Harnessing Microexplosions for Rapid Pd–N Single‐Atom Catalyst Formation

The scalable and energy‐efficient synthesis of single‐atom catalysts (SACs) is critically challenged by the trade‐off between high energy consumption and metal aggregation in conventional thermal activation. Herein, a microexplosive synthesis reactor (MER) is proposed that leverages spatially confined acetylacetonate deflagration within micron‐channels (800 µm) to achieve ultrafast atomic dispersion (<20 ms) of palladium. This design decouples metal anchoring thermodynamics from aggregation kinetics by generating localized ultrahigh temperatures (>1500 K, heating rate 10 5 K s −1 ) while maintaining the bulk reactor temperature below 200 °C, thereby suppressing atomic migration and agglomeration. Through synchrotron characterization and multiscale simulations, a three‐step mechanism encompassing precursor sublimation‐induced spatial confinement, non‐equilibrium combustion waves, and N‐coordination stabilization is identified. The resulting Pd─N 4 SACs demonstrate exceptional activity and stability (>200 h) in the hydrogenation of biomass‐derived 5‐hydroxymethylfurfural (HMF), outperforming nanoparticle benchmarks by 2–3 orders of magnitude due to optimized electronic structure and maximized active site accessibility. Remarkably, the MER process reduces energy consumption by 98% compared to pyrolysis methods and enables scalable production (kilogram‐level) with batch‐to‐batch consistency. This strategy is universally applicable to 8 metals (e.g., Pd, Pt, Co), establishing a fundamental and practical platform for sustainable SAC manufacturing with minimized carbon footprint.