Structure and composition of the nanocrystalline phases in a MgO-TiO2 system prepared via sol-gel technique

Samples in the MgO-TiO2 system were prepared via the sol-gel technique with titanium and magnesium ethoxides as precursors and HNO3 as hydrolysis cata lyst. The analyzed magnesia to titania weight ratios were 0.1:0.9, 0.5:0,5, ana 0.9:0.1 (0.05, 0.5, and 4.0 MgO: TiO2 molar ratios). Samples were char acterized with X-ray powder diffraction, differential thermal analysis, and thermogravimetry. To quantify the concentration and the crystallography of the phases in the samples, their crystalline structures were refined by us ing the Rietveld method. In addition to periclase, anatase, and rutile, thr ee intermediate compounds were observed: karooite (MgTi2O5), geikielite (Mg TiO3), and qandilite (Mg2TiO4). The formation of the above crystalline phas es in the samples occurred after an exothermic reaction at 200 degrees C, a nd their dehydroxylation above 300 degrees C. Karooite was abundant only in titania-rich samples, while geikielite and qandilite concentrations were h igh in the samples with equal magnesia to titania weight percent. Phase con centrations depended on the annealing temperature of the sample and its MgO content. Magnesium was soluble in anatase, but not in rutile; the solubili ty, however, was low.