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To overcome this limitation, we introduce an innovative electrochemical\u2010chemical sequential strategy that replaces OER with methanol oxidation (MOR). Our decoupled process comprises cathodic hydrogen evolution reaction (HER) paired with anodic Ni(OH)\n                    <jats:sub>2<\/jats:sub>\n                    oxidation to NiOOH in 1\u00a0M KOH electrolyte, followed by spontaneous NiOOH reduction\n                    <jats:italic>via<\/jats:italic>\n                    MOR, selectively generating formic acid (HCOOH) with 95% formic acid Faraday efficiency in neutral electrolyte. Crucially, we developed a scalable bottom\u2010up method to electrochemically prepare the active NiOOH catalyst directly from Ni(OH)\n                    <jats:sub>2<\/jats:sub>\n                    particles. This catalyst achieved a HCOOH yield of 48.25\u00a0mmol per kg\u00a0catalyst. Collectively, this strategy establishes an efficient and recyclable pathway for alkaline hydrogen production integrated with high\u2010value formic acid synthesis in neutral media.\n                  <\/jats:p>","DOI":"10.1002\/smll.202511050","type":"journal-article","created":{"date-parts":[[2025,12,22]],"date-time":"2025-12-22T12:13:06Z","timestamp":1766405586000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Spontaneous Neutral\u2010pH Organic Oxidation on Trivalent Nickel Enables Spatially Separated H2 and Organic Products"],"prefix":"10.1002","volume":"22","author":[{"given":"Bochuan","family":"Chen","sequence":"first","affiliation":[{"name":"Collaborative Innovation Center of Advanced Microstructures National Laboratory of Solid State Microstructures College of Engineering and Applied Sciences Nanjing University  Hankou Road Nanjing Jiangsu P. R. 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