氧化锑锡（ATO）的制备及其性能的研究

发布时间：2018-06-18 08:57

本文选题：锑掺杂二氧化锡(ATO) + 液相法　；参考：《西南交通大学》2015年硕士论文

【摘要】：近年来,锑掺杂二氧化锡(ATO)作为透明导电氧化物材料,凭其化学稳定性,高电导率,浅色透明性等优良性质,在很多领域有着广泛的应用,是近年来飞速发展的种新型功能材料。目前制备ATO的方法较多,最为常用的为液相法,其制备工艺流程简单,过程易于控制且生产成本低,但需要在溶液中合成ATO颗粒。由于水的存在,金属离子不仅会水解,影响了ATO粉体的纯度,而且由于水的作用,颗粒会严重团聚,并且晶粒易长大。因此使用传统的液相法难以制备出粒径小、电阻低且分散性好的ATO粉体材料。此外,液相法中沉淀剂常用氨水有挥发性不易运输和存储,因而也限制了其应用。基于上述液相法制备ATO粉体的问题,本论文研究目的是探索优于传统液相法的非水相方法制备高性能的ATO材料。本论文采用了三种不同液相法制备ATO纳米导电颗粒,分别为扩散共沉淀法、溶剂热法、直接沉淀法。该三种方法均采用五水四氯化锡与三氯化锑为试剂原料,醇类溶液作为溶剂。并通过红外光谱分析、X射线衍射分析、扫描电镜分析、四探针电阻测试等方法表征了三种方法制备的ATO颗粒性能,从而对比选择出最佳制备方法,并深入研究其形成机制。由于水在溶剂中会严重影响ATO纳米导电颗粒的性能,本论文还讨论了水的含量对ATO材料的影响。还考察不同掺杂量对ATO粉体的粒径、电阻率及微观结构的影响,从而确定获得粒径小、电阻低的ATO材料的最佳掺杂量。实验结果显示,在三种方法中,扩散共沉淀法制备的ATO纳米颗粒导电性能、分散性能等都相对较好,用醇类溶液作为溶剂时,ATO前驱体主要以配位化合物的形式出现。通过煅烧,ATO前驱体中的结晶水、有机物蒸发和分解,最终得到ATO粉体。实验结果表明,ATO颗粒的电阻率和粒径都随着锑掺杂量的增加先减小后增加。溶剂中水的存在会引起金属离子的水解以及ATO纳米颗粒团聚和晶粒长大,从而不利于制备粒径小、电阻低的ATO颗粒。本论文采用的三种方法都能成功将锑完全掺杂进入二氧化锡晶格中,且经过煅烧后的ATO仍是单一固溶体。扩散共沉淀法制备的ATO纳米导电颗粒最高电导率为26.67 s.cm-1,颗粒平均粒径在5-10nnm,直接沉淀法制备的ATO颗粒最高产率可达88%以上。本研究将为制备粒径小、电阻低和颗粒分散的ATO粉体提供了工艺简单、生产效率高、生产成本低的新途径。
[Abstract]:In recent years, antimony doped tin dioxide (ATO), as a transparent conductive oxide material, has been widely used in many fields because of its excellent properties such as chemical stability, high conductivity, light color transparency, etc. It is a new functional material developed rapidly in recent years. At present, there are many methods to prepare ATO, the most commonly used method is liquid phase method. Its preparation process is simple, the process is easy to control and the production cost is low, but it is necessary to synthesize ATO particles in solution. Because of the existence of water, the metal ions not only hydrolyze, which affect the purity of ATO powder, but also the particles will be agglomerated seriously and the grain will grow up easily because of the effect of water. Therefore, it is difficult to produce ATO powder with small particle size, low resistance and good dispersion by traditional liquid phase method. In addition, ammonia, a common precipitator in liquid phase, is volatile and difficult to transport and store, thus limiting its application. Based on the problem of preparing ATO powder by liquid phase method mentioned above, the purpose of this paper is to explore the preparation of high performance ATO materials by non-aqueous phase method which is superior to the traditional liquid phase method. In this paper, ATO nanoparticles were prepared by three different liquid phase methods: diffusion co-precipitation method, solvothermal method and direct precipitation method. All the three methods used stannous chloride pentahydrate and antimony trichloride as raw materials and alcohol solution as solvent. The properties of ATO particles prepared by the three methods were characterized by X-ray diffraction analysis, scanning electron microscope analysis and four-probe resistance test. The optimum preparation methods were compared and the formation mechanism of ATO particles was studied. The effect of water content on the properties of ATO nanoparticles was also discussed. The effects of different doping amount on the particle size, resistivity and microstructure of ATO powder were also investigated, and the optimum doping amount of ATO material with small particle size and low resistance was determined. The experimental results show that the conductivity and dispersion of ATO nanoparticles prepared by diffusion coprecipitation method are relatively good. When alcohol solution is used as solvent, the precursor of ATO mainly appears in the form of coordination compound. The ATO powder was obtained by calcining the crystal water in the precursor of ATO, evaporation and decomposition of organic matter. The experimental results show that the resistivity and particle size of ATO particles decrease firstly and then increase with the increase of antimony doping content. The presence of water in the solvent will lead to the hydrolysis of metal ions, the agglomeration of ATO nanoparticles and grain growth, which is not conducive to the preparation of ATO particles with small particle size and low resistance. The three methods used in this paper successfully doped antimony into tin dioxide lattice, and the calcined ATO is still a single solid solution. The maximum conductivity of ATO nanoparticles prepared by diffusion coprecipitation method is 26.67 s 路cm ~ (-1), the average particle size is 5-10 nm 路m ~ (-1), and the highest yield of ATO nanoparticles prepared by direct precipitation method is over 88%. This study will provide a new way for the preparation of ATO powders with small particle size, low resistance and dispersed particle size, high production efficiency and low production cost.
【学位授予单位】：西南交通大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ134.32

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