Lithium cobalt oxide is synthesized by a novel solution combustion procedure. In this synthesis, a solution mixture of lithium nitrate, cobalt nitrate and glycine fuel is heated to 500, 600 and 700 °C for 3 hours to obtain an ordered crystalline-layered compound. Physical properties of the synthesized cathode materials were evaluated using a XRD, SEM and particle size analyzer. The charge-discharge cycling characteristics of the synthesized lithium cobalt oxide heated at 700 °C exhibited better performance than other materials.