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Hierarchical CuO microspheres have been successfully synthesized by chemical bath deposition, during which Cu(OH) 2 nanorobs firstly transform into CuO nanosheets and then these nanosheets spontaneously self-assemble to form CuO microspheres. Detailed characterization of the synthesized nanomaterials was performed utilizing X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and UV–Vis absorption spectra to study their crystalline phase, morphology and optical property. Additionally, photocatalytic performance of Cu(OH) 2 /CuO composite and pure CuO nanostructures was evaluated. Optical gaps of them are 2.75 eV and 1.33 eV respectively, showing a significant enhancement in the photocatalytic property in comparison with commercial CuO as demonstrated in photodegradation of methyl blue (MB). A growth mechanism for the formation of CuO nanostructure was also proposed. [ABSTRACT FROM AUTHOR]