锰掺杂触发NiSe2催化剂动态相变以促进尿素氧化反应

doi:10.1016/S1872-2067(26)65138-8

催化学报 ›› 2026, Vol. 88: 335-346.DOI: 10.1016/S1872-2067(26)65138-8

锰掺杂触发NiSe₂催化剂动态相变以促进尿素氧化反应

张颖贞^a^,^b, 张伟^b, 黄章政^b, 蔡伟龙^a^,^b, Yun Hau Ng^d^,^e, 黄剑莹^b^,^*(), 赖跃坤^a^,^b^,^c^,^*()

^a 清源创新实验室, 福建泉州 362801, 中国
^b 福州大学化工学院, 国家化肥催化剂工程研究中心, 福建福州 350116, 中国
^c 武汉纺织大学, 纺织新材料与先进加工全国重点实验室, 湖北武汉 430073, 中国
^d 香港城市大学能源与环境学院, 香港 999077, 中国
^e 阿卜杜拉国王科技大学物理科学与工程系, 可再生能源与存储技术中心, 图瓦尔, 沙特阿拉伯

收稿日期:2025-12-12 接受日期:2026-02-21 出版日期:2026-09-18 发布日期:2026-09-05
通讯作者: *电子信箱: yklai@fzu.edu.cn (赖跃坤),
jyhuang@fzu.edu.cn (黄剑莹).
基金资助:
国家自然科学基金委员会国际合作与交流项目(22361162607);国家重点研发计划(2022YFB3804905);国家自然科学基金(22375047);国家自然科学基金(22378071);国家自然科学基金(22378068);福建省自然科学基金(2022J01568);111项目(D17005);中国博士后基金(2024M761750)

Mn-triggered dynamic phase transition in NiSe₂ catalyst via doping engineering for boosted urea electrolysis

Yingzhen Zhang^a^,^b, Wei Zhang^b, Zhangzheng Huang^b, Weilong Cai^a^,^b, Yun Hau Ng^d^,^e, Jianying Huang^b^,^*(), Yuekun Lai^a^,^b^,^c^,^*()

^a Qingyuan Innovation Laboratory, Quanzhou 362801, Fujian, China
^b College of Chemical Engineering, Fuzhou University, Fuzhou 350116, Fujian, China
^c State Key Laboratory of New Textile Materials and Advanced Processing, Wuhan Textile University, Wuhan 430073, Hubei, China
^d School of Energy and Environment, City University of Hong Kong, Kowloon Tong 999077, Hong Kong SAR, China
^e Center for Renewable Energy and Storage Technologies (CREST), Physical Science and Engineering (PSE) Division, King Abdullah University of Science and Technology (KAUST), Thuwal 23955-6900, Saudi Arabia

Received:2025-12-12 Accepted:2026-02-21 Online:2026-09-18 Published:2026-09-05
Supported by:
The International Cooperation and Exchanges NSFC(22361162607);The National Key Research and Development Program of China(2022YFB3804905);The National Natural Science Foundation of China(22375047);The National Natural Science Foundation of China(22378071);The National Natural Science Foundation of China(22378068);The Natural Science Foundation of Fujian Province(2022J01568);The 111 Project(D17005);The China Postdoctoral Science Foundation(2024M761750)

