氧化铜纳米粉体的制备工艺研究

Study on Preparation of Copper Oxide Nanopowders

以三水硝酸铜为反应物,氨水为络合剂,氢氧化钠为沉淀剂,乙醇水混合溶液为反应溶剂,聚乙二醇为分散剂,采用络合沉淀法,成功制备出平均粒径约20 nm的氧化铜单晶纳米粉体。通过单因素实验和正交实验考察了硝酸铜溶液初始浓度、反应温度及氢氧化钠与硝酸铜物质的量比等因素对产物粒径大小的影响,利用X射线衍射(XRD)、透射电镜(TEM)和红外光谱仪(FT-IR)等对产物进行表征分析。研究结果表明,影响其粒径大小主要因素的主次顺序依次是:反应温度,硝酸铜溶液初始浓度及氢氧化钠与硝酸铜的物质的量比;优化制备工艺条件为:反应温度70℃,硝酸铜溶液初始浓度0.3 mol/L,氢氧化钠与硝酸铜的物质的量比3∶1,氨与硝酸铜的物质的量比5∶1;氧化铜纳米粉体的红外吸收峰出现了红移和蓝移同时并存的反常现象。

Using Cu （NO3 ）2 3 HzO as reactants, ammonia as complex agent, sodium hydroxide as precipita- tor, and polyethylene glycol as dispersant, ethanol and distilled water as solvent, copper oxide single crys- tal nanopowders which have average diameter about 20 nm are prepared by complex precipitation method. Mono -factor experiments and muhifactor orthogonal experiments are adopted to explore the influences of these factors, such as, the initial concentration of Cu （ NO3 ） 2, reaction temperature, molar ratio of sodium hydroxide and copper ion etc. on diameter of copper oxide nanopowders. And transmission electron micro- scope （TEM） and fourier transform infrared spectroscopy （FT -IR） , X -ray diffraction （XRD） are used to characterize and analyze the morphology, structure and property of products prepared. The experiment result shows that the diameter of copper oxide nanopowders is mostly influenced by reaction temperature, concentration of copper nitrate, ratio of sodium hydroxide and copper ion. The optimum conditions prepar- ing copper oxide nanopowders are as follows： reaction temperature 70 C, concentration of copper nitrate O. 3 mol/L, molar ratio of sodium hydroxide and copper nitrate 3 ： 1, molar ratio of ammonia and copper ion 5 ： 1. FT - IR absorption spectrum declares that copper oxide nanopowders are characterized by both red and blue shift anomaly