Electrodegradation of nitrogenous pollutants in sewage: from reaction fundamentals to energy valorization applications

Ming-Lei Sun , Hao-Yu Wang , Yi Feng , Jin-Tao Ren , Lei Wang and Zhong-Yong Yuan *
School of Materials Science and Engineering, Smart Sensing Interdisciplinary Science Center, Nankai University, Tianjin 300350, China. E-mail: zyyuan@nankai.edu.cn

First published on 5th November 2024

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Ming-Lei Sun

Ming-Lei Sun received his BE degree in 2019 from Nankai University. He is currently a PhD candidate in Nankai University under the supervision of Prof. Zhong-Yong Yuan. His research interest focuses on the fabrication of advanced nanomaterials for energy-related applications.

Zhong-Yong Yuan

Zhong-Yong Yuan received his PhD in Physical Chemistry from Nankai University in 1999. He worked as a postdoctoral fellow at the Institute of Physics, Chinese Academy of Sciences from 1999 to 2001. He then moved to Belgium, working as a research fellow at the University of Namur from 2001 to 2005, prior to joining Nankai University as a full professor. In 2016, he was elected as a fellow of the Royal Society of Chemistry (FRSC). His research interests are mainly focused on the self-assembly of hierarchically nanoporous and nanostructured materials for energy and environmental applications.

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1. Introduction

The interconversion among dinitrogen and other N-containing compounds underpins one of the most crucial global biogeochemical cycles on the earth – the natural nitrogen cycle.^1–4 The sound operation of this cycle plays a pivotal role in sustaining life across the entire spectrum of organisms, ranging from the tiniest bacteria to the most complex beings. However, excessive emission of active nitrogen-containing species into natural water bodies through anthropogenic activities severely disrupts the nitrogen cycle and further results in urgent environmental and health-related issues.^5–10 The majority of waste nitrogen-containing species are discharged into the water cycle through runoff from agricultural lands, urban surfaces, and treated sewage, exceeding the natural degradation capacity of the water system toward these contaminants.^11–13 Waste nitrogen-containing species in the form of nitrates, nitrites, ammonia nitrogen, hydrazine, and urea seriously ruin the water ecological balance and cause great damage to human life.

Given the urgency to address nitrogenous pollutants in sewage, several approaches, including biological treatment methods, physical adsorption methods, redox methods, and precipitation methods, have been proposed.^12,14,15 Chemical-physical methods consist of filtration techniques involving the use of cross flow filtration membranes and other separators, such as ultrafiltration methods, nanofiltration methods, reverse osmosis (RO), electrodialysis, and ion exchange methods.^16–18 However, these techniques face challenges due to high energy consumption, low removal efficiency, and selective removal capability. Biological methods, using living organisms to remove or degrade contaminants in sewage, are one of the most important techniques and can be effective in treating various types of wastewaters, such as activated sludge processes, microorganism trickling filters, biological aerated filters, bioaugmentation, and anaerobic digestion.^19,20 Nevertheless, the development of these biological methods is limited by the high space requirement, long treatment time, sludge production, and high operating costs. Through a profound comprehension of electrochemical reactions and the advancement of relevant devices, electrochemical degradation of nitrogenous pollutants emerges as a promising method with distinct advantages: high efficiency, wide generality, easy operability, retrievability, environmental friendliness with no second pollution, and low cost.^21–23 Specifically, electrochemical degradation technologies are capable of achieving enhanced treatment efficiencies across a wide range of pollutants.²⁴ Electrochemical degradation technologies also offer a lower footprint and reduced space requirements compared to conventional methods, allowing for more efficient management of high contaminant concentrations.²⁵ Besides, the technologies can selectively remove pollutants without producing excess biomass or solids, thereby reducing the costs and environmental impact associated with sludge management.²⁶ Furthermore, additional energy recovery or chemical feedstocks can be produced during the electrochemical processes, thereby reducing overall energy consumption.²⁷

