Despite their remarkable mechanical, optical, and electrical properties, inorganic particles and dynamic polymer assemblies encounter difficulties in their compatibility with regards to structural order and complexity. Here, covalent organic frameworks (COFs) constructed through reversible coupling reactions were exploited as dynamic porous polymers to prepare inorganic nanocrystal-polymer assemblies. Under an in situ growth process, carbon quantum dots (CDs) were gradually prepared in the COF cavity, with a narrow size distribution (2 ± 0.5 nm). The well-established assemblies achieve effective energy transfer from the inorganic to the organic part (efficiency > 80%), thus rendering a ∼130% increase in quantum yield compared with the pristine COF network. Notably, the hybrid material realizes a simple, selective, and sensitive diagnostic tool for urine copper, surpassing the detection limit of COF solid by 150 times. Beyond the scientific and fundamental interests, such hybrid assemblies are attractive from technological perspectives as well, for example, in energy storage, electronics, catalysis, and optics.
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