Hydrogen production by water splitting was examined over mesoporous niobium oxide photocatalysts, prepared by evaporation-induced self-assembly (EISA) method. A series of Pt, Au, Cu and NiO nanoparticles were loaded as cocatalyst to enhance the photocatalytic activity of mesoporous niobium oxide. The influences of the preparation parameters on the characteristics of the mesoporous niobium oxide photocatalysts and their photocatalytic activities were investigated in detail. The catalysts were characterized by powder X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), N-2 sorption and ultraviolet-visible spectroscopy (UV-vis) and nitrogen adsorption-desorption isotherm. The photocatalytic water splitting are preformed in an aqueous MeOH, used as sacrificial hole scavengers under UV light irradiation. The rate of H-2 evolution from an aqueous methanol solution under UV irradiation significantly changed with the variation of loading metal, and Pt loaded niobium oxide catalyst exhibited the highest photoactivity, with a rate of H-2 production of 4647 mu mol h(-1) g(-1) which was about 2.2, 2.9 and 6.5 times than Au, Cu and NiO photocatalysts, respectively. (C) 2011 Elsevier B.V. All rights reserved.