ABSTRACT The LiNi1/3Co1/3Mn1/3O2 has been intensively investigated and viewed as a promising cathode material to be utilized in rechargeable lithium-ion batteries because of its high capacity, good thermal stability and excellent rate capability. In our laboratory, LiNi1/3Co1/3Mn1/3O2 has been prepared using Self-Propagating Combustion Method, which is utilized reaction between metal nitrates and combustion agent. In this study, three different combustion agents have been used. There are glycine, hexamethylene tetramine (HMTA) and citric acid. The voluminous loose LiNi1/3Co1/3Mn1/3O2 powder that produced from self propagating combustion reaction was calcined at the temperature of 800oC and electrochemically characterized using electrochemical system. Electrochemical analysis indicated that the discharge capacity is dependance to the calcination temperature and the type of combusting agent has been used. The highest specific capacity of LiNi1/3Co1/3Mn1/3O2 at 211 mAh/g was achieved when glycine was used and calcined at temperature between 700 to 800oC. Rate discharge capacity of LiNi1/3Co1/3Mn1/3O2 powder is higher when synthesizing using HMTA and glyine compare to the citric acid.