Lithium cobalt oxide (LiCoO<inf>2</inf>) powder was prepared by co-precipitation method and annealed at different temperatures of between 300 and 700 °C. The effect of annealing temperature and effect washing process with deionized water on the crystal structures of the prepared LiCoO<inf>2</inf> powders were thoroughly studied by Synchrotron powder X-Ray Diffraction (Syn-XRD), X-ray Absorption Spectroscopy (XAS), Dispersive Raman Microscopy (Raman) techniques. The change in chemical composition as a function of annealing temperature was also investigated by X-ray Photoelectron Spectroscopy (XPS) technique. The crystal structural results identified the phase evolution of the prepared LiCoO<inf>2</inf> powders upon heat treatment. The formation of HT-LiCoO<inf>2</inf> phase was observed at annealing temperature as low as 300 °C.
