次磷酸根界面改性Co(OH)2/Cu纳米线实现2.8 A·cm‒2高电流密度下硝酸盐还原制氨

doi:10.1016/S1872-2067(26)65241-2

催化学报 ›› 2027, Vol. 92: 365-375.DOI: 10.1016/S1872-2067(26)65241-2

次磷酸根界面改性Co(OH)₂/Cu纳米线实现2.8 A·cm^‒2高电流密度下硝酸盐还原制氨

周瑞晗^a, 夏缇萱^a, 杨迎晨^a, 徐东波^a^,^b^,^*(), 施伟东^a^,^c^,^*()

^a 江苏大学化学化工学院, 江苏镇江 212013
^b 南京工程学院江苏省先进结构材料及应用技术重点实验室, 江苏南京 211167
^c 江苏科技大学环境与化学工程学院, 江苏镇江 212100

收稿日期:2026-02-28 接受日期:2026-05-15 出版日期:2027-01-02 发布日期:2026-10-30
通讯作者: *电子信箱: xudb39@ujs.edu.cn (徐东波),
swd1978@ujs.edu.cn (施伟东).
基金资助:
国家自然科学基金(22225808);国家自然科学基金(U24A20551);江苏省自然科学基金(BK20230551);江苏省先进结构材料与应用技术重点实验室开放项目(ASMA202503)

Co(OH)₂/Cu NWs with interface modification of hypophosphite ions for sustainable ammonia synthesis from nitrate at ~2.8 A·cm^-2

Ruihan Zhou^a, Tixuan Xia^a, Yingchen Yang^a, Dongbo Xu^a^,^b^,^*(), Weidong Shi^a^,^c^,^*()

^a School of Chemistry and Chemical Engineering, Jiangsu University, Zhenjiang 212013, Jiangsu, China
^b Jiangsu Key Laboratory of Advanced Structural Materials and Application Technology, Nanjing Institute of Technology, Nanjing 211167, Jiangsu, China
^c School of Environmental and Chemical Engineering, Jiangsu University of Science and Technology, Zhenjiang 212100, Jiangsu, China

Received:2026-02-28 Accepted:2026-05-15 Online:2027-01-02 Published:2026-10-30
Contact: *E-mail: xudb39@ujs.edu.cn (D. Xu),
swd1978@ujs.edu.cn (W. Shi).
Supported by:
National Natural Science Foundation of China(22225808);National Natural Science Foundation of China(U24A20551);Natural Science Foundation of Jiangsu Province(BK20230551);Opening Project of Jiangsu Key Laboratory of Advanced Structural Materials and Application Technology(ASMA202503)

摘要/Abstract

摘要：

近年来, 电化学硝酸盐还原(NO₃RR)被视为实现绿色可持续合成氨的一种有效手段. 然而, NO₃RR涉及复杂的多电子转移与质子化过程, 缓慢的反应动力学限制了氨的产率和电流密度, 复杂的反应路径也对产物的选择性构成了挑战. 尤其是在大电流密度条件下, 析氢(HER)竞争反应以及含氮中间副产物的生成造成了法拉第效率(FE)的下降. 为了满足规模化工业生产的需要, 设计能够在高电流密度条件下维持高FE的硝酸盐到氨转化的电催化剂至关重要. 当前针对NO₃RR电催化剂的研究不断取得新的突破, 但是实现高产率与大电流密度大多依赖提高硝酸盐浓度, 考虑到硝酸盐本身的经济价值远远高于氨, 现实情况下不可能直接使用硝酸盐作为合成氨的原料, 自然水体与污水中的硝酸盐浓度很低, 通过富集浓缩得到高浓度硝酸盐溶液的成本极大, 电催化剂在有限硝酸盐浓度下的性能更具有实际意义.

