The purpose of this research is to fabricate Cu-Ni nanoparticles of different sizes to investigate the topography and structural properties of these nanoparticles. Therefore, Cu-Ni nanoparticles in a carbon thin film were prepared by co-deposition of RF-sputtering and RF-PECVD. Samples containing Cu nanoparticle were grown on carbon substrate in attendance acetylene and then Ni layers with different thicknesses were grown over these Cu nanoparticles. Topography and structural properties were investigated by atomic force microscopy (AFM) and scanning electron microscopy (SEM), respectively.