双壳层空心纳米球NiCo₂S₄@CoS₂/MoS₂: 通过协同效应增强析氧催化活性用于水分解

doi:10.1016/S1872-2067(25)64727-9

催化学报 ›› 2025, Vol. 74: 394-410.DOI: 10.1016/S1872-2067(25)64727-9

双壳层空心纳米球NiCo₂S₄@CoS₂/MoS₂: 通过协同效应增强析氧催化活性用于水分解

陈阳^a, 唐宇^b, 韩雷云^a, 刘佳颜^a, 华英杰^c, 赵旭东^a, 刘晓旸^a^,^c^,^*()

^a吉林大学化学学院, 无机合成与制备化学全国重点实验室, 吉林长春 130012
^b吉林大学物理学院, 先进电池物理与技术教育部重点实验室, 吉林长春 130012
^c海南师范大学化学与化工学院, 海南省电化学能量存储与能量转换重点实验室, 海南海口 571158

收稿日期:2024-12-09 接受日期:2025-04-11 出版日期:2025-07-18 发布日期:2025-07-20
通讯作者: *电子信箱: liuxy@jlu.edu.cn (刘晓旸).
基金资助:
国家自然科学基金(2217010508);国家自然科学基金(21731068)

Dual-shell hollow nanospheres NiCo₂S₄@CoS₂/MoS₂: Enhancing catalytic activity for oxygen evolution reaction and achieving water splitting via the unique synergistic effects of mechanisms of adsorption-desorption and lattice oxygen oxidation

Yang Chen^a, Yu Tang^b, Leiyun Han^a, Jiayan Liu^a, Yingjie Hua^c, Xudong Zhao^a, Xiaoyang Liu^a^,^c^,^*()

^aState Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012, Jilin, China
^bKey Laboratory of Physics and Technology for Advanced Batteries (Ministry of Education), College of Physics, Jilin University, Changchun 130012, Jilin, China
^cKey Laboratory of Electrochemical Energy Storage and Energy Conversion of Hainan Province, School of Chemistry and Chemical Engineering, Hainan Normal University, Haikou 571158, Hainan, China

Received:2024-12-09 Accepted:2025-04-11 Online:2025-07-18 Published:2025-07-20
Contact: *E-mail: liuxy@jlu.edu.cn (X. Liu).
Supported by:
National Natural Science Foundation of China(2217010508);National Natural Science Foundation of China(21731068)

摘要/Abstract

摘要：

随着环境和能源问题日益严重, 清洁和可再生能源是碳基燃料的有希望的替代品. 析氧反应(OER)是水分解、燃料电池和二氧化碳还原等先进能源系统中的关键半反应. 然而, 缓慢的动力学和刚性O-O键的高能量障碍阻碍了这些技术的发展. OER主要有两种机制, 即吸附物演化机制(AEM)和晶格氧机制(LOM). 在AEM中, 金属位点充当氧化还原中心, 涉及氧中间体, 并将最小过电位限制在0.37 V. 在LOM中, 晶格氧参与O₂的生成, 打破了AEM的制约关系限制, 并提供了更有利的热力学条件. 然而, 晶格氧的参与可能导致结构失调和性能下降. 构建结合AEM和LOM的机制可以平衡催化活性和稳定性. 开发同时激活金属和晶格氧氧化还原对的耦合催化系统仍然是一个重大挑战.