本文通过电化学沉积的方法结合催化剂的原位重构, 在Cu纳米线(Cu NWs)基底上负载了次磷酸根修饰的氢氧化钴纳米片(P-Co(OH)₂), 构建了P-Co(OH)₂/Cu NWs串联催化剂, 硝酸根先在铜表面快速转化为亚硝酸根, 随后亚硝酸根在P-Co(OH)₂表面进一步脱氧和质子化生成氨, 催化剂在浓度为0.1 mol·L^-1的硝酸盐溶液中在-0.7 V vs. RHE的工作电位下实现了96.8%的法拉第效率, 在-1 V vs. RHE的工作电位下, 达到了204.3 mg·h^-1·cm^-2的高氨产率, 法拉第效率仍能维持在93.4%, 远远超过Cu NWs基底, 并且能够在2.8 A·cm^-2平均电流密度下稳定运行20个循环(每个循环1 h)后性能没有衰减. X射线光电子能谱和红外光谱证实了次磷酸根的存在. DMPO-H自旋捕获测试表明, 次磷酸根加速了水的解离产生活性氢自由基, 并且作用于NO₃RR过程. 原位红外光谱结果表明, P-Co(OH)₂/Cu NWs有更强的脱氧和加氢活性. 循环伏安法测试与原位拉曼光谱结果表明, 次磷酸根有利于诱导生成和保持金属态钴活性相. 通过密度泛函理论计算发现, 在NO₃RR过程中原位生成的Co⁰调节反应中间体吸附, 优化反应路径, 降低了电位决定步骤*NO到*NOH的反应能垒, 对*H的强吸附还避免了过度的HER竞争反应. 通过对比金属Co与Co(OH)₂中表面钴原子态密度差异发现, 金属Co中Co原子的d带中心靠近体系的费米能级, 从而调节了NO₃RR的中间体吸附与电子转移过程.

综上, 本工作通过简单的电化学沉积制备了P-Co(OH)₂/Cu NWs串联催化剂, 该催化剂在有限硝酸盐浓度下展现出卓越的NO₃RR性能, 其在大电流密度工况下的稳定性也得到验证, 并且通过原位的测试和理论计算揭示了次磷酸根的作用机制, 为设计高性能NO₃RR电催化剂提供了新的思路.

关键词: 硝酸盐还原, 工业电流密度, 次磷酸根, 氨, 界面修饰

Abstract:

Ammonia production via nitrate electroreduction (NO₃RR) offers an environmentally benign alternative, yet it is still extremely difficult to simultaneously attain superior Faradaic efficiency and long-lasting durability when operating at the high current densities. Herein, we report a self-supporting electrode comprising Cu nanowires uniformly coated with cobalt hydroxide incorporating surface-coordinated hypophosphite ions (H₂PO₂^-) (denoted as P-Co(OH)₂/Cu NWs), directly fabricated on Cu foam. The P-Co(OH)₂/Cu NWs catalyst exhibited remarkable NO₃RR performance in 0.1 mol·L^-1 NaNO₃/1 mol·L^-1 NaOH, producing NH₃ at a rate of 204.3 mg·h^-1·cm^-2 (-1.0 V) with a peak Faradaic efficiency of 96.8% (-0.7 V), both potentials referenced to RHE. Notably, the electrode maintains stable electroactivity and NH₃ selectivity over 20 consecutive test cycles (1 h per cycle) under approximately 2.8 A·cm^-2. In-situ attenuated total reflection Fourier transform infrared spectroscopy reveals that the P-Co(OH)₂/Cu NWs electrode promotes enhanced deoxygenation of *NO₃ and deep hydrogenation of *NO_x intermediates. Cyclic voltammetry test and In-situ Raman spectroscopy demonstrate that the incorporated H₂PO₂^- induce and stabilize the in-situ formation of metallic Co⁰ phase under operative electrolysis conditions. Density functional theory calculations further elucidate that the metallic Co⁰ phase, generated in situ during NO₃RR, optimizes the adsorption energetics of *NOH, thereby substantially facilitating the energy-demanding step (*NO → *NOH) relative to Co(OH)₂, while concurrently strengthening *H adsorption. This work presents a viable electrode design strategy for securing efficient and stable electrocatalytic NO₃^--to-NH₃ conversion under high-rate operation.

