Microwave‐Assisted Efficient Intercalation for Fast Fabrication of High‐Quality and Large‐Size Single‐Layer Ti3C2Tx Nanosheets

Abstract A novel microwave‐assisted intercalation (MAI) strategy is proposed for fast and efficient intercalation of layered MXene to prepare large‐size single‐layer MXene. After LiF‐HCl etching of Ti 3 AlC 2 , the as‐prepared multi‐layer Ti 3 C 2 T x (M‐T) are intercalated with Li 3 AlF 6 as an intercalator and ethylene glycol (EG) as a solvent under microwave irradiation for 5 min. Furthermore, the dispersed high‐quality large‐sized single‐layer Ti 3 C 2 T x (S‐T) nanosheets with a thickness of 1.66 nm and a large lateral size over 20 µm are achieved with a yield of over 60% after a further ultrasonic delamination followed by electrostatic precipitation, acid washing, and calcination. In addition, Pd/S‐T composite catalyst, which is constructed with Pd nanoparticles supported on the as‐prepared S‐T nanosheets, exhibits an excellent performance for rapid and efficient selective hydrogenation of nitroarenes with H 2 under a mild condition. At room temperature, full conversion of nitrobenzene and 100% aniline selectivity are achieved over Pd/S‐T catalyst in 20 min with 0.5 MPa of H 2 pressure. This work provides a novel method for facile, fast, and large‐scale preparation of single‐layer MXene and develops a new approach for constructing efficient nanocatalytic systems.