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Based on the experimental and theoretical radiation attenuation, this study produced and tested a composite material made of polyester reinforced with SnO at varied concentrations and abbreviated as Pol-SnOx, where x = 0–60% with steps of 20 wt% Also, the polyester samples were doped with SnO of different particle sizes: Micro, Nano, and 50% Micro/50% Nano mix to investigate the effect of the particle size on the radiation attenuation performance. In the photon energy range of 0.015–15 MeV, their radiation shielding properties were empirically determined using an HPGe detector and theoretically determined using Phy-X/PSD software. The linear attenuation coefficient (LAC) values dropped from 1.361 to 0.022 cm−1 for Pol-SnO0, from 13.611 to 0.033 cm−1 for Pol-SnO20, from 31.700 to 0.049 cm−1 for Pol-SnO40, and from 61.076 to 0.076 cm−1 for Pol-SnO60 in the photon energy (Eγ) range from 0.015 to 15 MeV. The LAC values of the fabricated Pol-SnOx samples increased as the SnO concentrations increased. Also, the addition of 50% Micro/50% Nano mix particle size of the SnO to the polyester significantly increased the values of the LAC. The percentages of LAC improvement of SnO nano-particles were 16.625%, 13.236%, 8.714%, and 7.935% at the Eγ values of 0.059, 0.661, 1.173, and 1.332 MeV, respectively. Also, the LAC values were enhanced by adding SnO containing 50% Micro/50% Nano mix particles by 19.097%, 15.271%, 9.854%, and 9.071% at the Eγ values of 0.059, 0.661, 1.173, and 1.332 MeV, respectively, when compared to microparticles. The addition of 50% Micro/50% Nano Mix of SnO with 60% content to the polyester showed the highest LAC and radiation protection efficiency and lowest half-value layer and transmission factor among the other samples due to increased SnO doping and interparticle distances of the Micro and Nano mix.