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

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 Ti3AlC2, the as‐prepared multi‐layer Ti3C2Tx (M‐T) are intercalated with Li3AlF6 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 Ti3C2Tx (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 H2 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 H2 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. A novel microwave‐assisted intercalation (MAI) strategy is proposed for efficient intercalation of layered MXene to prepare large‐sized single‐layer MXene. After intercalation of multi‐layer Ti3C2Tx (M‐T) with Li3AlF6 as an intercalator and ethylene glycol as a solvent under microwave irradiation for 5 min, high‐quality large‐sized single‐layer Ti3C2Tx nanosheets (S‐T) are achieved finally by a series simple treatments.