Nickel ferrite NiFe2O4 is a typical soft magnetic ferrite with high electrical resistivity used as high frequency magnetic material. Neodymium (Nd3 t ) doped NiFe2O4 materials were fabricated using solid state reaction. The properties of the obtained material were investigated by X-Ray Diffraction (XRD), Scanning Electron Microscope (SEM), Fourier-Transform Infrared Spectroscopy (FT-IR), magnetic measurements on SQUID and M?ssbauer spectroscopy. It was found that the material consists of two different phases:Nd3 t doped NiFe2O4 and NdFeO3. The Nd3 t ions occupy cation sites of the NiFe2O4 inverse spinel structure. NdFeO3 phase occurred when the level of Nd3 t atoms exceed a percolation limit. The presence of both phases was confirmed by SEM observations. The M?ssbauer spectra analysis showed two sextets, which can be ascribed to iron atoms in tetrahedral and octahedral positions. From their intensities it is concluded that Nd3 t occupies octahedral sites in the spinel structure of NiFe2O4, which were originally occupied by Ni2 t .