A new photocatalytic system using anatase TiO2 loaded onto pyrite FeS2 (FeS2/TiO2) was developed to enhance the production of hydrogen. The FeS2 (3.0, 5.0, 10.0, and 15.0 wt-%)/TiO2 particles in SEM photos showed a core/shell structure composed of pyrite FeS2 with a grape-like morphology of length of similar to 1.0 mu m and anatase TiO2 of diameter <50 nm. The evolution of H-2 by methanol/water (1: 1) photo splitting over FeS2/TiO2 in a liquid system was enhanced as compared with that obtained using pure TiO2 and FeS2. In particular, 9.8 mmol of H-2 gas was produced in 10 h when 0.5 g of a 10.0 wt-% FeS2/TiO2 core/shell composite was used. Hydrogen production was increased by adding KOH electrolyte to 11.2 mmol. On the basis of cyclic voltammetry (CV) and UV-visible spectra results, this photoactivity of the FeS2/TiO2 composite was attributed to a shorter band gap than those of pure TiO2 and FeS2. (C) 2013 Elsevier B.V. All rights reserved.