Fischer‐Tropsch synthesis (FTS) is an effective route to produce olefins, gasoline, diesel, and oxygenates from syngas (CO + H2). However, it still remains a challenge for regulating the product distribution of FTS. Here, a series of Co/C sub‐microreactors with precise designed nanoarchitectures are synthesized for selective syngas conversion. Through a combination of surface protection‐assisted etching and following carbonization process, Co/C sub‐microreactors with solid cube, double‐shelled hollow box, and hollow box architectures, namely, Co/C‐Cube, Co/C‐DBox, Co/C‐Box can be obtained. In FTS, comparing with solid Co/C‐Cube, double‐shelled hollow structured Co/C‐DBox is inclined to grow long‐chain hydrocarbon products, whereas hollow structured Co/C‐Box avails the formation of short‐chain hydrocarbon chemicals. Therefore, shape selective catalysis and controlled product distribution of FTS are realized by tuning the architectures of Co/C sub‐microreactors. It is expected to fundamentally unravel the heterogeneous catalytic process via upfront designing and precisely regulating the architectures of micro/nanoreactors.
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