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While the phase behavior of rod\u2013sphere mixtures has been explored in 2D and 3D bulk systems, it has remained unexplored in smaller 3D assemblies. Especially, when combining plasmonic and semiconductor nanoparticles, assemblies with defined particle arrangements offer unique optical and (photo)catalytic properties. In this work, we achieved the assembly of binary 3D assemblies tunable in size and phase behavior. Specifically, we assembled semiconductor TiO2 nanorods and plasmonic Au nanospheres under spherical confinement and explored their phase behavior in experiments and simulations. Through evaporation-driven assembly of emulsion droplets, binary supraparticles were prepared with a phase tunable from colloidal membranes, consisting of single rod layers, to binary smectic phases, composed of alternating rod\u2013sphere smectic layers. Colloidal membranes were obtained for a sphere-to-rod number ratio (NAu\/NTiO2) of 5, while lowering this ratio to 0.6 resulted in a binary smectic ordering, as confirmed with advanced electron microscopy. Through numerical simulations, we show that the binary smectic phase is stable for 0 &amp;lt; NAu\/NTiO2 \u2264 1 in agreement with experiments. Our binary supraparticle platform provides structures with multi-length scale control for applications in photocatalysis, energy storage, and sensing.<\/jats:p>","DOI":"10.1021\/acsnano.6c12966","type":"journal-article","created":{"date-parts":[[2026,9,25]],"date-time":"2026-09-25T20:04:29Z","timestamp":1790366669000},"page":"27415-27427","source":"Crossref","is-referenced-by-count":0,"title":["Self-Assembly of\nAu\/TiO2 Sphere\u2013Rod\nMixtures into Binary Supraparticles"],"prefix":"10.1021","volume":"20","author":[{"ORCID":"https:\/\/orcid.org\/0009-0008-6350-5440","authenticated-orcid":true,"given":"Marianne","family":"Bijl","sequence":"first","affiliation":[{"name":"Utrecht University , , Universiteitsweg 99, ,","place":["Utrecht, The Netherlands, 3584 CG"]},{"name":"Utrecht University , , Princetonplein 1 , ,","place":["Utrecht, The Netherlands, 3584 CC"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0078-8988","authenticated-orcid":true,"given":"Andre\u0301 F. V.","family":"Matias","sequence":"additional","affiliation":[{"name":"Utrecht University , , Princetonplein 1 , ,","place":["Utrecht, The Netherlands, 3584 CC"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Luka\u0301s\u030c","family":"Kola\u0301cny\u0301","sequence":"additional","affiliation":[{"name":"University of Chemistry and Technology Prague , , Technicka\u0301 5 , ,","place":["Prague, Czech Republic, 166 28"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3147-7867","authenticated-orcid":true,"given":"Erik","family":"Betz-Gu\u0308ttner","sequence":"additional","affiliation":[{"name":"Utrecht University , , Universiteitsweg 99, ,","place":["Utrecht, The Netherlands, 3584 CG"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3147-4941","authenticated-orcid":true,"given":"Martin","family":"Vesely\u0301","sequence":"additional","affiliation":[{"name":"University of Chemistry and Technology Prague , , Technicka\u0301 5 , ,","place":["Prague, Czech Republic, 166 28"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9166-6478","authenticated-orcid":true,"given":"Marjolein","family":"Dijkstra","sequence":"additional","affiliation":[{"name":"Utrecht University , , Princetonplein 1 , ,","place":["Utrecht, The Netherlands, 3584 CC"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9832-289X","authenticated-orcid":true,"given":"Jessi E. 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