Structural regulation strategies of nitrogen reduction electrocatalysts

doi:10.1016/S1872-2067(24)60123-3

Abstract

Abstract:

Ammonia is a carrier of high energy density and a good hydrogen storage substance. The Haber-Bosch process accounts for 90% of the world's ammonia production, which relies on natural gas and fossil resources as energy sources, not only polluting the ecological environment, but also accelerating the consumption of resources. To explore new ways to synthesize ammonia and reduce carbon emissions, electrocatalytic nitrogen reduction reaction (NRR) to produce ammonia has been emerged owing to the advantages of environmental protection, low energy consumption and mild reaction conditions. Here, we systematize the NRR mechanisms, including dissociation mechanism, association mechanism (involving distal pathway, alternative path, and enzymatic mechanism), and Mars-van Krevelen mechanism. Then, theoretical calculations, performance parameters, synthesis methods, and types of NRR electrocatalysts are detailedly introduced. Moreover, effective strategies to optimize the electronic structures of NRR electrocatalysts are emphatically discussed, including d-band center modulation (involving monoatomic dispersion, doping strategy, defect engineering, interface engineering, and strain effect), p-band center modulation, and other regulation strategies (involving construction of heterojunction, electron spin state modulation, phase interface engineering, and lithium ion mediation). Furthermore, we introduce NRR-related cell design and development. In addition, we evaluate relevant NRR experimental techniques, including N adsorption characterization techniques and methods for identification of active sites. Finally, the future challenges and opportunities concerning the improvement of NRR catalysts are outlined.

Key words: Nitrogen reduction reaction, Haber-Bosch process, Detection method, Electronic structure, Reaction mechanism

Siyu Chen, Jingqi Guan. Structural regulation strategies of nitrogen reduction electrocatalysts[J]. Chinese Journal of Catalysis, 2024, 66: 20-52.

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Figures/Tables 33

Fig. 1. The development history of NRR.

Table 1 Comparison of NRR performance on various electrocatalysts.

Electrocatalyst	Electrolyte	Potential (V vs. RHE)	NH₃ yield	Faraday efficiency (%)	Ref.
Pd-NTA-NF	0.1 mol L^-1 Na₂SO₄	-0.15	5.45 μg h^-1 cm^-2	20.10	[45]
La₂O₃@C	0.1 mol L^-1 Na₂SO₄	-0.3	20.59 μg h^-1 mg^-1	17.10	[46]
MoS₂	0.1 mol L^-1 Na₂SO₄	-0.5	8.08 × 10^-11 mol s^-1 cm^-2	1.17	[47]
FeRu-CNS	0.1 mol L^-1 Na₂SO₄	-0.2	43.9 μg h^-1 mg^-1	29.30	[48]
V-C₃N₄	0.1 mol L^-1 Na₂SO₄	-0.3	31.41 μg_NH3 h^-1 mg_cat^-1	76.53	[49]
V-NG	0.1 mol L^-1 Na₂SO₄	-0.2	19.88 μg_NH3 h^-1 mg_cat^-1	13.69	[49]
B-Mo₂C/NC-50	0.5 mol L^-1 K₂SO₄	-0.5	42.9 μg h^-1 mg^-1	36.90	[50]
FL-MoS₂-20	1 mol L^-1 K₂SO₄	-0.5	92.95 μg h^-1 mg^-1	20.80	[51]
AuHNCs	0.5 mol L^-1 LiClO₄	-0.5	3.98 μg h^-1 cm^-2	30.20	[52]
MoO_3-_x/MXene	0.5 mol L^-1 LiClO₄	-0.4	95.8 μg h^-1 mg^-1	21.20	[53]
Cl-RGO	0.05 mol L^-1 H₂SO₄	-0.3	0.9 μg h^-1 mg_cat^-1	5.97	[54]
Np-B₁₃C₁₂	0.05 mol L^-1 H₂SO₄	-0.05	91.28 μg h^-1 mg_cat^-1	35.53	[55]
2D-C₃N₄-NV	0.1 mol L^-1 HCl	-0.3	17.85μg h^-1 mg_cat^-1	10.96	[56]
D-FeN/C	0.1 mol L^-1 KOH	-0.4	24.8 μg h^-1 mg_cat^-1	15.80	[57]
Ru SAs/g-C₃N₄	0.5 mol L^-1 NaOH	0.05	23.0 μg mg_cat^-1 h^-1	8.30	[58]

Table 2 Basic processes of different ENRR mechanisms.

