一步电沉积法制备硫化镍/泡沫镍材料及其赝电容性能研究

doi:10.11949/0438-1157.20191423

摘要/Abstract

摘要：

通过一步电化学沉积法在泡沫镍(Ni foam，NF)集流体上制备了3D硫化镍(Ni₃S₂)材料，利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、拉曼光谱(Raman)、X射线光电子能谱(XPS)等对所制备材料的物化结构和形貌进行了表征，并采用循环伏安法(CV)、恒流充放电法(GCD)研究了其作为超级电容器电极的电化学性能。测试结果表明，制备的Ni₃S₂/NF-10材料具有相互连接的3D结构，表现出优异的赝电容性能。在1 A/g电流密度下，比电容高达2850 F/g。将电流密度提高到10 A/g，该材料比电容仍能达到1972 F/g，说明其具有优异的倍率性能。测试结果表明所制备的Ni₃S₂材料有望应用于电化学储能领域。

关键词: 超级电容器, 硫化镍, 赝电容, 电沉积, 电化学, 泡沫镍

Abstract:

In this work, a facile one-step electrodeposition method is developed to prepare 3D Ni₃S₂ interconnected nanosheet arrays on Ni foam as electrodes for suprecapacitors, resulting in excellent pseudocapacitance performance. The composition, microstructure and morphology of the prepared Ni₃S₂ materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). The electrochemical capacitance properties were tested by cyclic voltammetry (CV), galvanostatic charge-discharge (GCD) measurements in a three-electrode system. Taking advantage of the highly conductive 3D architectures, the Ni₃S₂/NF-10 electrode exhibits a superior specific capacitance of 2850 F/g at current density of 1 A/g. Remarkably, a specific capacitance of 1972 F/g could be still achieved at a high current density of 10 A/g, indicating its excellent rate capability. With the increase of the electrodeposition time, the 3D architectures of Ni₃S₂ begin to disappear, resulting in a reduced specific capacitance. The appropriate electrodeposition conditions is the key of preparation of high performance electrode materials. Test results show that the prepared Ni₃S₂ material is expected to be used in the field of electrochemical energy storage.

Key words: supercapacitor, Ni₃S₂, pseudocapacitance, electrodeposition, electrochemistry, Ni foam

中图分类号:

TQ 152

赵少飞, 刘鹏, 李婉萍, 曾小红, 钟远红, 余林, 曾华强. 一步电沉积法制备硫化镍/泡沫镍材料及其赝电容性能研究[J]. 化工学报, 2020, 71(4): 1836-1843.

Shaofei ZHAO, Peng LIU, Wanping LI, Xiaohong ZENG, Yuanhong ZHONG, Lin YU, Huaqiang ZENG. One-step electrodeposition and pseudocapacitance properties of 3D Ni₃S₂ supported on Ni foam[J]. CIESC Journal, 2020, 71(4): 1836-1843.

图/表 7

图1 Ni3S2的XRD、拉曼及XPS谱图

Fig.1 XRD pattern, Raman and XPS spectrum of Ni3S2

图2 Ni3S2@NF材料的SEM 图

Fig.2 SEM images of Ni3S2@NF

图3 不同扫描速率下Ni3S2@NF-10电极的循环伏安曲线及峰电流与扫描速率的关系

Fig.3 CV curves of Ni3S2@NF-10 electrode obtained at various scan rates and relationship between peak current and scan rate

图4 Ni3S2@NF-10在不同电流密度下的放电曲线及不同材料的比电容

Fig.4 Galvanostatic discharge curves of Ni3S2@NF-10 and specific capacitance of Ni3S2@NF-10, 20, 40@NF at different current density

图5 Ni3S2@NF-10,20,40在5和100 mV/s扫速下的CV曲线

Fig.5 CV curves of Ni3S2@NF-10,20,40 at 5 and 100 mV/s

图6 Ni3S2@NF-10循环性能曲线及2000次循环后的SEM图

Fig.6 Cycling performance of Ni3S2@NF-10 at current density of 10 A/g and SEM image of Ni3S2@NF-10 after 2000 cycles

表1 不同电极材料电化学性能比较

Table 1 Comparison of electrochemical performance of reported electrodes with Ni3S2/NF-10

电极材料	电流密度/(A/g)	比电容/(F/g)	循环后比电容/(F/g)	文献
3D Ni₃S₂纳米片@NF	2	1370	1075.9(1000次，6 A/g)	[5]
核壳结构Ni₃S₂@NF	0.8	736.64	604(1000次，0.8 A/g)	[7]
NiCo₂S₄ 纳米片@C	1	1394.5	1581.4(10000次，10 A/g)	[15]
Ni₃S₂纳米柱/石墨烯@NF	1	1900	950(2000次，10 A/g)	[17]
Ni₃S₂纳米片@NF	2	2885	1000(10000次，50 A/g)	[21]
Ni₃S₂ 纳米片@NF	1	773.6	575(5000次，5 A/g)	[22]
Ni₃S₂-Cu_1.8S 纳米片@NF	1	1686	766.8(1000次，10 A/g)	[26]
NiCo₂S₄纳米阵列@NF	1	1777	815(3000次，10 A/g)	[27]
NiCo₂S₄纳米片@NF	1	1956	1722(5000次，2 A/g)	[28]
Ni₁Co₁-S@NF	0.5	2553.9	1914.6(10000次，20 A/g)	[29]
Ni₃S₂-NiS	5	1077.3	660.5(10000次，20A/g)	[30]
3D Ni₃S₂@NF-10	1	2850	744(2000次，10 A/g)	本文

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