Thermal study of the anatase–rutile structural transitions in sol-gel synthesized titanium dioxide powders

Abstract

Titanium dioxide powders were synthesized by the sol?gel process using titanium tetrabutoxide as the precursor. The syntheses were performed in saturated aqueous solutions of KCl, CaCl2, NiCl2, CoCl2 and MnCl2, and in dimethylformamaide (DMF) and dimethylsulfoxide (DMSO) solutions. The obtained X-ray diffraction patterns show that all samples were crystalline (anatase phase) with some minor amounts of a brookite phase. It is worth noting that the anatase phase was obtained independent of any previous or further treatment of the synthesized powder, such as hydrothermal or heat treatment. For the titanium dioxide powders synthesized in saturated aqueous solution of metal chlorides (mean crystallite size = 11 nm), the anatase?rutile transition occurred in the range 455?570 ?C, depending on the considered sample, as verified by DTA analysis. In the powders synthesized in DMF or DMSO solutions (means crystallite size = 6 nm), the same structural transition occurred at 485 ?C.