Cu/Fe2O3异质界面协同级联催化硝酸盐高效电还原为氨

doi:10.1016/S1872-2067(24)60194-4

催化学报 ›› 2025, Vol. 68: 404-413.DOI: 10.1016/S1872-2067(24)60194-4

• 论文 • 上一篇

Cu/Fe₂O₃异质界面协同级联催化硝酸盐高效电还原为氨

张翔, 李苇杭, 张进, 周豪慎, 钟苗^*()

南京大学现代工程与应用科学学院, 先进微结构协同创新中心, 固体微结构国家实验室, 地球关键材料循环前沿科学中心, 江苏南京 210023

收稿日期:2024-09-14 接受日期:2024-11-04 出版日期:2025-01-18 发布日期:2025-01-02
通讯作者: * 电子信箱: miaozhong@nju.edu.cn (钟苗).
基金资助:
国家自然科学基金(22272078);国家自然科学基金(22409087);催化基础国家重点实验室开放基金(2024SKL-A-016);江苏省“双创人才”计划

Efficient nitrate electroreduction to ammonia via synergistic cascade catalysis at Cu/Fe₂O₃ hetero-interfaces

Xiang Zhang, Weihang Li, Jin Zhang, Haoshen Zhou, Miao Zhong^*()

Collaborative Innovation Centre of Advanced Microstructures, National Laboratory of Solid State Microstructures, Frontiers Science Center for Critical Earth Material Cycling, College of Engineering and Applied Sciences, Nanjing University, Nanjing 210023, Jiangsu, China

Received:2024-09-14 Accepted:2024-11-04 Online:2025-01-18 Published:2025-01-02
Contact: * E-mail: miaozhong@nju.edu.cn (M. Zhong).
Supported by:
National Natural Science Foundation of China(22272078);National Natural Science Foundation of China(22409087);State Key Laboratory of Catalysis(2024SKL-A-016);“Innovation and Entrepreneurship of Talents plan” of Jiangsu Province

摘要/Abstract

摘要：

氨(NH₃)是一种重要的化学品, 广泛用于合成化肥、药品、纺织品和其他行业. 传统Haber-Bosch工艺用于NH₃合成, 该工艺需高温高压条件. 另一方面, 工业废水中的过量硝酸盐(NO₃⁻)会导致水体污染. 通过电催化手段, 可以高效率、高选择性的将NO₃⁻还原为NH₃, 不仅能够处理环境问题, 还提供了一种绿色可持续的NH₃合成途径. 然而, NO₃⁻还原(NO₃⁻RR)过程复杂, 涉及8电子和9质子的转移, 并可能伴随强烈的析氢竞争反应(HER). 单一金属催化剂难以在低电位下同时具备对NO₃⁻和亚硝酸根(NO₂⁻)的高效吸附和还原能力.
针对该问题, 本文设计了Cu-Fe₂O₃异质结构催化剂, 利用其界面上的双位点有效分步催化实现NO₃⁻到NO₂⁻和NO₂⁻到NH₃的电还原过程. 扫描电镜、透射电镜、X-射线衍射和X-射线光电子能谱等表征手段证实了Cu和Fe₂O₃在泡沫镍基底上的致密生长, 并确定了其价态和体相组成. 在0.1 mol L⁻¹ KNO₃和1 mol L⁻¹ KOH的电解液中, Cu-Fe₂O₃在−0.27 V_RHE下展示了接近100%的NH₃法拉第效率, 并在−0.35 V_RHE下实现了2.71 mmol h⁻¹ cm⁻²的高NH₃产率, 远超单独使用Cu或Fe₂O₃催化剂的性能. 同时, −0.27 V_RHE下的半池能量效率超过35%, 且在宽NO₃⁻浓度范围内(0.05−1 mol L⁻¹), NH₃选择性均保持在90%以上. 通过¹⁵N同位素标记确定了氮源完全来自KNO₃. 计时电流测试表明, 反应3 h后, NO₃⁻的去除率高达98%. 线性扫描伏安法测试(LSV)结果表明, Cu催化剂相较于Fe₂O₃具有更正的NO₃⁻还原到NO₂⁻起始电位(0.39 V_RHE), 并在−0.2到−0.3 V_RHE区间里出现NO₂⁻积累的电流平台. 由此可见, Cu对NO₃⁻的吸附和转化为NO₂⁻的能力相较于Fe₂O₃更为优异. 然而由于Cu对*N的吸附能力较弱, 导致NO₂⁻更容易脱附并在表面积累. 相比之下, Fe₂O₃在NO₂⁻溶液中的起始电位(>0.3 V_RHE)远高于在NO₃⁻溶液中的起始电位(0.1 V_RHE), 表明其具有较强的*N吸附能力, 能够更有效地将NO₂⁻进一步还原为NH₃. 原位拉曼和原位红外光谱分析进一步证实了NO₃⁻RR过程中中间体的生成, Cu上的NO₂⁻出现电位(0.3 V_RHE)明显早于Fe₂O₃ (0.1 V_RHE). Fe₂O₃上NO₂⁻和NH₃的起始电位相同(0.1 V_RHE), 而Cu-Fe₂O₃上NO₂⁻和NH₃的反应起始电位(0.4 V_RHE)显著正于Cu和Fe₂O₃的反应起始电位, 这进一步证明了Cu将NO₃⁻还原为NO₂⁻, Fe₂O₃将NO₂⁻还原为NH₃的级联催化, 与LSV结论一致.
本文为NO₃⁻电还原提供了一种催化剂设计的新思路, 通过Cu-Fe₂O₃异质结构实现了更低的反应开启电位(0.4 V_RHE). 在低工作电位下(−0.27 V_RHE)实现了423 mA cm⁻²的电流密度, 接近100%的NH₃选择性和98%的NO₃⁻转化率, 展现了该级联催化剂在可持续NH₃合成和废水处理中的潜力.

