Bismuth ions (Bi3+)-doped TiO2 nanocrystals have been synthesized by citric acid sol–gel combustion method using bismuth nitrate pentahydrate (Bi(NO3)3·5H2O) and titanium chloride (TiCl4) as raw materials. The obtained products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and UV–vis absorption spectra. The experiments demonstrated that Bi3+ doping in TiO2 enhances the photocatalytic degradation ratio of methyl orange in aqueous suspension and the optimal dopant of Bi3+ in TiO2 is about 3 % .