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Abstract

The small-angle x-ray scattering (SAXS) technique was used to investigate inhomogeneities on the scale of 10 to 600 Å in acid-catalyzed titania–silica and zirconia–silica xerogels. SAXS of (TiO2)x(SiO2)1−x and (ZrO2)x(SiO2)1−x xerogels with x < 0.1, in which there was no phase separation, showed the presence of two types of inhomogeneity. For Q < 0.05 Å−1 there was a clear departure from Porod scattering which showed that xerogel powder particle surfaces were rough. For 0.1 < Q < 0.4 Å−1 there was a plateau feature corresponding to micropores within the silica-based network, and this feature changes with heat treatment. SAXS of xerogels with x > 0.3 showed the presence of phase-separated regions of metal oxide, which were initially amorphous and crystallized at higher temperatures. A (TiO2)0.18(SiO2)0.82 xerogel that was not initially phase separated became phase separated after heat treatment at 750 °C due to reduced solubility of Ti in the silica network.

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References

  1. P.C. Shultz and H.T. Smyth, in Amorphous Materials, edited by E.W. Douglas and B. Ellis (Wiley, London, United Kingdom, 1972).

    Google Scholar 

  2. M. Itoh, H. Hattori, and K.J. Tanabe, J. Catal. 35, 225 (1974).

    Article  CAS  Google Scholar 

  3. M. Nogami, J. Non-Cryst. Solids 69, 415 (1985).

    Article  CAS  Google Scholar 

  4. J.B. Miller and E.I. Ko, J. Catal. 159, 58 (1996).

    Article  CAS  Google Scholar 

  5. C.J. Brinker and G.W. Scherer, Sol-Gel Science (Academic Press, San Diego, CA, 1990).

    Google Scholar 

  6. J.S. Rigden, R.J. Newport, M.E. Smith, P.J. Dirken, and G. Bushnell-Wye, J Mater. Chem. 6, 337 (1996).

    Article  CAS  Google Scholar 

  7. J.K. Walters, J.S. Rigden, P.J. Dirken, M.E. Smith, W.S. Howells, and R.J. Newport, Chem. Phys. Lett. 264, 539 (1997).

    Article  CAS  Google Scholar 

  8. M. Emili, L. Incoccia, S. Mobilio, G. Fagherazzi, and M. Guglielmi, J. Non-Cryst. Solids 74, 129 (1985).

    Article  CAS  Google Scholar 

  9. O. Stachs, T. Gerber, and V. Petkov, J. Mater. Sci. 32, 4209 (1997).

    Article  CAS  Google Scholar 

  10. Z. Liu and R.J. Davis, J. Phys. Chem. 98, 1253 (1994).

    Article  CAS  Google Scholar 

  11. D.M. Pickup, G. Mountjoy, G.W. Wallidge, R.J. Newport, and M.E. Smith, Phys. Chem. Chem. Phys. 1, 2527 (1999).

    Article  CAS  Google Scholar 

  12. K.L. Walther, A. Wokaun, B.E. Handy, and A. Baiker, J. Non-Cryst. Solids 134, 47 (1991).

    Article  CAS  Google Scholar 

  13. S.W. Lee and R.A. Condrate, J. Mater. Sci. 23, 2951 (1988).

    Article  CAS  Google Scholar 

  14. P.J. Dirken, M.E. Smith, and H.J. Whitfield, J. Phys. Chem. 99, 395 (1995).

    Article  CAS  Google Scholar 

  15. R. Anderson, G. Mountjoy, R.J. Newport, and M.E. Smith, J. Non-Cryst. Solids 232–234, 72 (1998).

    Article  Google Scholar 

  16. G. Mountjoy, D.M. Pickup, G.W. Wallidge, R. Anderson, J.M. Cole, R.J. Newport, and M.E. Smith, Chem. Mater. 11, 1253 (1999).

    Article  CAS  Google Scholar 

  17. K. Okasaka, H. Nasu, and K. Kamiya, J. Non-Cryst. Solids 136, 103 (1991).

    Article  CAS  Google Scholar 

  18. L.A. Feigin and D.I. Svergun, Structure Analysis by Small-Angle X-ray and Neutron Scattering (Plenum Press, New York, 1987).

    Book  Google Scholar 

  19. I.M. Miranda Salvado, F.M.A. Margaca, and J. Teixeira, J. Non-Cryst. Solids 163, 115 (1993).

    Article  CAS  Google Scholar 

  20. F.M.A. Margaca, I.M. Miranda Salvado, and J. Teixeira, J. Non-Cryst. Solids 209, 143 (1997).

    Article  CAS  Google Scholar 

  21. T. Kamiya, M. Mikami, and K. Suzuki, J. Non-Cryst. Solids 150, 157 (1992).

    Article  Google Scholar 

  22. M. Ramirez-del-Solar, L. Esquivias, A.F. Craievich, and J. Zarzycki, J. Non-Cryst. Solids 147–148, 206 (1992).

    Article  Google Scholar 

  23. M. Nogami and K. Nagasaka, J. Non-Cryst. Solids 109, 79 (1989).

    Article  CAS  Google Scholar 

  24. B.E. Yoldas, J. Non-Cryst. Solids 38–39, 81 (1980).

    Article  Google Scholar 

  25. P.W. Schmidt, J. Appl. Crystallogr. 24, 414 (1991).

    Article  CAS  Google Scholar 

  26. S.K. Sinha, E.B. Sirota, and S. Garoff, Phys. Rev. B 38, 2297 (1988).

    Article  CAS  Google Scholar 

  27. O. Glatter and O. Kratky, Small Angle X-ray Scattering (Academic Press, London, United Kingdom, 1982), p. 121.

    Google Scholar 

  28. O. Stachs, T. Gerber, Y. Beyer, and H. Burger, J. Non-Cryst. Solids 180, 197 (1995).

    Article  CAS  Google Scholar 

  29. B. Himmel, T. Gerber, and H. Burger, J. Non-Cryst. Solids 119, 1 (1990).

    Article  CAS  Google Scholar 

  30. O. Stachs, V. Petkov, and T. Gerber, J. Appl. Crystallogr. 30, 670 (1997).

    Article  CAS  Google Scholar 

  31. B.E. Warren, X-ray Diffraction (Addison-Wesley, Reading, United Kingdom, 1969), p. 253.

    Google Scholar 

  32. B.N. Nair, W.J. Elferink, K. Keizer, and H. Verweij, J. Colloid Interface Sci. 178, 565 (1996).

    Article  CAS  Google Scholar 

  33. D.W. Schaefer and K.D. Keefer, Phys. Rev. Lett. 53, 1383 (1984).

    Article  CAS  Google Scholar 

  34. A. Nakano, R.K. Kalia, and P. Vashishta, Phys. Rev. Lett. 73, 2336 (1994).

    Article  CAS  Google Scholar 

  35. M. Teubner and R. Strey, J. Chem. Phys. 87, 3195 (1987).

    Article  CAS  Google Scholar 

  36. J.-C. Li and D.K. Ross, J. Phys.: Condens. Matter 6, 351 (1994).

    CAS  Google Scholar 

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Mountjoy, G., Rigden, J.S., Anderson, R. et al. Articles. Journal of Materials Research 15, 1998–2005 (2000). https://doi.org/10.1557/JMR.2000.0287

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  • DOI: https://doi.org/10.1557/JMR.2000.0287

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