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过程工程学报 ›› 2021, Vol. 21 ›› Issue (11): 1338-1345.DOI: 10.12034/j.issn.1009-606X.220355

• 材料工程 • 上一篇    下一篇

二氧化钼纳米棒的制备及电化学性能研究

高增礼1,2,3， 衣守志1*， 唐海燕2,3*， 徐红彬2,3,4   

  1. 1. 天津科技大学化工与材料学院，天津 300222 2. 中国科学院绿色过程与工程重点实验室(中国科学院过程工程研究所)，北京 100190 3. 中国科学院过程工程研究所湿法冶金清洁生产技术国家工程实验室，北京 100190 4. 中国科学院大学，北京 100049
  • 收稿日期:2020-11-03 修回日期:2021-01-04 出版日期:2021-11-28 发布日期:2021-11-29
  • 通讯作者: 唐海燕 hytang@ipe.ac.cn
  • 作者简介:高增礼(1994-)，男，河北省沧州市人，硕士研究生，化学工程专业，E-mail: 15122541555@163.com；通讯联系人，衣守志，E-mail: yshzh@tust.edu.cn；唐海燕，E-mail: hytang@ipe.ac.cn.
  • 基金资助:
    聚合物诱导辅助原位氢还原湿法制备纳米钼粉过程机理与调控方法

Preparation and electrochemical performance investigation of molybdenum dioxide nanorods

Zengli GAO1,2,3,  Shouzhi YI1*,  Haiyan TANG2,3*,  Hongbin XU2,3,4   

  1. 1. College of Chemical Engineering and Materials, Tianjin University of Science and Technology, Tianjin 300222, China 2. CAS Key Laboratory of Green Process and Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190, China 3. National Engineering Laboratory of Hydrometallurgy Cleaner Production Technology, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190, China 4. University of Chinese Academy of Sciences, Beijing 100049, China
  • Received:2020-11-03 Revised:2021-01-04 Online:2021-11-28 Published:2021-11-29

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摘要： MoO2纳米棒具有高电导率、高熔点及比容量较大，在超级电容器电极材料领域应用前景广泛。现有MoO2纳米棒制备方法大多存在操作复杂、收率低、成本高、易引入杂质等问题，且这些方法制备的MoO2产品存在形貌不均一、分散性差、电化学性能低的问题。基于此，本工作以双氧水和钼粉制备的过氧钼酸前驱体为钼源，PEG (8000)为模板剂制备出带状结构含钼杂化物，然后以浆态带状杂化物为原料采用两段式全湿法工艺制备纳米棒状MoO2。利用X射线衍射(XRD)、X射线光电子能谱(XPS)、X射线能谱(EDS)和扫描电子显微镜(SEM)等对二氧化钼纳米棒的物相、表面组成与形貌进行了分析，同时分别采用三电极和两电极体系研究了MoO2纳米棒的电化学电容行为，考察了MoO2纳米棒直接作为电极组装电容的性能。结果表明，所制的MoO2为长约500~800 nm、宽约100~200 nm的棒状结构，形貌与尺寸均匀，具有良好的分散性和较高的纯度。以MoO2纳米棒制备的电极在1 A/g的电流密度下，三电极和两电极体系所测得比电容分别为366.7和290.4 F/g；在5 A/g电流密度下循环充放电2000次后电容保持率均高于72%，展现出了良好的电化学性能。该研究结果可为纳米金属氧化物的制备提供新方法。

关键词: 二氧化钼, 纳米棒, 湿法, 制备, 电化学性能

Abstract: With high conductivity, high melting point and large specific capacity, molybdenum dioxide (MoO2) nanorods have a wide application prospect in the field of electrode materials for supercapacitors. Although there are many methods to prepare MoO2 nanorods, most of them have disadvantages of a complicated process, low yield, high production cost and easy to introduce impurities. Moreover, the prepared MoO2 products have the characteristics of non-uniform morphology, poor dispersibility and inferior electrochemical performances. In this work, the precursor of peroxymolybdic acid prepared by hydrogen peroxide and molybdenum powder was used as the source of molybdenum, and PEG (8000) was used as the template. The molybdenum-containing hybrid with a band structure was prepared by mixing the precursor and template with stirring and thermal insulation. The nano-rod-shaped MoO2 was prepared through a two-stage hydrometallurgical process using the hybrid compound as raw material. X-ray diffractometer (XRD), X-ray photoelectron spectrometer (XPS), X-ray energy spectrometer (EDS) and scanning electron microscope (SEM) were used to analyze the phase, surface composition and morphology of the obtained MoO2 nanorods. The electrochemical capacitance behavior of MoO2 nanorods was studied using a three-electrode system and two-electrode system, and the performance of MoO2 nanorods as electrode assembly capacitors was also investigated. The results showed that the prepared MoO2 had a rod-like structure with 500 to 800 nm in length and with 100 to 200 nm in width. The MoO2 had uniform morphology and size with good dispersion and high purity. The specific capacitance of MoO2 nanorods was 366.7 F/g for the three-electrode system at the current density of 1 A/g, and the specific capacitance for the two-electrode system was 290.4 F/g, and the capacitance retention rate was higher than 72% after 2000 cycles of charging and discharging at 5 A/g current density, both showing the good electrochemical performance of MoO2 nanorods. The research results of this study can provide a new method for the preparation of other nano metal oxides.

Key words: molybdenum dioxide, nanorods, hydrometallurgy, preparation, electrochemical performance