高等学校化学学报 ›› 2015, Vol. 36 ›› Issue (3): 436-441.doi: 10.7503/cjcu20140670

• 研究论文: 无机化学 • 上一篇    下一篇

β-MnO2α-Mn2O3纳米棒的自牺牲模板法制备、 表征和应用

赵红远, 刘兴泉(), 张峥, 吴玥, 杨光, 陈炳, 熊伟强   

  1. 电子科技大学微电子与固体电子学院, 电子薄膜与集成器件国家重点实验室, 成都 610054
  • 收稿日期:2014-07-18 出版日期:2015-03-10 发布日期:2015-02-04
  • 作者简介:联系人简介: 刘兴泉, 男, 博士, 教授, 博士生导师, 主要从事新能源材料与集成能源器件研究. E-mail: Lxquan@uestc.edu.cn
  • 基金资助:
    国家自然科学基金(批准号: 21071026)和电子科技大学杰出人才引进项目(批准号: 08JC00303)资助

Preparation of β-MnO2 and α-Mn2O3 Nanorods via a Self-sacrificing Template Route and Their Characterization and Application

ZHAO Hongyuan, LIU Xingquan*(), ZHANG Zheng, WU Yue, YANG Guang, CHEN Bing, XIONG Weiqiang   

  1. State Key Laboratory of Electronic Thin Film and Integrated Devices, School of Microelectronics and Solid State Electronics,University of Electronic Science and Technology of China, Chengdu 610054, China
  • Received:2014-07-18 Online:2015-03-10 Published:2015-02-04
  • Contact: LIU Xingquan E-mail:Lxquan@uestc.edu.cn
  • Supported by:
    † Supported by the National Natural Science Foundation of China(No.21071026) and the Outstanding Talent Introduction Project of University of Electronic Science and Technology, China(No.08JC00303)

摘要:

在150 ℃下, 仅以高锰酸钾溶液和无水乙醇为原料, 通过水热反应合成前驱体γ-MnOOH纳米棒. 以γ-MnOOH纳米棒为自牺牲模板, 分别在350和600 ℃下煅烧90 min, 制备出高纯度的β-MnO2α-Mn2O3纳米棒. 采用X射线粉末衍射(XRD)、 扫描电子显微镜(SEM)及热重分析(TGA)等对所制备的样品进行表征. 结果表明, 前驱物γ-MnOOH为高纯度的纳米棒状晶体, 直径约100~300 nm, 长度可达数微米, 且终产物β-MnO2α-Mn2O3均具有较高的纯度, 也很好地保持了前驱物的纳米棒状结构. 以二者为锰源, 通过固相反应合成出尖晶石LiMn2O4正极材料. 当充放电倍率为0.5 C时, 其首次放电比容量分别可达到120.4和123.9 mA·h/g, 而且表现出良好的循环性能和倍率性能.

关键词: β-MnO2, α-Mn2O3, 纳米棒, 自牺牲模板法

Abstract:

Pure-phased γ-MnOOH nanorods were synthesized at 150 ℃ for 20 h through a hydrothermal reaction process, during which KMnO4 was reduced by CH3CH2OH under autogeneror pressure. With γ-MnOOH nanorods as self-sacrificing template, β-MnO2 and α-Mn2O3 nanorods were prepared by calcining at 350 and 600 ℃ for 90 min, respectively. The materials were characterized by X-ray diffraction(XRD), scanning electron microscopy(SEM) and thermal-gravimetric analysis(TGA). The results showed that γ-MnOOH nanorods had good crystallographic quality and the diameters were about 100—300 nm, the length could be as long as several micrometers. The morphology and microstructure were well reserved in β-MnO2 and α-Mn2O3 products and no other morphology of impurities was observed. With β-MnO2 and α-Mn2O3 nanorods as manganese sources, spinel LiMn2O4 samples were prepared by solid state method. At the charge/discharge rate of 0.5 C, the LiMn2O4 samples could deliver the initial discharge capacities of 120.4 and 123.9 mA·h/g, respectively, and present good cycling stability and rate performance.

Key words: β-MnO2, α-Mn2O3, Nanorod, Self-sacrificing template route

中图分类号: