电催化硝酸根还原合成氨: 关于铁/铜基催化剂的研究展望

doi:10.1016/S1872-2067(23)64605-4

催化学报 ›› 2024, Vol. 58: 25-36.DOI: 10.1016/S1872-2067(23)64605-4

电催化硝酸根还原合成氨: 关于铁/铜基催化剂的研究展望

陈丽丽^a, 郝彦衡^a, 褚健意^a, 刘松^b, 白凤华^a,*(), 罗文豪^a,*()

^a内蒙古大学化学化工学院, 内蒙古自治区稀土材料化学与物理重点实验室, 内蒙古呼和浩特010021
^b东北林业大学化学化工与资源利用学院, 黑龙江哈尔滨150040

收稿日期:2023-11-02 接受日期:2024-01-15 出版日期:2024-03-18 发布日期:2024-03-28
通讯作者: *电子信箱: w.luo@imu.edu.cn (罗文豪),f.h.bai@imu.edu.cn (白凤华).
基金资助:
国家自然科学基金(22078316);内蒙古大学骏马计划资助(10000-23112101/081);内蒙古青年科技人才资助(NJYT24019)

Electrocatalytic nitrate reduction to ammonia: A perspective on Fe/Cu-containing catalysts

Lili Chen^a, Yanheng Hao^a, Jianyi Chu^a, Song Liu^b, Fenghua Bai^a,*(), Wenhao Luo^a,*()

^aInner Mongolia Key Laboratory of Chemistry and Physics of Rare Earth Materials, College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021, Inner Mongolia, China
^bChemical Engineering and Resource Utilization, College of Chemistry, Northeast Forestry University, Harbin 150040, Heilongjiang, China

Received:2023-11-02 Accepted:2024-01-15 Online:2024-03-18 Published:2024-03-28
Contact: *E-mail: w.luo@imu.edu.cn (W. Luo),f.h.bai@imu.edu.cn (F. Bai).
About author:Fenghua Bai (College of Chemistry and Chemical Engineering, Inner Mongolia University) obtained her Ph.D. in 2008 from Inner Mongolia University (China). Since 2008, she has been working in Inner Mongolia University as an associate professor. In 2012, she was a visiting scholar at University of Exeter in UK. She has been a vice dean of School of Chemistry and Chemical Engineering, Inner Mongolia University since 2015. She was appointed as an associate editor of Mater. Today Sustain. since 2023. Her research interests lie in the development of new catalytic materials for the sustainable production of chemicals from biomass, carbon dioxide, syngas or waste streams.
Wenhao Luo (College of Chemistry and Chemical Engineering, Inner Mongolia University) obtained his Ph.D. in Inorganic Chemistry and Catalysis in 2014 from Utrecht University (Netherlands), supervised by Prof. Bert Weckhuysen and Prof. Pieter Bruijnincx. Afterwards, he worked with Prof. Johannes Lercher as a postdoctoral fellow at Technical University of Munich (Germany). In 2016‒2023, he joined Prof. Tao Zhang's group in Dalian Institute of Chemical Physics (DICP) as an associate professor. He was a visiting scholar in the group of Prof. Andrew Beale in 2017 at University College London (UK). He became a full professor at Inner Mongolia University in 2023, where he has worked since then on heterogeneous catalysis, environmental catalysis, operando spectroscopic characterization, renewable energy, and sustainable chemistry.
Supported by:
National Natural Science Foundation of China(22078316);funding of Inner Mongolia University(10000-23112101/081);funding of Inner Mongolia Youth Science and Technology Talents(NJYT24019)

摘要/Abstract

摘要：

氨(NH₃)是现代工业的重要化工原料之一, 因其具有较高的能量密度、便于运输和储存的特点而被认为是一种非常有前景的储氢材料和可再生能源载体. 电催化硝酸根还原(NO₃RR)是一种理想的绿色合成氨策略, 同时可应用于废水中硝酸根(NO₃^-)污染的去除. 然而, NO₃RR涉及多个电子和质子转移过程, 且存在析氢反应(HER)等竞争反应, 导致NO₃RR的法拉第效率(FE)和选择性较低. 近年来, 精准构筑NO₃RR电催化剂, 实现高效合成氨逐步成为电催化领域的研究热点. 其中, 铁/铜基催化剂因其优异的催化性能和经济可行性而备受关注. 因此, 对近年来具有代表性的铁/铜基催化剂的研究进展进行总结是非常必要的.

