Nanosized spinel nickel ferrite particles have attracted considerable attention and efforts continue to investigate them for their technological importance to the microwave industries, high speed digital tap or disk recording, repulsive suspension for use in levitated railway systems, ferrofluids, catalysis and magnetic refrigeration systems. Nanosize nickel ferrite powders (NiFe2O4) have been prepared by combustion reaction using nitrates and urea as fuel. The resulting powders were characterized by X-ray diffraction (XRD), BET, and transmission electron microscopy (TEM). The results showed nanosize nickel ferrite powders with high specific surface area (55.21 m2/g). The powders showed extensive XRD line broadening and the crystallite size calculated from the XRD line broadening was 18.0 nm. The samples were uniaxially compacted by dry pressing, sintered at 1200°C/2h and characterized by bulk density, SEM and magnetic properties measurements. The samples showed uniform microstructures with grain size of 4.45 μm, maximum flux density of 0.18T, field coercive of the 488 A/m, and hysteresis loss of 47.58 W/kg.