Supercapacitors are regarded to be highly probable candidates for next-generation energy storage devices. Herein, a bimetallic Co/Ni MOF is used as a sacrificial template through an alkaline hydrolysis and selective oxidation process to prepare an accordion like ternary Nico(2)O(4)/beta-NixCo1-x(OH)(2)/alpha-NixCo1-x(OH)(2) composite, which is composed of Co/Ni(OH)(2) nanosheets with large specific surface as the frame and Nico(2)O(4) nanoparticles with high conductivity as the insertion, for supercapacitor application. This material exhibits both high specific capacitance (1315 F.g(-1) at 5 A.g(-1)) and excellent cycle performance (retained 90.7% after 10 000 cycles). This hydrolysis-oxidation process, alkali hydrolysis followed by oxidation with H2O2, offers a novel approach to fabricate the Ni/Co-based electrode materials with enhanced supercapacitor performance.