Abstract: | Microreactors for nanoparticle (NP) synthesis offer advantages over batch reactions in terms of scale‐up and integration with online analyses. Herein, two microreactors (i.e., a duo‐microreactor) are integrated to achieve sequential reactions for the synthesis of bimetallic NPs with architectural control. The generality of the duo‐microreactor is shown with the synthesis of branched Pd‐Pt NPs and core@shell Pd@Au NPs, both achieved by synthesizing Pd nanocubes in the first part of the duo‐microreactor and then using those nanocubes downstream as seeds for Pt or Au deposition. Control of the dimensions of these NPs is further demonstrated and achieved by tailoring metal precursor concentrations inline. This microreactor methodology is anticipated to be applicable to other bimetallic NP systems. |