Efforts have been focused on enhancing the electrochemical degradation of nitrogenous pollutants by fostering a comprehensive understanding of the underlying electrochemical processes, including nitrate and nitrite reduction reactions (NtrRRs), ammonia oxidation reactions (AORs), hydrazine oxidation reactions (HzORs) and urea oxidation reactions (UORs), and synthesizing corresponding catalysts with high efficiency.^28–30 Capitalizing on the traits of contaminated substrates and their corresponding electro-reactions, a synergistic integration of tailored reactions with specialized energy devices including water electrolysis systems, metal–air batteries, and fuel cells holds great promise in generating added values, encompassing hydrogen production, electrical output, and valuable chemical production (Fig. 1). For instance, through the integration of the NtrRR cathode with the Zn anode, the Zn-nitrate batteries demonstrate the capability to facilitate the generation of valuable chemicals, NH₃, on the cathode and simultaneous output of electricity during the nitrate denitration process. Parallelly, investigating the utilization of N-pollutants (ammonia, urea, and hydrazine) with high energy density in sewage, along with their corresponding electro-oxidation reactions, offers a promising approach for advancing the direct fuel cells, enabling the efficient generation of power and the facilitation of the simultaneous removal of these contaminants. Hybrid water splitting systems, constructed by replacing the conventional oxygen evolution reaction with electro-oxidation of N-containing pollutants, could realize the energy-saving and efficient hydrogen production during the degradation processes.

Many reviews summarizing previous studies on these electrochemical processes, with a primary focus on providing insights into one or two aspects such as the reaction mechanisms, related catalysts, or simple energy devices, have been published.^31–33 For instance, Yang et al. summarized the acquired knowledge of rational catalyst design and the underlying reaction mechanisms for four nitrogen reactions, namely, the nitrogen reduction reaction, nitrogen oxidation reaction, nitrate reduction reaction, and ammonia oxidation reaction.³¹ Guo et al. provided a thorough review on the key nitrogen species (dinitrogen, ammonia, and hydrazine) and their transformation processes, encompassing the nitrogen reduction reaction, ammonia oxidation reaction, and hydrazine oxidation reaction.³⁴ The research progresses in revealing the reaction mechanism and developing relevant electrocatalysts were systematically highlighted. However, these reviews mainly focus on the mechanisms and catalyst design of concerned nitrogen electrochemical reactions, lacking detailed discussion on the derived devices and applications. As a review on nitrogenous species electrocatalytic energy devices, Wang et al. presented a discussion on the small molecule-assisted water electrolyzer for hydrogen output and simultaneous degradation of pollutants such as urea and hydrazine.³⁵ Lyu et al. lucidly discussed the basic principle of direct ammonia fuel cells and systematically summarized the advanced strategies for high-performance electrocatalysts.³⁶ Zhang et al. briefly summarized the multifaceted applications of the ammonia oxidation reaction, including its use in direct ammonia fuel cells (DAFCs), its coupling with the hydrogen evolution reaction (HER), and its significance in ammonia-containing sewage purification.³⁷ Nevertheless, these articles solely focus on a specific individual energy device. There is still a lack of comprehensive reviews regarding the electrochemical degradation processes of nitrogenous pollutants in sewage, along with these energy storage and conversion devices. Thus, it is crucial to have a comprehensive review to elaborately illuminate the reaction mechanisms of various nitrogenous pollutant-involved electrolytic reactions (nitrate reduction reaction, nitrite reduction reaction, ammonia oxidation reaction, urea oxidation reaction and hydrazine oxidation reaction), the design of corresponding electro-catalysts, and the valorization approaches in electrolytic degradation processes with tailored energy devices (metal-nitrate/nitrite batteries, nitrogen pollutant-driven direct fuel cells, and hybrid water electrolyzers).

