Fe‐Based Bimetallic Catalysts for Activating PMS to Degrade Antibiotics: Synergistic Effects, Pathway Regulation, and Environmental Applications

ABSTRACT Fe‐based bimetallic catalysts have emerged as promising materials for peroxymonosulfate (PMS) activation toward antibiotic degradation in water, offering enhanced electron transfer, improved active site regeneration, and tunable reaction pathways over monometallic counterparts. This review systematically summarizes recent advances in their design and application, with a focus on synergistic mechanisms and the precise regulation of radical and non‐radical pathways. We classify these catalysts into four synergistic types—endogenous electron donors, coupled redox cycles, electronic structure modifiers, and anionic coordination—and outline mainstream synthesis strategies including coprecipitation, solvothermal, pyrolysis, impregnation, and electrochemical deposition. The core of this review elucidates how bimetallic centers act as regulatory hubs to steer PMS activation toward radical routes (SO 4 • − and •OH) and non‐radical routes ( 1 O 2 , high‐valent metal‐oxo species, and direct electron transfer). Using fluoroquinolones, sulfonamides, tetracyclines, and β‐lactams as model antibiotics, we further demonstrate how catalyst design governs specific degradation pathways and influences the evolution of environmental toxicity. Finally, we address key practical challenges including complex water matrix interference and catalyst deactivation, and outline future directions toward atomic‐level design, in situ characterization, and engineering integration for sustainable water purification.