This study has been devoted to investigating the radiation shielding performance of Poly(vinyl chloride)-based nanostructures lead oxide (PbO) and tungsten oxide (WO3) reinforced composites.The SEM (SEM) images depicted the particle size and morphol. of nanostructures such as PbO nanorods and WO3 nanoparticles.X-ray diffraction (XRD) results demonstrated a successful fabrication of a hybrid nanocomposite.The gamma-ray spectroscopy experiments have been carried out using a NaI(Tl) scintillation detector and Cs-137, Co- 60, and AM-241 sources and X-ray.The different weight percentages of each by mass were 5, 10, 20, 30, and 40 wt %, of mixed composite (35, 30, 20, 10, 5 wt % WO3 + 5, 10, 20, 30, 35 wt % PbO).The mass attenuation coefficients of the investigated composites were measured as a function of gamma-ray energies and X-rays utilizing standard radioactive sources.Increasing the PbO or WO3 nanostructures′ weight percentages in the nanocomposites leads to increased radiation attenuation.Based on the results, the best radiation attenuation, the optimal half-value layer, the tenth value layer, and the mean free path were for PVC/WO3 5% + 35% PbO and PVC/WO3 10% + 30% PbO hybrid nanocomposite for Am-241, Cs-137, Co-60, and X-ray that replaced hybrid nanocomposite PVC/PbO 40%.