Abstract: The ferrites of Cuo-ZnO-Fe2o3 solid solution series near the molar ratio of ZnxCu1-x were prepared by direct heating of their coprecipitated hydroxides using NH4OH as precipitating agent where x=0.0, 0.2, 0.5, 0.8 and 1.0. Additional amounts of Cu and Zn sulphates were added to compensate the loss during the coprecipitation of the hydroxides. The ferritized samples were characterized by chemical analysis, XRD. DTA, TGA and SEM. XRD of both Zn0.2Cu0.8Fe2O4 and Zn0.5Cu0.5 Fe2O4 that indicates the formation of a heterogeneous ferrite material of ZnFe2O4 and CuFe2O4 mixed with variable amounts of α-Fe2O3. Zn and Cu ferrites were observed only in Zn0.8Cu0.2Fe2O4.From TGA-time relation, the activation energy of the different transformation phases were calculated. It is found that, the activation energy of ZnFe2O4 is slightly equal to 3/2 of that for CuFe2O4. Dielectric measurements show that the electrical behaviour depends on the ordering and disordering of the phases.