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Two-dimensional material Ti3C2Tx (T = OH, O, F) attracts great attention due to its excellent performance in energy storage. The functional groups on the surface have tremendous influence on its electrochemical performance. Herein, Ti3C2Tx powders with different surface chemistry were obtained via the etching with sodium hydroxide and hydrofluoric acid and used as anode materials for Li-ion batteries. Alkali etched Ti3C2Tx (mass loading: 1.24 mg cm−2) possesses a larger c-lattice parameter and functional groups without fluorine terminated, showing nearly twice capacities higher than that of Ti3C2Tx etched by hydrofluoric acid (mass loading: 1.06 mg cm−2) at current density of 0.5 A g−1. It is suggested that fluorine-free Ti3C2Tx etched via alkali is more promising for lithium-ion batteries than its fluorine-containing counterpart. Keywords: MXene, Sodium hydroxide, Lithium-ion batteries, Anode