| Summary: | Herein we report that novel two-dimensional (2D) Ti<sub>3</sub>Si<sub>0.75</sub>Al<sub>0.25</sub>C<sub>2</sub> (TSAC) nanosheets, obtained by sonically exfoliating their bulk counterpart in alcohol, performs promising electrochemical activities in a reversible lithiation and delithiation procedure. The as-exfoliated 2D TSAC nanosheets show significantly enhanced lithium-ion uptake capability in comparison with their bulk counterpart, with a high capacity of ≈350 mAh g<sup>−1</sup> at 200 mA g<sup>−1</sup>, high cycling stability and excellent rate performance (150 mAh g<sup>−1</sup> after 200 cycles at 8000 mA g<sup>−1</sup>). The enhanced electrochemical performance of TSAC nanosheets is mainly a result of their fast Li-ion transport, large surface area and small charge transfer resistance. The discovery in this work highlights the uniqueness of a family of 2D layered MAX materials, such as Ti<sub>3</sub>GeC<sub>2</sub>, Ti<sub>3</sub>SnC<sub>2</sub> and Ti<sub>2</sub>SC, which will likely be the promising choices as anode materials for lithium-ion batteries (LIBs).
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