微波水热法用于制备纳米氧化锌粉体的研究

Study on preparation of ZnO nanopowder by microwave-hydrothermal method

以氯化锌和氢氧化钠为原料,采用微波水热法制备了纳米氧化锌粉体,并采用X射线衍射(XRD)和透射电镜(TEM)对粉体的粒度、形貌、纯度进行了表征。通过单因素实验考察了反应温度、微波反应时间、微波功率、锌离子与氢氧根的浓度比等因素对氧化锌粉体的产率和粒径的影响,再通过正交试验得到最优制备条件。最佳制备工艺条件:锌离子与氢氧根的浓度比为1∶1.2、反应温度为120℃、反应时间为10 min、微波功率为500 W。在此条件下所得氧化锌粉体的晶型为六方晶相,产率达到93.5%,平均粒度约70 nm,粒径分布较窄,结晶完整。

A process of microwave-hydrothermal method was established to synthesize ZnO nanopowders, using zinc chloride and sodium hydroxide as raw materials.Besides,the particle size,morphology,and purity of the prepared product were characterized by X-ray diffraction （XRD） and transmission electron microscope （TEM）.The influences of reaction temperature,microwave radiation period,microwave power,and concentration ratio of Zn2＋ to OH- on yield and size of ZnO nanopowders were investigated by single factor experiments and the optimum preparation conditions were obtained by orthogonal experiments.Experiment results indicated that： under the temperature of 120 ℃ ,c （Zn2＋）：c （OH-）=1：1.2 ,microwave radiation period of 10 min,and microwave power of 500 W,nano-sized ZnO with an average size of 70 nm,belonging to hexagonal system,could be produced and the yield reached 93.5%.Moreover,the crystallite sizes of the prepared samples were mostly uniform with narrow size distribution.