The rates of photocatalytic production of H 2 by Pt/N-doped TiO 2 are significantly affected by the hydrolysis temperature applied during the sol-gel process. Production rates increase as the hydrolysis temperature decreases from 40 to 20°C. The effects of the hydrolysis temperature on the properties and water-splitting behavior of photocatalysts were investigated. Characterization results showed that hydrolysis temperatures higher than 40°C induce the formation of the rutile phase and particle agglomeration, reduce the N-dopant content, and decrease the range of visible-light absorption. In this study, a low hydrolysis temperature of about 20°C is optimal for the sol-gel preparation of N-doped TiO 2 ; this temperature favors the formation of high-purity anatase, small particle size, extensive visible-light absorption, and excellent rates of photocatalytic production of H 2 (about 2100 lmol h -1 g -1 ).