With the rapid development of the electrodegradation of nitrogenous pollutants in recent years, including a deeper understanding of electrocatalytic reactions and the development of advanced energy devices (Fig. 2a), a comprehensive review is imperative to comprehensively encompass the advancements in this rapidly growing field and to inspire further scientific endeavors. Herein, we frame this review to provide comprehensive and novel insights into the electrodegradation processes of nitrogenous pollutants, mainly ammonia nitrogen, hydrazine, urea, and nitrate, and relevant energy valorization strategies, highlighting the reaction mechanisms, activity descriptors, electrocatalyst design, and the operational parameters of actuated electrodes in tailored energy conversion devices (Fig. 2b). We commence by providing an overview of the reactions involved, covering aspects such as reaction mechanisms and theoretical principles, to provide basic knowledge for better catalyst design and operation of energy devices. The detailed screening for active electrocatalysts, along with the advanced catalyst design to enhance the catalytic performance, is also presented. Then, we scientifically and systematically introduce the strategies to promote energy valorization during sewage disposal processes with the assistance of tailored electrochemical devices, encompassing (i) electricity and ammonia production with Zn-nitrate/nitrite batteries, (ii) electricity production with direct fuel cells, and (iii) hydrogen production with hybrid water electrolysis devices. We also provide a concrete analysis of the available wastewater streams, pollutant accumulation, and the electrolyte effects, to comprehensively evaluate the practical feasibility. Finally, given the gap between practical application and experimental trials mainly resulting from the fact that the pollutants are usually much more dilute in wastewater, the challenges and prospects of the current status of these promising processes are also given to deepen the understanding of various systems and evaluate their potential applications.

2. Reaction mechanisms

The enrichment of nitrogenous pollutants, originating from the discharge of industrial wastewater and the over-use of fertilizers, adversely impacts the environment and human health.^38–42 Unlike the conventional degradation methods, the electrochemical degradation of N-containing contaminants provides an innovative and efficient approach for economic water purification and restoring the disrupted nitrogen cycle. Electrochemical reactions serve as the cornerstone for the energy storage and conversion devices, playing a pivotal role in their operation and functionality. It becomes imperative to possess a holistic grasp of the intricacies surrounding redox electrochemical reactions and their corresponding catalysts. Given the intricate electrochemical conversion of different N-containing species, the correlation between the standard equilibrium potentials and the pH is illustrated in Fig. 3a.⁴³ The reaction fundamentals for the involved degradation reactions, coupled with the current understanding of smart electrocatalysts, are necessary and thus contribute to the realization of additional values. The schematic diagram of polarization curves for the involved reaction is depicted in Fig. 3b. In this section, the reaction mechanisms and paths are presented and discussed in detail.

2.1 NtrRR

The diversity of reaction pathways and the resulting final products during the NtrRR process greatly hinge on the nature of applied active sites. Thus, it is crucial to comprehend the mechanism and reaction pathway of NtrRR, a proton-coupled electron transfer reaction, with multi-electron steps. N₂ and NH₃ are the thermodynamically stable products in the NtrRR process related to a five-electron transfer to produce N₂ (reaction (1)) and an eight-electron transfer to generate NH₃ (reaction (2)), respectively.⁴⁴

NO3− + 3H2O + 5e− → 1/2N2 + 6OH− E0 = 1.99 V vs. RHE (pH = 14)	(1)

NO3− + 6H2O + 8e− → NH3 + 9OH− E0 = 0.69 V vs. RHE (pH = 14)	(2)

