微流体沉淀剂法制备铟锡氧化物纳米粉体及其表征  

Preparation and Characterization of Indium Tin Oxide Nano Powders Prepared by Microfluidic Precipitation Method

作　　者：夏先禹 杨四齐 张利华 白希为[1,2] 姚浩 XIA Xianyu;YANG Siqi;ZHANG Lihua;BAI Xiwei;YAO Hao(Key Laboratory of Unconventional Metallurgy,Ministry of Education,Kunming University of Science and Technology,Kunming 650093,China;Faculty of Metallurgical and Energy Engineering,Kunming University of Science and Technology,Kunming 650093,China;State Key Laboratory of Complex Non-ferrous Metal Resources Clean Utilization,Kunming University of Science and Technology,Kunming 650093,China)

机构地区：[1]昆明理工大学非常规冶金教育部重点实验室,昆明650093 [2]昆明理工大学冶金与能源工程学院,昆明650093 [3]昆明理工大学省部共建复杂有色金属资源清洁利用国家重点实验室,昆明650093

出　　处：《有色金属工程》2023年第10期16-21,共6页Nonferrous Metals Engineering

基　　金：国家自然科学基金资助项目(52164040);云南省基础研究计划面上项目(202101AT070121);“兴滇英才支持计划”青年人才项目(YNWR-QNBJ-2019-150)。

摘　　要：采用微流体沉淀法,以InCl_(3)·4H_(2)O和SnCl_(4)·5H_(2)O作为原料、NH_(3)·H_(2)O和Na_(2)CO_(3)分别作为沉淀剂,在毛细管微反应器中成功制备出铟锡氧化物(ITO)纳米粉体。利用X射线衍射(XRD)和透射电子显微镜(TEM)对其物相和形貌进行分析,并测量其粒径尺寸和分布,通过选区电子衍射(SAED)确定晶体结构,利用傅里叶变化红外光谱仪(FT-IR)和四探针方阻电阻率测量仪对其光电性能进行表征。结果表明,前驱体在650℃下煅烧2 h可以得到良好结晶度和立方体的纯净ITO纳米粉体,均为分散性良好、粒径分布窄的椭球形多晶晶体。与Na_(2)CO_(3)作为沉淀剂相比,NH_(3)·H_(2)O制备得到的ITO纳米粉体粒径更小、分布更均匀,因此具有更为优异的光电性能,对红外光的透过率及电阻率值分别为0.31%和(1.56±0.19)Ω·cm,而Na_(2)CO_(3)条件下分别为0.81%和(5.79±0.33)Ω·cm。Indium-tin oxide(ITO)nano powders were successfully prepared in a capillary microreactor via microfluidic precipitation method with InCl_(3)·4H_(2)O and SnCl_(4)·5H_(2)O as raw materials and NH_(3)·H_(2)O and Na_(2)CO_(3)as precipitants,respectively.The crystal structure and morphology were characterized by X-Ray Diffraction(XRD)and Transmission Electron Microscopy(TEM),and the particle size distribution were measured.The crystal structure was determined by Selected Area Electron Diffraction(SAED),and the photoelectric properties were characterized by Fourier Transform Infrared Spectroscopy(FT-IR)and four-probe square resistance resistivity measurement,respectively.The results showed that the precursors could be calcined at 650℃for_(2)h to obtain pure ITO nano powders with good crystallinity and cubic structure,all of which were ellipsoidal polycrystalline crystals with good dispersion and narrow particle size distribution.Compared with Na_(2)CO_(3)as the precipitant,the ITO nano powders prepared by NH_(3)·H_(2)O had smaller particle size and more uniform size distribution,and thus had more excellent optoelectronic properties,and its transmittance and resistivity values for infrared light were 0.31%and(1.56±0.19)Ω·cm,respectively,compared with 0.81%and(5.79±0.33)Ω·cm under Na_(2)CO_(3)conditions.

关 键 词：铟锡氧化物 纳米粉体 微反应器 微流体沉淀 光电性能 

分 类 号：TB383[一般工业技术—材料科学与工程] O614.37[理学—无机化学]