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This study investigates the influence of varying degrees of deuteration on the photophysical properties of TPE across different aggregation states. Through the synthesis of partially and fully deuterated TPE derivatives (TPE\u20105d, TPE\u201010d, and TPE\u201020d), combined with steady\u2010state fluorescence spectroscopy, time\u2010resolved fluorescence measurements, transient absorption spectroscopy, and density functional theory (DFT) calculations, we elucidate the dual role of deuteration in modulating nonradiative decay pathways. In loosely packed nanoaggregates, increased deuteration enhances photoluminescence quantum yields (PLQY) and extends fluorescence lifetimes by reducing internal conversion rates. Conversely, in tightly packed crystalline states, deuteration leads to decreased PLQY and shortened lifetimes, attributable to the Duschinsky rotation effect (DRE), which enhances inter\u2010mode coupling and internal conversion. Additionally, deuteration significantly prolongs the operational lifetime of blue organic light\u2010emitting diode (OLED) devices, doubling the device lifespan in TPE\u201020d compared to TPE. This work underscores the necessity of evaluating structure\u2013property relationships at the aggregate level, rather than solely at the molecular level, to fully comprehend and optimize AIE phenomena. These findings highlight the potential of isotope engineering in designing durable and efficient AIE luminogens for applications in optoelectronics and bioimaging.<\/jats:p>","DOI":"10.1002\/anie.202511678","type":"journal-article","created":{"date-parts":[[2025,7,8]],"date-time":"2025-07-08T10:50:43Z","timestamp":1751971843000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":18,"title":["Isotope Engineering of Tetraphenylethylene: Aggregate\u2010Dependent Enhancement of Luminescence Efficiency"],"prefix":"10.1002","volume":"64","author":[{"given":"Siwei","family":"Zhang","sequence":"first","affiliation":[{"name":"Department of Chemistry Hong Kong Branch of Chinese National Engineering Research Center for Tissue Restoration and Reconstruction Division of Life Science and State Key Laboratory of Molecular Neuroscience The Hong Kong University of Science and Technology  Kowloon Hong Kong 999077 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Fulong","family":"Ma","sequence":"additional","affiliation":[{"name":"Department of Chemistry Hong Kong Branch of Chinese National Engineering Research Center for Tissue Restoration and Reconstruction Division of Life Science and State Key Laboratory of Molecular Neuroscience The Hong Kong University of Science and Technology  Kowloon Hong Kong 999077 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jinhui","family":"Jiang","sequence":"additional","affiliation":[{"name":"Department of Chemistry Hong Kong Branch of Chinese National Engineering Research Center for Tissue Restoration and Reconstruction Division of Life Science and State Key Laboratory of Molecular Neuroscience The Hong Kong University of Science and Technology  Kowloon Hong Kong 999077 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Bo","family":"Wu","sequence":"additional","affiliation":[{"name":"School of Environmental and Chemical Engineering Wuyi University  Jiangmen Guangdong 529020 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Junyi","family":"Gong","sequence":"additional","affiliation":[{"name":"Faculty of Chemistry Shenzhen MSU\u2010BIT University  Longgang District Shenzhen Guangdong 518172 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Guang","family":"Xu","sequence":"additional","affiliation":[{"name":"Guangdong Basic Research Center of Excellence for Aggregate Science School of Science and Engineering, Shenzhen Institute of Aggregate Science and Technology The Chinese University of Hong Kong (CUHK\u2010Shenzhen)  Shenzhen Guangdong 518172 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chao","family":"Li","sequence":"additional","affiliation":[{"name":"Department of Chemistry The Hong Kong University of Science and Technology  Clear Water Bay Kowloon Hong Kong 999077 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Tengteng","family":"Chen","sequence":"additional","affiliation":[{"name":"Department of Chemistry The Hong Kong University of Science and Technology  Clear Water Bay Kowloon Hong Kong 999077 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ryan T. 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