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Here, a new class of high\u2010entropy\u2010like nanoparticles is reported, based entirely on post\u2010transition metals, Ga, In, Sn, Zn, and Bi, which undergo core\u2010level nanoscale homogenization via low\u2010temperature sonication. Starting from a bulk high\u2010entropy\u2010like melt, with clear phase segregation, including Ga\u2010rich, Zn\u2010rich, and Bi\u2010rich domains, ultrasonic agitation is applied to disrupt their immiscibility. The resulting cavitation and shear forces promote rapid mixing and atomic\u2010level diffusion, forming uniformly distributed high\u2010entropy\u2010like, compositionally complex nanoparticles with a core\u2010shell structure. When applied for electrochemical carbon dioxide reduction, the nanoparticles exhibit high current densities with a selectivity toward formates. The finding demonstrates a scalable route to high\u2010entropy\u2010like nanoparticles derived from post\u2010transition metals, circumventing the need for high\u2010temperature or shock\u2010based synthesis, while also expanding the compositional space into softer, low\u2010melting\u2010point systems.<\/jats:p>","DOI":"10.1002\/smll.202509123","type":"journal-article","created":{"date-parts":[[2025,11,24]],"date-time":"2025-11-24T10:44:21Z","timestamp":1763981061000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Homogenization of Post\u2010Transition Metal Alloys into High\u2010Entropy\u2010Like Nanoparticles"],"prefix":"10.1002","volume":"22","author":[{"given":"Francois\u2010Marie","family":"Allioux","sequence":"first","affiliation":[{"name":"School of Chemical and Biomolecular Engineering The University of Sydney  Darlington NSW 2008 Australia"},{"name":"School of Chemical Engineering University of New South Wales (UNSW)  Kensington NSW 2052 Australia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Luis G. 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