NiCoO₂ microspheres were successfully synthesized via an easy hydrothermal method, followed by an annealing process at 350 °C under a nitrogen atmosphere. The X-ray diffraction results show that a single phase NiCoO₂ was synthesized. The results of electrochemical measurements show that the NiCoO₂ exhibits a high specific capacitance of 760 and 470 F g⁻¹ at current densities of 1 and 16 A g⁻¹, respectively, and the specific capacitance retention is 40.9% after 5000 cycles at the current density of 16 A g⁻¹. This reveals the great potential of NiCoO₂ as an electrode material for high-performance supercapacitors.