The growing use of nuclear radiation and the harmful effects of radiation exposure underscore the need for continued research into materials for radiation shielding. In the current study, shielding features of B4C, Fe2O3, Al2O3, and their composites (xB4C/yFe2O3/zAl2O3, x:y:z=1:1:1, 3:4:3, and 3:3:4 wt%) were evaluated. The samples were analyzed using scanning electron microscopy (SEM) and x-ray diffraction (XRD). The gamma shielding parameters for the samples were determined using the Phy-X/PSD program. The results indicate that the sample S2 (Fe2O3) has a higher capacity to absorb γ-rays than the other analyzed samples. This is also supported by the notably lower mean free path and half-value layer values for S2 compared to the other samples. The experimental values ofMACfor bulk and nano-samples at energy 0.662MeVemitted from 137Cs isotope have been compared. Additionally, sample S1 (B4C) demonstrates significantly higher fast neutron attenuation than the other samples with a removal attenuation coefficient of 0.095 cm−1. Moreover, Thermal neutron scattering cross-sections of prepared samples were calculated for neutron energy of 0.025 eV with a neutron flux of 108 n/cm2/s. Therefore, the study found that thickness 1mmof S1 sample prevented 67% of the incident neutrons, while thickness 2mmwas able to prevent almost all neutrons, which indicates that S1 sample is better compared to the other investigated samples. Meanwhile, the results indicate that the composites S4, S5, and S6 are highly efficient in shielding both gamma rays and neutrons.