In this work, a low-temperature solvothermal method has been developed to synthesize visible-light-responsive S-doped TiO2 nanocrystal photocatalyst, using thiourea as the sulfur source to enhance sulfur incorporation into TiO2 lattice. The effects of different S:Ti molar ratio on the crystal structure, chemical composition, surface property and catalytic performance have been studied. X-ray photoelectron spectroscopy (XPS) analysis and Fourier transform infrared (FT-IR) spectra displayed that the TiO2 was modified by the S element incorporated into the TiO2 network to form Ti-O-S bond, which therefore led to the formation of intermediate energy level just above the O 2p valance band, and caused the absorption edge of TiO2 to shift into the visible light region up to 500 nm. Characterization results show that the pure nanocrystal anatase structure, with both the degree of S doping and oxygen vacancies makes contribution to the exceptional photocatalytic activity of TONS in visible-light degradation of Methylene Blue (MB) and phenol molecules. (C) 2011 Elsevier B.V. All rights reserved.