钨掺杂稳定钼酸钴的钴-氧-钼点对点连接结构用于中性析氧反应

doi:10.1016/S1872-2067(25)64748-6

催化学报 ›› 2025, Vol. 76: 146-158.DOI: 10.1016/S1872-2067(25)64748-6

钨掺杂稳定钼酸钴的钴-氧-钼点对点连接结构用于中性析氧反应

王舟舟, 周前程, 罗丽, 史雅然, 李浩然, 王春春, 林可聖, 王成思, 朱利兵, 韩凌云, 邢卓(), 余颖()

华中师范大学物理科学与技术学院纳米科技研究所, 湖北武汉 430079

收稿日期:2025-04-01 接受日期:2025-05-01 出版日期:2025-09-18 发布日期:2025-09-10
通讯作者: 邢卓,余颖
基金资助:
国家重点研发计划(2022YFB3803600);国家自然科学基金(52472205);国家自然科学基金(12275199);华中师范大学中央高校基本科研业务费(CCNU25ZH006);华中师范大学优秀研究生教育创新资助(2024CXZZ148);华中师范大学大学生创新创业训练计划(202510511088)

Suppressing catalyst reconstruction in neutral electrolyte: stabilizing Co-O-Mo point-to-point connection of cobalt molybdate by tungsten doping for oxygen evolution reaction

Zhouzhou Wang, Qiancheng Zhou, Li Luo, Yaran Shi, Haoran Li, Chunchun Wang, Kesheng Lin, Chengsi Wang, Libing Zhu, Linyun Han, Zhuo Xing(), Ying Yu()

Institute of Nanoscience and Nanotechnology, College of Physical Science and Technology, Central China Normal University, Wuhan 430079, Hubei, China

Received:2025-04-01 Accepted:2025-05-01 Online:2025-09-18 Published:2025-09-10
Contact: Zhuo Xing, Ying Yu
Supported by:
National Key Research and Development Program of China(2022YFB3803600);National Natural Science Foundation of China(52472205);National Natural Science Foundation of China(12275199);self-determined research funds of CCNU from the colleges’ basic research and operation of MOE(CCNU25ZH006);Excellent Doctoral Dissertation Cultivation Grant from Central China Normal University(2024CXZZ148);National Undergraduate Training Program for Innovation and Entrepreneurship for Central China Normal University(202510511088)

摘要/Abstract

摘要：

中性电解质环境温和, 对电解槽和催化剂的腐蚀性低, 因此是开发新型电解水设备的良好介质. 并且, 中性析氧反应(OER)是众多电化学反应的基础, 如电化学二氧化碳还原和微生物电解池都需要采用中性电解质, 前者有利于提高二氧化碳溶解度, 后者可维持较好的生物生长环境. 然而, 中性OER的过电位通常很高且稳定性差, 这主要是因为中性电解质中的反应物浓度极低造成OER动力学缓慢. 催化剂重构是提升碱性OER性能的有效策略. 例如, 过渡金属钼酸盐材料在碱性OER过程中往往会经历钼酸根的析出, 并伴随着过渡金属(Ni, Co等)的重构形成羟基氧化物活性相, 从而提升活性与稳定性. 然而, 这种过渡金属钼酸盐催化剂在中性OER中却表现不佳, 相关机制的研究匮乏.

本文合成了一种钨掺杂的钼酸钴(WDCMO)催化剂, 用于中性电解质下高效持久的OER. 表征和实验结果表明, 在中性介质中, 由于OH^-浓度极低, 催化剂重构过程中, 随着钼的溶解, 另一过渡金属组分难以得到充足的羟基补充, 从而阻碍了活性相羟基氧化物的形成. 而W的引入稳定了CoMoO₄结构中Co-O-Mo的点对点连接, 并防止OER过程中表面Co和Mo活性位点被氧化至高价态, 从而维持表面结构稳定, 避免组分析出并抑制催化剂重构. 同时, W掺杂促进了CoMoO₄电荷转移, 并优化了*OH中间体的吸附, 从而加快反应动力学, 提高中性OER的本征活性. 因此, 在pH = 7的中性电解质中, WDCMO电极在10 mA cm^-2的电流密度下的OER过电位为302 mV, 比未掺杂W的电极低182 mV. 此外, 掺杂W后, 钼酸钴稳定性从50 h提升至320 h, 电压衰减从2.82降至0.29 mV h^-1.

综上, 本文利用快速制备方法成功合成一种具有较高催化活性和稳定性的非贵金属基催化剂, 并研究了中性介质中催化剂重构对析氧反应的性能影响. 本研究为合理设计基于过渡金属氧化物的中性析氧电催化剂提供了新认识.

关键词: 中性析氧反应, 抑制催化剂重构, 钼酸钴, 钨掺杂, 稳定性

Abstract:

Neutral oxygen evolution reaction (OER) is a crucial half-reaction for electrocatalytic chemical production under mild condition, but with limited development due to low activity and poor stability. Herein, a tungsten-doped cobalt molybdate (WDCMO) catalyst was synthesized for efficient and durable OER under neutral electrolyte. It is demonstrated that catalyst reconstruction is suppressed by W doping, which stabilizes the Co-O-Mo point-to-point connection in CoMoO₄ architecture and stimulates to a lower valence state of active sites over the surface phase. Thereby, the surface structure maintains to avoid compound dissolution caused by over-oxidation during OER. Meanwhile, the WDCMO catalyst promotes charge transfer and optimizes *OH intermediate adsorption, which improves reaction kinetics and intrinsic activity. Consequently, the WDCMO electrode exhibits an overpotential of 302 mV at 10 mA cm^-2 in neutral electrolyte with an improvement of 182 mV compared with CoMoO₄ electrode. Furthermore, W doping significantly improves the electrode stability from 50 h to more than 320 h, with a suppressive potential attenuation from 2.82 to 0.29 mV h^-1. This work will shed new light on designing rational electrocatalysts for neutral OER.

