The differential thermal analysis (DTA) curves were measured at different heating rates in flow-ing air for studying the synthesis of the spinel LiMn2O4 with Li2CO3 and MnO2. The reaction be-gan at about 503K, and finishedatabout 873K. The apparentactivation energy of Kissinger method(1-δ)1.67Coats-Redfern integral method was used to analyze the DTA curves of the samples at different heating rates, and the calculated apparent activation energy and frequency factor were diffraction (XRD) and scanning electron microscope (SEM) results shown that the synthesized LiMn2O4 possesses pure phase, regular shape and normal particle distribution.