Rapid Melt‐Quenching Enables General Synthesis of High‐Loading Single‐Atom Catalysts with Bicontinuous Nanoporous Structure

Abstract Single‐atom catalysts have attracted extensive attention due to their unique atomic structures and extraordinary activities in catalyzing chemical reactions. However, the lack of general and efficient approaches for producing high‐density single atoms on suitably tailored supporting matrixes hinders their industrial applications. Here, a rapid melt‐quenching strategy with high throughput to synthesize single atoms with high metal‐atom loadings of up to 9.7 wt% or 2.6 at% on nanoporous metal compounds is reported, representing several‐fold improvements compared to benchmarks in the literature. Mechanism characterizations reveal that the high‐temperature melting provides the essential liquid environment and activation energy to achieve the atomization of metals, while the following rapid‐quenching pins the isolated metal atoms and stabilizes the coordination environment. In comparison with carbon‐supported single‐atom catalysts, various collaboration combinations of single atoms and nanoporous metal compounds can be synthesized using the strategy, thus achieving efficient hydrazine oxidation‐assisted H₂ production. This synthesis protocol is highly compatible with automatic operation, which provides a feasible and general route to design and manufacture specific single‐atom catalysts with tunable atomic metal components and supporting matrixes, thus promoting the deployment of single‐atom catalysts for various energy technology applications.