Lithium cobaltite, LiCo(2)0(4), prepared by thermal decomposition of nitrates salts was synthesized at 400 °C. X-ray Rietveld refinement showed the presence of two phases: a cubic spinel (Co(3)0(4)) and other corresponding to spinel-like, which could not be classified as LiCo(2)0(4) or LiCo0(2) since both crystallized in Fd3m S.G. Electrochemical determinations (charge-discharge curves and impedance spectroscopy measurements) showed that Li+ ion is inserted into the spinel lattice, with D = 8 10-16 cm s-1 at 2.00-2.25 V potential range whereas lithium extraction occurred at 3.2-3.8 V potential range.