Ultra-Efficient Synthesis of Nb₄C₃T_x MXene via H₂O-Assisted Supercritical Etching for Li-Ion Battery

Nb4C3Tx MXene has shown extraordinary promise for various applications owing to its unique physicochemical properties. However, it can only be synthesized by the traditional HF-based etching method, which uses large amounts of hazardous HF and requires a long etching time (> 96 h), thus limiting its practical application. Here, an ultra-efficient and environmental-friendly H2O-assisted supercritical etching method is proposed for the preparation of Nb4C3Tx MXene. Benefiting from the synergetic effect between supercritical CO2 (SPC-CO2) and subcritical H2O (SBC-H2O), the etching time for Nb4C3Tx MXene can be dramatically shortened to 1 h. The as-synthesized Nb4C3Tx MXene possesses uniform accordion-like morphology and large interlayer spacing. When used as anode for Li-ion battery, the Nb4C3Tx MXene delivers a high reversible specific capacity of 430 mAh g(-1) at 0.1 A g(-1), which is among the highest values achieved in pure-MXene-based anodes. The superior lithium storage performance of the Nb4C3Tx MXene can be ascribed to its high conductivity, fast Li+ diffusion kinetics and good structural stability.