正交试验优化溶胶凝胶法制备纳米氧化锌

Optimization of Sol Gel Preparation of Nano ZnO by Orthogonal Test

以醋酸锌和草酸为原料,利用溶胶凝胶法制备纳米氧化锌晶体。用正交实验法考查了纳米氧化锌制备过程中醋酸锌浓度、草酸与醋酸锌摩尔比、溶剂用量V_(乙醇)∶V_(水)、柠檬酸三铵与醋酸锌质量比的影响,优化了制备过程中的搅拌温度及搅拌时间、反应温度及反应时间、真空干燥温度及真空干燥时间、煅烧温度及煅烧时间。采用X射线衍射、扫描电镜、红外光谱对样品的结构等性能进行了考查。结果表明:制备的纳米氧化锌具有六方晶体结构。研究发现,醋酸锌浓度为0.4 mol/L,草酸与醋酸锌摩尔比为1∶1,溶剂用量V_(乙醇)∶V_(水)为1∶1,柠檬酸三铵与醋酸锌质量比8%,搅拌温度为90℃,搅拌时间为1 h,反应温度为60℃,反应时间为0.5 h,真空干燥温度为60℃,真空干燥时间为2.5 h,煅烧温度为700℃,煅烧时间为2 h,所制备的纳米氧化锌纯度高,分散性好,晶型良好。

In this paper,zinc acetate and oxalic acid were used as raw materials to prepare nano zinc oxide crystals by sol gel method.During the experiment,the effects of the concentration of zinc acetate,the molar ratio of oxalic acid to zinc acetate,the amount of solvent Vethanol∶Vwater,the mass ratio of ammonium citrate to zinc acetate on the preparation of nano zinc oxide were investigated by orthogonal experiment.The stirring temperature and stirring time,reaction temperature and reaction time,vacuum drying temperature and vacuum drying time,calcination temperature and calcination time were optimized.The structure and properties of the samples were investigated by X-ray diffraction,scanning electron microscopy and infrared spectroscopy.The experimental results show that the prepared nano ZnO has hexagonal crystal structure.It was found that the nano zinc oxide prepared by the method of zinc acetate concentration 0.4 mol/L,molar ratio of oxalic acid to zinc acetate 1∶1,solvent dosage Vethanol∶Vwater 1∶1,mass ratio of ammonium citrate to zinc acetate 8%,stirring temperature 90℃and stirring time 1 h,reaction temperature 60℃and reaction time 0.5 h,vacuum drying temperature 60℃and vacuum drying time 2.5 h,calcination temperature 700℃and calcination time 2 h has high purity and good dispersion.The crystal form is good.