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Sol-gel synthesis of complex titanates in micro-emulsions
Journal article   Peer reviewed

Sol-gel synthesis of complex titanates in micro-emulsions

C J Barbé, R Graf, K S Finnie, M Blackford, R Trautman and John R Bartlett
Journal of Sol-Gel Science and Technology, Vol.26(1-3), pp.457-462
2003
url
https://doi.org/10.1023/A:1020706106450View
Published Version

Abstract

Materials Engineering reverse micelles microemulsions multicomponent titanates nanoparticles
Amorphous precursor nanopowders of zirconolite (CaZrTi2O7) were prepared using a water-in-oil micro-emulsion synthesis, with Ti(OiC3H7)4, Zr(OnC3H7)4 and either Ca(OC2H5)2 or an aqueous Ca(NO3)2 solution as precursors. The stoichiometry and structural evolution of the nanoparticles were investigated using a range of techniques, including ICP-MS, TEM, gas adsorption and vibrational spectroscopy. The use of Ca(OC2H5)2 led to slightly sub-stoichiometric nanopowders (CaxZrTi2O6+x, x = 0.8), following washing. Lower values of x were obtained in the washed nanopowders when using Ca(NO3)2, with x = 0.004, 0.022 or 0.52 at pH 2, 7 or 13, respectively. In the latter system, a comparison between the washed and unwashed nanopowders revealed that 25% of the calcium was lost during washing. The Ca(NO3)2 was found to form unstable tetraamine complexes within the reverse micelles at high pH, which transformed into Ca(OH)2 on ageing. The Ca(OH)2 can then interact with the hydrolysed titanium/zirconium alkoxides, and thus be integrated chemically into the final nanoparticle structure.

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