Key words: Nitrate reduction, Industrial current density, Hypophosphite ion, Ammonia, Interface modification

周瑞晗, 夏缇萱, 杨迎晨, 徐东波, 施伟东. 次磷酸根界面改性Co(OH)₂/Cu纳米线实现2.8 A·cm^‒2高电流密度下硝酸盐还原制氨[J]. 催化学报, 2027, 92: 365-375.

Ruihan Zhou, Tixuan Xia, Yingchen Yang, Dongbo Xu, Weidong Shi. Co(OH)₂/Cu NWs with interface modification of hypophosphite ions for sustainable ammonia synthesis from nitrate at ~2.8 A·cm^-2[J]. Chinese Journal of Catalysis, 2027, 92: 365-375.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65241-2

https://www.cjcatal.com/CN/Y2027/V92/I1/365

图/表 5

Fig. 1. (a) Schematic diagram depicting the preparation of P-Co(OH)2. SEM image of Cu(OH)2 NWs (b), Cu NWs (c), and P-Co(OH)2/Cu NWs (d). EDS mapping images (e), TEM images (f), and HRTEM images (g) of P-Co(OH)2/Cu NWs.

Fig. 2. XRD pattern (a), CV curves (b), Co 2p (c), O 1s (d) XPS spectra, and FT-IR spectra (e) of P-Co(OH)2/Cu NWs and Co(OH)2/Cu NWs.

Fig. 3. The potential-dependent FE of ammonia (a), The ammonia yield rate (b), and the selectivity of NO2- (c) for Cu NWs, Co(OH)2/Cu NWs, P-Co(OH)2/Cu NWs and P-Co(OH)2/CC in 0.1 mol·L-1 NaNO3 and 1 mol·L-1 NaOH. (d) NO3- removal of catalysts measured in a 1 mol·L-1 NaOH with 0.1 mol·L-1 NO3- electrolyte at -0.7 V vs. RHE. (e) The NH3 yield rate and FE of P-Co(OH)2/Cu NWs at -1 V vs. RHE in cycling tests conducted continuously for 20 h. (f) 1H NMR spectra using 15NO3- and 14NO3- over P-Co(OH)2/Cu NWs. (g) comparison of NO3RR performance of P-Co(OH)2/Cu NWs with reported state-of-the-art electrocatalysts in 0.1 mol·L-1 NO3-. (h) comparison of NH3 yield rate for recently reported state-of-the-art electrocatalysts with different concentrations of NO3-.

Fig. 4. (a,b) CV curves in 1 mol·L-1 NaOH. (c) CV curves in 1 mol·L-1 NaOH + 0.1 mol·L-1 NaNO3. In-situ Raman spectra (d,e), in-situ ATR-IR spectra (f,g), and EPR spectra (h,i) in 1 mol·L-1 NaOH with and without 0.1 mol·L-1 NaNO3 of P-Co(OH)2/Cu NWs, Co(OH)2/Cu NWs and Cu NWs.

Fig. 5. (a) Gibbs free energy diagram of NO3- to NO2- generated during NO3RR. (b) Adsorption energy of NO3- and NO2-. (c) The hydrogen evolution reaction pathways on Cu (111), Co(OH)2 (101), and Co(101). (d) Gibbs free energy diagram of NO2- to NH3 generated during NO3RR. (e) PDOS along with d-band center for Co(OH)2 and Co.

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次磷酸根界面改性Co(OH)₂/Cu纳米线实现2.8 A·cm^‒2高电流密度下硝酸盐还原制氨

Co(OH)₂/Cu NWs with interface modification of hypophosphite ions for sustainable ammonia synthesis from nitrate at ~2.8 A·cm^-2

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