金属氧化物电催化硝酸盐还原合成氨研究进展

doi:10.15541/jim20240102

无机材料学报 ›› 2024, Vol. 39 ›› Issue (9): 979-991.DOI: 10.15541/jim20240102 CSTR: 32189.14.10.15541/jim20240102

金属氧化物电催化硝酸盐还原合成氨研究进展

杨鑫¹^,²^,³(), 韩春秋²^,⁴, 曹玥晗²(), 贺桢², 周莹¹^,²()

1.西南石油大学油气藏地质及开发工程全国重点实验室, 成都 610500
2.西南石油大学新能源与材料学院, 成都 610500
3.天府永兴实验室, 成都 610213
4.三峡大学材料与化工学院, 宜昌 443002

收稿日期:2024-03-05 修回日期:2024-04-07 出版日期:2024-09-20 网络出版日期:2024-04-19
通讯作者: 曹玥晗, 副研究员. E-mail: yhcao419@163.com;
周莹, 教授. E-mail: yzhou@swpu.edu.cn
作者简介:杨鑫(1999-), 男, 硕士研究生. E-mail: yangxin9633@outlook.com
基金资助:
国家重点研发计划(2020YFA0710000);天府永兴实验室科技攻关任务重大项目(2023KJGG15);成都市国际科技合作项目(2021-GH02-00052-HZ)

Recent Advances in Electrocatalytic Nitrate Reduction to Ammonia Using Metal Oxides

YANG Xin¹^,²^,³(), HAN Chunqiu²^,⁴, CAO Yuehan²(), HE Zhen², ZHOU Ying¹^,²()

1. National Key Laboratory of Oil and Gas Reservoir Geology and Exploitation, Southwest Petroleum University, Chengdu 610500, China
2. School of New Energy and Materials, Southwest Petroleum University, Chengdu 610500, China
3. Tianfu Yongxing Laboratory, Chengdu 610213, China
4. College of Materials and Chemical Engineering, Three Gorges University, Yichang 443002, China

Received:2024-03-05 Revised:2024-04-07 Published:2024-09-20 Online:2024-04-19
Contact: CAO Yuehan, associate professor. E-mail: yhcao419@163.com;
ZHOU Ying, professor. E-mail: yzhou@swpu.edu.cn
About author:YANG Xin (1999-), male, Master candidate. E-mail: yangxin9633@outlook.com
Supported by:
National Key R&D Program of China(2020YFA0710000);Key Grant Technologies Project of Tianfu Yongxing Laboratory(2023KJGG15);International Science and Technology Cooperation Project of Chengdu(2021-GH02-00052-HZ)

摘要/Abstract

摘要：

氨不仅是合成化肥的主要原料之一, 而且是一种高能量密度的新型燃料。近年来, 电催化硝酸盐还原合成氨作为一种绿色可持续的合成途径, 具有能源利用率高、碳排放量低等特点, 因此受到了广泛关注, 有望替代高能耗和高碳排放的Haber-Bosch法来高效合成氨。然而, 目前该技术的反应效率、产物选择性以及催化材料稳定性都难以满足应用需求, 迫切需要寻找高效的催化材料, 从而促进电催化硝酸盐还原合成氨技术的进一步发展。近年来, 金属氧化物催化材料在电催化硝酸盐还原合成氨领域展现出良好的催化性能。基于此, 本文综述了金属氧化物电催化硝酸盐还原合成氨的研究进展, 重点概述了电催化硝酸盐还原合成氨的反应机理, 系统介绍了用于电催化硝酸盐还原合成氨的Cu基、Fe基和Ti基等典型催化材料, 以及通过形貌调控、表面重构、氧空位构造、元素掺杂和金属助催化材料负载等策略提高催化反应效率、产物选择性及催化材料稳定性的最新研究进展。最后, 展望了电催化硝酸盐还原合成氨领域面临的挑战及未来的研究方向。

关键词: 电催化, 硝酸盐还原合成氨, 金属氧化物, 调控策略, 综述

Abstract:

Ammonia serves not only as a primary raw material in synthetic fertilizers, but also as a novel high-energy- density fuel. In recent years, electrocatalytic nitrate reduction for ammonia synthesis has gained extensive attention as a green and sustainable approach due to its potential as an eco-friendly and sustainable way that could replace the energy-intensive and high-carbon-emission Haber-Bosch process. Nevertheless, the efficient electrocatalytic ammonia synthesis is still hampered by low reaction efficiency and product selectivity as well as catalyst stability. Hence, there is a pressing need to develop efficient catalysts to advance electrocatalytic nitrate reduction for ammonia synthesis. Recently, metal oxide catalysts have been at the center of attention for their superior performance in electrocatalytic nitrate reduction for ammonia synthesis. This review consolidates the developments of metal oxide electrocatalysts converting nitrate to ammonia, focusing on elucidating the reaction mechanism and introducing typical metal-based (Cu, Fe, Ti, etc.) catalysts. Additionally, it discusses the latest research progress in enhancing catalytic reaction efficiency, product selectivity, and material stability through strategies like morphology control, surface reconstruction, oxygen vacancy engineering, element doping, metal-assisted catalyst loading, etc. Finally, the paper outlines the challenges and future research directions in the realm of electrocatalytic nitrate reduction for ammonia synthesis.