Although the practical reaction paths of NtrRR are complicated and encompass numerous intermediates, the reaction initiates with the adsorption of aqueous NO₃⁻. It is worth mentioning that the adsorbed NO₂*, formed through the reduction of adsorbed NO₃* (the most accepted rate-determining process), is recognized as a stable intermediate and demarcation point whose reaction orientation determines the final products. On the one hand, the adsorbed NO₂* may desorb from the electrode surface and further transform into several side products including NO₂ and HNO₂via non-electrochemical processes. On the other hand, the adsorbed NO₂* absorbs more charge/H_ads and further decomposes into NO* for N₂ and NH₃ fabrication. The reduction of NO₃* to NO₂* significantly influences the whole reaction rate and is identified as a mass-transfer-limited process according to Fick's law. The possible reaction paths toward N₂ and NH₃, along with involved intermediates, are illustrated in Fig. 4a.^45–50 Path I, II, and III were proposed for the NtrRR to N₂. In Path I named the Vooys-Koper mechanism, the adsorbed NO* combines with a mobile NO, acquires a proton and an electron, and transforms into HN₂O₂.⁴⁶ The resulting HN₂O₂ is eventually reduced to N₂ through two successive proton–electron transfer reactions. In this reaction path, the intermediate N₂O*, a weakly ligating molecule, has a propensity to escape from the catalytic surface, resulting in poor selectivity towards N₂. The reaction path over Pt(100) is presented in Path II and known as the Duca-Feliu-Koper mechanism.⁴⁷ The amalgamation between NO* and NH₂* resulting from the hydrolysis reaction with the electron transfer leads to the generation of NH₂NO*, which can subsequently decompose into N₂. Compared to Path I, the Duca-Feliu-Koper mechanism outperforms in the conversion of NO₂* into N₂ with high selectivity owing to the high binding energy of NO* and NH₂*. Regarding Path III, the N₂ species is synthesized through the integration of the N* species formed by the decomposition of adsorbed NO*.⁴⁵ Path IV and V manifest the possible reaction path toward NH₃. NH₃ is generated through the sequential hydrogenation reactions of N* in Path IV, while Path V, known as the ammonia formation mechanism, describes several consecutive proton–electron transfer reactions from adsorbed NO* to NH₃.^48–50 The NtrRR processes described above occur through both hydrogen adsorption and electron reduction pathways. Paths I, II, and III are mediated by electrons (electron-mediated route), while Path IV and V are thought to be mediated by H_ads (H-mediated route). The reduction path mediated by H_ads intermediates presents a thermodynamic advantage over electron-mediated reduction paths due to its high reduction potential. Besides, the indirect NtrRR processes can occur, resulting in the formation of side products such as HNO₂, NO₂, and NO. Under highly acidic conditions and high nitrate concentrations (1.0–4.0 M), the protonation of desorbed NO₂⁻ to form HNO₂ triggers two autocatalytic mechanisms (Vetter mechanism and Schmid mechanism).⁵¹ In Path VI, recognized as the Vetter mechanism, HNO₂ reacts with HNO₃ to produce N₂O₄, which could be reduced to form two NO₂ molecules.⁵² Unlike the Vetter mechanism, the Schmid mechanism (Path VII) posits that NO⁺, formed from the protonation of HNO₂, is the electrochemically active species.⁵³ In Path VII, NO⁺ is electrochemically reduced to NO and subsequently converted into HNO₂.

In practical sewages, large amounts of Cl⁻ usually exist and can alter the reaction direction. It is worth noting that NH₃*/NH₄⁺ can be converted into N₂ in the presence of Cl⁻ according to the “breakpoint chlorination theory”. Precisely, the presence of Cl⁻ can be electro-oxidized to active chlorine species (Cl₂ and HOCl) that can then non-electrochemically oxidize the generated NH₃ to N₂ (reaction (3) and (4)).

Electrochemical oxidization of Cl⁻:

2Cl− → Cl2 + 2e−	(3)

Cl2 + H2O → HOCl + H+ + Cl−	(4)

The reaction pathways taking place on diverse electrode surfaces, which is impacted by both the nature of catalysts and the applied potentials, exhibit marked dissimilarities and are currently an ongoing area of investigation.

2.2 AOR

Given the lower oxidation onset potential, an alkaline medium (pH > 9.25) is thermodynamically and kinetically preferred compared to acidic conditions for AORs. Under acidic conditions, the existing NH₄⁺ exhibits coulombic repulsion towards the catalyst surface with oxidative potentials, culminating in undesirable chemical and electrochemical corrosion issues.^54–56 The ideal AOR is a six-electron transfer process to output non-polluting N₂ (reaction (5)). However, side reactions including incomplete oxidation and peroxidation are inevitable in practical operation, resulting in the formation of undesirable products such as N₂H₄ and NO_x, due to the overlap of the electrochemical windows of the AOR and water oxidation.^57–59

2NH3 + 6OH− → N2 + 6H2O + 6e− E0 = 0.06 V vs. RHE (pH = 14)	(5)

The reaction path of two widely accepted mechanisms, namely the Oswin–Salomon mechanism and the Gerischer–Mauerer mechanism, for AORs are presented in Fig. 4b. The Oswin–Salomon mechanism describes three successive OH⁻-assisted deprotonation processes from adsorbed NH₃* to N* (NH₃* → NH₂* → NH* → N*) followed by the coupling process of two formed N* to N₂.⁶⁰ Meanwhile, the Gerischer–Mauerer mechanism is more complicated, involving both the dimerization of NH_x* (x = 1 and 2) into N₂H_x* (x = 1, 2, 3, and 4) and the OH⁻-assisted deprotonation processes from N₂H_x* to N₂*.⁶¹ It is worth underscoring that the rate-determining process of AOR may not be an electrochemical process but rather the N–N coupling process – a non-electrochemical process whose kinetics are contingent upon the properties of the active sites. The Oswin–Salomon pathway solely entails N–N coupling transpiring in the final step to generate N₂ while the N–N coupling processes are pervasive throughout the Gerischer–Mauerer pathway.

