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Charge transfer mediators have emerged as critical interfacial components bridging photoelectrodes, cocatalysts, and conductive substrates, enabling directional carrier transport, suppressed recombination, and enhanced catalytic activity. However, their roles, design principles, and mechanisms in PEC systems remain insufficiently understood. This review systematically defines charge transfer mediators in PEC water splitting, clarifies their multifunctional roles in charge transfer, charge storage, and interfacial protection, and summarizes representative material platforms, including carbon\u2010based materials, MXenes, metal oxides, molecular materials, nonmetal nitrides, and other emerging mediators. Particular emphasis is placed on the relationship between mediator structures, interfacial configurations, electronic properties, and PEC performance. Advanced characterization techniques and theoretical approaches for elucidating charge transfer pathways and reaction mechanisms are also discussed to establish structure\u2010property\u2010performance correlations. Finally, key challenges and future perspectives are highlighted, positioning charge transfer mediators as an emerging paradigm for constructing efficient, stable, and practical PEC systems.<\/jats:p>","DOI":"10.1002\/adma.75313","type":"journal-article","created":{"date-parts":[[2026,10,9]],"date-time":"2026-10-09T07:43:50Z","timestamp":1791531830000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Charge Transfer Mediators in Photoelectrochemical Water Splitting: From Interfacial Regulation to Rational Design"],"prefix":"10.1002","author":[{"given":"Yurou","family":"Song","sequence":"first","affiliation":[{"name":"State Key Laboratory of Fine Chemicals Frontiers Science Center for Smart Materials Oriented Chemical Engineering School of Chemical Engineering Dalian University of Technology  Dalian P. R. 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