Here, hierarchically meso/nanoporous TiO2 was successfully fabricated by a facile and efficient hydrolysis and calcination method using Ti(OC4H8)(4) and K2S2O8 as precursors. The hydrosol was firstly prepared by drop-wise adding ethanol dissolved Ti(OC4H8)(4) solution into acetone dissolved K2S2O8 solution under a vigorous stirring and heating condition. After being sufficiently hydrolyzed, the hydrosol was calcined to promote the crystallization of TiO2 and successfully dope S and C on TiO2. The calcination temperature significantly affects the doping of S and C on TiO2, crystallization of TiO2, formation of hierarchically meso/nanoporous structure of TiO2 and its light absorption capability. The S- and C-codoped TiO2 exhibits high photocatalytic H-2 generation efficiency in a water/methanol sacrificial reagent system under the irradiation of UV light. The high photocatalytic efficiency is dependent on the comprehensively competing effects of the codoping of S and C, crystallization, specific surface area and light absorption capability. The S- and C-codoped TiO2 calcined at 600 degrees C demonstrates the highest photocatalytic H-2 generation efficiency, which is ascribed to the balanced synergy of the abovementioned factors. (C) 2012 Elsevier B.V. All rights reserved.