Single phase LiNi 1 - y Co y O 2 (y=0.7) with fine particles were prepared by two different low-temperature methods, namely sol-gel and combustion techniques. It was found that bulk quantities of submicron-sized particles of layered LiNi 0 . 3 Co 0 . 7 O 2 can be obtained at temperatures below 400 o C by these solution techniques. The methods involved the mixing of either acetates or nitrates of the metals, Ni and Co, with a chelating agent, carboxylic acid (sol-gel method) or a complexing agent, glycine (combustion method) in an aqueous medium. Both carboxylic acid and glycine acted as fuels, decomposed the homogeneous precipitate of metal complexes at low temperature, and yielded the free impurity LiNi 0 . 3 Co 0 . 7 O 2 compound. The synthesized products were characterized by structural (XRD, SEM), spectroscopic (FTIR) and thermal (DTA-TG) analyses. The electrochemical performance of the synthesized products in rechargeable Lithium cells were evaluated using a non-aqueous organic electrolyte mixture of 1M LiPF 6 in EC+DMC. The electrochemical behavior of synthesized LiNi 0 . 7 Co 0 . 3 O 2 is discussed in relation with its synthesis procedures.