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The synthesis of bimetallic iron\u2010nickel\u2010benzene\u20101,3,5\u2010tricarboxylate\/nickel foam (FeNi\u2010BTC\/NF)\u00a0MOF\u00a0is reported using a binder\u2010free one\u2010pot method by immersing nickel foam (NF) into a solution of benzene\u20101,3,5\u2010tricarboxylic acid (BTC), N,N\u2010dimethylformamide (DMF), and iron (Fe) salts. FeNi\u2010BTC\/NF exhibits a low overpotential of 276\u00a0mV at 100\u00a0mA\u00a0cm\n                    <jats:sup>\u2212<\/jats:sup>\n                    <jats:sup>2<\/jats:sup>\n                    , a Tafel slope of 94\u00a0mV\u00a0dec\n                    <jats:sup>\u22121<\/jats:sup>\n                    , and stability exceeding 120 h. The Fe\u2010Ni interaction facilitates the formation of a stable gamma\u2010nickel oxyhydroxide (\u03b3\u2010NiOOH) phase, preventing its reversion to nickel hydroxyide (Ni(OH)\u2082), which is crucial for improving oxygen evolution reaction (OER) performance. This phase transition, revealed via in situ Raman spectroelectrochemical analysis, enhances electrocatalytic activity. Additionally, high\u2010valent Fe modulates the electronic structure of Ni, enabling FeNi\u2010BTC\/NF to transform into \u03b3\u2010NiOOH at higher potentials, with Fe and \u03b3\u2010NiOOH synergistically boosting OER\u00a0efficiency. The findings offer insights into Fe\/Ni atom interactions and phase transformations in FeNi\u2010BTC\/NF MOFs for enhanced water splitting.\n                  <\/jats:p>","DOI":"10.1002\/smll.202501142","type":"journal-article","created":{"date-parts":[[2025,4,24]],"date-time":"2025-04-24T05:18:55Z","timestamp":1745471935000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":19,"title":["Real\u2010Time Monitoring of Fe\u2010Induced Stable \u03b3\u2010NiOOH in Binder\u2010Free FeNi MOF Electrocatalysts for Enhanced Oxygen Evolution"],"prefix":"10.1002","volume":"21","author":[{"given":"Kuan\u2010Lun","family":"Chen","sequence":"first","affiliation":[{"name":"Department of Chemistry National Cheng Kung University  No.1, University Road Tainan 701401 Taiwan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yu\u2010Hsuan","family":"Chou","sequence":"additional","affiliation":[{"name":"Department of Chemistry National Cheng Kung University  No.1, University Road Tainan 701401 Taiwan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Tsai\u2010Jen","family":"Lin","sequence":"additional","affiliation":[{"name":"Department of Chemistry National Cheng Kung University  No.1, University Road Tainan 701401 Taiwan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Mu\u2010Jeng","family":"Cheng","sequence":"additional","affiliation":[{"name":"Department of Chemistry National Cheng Kung University  No.1, University Road Tainan 701401 Taiwan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Po\u2010Keng","family":"Hsiao","sequence":"additional","affiliation":[{"name":"Department of Materials Science National University of Tainan  Tainan 700301 Taiwan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ying\u2010Chih","family":"Pu","sequence":"additional","affiliation":[{"name":"Department of Materials Science National University of Tainan  Tainan 700301 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