超高过电位诱导NiS2深度重构显著提高HER性能

doi:10.1016/S1872-2067(24)60286-X

催化学报 ›› 2025, Vol. 72: 230-242.DOI: 10.1016/S1872-2067(24)60286-X

超高过电位诱导NiS₂深度重构显著提高HER性能

冯超^a^,^b^,¹, 邵佳新^a^,¹, 吴汉洋^a, 杨恒攀^a, 蔚佳莹^d^,^*(), 胡琪^a^,^*(), 何传新^a^,^*()

^a深圳大学化学与环境工程学院, 广东深圳 518060, 中国
^b石河子大学化学化工学院, 化工绿色加工国家重点实验室孵化基地, 新疆石河子 832003, 中国
^c格但斯克工业大学化学科学学院, 化学工程与技术系, 80-233, 波兰
^d深圳科技大学集成电路与光电芯片学院, 广东深圳 518118, 中国

收稿日期:2024-12-09 接受日期:2025-02-08 出版日期:2025-05-18 发布日期:2025-05-20
通讯作者: *电子信箱: yujiaying@sztu.edu.cn (蔚佳莹),hq2016@szu.edu.cn (胡琪),hecx@szu.edu.cn (何传新).
作者简介:¹共同第一作者.
基金资助:
国家自然科学基金(U21A20312);国家自然科学基金(22379100);国家自然科学基金(22309115);深圳市科技计划经费(20231121200418001);广东省基础与应用基础研究基金(2022B1515120084);广东省教育厅重点项目经费(2023ZDZX3020);新疆维吾尔自治区天池英才计划(青年博士项目)(2025)

Ultra-high overpotential induces NiS₂ deep reconstruction to significantly improve HER performance

Chao Feng^a^,^b^,¹, Jiaxin Shao^a^,¹, Hanyang Wu^a, Afaq Hassan^c, Hengpan Yang^a, Jiaying Yu^d^,^*(), Qi Hu^a^,^*(), Chuanxin He^a^,^*()

^aCollege of Chemistry and Environmental Engineering, Shenzhen University, Shenzhen 518060, Guangdong, China
^bSchool of Chemistry and Chemical Engineering/State Key Laboratory Incubation Base for Green Processing of Chemical Engineering, Shihezi University, Shihezi 832003, Xinjiang, China
^cDepartment of Chemical Engineering and Technology, Faculty of Chemical Sciences, Gdańsk University of Technology, Gdansk 80-233, Poland
^dCollege of Integrated Circuits and Optoelectronic Chips, Shenzhen Technology University, Shenzhen 518118, Guangdong, China

Received:2024-12-09 Accepted:2025-02-08 Online:2025-05-18 Published:2025-05-20
Contact: *E-mail: yujiaying@sztu.edu.cn (J. Yu), hq2016@szu.edu.cn (Q. Hu), hecx@szu.edu.cn (C. He).
About author:¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(U21A20312);National Natural Science Foundation of China(22379100);National Natural Science Foundation of China(22309115);Shenzhen Science and Technology Program(20231121200418001);Guangdong Basic and Applied Basic Research Foundation(2022B1515120084);Key Project of Department of Education of Guangdong Province(2023ZDZX3020);Tianchi Talent Program (Young Doctoral Program) of Xinjiang Uygur Autonomous Region(2025)

摘要/Abstract

摘要：

过渡金属硫化物(TMS)因具有高活性、电子结构的可调性大以及合成方法简单等优势, 广泛应用于碱性电解水制氢过程. 然而, 相对于Pt基电催化剂的高析氢反应(HER)活性, TMS在性能方面还有巨大的提升空间. 本文旨在通过简单且通用的策略来改性TMS以大幅提高其碱性电解水制氢性能. 目前的一些研究工作采用杂原子掺杂工程、异质结构工程、缺陷工程和非晶态工程等措施来提升TMS的碱性HER性能. 然而, 上述措施的实现都需要对TMS电催化剂进行繁琐而精细的设计与制备. 复杂的制备工艺所带来的高成本和不稳定性限制了其进一步的应用. 在此, 我们提出并验证了一种通过超高过电位诱导TMS深度重构进而显著提升其HER性能的普适性方法.

此方法对于研究规模化电解水制氢工艺中高电压和大电流密度下TMS的重构过程及其构效关系具有一定的指导作用.

本文选取NiS₂作为模型电催化剂, 开发了一种通过超高过电位诱导其深度重构进而显著提高其HER性能的简单而通用的策略. 研究了从常规工作电位到超高过电位的作用下所诱导NiS₂发生的重构现象对其电催化析氢性能的影响规律. 实验结果表明, 超高过电位诱导重构后, NiS₂@CC-900 (900表示过电位为900 mV)样品的HER性能得到了最显著的增强. 与161 mV (对应于10 mA cm^-2)的初始过电位相比, 重构样品的过电位仅为94 mV, 降低了67 mV (42%). 在长达25小时的稳定性测试中, 对应的电流密度仅衰减2%, 证实了深度重构后的样品具有优异的循环稳定性. 原位和非原位表征结果表明, NiS₂在重构过程中随着过电位的变化逐渐重构为Ni/Ni₃S₂异质界面结构, 异质界面的协同作用更有利于提高其HER性能, 与理论计算结果一致. 密度泛函理论计算结果表明, 深度重构产物(Ni/Ni₃S₂)能更好地促进电子转移过程, 调节d带中心的位置, 从而优化HER过程, 还证实了Ni/Ni₃S₂异质界面结构能够更好的促进H*的吸附/解吸过程并具有更快的HER动力学. 此外, 上述的简单策略具有良好的普适性, 也同样适用于CoS₂和FeS₂. 采用同样的方式, 分别对CoS₂@CC和FeS₂@CC进行了超高过电位处理和HER性能测试. 结果表明, 经过900 mV过电位处理后的CoS₂@CC-900和FeS₂@CC-900样品在10 mA cm^-2的电流密度下的对应过电势仅为154和190 mV, 与初始样品CoS₂@CC (213 mV)和FeS₂@CC (239 mV)相比, 分别降低了59和49 mV.

