Pure Co3O4 and CoFe2O4 phases are obtained by co-precipitation method at calcination temperature 500 °C. FeCo2O4 material undergoes spinodal decomposition at calcination temperatures 500–800 °C. The Co2+ ions are identified as the active species. Supported catalysts display a better catalytic activity than their bulk analogs in the total ethanol oxidation. The values of the activation energies obtained are relatively low compared with those of literature.