【作者】 吉宇杰；

【导师】 杨德仁；

【作者基本信息】 浙江大学 ， 材料物理与化学， 2004， 硕士

【摘要】 纳米科技是21世纪非常重要的、将对人类的生存和发展产生显著影响的科技领域。纳米结构无论从基础研究的角度来说，还是从性能与应用的角度来看，都有着特殊重要的意义，可以说纳米结构的合成和组装是整个纳米科技的基础。由于硫族化合物具有特殊的光电性质，因此研究其纳米结构的合成与组装具有十分重要的意义。 本文在传统水热和溶剂热方法的基础上，提出了巯基乙酸辅助水热合成新工艺技术，并用其成功合成了SnSx、PbS和CuS的各种纳米结构。同时利用X射线衍射、透射电镜、扫描电镜、拉曼光谱等测试手段对每一种结构进行了表征和分析。研究了温度、时间、硫源等各种因素对这些硫化物纳米结构及其物相的影响，从而得到了制备各种纳米结构硫化物的最佳条件。并且对于某些结构的形成机理进行了初步探讨。 实验表明，利用巯基乙酸辅助水热合成技术可以制备SnS₂纳米带、SnS₂叶片状结构和SnS薄片状结构。在SnSx纳米结构的制备过程中，锡硫配比、反应温度和硫源是影响产物纳米结构和物相的主要因素。当反应温度200℃和反应时间48小时保持不变时，锡硫摩尔比为1：4可以得到SnS₂纳米带；锡硫摩尔比为1：10则为SnS薄片状结构；而摩尔比低于1：4时，产物中还有SnO₂颗粒存在。若保持锡硫摩尔比为1：4，在160℃下反应24小时，得到的产物为SnS₂叶片状结构。 通过巯基乙酸辅助水热合成技术还可以制备PbS星状结构和PbS纳米棒。以醋酸铅和硫脲为先驱体，pH值大于10，在200℃下反应24小时，是制备PbS星状结构的最佳条件；改变硫源或体系pH值小于7时，所得产物均为PbS纳米颗粒。以硫酸铅和硫化钠为先驱体，在200V下反应24小时，是制备PbS纳米棒的最佳条件；当用其它可溶性铅盐取代硫酸铅为铅源时，产物都为PbS纳米颗粒。 通过巯基乙酸辅助水热合成技术，以硫代乙酰胺为硫源，可以制备CuS亚浙江大学硕士学位论文吉宇杰2004年3月微米空心球结构。扫描和透射电镜照片显示，这是一种由纳米颗粒组成的球状空心结构，X射线衍射和能谱分析表明该结构是由CuS晶体组成的。在制备CuS亚微米空心球结构过程中，硫源对所得产物的微观形貌和物相结构起着非常重要的作用。更多还原

【Abstract】 Nanotechnology will be a strategic branch of science and engineering for the next century, one that will dramatically impact on the health, wealth, and security of the world’s people. As the basis of the whole nanotechnology, nanostructures have significant effect on theories and applications. Also, owing to their distinguished optical and electronic properties, the synthesis of sulfide nanostructures has been a primary focus.In this paper, we reported a thioglycolic acid (TGA) assisted hydrothermal method to prepare sulfide nanostructures, such as SnSx, PbS and CuS. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Raman spectroscopy, and so on. The effects of reaction conditions including reaction temperature, time, and sulfur source on nanostructures and phase of the resulting products were studied. Furthermore, the mechanism of some sulfide structures was preliminary presented.Belt-like, leaf-like, and sheet-like SnSx (x=l,2) nanostructures were synthesized by thioglycolic acid assisted hydrothermal process using different ratio of sulfur and tin, temperature, and sulfur source. Keeping the temperature at 200 癈 for 48h, that the ratio of sulfur and tin was 1:4 could obtain the SnS2 nanobelts, and that the ratio was 1:10 could obtain the sheet-like SnS crystals. Moreover, using the ratio of 1:4 at 160C for 24h could obtain the leaf-like SnS2 nanostructures.Star-shaped and rod-like PbS nanostructures were also synthesized by thioglycolic acid assisted hydrothermal process. When using Pb(Ac)2 and thiourea as reactants, keeping pH value more than 10, the autoclave was maintained at 200C for 20h, the products were well crystallized star-shaped PbS nanostructures. Moreover, in our work, it was found that the PbS nanoparticles were formed by using other sulfursource or a pH value less than 7 in the hydrothermal method. When using PbSO4 and Na2S as reactants, the autoclave was maintained at 200C for 20h, the products were PbS nanorods.Using thioacetamide as sulfur source, CuS submicrometer hollow spheres consisting of nanoparticles were fabricated by thioglycolic acid assisted hydrothermal process. Furthermore, in this experiment, sulfur source played important role on the morphology and phase of products.更多还原