TiO2 nanocrystals were prepared by solvothermal treatment in oleic acid at 250 °C of amorphous TiO2 nanoparticles. The latter were prepared by sol–gel processing in dodecylamine at 100 °C of starting solutions synthesized from TiCl4. For preparing Pt/TiO2 nanocomposites, with Pt/Ti nominal atomic ratio of 0.05, the required amount of Pt precursor was added to the amorphous TiO2 nanoparticles before heating at 250 °C. Control synthesis experiments, evaluated by X-ray diffraction and X-ray photoelectron spectroscopy showed Pt(acac)2 as the best Pt precursor, and 250 °C as the optimum temperature for simultaneous TiO2 crystallization and efficient Pt nucleation. Transmission electron microscopy observations evidenced Pt nanocrystals dispersed in the surrounding TiO2 host, with a mean size of 4 nm. The TiO2 host was constituted of rod-shaped anatase nanocrystals. Comparison with pure TiO2 showed …