Binary transition metal oxides exhibit improved properties including good redox potentials and electrical conductivities compared with single metal oxides as electrode materials in energy storage. Herein, ZIF-67 is prepared by a one-step method using Co 2+ as the central metal ion, 2-methylimidazole as the organic ligand, and methanol as an organic solvent at room temperature. Hollow NiCo 2 O 4 and sheet-like Co 3 O 4 /NiCo 2 O 4 derived from bimetallic imidazolate framework precursors were synthesized by adding cobalt and nickel ions in appropriate proportions. A hollow and porous structure is achieved for the reaction between a nickel salt and ZIF-67, and this unique nanostructure provides a high active surface area, which is beneficial to the electrochemical properties. Several samples are prepared and used as electrode materials for electrochemical tests in 6 M KOH. As a result, the Co 3 O 4 /NiCo 2 O 4 electrode with a sheet nanostructure showed a high specific capacitance of 846 F g −1 at a current density of 0.5 A g −1 . This Co 3 O 4 /NiCo 2 O 4 electrode material is promising for future studies on high-performance supercapacitors to solve emerging energy-related problems. [Formula: see text]