In this paper, Fe/C codoped TiO2 powders are successfully synthesized by the sol‐gel method. The crystalline size and interplanar spacing of doped TiO2 were smaller than undoped TiO2 powders. The narrow bandgap of TiO2 powders were observed by doping and the light absorption edge shift to longer wavelength, especially for Fe/C codoped TiO2 powders, and extended to 460 nm. Photoluminescence spectra showed similar luminescence band shape except for relative intensity under the excited source of 320 nm and Fe/C codoped TiO2 powders exhibited the weakest luminous intensity. Compared with undoped powders, doped TiO2 could significantly improve the photocatalytic degradation in methyl orange aqueous solution, and Fe/C codoped TiO2 powders exhibited optimal performance among other photocatalyst under ultraviolet light irradiation and also showed better stability in the air environment.