Polymerization at the liquid–liquid interface has attracted much attention for synthesizing ultrathin polymer films for molecular sieving. However, it remains a major challenge to conduct this process outside the alkane–water interface since it not only suffers water‐caused side reactions but also is limited to water‐soluble monomers. Here, we report the interfacial polymerization at the alkane/ionic liquid interface (IP@AILI) where the ionic liquid acts as the universal solvent for diversified amines to synthesize task‐specific polyamide nanofilms. We propose that IP@AILI occurs when acyl chloride diffuses from the alkane into the ionic liquid instead of being triggered by the diffusion of amines as in the conventional alkane–water system, which is demonstrated by thermodynamic partitioning and kinetic monitoring. The prepared polyamide nanofilms with precisely adjustable pore sizes display unprecedented permeability and selectivity in various separation processes.

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We report to visualize and monitor the interfacial polymerization by aggregation-induced emission (AIE) effect at the alkane-ionic liquid interface. Quantitative AIE emisison can be used to track real-time monomer consumption,...

Polymerization at the liquid–liquid interface has attracted much attention for synthesizing ultrathin polymer films for molecular sieving. However, it remains a major challenge to conduct this process outside the alkane–water interface since it not only suffers water‐caused side reactions but also is limited to water‐soluble monomers. Here, we report the interfacial polymerization at the alkane/ionic liquid interface (IP@AILI) where the ionic liquid acts as the universal solvent for diversified amines to synthesize task‐specific polyamide nanofilms. We propose that IP@AILI occurs when acyl chloride diffuses from the alkane into the ionic liquid instead of being triggered by the diffusion of amines as in the conventional alkane–water system, which is demonstrated by thermodynamic partitioning and kinetic monitoring. The prepared polyamide nanofilms with precisely adjustable pore sizes display unprecedented permeability and selectivity in various separation processes.

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Interfacial polymerization is a prevalent approach for synthesizing high-performance materials. However, monitoring the polymer growth during this process has posed significant challenges. To overcome this, we have harnessed the aggregationinduced emission effect to enable in situ and real-time observation of the entire interfacial polymerization process. By employing a confocal laser scanning microscope, we have acquired clear images of the polymer and characterized the evolution of its structural heterogeneity, utilizing the environmental sensitivity of the fluorescent AIE moiety. Intriguingly, our study revealed that the polymer density is higher away from the interface, in contrast to the expected homogeneity. The changing ratio of the two monomers in the reaction region accounts for this density gradient. Additionally, we have demonstrated the precise growth kinetics of the polymer under various conditions. Our results provide a novel platform for elucidating the mechanisms and properties of interfacial polymerization.