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The gamma-radiation shielding capabilities of a Ni 0.2 Mg x Zn 0.8-x Fe 2 O 4 nanocrystal, synthesized using the sol-gel auto-ignition process, were described in the present investigation. The synthesized materials were analyzed using different techniques such as XRD, UV–Vis, FTIR, FE-SEM, and EDS to investigate their structural, optical, and functional group morphological properties, and elemental analysis. Additionally, utilizing various gamma-ray sources and a NaI (Tl) scintillation detector, we investigated the gamma-ray shielding parameters for the prepared materials. The cubic spinel structure of all produced Nanoferrites is clear from X-ray diffractograms, which show no contaminated phases. Pellets of nanocrystalline spinel ferrites have been exposed to gamma radiation from various sources by varying the intensity of the radiation dose. Utilizing Phy-X/PSD Software, a comparative analysis of the mass and linear attenuation coefficients, mean free path, half value layer, tenth value layer, effective atomic number, and effective electron density for synthesized spinel ferrites is performed at 122–1330 keV. Using the geometric progression (G-P) fitting technique, the gamma-ray energy absorption build-up factor (EABF) for four selected ferrites is explored at incident photon energy levels ranging from 0.015 to 15 MeV. It is found that the Compton scattering process is mostly responsible for the EABF maximum in an intermediate region. K1 has a higher EABF value than other ferrites, which is largely determined by the crystallite size effect and the chemical composition of the material. There is a good agreement between the theoretical and experimental results. Among the studied samples, sample K1 and K4 have superior gamma-ray and fast neutron attenuation capabilities respectively than its counterparts. The current study offers a thorough examination of the chosen iron oxides in the context of gamma and neutron radiation. • The values of μ m , μ, Z eff , λ, HVL, TVL were determined experimentally using NaI (Tl) detector. • Experimental results have been supported with Phy-X/PSD Software values. • The energy absorption buildup factor have been calculated using G.P. fitting method. • The values of macroscopic removal cross-sections for neutrons were determined. • Measured data in mixed neutron-gamma radiation field are useful in nuclear medicine application. [ABSTRACT FROM AUTHOR]