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NiFe\u2010based electrocatalysts have garnered significant attention due to their high OER activity; however, the need for a rapid and efficient electrode fabrication method and a clear understanding of the role of Fe in enhancing OER activity remains unresolved. Herein, a highly active NiFe\u2010based OER electrocatalyst self\u2010supported on carbon fiber paper (CFP) is developed using a versatile and rapid thermal shock method, requiring only 30\u2009s of heat treatment. The as\u2010prepared Fe<jats:sub>1<\/jats:sub>Ni<jats:sub>1<\/jats:sub>\/CFP shows a current density of 493\u2009mA\/cm<jats:sup>2<\/jats:sup> at 1.7\u2009V vs reversible hydrogen electrode (RHE) and a low overpotential of 247\u2009mV at 10\u2009mA\/cm<jats:sup>2<\/jats:sup>, with excellent long\u2010term durability in alkaline\u00a0conditions. In\u2009situ Raman spectroscopy, pH\u2010dependance activity test, and electronic structure calculations reveal that Fe not only promotes the oxidation of adjacent Ni but also accelerates the deprotonation of adsorbed \u2013OH groups and stabilizes oxo\u2010intermediates, thus, displaying both direct and indirect effects and enhancing the overall OER performance. This article provides a foundation for developing cost\u2010effective electrocatalysts for hydrogen production and other sustainable energy applications while enhancing the understanding of the role of Fe in NiO catalysts.<\/jats:p>","DOI":"10.1002\/cssc.202500281","type":"journal-article","created":{"date-parts":[[2025,5,29]],"date-time":"2025-05-29T08:40:02Z","timestamp":1748508002000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":5,"title":["Experimental and Theoretical Insights into the Role of Iron in the Rapidly Fabricated Ni\/Fe Electrodes for the Oxygen Evolution Reaction"],"prefix":"10.1002","volume":"18","author":[{"given":"Yue","family":"Wang","sequence":"first","affiliation":[{"name":"Department of Heterogeneous Catalysis Max\u2010Planck\u2010Institut f\u00fcr Kohlenforschung  Kaiser\u2010Wilhelm\u2010Platz 1 D\u201045470 M\u00fclheim an der Ruhr Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Gustavo T.","family":"Feliciano","sequence":"additional","affiliation":[{"name":"Department of Molecular Theory and Spectroscopy Max\u2010Planck\u2010Institut f\u00fcr Kohlenforschung  Kaiser\u2010Wilhelm\u2010Platz 1 D\u201045470 M\u00fclheim an der Ruhr Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ashwani","family":"Kumar","sequence":"additional","affiliation":[{"name":"Department of Heterogeneous Catalysis Max\u2010Planck\u2010Institut f\u00fcr Kohlenforschung  Kaiser\u2010Wilhelm\u2010Platz 1 D\u201045470 M\u00fclheim an der Ruhr Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6012-3027","authenticated-orcid":false,"given":"Alexander A.","family":"Auer","sequence":"additional","affiliation":[{"name":"Department of Molecular Theory and Spectroscopy Max\u2010Planck\u2010Institut f\u00fcr Kohlenforschung  Kaiser\u2010Wilhelm\u2010Platz 1 D\u201045470 M\u00fclheim an der Ruhr Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8552-7028","authenticated-orcid":false,"given":"Harun","family":"T\u00fcys\u00fcz","sequence":"additional","affiliation":[{"name":"Department of Heterogeneous Catalysis Max\u2010Planck\u2010Institut f\u00fcr Kohlenforschung  Kaiser\u2010Wilhelm\u2010Platz 1 D\u201045470 M\u00fclheim an der Ruhr Germany"},{"name":"Catalysis and Energy Materials Group IMDEA Materials Institute  Calle Eric Kandel 2 28906 Getafe Madrid Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2025,6,24]]},"reference":[{"key":"e_1_2_7_2_1","first-page":"558","volume":"57","author":"T\u00fcys\u00fcz H.","year":"2024","journal-title":"Acc. 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