The existence of N–N coupling processes, along with the tendency of different pathways, presents a huge challenge for the selection of AOR catalysts. The pH of the electrolyte can also influence the reaction orientation. The electrochemical AOR processes depend greatly on the pH and necessitate a pH value > 9.25, because ammonia cannot be oxidized in its NH₄⁺ form on the anode surface. Generally, as the concentration of OH⁻ increases, the peak current of the AOR to N₂ shows a linear increase, accompanied by a corresponding decrease in the onset potential.^62–64 In practical acid wastewater, the presence of high-concentration Cl⁻ ions (typically > 300 mg L⁻¹) can exert great impact on the AOR processes and achieve the indirect nonelectrochemical AOR processes. Under the influence of oxidation potential, Cl⁻ ions are electrochemically converted into active chlorine species (Cl₂ and HOCl), which then react with NH₃ under strongly acidic conditions through nonelectrochemical path, Cl⁻ → Cl₂ → HOCl → NH₂Cl → NHCl₂ → N₂ (reaction (6) and (7)).⁶⁵ The HOCl can also react with intermediates such as NH₄⁺ and NHCl₂ to produce nitrate and NCl₃ (reaction (8)–(10)).⁶⁶

Active Cl-mediated nonelectrochemical AOR processes:

3HOCl + 2NH3 → N2 + 3H+ + 3Cl− + 3H2O	(6)

3HOCl + 2NH3 → N2 + 5H+ + 3Cl− + 3H2O	(7)

HOCl + NH4+ → H+ + NH2Cl + H2O	(8)

HOCl + NH2Cl →NHCl2 + H2O	(9)

HOCl + NHCl2 →NCl3 + H2O	(10)

The electrode potential can also impact the reaction path and product distribution. Multiple products of the AOR processes were simultaneously detected by using a novel experimental approach combining online electrochemical mass spectrometry (OLEMS) and ion chromatography (IC), demonstrating the dependence of AOR selectivity on Pt/C surface conditions.⁶⁷ In the low-potential region (0.40–0.82 V vs. RHE), NH₃ underwent dissociative adsorption to form NH_x,ads and subsequently dimerized to N₂H_y,ads, which was the main precursor of N₂. NH_x,ads and N₂H_y,ads served as the surface precursors for NO and NH₂OH, respectively, which were produced via minor routes and detected for the first time in this potential region. In the high-potential region (exceeding 0.82 V vs. RHE), adsorbed O²⁻ was the main oxygenated surface species, owing to the strong interactions between OH⁻ and oxidized Pt. New reaction oxidized products such as NO, NO₂, and N₂O were detected via novel AOR routes. NO₂, N₂H₄, and NH₂OH were deemed as minor products, with N₂ remaining as the predominant product of the AOR in the high-potential region. Advanced investigations are still imperative to elucidate the reaction mechanism and pathway.

2.3 HzORs

Hydrazine serves as a transitive intermediate in the conversion between N₂ and NH₃. The quintessential HzOR is a simple relative reaction related to a four-electron transfer process with dinitrogen production (reaction (11)). As shown in Fig. 3b, the required potential for HzORs (−0.33 V vs. RHE) is notably lower than that of AORs, particularly in an alkaline solution. Furthermore, the absence of the non-electrochemical N–N coupling steps in the HzOR process plays a crucial role in promoting the reaction kinetics due to the double N-atom configuration of N₂H₄.

N2H4 + 4OH− → N2 + 4H2O + 4e− E0 = −0.33 V vs. RHE (pH = 14)	(11)

Regarding the reaction path, although the order of removal of H may be different, the HzOR process can be viewed as a part of the Gerischer–Mauerer mechanism for AORs.⁶⁸ The specific reaction path is presented in Fig. 4c, manifesting successive OH⁻-assisted deprotonation processes of the adsorbed N₂H₄ to synthesize N₂.

