Spinel lithium manganese oxide LiMn2O4 and its substituted forms LiCo0.16Mn1.84O4 were prepared by annealing of the mixed precursors which were synthesized by low heating solid state coordination method using lithium acetate, cobalt acetate, manganese acetate and oxalic acid as starting materials. The structures and morphologies of the LiMn2O4 and LiCo0.16Mn1.84O4 were investigated as a function of annealing temperature. The results show that all samples in different annealing temperature have the same spinel structure. The higher the annealing temperature, the more complete the crystal structure, and the larger the particle size. In addition, the LiMn2O4 and LiCo0.16Mn1.84O4 were used as cathode active materials for lithium secondary batteries and their charge/discharge properties have been investigated. As a result, it could be seen that low heating solid state coordination method is an effective method to prepare lithium manganese oxide (LiM2O4) and its substituted forms. (c) 2006 Springer Science + Business Media, Inc.