Pure and nickel-doped cadmium sulphide (NixCd1-xS where x= 2.5%, 5%, 7.5%) nanostructure thin films were successfully prepared by spray pyrolysis method on glass substrate at 350 °C. The films characterized using X-ray crystallography diffractmeter, Scanning Electron Microscope, Atomic Force Microscope and Uv-visible analysis in order to explore the properties of thin film. Structural studies revealed that the deposited films exhibit hexagonal structure with strong intensity at (002) plane. Structural parameters such as crystallite size, strain and dislocation density were calculated for films with different doping concentration. AFM measurements showed that the average diameter increased with increasing Ni doping, where surface roughness and root mean sequre decreased with increasing Ni doping, SEM images show that thin film have been grown and converted into nanowire with increasing of Ni content.Finally, Uv-visible analysis show that the optical band gap of CdS decreased from 2.44 to 2.38 eV with increasing of Ni doping concentrations.