Title: 奈米級銅金屬之合成
Synthesis of Copper Nano-Particles
Authors: 邱靜雯
Ching-Wen Chiu
Hsin-Tien Chiu
Keywords: 銅金屬粉末;奈米尺寸;矽烷化合物;Copper nano particles;Copper tert-butoxide;Copper Chloride;Tetrakistrimethylsilylsilane
Issue Date: 2000
Abstract: 奈米級銅金屬之合成 研究生:邱靜雯 指導教授:裘性天 國立交通大學應用化學研究所 摘要 在本研究中,利用Si(SiMe3)4做為還原劑,成功地將CuCl2及[CuO-t-Bu]4還原成奈米級的銅金屬粉末,經由XPS,TEM,XRD,ICP-Mass及EA來鑑定粉末的特性及組成,並使用NMR及GC-MS來分析其附產物。 在將CuCl2還原成銅金屬的反應中,CuCl2會先被還原成CuCl,然後再被還原成銅金屬,且由TEM的結果中可知此銅金屬粉末的顆粒大小約在50到100 nm之間。而在附產物的分析中,發現低溫反應與高溫反應的附產物非常的相似,推測Si(SiMe3)4移去CuCl2與CuCl中的氯的方式很類似。 在343 K時,利用Si(SiMe3)4將[CuO-t-Bu]4還原成銅金屬的反應中,發現過量的pyridine的存在是很重要的,推測pyridine會與[CuO-t-Bu]4配位,促進此四聚體的結構分解,使得Si(SiMe3)4比較容易將tBuO這個配位基移除。由TEM的結果中得知,未經熱處理之粉末的粒徑大小為5到20 nm,在經過ED圖形的比對後,證實此奈米粉末為銅金屬。
Synthesis of Cu nano particles Student: Ching-Wen Chiu Advisor: Hsin-Tien Chiu Institute of Applied Chemistry, National Chiao Tung University Abstract Copper nano particles were successfully synthesized by reacting Si(SiMe3)4 with CuCl2 and [CuO-t-Bu]4, respectively. These collected powders were characterized using x-ray photoelectron spectroscopy (XPS), x-ray diffraction (XRD), transmission electron microscopy (TEM), ICP-Mass and elemental analysis (EA). The analyses of reaction by-products were achieved through nuclear magnetic resonance (NMR) and gas-chromatography Mass (GC-MS). Combing all the results from XPS, XRD, EA and ICP-Mass, we know that Si(SiMe3)4 reduces CuCl2 to CuCl then to metallic Cu as the temperature increased. From the TEM studies, the particle size of these metallic copper powders was distributed from 50 nm to 100 nm. From the NMR and GC-MS experiments, it is speculated that the reaction pathways of reducing CuCl2 into CuCl and reducing CuCl into Cu are similar. Si(SiMe3)4 reduces [CuO-t-Bu]4 into metallic copper powder at 373 K in the presence of excess pyridine. In this reaction the role of pyridine is important. We propose that pyridine actively assists the dissociation of the tetrameric [CuO-t-Bu]4. The TEM of the as-prepared powder indicates that the particle size distribution is between 5 nm to 20 nm.
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