Structurally Tunable Patterned Fluorescent Polymer Arrays for Room‐Temperature Volatile Organic Compounds Sensing

ABSTRACT Volatile organic compounds (VOCs) pose significant threats to both the environment and human health due to their toxicity. Therefore, there is an urgent need to develop efficient VOC sensing technologies operating under ambient conditions. Conventional fluorescent materials often suffer from aggregation‐caused quenching in the solid state, while aggregation‐induced emission (AIE) materials are typically limited by crystallization‐induced performance degradation. In this study, a novel fluorescent polymer sensor material by covalently grafting the prototypical AIE molecule tetraphenylethylene (TPE) as a side group onto the poly(ether sulfone) (PES) main chain is reported. This molecular design effectively suppresses TPE crystallization and significantly enhances the solid‐state photoluminescence quantum yield (PLQY = 55.47%). Furthermore, a capillary bridge‐mediated assembly strategy is employed to fabricate patterned fluorescent microwire arrays to improve the gas sensing performance. Based on this strategy, a sensor array composed of five different fluorescent polymers is constructed. When combined with principal component analysis (PCA), the array successfully achieves efficient classification and identification of eight representative VOC, including structurally similar analytes such as methanol‐ethanol and benzene‐toluene. The fluorescent polymer sensor arrays and patterning strategy developed in this work offer a promising platform for applications in environmental monitoring, biomedical diagnostics, and industrial process control.