Spinel LiMn2O4 is one of the promising cathode materials used in commercial Li-ion batteries. In this study, Ni was partially substituted in order to give the material LiMn1.8Ni0.2O4, which was successfully synthesized using a self-propagating combustion (SPC) method. Results from Simultaneous Thermogravimetric Analysis (STA) show the small mass loss about 4.6%. The precursor then was calcined at temperature of 800 °C for 24 h, 48 h and 72 h. X-Ray Diffraction (XRD) confirms that the final products are pure and single phase with no impurities present. The morphology and crystallite size of pure samples are examined using Field Emission Scanning Electron Microscope (FESEM). The result shows that all the materials consist of crystalline particles with smooth surface and polyhedral shaped materials.