铜氨络合物冷冻干燥法制备氧化铜纳米粉体的实验研究

Experimental study on copper oxide nanopowder prepared through cuprammonian complex freeze-drying process

本文以无机化合物硫酸铜和氢氧化钠为原料,选取铜氨络合物为前驱体,采用冷冻干燥法制备出氧化铜纳米粉体。粉体形态分别为粒径为20～50nm的实心颗粒和粒径大于200nm带有约10nm均匀孔隙的多孔颗粒。进行了TEM、SEM和XRD检测。文中详细介绍了前驱体溶液的制备、冷冻、冻干和样品测试的实验全过程,给出了前驱体制备及分解的反应原理;就前驱体物质选取以及冷冻方式和煅烧分解条件对所制粉体品质的影响,作了讨论。

A new preparation process of copper oxide nanopowder was developed through freeze-drying technique, with copper sulphate and sodium hydroxide as raw materials and cuprammonian complex as precursor. The nanopowder is in form of the solid particles in 20-50nm diameter and the porous particles whose size are over 200nm with about 10nm porosity, and TEM, SEM and XRD were used to test the nanopowder. The whole experiment process is described in detail, including preparation of the precursor solution, freezing, freeze-drying and sample testing, with the reactions in its preparation/ decomposition discussed. In addition, how the choice of precursor, the way to freeze and the conditions for calcination/ decomposition affect the quality of the nanopowder thus prepared are also discussed.