The one dimensional (1D) Ni-ZnO nanoparticles have been synthesized by a simple hydrothermal method. A novel photocatalyst of nanostructured Ni-ZnO which immobilized on polyacrylonitrile nanofibers were successfully fabricated using electrospinnig technique. The structures of nanofibers were characterized by various techniques including Scanning Electron Microscope (SEM), X-ray powder Diffraction (XRD), Fourier transform infrared (FT-IR), UV-Vis diffuse reflectance (DR) and thermogravimetric analys (TGA). The Ni-ZnO/PAN nanofibers photodegradation efficiency was optimized with factorial design method in order to act highly effective in the photocatalytic degradation of Methyle orange (MO). The highest decolorizing efficiencies using introduced material were achieved by 0.8 g l(-1) of catalyst and 10 mg l(-1) of MO at natural pH under visible light irradiation. The obtained results exhibited that Ni-ZnO/PAN nanofibers have high visible light photocatalitic activities. Overall, the presented material can be used as an efficient, low cost and healthily secure photocatalyst in the field of water treatment.