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Recently, intercalation of native metal atoms into the van der Waals gaps of 2D layered transition metal dichalcogenides (TMDs) has been developed to form 2D non\u2010layered magnetic TMDs, while only succeeded in limited systems (e.g., Cr<jats:sub>2<\/jats:sub>S<jats:sub>3<\/jats:sub>, Cr<jats:sub>5<\/jats:sub>Te<jats:sub>8<\/jats:sub>). Herein, composition\u2010controllable syntheses of 2D non\u2010layered iron selenide nanosheets (25% Fe\u2010intercalated triclinic Fe<jats:sub>5<\/jats:sub>Se<jats:sub>8<\/jats:sub> and 50% Fe\u2010intercalated monoclinic Fe<jats:sub>3<\/jats:sub>Se<jats:sub>4<\/jats:sub>) are firstly reported, via a robust chemical vapor deposition strategy. Specifically, the 2D Fe<jats:sub>5<\/jats:sub>Se<jats:sub>8<\/jats:sub> exhibits intrinsic room\u2010temperature ferromagnetic property, which is explained by the change of electron spin states from layered 1T'\u2010FeSe<jats:sub>2<\/jats:sub> to non\u2010layered Fe\u2010intercalated Fe<jats:sub>5<\/jats:sub>Se<jats:sub>8<\/jats:sub> based on density functional theory calculations. In contrast, the ultrathin Fe<jats:sub>3<\/jats:sub>Se<jats:sub>4<\/jats:sub> presents novel metallic features comparable with that of metallic TMDs. This work hereby sheds light on the composition\u2010controllable synthesis and fundamental property exploration of 2D self\u2010intercalation induced novel TMDs compounds, by propelling their application explorations in nanoelectronics and spintronics\u2010related fields.<\/jats:p>","DOI":"10.1002\/adma.202207276","type":"journal-article","created":{"date-parts":[[2022,10,20]],"date-time":"2022-10-20T05:44:08Z","timestamp":1666244648000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":54,"title":["Composition\u2010Controllable Syntheses and Property Modulations from 2D Ferromagnetic Fe<sub>5<\/sub>Se<sub>8<\/sub> to Metallic Fe<sub>3<\/sub>Se<sub>4<\/sub> Nanosheets"],"prefix":"10.1002","volume":"35","author":[{"given":"Yahuan","family":"Huan","sequence":"first","affiliation":[{"name":"School of Materials Science and Engineering Peking University  Beijing 100871 P. R. 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