Pure TiO2, single-doped and (Fe. Ni) co-doped TiO2 nanoparticles were successfully prepared by alcohol-thermal method with tetrabutyl titanate as the Ti source. The prepared samples were characterized by Xray powder diffraction (XRD), Brunauer-Emmett-Teller (BET) measurement, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM). UV-visible spectroscopy (UV-vis) and photoluminescence spectroscopy (PL). UV-vis absorption indicates that the co-doped TiO2 exhibits a good absorption of visible light, and the optimal molar ratio of Fe and Ni to Ti is 5.0% and 4.0%, respectively. The photoluminescence spectroscopy indicates that the separation efficiency of photo-induced electrons and holes is improved by the co-doping method. The nano TiO2 samples possess pure anatase phase and doping TiO2 with metal ions can suppress the crystal growth of the particles. The particle sizes of 5.0% Fe-4.0% Ni/TiO2 are about 14 nm. The specific surface area of 5.0% Fe-4.0% Ni co-doped TiO2 is 98.35 m(2)/g while that of the un-doped is 43.13 m(2)/g. The photocatalytic activities of the catalysts were estimated by detecting the H-2 evolution rate from water, and the average maximum H2 evolution rate was 361.64 mu mol.h(-1).g(cat)(-1) (with a measured time of 6 h) using 5.0% Fe-4.0% Ni/TiO2 catalyst. The H-2 evolution rate was detected in the mixture of ethanol and water under visible light irradiation (lambda >400 nm). Additionally, the mechanism of H2 evolution by water splitting is proposed. (C) 2012 Elsevier B.V. All rights reserved.