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The spatial arrangement and positioning of AIEgens and inorganic compounds in AIEgen\u2010functionalized OINPs determine the structures, properties, and functionalities of the self\u2010assembled nanomaterials. In this work, a facile and general emulsion self\u2010assembly tactic for synthesizing well\u2010defined AIEgen\u2010functionalized OINPs is proposed by coassembling alkane chain\u2010functionalized inorganic nanoparticles with hydrophobic organic AIEgens. As a proof of concept, the self\u2010assembly and structural evolution of plasmonic\u2010fluorescent hybrid nanoparticles (PFNPs) from concentric circle to core shell and then to Janus structures is demonstrated by using alkane chain\u2010modified AuNPs and AIEgens as building blocks. The spatial position of AuNPs in the signal nanocomposite is controlled by varying the alkane ligand length and density on the AuNP surface. The mechanism behind the formation of various PFNP nanostructures is also elucidated through experiments and theoretical simulation. The obtained PFNPs with diverse structures exhibit spatially tunable optical and photothermal properties for advanced applications in multicolor and multimode immunolabeling and photothermal sterilization. This work presents an innovative synthetic approach of constructing AIEgen\u2010functionalized OINPs with diverse structures, compositions, and functionalities, thereby championing the progressive development of these OINPs.<\/jats:p>","DOI":"10.1002\/adma.202313381","type":"journal-article","created":{"date-parts":[[2024,4,22]],"date-time":"2024-04-22T08:18:44Z","timestamp":1713773924000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":22,"title":["A Ligand\u2010Directed Spatial Regulation to Structural and Functional Tunability in Aggregation\u2010Induced Emission Luminogen\u2010Functionalized Organic\u2013Inorganic Nanoassemblies"],"prefix":"10.1002","volume":"36","author":[{"given":"Xirui","family":"Chen","sequence":"first","affiliation":[{"name":"State Key Laboratory of Food Science and Resources School of Food Science and Technology Nanchang University  Nanchang 330047 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