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Although prior studies have correlated electrochemical behavior with pre\u2010formed structural motifs, the pathways by which these motifs emerge during synthesis remain unclear. Here, we track the structural evolution of layered sodium manganese oxide during solid\u2010state synthesis using time\u2010resolved X\u2010ray diffraction coupled with a real\u2010time micro\u2010furnace. We show that oxygen uptake and Mn oxidation occur predominantly during cooling, triggering oxygen\u2010mediated reconstruction into a framework enriched with manganese vacancies (\u25a1Mn) and stacking faults. By kinetically regulating the cooling process, we reveal that slow cooling promotes a spatially homogeneous stacking\u2010fault\u2010rich architecture that suppresses in\u2010plane Mn migration and mitigates irreversible O\n                    <jats:sub>2<\/jats:sub>\n                    release. High\u2010resolution microscopy directly visualizes the development of stacking faults, while density functional theory shows that these defects substantially increase the barrier for Mn migration. Together, these findings identify cooling\u2010driven oxygen\u2010mediated reconstruction as a previously underappreciated synthetic lever for defect engineering and establish a general design principle for stabilizing oxygen redox in layered sodium cathodes.\n                  <\/jats:p>","DOI":"10.1002\/advs.78064","type":"journal-article","created":{"date-parts":[[2026,10,7]],"date-time":"2026-10-07T06:04:38Z","timestamp":1791353078000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Regulating Oxygen\u2010Mediated Reconstruction during Cooling: A New Design Principle for High\u2010Capacity Sodium Manganese Oxide Cathodes"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0009-0000-8809-7780","authenticated-orcid":false,"given":"Seungmin","family":"Lee","sequence":"first","affiliation":[{"name":"Chemistry Division Brookhaven National Laboratory  Upton New York 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