Synthesis and Catalytic Performance of ZnCo ₂ O ₄ Microcubes via a Sacrificial Template Route

Abstract ZnCo 2 O 4 microcubes composed of connected nanoparticles are synthesized with Zn─Co oxalate microcubes as a sacrificial template in an aqueous solution. The XRD, SEM, TEM, TG‐DTA, and FT‐IR characterizations were used to investigate the substitution‐oxidation process (i.e., Zn─Co oxalate→ZnO/Co(OH) 2 →ZnCo 2 O 4 ). The molarity of the Zn/Co ratio is an important factor influencing the morphology of ZnCo 2 O 4. The photocatalytic degradation of rhodamine B (RhB) demonstrates that the as‐prepared ZnCo 2 O 4 microcubes possess high photocatalytic performance in the visible range, and their band gap is 1.67 eV. The degradation rate of RhB by ZnCo 2 O 4 microcubes can reach 60% under visible light for 2 h. At the same time, the catalytic decomposition of H 2 O 2 can reach 92% under the conditions of an initial H 2 O 2 concentration of 9.52 mg L −1 and pH 7.