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A series of ZnO-CeO 2 binary oxides with a novel hydrangea-like morphology and meso-/macroporous hierarchical structure of high surface area (around 100 m 2 /g) were synthesized by a simple one-pot hydrothermal process in the presence of triblock copolymer F127. Homogeneous mixing of wurtzite ZnO and cubic phase CeO 2 and the coexistence of Ce 3+ and Ce 4+ on the surface of the synthesized ZnO-CeO 2 materials were confirmed. UV/Vis diffuse reflectance spectra show that the absorption edges of the binary oxides shift remarkably to the visible range relative to those of pure ZnO and CeO 2 . Their photoactivities were tested by photodegradation of Rhodamine B under UV and visible light irradiation, and excellent photocatalytic performance for organic waste degradation was found in the synthesized hydrangea-like meso-/ macroporous ZnO-CeO 2 materials. Furthermore, their application as heterogeneous catalysts for CO removal was evaluated, and the results indicate that the synthesized ZnO-CeO 2 materials exhibit efficient activity for removing CO by catalytic oxidation, demonstrating a promising potential in environmental remediation.