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In this study, synchrotron\u2010based in situ X\u2010ray photoemission spectroscopy experiments provide insights into the coke deposition on ZSM\u20105 catalysts with different Si\/Al ratios during methanol\u2010to\u2010hydrocarbons conversion, which is an industrially relevant reaction. Surface\u2010sensitive C\u00a01s X\u2010ray photoemission spectroscopy with a probing depth \u22481\u00a0nm demonstrates that the less acidic ZSM\u20105 zeolites exhibit a more pronounced coke accumulation on crystal surfaces and promote the formation of highly condensed, graphite\u2010like structures than the higher acidic ones. Analysis of coking kinetics, lattice deformation, and coke composition using Raman, in situ infrared, and\n                    <jats:italic>operando<\/jats:italic>\n                    UV\u2010vis spectroscopies further supports enhanced surface coking in low\u2010acidity, slowly deactivating catalysts and more prominent micropore coke formation in high\u2010acidity, fast\u2010deactivating catalysts. The results indicate that acid site density governs both the kinetics and the preferential location of coke, shedding light on the fundamental nanoscale processes underlying coke\u2010induced deactivation of zeolite catalysts.\n                  <\/jats:p>","DOI":"10.1002\/anie.7876229","type":"journal-article","created":{"date-parts":[[2026,6,13]],"date-time":"2026-06-13T16:51:45Z","timestamp":1781369505000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["Spatial Evolution of Coke in ZSM\u20105 Catalysts During Methanol\u2010to\u2010Hydrocarbons Conversion Revealed by In Situ X\u2010Ray Photoelectron Spectroscopy"],"prefix":"10.1002","volume":"65","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-4683-6447","authenticated-orcid":false,"given":"Luca","family":"Artiglia","sequence":"first","affiliation":[{"name":"PSI Center for Energy and Environmental Sciences Paul Scherrer Institute  Villigen Switzerland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hannes","family":"Frey","sequence":"additional","affiliation":[{"name":"Institute For Chemical and Bioengineering Department of Chemistry and Applied Biosciences ETH Zurich  Zurich Switzerland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Lo\u00efc","family":"B\u00e9nariac\u2010Doumal","sequence":"additional","affiliation":[{"name":"J. 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