Nanocrystalline copper-cobalt ferrites with composition Cu 1-x Co x Fe 2 O 4 , where x = 0.2 and 0.8, were synthesized by mechanochemical treatment of co-precipitated precursors. The ferrite powders were characterized by XRD and Mössbauer spectroscopy. Results proved obtaining of spinel ferrites with crystallite size smaller than 10 nm. Increasing of crystallite size of samples with increasing of mechanochemical treatment duration was established, too. Catalytic properties of obtained ferrites were tested in reactions of oxidation of CO, methanol and dimethyl ether. High catalytic activity of nanocrystalline copper-cobalt ferrites toward CO and CH 3 OH (about 100% conversions of CO and CH 3 OH at 160°C) and moderate activity toward (CH 3 ) 2 O oxidation were established. The results obtained revealed that the Co/Cu atomic ratio is an important factor determinant the behavior of catalysts toward methanol and DME oxidation.