Photocatalytic activity of mesoporous titania supported nickel oxide photocatalyst synthesized by single-step sol-gel (SSSG) process combined with surfactant-assisted template method was investigated for hydrogen evolution from an aqueous methanol solution, in comparison with one prepared by conventional incipient wetness impregnation (IWI) method. In single-step sol-gel process, nickel precursor was introduced into the titania sol prepared with the aid of a surfactant template behaving as pore-controlling agent to attain meso-scaled pore. The single-step sol-gel photocatalyst was experimentally found to enhance the photocatalytic evolution of hydrogen rather than the impregnated one. The optimum level of nickel loading in photocatalytic activity test for single-step sol-gel method was slightly higher than that for incipient wetness impregnation method. Characterization results demonstrated the significant modification of physical characteristics of the single-step sol-gel photocatalyst, anticipated to relating to the observation of higher photocatalytic hydrogen evolution activity. (c) 2004 International Association for Hydrogen Energy. Published by Elsevier Ltd. All rights reserved.