Five NiO/TiO(2)materials with a different mass ratio of NiO to TiO2(3.3, 6.7, 16.3, 23.7, and 36.8%) were synthesized by wet impregnation process and characterized by DR UV-vis, scanning electron microscope, transmission electron microscopy, X-ray diffraction method, N(2)physisorption, and temperature-programmed reduction.The characterization confirmed the existence of nano-sized cubic NiO on the commercial TiO2. The observed interaction between TiO(2)and NiO phases confirmed that the obtained material does not constitute a physical mixture of two species. The photocatalytic hydrogen generation efficiency [monitored by gas chromatography-thermal conductivity detector (GC-TCD)] of these materials from methanol-water mixtures under simulated solar radiation and artificial UV radiation was investigated. For some synthesized NiO/TiO(2)materials, higher photocatalytic efficiency was found compared with the commercial TiO(2)Degussa P25 catalyst. Also, the obtained results showed that 0.125 g L(-1)of 6.7%NiO/TiO(2)and 5% (v/v) of methanol were the optimal operating parameters. Furthermore, for the most efficient photocatalytic system under the influence of simulated solar radiation, a 1.8 times higher hydrogen production rate was achieved compared to that under the influence of artificial UV radiation.