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Here we combine time\u2010resolved in situ x\u2010ray absorption spectroscopy (TR\u2010XAS) at both the Co and Ni K\u2010edges with density\u2010functional tight\u2010binding molecular dynamics (DFTB\u2010MD) simulations to investigate the laser\u2010driven transformation of NiCo\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>4<\/jats:sub>\n                    into a metallic NiCo alloy in ethanol. Considering the results from TR\u2010XAS and DFTB\u2010MD simulations, the reduction is initiated by hydrogen atom transfer from the\n                    <jats:italic>\u03b1<\/jats:italic>\n                    \u2010C\u2500H bond of ethanol to a surface lattice oxygen, generating an\n                    <jats:italic>\u03b1<\/jats:italic>\n                    \u2010hydroxyethyl radical; the oxygen is subsequently released as water and the alcohol is dehydrogenated to acetaldehyde. Even though the initial hydrogen transfer is facile, the release of lattice oxygen is entropy\u2010driven and becomes accessible only at temperatures of order 10\n                    <jats:sup>3<\/jats:sup>\n                    K, so that the extent of reduction is governed by the transient local temperature and hence by the laser fluence: complete reduction occurs at fluences \u2265100 mJ\/pulse, yielding a metallic surface that achieves a Faradaic efficiency of 86.6% for NH\n                    <jats:sub>3<\/jats:sub>\n                    formation in electrochemical nitrate reduction. These findings establish a mechanistic framework for the rational control of PLI\u2010synthesized metal\u2010based electrocatalysts.\n                  <\/jats:p>","DOI":"10.1002\/anie.8536600","type":"journal-article","created":{"date-parts":[[2026,9,16]],"date-time":"2026-09-16T07:38:29Z","timestamp":1789544309000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Direct Observation of Radical\u2010Mediated Oxide\u2010to\u2010Alloy Transformation in Solution Under Pulsed Laser Irradiation"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0009-0002-0163-6329","authenticated-orcid":false,"given":"Woo Hyeok","family":"Kim","sequence":"first","affiliation":[{"name":"Department of Applied Chemistry Kyung Hee University  Yongin Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Sieon","family":"Jung","sequence":"additional","affiliation":[{"name":"Department of Chemistry (BK21 FOUR) Research Institute of Advanced Chemistry Gyeongsang National University  Jinju Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ahreum","family":"Min","sequence":"additional","affiliation":[{"name":"Department of Chemistry (BK21 FOUR) Research Institute of Advanced Chemistry Gyeongsang National University  Jinju Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9268-171X","authenticated-orcid":false,"given":"Raja Arumugam","family":"Senthil","sequence":"additional","affiliation":[{"name":"Department of Chemistry (BK21 FOUR) Research Institute of Advanced Chemistry Gyeongsang National University  Jinju Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Juhyeon","family":"Park","sequence":"additional","affiliation":[{"name":"Department of Chemistry (BK21 FOUR) Research Institute of Advanced Chemistry Gyeongsang National University  Jinju Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0000-8462-8353","authenticated-orcid":false,"given":"Wonil","family":"Seo","sequence":"additional","affiliation":[{"name":"Department of Chemistry The Catholic University of Korea  Bucheon Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0006-5711-342X","authenticated-orcid":false,"given":"Seung Yeon","family":"Choi","sequence":"additional","affiliation":[{"name":"Department of Applied Chemistry Kyung Hee University  Yongin Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0001-1127-6892","authenticated-orcid":false,"given":"Junu","family":"Bae","sequence":"additional","affiliation":[{"name":"Department of Applied Chemistry Kyung Hee University  Yongin Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Cheolhee","family":"Yang","sequence":"additional","affiliation":[{"name":"Department of Applied Chemistry Kyung Hee University  Yongin Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8885-1552","authenticated-orcid":false,"given":"In\u2010hui","family":"Hwang","sequence":"additional","affiliation":[{"name":"Pohang Accelerator Laboratory POSTECH  Pohang Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7783-0200","authenticated-orcid":false,"given":"Joonghan","family":"Kim","sequence":"additional","affiliation":[{"name":"Department of Chemistry The Catholic University of Korea  Bucheon Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6370-0907","authenticated-orcid":false,"given":"Tae Wu","family":"Kim","sequence":"additional","affiliation":[{"name":"Department of Applied Chemistry Kyung Hee University  Yongin Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5729-5418","authenticated-orcid":false,"given":"Myong Yong","family":"Choi","sequence":"additional","affiliation":[{"name":"Department of Chemistry (BK21 FOUR) Research Institute of Advanced Chemistry Gyeongsang National University  Jinju Republic of Korea"},{"name":"Core\u2010Facility Center for Photochemistry &amp; 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