Research progress of inhibiting hydrogen evolution in electro-catalytic ammonia synthesis

doi:10.16085/j.issn.1000-6613.2020-2520

Abstract

Abstract:

The Haber-Bosch process is of high energy consumption and high CO₂ emissions. Electro-catalytic nitrogen reduction reaction (NRR) is a novel process which works at room temperature and atmospheric pressure with N₂ input. It has the advantages of low cost, mild reaction conditions and environmental friendliness. However, due to its high overpotential, low current density and low selectivity, electrocatalytic NRR currently is still in the laboratory research stage. Particularly, the Faraday efficiency is severely limited by the hydrogen evolution reaction (HER). In this paper, we introduced the reaction mechanism of ammonia synthesis by electrocatalytic NRR. Moreover, we reviewed the competition mechanism between HER and NRR, mainly from the adsorption and activation of nitrogen and the specific reaction of electroreduction stages. This article focused on the latest research achievements in controlling HER by rational catalysts and reaction system design. Finally, we summarized the challenges in the development of electrocatalytic NRR for ammonia synthesis and gave the corresponding solutions. The potential application of electrocatalytic NRR ammonia synthesis under mild conditions is proposed.

Key words: electrochemistry, catalyst, activation, selectivity, ammonia, nitrogen reduction reaction, hydrogen evolution reaction

摘要：

传统工业合成氨Haber-Bosch工艺条件要求严苛，并且存在高能耗以及高CO₂排放问题。电催化氮气还原（nitrogen reduction reaction, NRR）是一种在常温常压下利用氮气合成氨的新工艺，具有成本低、反应条件温和、环境友好等优势。但该反应所需过电位较高，水解析氢反应（hydrogen evolution reaction, HER）竞争明显，导致电流密度和选择性较低，无法达到工业应用水平。本文在介绍电催化NRR合成氨的反应机理的基础上，主要从氮气分子的吸附活化和电还原阶段反应过程出发，综述了电催化氮气还原合成氨反应中HER与NRR的竞争机制。重点梳理了通过设计催化剂和反应体系抑制HER的国内外最新研究成果，最后对电催化NRR合成氨面临的挑战和机遇进行了展望。

关键词: 电化学, 催化剂, 活化, 选择性, 氨, 氮气还原, 析氢反应

CLC Number:

TQ113.2

ZHANG Ting, SUN Xiaohong, YU Hongbing, DONG Heng. Research progress of inhibiting hydrogen evolution in electro-catalytic ammonia synthesis[J]. Chemical Industry and Engineering Progress, 2021, 40(12): 6670-6687.

张婷, 孙晓红, 于宏兵, 董恒. 电催化氮气还原合成氨反应中抑制水解析氢竞争的研究进展[J]. 化工进展, 2021, 40(12): 6670-6687.

Figures/Tables 14

项目	反应方程式	E⁰（vs. SHE）/V
R1	N₂+e^- $? → ?$ N₂*	-3.37（pH=0）
R2	N₂+H⁺+e^- $? → ?$ N₂H*	-3.20（pH=0）
R3	N₂+2H⁺+2e^- $? → ?$ N₂H₂*	-1.10（pH=0）
R4	N₂+4H⁺+4e^- $? → ?$ N₂H₄*	-0.36（pH=0）
R5	N₂+6H⁺+6e^- $? → ?$ 2NH₃	0.148（pH=0）
R6	2H⁺+2e^- $? → ?$ H₂	0（pH=0）
R7	N₂+6H₂O+6e^- $? → ?$ 2NH₃+6OH^-	-0.763（pH=14）
R8	2H₂O+2e^- $? → ?$ H₂+2OH^-	-0.828（pH=14）

项目	反应方程式	E⁰（vs. SHE）/V
R1	N₂+e^- $? → ?$ N₂*	-3.37（pH=0）
R2	N₂+H⁺+e^- $? → ?$ N₂H*	-3.20（pH=0）
R3	N₂+2H⁺+2e^- $? → ?$ N₂H₂*	-1.10（pH=0）
R4	N₂+4H⁺+4e^- $? → ?$ N₂H₄*	-0.36（pH=0）
R5	N₂+6H⁺+6e^- $? → ?$ 2NH₃	0.148（pH=0）
R6	2H⁺+2e^- $? → ?$ H₂	0（pH=0）
R7	N₂+6H₂O+6e^- $? → ?$ 2NH₃+6OH^-	-0.763（pH=14）
R8	2H₂O+2e^- $? → ?$ H₂+2OH^-	-0.828（pH=14）