2.4 UORs

The alkaline UOR is thermodynamically and kinetically ascendant in view of the existence of electrode corrosion and repulsion issues in neutral/acidic UORs. The UOR in an alkaline aqueous solution is a six-electron transfer reaction with the evolution of N₂ and CO₂ (reaction (12)), involving multiple intermediate transfer steps.⁶⁹ The generation of side products such as N₂O, NO₂, and CO resulting from the inadequate oxidation and/or the overoxidation of urea is usually ineluctable.⁷⁰

CO(NH2)2 + 6OH− → N2 + 5H2O + CO2 + 6e− E0 = 0.37 V vs. RHE (pH = 14)	(12)

The two mainstream reaction paths of UORs, mainly differing from the involved N–N coupling processes, are presented in Fig. 5a. The ramification of these two paths is the reaction orientation of the adsorbed CO(NHNH₂)* stemming from the dehydrogenation of adsorbed CO(NH₂)₂* species. Path I precedes the C–N cleavage/oxidation reaction with the intramolecular N–N coupling process while the C–N cleavage/oxidation reaction occurs prior to the intermolecular N–N coupling process in Path II.^30,71 The existence of the sluggish intermolecular N–N coupling process severely restricts the viability of path II in comparison to the rapid intramolecular N–N coupling process in Path I. The desorption of CO* or COO* with the biggest reaction battery is confirmed as the rate-determining process of the UOR, whether in path I or II. The coverage of CO or CO₂ on the electrode surface may lead to the poisoning of catalytic activity and a short catalytic lifetime.^72,73

Urea, which is an important product of protein metabolism, is synthesized in the liver, transported through the bloodstream to the kidneys, and ultimately eliminated from the body in the urine. The possible reaction pathways under acidic solutions, physiological buffer and saline solutions should be taken into consideration. In acidic electrolytes, analogical to path II, urea undergoes slow hydrolysis, breaking the C–N bond to produce NH_x and the intermediate NH₂CO* or NH₂COO*, which is then electrophilically attacked by chemisorbed hydrogen atoms, leading to the cleavage of another C–N bond and the formation of CO₂*. In physiological buffer or saline solutions, the presence of Cl⁻ can greatly impact the UOR processes mainly on the noble catalyst surfaces.^75–77 The possible reaction paths of UORs in saline solutions and physiological buffers are presented in Fig. 5b and c, respectively.⁷⁴ Similar to Cl⁻-impacted NtrRR to N₂ and active Cl-mediated AOR processes, the Cl⁻ may convert into active chlorine species such as Cl₂ and HOCl, via in situ electrochemical reactions (reaction (3) and (4)), which can oxidize the urea molecules via direct chemical reactions, especially in the acid and neutral solutions.⁷⁸ The active Cl-mediated UOR processes are listed as follows (reaction (13) and (14)):⁷⁷

3HOCl + CO(NH2)2 → N2 + CO2 + 3H+ + 3Cl− + 2H2O	(13)

CO(NH2)2 + H2O → N2 + CO2 + 6H+ + 6e−	(14)

Other reaction conditions such as the applied potential and urea substrate concentration can also influence the reaction paths. The influence of different applied potentials mainly reflected in the competitive reactions including oxygen evolution reactions (OERs) and chlorine oxidation reactions (CORs) due to the similar active species or potential interval.⁷⁹ Besides, the applied potential potently affects the active Cl-mediated UOR processes by altering the dispersal behaviors of Cl species.⁷⁷ Though the active Cl-mediated UOR processes can significantly improve the UOR to N₂, many intermediates and by-products such as chloramines and oxychlorides may be generated during the electrochemical processes.^80,81 Although the kinetic of UORs present no obvious change with varying urea concentrations, it was found that the increasing urea concentration could effectively improve the UOR activity via inhibiting the slide reactions such as OERs and CORs, by reducing the coverage area of OH⁻ and Cl⁻.^82–85 Besides, the increased urea concentration can enhance the UOR to N₂via promoting the intermolecular N–N coupling reaction pathway (path I).⁸⁶ The practical reaction processes are more complicated and still need further research.

