Department of Chemistry, Faculty of Science, University of Guilan, P.O. Box 1914, Rasht, Iran.
Department of Chemistry, Faculty of Science, University of Guilan, P.O. Box 1914, Rasht, Iran.
Spectrochim Acta A Mol Biomol Spectrosc. 2014 Apr 5;123:142-50. doi: 10.1016/j.saa.2013.12.050. Epub 2013 Dec 18.
The synthesis of CuS nanomaterial in MCM-41 matrix has been realized by chemical synthesis between MCM-41, copper sulfate pentahydrate and thiourea via a solvothermal method in ethylene glycol and water, separately. X-ray diffraction analysis (XRD), diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and fourier transform infrared (FT-IR) were used to characterize the products. At synthesized CuS/MCM-41 sample in ethylene glycol, X-ray diffraction and diffuse reflectance spectroscopy showed pure covellite phase of copper sulfide with high crystality. But prepared CuS/MCM-41 sample in water shows the covellite, chalcocite and the djurleite phase of copper sulfide nanostructures. The formation of CuS nanostructures was confirmed by FT-IR. Photocatalytic activity of CuS/MCM-41 nanocomposites was studied for degradation of Methylene Blue (MB) under visible light. The CuS/MCM-41 nanocomposite is more effective nanocatalyst than synthesized CuS/MCM-41 sample in water for degradation of methylene blue. Several parameters were examined, catalyst amount (0.1-1gL(-1)), pH (1-13) and initial concentration of MB (0.96-10ppm). The extent of degradation was estimated from the residual concentration by spectrophotometrically. The support size was obtained in the range 60-145nm by TEM. In the same way, the average size of copper sulfide in CuSMCM-41E and CuS/MCM-41W nanostructures were obtained about 10nm and 16nm, respectively.
通过在乙二醇和水中分别进行溶剂热法，在 MCM-41 介孔分子筛、五水硫酸铜和硫脲之间进行化学合成，实现了 CuS 纳米材料在 MCM-41 基质中的合成。采用 X 射线衍射分析（XRD）、漫反射光谱（DRS）、扫描电子显微镜（SEM）、透射电子显微镜（TEM）和傅里叶变换红外光谱（FT-IR）对产物进行了表征。在乙二醇中合成的 CuS/MCM-41 样品中，X 射线衍射和漫反射光谱显示出具有高结晶度的纯蓝铜矿相的硫化铜。但是在水中制备的 CuS/MCM-41 样品显示出蓝铜矿、辉铜矿和铜硫代亚砷酸盐相的硫化铜纳米结构。FT-IR 证实了 CuS 纳米结构的形成。研究了 CuS/MCM-41 纳米复合材料在可见光下对亚甲基蓝（MB）的降解的光催化活性。CuS/MCM-41 纳米复合材料比在水中合成的 CuS/MCM-41 样品更有效，是用于亚甲基蓝降解的纳米催化剂。考察了几种参数，包括催化剂用量（0.1-1gL(-1)）、pH 值（1-13）和 MB 的初始浓度（0.96-10ppm）。通过分光光度法从残留浓度估计降解程度。通过 TEM 获得了载体尺寸在 60-145nm 范围内。同样，在 CuS/MCM-41E 和 CuS/MCM-41W 纳米结构中，铜硫化物的平均尺寸分别约为 10nm 和 16nm。
