The organic films containing metal particles were prepared by rf ion plating system. The metal was evaporated during plasma polymerization of organic monomer, in order to make polymer–metal composite materials. The organic films containing metal obtained was observed by transmission electron microscopy to study the structures, and measured by x-ray photoelectron spectroscopy to find the ratio of components. These films were found to have mixed metal and metal carbide. Moreover, these films showed the characteristics of semiconductorlike electrical properties.