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The role of transesterification in the multistep “prehydrolysis” sol/gel synthesis of aluminum-rich aluminosilicate gels

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Abstract

Using a prehydrolysis technique, transparent gels with very high aluminum content can be achieved with the use of isopropanol. Here 13C, 27Al, 29Si and 17O NMR at various stages of preparation show that when the aluminum added exceeds the number that silanols can fully protect, the excess aluminum alkoxide groups readily undergo transesterification with isopropanol. The aluminum isopropoxide (Al–OPri) groups thus formed are shown to be sufficiently stable that attack by water is impeded, thus allowing the remaining silicon alkoxide groups to hydrolyze and condense to form a homogeneous gel.

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References

  1. M. Reese, J. Sanchez, and A. V. McCormick, in Synthesis and Processing of Ceramics: Scientific Issues, edited by W. E. Rhine, T. M. Shaw, R. J. Gottschall, and Y. Chen (Mater. Res. Soc. Symp. Proc. 249, Pittsburgh, PA, 1992), p. 69.

    Google Scholar 

  2. G. A. Pozarnsky and A. V. McCormick, J. Non-Cryst. Solids 190 (3), 212 (1995).

    Article  CAS  Google Scholar 

  3. G. A. Pozarnsky, E. Westenberg, and A. V. McCormick, J. Sol-Gel Science and Technology 3, 57 (1994).

    Article  CAS  Google Scholar 

  4. R. K. Iler, The Chemistry of Silica (New York, 1979).

  5. C. L. Thomas, Ind. Eng. Chem. 4 (1), 2564 (1949).

    Article  Google Scholar 

  6. G. Carturan, J. Non-Cryst. Solids 29 (41), 954 (1978).

    Google Scholar 

  7. C. J. Brinker and G. W. Scherer, Sol-Gel Science (Academic Press, New York, 1990).

    Google Scholar 

  8. J. C. Pouxviel and J. P. Boilot, Ultrastructure Processing of Advanced Ceramics, edited by J. D. MacKenzie and D. R. Ulrich (Wiley, New York, 1987), p. 197.

  9. B. Yoldas, J. Mater. Sci. 11 (4), 1822 (1979).

    Google Scholar 

  10. B. Yoldas, J. Non-Cryst. Solids 63, 150 (1984).

    Article  Google Scholar 

  11. J. Jonas, A. D. Irwin, and J. S. Holmgren, Ultrastructure Processing of Advanced Ceramics, edited by J. D. MacKenzie and D. R. Ulrich (Wiley, New York, 1987), p. 303.

  12. J. Jonas, A. D. Irwin, and J. S. Holmgren, J. Mater. Sci. 23, 2908 (1988).

    Article  Google Scholar 

  13. W. G. Fahrenholtz, S. L. Hetala, D. M. Smith, A. J. Hurd, C. J. Brinker, and W. L. Earl 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. Symp. Proc. 180, Pittsburgh, PA, 1990), p. 229.

  14. B. Yoldas, J. Mater. Sci. 8 (3), 489 (1978).

    Google Scholar 

  15. D. M. Krol and J. G. van Lierop, J. Non-Cryst. Solids 63 131 (1984).

  16. S. Dire and F. Babonneau, J. Non-Cryst. Solids 167, 29 (1994).

    Article  CAS  Google Scholar 

  17. J. C. Pouxviel, J. P. Boilot, J. C. Beloeil, and J. Y. Lallemand, J. Non-Cryst. Solids 89, 345 (1987).

    Article  CAS  Google Scholar 

  18. J. W. Akitt, Prog. NMR Spec. 21, 1 (1989).

    Article  Google Scholar 

  19. E. Lippmaa, A. Samoson, and M. Magi, J. Am. Chem. Soc. 108, 1730 (1989).

    Article  Google Scholar 

  20. D. Mueller, D. Hoebbel, and W. Gessner, Chem. Phys. Lett. 84 (1), 25 (1981).

    Article  CAS  Google Scholar 

  21. G. Harvey and L. S. D. Glasser, Zeolite Synthesis, ACS, Symposium Series, edited by M. L. Occelli and H. E. Robson (1988), Vol. 398, p. 49.

  22. T. H. Walter, G. L. Turner, and E. Oldfield, J. Magn. Res. 76, 106 (1988).

    CAS  Google Scholar 

  23. T. H. Walter and E. Oldfield, J. Phys. Chem. 93, 6744 (1989).

    Article  CAS  Google Scholar 

  24. H. Y.C. Timken, S. E. Schramm, R. J. Kirkpatrick, and E. Oldfield, J. Phys. Chem. 91, 1054 (1987).

    Article  CAS  Google Scholar 

  25. S. Schramm and E. Oldfield, J. Am. Chem. Soc. 106, 2502 (1984).

    Article  CAS  Google Scholar 

  26. H. Y. C. Timken, G. L. Turner, J. P. Gilson, L. B. Welsh, and E. Oldfield, J. Am. Chem. Soc. 108, 7231 (1986).

    Article  CAS  Google Scholar 

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

    Article  CAS  Google Scholar 

  28. P. J. Dirken, M. E. Smith, and H. J. Whitfield, J. Phys. Chem. 99, 345 (1995).

    Article  Google Scholar 

  29. D. Bradley, Metal Alkoxides (Wiley, New York, 1978).

    Google Scholar 

  30. J. Livage, M. Henry, and C. Sanchez, Prog. Solid State Chem. 18 (4), 259 (1988).

    Article  CAS  Google Scholar 

  31. M. Henry, J. P. Jolivet, and J. Livage, Structure and Bonding 77, 154 (1991).

    Google Scholar 

  32. K. Jones, T. J. Davies, H. G. Emblem, and P. Parkes in Better Ceramics Through Chemistry II, edited by C. J. Brinker, D. E. Clark, and D. R. Ulrich (Mater. Res. Soc. Symp. Proc. 73, Pittsburgh, PA, 1986), p. 111.

  33. R. C. Mehrotra in Better Ceramics Through Chemistry III, edited by C. J. Brinker, D. E. Clark, and D. R. Ulrich (Mater. Res. Soc. Symp. Proc. 121, Pittsburgh, PA, 1988), p. 81.

  34. P. Li, B. A. Ferfuson, and L. F. Francis, J. Mater. Sci. 30, 4076 (1995).

    Article  CAS  Google Scholar 

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Author notes

  1. G. A. Pozarnsky

    Present address: Center for Advanced Materials Processing (CAMP), Clarkson University, Potsdam, New York, 13699, USA

Authors and Affiliations

  1. Department of Chemical Engineering and Materials Science, University of Minnesota, Minneapolis, Minnesota, 55455-0132, USA

    G. A. Pozarnsky & A. V. McCormick

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  1. G. A. Pozarnsky
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  2. A. V. McCormick
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Pozarnsky, G.A., McCormick, A.V. The role of transesterification in the multistep “prehydrolysis” sol/gel synthesis of aluminum-rich aluminosilicate gels. Journal of Materials Research 11, 922–927 (1996). https://doi.org/10.1557/JMR.1996.0115

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  • DOI: https://doi.org/10.1557/JMR.1996.0115

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