二硫化钼纳米结构制备和表征研究

发布时间：2018-02-26 03:06

本文关键词： 二硫化钼纳米结构水热法光催化　出处：《中国计量学院》2015年硕士论文　论文类型：学位论文

【摘要】：从上世纪90时代开始,由于纳米科技以及纳米材料研究的飞速发展,世界许多国家争相研究和开发纳米材料的应用,努力使得其产业化的形成,如今,纳米技术已经和信息技术以及生物技术一般,成为当今社会经济发展的重要技术之一和战略制高点。二硫化钼作为作为新型的纳米材料,在催化剂、固体润滑剂、锂电池、储氢、析氢、光电学等方面有着巨大的应用前景,被人们广泛的研究。无机纳米材料的性能和其尺寸大小以及形貌息息相关,制备和研究不同形貌(纳米花、纳米棒、纳米微球等等)的二硫化钼有着极其重要的意义。本文用水热法成功制备多种纳米形态的二硫化钼,在实验过程中实现了对二硫化钼纳米结构和尺寸的控制,并研究了不同结构和尺寸的纳米二硫化钼对光催化性能的重要影响,主要工作如下：1.钼酸钠和硫代乙酰胺作为原材料,硅钨酸作为添加剂,成功用水热法制备出高纯度纳米花状二硫化钼。经过XRD、SEM、EDS等手段进行表征之后,证明产物确实为二硫化钼,并且该二硫化钼形状为纳米花状,颗粒的直径约为300纳米,由几十上百片纳米花瓣构成,每一片花瓣的厚度约为十个纳米；实验表明,硅钨酸的剂量对合成MoS2的大小和形貌有着重大的影响,初步阐述了二硫化钼纳米花状的形成机理。2.水热法合成二硫化钼纳米棒。实验用棒状三氧化钼和Na2S·9H2O在酸性条件下合成二硫化钼纳米棒,其中,三氧化钼是用钼酸钠、盐酸制备而成的棒状结构。产物用XRD、SEM手段进行表征,证明产物确实为棒状二硫化钼。研究了反应时间对实验的影响,初步讨论了二硫化钼纳米棒的形成机理。3.钼酸铵、盐酸羟胺、Na2S·9H2O为前驱体,水热合成球状纳米二硫化钼。产物运用XRD和SEM手段进行表征,证明实验制备出的物质确实是二硫化钼,并研究了PH值以及反应温度对于实验产物的最终结构和尺寸的影响。4.用实验制备的三种不同形貌的二硫化钼进行甲基橙的光催化降解实验。经过多次重复实验,得出光催化效率最高的为纳米花状二硫化钼,同时对催化剂剂量、PH、光照方式和甲基橙浓度等对光催化有重要影响的因素进行了研究。为二硫化钼大规模工业化处理污染提供了依据。
[Abstract]:Since the 1990s in 0th century, due to the rapid development of nanotechnology and nanomaterials research, many countries all over the world are scrambling to research and develop the application of nanomaterials, and strive to make their industrialization come into being. Nanotechnology, like information technology and biotechnology, has become one of the most important technologies and strategic commanding points in social and economic development. Molybdenum disulfide as a new nano-material, in catalyst, solid lubricant, lithium battery, Hydrogen storage, hydrogen evolution, photoelectricity and so on have great application prospects, and have been widely studied. The properties of inorganic nanomaterials are closely related to the size and morphology of inorganic nanomaterials, the preparation and study of different morphologies (nanorods, nanorods, nanorods, nanorods, etc.). Molybdenum disulfide (molybdenum disulfide) is of great significance. In this paper, molybdenum disulfide nanoparticles have been successfully prepared by hydrothermal method, and the size and structure of molybdenum disulfide nanostructures have been controlled. The important effect of nano-molybdenum disulfide with different structure and size on photocatalytic performance was studied. The main work is as follows: 1. Sodium molybdate and thioacetamide as raw materials, silicotungstic acid as additives, High purity nanocrystalline molybdenum disulfide was prepared by hydrothermal method. It was proved that the product was molybdenum disulfide, and the shape of molybdenum disulfide was nanometer, and the diameter of the particle was about 300 nm. It consists of dozens of hundreds of nano-petals, each of which is about ten nanometers thick. Experiments show that the dosage of silicotungstic acid has a significant effect on the size and morphology of MoS2 synthesis. The formation mechanism of molybdenum disulfide nanoscale flowerlike was described. 2. Molybdenum disulfide nanorods were synthesized by hydrothermal method. Molybdenum disulfide nanorods were synthesized by rod-like molybdenum trioxide and Na2S 路9H2O under acidic conditions, among which molybdenum trioxide was prepared by sodium molybdate. The rod-like structure prepared by hydrochloric acid was characterized by XRDX SEM, and it was proved that the product was rod-like molybdenum disulfide. The influence of reaction time on the experiment was studied, and the formation mechanism of molybdenum disulfide nanorods was discussed preliminarily. Hydroxylamine hydrochloride Na _ 2S 路9H _ 2O was used as precursor for hydrothermal synthesis of spherical nano-molybdenum disulfide. The product was characterized by XRD and SEM. The effects of PH value and reaction temperature on the final structure and size of the product were studied. 4. Photocatalytic degradation of methyl orange with three molybdenum disulfide (molybdenum disulfide) with different morphologies was studied. The highest photocatalytic efficiency of molybdenum disulfide nanoparticles was obtained. At the same time, the factors which have important influence on photocatalysis, such as catalyst dosage, light mode and methyl orange concentration, have been studied, which provides the basis for large-scale industrial treatment of pollution by molybdenum disulfide.
【学位授予单位】：中国计量学院
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TB383.1;TQ136.12

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