The Li4Ti5O12/LiMn2O 4 cell holds promise for safer operation of lithium-ion batteries. In this study, Li4+xTi5[Ai]O12 anode powder was prepared by chemical lithiation of Li1-yTi5O12 in the presence of an excess of butylithium (LiC4H9) in hexane solution, and Li1-yMn2O4 cathode powder was prepared by chemical delithiation of LiMn2O4 spinel using NO2BF4 oxidizer in an acetonitrile medium. Thermal gravimetric analysis showed that the Li1-yMn2O4 releases oxygen starting at 200°C with an overall oxygen loss of 6 wt% at 500°C, whereas the Li4+xTi5O12 gains oxygen starting at 200°C with an overall oxygen gain of 4 wt% at 500°C. The reactivity of Li4+xTi5O12 and Li 1-yMn2O4 powders in the presence of electrolyte was also investigated by differential scanning calorimetry between room temperature and 375°C. The results suggest that the Li4+xTi 5O12 anode is thermally more stable compared with the conventional lithiated graphite anode.