Key words: electrocatalysis, nitrate reduction to ammonia, metal oxide, modulation strategy, review

中图分类号:

TQ113
TQ13

杨鑫, 韩春秋, 曹玥晗, 贺桢, 周莹. 金属氧化物电催化硝酸盐还原合成氨研究进展[J]. 无机材料学报, 2024, 39(9): 979-991.

YANG Xin, HAN Chunqiu, CAO Yuehan, HE Zhen, ZHOU Ying. Recent Advances in Electrocatalytic Nitrate Reduction to Ammonia Using Metal Oxides[J]. Journal of Inorganic Materials, 2024, 39(9): 979-991.

图/表 9

图1 电催化硝酸盐还原制N2/NH3主要过程

Fig. 1 Main process of electrocatalytic production for N2/NH3

表1 用于eNitRR研究的金属氧化物的性能

Table 1 Properties of metal oxides used in the study of eNitRR

Catalyst	NH₃ yield rate	Faraday efficiency, FE/%	Stability/h	Ref.
TiO_2-_x	45.00 µmol·h^-1·mg^-1	85.00	16.00	[40]
Ru/TiO₂	35.35 µmol·h^-1·cm^-2	>90.00	4.50	[41]
Pd/TiO₂	66.00 μmol·h^-1·cm^-2	92.00	12.00	[42]
PdCu/TiO_2-_x	322.70 μmol·h^-1·cm^-2	80.10	48.00	[43]
Co-TiO₂/TP	1127.00 μmol·h^-1·cm^-2	98.20	24.00	[44]
Fe₂TiO₅	0.73 mmol·h^-1·mg^-1	87.60	6.00	[45]
ZnCr₂O₄	1197.65 μmol·h^-1·mg^-1	90.20	15.00	[46]
Fe₂O₃	328.17 μmol·h^-1·cm^-2	69.80	5.00	[47]
Fe₃O₄/SS	596.76 μmol·h^-1·cm^-2	91.50	4.00	[48]
Cu/Fe₃O₄	10.56 mmol·h^-1·mg^-1	100.0	-	[49]
NiO₄	1.83 mmol·h^-1·mg^-1	94.70	72.00	[32]
Co₃O₄/NiO	6.93 μmol·h^-1·mg^-1	-	3.00	[50]
Cu/Cu₂O	219.80 μmol·h^-1·cm^-2	93.90	12.00	[51]
Cu₂O	0.14 mmol·h^-1·cm^-2	99.80	20.00	[52]
PdCu/Cu₂O	190.00 μmol·h^-1·cm^-2	94.30	12.00	[28]
CoO NC/graphene	25.63 mmol·h^-1·mg^-1	>98.00	6.00	[53]
Cu/Co₃O₄	1.11 mmol·h^-1·cm^-2	100.70	60.00	[54]
S/Co₃O₄	174.20 μmol·h^-1·mg^-1	89.90	7.00	[55]
Cu/MnO_x	1.72 mmol·h^-1·mg^-1	86.20	6.00	[56]
CuO@MnO₂/CF	0.24 mmol·h^-1·cm^-2	94.90	10.00	[57]

图2 金属氧化物选择性调控电催化硝酸盐还原合成NH3

Fig. 2 Metal oxides for selective regulation of eNitRR

图3 Cu/Cu2O NWAs的催化性能[63]

Fig. 3 Catalytic performance of Cu/Cu2O NWAs[63] (a) Nitrate conversion efficiency and FE at different voltages; (b) Nuclear magnetic resonance (NMR) spectra of nitrogen sources; (c) Raman spectra; (d) In-situ mass spectrometry spectra; (e) Free energy image

图4 Cu/Cu2O的催化性能表征[51]

Fig. 4 Characterization of catalytic performance of Cu/Cu2O[51] (a) FE of NH3 and NO2− at different potentials; (b) Corresponding NH3 generation rates and bias current densities at different potentials; (c) Potential-induced electrocatalytic reconstruction of Cu2O cube; (d) Free energy diagram

图5 Fe3O4/SS的催化性能表征[48]

Fig. 5 Characterization of catalytic performance of Fe3O4/SS[48] (a) Current density of different product fractions; (b) Ammonia-producing activity of Fe3O4/SS; (c) Cyclic test of Fe3O4/SS at -0.50 V; (d) Free energy diagram

图6 Cu-Fe3O4的催化性能表征[49]

Fig. 6 Characterization of catalytic performance of Cu-Fe3O4[49] (a) NH3 yield and FE of Cu-Fe3O4; (b) Comparison of ammonia yields of different catalytic materials; (c) Free energy diagram

图7 TiO2-x的催化性能表征[40]

Fig. 7 Characterization of catalytic performance of TiO2-x[40] (a) NO3- conversion rates and NH3 FE of TiO2-x; (b) TiO2-x ammonia production cycle test; (c) Differential electrocatalytic mass spectra; (d, e) Free energy diagrams of (d) TiO2 and (e) TiO2-x

图8 PdCu NPs/TiO2-x的催化性能表征[43]

Fig. 8 Characterization of catalytic performance of PdCu NPs/TiO2-x[43] (a) Ammonia production activity and FE of different materials; (b) Product selectivity of different materials; (c, d) Partial crystal orbital layouts of (c) TiO2-x and (d) PdCu NPs/TiO2-x; (e) Density of states diagram; (f) Schematic diagram of catalytic kinetics of the d band center

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金属氧化物电催化硝酸盐还原合成氨研究进展

Recent Advances in Electrocatalytic Nitrate Reduction to Ammonia Using Metal Oxides

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