电催化硝酸盐还原合成氨过程中活性氢的原位电化学表征技术

doi:10.61558/2993-074X.3619

电化学（中英文） ›› 2026, Vol. 32 ›› Issue (8): 2517003. doi: 10.61558/2993-074X.3619

电催化硝酸盐还原合成氨过程中活性氢的原位电化学表征技术

李红梅^a, 易梅^b, 晋兆宇^b, 解明皓^c, 郭勇^a^,^*()(), 李盼盼^e^,^*()()

^a 四川大学化学学院，四川成都 610065
^b 电子科技大学基础与前沿研究院，四川成都 611731
^c Materials Science and Engineering Program and Walker Department of Mechanical Engineering, The University of Texas at Austin, Austin, Texas 78712, United States
^d Department of Chemistry, College of Science, University of Sulaimani, Sulaimani City, Kurdistan Region 46002, Iraq
^e 四川大学材料科学与工程学院，四川成都 610065

收稿日期:2026-03-25 修回日期:2026-05-05 接受日期:2026-06-11 发布日期:2026-06-11 出版日期:2026-08-28

In situ Electrochemical Characterization Techniques for Active Hydrogen in Electrocatalytic Nitrate Reduction to Ammonia

Hong-Mei Li^a, Me Yi^b, Zhao-Yu Jin^b, Ming-Hao Xie^c, Khalid M. Omer^d, Yong Guo^a^,^*()(), Pan-Pan Li^e^,^*()()

^a College of Chemistry, Sichuan University, Chengdu 610065, P. R. China
^b Institute of Fundamental and Frontier Sciences, University of Electronic Science and Technology of China, Chengdu 611731, P. R. China
^c Materials Science and Engineering Program and Walker Department of Mechanical Engineering, The University of Texas at Austin, Austin, Texas 78712, United States
^d Department of Chemistry, College of Science, University of Sulaimani, Sulaimani City, Kurdistan Region 46002, Iraq
^e College of Materials Science and Engineering, Sichuan University, Chengdu 610065, P. R. China

Received:2026-03-25 Revised:2026-05-05 Accepted:2026-06-11 Online:2026-06-11 Published:2026-08-28
Contact: *Yong Guo, E-mail: guoy@scu.edu.cn； Pan-Pan Li, E-mail: panpanli@scu.edu.cn E-mail:guoy@scu.edu.cn;panpanli@scu.edu.cn
About author:Author Contributions
Hong-Mei Li: Investigation and original draft preparation.
Me Yi, Zhao-Yu Jin, Ming-Hao Xie, Khalid M. Omer: Investigation, review and editing.
Yong Guo, Pan-Pan Li: Supervision, funding acquisition, writing-review and editing.
All authors read and approved the final manuscript.

摘要/Abstract

摘要：

电催化硝酸盐还原合成氨（NitRR）是一条将环境污染治理与高附加值化学品生产相结合的绿色可持续路径。然而，其活性与选择性受限于瞬态中间体——活性氢（*H）的生成、消耗与动态平衡。实现活性氢的精准调控，必须首先依赖于先进的原位电化学表征技术对其行为进行全面解析。尽管已有综述从调控策略、原位表征总览等角度进行论述，但系统评述如何合理选用原位电化学技术对NitRR中的*H进行专门表征，并清晰界定各技术的“检测对象、定量精度与应用边界”的工作仍属空白。本文旨在填补这一方法学空缺，系统梳理了用于解析NitRR中*H行为的原位电化学表征技术，包括原位谱学技术、原位电化学方法和扫描电化学显微镜技术。基于这些先进表征技术，在该综述中，我们重点构建了一个针对NitRR过程中*H表征的“问题导向”的多层次方法学框架。通过阐述这些技术的原理、应用实例与适用范围，旨在为后续活性氢研究中的表征技术选择提供可靠依据，从而深化对NitRR微观机制的理解。此外，还探讨了未来的研究方向和发展趋势，为推动高效、高选择性绿色氨合成技术的发展提供了相关指导。

关键词: 硝酸盐还原, 活性氢, 原位电化学表征技术, 电合成氨

Abstract:

Electrocatalytic nitrate reduction to ammonia (NitRR) represents a sustainable pathway that integrates environmental remediation with the production of high-value ammonia. However, the activity and selectivity of this process are limited by the generation, consumption, and dynamic equilibrium of the key transient intermediate—active hydrogen (*H). Precise modulation of *H necessitates a comprehensive understanding of its behavior, which relies fundamentally on advanced in situ electrochemical characterization techniques. However, a systematic review dedicated to the rational selection and application of in situ electrochemical techniques for the specific characterization of *H in NitRR, with clear definitions of each technique’s “detectable targets, quantitative accuracy, and application boundaries” remains absent. This review aims to fill this methodological gap by systematically summarizing in situ electrochemical techniques for probing *H behavior in NitRR, including in situ spectroscopic techniques, in situ electrochemical methods, and scanning electrochemical microscopy. We construct a problem-oriented hierarchical methodological framework tailored for *H characterization in NitRR. By detailing the principles, representative applications, and limitations of these techniques, this review provides a reliable guide for selecting appropriate characterization methods in future *H research, thereby deepening the mechanistic understanding of NitRR. Additionally, future research directions and development trends are discussed, offering insights to advance efficient and selective green ammonia synthesis technologies.

