In this paper, Fe-TiO2 and Fe-fullerene/TiO2 composite photocatalysts were prepared with titanium (IV) n-butoxide (TNB) by a sol-gel method. TiO2, Fe-TiO2 and Fe-fullerene/TiO2 were characterized by scanning electron microscopy (SEM), Transmission electron microscope (TEM), specific surface area (BET), X-ray diffraction analysis (XRD) and energy dispersive X-ray spectroscopy (EDX). The photocatalytic activities were evaluated by the photocatalytic oxidation of methylene blue (MB) solution. XRD patterns of the composites showed that the photocatalyst composite contained a typical single and clear anatase phase. The surface properties shown by SEM presented a characterization of the texture on Fe-fullerene/TiO2 composites and showed a homogenous composition in the particles for the titanium sources used. The EDX spectra for the elemental identification showed the presence of O, C and Ti elements. Moreover, peaks of the Fe element were observed in the Fe-TiO2 and Fe-fullerene/TiO2 composites. The degradation of MB solution by UV-light irradiation in the presence of photocatalyst compounds was investigated in complete darkness. The degradation of MB concentration in aqueous solution occurred via three kinds of physical phenomena: quantum efficiency of the fullerene; organo-metallic reaction of the Fe compound; and decomposition of TiO2. The degradation rate of the methylene blue solution increased when using Fe-fullerene/TiO2 compounds.