An iodine and boron co-doped TiO2 photocatalyst was prepared by the hydrolyzation-precipitation method. X-ray diffraction (XRD), ultraviolet-visible diffuse reflectance spectroscopy (UV-Vis DRS), and X-ray photoelectron spectroscopy (XPS) were applied to characterize the crystalline structure, light absorbing ability, and the chemical state of iodine and boron in the photocatalysts. The results of photocatalytic degradation of methyl orange demonstrated that the I-B-TiO2 catalyst prepared at 400 °C for 3 h exhibited the highest photocatalytic activity with a methyl orange degradation ratio...