, (1990), p. 281. (e) K. J. Shea, D. A. Loy, E. M. Russick, in Better Ceramics Through Chemistry V edited by M. J. Hampden-Smith, W. G. Klemperer and C. J. Brinker, (Mater. Res. Soc. Proc, 271, Pittsburgh, PA 1992), p. 699. (f) R. J. P. Corriu, J. J. E. Moreau, P. Thepot, M. W. C. Man, Chem. Mater. 4, 1217, (1992). (g) J. H. Small, K. J. Shea, D. A. Loy, J. Non- Cryst. Solids, 160, 234, (1993).CrossRefGoogle Scholar
2 Jamison, G. M., Loy, D. A., Shea, K. J., Chem. Mater. 5, 1193, (1993).CrossRefGoogle Scholar
3 Oviatt, H. W. Jr., Shea, K. J., Small, J. H., Chem. Mater. 5, 943, (1993).CrossRefGoogle Scholar
4 Experiments are underway to determine the effect, if any, of solvent on the final surface area of the hexylene-bridged gels. No effect was noticed with phenylene-bridged polysilsesquioxanes.Google Scholar
5 Solid State 13C and 29Si CP MAS NMR experiments were carried out using 1.5 millisecond cross polarization times with 4 second delays over 4096 averages.Google Scholar
6 The peaks correspond with those seen in the solution 13C NMR spectrum of monomer 2: 13C NMR (100.6 MHz, CDC13) δ 57.9 (£H20), 32.8 (a), 22.6 (b), 18.3 (ÇH3CH2O), 13.75(c),-5.0(d).Google Scholar
7 The 29Si NMR resonance for the unreacted monomer 2 lies at -4.3 ppm.Google Scholar
8 No T0 resonances are observed in the bridged polysilsesquioxanes and are presumed to lie below the detection threshold for solid state 29Si CP MAS NMR.Google Scholar
9 Lowell, S; Shields, J. E. Powder Surface Area and Porosity; Chapman and Hall: London, 1984.CrossRefGoogle Scholar

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