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The scope of the present work is in enhancing the particle size, and dielectric properties of Mg-substituted Cobalt ferrites nanoparticles prepared by sol–gel auto combustion method. The different ratios of Mg-substituted Co Ferrites (Co[Formula: see text]MgxFe2O4([Formula: see text], 0.05, 0.10, 0.15, 0.20 and 0.30)) are calcinated at 850[Formula: see text]C. The synthesized nanoparticles were characterized by powder XRD, FTIR, FE-SEM, EDX techniques and dielectric behavior. The structural parameters were confirmed from powder XRD and the average particle size is obtained from 39 to 67 nm due to the substitution of Mg[Formula: see text] which was calculated by Debye Scherrer’s formula. FE-SEM showed the surface morphology of the different ratio of the sample. The dielectric loss has measured the frequency range of 50[Formula: see text]Hz–5[Formula: see text]MHz. From electrical modulus, conductivity relaxation and thermal activation of charge carriers has been discussed.