ZnFe 2 O 4 was prepared by a soft mechanochemical route from two starting combinations of powders: (1) Zn(OH) 2 /α-Fe 2 O 3 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 ZnFe 2 O 4 spinel phase that was monitored by XRD, TEM, IR and Raman spectroscopy. The spinel phase was first observed after 4h of milling and its formation was completed after 18h in both the cases of starting precursors. The synthesized ZnFe 2 O 4 has a nanocrystalline structure with a crystallite size of about 20.3 and 17.6nm, 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, Mössbauer measurements were done. Estimated degree of inversion is about 0.58 for both starting mixtures. The magnetic properties of the prepared ZnFe 2 O 4 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.