CuO pricky microspheres have been synthesized without additives by calcination after hydrothermal treatment at [Formula: see text]C for 6[Formula: see text]h. The product was characterized by SEM, TEM, EDS, etc. The unique pricky microspheres were formed with NH4HCO3 and urea as precipitators. Through a series of reaction experiments, the possible formation mechanism of nucleation, growth and secondary growth was proposed. With the assistance of H2O2, the degradation rate of RhB aqueous solution reached 87.16% after 50 min by simulated visible light degradation, which proved the good photocatalytic performance of the CuO pricky microspheres. After four cycles of degradation experiments, the degradation rate of RhB aqueous solution is still above 80%. The radical capture experiments showed that the main active groups in the degradation process were ⋅OH and ⋅O2−, and the mechanism of photocatalytic degradation of Rhb was proposed.
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