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Herein, we developed a therapeutic nanoplatform utilizing bismuth (Bi)\u2010doping techniques to control the release of copper (Cu) ions, enabling synergistic ion interference therapy, chemodynamic therapy (CDT) and photothermal therapy (PTT) for tumor treatment. Based on the instability of Bi\u2010based compounds in the tumor microenvironment (TME), Bi ions are preferentially released from Bi\u2010doped CuS nanosheets (Bi\u2010CuS NSs), exposing more Cu vacancies and facilitating Cu ion release compared to CuS NSs. More importantly, upon cellular internalization, the released copper ions induce ionic homeostasis disruption, leading to cuproptosis in liver cancer cells. Simultaneously, the Cu vacancies generated by ion release enhance the peroxidase\u2010like activity to produce more reactive oxygen species and improve the photothermal conversion efficiency to induce localized hyperthermia, synergistically amplifying tumor cell destruction. Consequently, Bi\u2010CuS NSs exhibit excellent potential for synergistic metal ion interference and photothermal\/chemodynamic therapy, enabling the multimodal treatment of hepatocellular carcinoma. This study presents a Bi\u2010mediated strategy for regulating Cu\u2010ion release and catalytic activity in metal\u2010based cancer nanomedicines.<\/jats:p>","DOI":"10.1002\/smll.76305","type":"journal-article","created":{"date-parts":[[2026,10,16]],"date-time":"2026-10-16T07:01:55Z","timestamp":1792134115000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Bismuth\u2010Triggered Copper Release From CuS Nanosheets Enables Synergistic Ion\u2010Interference and Chemodynamic\/Photothermal Therapy"],"prefix":"10.1002","author":[{"given":"Ziwei","family":"Su","sequence":"first","affiliation":[{"name":"School of Chemistry and Chemical Engineering Anhui University  Hefei Anhui People's Republic of China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hongkang","family":"Xu","sequence":"additional","affiliation":[{"name":"School of Chemistry and Chemical Engineering Anhui University  Hefei Anhui People's 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