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In this work we studied the effect of mechanochemical activation on the formation of the cobalt ferrite phase from iron and cobalt oxalates. X-ray phase, X-ray diffraction and synchronous thermal analysis, scanning electron microscopy, low-temperature nitrogen adsorption-desorption method were used to study the composition and properties of the resulting product. It has been established that cobalt ferrite is formed at a temperature of 1100 °C during solid-phase interaction of the initial components, and the use of mechanochemical activation of the initial components in a roller-ring vibration mill makes it possible to reduce the synthesis temperature to 400 °C. It is shown that CoFe2O4 obtained using the method of mechanochemical synthesis has a more developed specific surface area and porous structure in comparison with cobalt ferrite obtained by the ceramic method.