Nanoscale composite materials containing multi-walled carbon nanotubes (MWCNT) and titania were prepared by using a modified sol-gel method. The composites were comprehensively characterized by thermogravimetric analysis, nitrogen adsorption-desorption isotherm, powder X-ray diffraction, scanning electron microscopy with energy dispersive X-ray analysis, transmission electron microscopy, X-ray photoelectron spectroscopy and UV-vis absorption spectroscopy. The analysis revealed the presence of titania crystallites of about 7.5 nm aggregated together with MWCNT in particles of 15-20 nm of diameter. The photoactivity of the prepared materials, under UV or visible irradiation, was tested using the conversion of phenol from model aqueous solutions as probe reaction. A synergy effect on the photocatalytic activities observed for the composite catalysts was discussed in terms of a strong interphase interaction between carbon and TiO2 phases by comparing the different roles of MWCNT in the composite materials. (C) 2007 Elsevier Ltd. All rights reserved.