Abstract: A visible-light responsible non-metal C-N-S-tertiary doped TiO₂ was synthesized by a sol-gel process using Ti(OC₄H₉)₄ and functional biology organic cystine as raw materials.The obtained photocatalysts were characterized by the means of X-ray powder diffraction(XRD),X-ray photoelectron spectroscopy(XPS),fourier transition infrared spectra(FT-IR),ultraviolet-visible diffuse reflectance spectroscopy(UV-Vis DRS).XRD showed that,by C,N and S tertiary-doping,the growth of TiO₂ crystallite was restrained and the temperature of phase transformation from anatase to rutile of TiO₂ was enhanced effectively.DRS showed the extension of light absorption edge in the range of visible-light was up to 800 nm.XPS analysis revealed that C and S existing on the surface of TiO₂ photocatalyst was the state of CO₃^2- and S⁶⁺,respectively.Nitrogen species could be ascribed to the form of N-Ti-O and Ti-O-N.And more hydroxyl groups were found on the C-N-S tertiary doped catalyst.The photocatalytic activities of the as-prepared photocatalysts were evaluated by degradation of Rhodamine B(RhB) in an aqueous suspension under visible light.It was found that C-N-S- tertiary doped TiO₂ exhibited improved photocatalytic activity compared with that of P25 TiO₂.Under the visible-light irradiation ranging from 470 to 800 nm for 2 h,an 83% removal rate of RhB could be achieved.