ABSTRACT Nanocomposites rationally designed in structure and component are highly desirable for the development of electrodes in lithium-ion battery application for that they can take full advantages of different structures and components to achieve superior electrochemical properties. A nanocomposite with the two-dimension (2D) NiO nanoplate of a hexagonal structure and zero-dimension (0D) Co3O4 nanoparticles was synthesized by the hydrothermal method. Scanning electron microscopy, high-resolution transmission electron microscopy, X-ray diffraction and X-ray photoelectron spectroscopy were employed to characterize the composition, morphology, microstructure and chemical state of the nanocomposite, respectively. As an anode material of lithium-ion battery, the nanocomposite exhibits greatly improved specific capacities and stable cyclability of 633mAhg−1 at a current density of 100mAg−1 up to 70 cycles, much higher than the corresponding building block alone. The outstanding performance of the NiO/Co3O4 nanocomposite is attributed to the hybrid structure and the synergistic effect of different components. This large-scale and cost-efficient synthesis can be extended for the design and synthesis of transition metal oxides composite for high-performance electrochemical energy storage.