低共熔溶剂中直接电解Bi2O3/CNTs制备Bi/CNTs复合材料

doi:10.12068/j.issn.1005-3026.2024.11.006

东北大学学报（自然科学版） ›› 2024, Vol. 45 ›› Issue (11): 1565-1570.DOI: 10.12068/j.issn.1005-3026.2024.11.006

低共熔溶剂中直接电解Bi₂O₃/CNTs制备Bi/CNTs复合材料

薛伟健, 李敏(), 邓逸凡, 厉英

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

收稿日期:2023-07-04 出版日期:2024-11-15 发布日期:2025-02-24
通讯作者: 李敏
作者简介:薛伟健（1997-），男，山东潍坊人，东北大学硕士研究生
厉英（1963-），女，辽宁沈阳人，东北大学教授，博士生导师.
基金资助:
国家自然科学基金资助项目(51904068);中央高校基本科研业务费专项资金资助项目(N2325023);辽宁省自然科学基金资助项目(2023-MSBA-091)

Preparation of Bi/CNTs Composites by Direct Electrolysis of Bi₂O₃/CNTs in Deep Eutectic Solvent

Wei-jian XUE, Min LI(), Yi-fan DENG, Ying LI

Key Laboratory for Ecological Metallurgy of Multimetallic Mineral，Ministry of Education，Northeastern University，Shenyang 110819，China.

Received:2023-07-04 Online:2024-11-15 Published:2025-02-24
Contact: Min LI
About author:LI Min， E-mail： lim@smm.neu.edu.cn

摘要/Abstract

摘要：

针对低温下金属氧化物溶解度及溶解速率低的现状，以多孔固态Bi₂O₃/CNTs（碳纳米管）复合圆片作为阴极，石墨棒作为阳极，在氯化胆碱-乙二醇低共熔溶剂电解液中直接进行电解获得Bi/CNTs复合材料.采用循环伏安法研究了固态Bi₂O₃电还原过程的电化学行为，伏安曲线上只存在一对氧化还原峰，表明固态Bi₂O₃被电还原为Bi是一步还原反应.采用恒电压电解法研究了电解电压对固态Bi₂O₃电脱氧的影响，XRD与EDS结果表明，在80 ℃，2.6 V电解4 h，固态Bi₂O₃/CNTs被完全电还原为Bi/CNTs；SEM结果表明，电解电压越大，产物的颗粒越大，表面孔隙越疏松.本文结果可为低共熔溶剂直接电解金属氧化物制备金属提供一种简单且绿色的方法.

关键词: Bi₂O₃/CNTs, 低共熔溶剂, Bi/CNTs, 电化学还原

Abstract:

To address the low solubility and slow dissolution rate of metal oxides at low temperatures， a porous Bi₂O₃/CNTs （carbon nanotubes） composite pellet was used as the cathode， and a graphite rod served as the anode to obtain Bi/CNTs composites through direct electrolysis in a deep eutectic solvent electrolyte composed of choline chloride and ethylene glycol. The electrochemical behavior of the electroreduction process of solid Bi₂O₃ was investigated via cyclic voltammetry. A single pair of redox peaks was observed on the cyclic voltammogram， indicating that the electroreduction of solid Bi₂O₃ to Bi is a one?step reduction reaction. The effect of electrolysis voltage on the electro?deoxidation of Bi₂O₃ was studied through constant voltage electrolysis. XRD and EDS analyses confirmed that Bi₂O₃/CNTs were completely reduced to Bi/CNTs at 2.6 V and 80 ℃ with 4 hours. SEM results revealed that increasing the electrolysis voltage led to larger particle sizes and more porous surface structures in the final products. The study provides a simple and environmentally friendly method for preparing metals by direct electrolysis of metal oxides using deep eutectic solvents.

Key words: Bi₂O₃/CNTs, deep eutectic solvent, Bi/CNTs, electrochemical reduction

中图分类号:

TF 817

薛伟健, 李敏, 邓逸凡, 厉英. 低共熔溶剂中直接电解Bi₂O₃/CNTs制备Bi/CNTs复合材料[J]. 东北大学学报（自然科学版）, 2024, 45(11): 1565-1570.

Wei-jian XUE, Min LI, Yi-fan DENG, Ying LI. Preparation of Bi/CNTs Composites by Direct Electrolysis of Bi₂O₃/CNTs in Deep Eutectic Solvent[J]. Journal of Northeastern University(Natural Science), 2024, 45(11): 1565-1570.

图/表 7

图1 石墨腔电极在80 ℃的ChCl-EG DES中获得的线性扫描伏安曲线

Fig.1 Linear scan voltammogram of graphite cavity electrode in ChCl-EG DES at 80 ℃

图2 填充Bi2O3的石墨腔电极在80 ℃的ChCl-EG DES中获得的循环伏安曲线

Fig.2 Cyclic voltammogram of graphite cavity electrode filled with Bi2O3 in a ChCl-EG DES at 80 °C

图3 80 °C的ChCl-EG DES中固态Bi2O3/CNTs复合物在不同恒电压电解4 h获得的电流-时间曲线图

Fig.3 I-t plots of solid Bi2O3/CNTs complex recorded in a ChCl-EG DES at 80 °C under different constant voltages for 4 h

图4 原料与不同恒电压电解4 h获得产物的XRD图

Fig.4 XRD patterns of raw material and the electrolytic products obtained by electrolysis under different constant voltages for 4 h

图5 原料与不同恒电压电解4 h获得产物的SEM图像

Fig.5 SEM images of raw material and the electrolytic products obtained by electrolysis under different constant voltages for 4 h（a）—CNTs；（b）—Bi2O3/CNTs；（c）—B2O3/CNTs，放大；（d）—2.2 V；（e）—2.4 V；（f）—2.6 V.

图6 在80 ℃不同恒电压电解4 h获得产物的EDS

Fig.6 EDS of the electrolytic products obtained by electrolysis under different constant voltages for 4 h at 80 °C

图7 ChCl-EG DES中固态Bi2O3/CNTs复合物的电还原机理示意图

Fig.7 Schematic illustration of the electrochemical reduction mechanism for the solid Bi2O3/CNTs complex in a ChCl-EG DES

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低共熔溶剂中直接电解Bi₂O₃/CNTs制备Bi/CNTs复合材料

Preparation of Bi/CNTs Composites by Direct Electrolysis of Bi₂O₃/CNTs in Deep Eutectic Solvent

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