Thin films of copper oxide nanoparticles mixed with 6% nickel oxide are deposited on glass and Si substrates with orientation (111) utilizing pulsed laser deposition technique for the manufacture of hydrogen gas sensor. The films are annealed in air at 400 °C for two hours, then the structural and morphological properties are characterized using x-ray diffraction and atomic force microscopy. The results of CuO:NiO/Si films are exhibited a polycrystalline monoclinic CuO and cubic NiO phases. In addition, the peak of Si located at 28.3º which refer to (111) direction. Furthermore, this peak becomes very broad with varying full width at half maximum for etching current density of 30 mA/cm2 at time of 30 min which confirms the formation of pores on the crystalline silicon surface. On the other hand, the average diameter of 84.31 nm and 34.98 nm for CuO:NiO on a glass substrate and PS, respectively, were obtained. A sponge-like structure is produced for PS which reveal that a part of pores transform to a larger structure. The peak sensitivity of 204.8% was observed at optimum operating temperature of 350°C.