关键词: 电催化, 起始电位, 硝酸盐还原成氨, 级联催化, 异质界面

Abstract:

Electrochemical nitrate (NO₃⁻) reduction offers a promising route for ammonia (NH₃) synthesis from industrial wastewater using renewable energy. However, achieving selective and active NO₃⁻ to NH₃ conversion at low potentials remains challenging due to complex multi-electron transfer processes and competing reactions. Herein, we tackle this challenge by developing a cascade catalysis approach using synergistic active sites at Cu-Fe₂O₃ interfaces, significantly reducing the NO₃⁻ to NH₃ at a low onset potential to about +0.4 V_RHE. Specifically, Cu optimizes *NO₃ adsorption, facilitating NO₃⁻ to nitrite (NO₂⁻) conversion, while adjacent Fe species in Fe₂O₃ promote the subsequent NO₂⁻ reduction to NH₃ with favorable *NO₂ adsorption. Electrochemical operating experiments, in situ Raman spectroscopy, and in situ infrared spectroscopy consolidate this improved onset potential and reduction kinetics via cascade catalysis. An NH₃ partial current density of ~423 mA cm⁻² and an NH₃ Faradaic efficiency (FE_NH3) of 99.4% were achieved at −0.6 V_RHE, with a maximum NH₃ production rate of 2.71 mmol h⁻¹ cm⁻² at −0.8 V_RHE. Remarkably, the half-cell energy efficiency exceeded 35% at −0.27 V_RHE (80% iR corrected), maintaining an FE_NH3 above 90% across a wide range of NO₃⁻ concentrations (0.05−1 mol L⁻¹). Using ¹⁵N isotopic tracing, we confirmed NO₃⁻ as the sole nitrogen source and attained a 98% NO₃⁻ removal efficiency. The catalyst exhibit stability over 106-h of continuous operation without noticeable degradation. This work highlights distinctive active sites in Cu-Fe₂O₃ for promoting the cascade NO₃⁻ to NO₂⁻ and NO₂⁻ to NH₃ electrolysis at industrial relevant current densities.

Key words: Electrocatalysis, Reaction onset potential, Nitrate reduction to ammonia, Cascade catalysis, Heterogeneous interface

张翔, 李苇杭, 张进, 周豪慎, 钟苗. Cu/Fe₂O₃异质界面协同级联催化硝酸盐高效电还原为氨[J]. 催化学报, 2025, 68: 404-413.

