以氯化铜(CuCl2 2H2O)和硫脲(CH4N2S,Tu)为原料,乙二醇(C2H6O2)为溶剂,用溶剂热法于140℃反应90 min成功制备了直径为2.2~4.8μm由纳米片组成的花状硫化铜(CuS)微米球超结构.用XRD,SEM,TEM,SAED,HRTEM以及UV-Vis等手段对产品进行了表征;以氙灯和高压汞灯为光源,亚甲基蓝为目标降解物评价了CuS超结构的光催化活性.结果表明,所制备的产品是六角相的CuS,经计算,其晶胞参数为a=0.3813 nm,c=1.6774 nm;所用溶剂、硫源、铜源及反应温度、反应时间对产品的形貌均有较大影响;UV-Vis分析表明,CuS微米球超结构的带隙能量为2.0 eV;光催化性能测试表明,所制备的CuS微米球超结构在紫外光区和可见光区均具有较高的光催化活性,但在可见光区的光催化活性更高,在35 W氙灯和450 W的高压汞灯下,光照30 min,亚甲基蓝的降解率分别达到98.7%和82.9%.此外,还讨论了硫化铜微米球超结构可能的形成机理.
Flower-like copper sulfide(CuS) microsphere superstructures with diameters of 2.2~4.8 ?m comprising nanoflakes were successfully synthesized by a facile solvothermal process at 140 ℃ for 90 min,employing copper chloride(CuCl2o2H2O) and thiourea(CH4N2S,Tu) as starting materials,ethylene glycol(C2H6O2) as the solvent.The products were characterized by means of XRD,SEM,TEM,SAED,HRTEM and UV-Vis techniques.The xenon lamp and high-pressure mercury lamp were used as light source to investigate the photocatalytic activity of CuS microspheres for the degradation of methylene blue.The result shows that the prepared products belong to hexagonal phase CuS with calculated cell parameters of a=0.3813 nm,c=1.6774 nm.It is also demonstrated that the morphology of the products is greatly influenced by solvents,different sources of sulfur and copper salt,reaction temperature and reaction time.UV-Vis analysis exhibits that the band gap energy of CuS microsphere superstructures is 2.0 eV.Photocatalytic tests indicate that the as-prepared CuS microspheres have high photocatalytic degradation rate for methylene blue under ultraviolet or visible regions,but the photocatalytic activity is higher in the visible region.The degradation rate of methylene blue is up to 98.7% and 82.9% after 30 min degradation under the irradiation of 35 W xenon lamp and 450 W high-pressure mercury lamp,respectively.In addition,the possible formation mechanism of CuS microsphere superstructures was also discussed.