本文首先简述了电化学NO₃RR合成氨可能发生的反应路径, 主要围绕铁/铜基电催化剂在NO₃RR中可能涉及的反应历程和相应的中间体. 在此基础上, 针对不同的反应机理系统归纳了三种催化剂设计策略, 包括单原子催化剂策略、双金属催化剂策略以及仿生催化剂策略等. 随后, 重点评析和讨论了原位实时表征技术, 如原位电化学质谱、原位X射线吸收光谱和原位红外/拉曼等, 在电催化NO₃RR合成氨研究领域中的代表性应用案例, 并阐明了原位表征技术的发展和联用对于揭示NO₃RR本征活性位和动态机理的关键作用. 最后, 系统总结了当前NO₃RR所面临的核心挑战并对其未来的研究机遇和发展方向进行了展望, 包括高效催化剂的关键描述符和设计策略, 探究固-液界面的前沿原位表征技术开发, 以及将NO₃RR与绿色反应(如二氧化碳转化和生物质转化等)高效耦联制备高值化学品.

综上所述, 尽管电催化NO₃RR合成氨目前仍面临诸多挑战, 随着实验方案、科学理论和原位表征技术的不断发展, 未来将会出现更多高效且稳定的NO₃RR催化剂. 本文旨在为高效电催化剂的理性开发, 深入理解其动态反应机理与催化剂构效关系提供参考.

关键词: 电催化, 硝酸根还原, 合成氨, 铁/铜基催化剂, 原位表征

Abstract:

Electrocatalytic reduction reaction of nitrate (NO₃RR) to ammonia is becoming ever more pivotal for the sustainable production of NH₃, alleviating the nitrate pollution and even for rebalancing the nitrogen cycle globally. Considerable efforts have been devoted to the rational development of catalyst systems in electrocatalytic NO₃RR to NH₃, and Fe/Cu-containing catalysts have shown significant advantages and are currently in the spotlight which have addressed remarkable attention and academic interest. In this Perspective, we first briefly discuss the possible reaction pathways of electrocatalytic NO₃RR to NH₃. Emphasis is put on the three catalyst approaches for enhancing the NO₃RR performance, based on the selected case studies of the most representative Fe/Cu-containing catalysts. Furthermore, this Perspective assesses the recent progress on the utility and application of the state-of-the-art in situ characterization technologies applied in recent showcases of electrocatalytic NO₃RR to NH₃, with a special focus on spectroscopies. Finally, the open challenges and outlook regarding the rational design of efficient electrocatalysts, the development of correlative in situ characterization technologies and the further coupling promising reactions for production of value-added products are examined for inspiring the future work.

Key words: Electrocatalysis, Nitrate reduction reaction, Ammonia synthesis, Fe/Cu-containing catalyst, In situ characterization

陈丽丽, 郝彦衡, 褚健意, 刘松, 白凤华, 罗文豪. 电催化硝酸根还原合成氨: 关于铁/铜基催化剂的研究展望[J]. 催化学报, 2024, 58: 25-36.

Lili Chen, Yanheng Hao, Jianyi Chu, Song Liu, Fenghua Bai, Wenhao Luo. Electrocatalytic nitrate reduction to ammonia: A perspective on Fe/Cu-containing catalysts[J]. Chinese Journal of Catalysis, 2024, 58: 25-36.

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图/表 8

Fig. 1. Illustration of electrochemical ammonia synthesis from nitrate polluted waste water.

