Formation of Mixed‐Metal Ceria Nanopeapod Composites within Scrolled Hexaniobate Nanosheets

Abstract Ceria hexaniobate nanopeapods have been prepared and their formation and assembly studied. Various sized ceria nanocubes (5 to 40 nm) were synthesized via a solvothermal approach with oleic acid and oleylamine capping agents. Utilizing a second solvothermal treatment, the nanoparticles were then captured within scrolling hexaniobate nanosheets to produce ceria@hexaniobate nanopeapods. In some instances, peapods were partially filled with ceria so that in a subsequent step, open sites could be filled with Au nanoparticles via in situ growth methods leading to arrangements of gold and ceria NPs within nanoscrolls. Studies on nanoparticle assembly and encapsulation were also carried out. Size‐selective preassembly of nanoparticles on hexaniobate nanosheet surfaces is observed prior to scrolling, after which smaller ceria NPs (ca. ≤ 10 nm) are efficiently captured inside scrolled nanosheets. Improved understanding and control of this behavior is important for further development of more intricate multicomponent particles assemblies and formations within varieties of tubular structures with different morphological and structural features.