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Despite extensive research, the role of alkali metals remains debated. In this study, Na\u2010modified ZrO\n                    <jats:sub>2<\/jats:sub>\n                    \u2010supported Cu catalysts are synthesized using different methods for the reverse water\u2010gas shift (RWGS) reaction to elucidate the role of Na\n                    <jats:sup>+<\/jats:sup>\n                    . Catalytic results show that activity strongly depends on the preparation method, with the one\u2010pot approach yielding three times higher activity than wet impregnation. The one\u2010pot method significantly enhances Cu\n                    <jats:sup>0<\/jats:sup>\n                    dispersion, preventing the loss of Cu sites due to agglomeration or coverage by Alkali. Although the prevailing view suggests that alkali metals favor the associative mechanism for CO formation. Combined in\u2010situ studies demonstrate that the redox mechanism is the main pathway for CO formation. In\u2010situ EPR and in\u2010situ CO\u2010DRIFTS results indicate that Na\u207a plays a critical role in facilitating the reoxidation of reduced Cu\n                    <jats:sup>0<\/jats:sup>\n                    sites by CO\n                    <jats:sub>2<\/jats:sub>\n                    dissociation during the reaction, eventually leading to CO formation. The results show that a high density of accessible Cu\n                    <jats:sup>0<\/jats:sup>\n                    sites with enhanced redox activity is essential for achieving superior catalytic performance. These findings are expected to advance the rational engineering of alkali\u2010modified surfaces, with enriched active sites and finely tuned redox behavior.\n                  <\/jats:p>","DOI":"10.1002\/advs.202506401","type":"journal-article","created":{"date-parts":[[2025,10,14]],"date-time":"2025-10-14T02:42:04Z","timestamp":1760409724000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":6,"title":["Unveiling Alkali\u2010Induced Redox Modulation: In\u2010Situ Spectroscopic Insights from RWGS on Alkali\u2010Modified ZrO\n                    <sub>2<\/sub>\n                    \u2010Supported Cu Catalysts"],"prefix":"10.1002","volume":"13","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-9161-1223","authenticated-orcid":false,"given":"Abdallah I. 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