WS<sub>2</sub>/C复合材料的制备及其电催化析氢性能研究

万磊; 史春薇; 余宗宝; 武宏大; 肖伟; 耿忠兴; 任铁强; 杨占旭

doi:10.1016/S1872-5813(21)60078-6

WS₂/C复合材料的制备及其电催化析氢性能研究

doi: 10.1016/S1872-5813(21)60078-6

辽宁石油化工大学石油化工学院，辽宁抚顺 113001

基金项目: 国家自然科学基金（21671092），辽宁省“兴辽英才”创新领军人才项目（XLYC1802057），辽宁省-沈阳材料科学国家研究中心联合研发基金（2019010280-JH3/301）和抚顺英才计划青年拔尖人才（FSYC202007001）资助

详细信息

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Tel: 13841322030，E-mail: zhanxuy@126.com

中图分类号: O646
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出版历程
- 收稿日期: 2020-03-01
- 修回日期: 2021-04-02
- 网络出版日期: 2021-04-19
- 刊出日期: 2021-09-30

Preparation of WS₂/C composite material and its electrocatalytic hydrogen evolution performance

School of Petrochemical Engineering, Liaoning Petrochemical University, Fushun 113001, China

Funds: The project was supported by the National Natural Science Foundation of China (21671092), Liaoning Province "Xing Liao Talents" Innovation Leading Talent Project (XLYC1802057), Liaoning Province-Shenyang National Research Center for Materials Science Joint R&D Fund Project (2019010280-JH3/301) and Young Top Talents of Fushun Talent Plan (FSYC202007001)

摘要

摘要: 以H₂WO₄和EDA为前驱体，通过机械搅拌与原位固相热解，得到WO₃/C中间体，通过高温硫化得到WS₂/C复合材料。通过X射线衍射（XRD）、扫描电子显微镜（SEM）、透射电子显微镜（TEM）、X射线光电子能谱（XPS）等仪器分析方法对制备的WS₂/C复合材料结构和形貌等进行表征。同时对材料进行了电催化稳态极化曲线（LSV）、塔菲尔斜率（Tafel）、循环稳定性（CP）和电化学阻抗（PEIS）和电化学活性表面积(ECSA)测试，分析了催化剂的电催化性能。结果表明，当WS₂/C复合材料的电流密度为10 mA/cm²时，过电位为179 mV，Tafel斜率为98 mV/dec。
- WS₂ /
- 电催化 /
- 析氢反应
Abstract: With H₂WO₄ and EDA as precursors, WO₃/C intermediate was obtained by mechanical stirring and in-situ solid-phase pyrolysis, then WS₂/C composite material was obtained by high temperature vulcanization. The WS₂/C composite was characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS) and other instrumental analysis methods. At the same time, the electrocatalytic performance of the catalyst was analyzed by the electrocatalytic steady-state polarization curve (LSV), Tafel slope (Tafel), cycle stability (CP), electrochemical impedance (PEIS) and electrochemically active surface area (ECSA) tests of the material. The results show that when the current density of the WS₂/C composite is 10 mA/cm², overpotential is 179 mV, and Tafel slope is 98 mV/dec.
- WS₂ /
- electrocatalysis /
- hydrogen evolution reaction

HTML全文

FIG. 920. FIG. 920.

FIG. 920. FIG. 920.

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图 1 WS₂/C复合材料的制备流程图

Figure 1 WS₂/C composite preparation flow chart

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图 2 (a) H₂WO₄和H₂WO₄/EDA材料；(b) WO₃/C材料和不同煅烧温度的WS₂/C复合材料XRD谱图

Figure 2 XRD patterns of (a) H₂WO₄ and H₂WO₄/EDA materials as well as (b) WO₃/C materials and WS₂/C composites at different calcination temperatures

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图 3 不同煅烧温度的WS₂/C的SEM照片：(a) WS₂/C-600；(b) WS₂/C-700；(c) WS₂/C-800

Figure 3 SEM images of WS₂/C at different calcination temperatures: (a) WS₂/C-600, (b) WS₂/C-700, (c) WS₂/C-800

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图 4 （（a）−（c））：H₂WO₄材料、H₂WO₄/EDA和WS₂/C-700复合材料的SEM照片；（d）：WS₂/C-700复合材料的TEM照片；（e）：WS₂/C-700复合材料的高分辨率TEM照片；（f）：WS₂/C-700复合材料的元素EDX mapping分布

Figure 4 (（a）−（c）) SEM images of H₂WO₄ materials, H₂WO₄/EDA and WS₂/C-700 composites; (d) TEM images of WS₂/C-700 composites; (e) High resolution TEM images of WS₂/C-700 composites; (f) EDX mapping distribution of elements of WS₂/C-700 composite

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图 5 WS₂/C-700复合材料的XPS谱图：(a)总谱、(b)钨谱、(c)硫谱和(d)碳谱

Figure 5 XPS spectra of WS₂/C-700 composite material: (a) total spectrum, (b) tungsten spectrum, (c) sulfur spectrum, (d) carbon spectrum

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图 6 WS₂/C-700复合材料的Raman谱图

Figure 6 Raman spectra of WS₂/C-700 composite

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图 7 不同煅烧温度下WS₂/C复合材料的孔径分布（a）和氮吸附-脱附等温曲线（b）

Figure 7 Pore size distribution diagram (a) and nitrogen adsorption isotherm diagram (b) of WS₂/C composites at different calcination temperatures

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图 8 WS₂/C-600、WS₂/C-700和WS₂/C-800复合材料的极化曲线（a）和Tafel曲线（b）

Figure 8 Polarization curve (a) and Tafel curve (b) of WS₂/C-600, WS₂/C-700 and WS₂/C-800 composite materials

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图 9 WS₂/C-600、WS₂/C-700和WS₂/C-800复合材料的电化学阻抗谱

Figure 9 Electrochemical impedance spectroscopy of WS₂/C-600, WS₂/C-700 and WS₂/C-800 composite materials

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图 10 （a）： WS₂/C-600、WS₂/C-700和WS₂/C-800复合材料在2000圈循环伏安测试前后的极化曲线；（b）： WS₂/C-700复合材料在0.5 mol/L H₂SO₄电解液中的恒电流曲线

Figure 10 (a): polarization curves of WS₂/C-600, WS₂/C-700 and WS₂/C-800 composites before and after 2000 cycles of cyclic voltammetry; (b): constant current curve of WS₂/C-700 composite in 0.5 M H₂SO₄ electrolyte

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图 11 WS₂/C-600、WS₂/C-700和WS₂/C-800复合材料在不同扫速下的双电层电容

Figure 11 Electric double layer capacitors of WS₂/C-600, WS₂/C-700 and WS₂/C-800 composite materials at different scanning speeds

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