In the present work, Li MO2 (Li CoO2, Li NiO2, LiMnO2, or LiFeO2) metal oxides of the transition lithium layers were modified to serve as cathode materials for lithium-ion batteries, usually prepared by combustion reaction for better electrochemical efficiency. Li: Co: Ni: Fe: O2 (LCNFO) powder was first prepared in a weight percentages mixture of 1:0.5:0.45:0.5:1 with citric acid as fuel, and de-ionized water DIW as a binding material, and then mixed with nitrate of lithium ion (Li+) and a Fe+3 to obtain a regular blend. With some addition of citric acid and de-ionized water, a powder was obtained, which then heated up to 900 °C for 8 h. Several investigations were carried out to examine the powder properties in order to adopt it for thermal and thermo-gravimetric analysis applications. The microstructure of the powder was investigated using X-ray diffraction (XRD) analysis. A well-selected annealing temperature can produce a pure single-phase LCNFO material with good electrochemical behavior. The particle size of the LCNFO material had been approximately measured from the XRD outcome, utilizing Scherer formula. The electrochemical properties of the LCNFO layers were studied, and surface topography of LCNFO powder was examined utilizing Atomic force microscopy AFM. The results show an enhancement in the properties of the LCNFO cathode material prepared by a combustion reaction in the air, which has a larger storage capacity, and thus, it considers a promising alternative to other LiCoO2, LiNiO2, and LiMnO2 cathode materials. This preparation method is simple and effective to produce such nanostructures layers with high quality and cost-effectiveness for portable batteries application. [ABSTRACT FROM AUTHOR]