低共熔溶剂电解固态Sb2S3/CNTs制备Sb/CNTs的研究

doi:10.12068/j.issn.1005-3026.2025.20230283

摘要/Abstract

摘要：

以固态Sb₂S₃/碳纳米管（carbon nanotubes，CNTs）为阴极，石墨为阳极，在氯化胆碱-乙二醇低共熔溶剂中直接电解制备Sb/CNTs.采用循环伏安法研究了固态Sb₂S₃的电化学还原行为，并系统研究了电解电压、电解时间及温度对固态Sb₂S₃电脱硫的影响.循环伏安法结果表明，低共熔溶剂中固态Sb₂S₃可被直接电化学还原为金属Sb且固态Sb₂S₃被电化学还原为金属Sb的反应是一步还原过程.XRD，EDS结果表明，电解电压越大，电解时间越长，固态Sb₂S₃的电脱硫越彻底.353 K温度下2.4 V电压电解6 h后固态Sb₂S₃/CNTs可被完全电化学还原为Sb/CNTs.SEM结果表明，电解电压越大，电解产物颗粒越小，表面孔隙越大.所得结果可为低温甚至室温直接电化学还原固态硫化物制备金属提供一种新路径.

关键词: 低共熔溶剂（DES）, 硫化锑, 锑, 电化学还原

Abstract:

Sb/CNTs（carbon nanotubes） nanotubes were prepared by electrolysis in choline chloride-ethylene glycol eutectic solvent using solid Sb₂S₃/CNTs as cathode and graphite as anode. The electrochemical reduction behavior of solid Sb₂S₃ was studied by cyclic voltammetry and the effects of electrolysis voltage， electrolysis time and temperature on the electro-desulfurization of solid-state Sb₂S₃ were systematically investigated. The cyclic voltammetry results show that solid-state Sb₂S₃ can be directly electrochemically reduced metallic Sb in the deep eutectic solvent， and the electrochemical reduction of solid-state Sb₂S₃ to metallic Sb is a one-step reduction process. The XRD and EDS results indicate that increasing the electrolysis voltage and extending the electrolysis time lead to more comprehensive electro-desulfurization of solid-state Sb₂S₃. After electrolysis at a voltage of 2.4 V for 6 h at 353 K， solid-state Sb₂S₃/CNTs can be completely electrochemically reduced to Sb/CNTs. SEM results indicate that as the electrolysis voltage increases， the particles of the electrolysis product become smaller and the surface porosity increases. The findings provide a novel pathway for the direct electrochemical reduction of solid sulfides to metals at low temperatures and even at room temperature.

Key words: deep eutectic solvent（DES）, antimony sulfide, antimony, electrochemical reduction

中图分类号:

TF 818

邓逸凡, 李敏, 薛伟健, 高炳亮. 低共熔溶剂电解固态Sb₂S₃/CNTs制备Sb/CNTs的研究[J]. 东北大学学报（自然科学版）, 2025, 46(2): 50-56.

Yi-fan DENG, Min LI, Wei-jian XUE, Bing-liang GAO. Study on Electrolysis of Solid Sb₂S₃/CNTs to Prepare Sb/CNTs Using Deep Eutectic Solvent[J]. Journal of Northeastern University(Natural Science), 2025, 46(2): 50-56.

图/表 8

图1 353 K下装有固态Sb2S3的石墨空腔电极在氯化胆碱-乙二醇低共熔溶剂中获得的循环伏安图

Fig. 1 Cyclic voltammogram using a graphite cavity electrode containing solid Sb2S3 in choline chloride-ethylene glycol eutectic solvent at 353 K

图2 固态Sb2S3原料及在353 K温度下2.0，2.2，2.4 V电压电解6 h后获得产物的XRD图

Fig. 2 XRD patterns of the solid Sb2S3 and the electrolytic products obtained by voltage of 2.0, 2.2, and 2.4 V for 6 h at 353 K

图3 固态Sb2S3原料及在353 K温度下2.4 V电压电解2，4，6 h后获得产物的XRD图

Fig.3 XRD patterns of the solid Sb2S3 and the electrolytic products obtained by voltage of 2.4 V for 2, 4, and 6 h at 353 K

图4 固态Sb2S3原料及在313，323，333，343，353 K温度下2.4 V电压电解6 h后获得产物的XRD图

Fig. 4 XRD patterns of the solid Sb2S3 and the electrolytic products obtained by voltage of 2.4 V for 6 h at 313, 323, 333, 343, and 353 K

图5 碳纳米管原料及多孔固态Sb2S3/CNTs复合圆片的SEM图（a）—碳纳米管原料；（b）—多孔固态Sb2S3/CNTs复合圆片.

Fig. 5 SEM images of the carbon nanotube raw material and the porous solid Sb2S3/CNTs pellet

图6 多孔固态Sb2S3/CNTs复合圆片及2.0，2.2，2.4 V电压电解6 h获得产物的SEM图（a）—多孔固态Sb2S3/CNTs复合圆片；（b）—2.0 V；（c）—2.2 V；（d）—2.4 V.

Fig. 6 SEM images of the porous Sb2S3/CNTs pellet and the electrolytic products obtained by voltage of 2.0, 2.2 and 2.4 V for 6 h

图7 2.0，2.2，2.4 V电压电解6 h后获得产物的EDS图

Fig. 7 EDS spectra of the electrolytic products obtained by voltage of 2.0, 2.2, and 2.4 V for 6 h

图8 Sb/CNTs复合物在氯化胆碱-乙二醇低共熔溶剂中的示意图

Fig. 8 Schematic diagram of Sb/CNTs complex in choline chloride-ethylene glycol eutectic solvent

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低共熔溶剂电解固态Sb₂S₃/CNTs制备Sb/CNTs的研究

Study on Electrolysis of Solid Sb₂S₃/CNTs to Prepare Sb/CNTs Using Deep Eutectic Solvent

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