Multi-walled carbon nanotube, TiO2 and Ni composite catalysts (MWNT-TiO2:Ni) were prepared by a modified chemical vapor deposition. The nanoscaled composite materials were extensively characterized by TG, SEM, Raman and UV-vis spectra. The photoactivity of the catalyst for H-2 evolution was investigated in the presence of methanol sacrificial reagent under visible light illumination. The rate of H-2 evolution was 38.1 mu mol/h at a weight ratio of MWNT/TiO2 equal to 4.4%. The experimental results were rationalized by assuming that MWNTs serve as photo sensitizer, synergetic with metallic Ni, greatly enhancing the activity of visible light-responsive photocatalyst. (c) 2006 Elsevier B.V. All rights reserved.