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化学液相共沉淀法制备ITO纳米粉体的工艺研究

Study on Process Nanosized ITO Powder Obtained by Chemical Liiquid Phase Coprecipitation

【作者】 魏坤

【导师】 黎铉海; 何超坤;

【作者基本信息】 广西大学 , 化学工艺, 2008, 硕士

【摘要】 氧化铟锡(ITO)是一种锡掺杂的半导体材料,铟消费量的80%以上用于铟锡氧化物透明电极。由ITO纳米粉体制成靶材,然后通过直流磁控溅射制成的ITO薄膜,是一种重掺杂、高简并的n型半导体,具有低电阻率、高可见光透射率和强烈反射红外光等一系列独特的光学电学性能,已广泛应用于电子计算机、能源、电子、光电、国防军事、航天航空、核工业和现代信息产业等高科技领域,在国民经济中的作用日趋重要。而获得高品质的ITO粉体是生产优质透明电极材料的关键。本论文以4N铟、锡锭为原料,以25%氨水为沉淀剂,采用点滴法滴加氨水的方式的化学液相共沉淀法来制备ITO纳米粉体。考察了反应初始铟浓度、反应温度、反应终点pH值和前驱体老化时间对ITO粉体粒径的影响。运用X射线衍射(XRD)、差热-热重分析(DTA-TG)、透射电镜(TEM)、场发射扫描电镜(SEM)、红外分析(FT-IR)等检测手段对粉体进行了表征。在液相中加入1%的硅酸钠,反应温度为60℃,反应终点pH值为8,老化制度为2h,煅烧制度为4h、800℃的工艺条件下,所制得的ITO纳米粉具有立方晶系结构,粉体粒径在20~40 nm之间,球形,颗粒均匀,且分散性能良好。该方法与以前的方法相比,原料来源简单,共沉淀工艺改善,反应条件更加温和,工艺设备简单,污染小,成本低,产品质量高,为ITO纳米粉体合成工艺开辟了一条新的工艺路线。

【Abstract】 Indium tin oxide (ITO) is a tin-doped semiconductor material. ITO material has consumed more than 80% of the indium produced over the world. ITO films are manufactured mostly by magnetron sputtering with an ITO ceramic as the target resource. ITO film is a heavily doped n-type semiconductor material. It shows a series of unique optical electrical properties, such as a low rate of resistance and high visible light transmission, and so on. It is widely used in computers, energy, electronics, optoelectronics, military defense, aerospace, nuclear industry, modern information industry and other high-tech fields. It plays an important role in the national economy. And preparing high-class ITO powder is crucial to produce high quality transparent electrode material.Based on 4 N indium and tin ingots, precipitation reagent ammonia (25% wt) added in drops, indium tin oxide (ITO) nanopowder synthesized by liquid chemical precipitation is studied. The effects of concentration of indium ion, reaction temperature, pH of reaction end and aging time of precursor on the size of ITO powder was investigated. It was characterized by X-ray diffraction (XRD), differential thermal analysis, thermogravimetric analysis (DTA-TG), transmission electron microscopy (TEM), field-emission scanning electron microscope(SEM), Infrared Spectrum(FT-IR) etc.. When the weight of added sodium silicate is 1%, the reaction temperature is 60℃, the pH value for the end of reaction is 8, aging time is 2 hour, calcining system is 4 hour and 800℃, ITO powder was prepared, which is a spherical, uniform particles, size in 20~40 nm, and it has cubic crystal structure and good dispersibility. Compared with previous methods, it exhibits advantages in simple source of raw materials, improvement in precipitation conditions and more moderate conditions, simple equipment, less pollution, low cost, high-quality products, and it studied a new process line of synthesis ITO nanopowder.

【关键词】 纳米ITO共沉淀法前驱体
【Key words】 nanometer powderindium tin oxide (ITO)precursorcorprecipitation
  • 【网络出版投稿人】 广西大学
  • 【网络出版年期】2009年 01期
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