Atomically dispersed OFeN active sites boost the selective decomposition of acidic <scp>H₂O₂</scp> into <scp>O₂</scp>

Abstract H 2 O 2 , 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 HO 2 − . 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 H 2 O 2 into O 2 . In situ FTIR confirmed atomically dispersed iron significantly enhanced the end‐adsorption of H 2 O 2 and in situ formed FeOOH, achieving a 100% decomposition rate and 98% O 2 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 H 2 O 2 decomposition reaction and offers a valuable reference in further developing systems for the decomposition of H 2 O 2 into O 2 .