NixCo1-x(OH)(2) composite microspheres with uniform sizes are successfully synthesized with the assistance of alkali solution by employing a bimetallic Co-Ni-metal organic framework (Co-Ni-MOF) as both the precursor and the self-sacrificing template. The as-obtained NixCo1-x(OH)(2) composite demonstrates excellent electrochemical performance, including a high specific capacitance of 1235.9 F g(-1) at a current density of 0.5 A g(-1), good electrochemical stability, with similar to 73% retention of its initial capacitance after 10 000 cycles, and a high rate capability; this composite exhibits great application prospects as a novel electrode material for supercapacitors.