Effect of Thermal Treatment at Inert Atmosphere on Structural and Magnetic Properties of Non-stoichiometric Zinc Ferrite Nanoparticles

Zinc ferrite nanoparticles were obtained by chemical methods (co-precipitation and thermal decomposition of metalorganic compounds) and systematically probed with volume (XRD, VSM), microscopic (TEM) and element sensitive probes (ICP-OES, Mössbauer Spectroscopy, XPS, XAFS). Magnetic studies proved the paramagnetic response of stoichiometric ZnFe2O4 (ZF) nanoparticles, while superparamagnetic behavior was observed in as-synthesized, non-stoichiometric ZnxFe3−xO (NZF) nanoparticles. Upon annealing up to 1400 °C in an inert atmosphere, a significant change in the saturation magnetization of NZF nanoparticles was observed, which rose from approximately 50 up to 140 emu/g. We attribute this effect to the redistribution of cations in the spinel lattice and reduction of Fe3+ to Fe2+ during high-temperature treatment. Iron reduction is observed in both ZF and NZF nanoparticles, and it is related to the decomposition of zinc ferrite and associated sublimation of zinc oxide.