This study aimed to develop an effective, environmentally benign composite catalyst composed of carbon materials and titanium dioxide ( TiO 2). Carbon-doped titanium dioxide ( C – TiO 2) was prepared by coating TiO 2 onto macro-mesoporous carbon (MMC). The structure, morphology and surface chemistry states of the C – TiO 2 were characterized by XRD, TEM, XPS, UV-vis and FTIR. The photocatalytic activity of C – TiO 2 was evaluated based on the decomposition of an aqueous methyl orange solution in visible light. C – TiO 2 significantly improved photocatalytic activity. A possible mechanism for the improvement of the photocatalytic activity of C – TiO 2 in visible light was proposed. The results of the analysis suggested that MMC played key roles as the support, absorbent, location of photo-generated electron transfer, and carbon-doping source during methyl orange photodegradation.