Reaction mechanism	Reaction mechanism	Electrocatalyst	Ref.
Dissociation mechanism	N₂ + 2^* → 2^N 2^N + 2e^- + 2H^* → 2^NH 2^NH + 2e^- + 2H⁺ → 2NH₃ + 2^*	Co/CeN	[61]
Association mechanism (distal pathway)	N₂ + ^* → ^N₂ ^N₂ + e^- +H+ → ^NNH ^NNH + e^- + H⁺ → ^NNH₂ ^NNH₂ + e^- + H^* → ^N + NH₃ ^N + e^- + H^* → ^NH ^NH + e^- + H⁺ → ^NH₂ ^NH² + e^- + H⁺ → NH₃ + ^*	PdFe₃	[62]
Association mechanism (alternative path)	N₂ + ^* → ^N₂ ^N₂ + e^- + H+ → ^NNH ^NNH + e^- + H⁺ → ^NHNH ^NHNH + e^- + H⁺ → ^NHNH₂ ^NHNH₂ + e^- + H+ → ^NH₂NH₂ ^NH₂NH₂ + e^- + H⁺ → ^NH₂ + NH₃ ^NH₂ + e^- + H⁺ → NH₃+ ^*	C-SiP-NSs	[63]
Association mechanism (enzymatic mechanism)	N₂+ ^* → ^NN ^NN^ + e^- + H^* → ^NH^N ^NH^N + e^- + H⁺ → ^NH^NH ^NH^NH + e^- + H⁺ → ^NH₂^NH ^NH₂^NH + e^- + H+ → ^NH₂^NH₂ ^NH₂^NH₂ + e^- + H⁺ → ^NH₂ + NH₃ ^NH₂ + e^- + H⁺ → NH₃ + ^*	Re@MoS₂	[64]
MvK mechanism	S-N + 3e^- + 3H⁺ → S-NH₃ S-NH₃ → S-N_V + NH₃ S-N_V + N₂ → NΞN-S NΞN-S + 3H⁺ + 3e^- → NH₃…N-S NH₃…N-S → N-S + NH₃	Fe₃Mo₃N	[65]

Fig. 2. Schematic diagram of ENRR on the surface of a electrocatalyst. (a) Dissociation mechanism; (b) association distal mechanism; (c) association alternating mechanism; (d) enzymatic mechanism.

Fig. 3. (a) Free energy graph of ENRR on PdFe3@G. Reproduced with permission [62]. Copyright 2023, Wiley-VCH GmbH. (b) Analysis of charge density difference of N2 on SiP. (c) N2 free energy diagram of alternate pathways at the C-SiP NSs zigzag Si site at 0 V. (d) Each step corresponds to the atomic configuration. Reproduced with permission [63]. Copyright 2022, Wiley-VCH GmbH.

Fig. 4. (a) Structure diagram of FeMo-co. (b) A comparison of the distal and alternating pathways, along with a diagram illustrating the differences in intermediates. Reproduced with permission [69]. Copyright 2011, American Chemical Society. (c) Volcanic maps of stepped and flat transition metal surfaces. Reproduced with permission [67]. Copyright 2024, ELSEVIER B.V. and Science Press.

Fig. 5. Diagram of Sabatier's principle.

Fig. 6. MvK mechanism diagram.

Fig. 7. Summary DFT diagram of a typical electrochemical NRR.

Table 3 Basic synthesis methods for ENRR materials.

Basic synthesis method	Strength	Weakness	Electrocatalyst	Ref.
Hydrothermal synthesis	simple operation, uniform size, high purity, and controllable morphology	long experiment period, and prone to agglomeration	Fe₂(MoO₄)₃/C	[79]
Sol-gel method	high product purity	the material is prone to deformation during heat treatment, and the composition and morphology of the product are affected by the solvent expulsion	BaCe_0.80Gd_0.10Sm_0.10O_3-_δ	[80]
Electrospinning technology	it can obtain finer-sized nanofibers with stronger material stability and more functionalities	the parameters of the experiment are very strict	FeNi-Co@CM	[81]
In-situ growth method	mild reaction condition, good catalytic effect, and low production cost	it requires precise control of the catalyst's growth conditions and a thorough understanding of its surface properties	nPd/NF	[82]

Fig. 8. (a) Schematic diagram of electronic feedback mechanism. Reproduced with permission [85]. Copyright 2023, American Chemical Society. (b) Partial state density of penta-TiP in a 2 × 2 cell. Reproduced with permission [88]. Copyright 2019, Royal Society of Chemistry. (c) The isosurface of the deformed charge density seen from the top view. (d) The deformed charge density of *NNH. Reproduced with permission [90]. Copyright 2018, WILEY-VCH.

