Preparation of 2D Polyaniline/MoO3−x Superlattice Nanosheets via Intercalation‐Induced Morphological Transformation for Efficient Chemodynamic Therapy

Abstract Organic intercalation of layered nanomaterials is an attractive strategy to fabricate organic/inorganic superlattices for a wide range of promising applications. However, the synthesis of 2D organic/inorganic superlattice nanosheets remains a big challenge. Herein, the preparation of 2D polyaniline/MoO 3− x (PANI/MoO 3− x ) superlattice nanosheets via intercalation‐induced morphological transformation from MoO 3 nanobelts, as efficient Fenton‐like reagents for chemodynamic therapy (CDT), is reported. Micrometer‐long MoO 3 nanobelts are co‐intercalated with Na + /H 2 O followed by the guest exchange with aniline monomer for in situ polymerization to obtain PANI/MoO 3− x nanosheets. Intriguingly, the PANI intercalation can induce the morphological transformation from long MoO 3 nanobelts to 2D PANI/MoO 3− x nanosheets along with the partial reduction of Mo 6+ to Mo 5+ , and generation of rich oxygen vacancies. More importantly, thanks to the PANI intercalation‐induced activation, the PANI/MoO 3− x nanosheets exhibit excellent Fenton‐like catalytic activity for generation of hydroxyl radical (·OH) by decomposing H 2 O 2 compared with the MoO 3 nanobelts. It is speculated that the good conductivity of PANI can facilitate electron transport during the Fenton‐like reaction, thereby enhancing the efficiency of CDT. Thus, the polyvinylpyrrolidone‐modified PANI/MoO 3− x nanosheets can function as Fenton‐like reagents for highly efficient CDT to kill cancer cells and eradicate tumors.