New route was used for preparation of mixed nickel-magnesium ferrite (Ni_0.5Mg_0.5Fe₂O₄). Various techniques were used to characterize the as prepared product such as X-ray diffraction (XRD), infrared (IR) spectroscopy, scanning electron micrographs (SEM), energy dispersive X-ray (EDX) and a vibrating sample magnetometer (VSM). The crystallite size, lattice constant, unit cell volume, density of Ni_0.5Mg_0.5Fe₂O₄ phase has been determined. The investigated method led to prepare single phase of spinel nickel-magnesium ferrite depending upon the XRD and IR results. SEM and EDX techniques showed the as synthesized materials were spongy, homogeneous and fragile. The concentrations of O, Ni, Fe and Mg species involved in Ni_0.5Mg_0.5Fe₂O₄ sample were investigated from the uppermost surface to the bulk layers. The saturation magnetization (Ms), remanence magnetization (Mr) and coercivity (Hc) of the as synthesized composite were 34 emu/g, 12 emu/g and 29 Oe, respectively.