In this work, spinel LiMn2O4 powder was synthesized from LiOH center dot H2O and MnOx by mechanical alloying (MA) for various MA times. The stoichiometry and crystal structure of the spinel were examined and their relation to the electrochemical behavior of the spine' was investigated. In this study, we find that, as a result of MA using stainless steel jar and balls, Fe and Cr contents increased and O content decreased with increasing MA time. The results from electrochemical study show that the stoichiometry of the spinel is closely related to the decreasing of initial discharge capacity and cyclic performance of the spinel. (C) 2013 Elsevier B.V. All rights reserved.