CeO2修饰Ni3S2纳米片用于高效电催化析氧

doi:10.1016/S1872-2067(20)63663-4

催化学报 ›› 2021, Vol. 42 ›› Issue (3): 482-489.DOI: 10.1016/S1872-2067(20)63663-4

CeO₂修饰Ni₃S₂纳米片用于高效电催化析氧

吴倩^a,†,*(), 高庆平^b,†, 孙丽梅^a, 郭焕美^a, 台夕市^a, 李丹^a, 刘莉^a, 凌崇益^c^,^#(), 孙旭平^d^,^$()

^a潍坊学院化学化工学院,山东潍坊261061
^b潍坊职业学院化学工程学院,山东潍坊262737
^c东南大学物理学院,江苏南京211189
^d电子科技大学基础与前沿研究院,四川成都610054

收稿日期:2020-05-13 接受日期:2020-06-20 出版日期:2021-03-18 发布日期:2021-01-23
通讯作者: 吴倩,凌崇益,孙旭平
作者简介:^*电话:(0536)8785283;电子信箱:qianwu2018@wfu.edu.cn;
^†共同第一作者.
基金资助:
国家自然科学基金(21801127);国家自然科学基金(21802104);潍坊市科技发展计划(2019GX002);潍坊高技术区科技惠民计划(2019KJHM10)

Facilitating active species by decorating CeO₂ on Ni₃S₂ nanosheets for efficient water oxidation electrocatalysis

Qian Wu^a,†,*(), Qingping Gao^b,†, Limei Sun^a, Huanmei Guo^a, Xishi Tai^a, Dan Li^a, Li Liu^a, Chongyi Ling^c^,^#(), Xuping Sun^d^,^$()

^aDepartment of Chemistry and Chemical Engineering,Weifang University,Weifang 261061,Shandong,China
^bDepartment of Chemical Engineering,Weifang Vocational College,Weifang 262737,Shandong,China
^cSchool of Physics,Southeast University,Nanjing 211189,Jiangsu,China
^dInstitute of Fundamental and Frontier Sciences,University of Electronic Science and Technology of China,Chengdu 610054,Sichuan,China

Received:2020-05-13 Accepted:2020-06-20 Online:2021-03-18 Published:2021-01-23
Contact: Qian Wu,Chongyi Ling,Xuping Sun
About author:^#E-mail:lingchy@seu.edu.cn;
^*Tel:+86-0536-8785283;E-mail:qianwu2018@wfu.edu.cn;
First author contact:^†These authors contributed equally to this work.
Supported by:
National Natural Science Foundation of China(21801127);National Natural Science Foundation of China(21802104);the Science and Technology Development Plan of Weifang City(2019GX002);the Science and Technology Huimin Plan of Weifang High-tech Zone(2019KJHM10)

摘要/Abstract

摘要：

电化学水分解制氢作为重要的生产氢能的新能源技术,包括氢气析出反应(HER)和氧气析出反应(OER). 然而,OER进行的是多步电子转移过程,动力学过程缓慢且过电位高,严重制约了电解水制氢的发展. 因此开发低成本、高效稳定的非贵金属催化剂替代贵金属催化剂(RuO₂,IrO₂)来降低过电位,减少能源消耗十分必要. Ni₃S₂由于其高导电性、高活性、低成本等优点,具有作为贵金属催化剂替代品的广阔应用前景,但其OER性能仍需进一步提高. 对已有的有效OER催化剂进行表界面调控是提高催化剂性能的一种有效策略. CeO₂中的Ce³⁺和Ce⁴⁺价态之间可以灵活过渡,使其具有良好的电子/离子导电性、可逆的表面氧离子交换和较高的储氧能力. CeO₂的多价性使其有机会与其它基质产生强烈的电子相互作用,良好的电子/离子导电性和较高的储氧能力是提高催化剂析氧活性的有利因素. 因此,用CeO₂对Ni₃S₂进行修饰是提高其析氧活性的有效途径. 基于此,本文运用水热和电沉积相结合的方法将CeO₂修饰到Ni₃S₂纳米片上,制备得到生长于泡沫镍上的Ni₃S₂-CeO₂纳米片阵列(Ni₃S₂-CeO₂/NF),并运用X射线粉末衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)、X射线光电子能谱(XPS)等手段进行了表征,以三电极系统测试了其电催化析氧性能及稳定性,并通过密度泛函理论计算进行了验证.
XRD结果表明,复合材料中确实存在Ni₃S₂和CeO₂. 通过SEM发现,泡沫镍基底上均匀分布着Ni₃S₂纳米片阵列; 电沉积CeO₂后,Ni₃S₂-CeO₂仍保持其纳米片特性,但表面变得粗糙. Ni₃S₂-CeO₂的TEM结果也证实了纳米片结构的形成,高分辨率TEM图像清晰的显示出Ni₃S₂和CeO₂之间具有明显的界面. XPS结果表明,Ni₃S₂-CeO₂的Ni 2p的结合能与Ni₃S₂相比出现负位移. 与纯CeO₂的Ce 3d谱图相比,Ni₃S₂-CeO₂杂化体系中Ce⁴⁺的比例明显增加,表明Ce的价态发生了重排,部分电子转移给了Ni元素. 这些结果均说明Ni₃S₂与CeO₂之间存在着较强的电子相互作用. 相应的电催化测试结果显示,在1.0 M KOH中,当电流密度达到20 mA cm^-2时,Ni₃S₂/NF需提供356 mV的过电位,Ni₃S₂-CeO₂/NF只需264 mV的过电位,仅次于RuO₂/NF. 而且,Ni₃S₂-CeO₂/NF在中性条件下也显示出了较理想的析氧活性. Ni₃S₂-CeO₂/NF的Tafel斜率明显低于CeO₂/NF和Ni₃S₂/NF,表明其具有良好的OER反应动力学. 循环伏安法和计时电位法结果均表明,Ni₃S₂-CeO₂/NF具有良好的电化学稳定性. 电化学阻抗谱测试结果表明,与Ni₃S₂/NF和CeO₂/NF相比,Ni₃S₂-CeO₂/NF明显具有更小的半圆直径,说明其电荷转移阻抗更小,进一步表明CeO₂的修饰有助于催化过程中电子的快速转移. 在非法拉第区域的循环伏安扫描曲线以及拟合扫描速度对电容电流曲线结果显示,Ni₃S₂-CeO₂/NF的最大电容值大于CeO₂/NF和Ni₃S₂/NF,表明其暴露了更多的活性位点,具有更大的电化学活性表面积; 而且,Ni₃S₂-CeO₂/NF在400和500 mV时的电催化析氧转换频率明显高于Ni₃S₂/NF和CeO₂/NF,进一步说明Ni₃S₂-CeO₂/NF具有更高的本征催化活性. 密度泛函理论计算表明,由于*OH,*O和*OOH与Ni₃S₂-CeO₂中的Ni和Ce原子相互作用的存在,使得反应中间产物与Ni₃S₂-CeO₂之间的结合强度较纯Ni₃S₂或CeO₂强,使其显示出了更高的OER性能.
在经过24 h连续电解后,SEM和TEM结果均表明,Ni₃S₂-CeO₂/NF材料仍保持了其纳米片形貌. 稳定性测试后的XPS结果表明,Ni 2p对应的峰强度降低,而与氧化镍物种对应的峰强度增强; S元素在Ni₃S₂-CeO₂表面的信号强度明显降低. 根据文献报道,在强烈的氧化环境下,过渡金属硫化物会部分转化为氧化物或氢氧化物,这通常被认为是OER过程的实际催化物种.

