Nanostructured CoFe 2 O 4 particles were prepared by a sonochemical approach, first by preparation of the amorphous precursor powders, followed by heat treatment at relatively very low temperatures. The precursor was prepared by sonochemical decomposition of solutions of volatile organic precursors, Fe(CO) 5 and Co(NO)(CO) 3 , in Decalin at 273 K, under an oxygen pressure of 100-150 kPa. The amorphous nature of these particles was confirmed by various techniques, such as scanning and transmission electron microscopy (SEM and TEM), electron microdiffraction, and X-ray diffractograms. Magnetic measurements, Mo ¨ssbauer, and electron paramagnetic resonance (EPR) spectral studies indicated that the as-prepared amorphous particles were superparamagnetic. The Mo ¨ssbauer parameters and the significantly low (45 emu/g) observed saturation of magnetization of the annealed sample, compared to that of the bulk sample (72 emu/g), reflected its nanocrystalline nature.