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This study explores the incorporation of Palm Oil Fuel Ash (POFA) and Polyethylene Terephthalate (PET) into concrete to enhance its gamma-ray shielding capabilities while addressing environmental sustainability. POFA, a by-product of the palm oil industry, is rich in silica and exhibits excellent pozzolanic properties that strengthen the concrete matrix and improve its durability. PET, a widely available plastic waste, provides flexibility and enhances the overall mechanical properties of the concrete. The research examines various proportions of POFA and PET in concrete mixtures, focusing on their effects on density, compressive strength, water absorption, and radiation attenuation efficiency. The experimental results demonstrate significant improvements in the physical and mechanical properties of the modified concrete. The optimized mix (M3.3) achieved the highest density, compressive strength of 18.23 MPa, and a linear attenuation coefficient of 22.14, making it suitable for gamma-ray shielding. Furthermore, the incorporation of POFA and PET reduced porosity and improved durability, ensuring the material’s long-term performance in radiation-sensitive environments. The findings indicate that POFA-PET concrete offers a sustainable, cost-effective alternative to conventional shielding materials, particularly for use in medical and nuclear facilities, while contributing to effective waste management by utilizing industrial and plastic waste.