催化剂	电解液	过电位/V	FE/%	氨产率	参考文献
贵金属
Au纳米笼	0.5mol/L LiClO₄	-0.4	30.2	3.9μg?h^-1?cm^-2	［45］
Au纳米棒	0.1mol/L KOH	-0.2	4	1.648μg?h^-1?cm^-2	［5］
Ru纳米粒子	0.01mol/L HCl	0.01	5.4	约0.2μg?h^-1?cm^-2	［7］
Rh纳米片	0.1mol/L KOH	-0.2	21.7	23.88μg?h^-1?cm^-2	［10］
Pd/C	0.1mol/L PBS	-0.1	8.2	4.5μg?h^-1?mg^-1	［11］
Au/TiO₂	0.1mol/L HCl	-0.2	8.11	21.4μg?h^-1?mg^-1	［69］
Pt/C	H⁺/Li⁺/NH₄⁺	-1.2	0.83	47.2μg?h^-1?cm^-2	［70］
过渡金属及其杂化物
Bi纳米片	0.1mol/L Na₂SO₄	-0.8	10.46	（2.54±0.16）μg?cm^-2?h^-1	［40］
Bi₄V₂O₁₁/CeO₂	0.1mol/L HCl	-0.2	10.16	23.21μg??h^-1?mg^-1	［52］
Fe₃S₄纳米片	0.1mol/L HCl	-0.4	6.45	75.4μg?h^-1?mg^-1	［71］
Fe/Fe₃O₄	0.1mol/L PBS	-0.3	8.29	0.19μg?h^-1?cm^-2	［72］
30% Fe₂O₃-CNT	0.5mol/L KOH	-0.2	0.16	0.65μg?h^-1?cm^-2	［51］
β-FeOOH	0.5mol/L LiClO₄	-0.7	6.7	23.32μg?h^-1?mg^-1	［39］
MoO₃纳米片	0.1mol/L HCl	-0.3	1.9	29.43μg?h^-1?mg^-1	［15］
Mo₂C纳米棒	0.1mol/L HCl	-0.3	8.13	95.1μg?h^-1?mg^-1	［73］
MoS₂	0.1mol/L Na₂SO₄	-0.5	1.17	8.08×10^-11mol?s^-1?cm^-2	［74］
Mo₂N	0.1mol/L HCl	-0.3	4.5	78.4μg?h^-1?mg^-1	［75］
MoN	0.1mol/L HCl	-0.3	1.15	3.01×10^-10mol?s^-1?cm^-2	［76］
MoS₂纳米花	0.1mol/L Na₂SO₄	-0.4	8.34	29.28μg?h^-1?mg^-1	［49］
Mo₂C	0.5mol/L Li₂SO₄	-0.3	1.1	11.3μg?h^-1?mg^-1	［77］
MoSe₂纳米球	0.1mol/L Na₂SO₄	-0.6	14.2	11.2μg?h^-1?mg^-1	［46］
SnO₂	0.1mol/L Na₂SO₄	-0.7	2.17	0.53μmmol?cm^-2?h^-1	［36］
Nb₂O₅	0.1mol/L HCl	-0.55	9.26	43.6μg?h^-1?mg^-1	［38］
NbO₂纳米颗粒	0.05mol/L H₂SO₄	-0.65	32	11.6μg?h^-1?mg^-1	［78］
TiO₂	0.1mol/L HCl	0.15	9.17	1.24×10^-10mol?s^-1?cm^-2	［79］
Fe-TiO₂	0.5mol/L LiClO₄	-0.4	25.6	25.47μg?h^-1?mg^-1	［80］
TiO₂/Ti	0.1mol/L Na₂SO₄	-0.7	2.5	5.60μg?h^-1?mg^-1	［48］
Cr-CeO₂	0.1mol/L Na₂SO₄	-0.4	3.7	16.4μg?h^-1?mg^-1	［14］
Cu-CeO₂	0.1mol/L Na₂SO₄	-0.45	19.1	5.3×10^-10mol?s^-1?cm^-2	［13］
MnO	0.1mol/L Na₂SO₄	-0.39	8.02	1.11×10^-10mol?s^-1?cm^-2	［81］
WO₃纳米片	0.1mol/L HCl	-0.3	7	17.28μg?h^-1?mg^-1	［16］
Cr₂O₃	0.1mol/L Na₂SO₄	-0.9	6.78	25.3μg?h^-1?mg^-1	［44］
