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过程工程学报 ›› 2024, Vol. 24 ›› Issue (8): 972-981.DOI: 10.12034/j.issn.1009-606X.223318

• 研究论文 • 上一篇    下一篇

KF-AlF3熔盐低温可视化电解NEU-1月壤仿真样

李承放1， 刘爱民1， 谢开钰1， 李得天2， 何成旦2， 王琎2， 王永军2， 石忠宁1*   

  1. 1. 东北大学多金属共生矿生态化冶金教育部重点实验室，辽宁 沈阳 110819 2. 兰州空间技术物理研究所真空技术与物理重点实验室，甘肃 兰州 730000
  • 收稿日期:2023-11-17 修回日期:2024-03-07 出版日期:2024-08-28 发布日期:2024-08-22
  • 通讯作者: 石忠宁 znshi@mail.neu.edu.cn
  • 基金资助:
    国家自然科学基金

Visualization electrolysis of NEU-1 lunar soil simulant in KF-AlF3 electrolyte at low-temperature

Chengfang LI1,  Aimin LIU1,  Kaiyu XIE1,  Detian LI2,  Chengdan HE2,  Jin WANG2, Yongjun WANG2,  Zhongning SHI1*   

  1. 1. Key Laboratory for Ecological Metallurgy of Multimetallic Mineral (Ministry of Education), Northeastern University, Shenyang, Liaoning 110819, China 2. Science and Technology on Vacuum Technology and Physics Laboratory, Lanzhou Institute of Physics, Lanzhou, Gansu 730000, China
  • Received:2023-11-17 Revised:2024-03-07 Online:2024-08-28 Published:2024-08-22

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摘要： 以57Fe-43Ni合金为惰性阳极、以镍网为阴极并用于盛装月壤仿真样，在650℃的43KF-57AlF3电解质体系中电解NEU-1月壤仿真样。利用透明槽可视化观察了电解过程中电极反应现象，并通过X-射线衍射(XRD)、能谱分析(EDS)和红外在线检测仪分别对电解质、阴极产物和阳极气体进行了表征。研究发现，在电解过程中电解质呈现三种不同颜色层，上层电解质为黄棕色，其冷凝后物相是KAlF4和Fe3O4；中层侧部为透明电解质，中心区域呈黑色，冷凝后物相为SiO2, NiO和Fe-Ni，在中层侧部还发现有少量Fe3O4和Al-Fe合金；下层呈蓝紫色，主要物相为Al, Al2O3和Fe-Ni-Si-Ti合金；阴极附近有小颗粒金属产物，阴极镍网外表面样品的主要成分为Fe (35.09wt%)，还含有少量的Ti (1.06wt%), Al (9.38wt%)和Si (3.62wt%)；电解过程中阳极底掌持续生成氧气，电解2 h后产生的气体中氧气的体积分数稳定在95vol%。

关键词: 月壤, 原位资源利用, 熔盐电解, 惰性阳极, 冰晶石

Abstract: Electrolysis of NEU-1 lunar regolith simulants was operated in 43KF-57AlF3 electrolyte at 650℃ in a quartz crucible. The Fe-Ni alloy was used as inert anode which consisted of 57Fe-43Ni and the cathode was made of nickel mesh with the lunar soil simulant in it. Electrode reaction phenomena during electrolysis were visualized using a see-through cell and electrolytes, cathode products and anode gas were characterized by X-ray Diffraction (XRD), Energy Display Spectrometer (EDS) and gas infrared on-line analyzer. The see-through cell was designed with a transparent quartz window in order to observe the phenomena during the electrolysis, It was found that different zones of the electrolyte showed different colors during the electrolysis. The electrolyte divided into three zones as the upper zone, the mid layer and the lower layer. Specifizally, in the upper zone, electrolyte appeared yellowish-brown, and its main phase were KAlF4 and Fe3O4 after condensation. The electrolyte in the mid-layer was transparent, while the center area was black, and the phases after condensation were SiO2, NiO, and Fe-Ni, along with small amount of Fe3O4 and Al-Fe alloy found in the side of mid-layer. The lower layer was bluish-purple metal fog with the predominant phases being Al, Al2O3, and Fe-Ni-Si-Ti alloy. The metal products were present in the form of fine particles located in the area close to the nickel mesh cathode. In the cathode nickel mesh, the main metal product was Fe (35.09wt%), with a small amount of Ti (1.06wt%), Al (9.38wt%), and Si (3.62wt%). It was found that gas bubbles were continuously generated at the bottom of the inert anode during the electrolysis in the see-through cell. Furthermore, an experiment was designed to collect the gas which generated by the electrolysis and detect the anode gas by using an on-line infrared gas analyzer. The result indicated that after 2 hours of electrolysis, the volume fraction of oxygen in the anode gas was stabilized at 95vol%.

Key words: lunar soil, in?situ resources utilization, molten salt electrolysis, inert anode, cryolite melts