高等学校化学学报 ›› 2017, Vol. 38 ›› Issue (7): 1110-1116.doi: 10.7503/cjcu20170046

• 研究论文: 无机化学 • 上一篇    下一篇

立方形貌ITO粉体的水热法制备及光电性能

张怡青, 刘家祥()   

  1. 北京化工大学, 材料电化学过程与技术北京市重点实验室,化工资源有效利用国家重点实验室, 北京 100029
  • 收稿日期:2017-01-18 出版日期:2017-07-10 发布日期:2017-06-20
  • 作者简介:联系人简介: 刘家祥, 男, 博士, 教授, 主要从事无机功能材料和固体废弃物利用研究. E-mail: ljxpost@263.net
  • 基金资助:
    北京市自然科学基金(批准号: 2142025)资助

Hydrothermal Preparation of Cubic ITO Powder and Its Photoelectric Performance

ZHANG Yiqing, LIU Jiaxiang*()   

  1. Beijing Key Laboratory of Electrochemical Process and Technology for Materials, State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, China
  • Received:2017-01-18 Online:2017-07-10 Published:2017-06-20
  • Contact: LIU Jiaxiang E-mail:ljxpost@263.net
  • Supported by:
    † Supported by the Natural Science Foundation of Beijing, China(No.2142025)

摘要:

以金属In和SnCl4·5H2O为原料, 采用水热法在120~140 ℃得到In(OH)3前驱体, 该前驱体在550 ℃下煅烧得到立方体形貌的氧化铟锡粉体. 研究了水热反应温度和反应时间对粉体形貌和晶型的影响. 通过热分析仪(TG-DSC)、 X射线衍射仪(XRD)、 拉曼光谱仪(Raman)、 透射电子显微镜(TEM)、 四探针电阻仪、 X射线光电子能谱仪(XPS)、 紫外-可见-近红外分光光度计以及荧光光谱仪对粉体进行了表征, 并对水热反应条件为140 ℃及12 h下制备的c-ITO的光电性能进行了分析. 结果表明, 随着水热反应温度的升高, ITO粉体形貌由立方体向不规则形貌转变, 粉体晶型出现少量的六方相. 在水热反应条件为140 ℃, 12 h, 铟离子与尿素的摩尔比为1∶5 时, 得到平均粒径为230 nm的立方体ITO粉体, 其电阻率为1.247 Ω·cm, 光学能带间隙为3.685 eV, 与c-In2O3相比其能带间隙更高, 室温下260 nm激发波长下粉体出现光致发光, 发射峰位于蓝光区域.

关键词: 立方体形貌氧化铟锡, 水热法, 光电性能

Abstract:

Cubic indium tin oxide(c-ITO) nanopowders were prepared by hydrothermal method under 120—140 ℃ to get the precursor and calcination at 550 ℃, using metal In and SnCl4·5H2O as the raw materials. The hydrothermal temperature and the reaction time influenced the morphology and the crystal structure of the ITO powders. The photoelectric performance of the c-ITO prepared under 140 ℃ for 12 h was analyzed. The ITO powders were also characterized by means of thermogravimetric-differential scanning calorimetry(TG-DSC) analysis, X-ray diffraction(XRD), Raman spectroscopy, transmission electron microscopy(SEM), four point probe resistance measurement, X-ray photoelectron spectroscopy(XPS) and UV-Vis spectrophotometry(UV-Vis). The results show that with the increase of hydrothermal temperature, ITO powders’ morphology changed from cubic to irregular shape, and a small amount of hexagonal phase crystal appeared. The average size of the c-ITO prepared after hydrothermal treatment at 140 ℃ for 12 h with n(In3+)∶n[CO(NH2)2]=1∶5 was 230 nm, and the c-ITO showed a better electrical performance with a low resistivity of 1.247 Ω·cm. Compared with c-In2O3, c-ITO has a higher optical band gap of 3.685 eV. The PL spectrum of c-ITO excitated with 260 nm wavelength was in blue light region.

Key words: Cubic indium tin oxide, Hydrothermal method, Photoelectric property

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