W₂N₃纳米片	0.1mol/L KOH	-0.2	11.67	（11.66±0.98）μg?h^-1?mg^-1	［56］
NiN₃	0.5mol/L LiClO₄	-0.8	—	115μg?cm^-2?h^-1	［82］
LaF₃	0.5mol/L LiClO₄	-0.45	16	55.9μg?h^-1?mg^-1	［83］
VN/Ti	0.1mol/L HCl	-0.5	2.25	5.14μg?h^-1?cm^-2	［44］
VN	0.05mol/L H₂SO₄	-0.1	6	20.2μg?h^-1?cm^-2	［28］
单金属原子催化剂（SACs）
ISAS-Fe/NC	0.5mol/L LiSO₄	-0.4	18.6	（62.9±2.7）μg?h^-1?mg^-1	［17］
Cu SAC^［N］	0.1mol/L KOH	-0.35	13.8	53.3μg?h^-1?mg^-1	［18］
Au/C₃N₄	5mmol/L H₂SO₄	-0.1	11.1	1.3mg?h^-1?mg^-1	［19］
Au-TiO₂	0.1mol/L HCl	-0.2	8.11	21.4μg?mg^-1?h^-1	［70］
Ru/NC	0.1mol/L HCl	-0.21	8	3.665mg?h^-1?mg^-1	［84］
Ru-ZrO₂/NC	0.1mol/L HCl	-0.1	21	约1mg?h^-1?mg^-1	［85］
碳基催化剂
B₄C	0.1mol/L HCl	-0.2	10.1	26.57μg?h^-1?mg^-1	［86］
B掺杂石墨烯	0.05mol/L H₂SO₄	-0.75	4.83	9.8mg?h^-1?cm^-2	［60］
N掺杂多孔碳	0.1mol/L KOH	-0.85	3.52	57.8μg?h^-1?cm^-2	［87］
N掺杂的碳纳米片	0.1mol/L HCl	-0.5	7.1	（97.18±7.13）mg?h^-1?cm^-2	［88］
S掺杂三维石墨烯	0.1mol/L HCl	-0.85	7.07	38.81μg?h^-1?mg^-1	［89］
S掺杂碳纳米球	0.1mol/L Na₂SO₄	-0.5	6.9	19.07μg?h^-1?mg^-1	［90］
S掺杂石墨烯	0.1mol/L HCl	-0.5	5.89	27.3μg?h^-1?mg^-1	［63］
Cl掺杂石墨	0.1mol/L HCl	-0.45	8.7	10.7μg?h^-1cm^-2	［68］
F掺杂石墨烯	0.1mol/L KOH	-0.7	4.2	9.3μg?h^-1?mg^-1	［91］
F掺杂多孔碳	0.1mol/L HCl	-0.2	54.8	197.7μg?mg^-1?h^-1	［92］
O掺杂石墨烯	0.1mol/L HCl	-0.45	12.6	21.3μg?h^-1?mg^-1	［65］
黑磷纳米片	0.01mol/L HCl	-0.6	5.07	31.37μg?h^-1?mg^-1	［93］
P掺杂石墨烯	0.1mol/L KOH	-0.65	20.82	32.33μg?h^-1?mg^-1	［64］
N，S-石墨烯	0.5mol/L LiClO₄	-0.6	5.8	7.7μg?h^-1?mg^-1	［94］
金属+碳基
Au/CeO_x-RGO	0.1mol/L KOH	-0.2	10.1	24.7μg?h^-1?mg^-1	［95］
FeP₂-rGO	0.1mol/L HCl	-0.4	21.99	22.13μg?h^-1?mg^-1	［96］
TA-rGO	0.1mol/L Na₂SO₄	-0.75	4.83	17.02μg?h^-1?mg^-1	［97］
MoS₂/石墨烯	0.1mol/L LiClO₄	-0.45	4.58	24.82μg?h^-1?mg^-1	［98］
TiO₂-rGO	0.1mol/L HCl	-0.9	3.3	15.13μg?h^-1?mg^-1	［45］
Mn₃O₄-rGO	0.1mol/L Na₂SO₄	-0.85	3.52	17.4μg?h^-1?mg^-1	［99］
Cr₂O₃-rGO	0.1mol/L Na₂SO₄	-0.6	7.33	33.3μg?h^-1?mg^-1	［100］
SnO₂/RGO	0.1mol/L HCl	-0.5	7.1	25.6μg?h^-1?mg^-1	［35］

