Titanium dioxide (TiO2) photocatalysts co-doped with iron (Fe) and niobium (Nb) were synthesized using a temperature-controlled sol-gel method. The photocatalysis products were characterized and the photocatalytic activities were evaluated by the degradation of aqueous methyl orange solution. Enhanced photocatalytic activity compared to undoped TiO2 was attributed to the cooperative effects of metal dopants, Fe and Nb.