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Here, we report a self\u2010intercalation strategy to engineer symmetry breaking in metallic NbS\n                    <jats:sub>2<\/jats:sub>\n                    by exploiting the intrinsic oxidation behavior of niobium. Electrochemical anodization precisely tailors the native oxide layer on Nb foil, which serves as a tunable Nb reservoir during space\u2010confined chemical vapor deposition (SCCVD), enabling spontaneous intercalation of excess Nb atoms into the van der Waals gaps of NbS\n                    <jats:sub>2<\/jats:sub>\n                    . Atomic\u2010resolution characterizations reveal the presence and disordered distribution of intercalated Nb atoms, accompanied by interlayer expansion and superlattice features. Quantitative scanning transmission electron microscopy analysis combined with Energy\u2010dispersive x\u2010ray spectroscopy measurements demonstrates continuously tunable intercalation concentrations in Nb\n                    <jats:sub>1+x<\/jats:sub>\n                    S\n                    <jats:sub>2<\/jats:sub>\n                    . Progressive Nb intercalation systematically enhances inversion symmetry breaking, leading to strengthened second\u2010harmonic generation responses. Robust room\u2010temperature ferroelectricity is achieved while preserving metallic transport, demonstrating the coexistence of ferroelectricity and metallicity in self\u2010intercalated Nb\n                    <jats:sub>1+x<\/jats:sub>\n                    S\n                    <jats:sub>2<\/jats:sub>\n                    . This work establishes an electrochemically oxidized metal precursor\u2013assisted self\u2010intercalation framework for symmetry engineering and multifunctional property modulation in metallic 2D materials.\n                  <\/jats:p>","DOI":"10.1002\/smll.75915","type":"journal-article","created":{"date-parts":[[2026,9,21]],"date-time":"2026-09-21T15:28:41Z","timestamp":1790004521000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Electrochemically Enabled Self\u2010Intercalation for Symmetry Breaking and Metallic Ferroelectricity in Nb\n                    <sub>1+x<\/sub>\n                    S\n                    <sub>2<\/sub>"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0009-0004-1336-3000","authenticated-orcid":false,"given":"Mengchen","family":"Wang","sequence":"first","affiliation":[{"name":"State Key Laboratory of Advanced Materials For Intelligent Sensing Key Laboratory of Organic Integrated Circuit Department of Chemistry School of Science &amp; Institute of Molecular Aggregation Science Ministry of Education &amp; Tianjin Key Laboratory of Molecular Optoelectronic Sciences Tianjin University  Tianjin People's Republic of China"},{"name":"Collaborative Innovation Center of Chemical Science and Engineering (Tianjin)  Tianjin People's Republic of China"},{"name":"Beijing National Laboratory For Molecular Sciences  Beijing People's Republic of China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9151-2727","authenticated-orcid":false,"given":"Qing","family":"Zhang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Advanced Materials For Intelligent Sensing Key Laboratory of Organic Integrated Circuit Department of Chemistry School of Science &amp; Institute of Molecular Aggregation Science Ministry of Education &amp; Tianjin Key Laboratory of Molecular Optoelectronic Sciences Tianjin University  Tianjin People's Republic of China"},{"name":"Collaborative Innovation Center of Chemical Science and Engineering (Tianjin)  Tianjin People's Republic of China"},{"name":"Beijing National Laboratory For Molecular Sciences  Beijing People's Republic of China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yongshuai","family":"Wang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Advanced Materials For Intelligent Sensing Key Laboratory of Organic Integrated Circuit Department of Chemistry School of Science &amp; Institute of Molecular Aggregation Science Ministry of Education &amp; Tianjin Key Laboratory of Molecular Optoelectronic Sciences Tianjin University  Tianjin People's Republic of China"},{"name":"Collaborative Innovation Center of Chemical Science and Engineering (Tianjin)  Tianjin People's Republic of China"},{"name":"Beijing National Laboratory For Molecular Sciences  Beijing People's Republic of 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Science &amp; Institute of Molecular Aggregation Science Ministry of Education &amp; Tianjin Key Laboratory of Molecular Optoelectronic Sciences Tianjin University  Tianjin People's Republic of China"},{"name":"Collaborative Innovation Center of Chemical Science and Engineering (Tianjin)  Tianjin People's Republic of China"},{"name":"Beijing National Laboratory For Molecular Sciences  Beijing People's Republic of China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0005-3688-1852","authenticated-orcid":false,"given":"Lin","family":"Li","sequence":"additional","affiliation":[{"name":"Beijing National Laboratory For Molecular Sciences  Beijing People's Republic of China"},{"name":"College of Chemistry Tianjin Normal University  Tianjin People's Republic of China"},{"name":"Key Laboratory of Advanced Intelligent Protective Equipment Technology (Hebei University of Technology) Ministry of Education  Tianjin People's Republic of 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