Fig. 2. Possible pathways proposed for Fe/Cu-containing catalysts in the electrocatalytic reduction of nitrate.

Table 1 Fe/Cu-containing catalysts for electrocatalytic NO3RR to NH3.

Cathode	Electrolyte	pH	Faradaic efficiency (%)	Yield	Applied potential	Ref.
Fe-N-C	0.50 mol L^‒1 KNO₃ + 0.1 mol L^‒1 K₂SO₄	7	75	0.46 mmol cm^‒2 h^‒1	-0.66 V vs. RHE	[40]
Fe-N₂O₂	0.5 mol L^‒1 KNO₃ + 0.1 mol L^‒1 K₂SO₄	7	92	9.2 mg h^-1 cm^-2	-0.68 V vs. RHE	[41]
Cu-N-C	0.1 mol L^‒1 KOH + 0.1 mol L^‒1 KNO₃	14	84.7	4.5 mg cm^-2 h^-1	-1.00 V vs. RHE	[42]
Cu-N-C	0.5 mol L^‒1 Na₂SO₄ + 50 mg L^‒1 NO₃^-	9.81	—	9.23 mg h^‒1 mg_cat^‒1	-1.50 V vs. SCE	[25]
Ni₁Cu-SAA	0.5 mol L^‒1 K₂SO₄ + 200 ppm NO₃^-	7	~100	326.7 μmol h^-1 cm^-2	-0.55 V vs. RHE	[43]
Cu/Ni-NC	0.5 mol L^‒1 Na₂SO₄ + 100 ppm NaNO₃	9.81	97.28	5480 mg h^-1 mg_cat^-1 cm^-2	-0.70 V vs. RHE	[44]
Cu₅₀Ni₅₀	1 mol L^‒1 KOH + 100 mmol L^‒1 KNO₃	14	∼95	—	-0.20 V vs. RHE	[19]
PdCu/Cu₂O	0.5 mol L^‒1 Na₂SO₄+ 100 ppm NO₃^-	9.82	94.32	0.190 mmol h^-1 cm^-2	-0.80 V vs. RHE	[45]
Co-Fe@Fe₂O₃	50 ppm NaNO₃ + 0.1 mol L^‒1 Na₂SO₄	7	85.2 ± 0.6	1505.9 μg h^-1 cm^-2	-0.745 V vs. RHE	[46]
Ru₁Cu₁₀/rGO	0.1 mol L^‒1 KNO₃ + 1 mol L^‒1 KOH	14	98	0.38 mmol cm^-2 h^-1	-0.05 V vs. RHE	[47]
Cu/Fe-TiO₂	0.5 mol L^‒1 Na₂SO₄+ 50 ppm NO₃^-	7	91.2	505.73 μg h^-1 cm^-2	-1.40 V vs. SCE	[48]
Fe/Cu-HNG	1 mol L^‒1 KOH + 0.1 mol L^‒1 KNO₃	14	92.51	1.08 mmol h^-1 mg^-1	-0.50 V vs. RHE	[49]
FeNPs@MXene	0.5 mol L^‒1 Na₂SO₄ + 100 mg L^-1 NO₃^-	7	—	0.51 mg h^-1 cm^-2	-0.95 V vs. RHE	[50]
Cu₅₀Co₅₀	0.1 mol L^‒1 KNO₃ +0.5 mol L^‒1 K₂SO₄	7	100 ± 1	4.8 mmol cm^-2 h^-1	-0.20 V vs. RHE	[51]
FeMo-N-C	0.05 mol L^‒1 PBS + 0.16 mol L^‒1 NO₃^-	6.3	94%	18.0 μmol cm^-2 h^-1	-0.45 V vs. RHE	[22]
TiO₂ NTs/CuO_x	0.5 mol L^‒1 Na₂SO₄ + 100 ppm NO₃^-	7	92.23	241.81 μg h^-1 cm^-2	-0.75V vs. RHE	[52]
CuCoSP	0.01 mol L^‒1 NO₃^- + 0.1 mol L^‒1 KOH	13	93.3 ± 2.1	1.17 mmol cm^-2 h^-1	-0.175 V vs. RHE	[53]
Cu-PTCDA	0.1 mol L^‒1 PBS + 500 ppm NO₃^-	7	77 ± 3	436 ± 85 μg h^-1 cm^-2	-0.40 V vs. RHE	[54]

Table 1 Fe/Cu-containing catalysts for electrocatalytic NO3RR to NH3.

