铝掺杂纳米氧化锌工艺的粒径控制研究

Study on the size control in preparation of Al-doped nano-zinc oxide

以均匀沉淀法作为纳米氧化锌铝掺杂的制备方法。通过正交试验,考察了铝离子掺杂量、煅烧温度等反应参数对纳米氧化锌粉体粒径的影响。结果表明:水解温度的影响最大,其次是煅烧时间,尿素配比和煅烧温度影响较小;最佳工艺为以OP-10做表面活性剂,锌离子浓度0.3 mol/L,水解时间4h,尿素与锌离子摩尔比为3,水解温度95℃,煅烧温度450℃,煅烧时间2 h,铝离子的最佳掺杂量(以锌离子的摩尔数为基准)5%。对铝掺杂纳米氧化锌进行了XRD、SEM粒径分析,结果表明掺杂效果良好,得到的铝掺杂纳米氧化锌粒径最小可达到20 nm。

Al-doped nano-zinc oxide is prepared by homogeneous precipitation method.The orthogonal experiment is applied for studying the preparation process.The effects of the doped amount of Al,calcination temperature and calcination time on size of nanometer-zinc oxide are inspected.The results show that the effect of hydrolysis temperature is maxium,secondly is calcination time,and the ratio of urea and calcination temperature have slight effect.The optimum conditions are obtained as follows：using OP-10 as surfactant,zinc ion concentration is 0.3 mol/L,the hydrolysis time is 4 h,the ratio of urea to zinc ion is 3,hydrolysis temperature is 95 ℃,calcination temperature is 450 ℃,the calcination time is 2 h,and the doped amount of A1 is 5％ （based on the mole number of zinc ion）.The Al-doped nano-zinc oxide is analyzed by XRD and SEM,which shows good dopping effect,and the minimum diameter of Aldoped nano-zinc oxide is 20 nm.