NiO nanoparticles with average particles size of 30nm are synthesized using a one-pot metal–organic framework-combustion (MOF-C) technique, for use as an anode material in rechargeable lithium ion batteries (LIBs). The structural and electronic properties of these nanoparticles are studied using various techniques, including powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and N2 adsorption/desorption studies. The as-synthesized NiO nanoparticles sustained reversible stable capacities of 748 and 410 mAh/g at applied current densities of 500 and 1000mA/g, respectively, after 100 cycles. Furthermore, the anode displays a notable rate capability, achieving a stable capacity of ∼200 mAh/g at a high current density of 10 A/g. These results indicate that the size of the NiO nanoparticles and their high surface area influence their electrochemical properties. Specifically, this combustion strategy is clearly favorable for improving the cyclability and rate capability of various metal oxides in rechargeable battery electrodes.