TiO2/ZnO composite nanofibers have been successfully prepared by electrospinning technique. X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, transmission electron microscopy, Raman spectrum, X-ray photoelectron spectroscopy and UV-Vis diffuse reflectance spectroscopy, were used to characterize the as-synthesized nanofibers. The photocatalytic studies revealed that the TiO2/ZnO nanofibers exhibited enhanced photocatalytic efficiency of photodegradation. Additionally, the recycling experiment of TiO2/ZnO nanofibers had been done, demonstrating that TiO2/ZnO nanofibers have high efficiency and stability.