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Here, we present a facile, high\u2010yield method for the synthesis, in situ intercalation, and delamination of Ti\n                    <jats:sub>3<\/jats:sub>\n                    C\n                    <jats:sub>2<\/jats:sub>\n                    T\n                    <jats:sub>x<\/jats:sub>\n                    MXene. In situ intercalation during hydrothermal\u2010assisted etching facilitates aluminum removal and promotes the delamination of MXene sheets. This approach reduces synthesis time to 6\u00a0h at 90\u00b0C, compared to up to 48\u00a0h 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\n                    <jats:sup>+<\/jats:sup>\n                    ions weaken van der Waals forces, enabling exfoliation into two\u2010dimensional MXenes. Comprehensive characterization confirms the method's high efficacy, yielding 74.2% \u00b1 3.7% delaminated nanosheets with a monolayer thickness of 1\u20131.5\u00a0nm. X\u2010ray diffraction confirms successful Al etching and effective delamination. X\u2010ray photoelectron and energy\u2010dispersive spectroscopies show surface terminations consisting of \u2013Cl, \u2013F, and \u2013O. The resulting MXene exhibits an electrical conductivity of 7 500 S cm\n                    <jats:sup>\u2212<\/jats:sup>\n                    <jats:sup>1<\/jats:sup>\n                    . This methodology offers a scalable, single\u2010step route to MXene synthesis, marking a significant advance and opening avenues for commercial applications of these materials.\n                  <\/jats:p>","DOI":"10.1002\/smtd.70871","type":"journal-article","created":{"date-parts":[[2026,7,28]],"date-time":"2026-07-28T09:31:11Z","timestamp":1785231071000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Hydrothermal\u2010Assisted In Situ Intercalation Synthesis of Ti\n                    <sub>3<\/sub>\n                    C\n                    <sub>2<\/sub>\n                    T\n                    <sub>x<\/sub>\n                    MXene in 6 Hours"],"prefix":"10.1002","volume":"10","author":[{"given":"Muhammad Imran","family":"Rameel","sequence":"first","affiliation":[{"name":"Department of Mechanical Engineering Kaunas University of Technology  Kaunas 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