Abstract:The layered structure LiMO 2 (M=Co, Ni and Mn) cathode materials for lithium ion batteries are under intensive investigation world-wide. In the present study, magnesium doped LiNiO 2 (LNO) samples with the chemical composition of LiNi 1-x Mg x O 2 (x= 0.02, 0.04, 0.06 and 0.08) are prepared by solid state reaction method at 775 o C for 20 h in air atmosphere. The crystal structure, morphology and bonding nature of the synthesized materials are systematically characterized by X-ray diffraction; field effect scanning electron microscopy and Fourier transform infrared spectroscopy. The Mg doped LiNiO 2 are found to have hexagonal structure of the α-NaFeO 2 (space group, m R3 ) from the XRD. From FESEM micrographs, it is found that the smooth and uniform particle size is in the range of 0.88-2.35 µm. The FT-IR shows the presence of two broad vibrational bands between 400 to 1000 cm -1 corresponding to the trigonally LiO 6 and MO 6 octahedra sites.