Abstract

Mixed‐metal nanoparticles present a challenging task for synthesis with high precision and reproducibility due to the complex interplay of compositional and reaction condition factors. The present study demonstrates a highly precise and automated flow chemistry technique for synthesizing AgAu alloy nanoboxes with tailored optical properties. The synthesis process involves a proportional–integral (PI) feedback control mechanism that enables accurate regulation of reaction parameters, such as the flow rate, to achieve the target AgAu nanoboxes having a desired UV–vis absorbance wavelength. The PI control algorithm is built on the first‐order plus dead‐time model, which correlates the flow rate of the precursors with the maximum absorbance peaks of the resultant nanoalloy products. Based on the difference between the real‐time measured UV–vis absorbance wavelength and the target wavelength, the flow rate of the precursor (i.e., reagent concentration) is tuned via an iterative process until the real‐time absorbance wavelength of the AgAu alloy nanoboxes is matched with the target setpoint. The implementation of a PI feedback control mechanism in a flow chemistry system can offer a highly versatile and universal strategy for generating on‐demand complex nanomaterials with significantly enhanced consistency and reliability by mitigating concentration variations and minimizing the need for human intervention.

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