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However, the Cu\u2212Zn based catalyst system employed in this process is very dynamic, especially in the presence of the products methanol and water. Deactivation needs to be prevented, but its origin and mechanism are hardly investigated at high conversion where product condensation is possible. Here, we report on the structural dynamics of a Cu\/ZnO\/ZrO<jats:sub>2<\/jats:sub> catalyst at 90\u2005bar and 40\u2009% CO<jats:sub>2<\/jats:sub> conversion (at equilibrium conditions), investigated in a dedicated metal\u2010based spectroscopic cell specially fabricated using additive manufacturing. This particular reactor configuration aims to mimic the high CO<jats:sub>2<\/jats:sub> conversion part of the catalyst bed and can induce product condensation, which is monitored by <jats:italic>operando<\/jats:italic> X\u2010ray absorption spectroscopy. While Cu remained mostly stable throughout the experiment, Zn underwent strong restructuring. The chosen reaction conditions, including the use of CO<jats:sub>2<\/jats:sub> as carbon source and <jats:italic>in situ<\/jats:italic> product condensation, were selected to provide insights under industrial conditions. This work is highlighting the importance of spectroscopic investigations at high conversion levels, offering insights into chemical transformations during deactivation, extending the concept of spatially resolved studies, and thus providing guidance for the design of more stable catalysts.<\/jats:p>","DOI":"10.1002\/anie.202423281","type":"journal-article","created":{"date-parts":[[2025,1,27]],"date-time":"2025-01-27T09:22:07Z","timestamp":1737969727000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":22,"title":["Monitoring the Fate of Zn in the Cu\/ZnO\/ZrO<sub>2<\/sub> Catalyst During CO<sub>2<\/sub>\u2010to\u2010Methanol Synthesis at High Conversions by <i>Operando<\/i> Spectroscopy"],"prefix":"10.1002","volume":"64","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-0740-1603","authenticated-orcid":false,"given":"Mariam L.","family":"Schulte","sequence":"first","affiliation":[{"name":"Institute for Chemical Technology and 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