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By the deposition of noble metal nanoparticles on a metal oxide substrate with a specific micro-/nanostructure, namely, yolk-shell structure, a remarkable improvement in photocatalytic performance can be achieved by the composites. Nevertheless, noble metal nanoparticles only distribute on the surface shell of metal oxide substrates when the conventional wet-chemistry reduction approach is employed. Herein, we proposed a novel acoustic levitation synthesis of Pt nanoparticles deposited on yolk-shell La₂O₃. The composites not only displayed well-defined, homogeneous distribution of Pt NPs on the exterior shell of La₂O₃ and the interior La₂O₃ core, but an enhanced chemical interaction between Pt and La₂O₃. The unique structure not only can display improved photocatalytic degradation rate toward methyl orange, but also may show great potential in fields of hydrogen generation, environmental protection, etc. The novel acoustic levitation synthesis can supplement the methodology of synthesizing well dispersed noble metal oxides over the whole yolk-shell structure through noble metal NPs deposition method.