Key words: Nitrate reduction reaction, Active hydrogen, In situ electrochemical characterization technique, ammonia electrosynthesis

李红梅, 易梅, 晋兆宇, 解明皓, 郭勇, 李盼盼. 电催化硝酸盐还原合成氨过程中活性氢的原位电化学表征技术[J]. 电化学（中英文）, 2026, 32(8): 2517003.

Hong-Mei Li, Me Yi, Zhao-Yu Jin, Ming-Hao Xie, Khalid M. Omer, Yong Guo, Pan-Pan Li. In situ Electrochemical Characterization Techniques for Active Hydrogen in Electrocatalytic Nitrate Reduction to Ammonia[J]. Journal of Electrochemistry, 2026, 32(8): 2517003.

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链接本文: https://electrochem.xmu.edu.cn/CN/10.61558/2993-074X.3619

https://electrochem.xmu.edu.cn/CN/Y2026/V32/I8/2517003

图/表 10

Representative characterization implication	Spatial location	Binding state and Formation pathway
Adsorbed hydrogen (H_ads)	Specific active sites on a homogeneous metal catalyst surface.	Formed via direct electrochemical reduction of H₂O or hydronium ions (e.g., Volmer step), chemisorbed as M-H bonds on metal atoms.	Serves as the direct hydrogen donor for hydrogenation steps of NO_x. Its coverage and binding energy critically influence intrinsic activity and product selectivity.
Spillover hydrogen	Migrates from the metal active sites where it is generated to the surface of adjacent supports (e.g., oxides, carbon) or secondary active sites.	Forms at metal sites and then migrates to the support via surface diffusion, overcoming an energy barrier. This process is often facilitated by metal-support interactions.	Extends the spatial range of active hydrogen, enabling the support surface or interface regions to participate in hydrogenation, potentially altering reaction pathways.
Interfacial hydrogen	Strictly localized at hetero-interfaces, e.g., the contact perimeter between metal nanoparticles and oxide supports, heterojunctions, or phase boundaries in core-shell structures.	Formed under the modulation of the unique electronic structure at interfaces (e.g., charge transfer, strong metal-support interaction), featuring a binding state that combines characteristics of both the metal and support.	Leverages interfacial synergistic effects, often exhibiting distinct reactivity and selectivity different from bulk metal or support, playing a key role in synergistic catalysis.
Lattice hydrogen	Can be incorporated into the catalyst lattice (bulk) or reside in sub-surface layers.	Hydrogen atoms incorporate into interstitial sites of metals or metal compounds under specific potentials or strong reducing conditions, forming hydrides or solid solutions.	Acts as a hydrogen reservoir, migrating to the surface to participate in reactions; can also indirectly affect catalytic performance by modulating lattice strain/electronic states.

Technique	Sensitivity/Information for *H
SI-SECM	Very High (Quantitative). Directly provides *H surface coverage, lifetime, and consumption kinetics.
Raman	High (Qualitative/Semi-quantitative, providing both direct and indirect evidence). Can directly identify M-H bonds under ideal conditions. However, it is more commonly used for indirect probing, such as reflecting *H behavior by monitoring the conversion of reaction intermediates.
ATR-IR	High (Qualitative/Semi-quantitative, providing both direct and indirect evidence). Under ideal conditions, it can directly detect M-H bonds to provide direct evidence for H. More commonly, it serves as an indirect probe, reflecting the balance of H generation and consumption by monitoring associated vibrational peaks like O-H/N-H.
ESR	High (Qualitative, for paramagnetic H). An authoritative method for detecting paramagnetic H species. However, the signal depends on the trapping agent and cannot be simply equated to the true interfacial *H concentration.
DEMS	Indirect. Reflects *H coverage and the activity of the recombination (HER) pathway indirectly by monitoring the formation kinetics of gaseous products.
CV	Indirect (Semi-quantitative). Estimates the relative H surface coverage by integrating the charge of hydrogen adsorption/desorption peaks, assessing the catalyst’s H generation/storage capacity.
EIS	Indirect. Indirectly estimates the relative coverage or adsorption strength of H by fitting elements related to H adsorption in the equivalent circuit model.
KIE	Indirect (Qualitative/Semi-quantitative). Infers whether the proton transfer step is rate-determining by comparing reaction rates in H₂O vs. D₂O, indirectly reflecting the kinetic importance of *H involvement.
Scavenger (t-BuOH)	Indirect (Qualitative). Infers *H participation indirectly by observing changes in NitRR activity after adding t-BuOH. However, the mechanism is not fully understood, and interferences exist.

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电催化硝酸盐还原合成氨过程中活性氢的原位电化学表征技术

In situ Electrochemical Characterization Techniques for Active Hydrogen in Electrocatalytic Nitrate Reduction to Ammonia

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