Copper Ferrite has been prepared by solid state synthesis of milled mixtures of copper basic carbonate [Cu(OH)2 · CuCO3] and iron (II) oxalate dihydrate [FeC2O4 · 2H2O]. The reaction mechanism has been studied by simultaneous TG/DSC analysis: the different steps of the mass loss process have been individuated along with the relevant enthalpy terms starting from both physical and mechanically activated mixtures. CuFe2O4 has been synthesized by annealing the mechanically activated mixture at 750–800 °C while no pure CuFe2O4 is obtained by annealing the physical mixture at temperatures as high as 1100 °C. CuFe2O4 has been characterized as concerns the molar het capacity, the tetragonal–cubic transition enthalpy and the Curie point.