纳米结构氧化亚铜和硫化铜的制备与相关性能研究
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摘要
本文利用化学液相法分别制备了纳米结构氧化亚铜和硫化铜，并研究了它们的相关性能。在蔗糖溶液中，利用抗坏血酸还原CuSO_4溶液，制得了粒径较均匀的Cu_2O纳米球。通过调节蔗糖浓度，纳米球直径可以在90-280nm范围内实现调控。并以抗坏血酸为还原剂，柠檬酸钠为配位剂，制得了平均边长为450nm的Cu_2O纳米方块。又以葡萄糖为还原剂，聚乙烯吡咯烷酮(PVP)为表面活性剂，制得了边长为0.5-1.5μm的Cu_2O亚微米八面体。在此基础上，利用柯肯达尔(Kirkendall)效应，将Na_2S溶液分别与Cu_2O纳米球和纳米方块反应，制得了Cu_(7.2)S_4纳米空心球和纳米盒子。研究表明，这两种空心产物分别经由Cu_2O/Cu_(7.2)S_4核/壳型纳米结构转化而来。通过柠檬酸钠的后处理，Cu_(7.2)S_4纳米空心球和纳米盒子可转化为CuS纳米空心球和纳米盒子。利用X射线衍射(XRD)、透射电镜(TEM)和场发射扫描电镜(FESEM)等测试手段对产物进行了结构表征，对反应条件和反应机理进行了探讨。
在Cu_(7.2)S_4纳米空心球对亚甲基蓝的吸附行为研究工作中，分别测定了温度20℃、35℃、50℃实验条件下的吸附等温线。数据分析表明，Freundlich和Langmuir两种等温式均能较好地定量模拟描述该吸附行为。吸附热力学研究表明，Cu_(7.2)S_4对亚甲基蓝的吸附是自发的吸热吸附，是熵增的过程。
Nanostructured cuprous oxide and copper sulfides powders have been prepared via a wet chemical route. Firstly, uniform Cu_2O nanospheres have been synthesized by reducing CuSO_4 with ascorbic acid in the sucrose solution, and the diameters of these nanospheres can be controlled in the range of 90-280 nm by changing the concentration of sucrose solution. Meanwhile, Cu_2O nanocubes (450 nm in edge length) are prepared with the coordination agent citrate. Cu_2O submicro-sized octahedron crystals (0.5-1.5μm in edge length) are prepared with the reducing agent glucose and the surfactant polyvinyl pyrrolidone. Secondly, Cu_(7.2)S_4 hollow nanospheres and nanoboxes are prepared from the reaction of the as-prepared Cu_2O nanospheres and nanocubes with Na_2S aqueous solution based on the Kirkendall effect, respectively. And the intermediates of the conversion, Cu_2O/Cu_(7.2)S_4 core/shell nanostructures have been recorded. Thirdly, by the subsequent treatment of Cu_(7.2)S_4 hollow samples with sodium citrate solution, CuS hollow nanospheres and nanoboxes are obtained. The samples are characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM). The reaction conditions are studied. Based on the experimental results, the possible formation mechanisms have been proposed.
In addition, the adsorption effect of the methylene blue (MB) dye on Cu_(7.2)S_4 hollow nanospheres is investigated. The adsorption isotherms at different temperature (20℃, 35℃, 50℃) were determined respectively. The data analysis shows that the adsorption of MB on Cu_(7.2)S_4 hollow nanospheres obeys Freundlich and Langmuir equations. Further study indicates that the adsorption is a spontaneous endothermic process with a positive entropy changes.
在Cu_(7.2)S_4纳米空心球对亚甲基蓝的吸附行为研究工作中，分别测定了温度20℃、35℃、50℃实验条件下的吸附等温线。数据分析表明，Freundlich和Langmuir两种等温式均能较好地定量模拟描述该吸附行为。吸附热力学研究表明，Cu_(7.2)S_4对亚甲基蓝的吸附是自发的吸热吸附，是熵增的过程。
Nanostructured cuprous oxide and copper sulfides powders have been prepared via a wet chemical route. Firstly, uniform Cu_2O nanospheres have been synthesized by reducing CuSO_4 with ascorbic acid in the sucrose solution, and the diameters of these nanospheres can be controlled in the range of 90-280 nm by changing the concentration of sucrose solution. Meanwhile, Cu_2O nanocubes (450 nm in edge length) are prepared with the coordination agent citrate. Cu_2O submicro-sized octahedron crystals (0.5-1.5μm in edge length) are prepared with the reducing agent glucose and the surfactant polyvinyl pyrrolidone. Secondly, Cu_(7.2)S_4 hollow nanospheres and nanoboxes are prepared from the reaction of the as-prepared Cu_2O nanospheres and nanocubes with Na_2S aqueous solution based on the Kirkendall effect, respectively. And the intermediates of the conversion, Cu_2O/Cu_(7.2)S_4 core/shell nanostructures have been recorded. Thirdly, by the subsequent treatment of Cu_(7.2)S_4 hollow samples with sodium citrate solution, CuS hollow nanospheres and nanoboxes are obtained. The samples are characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM). The reaction conditions are studied. Based on the experimental results, the possible formation mechanisms have been proposed.
In addition, the adsorption effect of the methylene blue (MB) dye on Cu_(7.2)S_4 hollow nanospheres is investigated. The adsorption isotherms at different temperature (20℃, 35℃, 50℃) were determined respectively. The data analysis shows that the adsorption of MB on Cu_(7.2)S_4 hollow nanospheres obeys Freundlich and Langmuir equations. Further study indicates that the adsorption is a spontaneous endothermic process with a positive entropy changes.
引文
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