This study presents the production of pure and different amounts of Ni-doped (4, 8, 12%) ZnS films on microscope glass substrate at 4005°C substrate temperature with Ultrasonic Spray Pyrolysis Technique and the effect of Ni doping on some physical properties of pure films. X-ray diffractometer (XRD), UV-Vis spectrophotometer, two-probe method and atomic force microscope (AFM) were used to analyze the structural, optical, electrical and surface properties of all films, respectively. XRD patterns contains broad peaks showing a low crystallinity level for the films. Ni doping caused ZnS films to have high absorbance values through the visible spectrum. Optical band gap energy values of ZnS:Ni thin films were determined to be between 3.71-3.96 eV. Two-probe measurements revealed that the electrical conductivity values of ZnS films increased significantly depending on the Ni doping. AFM results showed that the films have an almost homogeneous distribution with a rough surface. No significant change was observed for the surface properties of the films due to the Ni doping. As a result of all analyzes; it was seen that Ni doping has an important effect on the optical and electrical properties of ZnS films, without modifying the crystalline structure or surface texture.