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化学学报
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化学学报 ›› 2011, Vol. 69 ›› Issue (23): 2812-2820.DOI: 10.6023/A1105043 上一篇    下一篇

研究论文

溶剂热法合成硫化铜花状微米球超结构及其光催化性能

谭志刚1, 朱启安*,1, 郭讯枝2,3, 张劲福1, 伍文雍1, 刘爱平1   

  1. (1湘潭大学化学学院 环境友好化学与应用省部共建教育部重点实验室 湘潭411105)
    (2中南大学国家卫生部肝胆肠外科研究中心 中南大学生物医学工程研究院 长沙 410008)
    (3宜春学院江西省天然药物活性成份研究重点实验室 宜春 336000)
  • 投稿日期:2011-05-04 修回日期:2011-07-20 发布日期:2011-07-29
  • 通讯作者: 朱启安 E-mail:zqa7887550@126.com
  • 基金资助:

    国家自然科学基金

Synthesis of Flower-Shaped CuS Microsphere Superstructures by a Solvothermal Route and Its Photocatalytic Properties

Tan Zhigang1; Zhu Qian*,1; Guo Xunzhi2,3; Zhang Jinfu1; Wu Wenyong1; Liu Aiping1   

  1. (1 Key Laboratory of Environmentally Friendly Chemistry and Applications of Ministry of Education, College of Chemistry, Xiangtan University, Xiangtan 411105)
    (2 National Hepatobiliary & Enteric Surgery Research Center, Ministry of Health, Institute of Biomedical Engineering of Central South University, Changsha 410008)
    (3 Yichun University, Key Laboratory of Jiangxi Province for Research on Active Ingredients in Natural Medicines, Yichun 336000)
  • Received:2011-05-04 Revised:2011-07-20 Published:2011-07-29

PDF

2705

被引次数

90

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2.2～4.8 µm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.

关键词: CuS, 溶剂热法, 微米球, 超结构, 光催化

Flower-like copper sulfide (CuS) microsphere superstructures with diameters of 2.2～4.8 µm comprising nanoflakes were successfully synthesized by a facile solvothermal process at 140 ℃ for 90 min, employing copper chloride (CuCl2•2H2O) 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.

Key words: CuS, solvothermal method, microsphere, superstructure, photocatalysis

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