实现金属和晶格氧位点的同时活化, 以构建兼容的多机制催化, 是OER研究中的一个重要目标, 因为这可以提供高度可用的活性位点并提升催化活性与稳定性. 本文提出了一种新方法, 利用钴镍-甘油酸酯球(CoNi-G SSs)作为自牺牲模板, 成功制备了具有卵黄壳结构的CoNi-G SSs@ZIF-67纳米球. 由此衍生的NiCo₂S₄@CoS₂/MoS₂双壳层空心纳米球(DSHSs)结合了AEM和LOM, 实现了协同的双重催化途径. 在电化学反应过程中, Ni作为调节剂, 促进了NiCo₂S₄中活性物种的完全重构, 显著提升了晶格氧活性并增强了OER的LOM反应途径. 表征结果表明, 阳极活化触发了金属和晶格氧位点的氧化还原, 并涉及氧空位的形成与重新填充. 通过OER的pH依赖性、四甲基铵阳离子吸附、原位拉曼光谱和¹⁸O同位素标记差分电化学质谱, 确认了一种与AEM和LOM兼容的OER催化机制. X射线光电子能谱和紫外光电子能谱分析证明了CoS₂/MoS₂异质结构的存在, 莫特-肖特基异质结构相互作用调节了异质界面处的电子结构, 优化了HER和OER中间体的吸附. 密度泛函理论计算表明, CoS₂/MoS₂中Mo的引入优化了AEM途径, 提升了水分解性能. 在Ni和Mo的共同调节下, NiCo₂S₄@CoS₂/MoS₂ DSHSs实现了AEM和LOM途径的协同催化, 最大限度地利用了表面金属和氧活性位点, 显著提高了OER催化活性. 得益于双机制的兼容性, 测试结果表明, NiCo₂S₄@CoS₂/MoS₂ DSHSs在碱性介质中对HER和OER表现出优异的电化学活性和催化稳定性, 在电流密度为10 mA cm^-2时, 相对于可逆氢电极(RHE)分别产生了-0.087和1.462 V的低电位. 组装的阴离子交换膜水分解装置在商业催化条件下(1 mol L^-1 KOH)可在1.74 V下提供500 mA cm^-2催化电流, 持续150 h, 衰减可忽略不计.

综上所述, 本研究为新型电催化剂的设计, 特别是在构建多元化合物和异质结构方面, 提供了重要参考. 这类催化剂能够协同激活金属位点和晶格氧, 从而显著提升OER反应的催化效率. 此外, 催化剂的结构优化、掺杂效应以及合理的电子结构调控将成为提升水分解反应动力学的关键技术. 这项工作为OER机制的理解和高性能水分解电催化剂的设计提供了重要见解, 同时为开发具有多壳结构的多功能材料开辟了新的途径.

关键词: 吸附物演化机制, 晶格氧机制, 水分解, ZIF-67, NiCo₂S₄@CoS₂/MoS₂, 双壳层空心纳米球

Abstract:

Activating both metal and lattice oxygen sites for efficient oxygen evolution reactions (OER) is a critical challenge. This study pioneers a novel approach, employing cobalt-nickel glycerate solid spheres (CoNi-G SSs) as self-sacrificial templates to synthesize yolk-shell structured CoNi-G SSs@ZIF-67 nanospheres. The derived NiCo₂S₄@CoS₂/MoS₂ double-shelled hollow nanospheres integrate the adsorbate evolution mechanism (AEM) and lattice oxygen mechanism (LOM), enabling synergistic dual catalytic pathways. Nickel modulation facilitates active species reconstruction in NiCo₂S₄, enhancing lattice oxygen activity and optimizing the LOM pathway. Characterization results indicate that anode activation triggered the redox processes of metal and lattice oxygen sites, involving the formation and re-filling of oxygen vacancies. Additionally, the CoS₂/MoS₂ heterostructure enhances the AEM pathway, as supported by density functional theory calculations, which demonstrate optimized adsorption of intermediates for both hydrogen evolution reaction and OER. The assembled anion exchange membrane water splitting device can deliver a catalytic current of 500 mA cm^-2 at 1.74 V under commercial catalytic operating conditions (1 mol L^-1 KOH) for 150 h, with negligible degradation. This work provides important insights into the understanding of OER mechanisms and the design of high-performance water-splitting electrocatalysts, while also opening new avenues for developing multifunctional materials with multi-shell structures.