催化剂	电解液	过电位/V	FE/%	氨产率	参考文献
贵金属
Au纳米笼	0.5mol/L LiClO₄	-0.4	30.2	3.9μg?h^-1?cm^-2	［45］
Au纳米棒	0.1mol/L KOH	-0.2	4	1.648μg?h^-1?cm^-2	［5］
Ru纳米粒子	0.01mol/L HCl	0.01	5.4	约0.2μg?h^-1?cm^-2	［7］
Rh纳米片	0.1mol/L KOH	-0.2	21.7	23.88μg?h^-1?cm^-2	［10］
Pd/C	0.1mol/L PBS	-0.1	8.2	4.5μg?h^-1?mg^-1	［11］
Au/TiO₂	0.1mol/L HCl	-0.2	8.11	21.4μg?h^-1?mg^-1	［69］
Pt/C	H⁺/Li⁺/NH₄⁺	-1.2	0.83	47.2μg?h^-1?cm^-2	［70］
过渡金属及其杂化物
Bi纳米片	0.1mol/L Na₂SO₄	-0.8	10.46	（2.54±0.16）μg?cm^-2?h^-1	［40］
Bi₄V₂O₁₁/CeO₂	0.1mol/L HCl	-0.2	10.16	23.21μg??h^-1?mg^-1	［52］
Fe₃S₄纳米片	0.1mol/L HCl	-0.4	6.45	75.4μg?h^-1?mg^-1	［71］
Fe/Fe₃O₄	0.1mol/L PBS	-0.3	8.29	0.19μg?h^-1?cm^-2	［72］
30% Fe₂O₃-CNT	0.5mol/L KOH	-0.2	0.16	0.65μg?h^-1?cm^-2	［51］
β-FeOOH	0.5mol/L LiClO₄	-0.7	6.7	23.32μg?h^-1?mg^-1	［39］
MoO₃纳米片	0.1mol/L HCl	-0.3	1.9	29.43μg?h^-1?mg^-1	［15］
Mo₂C纳米棒	0.1mol/L HCl	-0.3	8.13	95.1μg?h^-1?mg^-1	［73］
MoS₂	0.1mol/L Na₂SO₄	-0.5	1.17	8.08×10^-11mol?s^-1?cm^-2	［74］
Mo₂N	0.1mol/L HCl	-0.3	4.5	78.4μg?h^-1?mg^-1	［75］
MoN	0.1mol/L HCl	-0.3	1.15	3.01×10^-10mol?s^-1?cm^-2	［76］
MoS₂纳米花	0.1mol/L Na₂SO₄	-0.4	8.34	29.28μg?h^-1?mg^-1	［49］
Mo₂C	0.5mol/L Li₂SO₄	-0.3	1.1	11.3μg?h^-1?mg^-1	［77］
MoSe₂纳米球	0.1mol/L Na₂SO₄	-0.6	14.2	11.2μg?h^-1?mg^-1	［46］
SnO₂	0.1mol/L Na₂SO₄	-0.7	2.17	0.53μmmol?cm^-2?h^-1	［36］
Nb₂O₅	0.1mol/L HCl	-0.55	9.26	43.6μg?h^-1?mg^-1	［38］
NbO₂纳米颗粒	0.05mol/L H₂SO₄	-0.65	32	11.6μg?h^-1?mg^-1	［78］
TiO₂	0.1mol/L HCl	0.15	9.17	1.24×10^-10mol?s^-1?cm^-2	［79］
Fe-TiO₂	0.5mol/L LiClO₄	-0.4	25.6	25.47μg?h^-1?mg^-1	［80］
TiO₂/Ti	0.1mol/L Na₂SO₄	-0.7	2.5	5.60μg?h^-1?mg^-1	［48］
Cr-CeO₂	0.1mol/L Na₂SO₄	-0.4	3.7	16.4μg?h^-1?mg^-1	［14］
Cu-CeO₂	0.1mol/L Na₂SO₄	-0.45	19.1	5.3×10^-10mol?s^-1?cm^-2	［13］
MnO	0.1mol/L Na₂SO₄	-0.39	8.02	1.11×10^-10mol?s^-1?cm^-2	［81］
WO₃纳米片	0.1mol/L HCl	-0.3	7	17.28μg?h^-1?mg^-1	［16］
Cr₂O₃	0.1mol/L Na₂SO₄	-0.9	6.78	25.3μg?h^-1?mg^-1	［44］
W₂N₃纳米片	0.1mol/L KOH	-0.2	11.67	（11.66±0.98）μg?h^-1?mg^-1	［56］
