Ultra‐Efficient Synthesis of Nb4C3Tx MXene via H2O‐Assisted Supercritical Etching for Li‐Ion Battery

Nb4 C3 Tx 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 H2 O-assisted supercritical etching method is proposed for the preparation of Nb4 C3 Tx MXene. Benefiting from the synergetic effect between supercritical CO2 (SPC-CO2 ) and subcritical H2 O （SBC-H2 O）, the etching time for Nb4 C3 Tx MXene can be dramatically shortened to 1 h. The as-synthesized Nb4 C3 Tx MXene possesses uniform accordion-like morphology and large interlayer spacing. When used as anode for Li-ion battery, the Nb4 C3 Tx 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 Nb4 C3 Tx MXene can be ascribed to its high conductivity, fast Li+ diffusion kinetics and good structural stability.