Key words: Adsorbate evolution mechanism, Lattice oxygen mechanism, Water-splitting, ZIF-67, NiCo₂S₄@CoS₂/MoS₂, Dual-shell hollow nanospheres

陈阳, 唐宇, 韩雷云, 刘佳颜, 华英杰, 赵旭东, 刘晓旸. 双壳层空心纳米球NiCo₂S₄@CoS₂/MoS₂: 通过协同效应增强析氧催化活性用于水分解[J]. 催化学报, 2025, 74: 394-410.

Yang Chen, Yu Tang, Leiyun Han, Jiayan Liu, Yingjie Hua, Xudong Zhao, Xiaoyang Liu. Dual-shell hollow nanospheres NiCo₂S₄@CoS₂/MoS₂: Enhancing catalytic activity for oxygen evolution reaction and achieving water splitting via the unique synergistic effects of mechanisms of adsorption-desorption and lattice oxygen oxidation[J]. Chinese Journal of Catalysis, 2025, 74: 394-410.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64727-9

https://www.cjcatal.com/CN/Y2025/V74/I7/394

图/表 11

Fig. 1. Schematic illustration of formation mechanism for NiCo2S4@CoS2/MoS2 DSHSs and NiCo2S4@CoS2 DSHSs.

Fig. 2. (a) XRD patterns of CoNi-G SSs (A) and CoNi-G SSs@ZIF-67 YSSs (B). (b) XRD patterns of NiCo2S4@CoS2/MoS2 DSHSs (A), NiCo2S4@CoS2 DSHSs (B), and NiCo2S4 YSSs (C).

Fig. 3. SEM (a-c) and TEM (d-f) images of CoNi-G SSs (a,d), CoNi-G SSs@ZIF-67 YSSs (b,e), and NiCo2S4@CoS2/MoSx -2/1 DSHSs (c,f).

Fig. 4. (a-c) SEM images of S-NiCoMo-2. (d,e) TEM images of S-NiCoMo-2. (f) HRTEM image of S-NiCoMo-2. (g) elemental mapping images of S-NiCoMo-2.

Fig. 5. (a) The XPS patterns of S-NiCoMo-2. High-resolution XPS spectra of Co 2p (b), Ni 2p (c); Mo 3d (d), and S 2p (e) of S-NiCoMo-2. (f) N2 adsorption-desorption isotherm measurements.

Fig. 6. Polarization curves (a), histograms of overpotentials at different current densities (b), and corresponding Tafel slopes (c) of S-NiCoMo-2, S-NiCoMo-4, S-NiCoMo-0, and NiCo2S4 YSSs towards HER. Polarization curves (d), histograms of overpotentials at different current densities (e) and corresponding Tafel slopes (f) of S-NiCoMo-2, S-NiCoMo-4, S-NiCoMo-0, and NiCo2S4 YSSs towards OER. (g, h) Cdl values of S-NiCoMo-2, S-NiCoMo-4, S-NiCoMo-0, and NiCo2S4 YSSs towards HER and OER were obtained from current density versus scan rates. (i) Nyquist plots and equivalent circuit for S-NiCoMo-2, S-NiCoMo-4, S-NiCoMo-0, and NiCo2S4 YSSs.

Fig. 7. (a) OER polarization curves of S-NiCoMo-4 and S-NiCoMo-2 in 1 mol L-1 KOH and 1 mol L-1 TMAOH, respectively. In situ Raman spectra of S-NiCoMo-4 (b) and S-CoMo-4 (c) during the applied potential range from OCP to 1.7 V vs. RHE. (d, e) show the DEMS measurements of the 32O2, 34O2, and 36O2 signals from the reaction products of 18O-labeled S-NiCoMo-4 and S-CoMo-4, respectively. (f) in situ Raman spectroscopy of HER on S-NiCoMo-4 at different potentials immediately after OER tests. (g) mechanism diagram of synergistic catalysis under AEM and LOM pathways.

