Abstarct: Nanometer size structures are an intermediate form of matter which exhibit exotic physical and chemical properties different from those observed in bulk three-dimensional materials. A reduction in particle size to nanometer scale results in various interesting properties compared with their bulk properties. Having a large surface area, mextal oxide nanomaterials show great advantages over conventional materials in many applications. NiO is considered to be a model semiconductor with p-type conductivity films due to its wide band-gap energy range from 3.6 to 4.0 eV. In recent years NiO nanostructures widly have been study duo to useful electrical and magnetical properties. This research include two sets of experiments. in first set of experiments NiO nano- structures syntesised by heat treatment in O2 atmospheric, that first Ni pelletswere prepared and then oxidized under specific conditions. in second set of experiments Nickel–lithium oxide alloy transparent conducting films deposited by spray pyrolysis technique .The sensing Performance of the NiO thin films were investigated by aceton vapor.Both nanostructures and thin films were characterized scanning electron microscopy, EDX analysis and X-ray diffraction.