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Here, we show that surface oxidation fundamentally alters this behavior in Cu\u2013Au nanoalloys by suppressing conventional surface segregation and driving twin\u2010boundary (TB)\u2010mediated chemical separation within the particle interior. Combining in situ electron microscopy, ambient\u2010pressure X\u2010ray photoelectron spectroscopy, and density functional theory, we reveal that oxidation redirects Au transport from the surface to internal TBs through uphill diffusion from Au\u2010poor to Au\u2010rich regions, producing alternating Au\u2010rich and Cu\u2010rich lamellae with local Au enrichment of up to \u223c50 at.%. This behavior is driven by the negative Cu\u2013Au mixing enthalpy, which favors heteroatomic bonding, while the CuO\n                    <jats:italic>\n                      <jats:sub>x<\/jats:sub>\n                    <\/jats:italic>\n                    overlayer inhibits Au surface segregation that would otherwise dominate. Consequently, surface oxidation acts as a chemical pump, redirecting atomic flux into the particle interior, where defect\u2010mediated segregation lowers the free energy by maximizing Cu\u2013Au bonding. These findings demonstrate how surface chemistry, alloy thermodynamics, and lattice defects collectively govern mass transport and internal chemical patterning, providing atomistic insight into the structural evolution and stability of nanoalloys under reactive environments.\n                  <\/jats:p>","DOI":"10.1002\/smll.75003","type":"journal-article","created":{"date-parts":[[2026,8,4]],"date-time":"2026-08-04T10:57:39Z","timestamp":1785841059000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Oxidation\u2010Induced Internal Chemical Patterning in Copper\u2013Gold Nanoalloys"],"prefix":"10.1002","volume":"22","author":[{"ORCID":"https:\/\/orcid.org\/0009-0006-1312-1495","authenticated-orcid":false,"given":"Zhikang","family":"Zhou","sequence":"first","affiliation":[{"name":"Materials Science and Engineering Program &amp; Department of Mechanical Engineering State University of New York  Binghamton New York USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hanlei","family":"Zhang","sequence":"additional","affiliation":[{"name":"Materials Science and Engineering Program &amp; Department of Mechanical Engineering State University of New York  Binghamton New York USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Dongxiang","family":"Wu","sequence":"additional","affiliation":[{"name":"Materials Science and Engineering Program &amp; Department of Mechanical Engineering State University of New York  Binghamton New York USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jianyu","family":"Wang","sequence":"additional","affiliation":[{"name":"Materials Science and Engineering Program &amp; Department of Mechanical Engineering State University of New York  Binghamton New York USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2943-2926","authenticated-orcid":false,"given":"Xiaobo","family":"Chen","sequence":"additional","affiliation":[{"name":"Materials Science and Engineering Program &amp; Department of Mechanical Engineering State University of New York  Binghamton New York USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chaoran","family":"Li","sequence":"additional","affiliation":[{"name":"Materials Science and Engineering Program &amp; Department of Mechanical Engineering State University of New York  Binghamton New York USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shan","family":"Yan","sequence":"additional","affiliation":[{"name":"Department of Chemistry State University of New York  Binghamton New York USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jing","family":"Li","sequence":"additional","affiliation":[{"name":"Department of Chemistry State University of New York  Binghamton New York USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5283-9647","authenticated-orcid":false,"given":"Adrian","family":"Hunt","sequence":"additional","affiliation":[{"name":"National Synchrotron Light Source II Brookhaven National Laboratory  Upton New York USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4046-9722","authenticated-orcid":false,"given":"Iradwikanari","family":"Waluyo","sequence":"additional","affiliation":[{"name":"National Synchrotron Light Source II Brookhaven National Laboratory  Upton New York USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0746-250X","authenticated-orcid":false,"given":"Chuanjian","family":"Zhong","sequence":"additional","affiliation":[{"name":"Department of Chemistry State University of New York  Binghamton New York USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9243-293X","authenticated-orcid":false,"given":"Guangwen","family":"Zhou","sequence":"additional","affiliation":[{"name":"Materials Science and Engineering Program &amp; 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