化学液相共沉淀法制备ITO纳米粉体的工艺研究
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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。
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.
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。
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.
引文
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[2]Liu J X,Gan Y,Zeng S N.Indium tin oxide nanosized composite powder prepared using waste ITO target[J].RARE METALS,2005,24(3):277-282
[3]李锦桥.ITO耙材的发展现状[J].新材料产业,2000,(12):35-36
[4]李万青.大厂矿田铟资源的保护和利用[J].世界有色金属,2001,(10):33-36
[5]烘托,秦得先,刘方成,等.铟市场形势及中国铟资源特点[J].云南地理环境研究,2004.16:27-31
[6]邹家炎.铟的提取、应用和新产品开发[J].广东有色金属学报,2002,12(9):16-20
[7]侬健桃.我国铟产业现状及发展[J].有色冶金,2002,(4):12-14
[8]黄小珂.广西铟工业发展浅论[J].有色金属,2003,55(1):140-145
[9]刘大春,杨斌,戴永年,等.云南省铟资源及其产业发展[J].广东有色金属学报,2005,15(1):1-3
[10]冯君从.铟价涨到1000美元/千克不是梦[J].中国通报,2005,(4):14
[11]陈薇,徐柳苏,李东,等.我国纳米铟的研究现状[J].沿海企业与科技,2005,2:129
[12]马勇,孔春阳.ITO薄膜的光学和电学性质及其应用[J].重庆大学学报(自然科学版),2002,25(8):114-117
[13]刁庚秀,陈文彬.ITO薄膜的溶胶-凝胶法制备,光电子技术,2004,24(12):249-253.
[14]王树林,夏冬林.ITO薄膜的制备工艺及进展[J].玻璃与搪瓷,2004,32(5):51-54
[15]袭著有,许启明,赵鹏,等.ITO薄膜特性及发展方向[J].西安建筑科技大学学报(自然科学版),2004,36(1):109-112
[16]陈世柱,李晶.溶胶-凝胶提拉法制备ITO透明导电膜[J].中国有色金属学报,2005,15(1):94-99
[17]史月艳,潘文辉,殷志强。氧化铟锡(ITO)膜的光学及电学性能[J].真空科学与技术,1994,14(1):35-40
[18]Zhu F R,Zhang K R,Guenther E,et al.Optimized indium tin oxide contact for organic light emitting[J].Thin Solid Films,2000,(363):314-317
[19]Lu H T,Yokoyama M.Plasma preparation on indium-tin-oxide anode surface for rganic light emitting diodes[J].Journal of Crystal Growth,2004,(260):186-190
[20]Bosscher W D,Dellaert K,Luys S,et al.液晶显示用玻璃的ITO镀层[J].现代显示,2006,(67):9-12
[21]于汉芹.ITO超细粉末的研制[J].有色矿冶,2000,16(1):35-38
[22]赖复兴,刘志勇,王红军,等.ITO废耙回收制备超细ITO粉末的研究[J].稀有金属快报,2005,24(2):27-29
[23]宋伟明,周惠良,胡奇林,等.铟锡氧化物纳米晶的溶胶凝胶法合成[J].宁夏大学学报(自然科学版),2000,21(4):339-341
[24]张贤高,贺平,贾志杰,等.ITO纳米粉的低温制备[J].电子元件与材料,2004,23(6):44-45
[25]周洪庆,吕军华,沈晓冬.ITO纳米粉制备及表面修饰研究[J].南京工业大学学报2004,26(4):28-30
[26]段学臣,陈振华,周立,等.超细氧化铟-氧化锡(ITO)复合粉末的研制与结构特性[J).稀有金属,1998,22(5):396-399
[27]刘雪颖,古映莹.共沉淀法制备纳米ITO粉末[J].广州化工,2005,33(1):31-45
[28]张艳峰,张久兴.化学共沉淀法制备纳米.ITO粉体及结构表征[J].功能材料,2003,34(5):573-574
[29]吕志伟,陈志飞,姚吉升.纳米ITO粉体的制备及应用[J].有色矿冶,2003,19(5):40-42
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