Layered LiCo 1−x Mg x O 2 (x=0.0, 0.1, 0.2, 0.3 and 0.5) oxide materials were synthesized using LiNO 3 , Co (NO 3 ) 2 , Mg(NO 3 ) 2 as the precursors, and the effect of the dopants on the electrochemical properties was investigated. thermogravimetric/differential thermal analysis was carried out to observe the phase transformations of LiCo 0.9 Mg 0.1 O 2 . The phase purity and cation environment of the synthesized oxides were characterized using X-ray diffraction and Fourier transform infrared spectroscopy. The particle size, nature, morphological properties and composition of the synthesized oxides were examined by TEM and SEM with energy dispersive X-ray spectroscopic analysis. Finally, the electrochemical behavior of the prepared layered materials was studied using cyclic voltammetry and charge-discharge cycling. LiCo 0.8 Mg 0.2 O 2 has good cycling results when compare to other doped and undoped materials. These results have been also supported by cyclic voltammograms.