Abstract: | We successfully fabricate a well‐defined inorganic/organic hybrid Cu2O@Cu/Co‐ZIF (ZIF=zeolitic imidazolate frameworks) by use of growth of dual‐metal Cu/Co‐ZIF on the obtained Cu2O hollow spheres. The key point of the strategy is coupling the in situ self‐sacrificing template. Cu2O and the coordination of metal ions (Cu+ and Co2+) with 2‐methylimidazole. This new hybrid was characterized by powder X‐ray diffraction, (scanning) transmission electron microscopy, energy‐dispersive spectroscopy mapping, in situ FT‐IR spectroscopy, UV/Vis diffuse reflection spectroscopy, N2 sorption measurements, and electron spin resonance. It was evidenced that Cu/Co‐ZIF nanocrystals have been assembled to continuous shells surrounding the Cu2O cores as well as in the voids between layers and inner pores. Cu2O@Cu/Co‐ZIF exhibits visible light responsiveness and holds potential as narrow band gap semiconductor and visible photocatalyst. |