Characterization of partially inverse spinel ZnFe2O4 with high saturation magnetization synthesized via soft mechanochemically assisted route

ZnFe2O4 was prepared by a soft mechanochemical route from two starting combinations of powders: (1) Zn(OH)(2)/alpha-Fe2O3 and (2) Zn(OH)(2)/Fe(OH)(3) mixed in a planetary ball mill. The mechanochemical treatment provoked reaction leading to the formation of the ZnFe2O4 spinel phase that was monitored by XRD, TEM, IR and Raman spectroscopy. The spinel phase was first observed after 4 h of milling and its formation was completed after 18 h in both the cases of starting precursors. The synthesized ZnFe2O4 has a nanocrystalline structure with a crystallite size of about 20.3 and 17.6 nm, for the cases (1) and (2), respectively. In the far-infrared reflectivity spectra are seen four active modes. Raman spectra suggest an existence of mixed spinel structure in the obtained nanosamples. In order to confirm phase formation and cation arrangement, Mossbauer measurements were done. Estimated degree of inversion is about 0.58 for both starting mixtures. The magnetic properties of the prepared ZnFe2O4 powders were also studied. The results show that the samples have a typical superparamagnetic-like behavior at room temperature. Higher values of magnetization in the case of samples obtained with starting mixture (2) suggest somewhat higher degree of cation inversion. (C) 2014 Elsevier Ltd. All rights reserved.