Xiang Zhang, Weihang Li, Jin Zhang, Haoshen Zhou, Miao Zhong. Efficient nitrate electroreduction to ammonia via synergistic cascade catalysis at Cu/Fe₂O₃ hetero-interfaces[J]. Chinese Journal of Catalysis, 2025, 68: 404-413.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60194-4

https://www.cjcatal.com/CN/Y2025/V68/I1/404

图/表 5

Fig. 1. (a) Schematic diagram of the cascade catalysis of NO3? electroreduction to NH3 on the Cu-Fe2O3 electrode. (b) LSV curves comparing Cu-Fe2O3, Cu, and Fe2O3 deposited on Ni foam in 1 mol L?1 KOH with 0.1 mol L?1 KNO3 (solid line) and without KNO3 (dashed line) at a scan rate of 5 mV s?1 (80% iR corrected). The orange line indicates a current density of 10 mA cm?2. (c) LSV curve at +0.1 to +0.4 VRHE. The gray line indicates the cathodic current density of 1 mA cm?2.

Fig. 2. Electrochemical analysis of NO3?RR using Cu-Fe2O3, Cu, and Fe2O3 catalysts loaded on Ni foams. LSV curves of Cu (a), Fe2O3 (b), and Cu-Fe2O3 (c) catalysts on Ni foams in 1 mol L?1 KOH and 0.1 mol L?1 KNO3 (80% iR corrected). (d) Tafel slopes of Cu, Fe2O3, and Cu-Fe2O3 catalysts on Ni foams in 1 mol L?1 KOH and 0.1 mol L?1 KNO3. FE (e) and yield rate (f) of NH3 for the catalysts at different potentials. (g) Partial current densities of NH3 (80% iR corrected) at different potentials with different catalysts. (h) EE of NH3 (80% iR corrected) with different catalysts. (i) FE and yield rate of NH3 for catalysts with different valence states of Fe species combined with Cu at ?0.6 VRHE.

Fig. 3. In situ Raman spectra at various potentials of Cu-Fe2O3 (a), Cu (b), and Fe2O3 (c). (d) In situ FTIR spectroscopy of Cu-Fe2O3 in 1 mol L?1 KOH and 0.1 mol L?1 KNO3.

Fig. 4. Electrochemical NO3?RR performance on Cu-Fe2O3 electrodes. (a) UV-vis absorption spectra of the electrolytes after the reduction reaction in 1 mol L?1 KOH with and without 0.1 mol L?1 KNO3 at ?0.6 VRHE and at OCP. The electrolyte was diluted to 500 times in volume before measurement. (b) 1H-NMR spectra of the NO3?RR electrolyte using K14NO3 and K15NO3 as the N source in 1 mol L?1 KOH electrolyte at ?0.6 VRHE. The reduction reaction was performed for 1 h. (c) NH3 yield rates at ?0.6 VRHE, measured using Nessler's reagent method and 1H-NMR spectroscopy. (d) LSV curves of Cu-Fe2O3 electrodes with different KNO3 concentrations in 1 mol L?1 KOH (80% iR corrected). (e) NH3 FE and yield rate of Cu-Fe2O3 at ?0.6 VRHE. (f) The time-dependent concentrations of NO3?, NO2? and NH3 and the corresponding FE during the NO3?RR process on Cu-Fe2O3 at ?0.6 VRHE. (g) The time-dependent concentrations of NO3?, NO2? and NH3 during the NO3?RR process using Cu-Fe2O3 at ?0.6 VRHE. (h) NO3?RR durability test using Cu-Fe2O3 at ?400 mA cm?2 in 1 mol L?1 KOH + 1 mol L?1 KNO3.

Fig. 5. Structure and composition characterization of the Cu-Fe2O3 catalyst after the 1-h NO3?RR. (a) SEM images of the Cu-Fe2O3 catalyst. (b-d) HRTEM images and the corresponding EDX elemental mapping images of Cu-Fe2O3. Fe 2p (e) and Cu 2p (f) narrow-scan XPS spectra of Cu-Fe2O3. (g) XRD patterns of Cu-Fe2O3, Cu, and Fe2O3 loaded on Ni foam.

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Cu/Fe₂O₃异质界面协同级联催化硝酸盐高效电还原为氨

Efficient nitrate electroreduction to ammonia via synergistic cascade catalysis at Cu/Fe₂O₃ hetero-interfaces

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