静电纺丝法制备纳米氧化铟锡及其导电性能
Fabrication of Indium Tin Oxide Nanostructures by Electrospinning and Their Electrical Conductivity
作者单位E-mail
任鑫川 东南大学化学化工学院, 南京 211189  
刘苏婷 东南大学化学化工学院, 南京 211189  
李志慧 东南大学化学化工学院, 南京 211189  
宋承堃 东南大学化学化工学院, 南京 211189  
代云茜 东南大学化学化工学院, 南京 211189 daiy@seu.edu.cn 
孙岳明 东南大学化学化工学院, 南京 211189 sun@seu.edu.cn 
摘要: 采用静电纺丝-溶胶凝胶法,以SnCl2、InCl3、聚乙烯吡咯烷酮(PVP)等为原料,乙醇胺为水解控制剂,合成了超细氧化铟锡(ITO)纳米纤维及富氧缺陷的ITO纳米颗粒。采用透射电子显微镜(TEM)、选区电子衍射(SAED)、扫描电子显微镜(SEM)、热重分析(TGA)、X射线衍射(XRD)、X射线电子能谱(XPS)、四探针电阻仪,系统研究了超细ITO纤维及颗粒的形貌、晶型、氧缺陷及导电性能。在400℃空气煅烧后,纤维中的PVP高分子骨架发生热分解,获得超细、多孔ITO纳米纤维,晶型为立方相。进一步升高煅烧温度至800℃,ITO纳米纤维转变为富氧缺陷的纳米颗粒,晶格氧空位含量高达38.9%。随着煅烧温度升高,Sn4+掺入到In2O3晶格中,发生晶格膨胀,晶面间距增大。煅烧温度由400℃升高至800℃,未发生立方相向六方相的转变,晶型稳定,晶粒尺寸从32 nm生长到44 nm,晶格应变(ε0)从1.42×10-2减小至1.04×10-2,应变诱导的晶格弛豫逐渐减小。此外,高温煅烧可抑制In2O3晶粒(111)晶面的增长,随着In2O3的(400)与(222)晶面比值(I(400)/I(222))的增加,ITO电导率逐渐升高。在800℃获得的ITO纳米晶粒导电率最高。
关键词: 纳米结构  氧化铟锡  氧空位  导电材料
基金项目: 中央高校基本业务费(No.3207042009C2)资助
Abstract: Indium tin oxide (ITO) nanofibers and ITO nanoparticles with enriched oxygen-defects were synthesized through facile electrospinning and sol-gel method. SnCl2, InCl3, and PVP (polyvinylpyrrolidone) were selected as precursors, while ethanolamine was employed as a hydrolysis controlling agent. The morphology, crystal structure, oxygen defects, and electrical performance of the ultrafine ITO nanofibers and nanoparticles were systematically characterized by transmission electron microscope (TEM), selection electron diffraction (SAED), scanning electron microscope (SEM), thermogravimetric analysis (TGA), X-ray diffraction (XRD), X-ray electron spectroscopy (XPS), and four point resistance tester. The ITO nanofibers were obtained by removal of the PVP matrix at 400℃, and fea-tured with ultrafine diameter, porous structure, and cubic phase. Furthermore, the resultant ITO nanofibers changed to oxygen-deficient nanoparticles with a high oxygen vacancy content of 38.9% at 800℃. The doping of Sn4+ ions into the In2O3 lattices leads to the expansion of the lattice and thus the increase of crystal plane spacing at elevated temperatures. When the temperature increased from 400 to 800℃, the size of ITO nanoparticles grown from 32 to 44 nm. Meanwhile, the lattice strain (ε0) decreased from 1.42×10-2 to 1.04×10-2 and the strain-induced lattice relax-ation decreased accordingly. No phase change from cubic structure to hexagonal structure was observed. Additionally, calcination at elevated temperature could hamper the (111) growth and thus cause the increase in the ratio of I(400)/I(222) in In2O3 that is proportional to the electrical conductivity of ITO. The maximized electrical conductivity of ITO nanoparticles was obtained upon a calcination temperature of 800℃.
Keywords: nanostructures  indium tin oxide  oxygen vacancy  conducting material
投稿时间:2020-10-06 修订日期:2020-11-13
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任鑫川,刘苏婷,李志慧,宋承堃,代云茜,孙岳明.静电纺丝法制备纳米氧化铟锡及其导电性能[J].无机化学学报,2013,29(18):.
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