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In Situ Studies of the Processing of Sol-Gel Produced Amorphous Materials Using Xanes, Saxs and Curved Image Plate XRD

Published online by Cambridge University Press:  10 February 2011

DM Pickup ,
G Mountjoy ,
RJ Newport ,
ME Smith ,
GW Wallidge  and
MA Roberts
DM Pickup
Affiliation:
contact author: d.m.pickup@ukc.ac.uk
G Mountjoy
Affiliation:
School of Physical Sciences, University of Kent at Canterbury, CT2 7NR, UK.
RJ Newport
Affiliation:
School of Physical Sciences, University of Kent at Canterbury, CT2 7NR, UK.
ME Smith
Affiliation:
Department of Physics, University of Warwick, Coventry, CV4 7AL, UK.
GW Wallidge
Affiliation:
Department of Physics, University of Warwick, Coventry, CV4 7AL, UK.
MA Roberts
Affiliation:
Daresbury Laboratory, Warrington, WA4 4AD, UK.
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Abstract

Sol-gel produced mixed oxide materials have been extensively studied using conventional, ex situ structural techniques. Because the structure of these materials is complex and dependent on preparation conditions, there is much to be gained from in situ techniques: the high brightness of synchrotron x-ray sources makes it possible to probe atomic structure on a short timescale, and hence in situ. Here we report recent results for mixed titania- (and some zirconia-) silica gels and xerogels. Titania contents were in the range 8–18 mol%, and heat treatments up to 500°C were applied. The results have been obtained from intrinsically rapid synchrotron x-ray experiments: i) time-resolved small angle scattering, using a quadrant detector, to follow the initial stages of aggregation between the sol and the gel; ii) the use of a curved image plate detector in diffraction, which allowed the simultaneous collection of data across a wide range of scattering at high count rate, to study heat treatments; and iii) x-ray absorption spectroscopy to explore the effects of ambient moisture on transition metal sites.

Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 590: Symposium R – Applications of Synchrotron Radiation Techniques…V , 1999 , 119
Copyright
Copyright © Materials Research Society 2000

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References

REFERENCES

[1] Shultz, PC and Smyth, HT Amorphous materials, ed Douglas, EW and Ellis, B (London: Wiley) 1972. M Itoh, H Hattori, and KJ Tanabe J. Catalysis 35, 225, 1974. M Nogami J. Non-Cryst. Solids 69, 415, 1985. JB Miller and EI Ko, J. Catalysis 159, 58, 1996.Google Scholar
[2] Holland, MA, Pickup, DM, Newport, RJ, Mountjoy, G and Smith, ME, these proceedings.Google Scholar
[3] Brinker, CJ and Scherer, GW, Sol-gel science: the physics and chemistry of sol-gel processing (San Diego: Academic Press) 1990.Google Scholar
[4] Rigden, JS, Walters, JK, Dirken, PJ, Smith, ME, Bushnell-Wye, G, Howells, WS and Newport, RJ, J. Phys.: Condens. Matter 9, 4001, 1997.Google Scholar
[5] Pickup, DM, Mountjoy, G, Wallidge, GW, Anderson, R, Cole, JM, Newport, RJ and Smith, ME, J. Mater. Chem. 9, 1299, 1999.10.1039/a809810gGoogle Scholar
[6] Pickup, DM, Mountjoy, G, Wallidge, GW, Newport, RJ and Smith, ME Phys. Chem. Chem. Phys. 1, 2527, 1999.10.1039/a901401bGoogle Scholar
[7] Mountjoy, G., Pickup, D.M., Wallidge, G.W., Anderson, R., Cole, J.M., Newport, R.J. and Smith, M.E., Chem. Mater. 11, 1253, 1999. See also G Mountjoy, DM Pickup, MA Holland, RJ Newport, GW Wallidge, ME Smith, these proceedings.10.1021/cm980644uGoogle Scholar
[8] Kamiya, T, Mikami, M and Suzuki, K J. Non-Cryst. Solids 150, 157, 1992.10.1016/0022-3093(92)90115-ZGoogle Scholar
[9] Ramirez-del-Solar, M, Esquivias, L, Craievich, AF and Zarzycki, J, J. Non-Cryst. Solids 147–148, 206, 1992.10.1016/S0022-3093(05)80619-2Google Scholar
[10] Nogami, M and Nagasaka, K, J. Non-Cryst. Solids 109, 79, 1989.10.1016/0022-3093(89)90445-6Google Scholar
[11] Yoldas, BE, J Non-Cryst. Solids 38–39, 81, 1980.10.1016/0022-3093(80)90398-1Google Scholar
[12] Feigin, LA and Svergun, DI, Structure analysis by small-angle x-ray and neutron scattering (New York: Plenum Press) 1987.10.1007/978-1-4757-6624-0Google Scholar
[13] Himmel, B, Gerber, T and Burger, H J. Non-Cryst. Solids 119, 1, 1990.10.1016/0022-3093(90)90234-DGoogle Scholar
[14] Roberts, MA, Finney, JL and Bushnell-Wye, G, Mater. Sci. Forum 278–281, 318, 1998.10.4028/www.scientific.net/MSF.278-281.318Google Scholar
[15] International Tables for x-ray Crystallography, Vol. IV (Kynoch, Birmingham), p71, 1974. F Hajdu, Acta. Cryst. A28, 250, 1972.Google Scholar
[16] Gaskell, PH, in Material Science and Technology Volume 9: Glasses and Amorphous Materials, edited by Zarzycky, J (VCH, Weinhaim) p175, 1991.Google Scholar
[17] Bianconi, A, x-ray absorption: principles, applications, techniques of EXAFS, SEXAFS and XANES ed. Koninbsberger, D.C. and Prins, R., Chapter 11 (Wiley, New York, 1987).Google Scholar
[18] Farges, F, Brown, GE, Navrotsky, A, Gan, H and Rehr, JJ Geochimica et Cosmochimica acta 60, 3023, 1996.10.1016/0016-7037(96)00144-5Google Scholar