An approach for the synthesis of copper nanoparticles ( CuNPs) embedded in poly ( vinylpyrrolidone) ( PVP) composite materials is proposed using a simultaneous irradiation process. The parameters, i.e., copper sulfate ( CuSO4) precursor, VP and PVP concentrations were optimized for synthesis of CuNPs under irradiation. Crosslinking of PVP system was analyzed by gel fraction and swelling degree using gravimetric measurement. Functionality, chemical composition and crystallinity of the CuNPs-PVP composite materials were characterized by FT-IR, SEM-EDS, XRD. Morphology of the CuNPs-PVP composite materials was observed using SEM. Light blue color of Cu2+ precursor in liquid polymer/monomer system changed to dark brown color of Cu in solid form. Stable CuNPs with the particle diameters ranging from ca.100 to 500 nm was successfully synthesized in the PVP solid materials. A simple and effective process for the preparation of the CuNPs-PVP composite materials serves as a new generation of process and functional nanomaterials for industrial applications.