Oxides precursors ZrxTi12xO2 (x50.22, 0.39, and 0.60) were
prepared by a hydrolytic sol–gel process. The amorphous mixed
oxides are homogeneous as deduced from electron microscopy
and XPS studies. The crystallization of these amorphous oxides
was studied by TGA–DTA and thermodi¤ractometry. Quantitative
analysis of the crystalline phases, obtained at 1000¡C, was
carried out by the Rietveld method. The samples are mixtures of
TiO2, Zr5Ti7O24, and ZrO2 oxides, and the stoichiometry of the
stable zirconium titanate phase was found to be Zr5Ti7O24 and
not ZrTiO4 (5Zr6Ti6O24). In this work, the power of Rietveld
reÞnements to determine phase ratios of very related (and thus
very overlapped) phases is shown.