Cathode	Electrolyte	pH	Faradaic efficiency (%)	Yield	Applied potential	Ref.
Fe-N-C	0.50 mol L^‒1 KNO₃ + 0.1 mol L^‒1 K₂SO₄	7	75	0.46 mmol cm^‒2 h^‒1	-0.66 V vs. RHE	[40]
Fe-N₂O₂	0.5 mol L^‒1 KNO₃ + 0.1 mol L^‒1 K₂SO₄	7	92	9.2 mg h^-1 cm^-2	-0.68 V vs. RHE	[41]
Cu-N-C	0.1 mol L^‒1 KOH + 0.1 mol L^‒1 KNO₃	14	84.7	4.5 mg cm^-2 h^-1	-1.00 V vs. RHE	[42]
Cu-N-C	0.5 mol L^‒1 Na₂SO₄ + 50 mg L^‒1 NO₃^-	9.81	—	9.23 mg h^‒1 mg_cat^‒1	-1.50 V vs. SCE	[25]
Ni₁Cu-SAA	0.5 mol L^‒1 K₂SO₄ + 200 ppm NO₃^-	7	~100	326.7 μmol h^-1 cm^-2	-0.55 V vs. RHE	[43]
Cu/Ni-NC	0.5 mol L^‒1 Na₂SO₄ + 100 ppm NaNO₃	9.81	97.28	5480 mg h^-1 mg_cat^-1 cm^-2	-0.70 V vs. RHE	[44]
Cu₅₀Ni₅₀	1 mol L^‒1 KOH + 100 mmol L^‒1 KNO₃	14	∼95	—	-0.20 V vs. RHE	[19]
PdCu/Cu₂O	0.5 mol L^‒1 Na₂SO₄+ 100 ppm NO₃^-	9.82	94.32	0.190 mmol h^-1 cm^-2	-0.80 V vs. RHE	[45]
Co-Fe@Fe₂O₃	50 ppm NaNO₃ + 0.1 mol L^‒1 Na₂SO₄	7	85.2 ± 0.6	1505.9 μg h^-1 cm^-2	-0.745 V vs. RHE	[46]
Ru₁Cu₁₀/rGO	0.1 mol L^‒1 KNO₃ + 1 mol L^‒1 KOH	14	98	0.38 mmol cm^-2 h^-1	-0.05 V vs. RHE	[47]
Cu/Fe-TiO₂	0.5 mol L^‒1 Na₂SO₄+ 50 ppm NO₃^-	7	91.2	505.73 μg h^-1 cm^-2	-1.40 V vs. SCE	[48]
Fe/Cu-HNG	1 mol L^‒1 KOH + 0.1 mol L^‒1 KNO₃	14	92.51	1.08 mmol h^-1 mg^-1	-0.50 V vs. RHE	[49]
FeNPs@MXene	0.5 mol L^‒1 Na₂SO₄ + 100 mg L^-1 NO₃^-	7	—	0.51 mg h^-1 cm^-2	-0.95 V vs. RHE	[50]
Cu₅₀Co₅₀	0.1 mol L^‒1 KNO₃ +0.5 mol L^‒1 K₂SO₄	7	100 ± 1	4.8 mmol cm^-2 h^-1	-0.20 V vs. RHE	[51]
FeMo-N-C	0.05 mol L^‒1 PBS + 0.16 mol L^‒1 NO₃^-	6.3	94%	18.0 μmol cm^-2 h^-1	-0.45 V vs. RHE	[22]
TiO₂ NTs/CuO_x	0.5 mol L^‒1 Na₂SO₄ + 100 ppm NO₃^-	7	92.23	241.81 μg h^-1 cm^-2	-0.75V vs. RHE	[52]
CuCoSP	0.01 mol L^‒1 NO₃^- + 0.1 mol L^‒1 KOH	13	93.3 ± 2.1	1.17 mmol cm^-2 h^-1	-0.175 V vs. RHE	[53]
Cu-PTCDA	0.1 mol L^‒1 PBS + 500 ppm NO₃^-	7	77 ± 3	436 ± 85 μg h^-1 cm^-2	-0.40 V vs. RHE	[54]

