Hydrothermal-Assisted In Situ Intercalation Synthesis of Ti₃C₂T_x MXene in 6 Hours

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 Ti₃C₂T_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.