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However, the complexity and dynamic behavior of SEIs have long hindered direct, chemically resolved visualization of fluoride\u2010rich domains, which is essential for decoding inorganic interphase dynamics and guiding rational battery formation. Here, tetrakis(4\u2010carboxyphenyl)ethylene (H\n                    <jats:sub>4<\/jats:sub>\n                    TCPE) is used as a fluorescent probe for convenient, semi\u2010quantitative visualization of alkali\u2010metal fluoride\u2010rich interphases, enabled by a crystalline\u2010lattice\u2010specific matrix coordination\u2010induced emission effect mechanism. Under this mechanism, crystalline NaF exclusively activates H\n                    <jats:sub>4<\/jats:sub>\n                    TCPE fluorescence through strong hydrogen\u2010bonding and coordination interactions that lock the probe's rotation, whereas the probe remains non\u2010emissive on other SEI components because these phases fail to impose sufficient steric confinement. This chemical contrast enables ex situ and\n                    <jats:italic>operando<\/jats:italic>\n                    imaging and reveals an unexpected formation\u2013breakdown\u2013regeneration lifecycle of the NaF\u2010rich framework during cycling. This probe\u2010enabled semi\u2010quantitative tracking further identifies 1.0\u00a0mA cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    as the optimal formation current density, yielding the most continuous NaF\u2010rich framework, minimizing capacity loss, and ensuring stable cycling. Ultimately, this accessible, chemically selective optical strategy opens new avenues for probing fragile battery interphases and tailoring electrochemical protocols for high\u2010performance energy storage.\n                  <\/jats:p>","DOI":"10.1002\/anie.3926577","type":"journal-article","created":{"date-parts":[[2026,9,4]],"date-time":"2026-09-04T08:36:09Z","timestamp":1788510969000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["A Chemically Selective Fluorescent Probe Visualizes the Non\u2010Monotonic Evolution of the NaF\u2010Rich Interphase in Sodium\u2010Metal Batteries"],"prefix":"10.1002","volume":"65","author":[{"given":"Xiaolin","family":"Guo","sequence":"first","affiliation":[{"name":"State Key Laboratory of Space Power\u2010Sources School of Chemistry and Chemical Engineering Harbin Institute of Technology  Harbin China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zijun","family":"Wang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Space Power\u2010Sources School of Chemistry and Chemical Engineering Harbin Institute of Technology  Harbin China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yining","family":"Lv","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Space Power\u2010Sources School of Chemistry and Chemical Engineering Harbin Institute of Technology  Harbin China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Min","family":"Niu","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Space Power\u2010Sources School of Chemistry and Chemical Engineering Harbin Institute of Technology  Harbin China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jiale","family":"Wan","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Space Power\u2010Sources School of Chemistry and Chemical Engineering Harbin Institute of Technology  Harbin China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jin","family":"Ren","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Space Power\u2010Sources School of Chemistry and Chemical Engineering Harbin Institute of Technology  Harbin China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7203-5788","authenticated-orcid":false,"given":"Zhijun","family":"Chen","sequence":"additional","affiliation":[{"name":"Key Laboratory of Bio\u2010Based Material Science and Technology of Ministry of Education Northeast Forestry University  Harbin China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4034-804X","authenticated-orcid":false,"given":"Liwei","family":"Dong","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Space Power\u2010Sources School of Chemistry and Chemical Engineering Harbin Institute of Technology  Harbin China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2383-3999","authenticated-orcid":false,"given":"Zuotao","family":"Lei","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Space Power\u2010Sources School of Chemistry and Chemical Engineering Harbin Institute of Technology  Harbin 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