Ultrafast Synthesis of MXenes in Minutes via Low‐Temperature Molten Salt Etching

Abstract Developing green and efficient preparation strategies is a persistent pursuit in the field of 2D transition metal nitrides and/or carbides (MXenes). Traditional etching methods, such as HF‐based or high‐temperature Lewis‐acid‐molten‐salt etching route, require harsher etching conditions and exhibit lower preparation efficiency with limited scalability, severely constraining their commercial production and practical application. Here, an ultrafast low‐temperature molten salt (LTMS) etching method is presented for the large‐scale synthesis of diverse MXenes within minutes by employing NH 4 HF 2 as the etchant. The increased thermal motion and improved diffusion of molten NH 4 HF 2 molecules significantly expedite the etching process of MAX phases, thus achieving the preparation of Ti 3 C 2 T x MXene in just 5 minutes. The universality of the LTMS method renders it a valuable approach for the rapid synthesis of various MXenes, including V 4 C 3 T x , Nb 4 C 3 T x , Mo 2 TiC 2 T x , and Mo 2 CT x . The LTMS method is easy to scale up and can yield more than 100 g Ti 3 C 2 T x in a single reaction. The obtained LTMS‐MXene exhibits excellent electrochemical performance for supercapacitors, evidently proving the effectiveness of the LTMS method. This work provides an ultrafast, universal, and scalable LTMS etching method for the large‐scale commercial production of MXenes.