摘要/Abstract

摘要： 电催化水分解制氢是实现“双碳”目标的重要途径, 但其阳极析氧反应动力学缓慢、热力学势垒高, 严重制约了整体能量效率. 利用热力学电位更低的尿素氧化反应(UOR)取代析氧反应, 不仅可以降低制氢能耗, 还能实现含氮废水的二次利用. 然而, UOR涉及多个中间体的吸脱附行为, 其反应路径的复杂性严重制约了尿素电解的整体效率. 研究表明, 镍基催化剂在工况下的活性相动态演化, 是决定其反应性能的核心因素. 但传统研究大多将催化剂活性相当作静态结构分析, 对反应过程中晶相的可逆转变机制及其与催化活性的内在关联缺乏深入研究. 因此, 精准调控并实时追踪催化剂在电化学条件下的动态结构演变, 已成为发展下一代高效能源转换材料的关键方向.
本研究提出一种锰掺杂工程策略, 通过将锰原子引入NiSe₂晶格, 构建了具有“动态相变触发器”功能的自适应电催化剂. 结果表明, 锰掺杂优化了NiSe₂的局域电子结构, 在阳极电位下引导其电化学重构为高活性的γ-NiOOH相, 并在尿素氧化过程中触发了γ-NiOOH与β-NiOOH之间的可逆结构循环. 原位拉曼光谱直接观测到自适应的相变过程: 锰的引入不仅促进了γ-NiOOH的优先形成, 更关键的是驱动了其在UOR过程中的持续可逆转变. 这种由锰介导的相循环机制有效抑制了γ-NiOOH的不可逆过氧化, 实现了活性位点的动态自再生, 从而在整个UOR过程中维持了优异的催化稳定性. 电化学测试表明, Mn/NiSe₂催化剂展现出低至1.26 V vs. RHE的起始电位, 其全电解池的产氢速率达到284.8 μmol h^-1, 是未掺杂NiSe₂体系的3.9倍. 密度泛函理论计算进一步揭示了锰的引入优化了镍位点的d带中心, 增强了尿素分子在催化剂表面的吸附能力(吸附能从-2.09 eV增至-4.66 eV), 同时显著降低了关键中间体CO(NH₂·NH₂)*中N-H键断裂的能垒(从3.45 eV降至3.11 eV), 从而加速了整体反应动力学. 值得注意的是, 电化学活性表面积归一化分析显示, 锰掺杂虽然大幅增加了电极的电化学活性面积, 但单位面积本征活性变化不明显. 这一看似矛盾的现象恰恰印证了本工作的核心设计理念: 锰的关键作用不在于创造本征活性更高的静态表面, 而在于作为“动态相变触发器”, 在反应工况下诱导并维持具有超高活性的γ-NiOOH相的动态循环, 实现活性位点的持续再生.
综上, 本工作揭示的“掺杂工程-动态相变”机制, 为突破静态设计、构建自适应催化剂提供了新策略. 该“动态相变触发器”理念可拓展至其他能源催化体系, 为开发下一代高性能能源转换材料提供新思路.

关键词: 尿素氧化反应, 氢气, NiOOH, 掺杂, 动态相变

Abstract:

Understanding and guiding the dynamic structural evolution of electrocatalysts under operating conditions is essential for advancing high-performance energy conversion systems. Herein, we report manganese-doped nickel selenide (Mn/NiSe₂) as a model platform to elucidate that dopant-induced reversible phase transitions suppress the irreversible over-oxidation of γ-phase nickel oxyhydroxide (γ-NiOOH), thereby achieving superior urea oxidation reaction (UOR) performance (with a low onset potential of 1.26 V vs. RHE) and accelerating urea-electrolysis hydrogen generation (284.8 μmol h^-1, 3.9 times that of pristine NiSe₂). In-situ Raman spectroscopy reveals that Mn acts as a dynamic phase-transition trigger, modulating the local electronic structure of NiSe₂ to promote its electrochemical reconstruction into highly active γ-NiOOH, and inducing a reversible γ-β structural regeneration during UOR. Density functional theory calculations further show that Mn doping optimizes the electronic state distribution of nickel sites, significantly strengthens urea adsorption (adsorption energy increases from -2.09 to -4.66 eV), and lowers the energy barrier for N-H bond cleavage in the key CO(NH₂·NH₂)* intermediate (from 3.45 to 3.11 eV). This work establishes a dopant-triggered dynamic phase regulation paradigm, and provides a novel strategy for designing self-adaptive electrocatalysts for complex energy conversion reactions.

