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

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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.

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References

  1. B. E. Yoldas, J. Non-Cryst. Solids 51, 105–121 (1982).

    Article  CAS  Google Scholar 

  2. D. P. Partlow and B. E. Yoldas, J. Non-Cryst. Solids 46, 153–161 (1981).

    Article  CAS  Google Scholar 

  3. S. P. Makherju, J. Non-Cryst. Solids 42, 477–488 (1980).

    Article  Google Scholar 

  4. D. R. Uhlmann, B. J. Zelinski, and G. E. Wnek, in “The Ceramist as Chemist — Opportunities for New Materials,” in Better Ceramics through Chemistry, edited by C. J. Brinker, D. E. Clark, and D. R. Ulrich (Elsevier, New York, 1984), pp. 59–70.

    Google Scholar 

  5. W. G. Klemperer, V. V. Mainz, and D. M. Millar, in “A Molecular Building Block Approach to the Synthesis of Ceramic Materials,” in Better Ceramics through Chemistry II, edited by C. J. Brinker, D. E. Clark, and D. R. Ulrich (Materials Research Society, Pittsburgh, PA, 1986), pp. 3–15.

    Google Scholar 

  6. R. A. Assink and B. D. Kay, in “1H NMR Studies of the Sol-Gel Transition,” in Better Ceramics through Chemistry, edited by C. J. Brinker, D. E. Clark, and D. R. Ulrich (Elsevier, New York, 1984), pp. 301–306.

    Google Scholar 

  7. L. W. Kelts, N. J. Effinger, and S. M. Melpolder, J. Non-Cryst. Solids 83, 353–374 (1986).

    Article  CAS  Google Scholar 

  8. The probe was designed and built by Bruker Instruments Inc.

  9. C. W. Turner and K. J. Franklin, J. Non-Cryst. Solids 91, 402–415 (1987).

    Article  CAS  Google Scholar 

  10. K. C. Chen, T. Tsuchiya, and J. D. Mackenzie, J. Non-Cryst. Solids 81, 227–237 (1986).

    Article  Google Scholar 

  11. H. Schmidt, H. Scholze, and A. Kaiser, J. Non-Cryst. Solids 63, 1–11 (1984).

    Article  CAS  Google Scholar 

  12. H. Schmidt and B. Seiferling, in “Chemistry and Applications of Inorganic-Organic Polymers (Organically Modified Silicates),” in Better Ceramics through Chemistry II, edited by C. J. Brinker, D. E. Clark, and D. R. Ulrich (Materials Research Society, Pittsburgh, PA, 1986), pp. 739–750.

    Google Scholar 

  13. W. G. Klemperer 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.

  14. R. K. Harris, J. Jones, and C. T. G. Knight, J. Mol. Spectrosc. 69, 95–103 (1980).

    CAS  Google Scholar 

  15. R. K. Harris and C. T. G. Knight, J. Mol. Spectrosc. 78, 273–278 (1982).

    CAS  Google Scholar 

  16. R. K. Harris and C. T. G. Knight, J. Chem. Soc. Faraday Trans. 79, 1525–1538 (1983).

    Article  CAS  Google Scholar 

  17. R. K. Harris and C. T. G. Knight, J. Chem. Soc. Faraday Trans. 79, 1539–1561 (1983).

    Article  CAS  Google Scholar 

  18. R. K. Harris, C. T. G. Knight, and W. E. Hull, J. Am. Chem. Soc. 103, 1577–1578 (1981).

    Article  CAS  Google Scholar 

  19. R. K. Iler, The Chemistry of Silica (John Wiley and Sons Inc., New York, 1979).

    Google Scholar 

  20. R. E. Russo and A. J. Hunt, J. Non-Cryst. Solids 86, 219–230 (1986).

    Article  CAS  Google Scholar 

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Kelts, L.W., Armstrong, N.J. A silicon-29 NMR study of the structural intermediates in low pH sol-gel reactions. Journal of Materials Research 4, 423–433 (1989). https://doi.org/10.1557/JMR.1989.0423

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  • DOI: https://doi.org/10.1557/JMR.1989.0423

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