Fig. 9. (a) Free energy scale of NH3 released by reducing metal nitrides. Reproduced with permission [93]. Copyright 2015, Royal Society of Chemistry. (b) Magnetic susceptibility of FePPc. (c) Magnetic susceptibility of FeMoPPc. (d) Diagram of N2 binding to transition metal. Reproduced with permission [94]. Copyright 2021, Wiley-VCH GmbH. (e) Calculated projected state density. (f) The charge differential density of N2 adsorbed on B doped C2N. Reproduced with permission [95]. Copyright 2019, Royal Society of Chemistry. (g) State density of absorbed *N2 on 2D C3N4 and 2D C3N4-NV. (h) Differential charge density on 2D C3N4 and 2D C3N4-NV. Reproduced with permission [56]. Copyright 2021, ELSEVIER. (i) PDOS adsorbing B atoms before and after N2 molecules. (j) Electron density difference of N2 molecule at B2 site. Reproduced with permission [55]. Copyright 2021, Wiley-VCH GmbH.

Fig. 10. (a) DOS display of Co, P, N in BPBL-Co-NNH. (b) DOS of P and N in BPBL-NNH. (c) Change in bond length of N2 molecule during reduction. Reproduced with permission [102]. Copyright 2021, ELSEVIER B.V. and Science Press. (d) XRD comparison of phenyldiene and al-phenyldiene exposed for 7 days at 90% relative humidity. (e) Raman spectrogram of phenylene and al-phenylene exposed for 7 days at 90% relative humidity. Reproduced with permission [103]. Copyright 2024, Wiley-VCH GmbH. (f) Schematic diagram of coupling of BP quantum dots with MnO2 nanosheets. Reproduced with permission [104]. Copyright 2020, WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fig. 11. HER inhibits the progress of ENRR, reducing the selectivity towards N2 molecules, which leads to a decrease in FE and product yield.

Fig. 12. (a) Reducing the concentration of protons in bulk solution to limit the rate of proton transfer. (b) Increasing the barrier of proton transfer to the surface to limit the proton transfer rate. (c) Limiting electron transport rates by requiring electrons to pass through thin insulators. (d) The use of light absorbers to provide a slow flow of electrons to limit the electron transport rate. Reproduced with permission [77]. Copyright 2016, American Chemical Society.

Fig. 13. (a) PDOS of Ru atoms on Ru SAs/g-C3N4 and Ru (0001). (b) Reaction free energy path of NRR on Ru (0001). Reproduced with permission [58]. Copyright 2019, WILEY-VCH. (c) Synthetic diagram of FeRu-CNS. (d) Fe-d orbital PDOS in FeN4 and FeRu-CNS. Reproduced with permission [48]. Copyright 2023, Royal Society of Chemistry. (e) Volcanic relationship between △Gmax and △d-p. Reproduced with permission [117]. Copyright 2023, John Wiley & Sons Australia, Ltd.

Fig. 14. (a,b) PDOS of Fe2(DOBDC) and Fe2Cl2(BBTA) before and after doping Mo. (c) PDOS of Mo, coordination atoms and *NN after N2 adsorption on Mo (II)-Fe2F2(BBTA), Mo (II)-Fe2Cl2(BBTA) and Mo(II)-Fe2Br2(BBTA). (d) Enhanced N2 activation diagram. (e) Charge transfer diagram of Fe-X-Mo. Reproduced with permission [120]. Copyright 2022, American Chemical Society. (f,g) N2 adsorbs to the Bader charge structure of B-Mo2C and β-Mo2C. Reproduced with permission [50]. Copyright 2022, Wiley-VCH GmbH.

Fig. 15. (a) State density and d-band center diagram of MoS2 at different VS concentrations. (b) △G and *N-*N bond lengths as d-band center functions. Reproduced with permission [51]. Copyright 2023, Elsevier B.V. (c) Difference in charge density of N2 adsorbed on MoO3/MXene and MoO3-x/MXene. (d) εd of Mo-3d in MoO3/MXene and MoO3-x/MXene. (e) Charge density differences. (f) NH3 yield of MoO3/MXene, MoO3-x/MXene, MoO3 and MoO3-x. Reproduced with permission [53]. Copyright 2021, Wiley-VCH GmbH.

Fig. 16. (a) AES spectral N signals of Ni/CeN and CeN before and after the NRR. Reproduced with permission [126]. Copyright 2020, American Chemical Society. (b,c) PDOS of Fe atoms in D states and N atoms in p states of FeN4-C and D-FeN4-C. (d) Schematic diagram of electron density differences between nitrogen-containing intermediates at FeN4-C and D-FeN4-C. Reproduced with permission [57]. Copyright 2022, Wiley-VCH GmbH.

