Three kinds of processes, high temperature solid state reaction, precipitation and sol-gel technique were used to synthsize spinel phase LiMn2O4. XRD, DTA-TG results show that phase-pure spinel LiMn2O4 could be synthesized under the lowest calcined temperature by the sol-gel technique compared to the precipitation method and solid state reaction. BET, SEM and electrochemical measurements results demonstrate that the features of the powders affect directly the electrochemical capacities; large specific area and small homogeneous grain size are of advantage for the lithium ion insertion and extraction in the charge and discharge process.