以Zn(NO_3)_2·6H_2O为原料,NaOH为碱源,非离子表面活性剂十二胺(DDA)为分散剂,通过咪唑基离子液体([Bmim]R,R=Cl,Br,BF_4,PF_6)辅助微波合成ZnO自主装微球。通过X射线衍射(XRD)和扫描电子显微镜(SEM)等分析测试手段系统研究了样品浓度、DDA添加量、离子液体种类和微波反应时间对样品的结构和形貌的影响。研究表明采用微波加热5~15 min可以制备出六方纤锌矿结构的ZnO自主装微球。添加DDA使微球的组成单元由ZnO纳米棒向层状ZnO转化,微球尺寸也由0.4μm增大至1μm。此外,离子液体的种类对微球的形成也有极大的影响,[Bmim]Cl和[Bmim]Br可以分别获得层状和棒状ZnO组成的微球,相同实验条件下[Bmim]BF_4和[Bmim]PF_6则不利于微球的合成。随着反应时间的增长,微球的尺寸有所长大,室温下微球具有光致发光的性能。
Zinc oxide self-assembled microspheres were synthesized via imidazolium ionic liquid([Bmim]R,R=Cl,Br,BF_4, PF_6) assisted microwave method using Zn(NO_3)_2·6H_2O as raw material, Na OH as alkali source and nonionic surfactant dodecylamine(DDA) as dispersant, respectively. The effects of precursor concentration, DDA amount, ionic liquid species and reaction time on the phase and the morphology of the resulting products were investigated by X-ray diffraction(XRD) and scanning electron microscope(SEM), respectively. The experimental results show that the Zn O self-assembled microspheres with hexagonal wurtzite structure can be obtained through microwave treatment for 5 ~ 15 min. The addition of DDA promoted the building blocks of the microspheres changed from nanorods to nanolayers, and the diameter was increased from about 0.4 μm to 1 μm. Moreover, the ionic liquid species also have great influence on the morphology of the resulting products. The building blocks of microspheres were Zn O nanolayers and nanorods prepared by [Bmim]Cl and [Bmim]Br, respectively. In the same experimental conditions, [Bmim]BF_4 and [Bmim]PF_6 were not beneficial to the formation of Zn O microspheres. The size of the microspheres was increased with increasing the reaction times. The microspheres exhibit luminescent property at room temperature.