| Summary: | In this study, two compounds of TiNb<sub>2</sub>O<sub>7</sub> and Ti<sub>2</sub>Nb<sub>10</sub>O<sub>29</sub> were successfully synthesized by mechanochemical method and post-annealing as an anode material for lithium-ion batteries. The effect of annealing atmosphere on the morphology, particle size, and electrochemical characteristics of two compounds was investigated. For these purposes, the reactive materials were milled under an argon atmosphere with a certain mole ratio. Subsequently, each sample was subjected to annealing treatment in two different atmospheres, namely argon and oxygen. Phase and morphology identifications were carried out by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) to identify the phases and evaluate the morphology of the synthesized samples. The charging and discharging tests were conducted using a battery-analyzing device to evaluate the electrochemical properties of the fabricated anodes. Annealing in different atmospheres resulted in variable discharge capacities so that the two compounds of TiNb<sub>2</sub>O<sub>7</sub> and Ti<sub>2</sub>Nb<sub>10</sub>O<sub>29</sub> annealed under the argon atmosphere showed a capacity of 60 and 66 mAh/g after 179 cycles, respectively, which had a lower capacity than their counterpart under the oxygen atmosphere. The final capacity of the annealed samples in the oxygen atmosphere is 72 and 74 mAh/g, respectively.
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