Filler particle size is an important particle that effects radiation attenuation performance of a composite shielding material but the effects of it have not been exploited so far. In this study, two mineral (hematite–ilmenite) with different particle sizes were used as fillers in a polymer-matrix composite and effects of particle size on shielding performance was investigated within a widerange of radiation energy (0–2000 keV). The thermal and structural properties of the composites were also examined. The results showed that as the filler particle size decreased the shielding performance increased. The highest shielding performance reached was 23% with particle sizes being between <7 and <74 µm.