关键词: Ni₃S₂-CeO₂纳米片, 氧析出反应, 碱性条件, 密度泛函理论计算

Abstract:

In the pursuit of stable,high performance Ni-based oxygen evolution reaction (OER) electrocatalysts,modifying the local chemical compositions or fabricating hybrid nanostructures to generate abundant interfaces for improving the water oxidation activity of electrocatalysts has emerged as an effective strategy. Herein,we report the facile development of a Ni3S2-CeO2 hybrid nanostructure via an electrodeposition method. Benefiting from the strong interfacial interaction between Ni3S2 and CeO2,the electron transfer is notably improved and the water oxidation activity of Ni3S2 nanosheets is significantly enhanced. In 1.0 M KOH,the Ni3S2-CeO2 electrocatalyst achieves a current density of 20 mA cm-2 at a low overpotential of 264 mV,which is 92 mV lower than that of Ni3S2. Moreover,Ni3S2-CeO2 exhibits superior electrochemical stability. Density functional theory calculations demonstrate that the enhanced OER electrocatalytic performance of Ni3S2-CeO2 can be ascribed to an increase in the binding strength of the reaction intermediates at the Ni3S2-CeO2 interface.

Key words: Ni3S2-CeO2 nanosheet, Oxygen evolution reaction, Alkaline conditions, Density functional theory calculations

吴倩, 高庆平, 孙丽梅, 郭焕美, 台夕市, 李丹, 刘莉, 凌崇益, 孙旭平. CeO₂修饰Ni₃S₂纳米片用于高效电催化析氧[J]. 催化学报, 2021, 42(3): 482-489.

Qian Wu, Qingping Gao, Limei Sun, Huanmei Guo, Xishi Tai, Dan Li, Li Liu, Chongyi Ling, Xuping Sun. Facilitating active species by decorating CeO₂ on Ni₃S₂ nanosheets for efficient water oxidation electrocatalysis[J]. Chinese Journal of Catalysis, 2021, 42(3): 482-489.

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图/表 5

Fig. 1. (a) XRD patterns of Ni3S2/NF and Ni3S2-CeO2/NF; SEM images of Ni3S2/NF (b) and Ni3S2-CeO2/NF (c); (d) TEM image of Ni3S2-CeO2; (e,f) HRTEM images of Ni3S2-CeO2.

Fig. 2. XPS spectra in the Ni 2p (a) and Ce 3d (b) regions.

Fig.3. (a) LSV curves for bare NF,RuO2/NF,CeO2/NF,Ni3S2/NF and Ni3S2-CeO2/NF at 5 mV s-1 scan rate in 1.0 M KOH; (b) Tafel plots of RuO2/NF,CeO2/NF,Ni3S2/NF and Ni3S2-CeO2/NF; (c) LSV curves for Ni3S2-CeO2/NF before and after 500 and 1000 cycles; (d) Time-dependent current density curves for Ni3S2-CeO2/NF in 1.0 M KOH.

Fig. 4. (a) Nyquist plots of CeO2/NF,Ni3S2/NF and Ni3S2-CeO2/NF with an equivalent circuit; (b) The calculated Cdl; (c) Oxidation peak current versus scan rate plots; (d) TOF plots for CeO2/NF,Ni3S2/NF and Ni3S2-CeO2/NF.

Fig. 5. (a) Calculated free energy diagrams for OER on CeO2,Ni3S2 and CeO2/Ni3S2 surfaces,as presented by red,black and blue lines,respectively. Structures of the reaction intermediates through the OER process on CeO2 (b),Ni3S2 (c) and CeO2/Ni3S2 (d) surfaces. Blue,yellow,offwhite,red and white balls represent the Ni,S,Ce,O and H atoms,respectively.

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CeO₂修饰Ni₃S₂纳米片用于高效电催化析氧

Facilitating active species by decorating CeO₂ on Ni₃S₂ nanosheets for efficient water oxidation electrocatalysis

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