Herein we report the effect of γ-irradiation on the structural and AC electrical properties of Ni-Zn nanoparticles synthesised via the citrate auto-combustion technique. The x-ray diffraction (XRD) analysis of the samples revealed a decreasing trend of the crystallite size with increasing concentration of Zn2+ ions, and -irradiation alters the crystallite size for more Ni2+ ion concentrations. The lattice constant was found to increase with Zn2+concentration, with the highest for x = 0.6. However, after irradiation, substantial change occurs. The lattice strain is greater for x = 1 as well as lower for x = 0.4. The observable modifications in the morphology of the samples upon irradiation are identified. The AC-electrical behaviour of the sample was studied before and after γ-irradiation in the frequency range of 1 MHz–23 MHz. Studies show that the dielectric constant increases on irradiation, whereas the dielectric loss and AC conductivity decline after irradiation. The dielectric relaxation changes from non-Debye to Havriliak–Negami relaxation, which is the significance of asymmetric broadness in the relaxation process. The collective AC electrical properties were signifies the radiation absorption response.