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However, the synthesis of 2D organic\/inorganic superlattice nanosheets remains a big challenge. Herein, the preparation of 2D polyaniline\/MoO<jats:sub>3\u2212<\/jats:sub><jats:italic><jats:sub>x<\/jats:sub><\/jats:italic> (PANI\/MoO<jats:sub>3\u2212<\/jats:sub><jats:italic><jats:sub>x<\/jats:sub><\/jats:italic>) superlattice nanosheets via intercalation\u2010induced morphological transformation from MoO<jats:sub>3<\/jats:sub>\u00a0nanobelts, as efficient Fenton\u2010like reagents for chemodynamic therapy (CDT), is reported. Micrometer\u2010long MoO<jats:sub>3<\/jats:sub>\u00a0nanobelts are co\u2010intercalated with Na<jats:sup>+<\/jats:sup>\/H<jats:sub>2<\/jats:sub>O followed by the guest exchange with aniline monomer for in\u00a0situ polymerization to obtain PANI\/MoO<jats:sub>3\u2212<\/jats:sub><jats:italic><jats:sub>x<\/jats:sub><\/jats:italic> nanosheets. Intriguingly, the PANI intercalation can induce the morphological transformation from long MoO<jats:sub>3<\/jats:sub>\u00a0nanobelts to 2D PANI\/MoO<jats:sub>3\u2212<\/jats:sub><jats:italic><jats:sub>x<\/jats:sub><\/jats:italic> nanosheets along with the partial reduction of Mo<jats:sup>6+<\/jats:sup> to Mo<jats:sup>5+<\/jats:sup>, and generation of rich oxygen vacancies. More importantly, thanks to the PANI intercalation\u2010induced activation, the PANI\/MoO<jats:sub>3\u2212<\/jats:sub><jats:italic><jats:sub>x<\/jats:sub><\/jats:italic> nanosheets exhibit excellent Fenton\u2010like catalytic activity for generation of hydroxyl radical (\u00b7OH) by decomposing H<jats:sub>2<\/jats:sub>O<jats:sub>2<\/jats:sub>\u00a0compared with the MoO<jats:sub>3<\/jats:sub>\u00a0nanobelts. It is speculated that the good conductivity of PANI can facilitate electron transport during the Fenton\u2010like reaction, thereby enhancing the efficiency of CDT. Thus, the polyvinylpyrrolidone\u2010modified PANI\/MoO<jats:sub>3\u2212<\/jats:sub><jats:italic><jats:sub>x<\/jats:sub><\/jats:italic> nanosheets can function as Fenton\u2010like reagents for highly efficient CDT to kill cancer cells and eradicate tumors.<\/jats:p>","DOI":"10.1002\/adhm.202202911","type":"journal-article","created":{"date-parts":[[2023,1,5]],"date-time":"2023-01-05T18:44:23Z","timestamp":1672944263000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":48,"title":["Preparation of 2D Polyaniline\/MoO<sub>3\u2212<\/sub><i><sub>x<\/sub><\/i> Superlattice Nanosheets via Intercalation\u2010Induced Morphological Transformation for Efficient Chemodynamic Therapy"],"prefix":"10.1002","volume":"12","author":[{"given":"Tingting","family":"Hu","sequence":"first","affiliation":[{"name":"State Key Laboratory of Chemical Resource Engineering Beijing Advanced Innovation Center for Soft Matter Science and Engineering Beijing University of Chemical Technology  Beijing 100029 P. 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