We present an innovative methodology for the synthesis of MXene membranes through a dual-stage process involving etching and subsequent thermal self-crosslinking. A molar ratio of 1 (Al):9 (F) using HCl/LiF was employed to convert raw TiAlC (MAX phase) into MXene within 48 h at 40 °C. This procedure predominantly yielded monolayers distinguished by diameters exceeding 500 nm, elevated crystallinity and a high overall yield.
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