以二水合氯化铜和硫代乙酰胺分别作为铜源和硫源,采用水浴法于65℃合成纳米硫化铜(CuS),然后采用水热法将纳米CuS与氧化石墨烯混合,加入抗坏血酸作为还原剂,在180℃下反应制备了纳米硫化铜/还原氧化石墨烯(CuS/RGO)复合材料。利用X射线衍射仪、X射线光电子能谱仪、拉曼光谱仪、扫描电子显微镜、比表面积及孔隙度分析仪、紫外-可见-近红外漫反射测试仪对复合材料进行了测试表征,以150W氙灯作为可见光源,在可见光照射下考察了纳米CuS、RGO和纳米CuS/RGO复合材料对亚甲基蓝(MB)的光催化降解性能。结果表明,纳米CuS均匀负载于RGO表面,复合材料的比表面积高达66.5m2/g,在波长300~700nm范围可见光吸收性能良好。在可见光照射120min条件下,用量均为0.03g的纳米CuS、RGO、纳米CuS/RGO复合材料对MB的降解率分别为38.4%、21.3%、78.5%,用量为0.1g的纳米CuS/RGO复合材料对MB降解率达到了98.6%,说明RGO的引入极大提高了纳米CuS在可见光区域的光催化活性。
Copper chloride dihydrate was used as copper source and thioacetamide was used as sulfur source.Nano-CuS was prepared by water bath method at 65℃,then CuS/RGO nanocomposites were prepared by mixed nano-CuS with GO at 180℃ by hydrothermal method,while ascorbic acid was added as reducing agent.All composites were characterized by XRD,XPS,Raman,SEM,BET,UV-Vis,and the photocatalytic activity of nano-CuS,RGO and CuS/RGO was evaluated by degradation of methylene blue under xenon lamps(150W) irradiation.The results showed that the nano-CuS was evenly composed with the RGO,and the specific surface area of the composite was 66.5m2/g,and the UV-Vis showed a outstanding visible light absorption performance.The degradation rate of 0.03g CuS,RGO,and CuS/RGO was 38.4%,21.3%,78.5% after 120min irradiation.The degradation rate of 0.1g CuS/RGO reached 98.6% after 120min of irradiation,which indicated that the introduction of RGO greatly improved the photocatalytic property of CuS in the visible light region.
[1] Xiang Q,Yu J,Jaroniec M.Graphene-based semiconductor photocatalysts[J].Chemical Society Reviews,2012,41(2):782-796.
[2] Zhang N,Zhang Y,Pan X,et al.Constructing ternary CdS-graphene-TiO2 hybrids on the flatland of graphene oxide with enhanced visible-light photoactivity for selective transformation[J].The Journal of Physical Chemistry C,2012,116(34):18023-18031.
[3] 陈良伟,王娟,田成成.花状ZnO/石墨烯复合微球制备及其光催化性能的研究[J].宿州学院学报,2016,31(2):115-117.
[4] 朱柏林.石墨烯/二硫化钼/硫化物复合光催化剂的制备及性能研究[D].泉州:华侨大学,2014.
[5] 张耀君,余淼,张力,等.一种新型石墨烯-粉煤灰基地质聚合物复合材料的制备及光催化应用[J].材料导报,2017,31(9):50-56,63.
[6] Qin Y,Sun Z,Zhao W,et al.Improved photocatalytic properties of ZnS/RGO nanocomposites prepared with GO solution in degrading methyl orange[J].Nano-Structures & Nano-Objects,2017,10:176-181.
[7] Zeng B,Liu W,Zeng W.Simple and environmentally-friendly synthesis of graphene-CdS hierarchical nanospheres and their photocatalytic performance[J].Journal of Materials Ence,2019,30(4):3753-3759.
[8] Babu S G,Vijayan A S,Neppolian B,et al.SnS2/rGO:an efficient photocatalyst for the complete degradation of organic contaminants[J].Materials Focus,2015,4(4):272-276.
[9] 汪永彬.石墨烯基金属硫化物(CuS,CdS)复合材料的制备及光催化性能研究[D].太原:中北大学,2014.
[10] Shi J,Zhou X,Liu Y,et al.Sonochemical synthesis of CuS/reduced graphene oxide nanocomposites with enhanced absorption and photocatalytic performance[J].Materials Letters,2014,126:220-223.
[11] Borthakur P,Boruah P K,Darabdhara G,et al.Microwave assisted synthesis of CuS-reduced graphene oxide nanocomposite with efficient photocatalytic activity towards azo dye degradation[J].Journal of Environmental Chemical Engineering,2016,4(4):4600-4611.
[12] Saranya M,Ramachandran R,Kollu P,et al.A template-free facile approach for the synthesis of CuS-rGO nanocomposites towards enhanced photocatalytic reduction of organic contaminants and textile effluents[J].RSC Advances,2015,5(21):1-3.
[13] 吴娟霞,徐华,张锦.拉曼光谱在石墨烯结构表征中的应用[J].化学学报,2014,72(3):301-318.