Nanoparticles of nickel ferrite are prepared from the precursors, mixed metal carboxylates. The precursors were characterized by IR, TG-DTA analysis. The precursor once ignited with burning splinter at room temperature, glows and the glow spreads over the entire bulk completing the autocatalytic combustion of the precursor to ultrafine ferrite. The particles size of nickel ferrites are determined by X-ray diffraction and TEM images. The surface morphology of ferrites is revealed by SEM images. The average particles size of the nickel ferrites was found to be ? 21 nm.