Abstract ZnO/PVC nanocomposites films have been prepared by the solvent casting method and investigated by various techniques. All results show good dispersion of ZnO nanoparticles in the polymeric matrix. XRD revealed that pure PVC films are partially crystalline with hallow peak but ZnO nanoparticles have wurtzite structure and the nanocomposite films were almost the same as those of ZnO with decrease in the degree of crystallization, causing increase in the amorphous region. FT-IR presented the same spectra for nanocomposites in the wavenumber range 700–3100 cm −1, weak band located at 500–700 cm −1,which can be attributed to stretching of ZnO bond and an increase of the bending band of OH at 1631 cm −1 was observed. The surface of the films was analyzed by SEM, which becomes rough with some small aggregates compared with pure PVC with good distribution in the entire surface region with bright spots. TEM revealed a regular crystalline lattice superimposed on an amorphous background due to carbon support and PVC matrix and the structure of these particles is hexagonal. In addition, the nanocomposites films have higher glass transition temperature, specific heat and thermal stability relative to those of pure PVC because of strong interaction among ZnO nanoparticles and PVC.