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Here, we establish design principles for thermally robust Al\u2010based nanocomposites by systematically assessing their thermal instability through correlated synchrotron X\u2010ray diffraction, high\u2010resolution microscopy, atom probe tomography, and nanoindentation following vacuum annealing between 160\u00b0C and 600\u00b0C. Angle\u2010resolved X\u2010ray diffraction (XRD) reveals Al crystallite evolution while high\u2010resolution microscopy unravels further instability mechanisms: At homologous temperature\n                    <jats:italic>\n                      T\n                      <jats:sub>hom<\/jats:sub>\n                    <\/jats:italic>\n                    \u2248 0.52 (\u223c210\u00b0C), Ni segregation to Al grain boundaries competes with Al\n                    <jats:sub>3<\/jats:sub>\n                    Ni formation. Hydroxylated ALD\u2010AlO\n                    <jats:italic>\n                      <jats:sub>x<\/jats:sub>\n                    <\/jats:italic>\n                    H\n                    <jats:italic>\n                      <jats:sub>y<\/jats:sub>\n                    <\/jats:italic>\n                    interlayers become mobile, driving swelling and oxidation of adjacent Al. At\n                    <jats:italic>\n                      T\n                      <jats:sub>hom<\/jats:sub>\n                    <\/jats:italic>\n                    \u2248 0.77 (\u223c450\u00b0C),\n                    <jats:italic>\u03ba<\/jats:italic>\n                    \u2010Al\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>3<\/jats:sub>\n                    crystallises, followed by interlayer rupture, while at\n                    <jats:italic>\n                      T\n                      <jats:sub>hom<\/jats:sub>\n                    <\/jats:italic>\n                    \u2248 0.94 (\u223c600\u00b0C) the nanolaminate architecture collapses into a coarsened Al(Ni) matrix with dispersed Al\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>3<\/jats:sub>\n                    inclusions. These coupled transformations progressively reduce hardness, transitioning from confined layer slip to matrix\u2013inclusion\u2010dominated deformation. Beyond elucidating degradation mechanisms, this work shows how hydrogen\u2010mediated interface dynamics and the dual role of alloyed\u2010Ni limit the thermal and mechanical stability, precisely identifying the onset temperatures, and providing a pathway to robust Al\u2010based PVD\/ALD nanocomposites.\n                  <\/jats:p>","DOI":"10.1002\/smll.75393","type":"journal-article","created":{"date-parts":[[2026,8,22]],"date-time":"2026-08-22T10:02:52Z","timestamp":1787392972000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Thermal Instability Pathways of Aluminum\u2010Based Nanocomposites: The Role of Alloying\u2010Element\u2010Driven Precipitation and Amorphous Interlayers"],"prefix":"10.1002","volume":"22","author":[{"ORCID":"https:\/\/orcid.org\/0009-0004-3513-4348","authenticated-orcid":false,"given":"Hendrik C.","family":"Jansen","sequence":"first","affiliation":[{"name":"Laboratory For Mechanics of 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