We recently developed a novel process Carbon Combustion Synthesis of Oxides (CCSO) to rapidly produce high purity, submicron, porous powders of complex oxides. The crystalline LiCoO2 nanoparticles were synthesized by carbon combustion synthesis, and characterized by TEM, XRD, and BET methods. The major parameters affecting the process are the carbon concentration in the reactant mixture and the ability of the oxygen infiltration to the reaction zone. A stable self-propagating reaction front can be obtained only at carbon and oxygen concentrations exceeding a critical value. We examined effects of process variables such as carbon concentration and flow of oxygen on the particle size and crystal structure. The average particle diameter increased with an increasing the concentration of carbon and oxygen flow rate. maximum combustion temperature by controlling the also led to an increase in the average diameter of the particles. The crystalline nanoparticles synthesized were nearly spherical, and their average particle diameters ranged from 60 to 200 nm. Electrochemical characterization of the synthesized lithium cobaltate was made using 8-channel battery analyzer with multiple charge-discharge cycles under constant voltage-constant current modes. The results are well comparable to best commercial cathode powders available, showing capacity about 200 mAh/g.