Key words: Neutral oxygen evolution reaction, Suppressive catalyst reconstruction, Cobalt molybdate, Tungsten doping, Stability

王舟舟, 周前程, 罗丽, 史雅然, 李浩然, 王春春, 林可聖, 王成思, 朱利兵, 韩凌云, 邢卓, 余颖. 钨掺杂稳定钼酸钴的钴-氧-钼点对点连接结构用于中性析氧反应[J]. 催化学报, 2025, 76: 146-158.

Zhouzhou Wang, Qiancheng Zhou, Li Luo, Yaran Shi, Haoran Li, Chunchun Wang, Kesheng Lin, Chengsi Wang, Libing Zhu, Linyun Han, Zhuo Xing, Ying Yu. Suppressing catalyst reconstruction in neutral electrolyte: stabilizing Co-O-Mo point-to-point connection of cobalt molybdate by tungsten doping for oxygen evolution reaction[J]. Chinese Journal of Catalysis, 2025, 76: 146-158.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64748-6

https://www.cjcatal.com/CN/Y2025/V76/I9/146

图/表 7

Fig. 1. Material preparation and morphology characterization. (a) Schematics of the material preparation. SEM image (b), HRTEM image (inset: SAED pattern) (c), the enlarged images of the blue dotted circle (d) and red dotted box (e) in Fig. 1(c). (f) Dark field TEM image and corresponding EDS elemental mapping of WDCMO, respectively.

Fig. 2. Chemical structure characterization. XRD patterns (a) and the enlarged region of the dotted box (b) in Fig. 2(a) for WDCMO and CMO catalysts. Raman spectra (c) and the enlarged region of the dotted box (d) in Fig. 2(c) for WDCMO and CMO catalysts. High resolution of Co 2p (e), Mo 3d (f), and W 4f (g) XPS spectra for WDCMO and CMO catalysts over the bulk and surface phase. Co K-edge XANES spectra (h), FT k3-weighted EXAFS signals (i), and WT-EXAFS (j) for Co foil, WDCMO, and CMO.

Fig. 3. Neutral OER performance in 1 mol L−1 PBS. Polarization curves at a scan rate of 5 mV s−1 (a), overpotentials at 10 and 100 mA cm−2 (b), Tafel plots (c), polarization curves normalized by ECSA (d), and Nyquist plots (e) for various electrodes. (f) Chronopotentiometry curves of WDCMO and CMO at a current density of 10 mA cm−2.

Fig. 4. Stability analysis. High resolution of outer Co 2p (a), inner Co 2p (b), outer W 4f (c), and inner W 4f XPS (d) spectra for WDCMO before and after OER over the bulk and surface phase. (e) XRD pattern of WDCMO-OER and CMO-OER electrodes. (f) Content of Mo for WDCMO and CMO before and after OER determined by ICP-OES. Raman spectrum of CMO-KOH (g) and WDCMO-KOH (h) electrode immersed in 1 mol L−1 KOH for different time. (i) XES of Co Kβ for WDCMO and CMO electrodes, as well as CMO-KOH and WDCMO-KOH electrode immersed in 1 mol L−1 KOH for 300 minutes.

Fig. 5. Kinetic analysis. Operando Bode phase plots of WDCMO (a) and CMO (b). The peak of phase angles varies with the potentials at low (c) and high (d) frequency region for WDCMO and CMO. (e) In-situ Raman spectrum of WDCMO electrode.

Fig. 6. Mechanism analysis. (a) Formation energy of the models for W replacing Co sites and Mo sites. (b) Bader charge analysis of outer W1 site and surrounding Co sites for WDCMO. (c) Electron localization function diagram for outer W1 site of WDCMO compare with the initial Mo site of CMO. (d) PDOS plots of Mo d, Co d, and O p states in WDCMO and CMO. (e) CO stripping curves of WDCMO and CMO. (f) Energy profiles for OER path over WDCMO and CMO. (g) Schematics of stability improvement by W doping.

Fig. 7. Neutral overall water splitting in 1 mol L−1 PBS. Polarization curves of HER (a), overpotentials at −10 mA cm−2 and current density at −0.2 V (vs. RHE) (b), Tafel plots (c), and polarization curves (d) of water electrolysis of as-prepared WDCMP and CMP electrodes. (e) Chronopotentiometry curves of WDCMO||WDCMP and CMO||CMP at a current density of 10 mA cm−2.

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钨掺杂稳定钼酸钴的钴-氧-钼点对点连接结构用于中性析氧反应

Suppressing catalyst reconstruction in neutral electrolyte: stabilizing Co-O-Mo point-to-point connection of cobalt molybdate by tungsten doping for oxygen evolution reaction

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