CuS花状空心微球制备工艺及其光降解性能研究

以硝酸铜、硫脲为原料, 聚乙烯吡咯烷酮(PVP)为表面活性剂, 采用一步溶剂热法制备了CuS花状空心微球。采用XRD、SEM-EDS、BET、UV-Vis DRS等手段对样品进行表征,并研究了样品对亚甲基蓝溶液的光-类芬顿降解行为, 考察了H₂O₂添加量、温度、pH值对光降解性能的影响。实验结果表明:制备的样品均为六方晶系铜蓝型结构的CuS, 其形貌受表面活性剂的影响; 3D花状空心微球结构由平均厚度约为30 nm的纳米片彼此交替相连组装而成; 添加了PVP的样品CuS花状空心微球的孔径减小, 比表面积和孔容积增大, 光降解性能提高了约30%; 在H₂O₂(30%)添加量0.8 mL、温度25 ℃、pH=6条件下, 可见光光照30 min后, CuS花状空心微球对亚甲基蓝的降解率可达93.0%。

Preparation and Photodegradation Property of Flower-like CuS Hollow Microspheres

The flower-like CuS hollow microspheres were successfully synthesized by one-step solvothermal method, with copper nitrate and thiourea as raw materials and polyvinylpyrrolidone (PVP) as a surfactant. The samples were characterized by means of XRD, SEM-EDS, BET and UV-Vis DRS. The degradation of methylene blue dyes by photo-Fenton-like reaction of the sample was studied. The effects of H₂O₂ additive amount, temperature and pH value on photodegradation performance were investigated. The experimental results showed that the synthesized samples were CuS of hexagonal crystal system with structure of covellite, and its morphology was affected by the surfactants. The 3D flower-like hollow microspheres were composed of nanosheets with an average thickness about 30 nm, which were alternatively connected to each other. The flower-like CuS hollow microspheres, after an addition of PVP, had smaller pore size, higher specific surface area and bigger pore volume, and its photodegradation performance was also improved by about 30%. With an addition of H₂O₂ (30%) at an amount of 0.8 mL, temperature at 25 ℃ and pH=6, the methylene blue was reduced by 93% after 30 min exposure to visible light.