ArtículoAbstract: Ti–Fe mixed oxides were prepared by sol-gel and used as photocatalysts for the generation H2 from water. The solids were characterized by SEM-EDS, N2 physisorption, XRD, UV–Vis and XPS spectroscopy. The mixed oxides present larger specific surface areas (83–205 m2/g) than that of pure TiO2 (64 m2/g). The XRD patterns of the Ti–Fe solids resemble that of anatase titania. The band gap energies of the solids vary from 3.0 to 2.5 eV and are smaller than that of TiO2 (3.2 eV). The mixed oxides were tested as photocatalysts in the production of hydrogen from water using methanol as a sacrificial agent. In all cases, their catalytic activities were higher than that exhibited by TiO2 after 10 h of reaction.