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In this work, NiO nanoparticles were synthesized using an ethanolic extract of Sargassum sp. as a biogenic mediator, and the influence of calcination temperature (300, 500, and 700 \u00b0C) on their physicochemical and electrocatalytic properties was systematically investigated. X-ray diffraction confirmed the formation of NiO cubic phase and showed an increase in crystallite size with increasing calcination temperature. FTIR, Raman, XPS, and EPR analyses revealed temperature-dependent changes in surface composition and defect chemistry, including mixed Ni2+\/Ni3+ species and oxygen-vacancy-related centers. EPR signals at g \u2248 2.0005\u20132.0006 are assigned to F+-type centers. Electrochemical measurements in 1.0 mol L\u20131 KOH showed that NiO-300 exhibited the highest OER activity, requiring an overpotential of 352 mV to reach 10 mA cm\u20132, compared with 368 and 356 mV for NiO-500 and NiO-700, respectively. Although NiO-300 displayed the lowest estimated electrochemically active surface area among the samples, it consistently showed the lowest charge-transfer resistance, indicating more favorable interfacial kinetics. Its enhanced performance is therefore associated with the combined effects of defect-related surface species, oxygen-vacancy-related centers, and improved charge-transfer dynamics. Chronopotentiometric measurements at 10 and 100 mA cm\u20132 further demonstrated the excellent electrochemical stability of NiO-300, while post-OER XRD and Raman analyses confirmed the preservation of its crystalline framework after prolonged operation.<\/jats:p>","DOI":"10.1021\/acsomega.6c05066","type":"journal-article","created":{"date-parts":[[2026,9,8]],"date-time":"2026-09-08T13:08:25Z","timestamp":1788872905000},"page":"52943-52958","source":"Crossref","is-referenced-by-count":0,"title":["Sustainable Synthesis\nof Defect-Rich NiO Nanoparticles\nfrom Seaweed for Enhanced Oxygen Evolution"],"prefix":"10.1021","volume":"11","author":[{"given":"Adiel Soares","family":"Ferreira","sequence":"first","affiliation":[{"name":"Universidade Federal Rural de Pernambuco (UFRPE) , , , ,","place":["Recife, PE, Brazil, 52171-900"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Johnnys da Silva","family":"Horte\u0302ncio","sequence":"additional","affiliation":[{"name":"Universidade Federal da Parai\u0301ba (UFPB) , , , ,","place":["Joa\u0303o Pessoa, PB, Brazil, 58.051-900"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7930-6234","authenticated-orcid":true,"given":"Andre\u0301 Luiz","family":"Menezes de Oliveira","sequence":"additional","affiliation":[{"name":"Universidade Federal da Parai\u0301ba (UFPB) , , , ,","place":["Joa\u0303o Pessoa, PB, Brazil, 58051-900"]},{"name":"Universidade Federal do Rio Grande do Norte , , , ,","place":["Natal, RN, Brazil, 59078-970"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2591-2770","authenticated-orcid":true,"given":"Rodolfo B. da","family":"Silva","sequence":"additional","affiliation":[{"name":"Universidade Federal da Parai\u0301ba (UFPB) , , , ,","place":["Joa\u0303o Pessoa, PB, Brazil, 58.051-900"]},{"name":"Universidade do Estado do Rio Grande do Norte (UERN) , , , ,","place":["Mossoro\u0301, RN, Brazil, 59610-090"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8296-5217","authenticated-orcid":true,"given":"Nykon","family":"Craveiro","sequence":"additional","affiliation":[{"name":"Universidade Federal de Pernambuco , , Av. Prof. Moraes Re\u0302go, 1235 , , ,","place":["Recife, PE, Brazil, 50670-901"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jose\u0301 Souto","family":"Rosa-Filho","sequence":"additional","affiliation":[{"name":"Universidade Federal de Pernambuco , , Av. Prof. Moraes Re\u0302go, 1235 , , ,","place":["Recife, PE, Brazil, 50670-901"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6095-512X","authenticated-orcid":true,"given":"Fausthon Fred","family":"da Silva","sequence":"additional","affiliation":[{"name":"Universidade Federal Rural de Pernambuco (UFRPE) , , , ,","place":["Recife, PE, Brazil, 52171-900"]},{"name":"Universidade Federal da Parai\u0301ba (UFPB) , , , ,","place":["Joa\u0303o Pessoa, PB, Brazil, 58.051-900"]},{"name":"Universidade Federal da Parai\u0301ba (UFPB) , , , ,","place":["Joa\u0303o Pessoa, PB, Brazil, 58051-900"]},{"name":"Universidade Federal de Pernambuco (UFPE) , , , ,","place":["Recife, PE, Brazil, 50670-901"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,8,24]]},"reference":[{"key":"2026090809082207400_cit1","doi-asserted-by":"publisher","DOI":"10.1016\/j.scitotenv.2020.142222","article-title":"The Impact\nof Natural Resources, Energy Consumption,\nand Population Growth on Environmental Quality: Fresh Evidence from\nthe United States of America","volume":"754","author":"Khan","year":"2021","journal-title":"Sci. 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