| Summary: | Herein, the spinel-layered cathode material Li<sub>1.33</sub>MnTiO<sub>4+z</sub> (0.8LiMnTiO<sub>4</sub>•0.2Li<sub>2</sub>Mn<sub>0.5</sub>Ti<sub>0.5</sub>O<sub>3</sub>) is investigated for the purpose of developing a high-capacity, low-cost, and environmentally friendly cathode for Li-ion batteries. Sol-gel synthesis is conducted and the relationships between synthesis temperature, structure, and electrochemical performance of the cathodes are studied. The effects of size and purity on the capacities of these cathodes are discussed. The samples fired at 500 and 600 °C contain an impurity phase of TiO<sub>2</sub>, thus delivering capacities of 208 and 210 mAh g<sup>−1</sup> at C/10, respectively. The sample fired at 700 °C without the impurity phase of TiO<sub>2</sub> shows a high capacity of 222 mAh g<sup>−1</sup> at C/10 and capacity retention of 90.5% after 100 cycles at 1C.
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