NiO is known for superior strength, corrosion resistance and low cost. NiO is believed to enhance hole extraction and reduce the nonradiative recombinations. Special structural properties of nickel oxide nanoparticles make itapplicable in different areas such as hole transporting material in perovskite and dye-sensitized solar cells. In this study, nickel oxide nanostructured particles were grown by co-precipitation and different parameters were optimized based onstructural phase and morphology. Using suitable solvents and binders, dispersions of the selected NiO nanoparticles and multiwalled carbon nanotubes (MWCNTs) were prepared for spin and spray coating techniques, respectively. Finally, the effect of the sintering process on different properties of the grown NiO and MWCNTs based single and bi-layered films were studied for crystalline phase identification, morphological, electrical, optical and wettability studies. Analysis ofobtained results indicated that the sintering effect has improved charge conductivity, mobility, film transmittance and resistance of layers to the moisture.