Synthesis by reverse micelles was used to produce NiMn2-xFexO4 with nanometric particle sizes for their use as conversion anode materials for lithium ion batteries. The hydroxide precursor was characterized by infrared spectroscopy and the decomposition was followed by thermal analysis. Cation distribution in the spinel structure of pristine samples was evaluated by Mossbauer spectroscopy evidencing that octahedral Fe3+ is substituted by Mn3+ ions in NiMnFeO4. Capacity values of 750 mA h g(-1) were retained for 50 cycles for NiMnFeO4 and NiFe2O4, respectively. A good kinetic response was observed in NiMnFeO4 at 2C. (C) 2010 Elsevier B.V. All rights reserved.