综上, 本研究不仅为诱导TMS深度重构显著提高其HER性能提供了一种极其简单且通用的策略, 而且为探索TMS在超高过电位下的动态重构机制和构建高效的非贵金属基电催化剂提供了一定的方法指导.

关键词: 硫化镍, 超高过电位诱导, 深度重构, 协同效应, 析氢反应

Abstract:

It is well known that transition metal sulfides (TMS) (i.e., NiS₂) undergo electrochemical reconstructions to generate highly active Ni₃S₂ during the process of hydrogen evolution reaction (HER) under overpotentials of < 500 mV. However, at higher overpotentials, Ni₃S₂ can theoretically be further restructured into Ni and thus form Ni/Ni₃S₂ heterogeneous interface structures, which may provide opportunities to further enhance HER activity of NiS₂. Here, we selected NiS₂ as a model electrocatalyst and investigated the influence of the reconstruction results induced from regular to ultrahigh overpotentials on its electrocatalytic hydrogen precipitation performance. The experimental results showed that the most significant enhancement of hydrogen precipitation performance was obtained for the NiS₂@CC-900 (900 means 900 mV overpotential) sample after the ultra-high overpotential induced reconstruction. Compared with the initial overpotential of 161 mV (10 mA cm^-2), the overpotential of the reconstructed sample reduced by 67 mV (42%). The characterization results showed that an ultra-high overpotential of 900 mV induced deep reconstruction of NiS₂, formed highly reactive Ni/Ni₃S₂ heterogeneous interfaces, which is more conducive to improved HER performance and match well with theoretical calculations results. We demonstrated ultrahigh overpotential was an effective strategy to induce NiS₂ deeply reconstruction and significantly improve its HER performance, and this strategy was also applicable to CoS₂ and FeS₂. This study provides an extremely simple and universal pathway for the reasonable construction of efficient electrocatalysts by induced TMS deeply reconstruction.

Key words: Nickel sulfide, Ultra-high overpotential induces, Deep reconstruction, Synergistic effect, Hydrogen evolution reaction

冯超, 邵佳新, 吴汉洋, 杨恒攀, 蔚佳莹, 胡琪, 何传新. 超高过电位诱导NiS₂深度重构显著提高HER性能[J]. 催化学报, 2025, 72: 230-242.

Chao Feng, Jiaxin Shao, Hanyang Wu, Afaq Hassan, Hengpan Yang, Jiaying Yu, Qi Hu, Chuanxin He. Ultra-high overpotential induces NiS₂ deep reconstruction to significantly improve HER performance[J]. Chinese Journal of Catalysis, 2025, 72: 230-242.

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图/表 7

Scheme 1. The composition and reconstruction diagram of NiS2@CC.

Fig. 1. i-t and LSV diagrams of NiS2@CC at different overpotentials. (a,b) 100 mV; (c,d) 300 mV; (e,f) 500 mV; (g,h) 700 mV; (i,j) 900 mV; (k,l) 1100 mV.

Fig. 2. HER electrocatalytic properties of NiS2@CC at all reduction potentials. (a) Overpotential distribution; (b) Tafel slope plots; (c) Nyquist plots; (d) i-t curve of NiS2@CC-900; (e) Comparison of the overpotential of the HER for NiS2@CC-900 with recently reported state-of-the-art catalysts at 10 mA cm?2.

Fig. 3. The SEM images of NiS2@CC (a) and NiS2@CC-900 (b). The HR-TEM images of NiS2@CC-900 (I-V: enlarged lattice planes, inverse Fast Fourier transform (FFT) pattern and corresponding line profiles) (c) and NiS2@CC (d). (e-l) Elemental distribution mapping images of the NiS2@CC and NiS2@CC-900.

Fig. 4. (a) In-situ Raman spectra of NiS2@CC at 900 mV. (b) Raman spectra of NiS2@CC and NiS2@CC-900 after long exposure in air.

Fig. 5. XPS diagrams of NiS2@CC, NiS2@CC-900 and NiS2@CC-900 (Ar) (argon ion etching at different times). (a) Ni 2p; (b) O 1s; (c) S 2p. XPS diagrams of NiS2@CC, NiS2@CC-900 and NiS2@CC-900 (Ar) (argon ion etching 90 s). (d) Ni 2p; (e) O 1s; (f) S 2p.

Fig. 6. (a) Theoretical energy barriers for the gradual reduction of NiS2 to NiS2/Ni3S2 and then to Ni/Ni3S2. (b,c) Schematic illustration of the HER activity enhancing mechanism of the NiS2@CC-900 sample in alkaline media. Density of states of NiS2 (d), NiS2/Ni3S2 (e) and Ni/Ni3S2 (f). The orange dotted line denotes the d-band center. (g) Calculated H2O adsorption energies free energies on NiS2, NiS2/Ni3S2 and Ni/Ni3S2, where more negative values mean stronger binding strength. (h) Energy barriers of water dissociation for NiS2, NiS2/Ni3S2 and Ni/Ni3S2. (i) ΔGH* diagram for NiS2, NiS2/Ni3S2 and Ni/Ni3S2.

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超高过电位诱导NiS₂深度重构显著提高HER性能

Ultra-high overpotential induces NiS₂ deep reconstruction to significantly improve HER performance

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