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A silicon-29 NMR study of the structural intermediates in low pH sol-gel reactions

Published online by Cambridge University Press:  31 January 2011

L. W. Kelts  and
N. J. Armstrong
L. W. Kelts
Affiliation:
Corporate Research Laboratories, Eastman Kodak Company, Rochester, New York 14650
N. J. Armstrong
Affiliation:
Corporate Research Laboratories, Eastman Kodak Company, Rochester, New York 14650
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Abstract

Silicon-29 NMR is used to study the structural intermediates in tetramethyl and tetraethyl orthosilicate (TMOS and TEOS) low pH sol-gel reactions. Differences in the number of compact ring structures are related to differences in gel times. Reactions are followed at various silicon: water: acid molar ratios.

Type
Articles
Information
Journal of Materials Research , Volume 4 , Issue 2 , April 1989 , pp. 423 - 433
Copyright
Copyright © Materials Research Society 1989

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References

REFERENCES

1Yoldas, B.E., J. Non-Cryst. Solids 51, 105–121 (1982).CrossRefGoogle Scholar
2Partlow, D.P. and Yoldas, B.E., J. Non-Cryst. Solids 46, 153–161 (1981).CrossRefGoogle Scholar
3Makherju, S. P., J. Non-Cryst. Solids 42, 477–488 (1980).Google Scholar
4Uhlmann, D.R., Zelinski, B.J., and Wnek, G. E., in “The Ceramist as Chemist–Opportunities for New Materials,” in Better Ceramics through Chemistry, edited by Brinker, C. J., Clark, D. E., and Ulrich, D. R. (Elsevier, New York, 1984), pp. 59–70.Google Scholar
5Klemperer, W. G., Mainz, V.V., and Millar, D. M., in “A Molecular Building Block Approach to the Synthesis of Ceramic Materials,” in Better Ceramics through Chemistry II, edited by Brinker, C.J., Clark, D. E., and Ulrich, D. R. (Materials Research Society, Pittsburgh, PA, 1986), pp. 3–15.Google Scholar
6Assink, R. A. and Kay, B. D., in “H NMR Studies of the Sol-Gel Transition,” in Better Ceramics through Chemistry, edited by Brinker, C.J., Clark, D. E., and Ulrich, D. R. (Elsevier, New York, 1984), pp. 301–306.Google Scholar
7Kelts, L. W., Effinger, N. J., and Melpolder, S. M., J. Non-Cryst. Solids 83, 353–374 (1986).CrossRefGoogle Scholar
8The probe was designed and built by Bruker Instruments Inc.Google Scholar
9Turner, C.W. and Franklin, K.J., J. Non-Cryst. Solids 91, 402–415 (1987).Google Scholar
10Chen, K. C., Tsuchiya, T., and Mackenzie, J. D., J. Non-Cryst. Solids 81, 221–231 (1986).CrossRefGoogle Scholar
11Schmidt, H., Scholze, H., and Kaiser, A., J. Non-Cryst. Solids 63, 1–11 (1984).Google Scholar
12Schmidt, H. and Seiferling, B., in “Chemistry and Applications of Inorganic-Organic Polymers (Organically Modified Silicates),” in Better Ceramics through Chemistry II, edited by Brinker, C. J., Clark, D. E., and Ulrich, D. R. (Materials Research Society, Pittsburgh, PA, 1986), pp. 739–750.Google Scholar
13Klemperer, W. G. has recently suggested that MeOH and HCl in these solutions will form MeCl and H2O (“Molecular Growth Pathways in Silica Sol-Gel Polymerization,” a seminar at the Better Ceramics through Chemistry III, April 1988, MRS Spring Meeting, Reno, NV). This reaction could account for a large amount of the extra hydrolysis observed, but we don't see its formation.CrossRefGoogle Scholar
14Harris, R. K., Jones, J., and Knight, C. T. G., J. Mol. Spectrosc. 69, 95–103 (1980).Google Scholar
15Harris, R. K. and Knight, C. T. G., J. Mol. Spectrosc. 78, 273–278 (1982).Google Scholar
16Harris, R. K. and Knight, C.T. G., J. Chem. Soc. Faraday Trans. 79, 1525–1538 (1983).CrossRefGoogle Scholar
17Harris, R. K. and Knight, C. T. G., J. Chem. Soc. Faraday Trans. 79, 1539–1561 (1983).Google Scholar
18Harris, R. K., Knight, C. T. G., and Hull, W. E., J. Am. Chem. Soc. 103, 1577–1578 (1981).CrossRefGoogle Scholar
19Her, R. K., The Chemistry of Silica (John Wiley and Sons Inc., New York, 1979).Google Scholar
20Russo, R.E. and Hunt, A.J., J. Non-Cryst. Solids 86, 219–230 (1986).CrossRefGoogle Scholar