Hydrothermal‐Assisted In Situ Intercalation Synthesis of Ti ₃ C ₂ T _x MXene in 6 Hours

ABSTRACT Despite the rapid expansion of MXene research, scalable and time‐efficient synthesis routes that simultaneously deliver high‐quality, high‐yield products remain limited. Here, we present a facile, high‐yield method for the synthesis, in situ intercalation, and delamination of Ti 3 C 2 T x MXene. In situ intercalation during hydrothermal‐assisted etching facilitates aluminum removal and promotes the delamination of MXene sheets. This approach reduces synthesis time to 6 h at 90°C, compared to up to 48 h in conventional protocols. The methodology employs a mild etchant system of hydrochloric acid and lithium fluoride, with lithium chloride as an in situ intercalant within a closed hydrothermal autoclave. Hydrothermal conditions enhance etchant reactivity and kinetics, while Li + ions weaken van der Waals forces, enabling exfoliation into two‐dimensional MXenes. Comprehensive characterization confirms the method's high efficacy, yielding 74.2% ± 3.7% delaminated nanosheets with a monolayer thickness of 1–1.5 nm. X‐ray diffraction confirms successful Al etching and effective delamination. X‐ray photoelectron and energy‐dispersive spectroscopies show surface terminations consisting of –Cl, –F, and –O. The resulting MXene exhibits an electrical conductivity of 7 500 S cm − 1 . This methodology offers a scalable, single‐step route to MXene synthesis, marking a significant advance and opening avenues for commercial applications of these materials.