Nano crystalline samples of nickel zinc ferrite, Ni0.5Zn0.5Fe2O4 were prepared by mechanochemical route in a planetary ball mill starting from two mixtures of the appropriate quantities of the powders: case (1) oxide powders: NiO, ZnO and alpha-Fe2O3 in one case, and in the second case (2) hydroxide powders: Ni(OH)(2), Zn(OH)(2) and Fe(OH)(3). In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 5 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman, IR and Mossbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase Ni0.5Zn0.5Fe2O4 samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. The deconvolution of Raman spectra allows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion. (C) 2014 Elsevier Ltd. All rights reserved.