Fig. 17. (a,b) The d orbital PDOS of Rh in Rh@SnO2 and Rh (111). Reproduced with permission [131]. Copyright 2022, American Chemical Society. (c) Change of work function on NPG@SnS2 and SnS2 (101) surfaces. (d) The energy of *H on S and on Sn. (e) Total accumulation of charge in the SnS2 layer and total consumption in the NPG layer. (f) Charge dissipation and accumulation on a single atom. (g) Overall shift of charge density from NPG layer to SnS2 layer. Reproduced with permission [132]. Copyright 2021, American Chemical Society.

Fig. 18. Effect of d-band position on tensile strain of transition metals.

Fig. 19. (a) The d orbital changes of Ti before and after N2 adsorption at 2.5% tensile strain. (b) The relationship between N-N distance and charge transfer (CT). (c) Relationship between △E*(N2) and the adsorption energies of *NNH, *NNH2, *N, *NH and *NH3. Reproduced with permission [138]. Copyright 2023, Wiley-VCH GmbH.

Fig. 20. (a) OV-BP-BiVO4 hyacanthosphere heterogenous combination diagram. (b,c) XRD comparison of OV-BP-BiVO4, BP-BIVO4 and BP. (d) XPS comparison diagram of V 2p in OV-BP-BiVO4, BP-BIVO4 and BP. Reproduced with permission [143]. Copyright 2022, Elsevier Inc. All rights reserved.

Fig. 22. (a) Application of Ru/Mo2C-NCNTs in Li-N2 cells. (b) Complete discharge/charging curve of Ru/Mo2C-NCNTs. (c) Cyclic diagram of Ru/Mo2C-NCNTs. (d) Characterization of Ru/Mo2C-NCNTs compared with other electrocatalysts. Reproduced with permission [146]. Copyright 2022, Elsevier B.V.

Fig. 23. (a) Octahedral d orbital splitting process. Reproduced with permission [150]. Copyright 2024, Wiley-VCH GmbH. (b-d) PDOS of N2 molecules with different adsorption structures in Fe@Mo2CS2. (e,f) The difference in charge density between vertical and horizontal adsorption structures of N2 molecules in Fe@Mo2CS2. (g) Gibbs free energy of N2 molecule in horizontal adsorption configuration. Reproduced with permission [149]. Copyright 2022, The Royal Society of Chemistry.

Fig. 24. (a) Schematic diagram of FeSA-NSC-900 synthesis. (b,c) FeN4 and FeN3S1 PDOS diagram. (d) Molecular orbital diagram of N2 in FeN4 and FeN3S1 and spin configuration of Fe. Reproduced with permission [151]. Copyright 2022, Wiley-VCH GmbH.

Fig. 25. (a) Schematic diagram of solid-solution two-phase interface. (b) Diagram of gas-solid-liquid three-phase interface. (c) Schematic diagram of some NRR devices. (d) Ammonia yield and FE of Pd/ACC catalysts at different potentials. Reproduced with permission [154]. Copyright 2019, Haiyan Science and Technology Review Publishing. (e,f) Hydrophilic and hydrophobic interface diagram. Reproduced with permission [155]. Copyright 2020, Wiley-VCH GmbH.

Fig. 26. Schematic diagram of anode and cathode reactions mediated by lithium.

Fig. 27. (a,b) Schematic diagram of working electrode crystal deposition without EtOH and LiBF4. Reproduced with permission [160]. Copyright 2024, The Royal Society of Chemistry. (c) Recovery test using Ni as cathode. Reproduced with permission [161]. Copyright 2024, Elsevier B.V. (d) The ESP of THF molecule was determined by DFT. (e) Probability distribution diagram of linear ether on lithium plate. Reproduced with permission [162]. Copyright 2023, American Chemical Society.

Fig. 28. (a-d) Diagram of unseparated cell (NS), liquid-liquid cell (L-L), gas-liquid (G-L) cell, and gas-gas (G-G) cell. (e) Diagram of a three-chamber cell (G-L-L).

Fig. 29. (a) FE at -0.8 V vs. NHE. (b-d) Diagram of binding energy and bond distance of N2 molecule under different anions. (e) Ammonia yields at -0.8 V vs. NHE. Reproduced with permission [173]. Copyright 2017, The Royal Society of Chemistry. (f) Schematic diagram of electrocatalytic synthesis of ammonia and acetone in ionic liquids. (g) Ammonia yield and FE. (h) Acetone yield and FE. Reproduced with permission [174]. Copyright 2021, The Royal Society of Chemistry.

Fig. 30. (a) Effects of different interface structures on NRR. Reproduced with permission [165]. Copyright 2022, The Royal Society of Chemistry. (b) Fe1.0HTNs used to simulate the human "alveolar" diagram. Reproduced with permission [177]. Copyright 2021, The Royal Society of Chemistry. (c) Diagram of the superoxygenophilic electrode and the corresponding three-phase reaction region. Reproduced with permission [180]. Copyright 2022, Elsevier B.V.

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