Bismuth-doped TiO2 submicrospheres were synthesized by ultrasonic spray pyrolysis. The prepared bismuth-doped titania was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UVvisible diffuse reflectance spectroscopy (UV-vis DRS), and X-ray photoelectron spectroscopy (XPS). Aqueous photocatalytic activity was evaluated by the decomposition of methyl orange under visible-light irradiation. The results indicate that doping of bismuth remarkably affects the phase composition, crystal structure, and the photocatalytic activity. The sample with 2% Bi exhibits the optimum photocatalytic activity. Copyright © 2012 Jianhui Huang et al.