[ ] powders for lithium ion batteries were synthesized from two separate raw material pairs of LiOH/MnO and . The powders prepared at 780 and and their difference of electrochemical properties were investigated. Both powders calcined at 780 and were composed of a single-phase spinel structure but those treated at showed a lower intensity ratio of to , a slightly larger lattice parameter, and an increased discharge capacity by 10% under voltage range. The XPS study on the oxidation states of manganese repealed that powders made from LiOH/MnO had less ion and gave better battery performances than those from .