Transition metallic oxides have attracted considerable attention for supercapacitor applications because of their superior electrochemical performance at relatively low cost. Co3O4/NiO nanofilms were successfully prepared by calcination of precursor -Co(OH)2/-Ni(OH)2. XRD, XPS, SEM and TEM techniques were used to characterize the composition and morphology of as-prepared samples. The results demonstrated that Co3O4/NiO nanofilms presented graphene-like morphology with shrinkage and wrinkles. The Brunauer-Emmett-Teller (BET) measurement showed that specific surface area of Co3O4/NiO was 176.5 m 2 /g. Electrochemical properties tests indicated that the Co3O4/NiO nanofilms had a higher specific capacitance and better rate capability than that of precursor -Co(OH)2/-Ni(OH)2 at high current density. As to the cycling performance, the specific capacitance of Co3O4/NiO electrode would first increase from 556 F/g to 710 F/g quickly at 2 A/g after 80 cycles and then remained stable. Therefore, compared with that of precursor -Co(OH)2/-Ni(OH)2, the capacitance performance of as-prepared Co3O4/NiO nanofilms was improved after calcination. The possible reason for the enhancement of capacitance performance was discussed.