LiCoO2 has been synthesized by a solid-state synthesis route involving the decomposition and intercalation of hydroxide precursors generated by precipitation and freeze-drying. Cyclic voltammetry of LiCoO2 obtained by heating at 100 degrees C for 2 h has shown this material to be electrochemically active with an initial discharge capacity of 92 mA h g(-1). Optimization of processing conditions reduced the firing time to as little as 2 h at 800 degrees C, producing LiCoO2 powders with high reversible capacity (142 mA h g(-1)), good rate capability, and good cyclabilily. The favourable performance of this oxide powder in LiCoO2/C lithium-ion cells using the present oxide powders shows the instant synthesis route to be promising and cost-effective for lithium-ion battery applications.