铟、锡、锑多元金属氧化物的制备

【作者】 袁留芳；

【导师】 陈厚和；

【作者基本信息】 南京理工大学 ， 军事化学与烟火技术， 2010， 硕士

【摘要】 本文采用化学共沉淀法和溶液燃烧合成法制备铟、锡、锑多元金属氧化物。通过X-射线衍射分析(XRD)、扫描电镜(SEM)、透射电镜(TEM)对产物进行表征,分析其晶型结构、粒径以及形貌。研究表明：共沉淀法和溶液燃烧合成法都能制备出铟、锡、锑多元金属氧化物,原子都有相应的掺杂,而且掺杂并没有引入新的相,并且借鉴ATO/ITO的制备方法成功制备出了铟、锑二元金属氧化物和铟、锡、锑三元金属氧化物。以SnCl4、SbCl3、In(NO3)3和氨水为原料,利用共沉淀法制备了多元金属氧化物。并以ATO为例,系统地研究了不同反应条件如反应体系pH值、前驱体洗涤次数、前驱体煅烧温度对产物的晶型结构、粒径的影响。随着反应体系的pH值升高,ATO粉体的衍射峰变弱,pH=2时,其衍射峰强度最强；增加前驱体洗涤次数和降低煅烧温度都会使ATO粒径变小。而在溶液燃烧法中,以SnCl4、SbCl3、In(NO3)3、硝酸钠和尿素为原料,燃烧合成了铟、锡、锑多元金属氧化物。并以ATO为例,系统地研究了不同反应条件如Sb/Sn掺量比、煅烧温度、煅烧时间对产物的晶型结构、粒径、形貌的影响。随着Sb/Sn掺量比增大,ATO特征衍射峰变弱,但晶粒尺寸没有太大变化,由SEM和TEM可以看出粉体有团聚,并且颗粒呈不规则球形。但是原子比例和投入比例不一致,有偏析。随着锻烧温度的升高,粉体晶化完全,粒径变大,粉体颜色也变蓝。而煅烧时间和晶粒尺寸呈线性关系,并不改变其晶型结构。更多还原

【Abstract】 In this paper, The multi-metal oxide of indium、tin and antimony were prepared by the method of chemical co-precipitation and solution combustion synthesis. And the products were characterized by XRD、SEM and TEM, were analyzed the crystal structure, particle size and morphology.The results showed that:both of the co-precipitation and solution combustion synthesis can prepare he multi-metal oxide of indium、tin and antimony. The atoms had a corresponding doping, and the doping did not produce a new phase. Using the preparation of ATO/ITO for reference, the binary oxides of indium、antimony and the ternary metal oxide of indium、tin and antimony were successfully prepared.Using SnCl4, SbCl3, In (NO3) 3 and ammonia as raw materials, the multi-metal oxide of indium、tin and antimony were prepared by the method of co-precipitation.Taking ATO as an example, the influence of different reaction conditions such as reaction pH, the frequency of washing precursor, reaction temperature on the crystal structure, particle size were investigated. In the co-precipitation, the diffraction peaks of the ATO powders became weaker when the pH of reaction system increased. When the pH was 2, the intensity of diffraction peak was the strongest. The particle size of ATO powders became small when increasing the frequency of washing precursor and decreasing the temperature of calclination.Using SnCl4, SbCl3, In (NO3) 3、sodium nitrate and urea as raw materials, the multi-metal oxide of indium、tin and antimony were prepared by the method of solution combustion synthesis. Taking ATO as an example, the influence of different reaction conditions such as Sb/Sn ratio, temperature and time of calcination on the crystal structure, particle size and morphology were systemly studied. In the combustion synthesis solution, when the Sb/Sn ratio increased, the characteristic diffraction peaks became weaker but the grain size didn’t change much. The SEM and TEM showed that the ATO powders agglomerated and the particles were irregular spherical. However, the atomic ratio had segregation with the proportion of investment. As the calcination temperature increasing, the powder fully crystallized, the particle size became bigger and the powders became blue. While there existed linear relationship between the time of the calcination and the grain size, and the time did not change the crystalline structure.更多还原