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Herein, we report the synthesis of hierarchical nickel\u2013cobalt\u2013copper borate ((Ni\n 1\/3<\/jats:sub>\n Co\n 1\/3<\/jats:sub>\n Cu\n 1\/3<\/jats:sub>\n )\n 3<\/jats:sub>\n B\n 2<\/jats:sub>\n O\n 6<\/jats:sub>\n ) nanosheets via a carbon dioxide (CO\n 2<\/jats:sub>\n ) laser irradiation method and investigate their eNO\n 3<\/jats:sub>\n RR performance in a 1\u00a0\n m<\/jats:sc>\n KOH electrolyte containing 0.1\u00a0\n m<\/jats:sc>\n KNO\n 3<\/jats:sub>\n . Initially, (Ni\n 1\/3<\/jats:sub>\n Co\n 1\/3<\/jats:sub>\n Cu\n 1\/3<\/jats:sub>\n )\n 3<\/jats:sub>\n B\n 2<\/jats:sub>\n O\n 6<\/jats:sub>\n is synthesized via CO\n 2<\/jats:sub>\n laser irradiation within a short processing period of 1\u00a0min, where this method enables a rapid material synthesis compared with conventional methods, such as hydrothermal, solvothermal, and wet\u2010chemical approaches. The (Ni\n 1\/3<\/jats:sub>\n Co\n 1\/3<\/jats:sub>\n Cu\n 1\/3<\/jats:sub>\n )\n 3<\/jats:sub>\n B\n 2<\/jats:sub>\n O\n 6<\/jats:sub>\n catalyst achieves a maximum NH\n 3<\/jats:sub>\n yield rate of 4.1 mg\u00a0h\n \u22121<\/jats:sup>\n cm\n \u22122<\/jats:sup>\n and a Faradaic efficiency of 90.69% at \u22120.3\u00a0V vs. the reversible hydrogen electrode. In\u2010depth analysis of eNO\n 3<\/jats:sub>\n RR kinetics using in situ Raman, ex situ X\u2010ray diffraction, and ex situ Fourier transform infrared spectroscopy reveals information on the reaction intermediates and reaction pathways involved. Extended density functional theory calculations further corroborate the experimental findings related to reaction intermediates and pathways during the eNO\n 3<\/jats:sub>\n RR. A zinc (Zn)\u2013NO\n 3<\/jats:sub>\n \u2212<\/jats:sup>\n battery assembled using (Ni\n 1\/3<\/jats:sub>\n Co\n 1\/3<\/jats:sub>\n Cu\n 1\/3<\/jats:sub>\n )\n 3<\/jats:sub>\n B\n 2<\/jats:sub>\n O\n 6<\/jats:sub>\n as the cathode and a Zn plate as the anode exhibits an open\u2010circuit voltage of 1.44\u00a0V at 12\u00a0mA\u00a0cm\n \u22122<\/jats:sup>\n .\n <\/jats:p>","DOI":"10.1002\/smll.76312","type":"journal-article","created":{"date-parts":[[2026,10,21]],"date-time":"2026-10-21T05:40:12Z","timestamp":1792561212000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["CO\n 2<\/sub>\n Laser\u2010Synthesized NiCoCu Borate Enables Efficient Nitrate\u2010to\u2010Ammonia Electrosynthesis and Durable Zinc\u2013Nitrate Batteries"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-0955-1576","authenticated-orcid":false,"given":"Jayesh","family":"Cherusseri","sequence":"first","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\/0000-0003-1687-862X","authenticated-orcid":false,"given":"Nivarthi Rajiv","family":"Bharadwaj","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\/0009-0000-8273-6182","authenticated-orcid":false,"given":"Pimjai","family":"Pimbaotham","sequence":"additional","affiliation":[{"name":"Department of Chemistry and Center of Excellence for Innovation in Chemistry Ubon Ratchathani University Ubon Ratchathani Thailand"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chae Eun","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\/0000-0001-5943-6878","authenticated-orcid":false,"given":"Siriporn","family":"Jungsuttiwong","sequence":"additional","affiliation":[{"name":"Department of Chemistry and Center of Excellence for Innovation in Chemistry Ubon Ratchathani University Ubon Ratchathani Thailand"},{"name":"Department of Chemical Engineering Faculty of Engineering Chulalongkorn University Bangkok Thailand"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5729-5418","authenticated-orcid":false,"given":"Myong 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