Abstract: Micro/nano-structured ZnO/S-doped TiO2 composite (ZnO/S-TiO2) has been successfully prepared by hydrothermal method. The structure and morphology of the ZnO/S-TiO2 composite were characterized by SEM, XRD and XPS. The effect of dosage of sulfur doping into titanium dioxide and calcination temperature on photocatalytic activity of ZnO/S-TiO2 composite was discussed. The result indicated that Ti-O-S bond existed and homogeneous S doped TiO2 nanoparticles could be formed on the surface of ZnO. Under the conditions of 0.8 mol% of sulfur doping and the calcination temperature of 500℃, the synthesized photocatalyst exhibited the best photocatalytic activity for degradation of phenanthrene.