Fig. 3. (a) NH3 yield rate at different partial current density for different catalysts (NC, FeNP/NC and Fe SAC). The inset shows schematic model of Fe-N4. Adapted with permission [40]. Copyright 2021, Springer Nature. (b) Time profile of NH4+ concentration for different Cu-based SAC and benchmark catalysts at ?1.5 V vs. SCE. The inset shows schematic model of Cu-N4. Adapted with permission [25]. Copyright 2022, Elsevier. (c) The electrocatalytic performance of Cu-NC, Ni-NC and Cu/Ni-NC in electrocatalytic NO3RR to NH3. Adapted with permission [44]. Copyright 2023, Wiley-VCH GmbH. (d) The impact of Cu-Ni alloy ratio on the NO3RR activity and the adsorption intermediates. Adapted with permission [19]. Copyright 2020, American Chemical Society. (e) The electrocatalytic performance of different Cu-Pd bimetallic and benchmark catalysts in NO3RR. Adapted with permission [45]. Copyright 2021, Elsevier. (f) The electrocatalytic performance of different Cu-Fe bimetallic and benchmark catalysts in NO3RR at ?1.4 V vs. SCE. Adapted with permission [48]. Copyright 2023, Elsevier.

Fig. 4. (a) Schematic illustration of FeNPs@MXene for NO3RR. Adapted with permission [50]. Copyright 2022, American Chemical Society. (b) Schematic diagram of Ni foam supported CuCo nanosheets via a one-step electro-deposition method. Adapted with permission [51]. Copyright 2022, Springer Nature. (c) Schematic illustration of the Cu/Co-based binary catalyst’s tandem catalytic process. Adapted with permission [53]. Copyright 2022, Springer Nature.

Fig. 5. (a) DEMS results of the Cu/Cu2O catalyst in NO3RR. Adapted with permission [37]. Copyright 2019, Wiley-VCH. (b) First-order derivatives of the operando XANES spectra recorded at different potentials in NO3RR. (c) Corresponding operando Cu K edge FT-EXAFS spectra at different potentials from fresh, 0.00 to -1.00 V vs. RHE. Adapted with permission [42]. Copyright 2022, American Chemical Society. (d) In situ ATR-FTIR spectra of Pd/NF obtained at -1.4 V vs. RHE in 0.1 mol L?1 NaNO3 solution. Adapted with permission [62]. Copyright 2023, Wiley-VCH. In situ Raman spectra of Ru1Cu10 (e) and Cu (f) during NO3RR at different potentials (V vs. RHE) in a 0.1 mol L?1 KNO3 + 1 mol L?1 KOH mixed solution. Adapted with permission [47]. Copyright 2023, Wiley-VCH.

Fig. 6. The future opportunities and directions for the development of electrocatalytic NO3RR.

Fig. 7. Radar charts of the electrocatalytic NO3RR performances of three catalyst strategies: Representative examples of single-atom catalysts [40?-42] (a), bimetallic catalysts [43,46,47] (b), and biomimetic catalysts (c) [51?-53].

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电催化硝酸根还原合成氨: 关于铁/铜基催化剂的研究展望

Electrocatalytic nitrate reduction to ammonia: A perspective on Fe/Cu-containing catalysts

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