X-ray diffraction, and Raman scattering study of nanostructured ZrO2-TiO2 oxides prepared by sol-gel

In the present work, we study the phase composition of ZrO2-TiO2 system by means of XRD and Raman spectroscopy, using also TG-ATD, and N2 adsorption isotherms as complementary characterization techniques. TiO2-ZrO2 samples of selected compositions (0, 10, 90, 50 and 100% in weight of TiO2) were prepared by sol-gel method and annealed at three different temperatures (400, 600 and 800 degrees C). Structural characterization reveals that only the pure oxides are crystalline at 400 degrees C: TiO2 as anatasa with a minor brookite component, and ZrO2 as a mixture of tetragonal (majority) and monoclinic phases. Following the 600 degrees C calcination, the TiO2-ZrO2 50-50% sample forms the ZrTiO4 mixed oxide, although this materials remains partly amorphous. In contrast, samples with higher and lower TiO2 content form solid solutions with, respectively, anatasa and tetragonal ZrO2 structures. Zirconium incorporation into the TiO2 lattice leads to the expansion of the unit cell parameters, and it stabilizes the anatase phase, hindering its transformation into rutile. Similarly, dissolving titanium atoms into the ZrO2 structure delays the transformation from the tetragonal to the monoclinic polymorph.