NiN₃	0.5mol/L LiClO₄	-0.8	—	115μg?cm^-2?h^-1	［82］
LaF₃	0.5mol/L LiClO₄	-0.45	16	55.9μg?h^-1?mg^-1	［83］
VN/Ti	0.1mol/L HCl	-0.5	2.25	5.14μg?h^-1?cm^-2	［44］
VN	0.05mol/L H₂SO₄	-0.1	6	20.2μg?h^-1?cm^-2	［28］
单金属原子催化剂（SACs）
ISAS-Fe/NC	0.5mol/L LiSO₄	-0.4	18.6	（62.9±2.7）μg?h^-1?mg^-1	［17］
Cu SAC^［N］	0.1mol/L KOH	-0.35	13.8	53.3μg?h^-1?mg^-1	［18］
Au/C₃N₄	5mmol/L H₂SO₄	-0.1	11.1	1.3mg?h^-1?mg^-1	［19］
Au-TiO₂	0.1mol/L HCl	-0.2	8.11	21.4μg?mg^-1?h^-1	［70］
Ru/NC	0.1mol/L HCl	-0.21	8	3.665mg?h^-1?mg^-1	［84］
Ru-ZrO₂/NC	0.1mol/L HCl	-0.1	21	约1mg?h^-1?mg^-1	［85］
碳基催化剂
B₄C	0.1mol/L HCl	-0.2	10.1	26.57μg?h^-1?mg^-1	［86］
B掺杂石墨烯	0.05mol/L H₂SO₄	-0.75	4.83	9.8mg?h^-1?cm^-2	［60］
N掺杂多孔碳	0.1mol/L KOH	-0.85	3.52	57.8μg?h^-1?cm^-2	［87］
N掺杂的碳纳米片	0.1mol/L HCl	-0.5	7.1	（97.18±7.13）mg?h^-1?cm^-2	［88］
S掺杂三维石墨烯	0.1mol/L HCl	-0.85	7.07	38.81μg?h^-1?mg^-1	［89］
S掺杂碳纳米球	0.1mol/L Na₂SO₄	-0.5	6.9	19.07μg?h^-1?mg^-1	［90］
S掺杂石墨烯	0.1mol/L HCl	-0.5	5.89	27.3μg?h^-1?mg^-1	［63］
Cl掺杂石墨	0.1mol/L HCl	-0.45	8.7	10.7μg?h^-1cm^-2	［68］
F掺杂石墨烯	0.1mol/L KOH	-0.7	4.2	9.3μg?h^-1?mg^-1	［91］
F掺杂多孔碳	0.1mol/L HCl	-0.2	54.8	197.7μg?mg^-1?h^-1	［92］
O掺杂石墨烯	0.1mol/L HCl	-0.45	12.6	21.3μg?h^-1?mg^-1	［65］
黑磷纳米片	0.01mol/L HCl	-0.6	5.07	31.37μg?h^-1?mg^-1	［93］
P掺杂石墨烯	0.1mol/L KOH	-0.65	20.82	32.33μg?h^-1?mg^-1	［64］
N，S-石墨烯	0.5mol/L LiClO₄	-0.6	5.8	7.7μg?h^-1?mg^-1	［94］
金属+碳基
Au/CeO_x-RGO	0.1mol/L KOH	-0.2	10.1	24.7μg?h^-1?mg^-1	［95］
FeP₂-rGO	0.1mol/L HCl	-0.4	21.99	22.13μg?h^-1?mg^-1	［96］
TA-rGO	0.1mol/L Na₂SO₄	-0.75	4.83	17.02μg?h^-1?mg^-1	［97］
MoS₂/石墨烯	0.1mol/L LiClO₄	-0.45	4.58	24.82μg?h^-1?mg^-1	［98］
TiO₂-rGO	0.1mol/L HCl	-0.9	3.3	15.13μg?h^-1?mg^-1	［45］
Mn₃O₄-rGO	0.1mol/L Na₂SO₄	-0.85	3.52	17.4μg?h^-1?mg^-1	［99］
Cr₂O₃-rGO	0.1mol/L Na₂SO₄	-0.6	7.33	33.3μg?h^-1?mg^-1	［100］
SnO₂/RGO	0.1mol/L HCl	-0.5	7.1	25.6μg?h^-1?mg^-1	［35］

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