Fig. 8. (a) Chronopotentiometry curves recorded at 10 mA cm-2 of S-NiCoMo-2 towards HER and S-NiCoMo-4 towards OER in 1.0 mol L-1 KOH solution. (b) Polarization curves at 10 mA cm-2 of S-NiCoMo-4||S-NiCoMo-2 and Pt/C||RuO2 couples towards overall water electrolysis. (c) Experimental and theoretical values of gas production for S-NiCoMo-4||S-NiCoMo-2. Electrolyte 1 mol L-1 KOH. (d) a drainage device fabricated using an H-type electrolytic cell. (e) Chronopotentiometry curves at 10 mA cm-2 of S-NiCoMo-2||S-NiCoMo-4 and Pt/C||RuO2 couples towards overall water electrolysis. (f) Comparison of the water electrolysis voltage obtained at a current density of 10 mA cm-2 from previous research and that achieved using our NiCo2S4@CoS2/MoS2 DSHSs catalyst in an alkaline medium. Optical image of the AEM water splitting device (g) and schematic diagram (h). (i) Stability testing of the S-NiCoMo-4|| S-NiCoMo-2 electrode pairs in EWS using the AEM water splitting device (constant current charging, current density = 0.5 A cm-2) in 1 mol L-1 KOH.

Fig. 9. (a) DFT calculated PDOS of isolated (002) MoS2 nanoparticles, (112) CoS2 surface and CoS2/MoS2 heterointerface. (b) Charge density difference at the CoS2/MoS2 heterointerface. (c) Band diagrams of semiconductor MoS2 and metallic CoS2 before and after the formation of Mott-Schottky interactions. (d) Schematic of the CoS2/MoS2 heterointerface illustrating electron transfer at the heterojunction.

Fig. 10. (a) Optimized crystal structures of (002) MoS2 nanoparticle, (112) CoS2 and CoS2/MoS2 heterointerface. (b-d) Gibbs free energy diagrams for HER at different H adsorption sites on the surfaces of MoS2, CoS2, and CoS2/MoS2, respectively. Insets in (b-d) represent the considered H adsorption sites on MoS2, CoS2, and CoS2/MoS2, respectively.

Fig. 11. (a) Water adsorption sites for MoS2, CoS2, and CoS2/MoS2. (b) Water adsorption energy on the MoS2, CoS2, and CoS2/MoS2 systems (Adsorption sites: Mo-top (MoS2); Mo-edge (MoS2); Co (CoS2); Co (CoS2/MoS2); and Mo (CoS2/MoS2)). Four proton transfer mechanisms of OER on the Co binding site on the surface of CoS2 under alkaline conditions (c) and the corresponding Gibbs free energy diagrams (e) for OER. Four proton transfer mechanisms of the proposed OER on the surface Co binding site of CoS2/MoS2 under alkaline conditions (d) and the corresponding Gibbs free energy diagrams for OER (f).

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双壳层空心纳米球NiCo₂S₄@CoS₂/MoS₂: 通过协同效应增强析氧催化活性用于水分解

Dual-shell hollow nanospheres NiCo₂S₄@CoS₂/MoS₂: Enhancing catalytic activity for oxygen evolution reaction and achieving water splitting via the unique synergistic effects of mechanisms of adsorption-desorption and lattice oxygen oxidation

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双壳层空心纳米球NiCo₂S₄@CoS₂/MoS₂: 通过协同效应增强析氧催化活性用于水分解

Dual-shell hollow nanospheres NiCo2S4@CoS2/MoS2: Enhancing catalytic activity for oxygen evolution reaction and achieving water splitting via the unique synergistic effects of mechanisms of adsorption-desorption and lattice oxygen oxidation

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Dual-shell hollow nanospheres NiCo₂S₄@CoS₂/MoS₂: Enhancing catalytic activity for oxygen evolution reaction and achieving water splitting via the unique synergistic effects of mechanisms of adsorption-desorption and lattice oxygen oxidation