This study describes a rapid synthesis of Co1-xCuxFe2O4 nanoparticles using sol–gel auto-ignition and the produced materials were examined using different techniques such as XRD (X-Ray Diffraction), UV–Vis (Ultraviolet–visible), (FTIR Fourier Transform Infrared Spectroscopy), FE-SEM (Field emission scanning electron microscopy), and EDS (Energy-dispersive X-ray spectroscopy) to explore their structural, optical, and functional group morphological properties, and elemental analysis. Additionally, utilizing several gamma-ray sources and a NaI (Tl) scintillation detector, we studied the gamma-ray shielding characteristics for the prepared materials. Experimental results were validated by the results of XCOM program and the Geant4 simulations. For four chosen ferrites, the gamma ray energy absorption build-up factor is investigated at 0.01–15 MeV incident photon energy and penetration depths of 1–40 mean free path, mfp, using the geometric progression fitting technique. Ferrite samples can be employed as radiation attenuators across a range of nuclear domains, as per the findings of this study. In comparison to the other spinel ferrites, the Co1-xCuxFe2O4 (x = 0.75) ferrite demonstrated superior shielding capabilities. Important details regarding the physio-chemical properties of spinel ferrites and their ability to shield against gamma radiation are provided in the present study.