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Synthesis and crystal structure of bis(thiomorpholinyldithiocarbamato) Zn(II): structural, optical, and photocatalytic studies of ZnS nanoparticles from the complex
Journal of Coordination Chemistry ( IF 2.2 ) Pub Date : 2020-04-17 , DOI: 10.1080/00958972.2020.1768248
Peter A. Ajibade 1 , Nolwazi Solomane 1
Affiliation  

Abstract Bis(thiomorpholinyldithiocarbamato) Zn(II) complex was synthesized and characterized by single crystal X-ray crystallography and spectroscopic techniques. The molecular structure of the compound revealed a dimeric Zn(II) complex in which each Zn(II) ion is bound to one chelating and two bridging thiomorpholine ligands. The compound was thermolyzed at 130 °C in octadecylamine (ODA), hexadecylamine (HDA), and oleylamine (OLA) to prepare ZnS nanoparticles. Powder X-ray diffraction (PXRD) of the ZnS nanoparticles indicates mixtures of hexagonal and cubic crystalline phases depending on thermolysis temperature. HRTEM micrographs showed well-defined nanoparticles with particle size of 3.3–4.8 nm for ODA-ZnS, 2.5–4.2 nm for OLA-ZnS, while HDA-ZnS shows slightly bigger nanoparticles with particle size of 3.3–5.4 nm. Estimated optical band gaps are 3.58 eV for ODA-ZnS, 3.69 eV for HDA-ZnS and 3.72 eV for OLA-ZnS which indicate blue shift of the absorption band edges with respect to bulk ZnS (3.56 eV). The as-prepared ZnS nanoparticles were used as photocatalysts for the degradation of methylene blue dye. The degradation efficiency of the as-prepared ZnS nanoparticles are 58% for ODA-ZnS, 53% for OLA-ZnS, and 43% for HDA-ZnS. ODA-ZnS nanoparticles were used for the recycling test and showed good photostability and recyclability with 57% recovery percentage. Graphical Abstract

中文翻译:

双(硫代吗啉基二硫代氨基甲酸) Zn(II) 的合成和晶体结构:复合物中ZnS 纳米颗粒的结构、光学和光催化研究

摘要 合成了双(硫代吗啉基二硫代氨基甲酸) Zn(II)配合物,并利用单晶X射线晶体学和光谱技术对其进行了表征。该化合物的分子结构揭示了一种二聚体 Zn(II) 复合物,其中每个 Zn(II) 离子与一个螯合和两个桥接硫代吗啉配体结合。该化合物在十八胺 (ODA)、十六胺 (HDA) 和油胺 (OLA) 中于 130 °C 下热解以制备 ZnS 纳米颗粒。ZnS 纳米粒子的粉末 X 射线衍射 (PXRD) 表明取决于热解温度的六方晶相和立方晶相的混合物。HRTEM 显微照片显示,ODA-ZnS 的粒径为 3.3-4.8 nm,OLA-ZnS 的粒径为 2.5-4.2 nm,而 HDA-ZnS 显示稍大的纳米颗粒,粒径为 3.3-5.4 nm。ODA-ZnS 的估计光学带隙为 3.58 eV,HDA-ZnS 为 3.69 eV,OLA-ZnS 为 3.72 eV,这表明吸收带边缘相对于体 ZnS (3.56 eV) 发生蓝移。所制备的硫化锌纳米颗粒用作降解亚甲蓝染料的光催化剂。所制备的 ZnS 纳米粒子的降解效率对于 ODA-ZnS 为 58%,对于 OLA-ZnS 为 53%,对于 HDA-ZnS 为 43%。ODA-ZnS 纳米颗粒用于回收测试,显示出良好的光稳定性和可回收性,回收率为 57%。图形概要 所制备的 ZnS 纳米粒子的降解效率对于 ODA-ZnS 为 58%,对于 OLA-ZnS 为 53%,对于 HDA-ZnS 为 43%。ODA-ZnS 纳米颗粒用于回收测试,显示出良好的光稳定性和可回收性,回收率为 57%。图形概要 所制备的 ZnS 纳米粒子的降解效率对于 ODA-ZnS 为 58%,对于 OLA-ZnS 为 53%,对于 HDA-ZnS 为 43%。ODA-ZnS 纳米颗粒用于回收测试,显示出良好的光稳定性和可回收性,回收率为 57%。图形概要
更新日期:2020-04-17
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