LAUSR

H2O2, a vital industrial material, poses a huge explosion risk due to its residual presence. Under acidic conditions, its stable peroxy‐bond hinders efficient decomposition into H+ or HO2−. In this study, we prepared a FeNC single‐atom catalyst via molecular self‐assembly and argon pyrolysis, regulating reactive oxygen species to convert H2O2 into O2. In situ FTIR confirmed atomically dispersed iron significantly enhanced the end‐adsorption of H2O2 and in situ formed FeOOH, achieving a 100% decomposition rate and 98% O2 selectivity, while minimizing the formation of harmful •OH radicals. Furthermore, we constructed a flow‐through amplification reactor that maintained a conversion rate of 100% even at a high space velocity of 75 h−1. This work provides a novel approach for H2O2 decomposition reaction and offers a valuable reference in further developing systems for the decomposition of H2O2 into O2.