Key words: Urea oxidation reaction, Hydrogen, NiOOH, Doping, Dynamic phase-transition

张颖贞, 张伟, 黄章政, 蔡伟龙, Yun Hau Ng, 黄剑莹, 赖跃坤. 锰掺杂触发NiSe₂催化剂动态相变以促进尿素氧化反应[J]. 催化学报, 2026, 88: 335-346.

Yingzhen Zhang, Wei Zhang, Zhangzheng Huang, Weilong Cai, Yun Hau Ng, Jianying Huang, Yuekun Lai. Mn-triggered dynamic phase transition in NiSe₂ catalyst via doping engineering for boosted urea electrolysis[J]. Chinese Journal of Catalysis, 2026, 88: 335-346.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65138-8

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图/表 6

Fig. 1. (a) Schematic illustration of Mn/NiSe2. SEM images of NF (b), Mn (c), NiSe2 (d), Mn/NiSe2 (e). HR-TEM images of NiSe2 (f) and Mn/NiSe2 (g). (h) EDS spectrum of Mn/NiSe2.

Fig. 2. High-resolution XPS spectra of Ni 2p (a), Se 3d (b), and Mn 2p (c) of NiSe2 and Mn/NiSe2, respectively. (d) Normalized XANES spectra near Ni K-edge of Ni foil, NiO, NiSe2 and Mn/NiSe2. WT-EXAFS spectra of NiSe2 (e) and Mn/NiSe2 (f) at the Ni K-edge. (g) FT-EXAFS spectra. Structural models of NiSe2 (h) and Mn/NiSe2 (i).

Fig. 3. (a) UOR performance of Mn/NiSe2 prepared at different etching times. E100, Eonset (b), and Ea (c) of NF, Mn, NiSe2, and Mn/NiSe2 for UOR. (d) Pulsed i-t curves recorded at alternating potentials of 1.35 V vs. RHE (oxidation) and 0.90 V vs. RHE (reduction) in 1.0 mol L-1 KOH for NiSe2 and Mn/NiSe2. (e) EIS spectra. (f) Differential pulse voltammetry curves of NiSe2 and Mn/NiSe2 towards UOR. (g) Comprehensive performance comparison of different catalysts. LSV curves (h) and Ea (i) of Mn/NiSe2 for UOR and OER.

Fig. 4. In-situ Raman spectra. NiSe2 for the OER (a) and UOR (b). Mn/NiSe2 for OER (c) and UOR in 1.0 mol L-1 KOH with 0.33 (d), 0.165 (e), and 0.0825 mol L-1 (f) urea. UOR on γ-Mn/NiOOH, in 1.0 mol L-1 KOH with 0.0825 (g) and 0.165 mol L-1 (h) urea.

Fig. 5. (a) Adsorption energy of CO(NH2)2 and H2O on NiOOH and Mn/NiOOH. Charge density difference of CO(NH2)2 adsorbed on NiOOH (b) and Mn/NiOOH (c). (d) The projected COHP of Mn/NiOOH and NiOOH for N-H interaction, respectively. (e) The calculated d-band center of Mn/NiOOH and NiOOH. (f) UOR pathways on NiOOH and Mn/NiOOH.

Fig. 6. (a) Schematic illustration of the urea-assisted water electrolysis for H2 production. Polarization curves (b) and time-dependent H2 production (c) of Mn/NiSe2||Mn/NiSe2 and NiSe2||NiSe2 in 1.0 mol L-1 KOH with 0.33 mol L-1 urea. Polarization curves (d) and H2 generation rate (e) of Mn/NiSe2||Mn/NiSe2 in 1.0 mol L-1 KOH with and without urea. (f) Comparison of cell voltage and H2 production rate for Mn/NiSe2 with other reported electrocatalysts.

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锰掺杂触发NiSe₂催化剂动态相变以促进尿素氧化反应

Mn-triggered dynamic phase transition in NiSe₂ catalyst via doping engineering for boosted urea electrolysis

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