Abstract: The sulfur-doped titanate and sodium titanate nanotubes(STNTs) were prepared by hydrothermal reaction of sodium hydroxide(NaOH) with titanium disulphide(TiS2),which was used as sulfur source and titanium source for the first time.The structure,morphology,sulfur-doped valence state and doped amount of the as-obtained STNTs were characterized by X-ray diffraction(XRD),high resolution transmission electron microscopy(HRTEM),scanning electron microscope(SEM),extended X-ray absorption fine structure(EXAFS),and energy dispersive X-ray(EDS).The photo-oxidation reaction of ethanol under visible light was used to probe the reaction,and the visible light-responsive photocatalytic activity of sulfur-doped titanate nanotube was investigated by means of in-situ gas chromatography(GC).The results indicated that S atoms were introduced into the lattice of titanate nanotubes as S^2-anions.The average size of wall thickness and diameter of STNTs were 2.9 nm and 9.7 nm,respectively.The visible light-responsive photocatalytic oxidation results indicated that the SNTTs with very low amount of doped sulfur showed higher photocatalytic activity than undoped TiO₂ nanotubes.