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Here, we report a high\u2010voltage upcycling strategy for spent LiNi\n                    <jats:sub>0.6<\/jats:sub>\n                    Co\n                    <jats:sub>0.2<\/jats:sub>\n                    Mn\n                    <jats:sub>0.2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    (NCM) based on near\u2010surface fluorine (F) regulation of residual rock\u2010salt layers. Molten\u2010salt relithiation recovers Li content and layered bulk framework, whereas subsequent fluorine treatment converts the remaining inert surface reconstruction into a thin F\u2010enriched rock\u2010salt interphase. Rather than impeding Li\n                    <jats:sup>+<\/jats:sup>\n                    transport, this interphase stabilizes the reconstructed surface, reduces oxygen defects, and mitigates electrolyte\u2010induced interfacial degradation. The resulting cathode with F\u2010enriched rock\u2010salt surface (RFNCM) delivers 208.7 mAh g\n                    <jats:sup>\u22121<\/jats:sup>\n                    at 0.1 C within 3.0\u20104.6 V, and retains 80.28% capacity after 400 cycles at 1 C and 25\u00b0C, and 80.93% after 200 cycles at 50\u00b0C. In situ X\u2010ray diffraction and gas\u2010evolution measurements reveal more homogeneous high\u2010voltage structural evolution and suppressed oxygen release, respectively. According to analysis results of XPS, in situ Raman and Density functional theory calculations, these improvements can be attributed to strengthened Ni\u2500O interactions and increased oxygen\u2010vacancy formation energies after fluorine incorporation. This work converts an unavoidable reconstruction product into a protective interphase for high\u2010voltage reuse of spent layered oxide cathodes.\n                  <\/jats:p>","DOI":"10.1002\/adma.75244","type":"journal-article","created":{"date-parts":[[2026,10,5]],"date-time":"2026-10-05T07:35:18Z","timestamp":1791185718000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Engineering Residual Rock\u2010Salt Reconstruction through Near\u2010Surface Fluorine Regulation for Stable 4.6 V Cycling of Regenerated Spent Layered Oxide Cathodes"],"prefix":"10.1002","author":[{"given":"Juan","family":"Wang","sequence":"first","affiliation":[{"name":"State Key Laboratory of Advanced Technology For Materials Synthesis and Processing Wuhan University of Technology  Wuhan Hubei China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhaopei","family":"Liu","sequence":"additional","affiliation":[{"name":"State 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