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金属铜及氧化亚铜纳米材料的非模板法制备与性质研究

Study on Template-free Preparation and Properties of Copper and Cuprous Oxide Nanometer Materials

【作者】 贺胜男

【导师】 王华林;

【作者基本信息】 合肥工业大学 , 应用化学, 2009, 硕士

【摘要】 论文用简单易行的无模板法制备铜及其氧化物纳米材料,并对材料性能进行了研究。先用简单的液相回流还原法制备了Cu2O纳米空心球前驱物,再用氢气还原法还原得到了Cu纳米空心球。在Cu2O前驱物的制备过程中,有机溶剂对球径的大小有影响,无水乙醇中制备的Cu2O空心球的平均粒径比叔丁醇体系小。由于叔丁醇体系制备Cu2O空心球的产率(75%)比无水乙醇体系(70%)稍高,选择叔丁醇溶剂体系制备Cu2O空心球作为氢气还原的前驱物。考察了还原温度和还原时间对于氢气还原Cu2O效率的影响,当反应时间2小时,还原温度在170℃左右时,基本可得到较纯的产物Cu空心球。紫外-可见吸收的光学特征图谱显示Cu2O前驱物样品和Cu纳米空心球与块体相应颗粒相比,都发生了较大程度的蓝移。同时,回流法制备的Cu2O纳米空心球,在经过较长时间的低温保存后,逐渐演变为具有核壳结构的纳米十四面体。在回流及氨气保护条件下,以叔丁醇为溶剂,乙酸铜为铜源,制备了纳米级金属铜空心球结构的。空心球的直径为400nm左右。还原剂的加入量对产物成分有重要影响。

【Abstract】 In this paper, the convenient template free processes for the preparation of copper and cuprous oxide nanometer materials are reported, and the properties of the materials are studied.Cu2O hollow nanospheres were first generated through a template free process, and then Cu hollow nanospheres were prepared with Cu2O hollow nanospheres as precursor and H2 as the reductant. During the preparation of the precursor, nanospheres formed in absolute alcohol were smaller in size than in tert-butyl alcohol in the similar reaction conditions. The Cu2O hollow nanospheres prepared in tert-butyl alcohol were chosen as the precursor, since the production rate(75%) is higher than in absolute alcohol(70%). The reduction time and temperature of hydrogen reduction were studied: the well-dispersed Cu hollow nanospheres can be fabricated at 170°C with a reduction time of 2 hours. Moreover, a remarkable blue-shift phenomenon was found in the ultraviolet–visible light (UV–visible) absorption spectra of both Cu and Cu2O hollow nanospheres. During the preservation of the Cu2O hollow nanospheres, a well-regulated tetrakaidecahedron of the surface morphology with a core-shell structure formed.Under the protection of NH3 gas, Cu hollow nanospheres were prepared by a refluxing method, with Tert-Butyl alcohol as the organic solvent, and acetate monohydrateas as the source of copper. The produtions are hollow nanospheres with a diameter of about 400nm. The dose of the reducer plays an important role on the purity of the production.

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