CoO–NiO–C nanocomposite materials with different morphology are successfully synthesized by using co-precipitation and subsequent pyrolytic carbon reduction method. The structure and morphology of obtained materials are investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The XRD patterns of samples display the diffraction peaks of 3CoO·5NiO cubic crystal. Moreover, the synthesis conditions which strongly impact on the morphology and electrochemical properties of the CoO–NiO–C materials are systematically investigated. When CoO–NiO–C materials are used as anodes for lithium ion batteries, the sample obtained at 600°C exhibits the best cycling performance, which shows a reversible capacity about 562mAhg−1 at the current density 100mAg−1 after 60 cycles. On the other hand, this material also exhibits a superior rate performance. The excellent performance of samples could be attributed to the small and uniform particle size and introducing of metal oxides composite structure, which could improve the kinetic behavior and accommodate the volume changes during cycling.