反应时间对微波冷凝回流制备PbS纳米材料形貌的影响

Effect of reaction time on the morphology of PbS nanomaterial via microwave method equipped with reflux condenser

采用微波辐射法并借助冷凝回流装置,在表面活性剂十六烷基三甲基溴化铵的保护下,以二甲基亚砜为溶剂,三水合醋酸铅和硫脲分别作为铅源和硫源,成功地合成了星形结构的PbS.利用扫描电子显微镜、X射线衍射仪和PL荧光光谱仪,对所得PbS纳米产物的形貌、物相和光学性能进行分析表征.并通过研究不同加热反应时间对产物形貌和微观结构的影响,得到了快速制备星形结构PbS的最佳条件.结果表明,在反应时间为10min时,可制备得到具有星形结构的PbS纳米材料,并具有单色发光特性.此外,对PbS纳米产物的生长机理也作了进一步研究探讨.

In the paper, star shaped PbS nanomaterial was rapidly synthesized in the presence of surface-ac- tivator CTAB via microwave method equipped with reflux condenser by adding DMSO as solvent. The re- action materials were PbAc2 .3H2O as lead source and thiocarbamide as sulfur source. A series of analyti- cal methods including X-ray diffraction （XRD）, field emission scanning electron microscopy （SEM）, and fluorescence spectrometer were used to characterize the crystalline phase, microstructure, and optical properties of as-synthesized samples. Based on experimental results and optimization of synthesis proces- ses, the properties of products were further improved. The results indicate that the PbS nanoproducts have star shaped morphology when reaction time lasted 10 rain. In addition, the formation mechanism of PbS star-shaped nanostructure is further discussed by analyzing the reaction process and the results obtained in this study.