Ultrafast Synthesis of Single‐Atom Catalysts for Electrocatalytic Applications

Abstract A recent development in catalytic research, single‐atom catalysts (SACs) are one of the most significant categories of catalytic materials. During preparation, individual atoms migrate and agglomerate due to the high surface free energy. The rapid thermal shock strategy addresses this challenge by employing instantaneous high‐temperature pulses to synthesize SACs, while minimizing heating duration to prevent metal aggregation and substrate degradation, thereby preserving atomic‐level dispersion. The resultant SACs exhibit exceptional catalytic activity, remarkable selectivity, and long‐term stability, which have attracted extensive attention in electrocatalysis. In this paper, cutting‐edge ultrafast synthesis techniques such as Joule heating, microwave radiation, pulsed discharge, and arc discharge are comprehensively analyzed. Their ability is emphasized to achieve uniform dispersion of separated metal atoms and optimize the catalytic activity for electrocatalytic applications. A systematic summary of SACs synthesized by these rapid methods is provided, with particular emphasis on their implementation in carbon dioxide reduction reaction (CO 2 RR), oxygen evolution reaction (OER), hydrogen evolution reaction (HER), and oxygen reduction reaction (ORR) systems. The review provides an in‐depth discussion on the rapid synthesis strategy for development trend, remaining challenges, and the application prospects in electrocatalysis.