Nanocrystalline mesoporous Ta2O5 photocatalyst was synthesized through a combined sol-gel process with surfactant-assisted templating mechanism under mild conditions. Controlled hydrolysis and condensation of tantalum pentaethoxide modified with acetylacetone in the presence of laurylamine hydrochloride surfactant aqueous solution ultimately yielded nanocrystalline Ta2O5 with mesoporous characteristic. The NiO cocatalyst loading at various contents was also performed by single-step sol-gel method, in which nickel precursor was incorporated into the completely hydrolyzed tantalum sol prior to the gelation step. The synthesized photocatalysts were methodically characterized by TG-DTA, XRD, N-2 adsorption-desorption, diffuse reflectance UV-vis spectra, SEM, and TEM analyses. The XRD patterns indicated that the cocatalyst was in a very high dispersion degree on mesoporous Ta2O5. N-2 adsorption-desorption isotherms and SEM observation verified that the photocatalysts possessed mesoporous structure. The surface area of the samples from BET method was quite high with very narrow monomodal pore size distribution estimated from BJH method. The photocatalytic performance of the materials was assessed via H, evolution from water using methanol as a hole scavenger under UV light irradiation. For unloaded Ta2O5 photocatalysts, the sample calcined at 700 degrees C showed the highest photocatalytic H, evolution activity. Moreover, the photocatalytic activity of such the sample was dramatically increased with the cocatalyst loading, exhibiting the optimum loading content at 5 wt.%. (c) 2005 Elsevier B.V. All rights reserved.