Radiation shielding composites based on polyvinyl chloride (PVC) reinforced with different weight ratios of Pb(NO3)2 (5, 10, and 20 wt%) were prepared using the solution-casting technique. Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy, and tensile testing method were used to characterize the PVC composite films. FTIR and XRD investigations illustrate the structural change and modification of the as-prepared PVC composites. The morphological analysis of the composite revealed that Pb(NO3)2 was dispersed uniformly within PVC polymer matrix. TGA revealed that the incorporation of Pb(NO3)2 improved the thermal stability of the investigated composites, whereas adding Pb(NO3)2 to the polymer matrix worsened its tensile properties. The as-prepared composite films were investigated for radiation-shielding of gamma-rays radioactive point sources (241Am, 133Ba, 137Cs, and 60Co). Linear attenuation coefficient (μ, cm−1), mass attenuation coefficient (μ/ρ, cm2/g), and half-value layer (HVL, cm) have been estimated from the obtained data using the MicroShield program. Reasonable agreement was attended between theoretical and experimental results. The deviation between the experiment and theoretical values of mass attenuation coefficient is being to be lower than 9%, and this can be correlated to the good distribution of Pb(NO3)2. The results revealed that adding Pb(NO3)2 to PVC polymer composites improved their mass attenuation coefficient. [ABSTRACT FROM AUTHOR]