In the present work, we report the detailed Powder XRD Rietveld refinement and elucidation of structural factors of Ni0.6Zn0.4GdyFe2-yO4 nanoferrites. The Ni0.6Zn0.4GdyFe2-yO4 nanoferrites synthesized via low-temperature citrate gel combustion technique for the various levels of Gd3+ ion concentration (y = 0.0, 0.1, 0.15 and 0.20). The generated structural factors signify the dependence on the concentration of Gd3+ ions. The prepared samples were found to crystallize in the Fd-3m space group and also identified their occupancies; some of the Fe3+ ions of the octahedral site at the 16d position will be replaced by Gd3+ ions. The lattice constant and crystallite size dropped to a low value for y = 0.1, and then, later, noticed the small increment. The crystallite sizes of the sample are to fall in the range of 26.1 nm–37.6 nm. The cation distribution among the tetrahedral (AII) and octahedral sites (BII) has been estimated. The obtained values correlate with Gd3+ ion concentration, and the radius variation of AII and BII sites signifies the migration of Fe3+ ions from the BII site to the AII sites. The force constant of Metal-Oxygen bonds was determined from the infrared spectrographs; the force constant was found to be relatively low with the BII site. The DC electrical conductivity infers the semiconducting nature and distinct phase of conductivity, which is attributed to the magnetic phase change due to temperature. The magnetic curie temperatures of the sample are obtained by the Arrhenius plot, which signifies the dependence of Gd3+ion concentration.
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