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Bimetallic catalysts have exhibited huge catalytic potential in the oxy-functionalization of alkanes. Here, we provide a valid strategy for encapsulating copper and zinc metal oxide nanoparticles by mesoporous SiO 2 . The prepared CuZn@mSiO 2 catalyst are yolk-shell nanospheres with a diameter of 600 nm and a large specific surface area around 1000 m 2 g À 1 . Bimetallic synergy between Cu and Zn was further analyzed by XRD, XPS and H 2 -TPR. The selective oxidation of cumene to acetophenone was used as a probe reaction to evaluate the activity of bimetallic yolk-shell catalysts, and the results showed excellent catalytic performance that promoted cumene to acetophenone transformation under mild conditions (80 °C, 5 h, H 2 O 2 as oxidant). Also, the recycling tests verified the robust stability and reusability for the catalyst. Finally, a reasonable reaction mechanism was proposed to better understand the oxidation pathway of cumene.