3. Theoretical principles and activity descriptors in the electrocatalyst design

Given the complexity of electrodegradation processes, theoretical principles and descriptors serve as crucial tools in experimental studies, guiding the rational optimization of electrocatalysts. Several theories and descriptors have been proposed for the design of efficient electrocatalysts, serving two significant functions in catalyst development: (1) providing a comprehensive understanding of structure–performance relationships at both electronic and atomic levels, and (2) expediting the discovery of advanced catalysts through straightforward and effective activity descriptors. In this section, we introduce the fundamental aspects of the reported catalytic theory and activity descriptors for the application in designing smart electrocatalysts.

3.1 Gibbs free energy

The Gibbs free energy (ΔG) serves as a thermodynamic descriptor to correlate the catalytic activity and can provide further thermodynamic explanations for the post-discussed principles.⁸⁷ Thus, we discuss the Gibbs free energy descriptor antecedent to others. The Gibbs free energy was determined using eqn (I) and (II), where ΔE denotes the adsorption energy of reactant N₂ and intermediates, ΔZPE represents the changes in the zero-point energy, TΔS reflects the entropy changes at the specified temperature, ΔG_U signifies the influence of electrode potential, E_T represents the total energy, E_adsorbate represents the free energy of adsorbed reactants and E_catalyst represents the free energy of applied electrocatalysts:⁸⁸

ΔG = ΔE + ΔZPE + TΔS + ΔGU	(I)

ΔE = GT − Ecatalyst − Eabsorbate	(II)

The density functional theory (DFT) serves as a powerful tool to calculate the Gibbs free energy of electrocatalysts. The computational hydrogen electrode (CHE) model was introduced to replace the free energy of an electron–proton pair with half the energy of a hydrogen molecule at U = 0 V vs. RHE, enabling the determination of reaction intermediate free energies as a function of applied electrode potential and pH.⁸⁹ In principle, this method can also ascertain the free energies of charged reaction intermediates. The CHE model becomes the cornerstone to calculate the Gibbs free energy and evaluate the electrocatalytic activity.

3.2 Sabatier principle

The Sabatier principle, a qualitative concept proposed for heterogeneous electrocatalysts, emphasizes the importance of appropriate adsorption energy for reactants in achieving ideal electrocatalysis (Fig. 6a).⁹⁰ The binding energy between electrocatalysts and reactants should be neither too strong nor too weak. The weak binding energy makes the reaction hard to occur, while the strong binding energy may suspend the reaction due to the enriched reaction intermediates that are difficult to desorb from the catalyst surface.⁹¹ This principle has been extensively used as a fundamental criterion for designing and screening suitable electrocatalysts.

The Sabatier principle is a qualitative theory and lacks precise numerical descriptions, rendering it incapable of accurately evaluating catalyst activity, predicting activity trends, or providing a logical basis for catalyst design.^93,94 Efforts were undertaken to establish correlations between the experimentally measurable physical properties of materials and their catalytic activity. The volcanic curve was proposed based on the Sabatier principle by integrating electrocatalytic activity with physical quantities such as enthalpy of formation and work function.⁹⁵ The volcanic curve makes success in the activity of a range of catalysts in relation to various physical quantities to a certain extent.⁹⁶ However, more efforts are still needed to explore the theoretical basis on account of the too strong empirical nature of volcanic curve.⁹⁷

The Sabatier principle can be explained by the Gibbs free energy.⁹⁸ Taking hydrogen evolution reaction (HER), a catalytic reaction with one reaction intermediate, as an example, the reaction path at acidic electrolytes is presented (eqn (III)).

	(III)

If the binding energy between H* and the electrocatalyst surface is too weak (ΔG₁ > 0), step I (H⁺ to H*) is thermodynamically unfavorable, thus while the binding energy between H* and electrocatalyst surface is too strong (ΔG₁ < 0), step II (H* to 1/2H₂) is thermodynamically unfavorable. Given that the rate-controlling process, the most thermodynamically unfavorable step, governs the entire electrocatalytic reaction, electrocatalysts with a moderate binding energy (ΔG₁ = 0), and consequently, no thermodynamically unfavorable steps are deemed as the ideal catalysts.

The traditional interpretation of the Sabatier principle relies solely on thermodynamic factors, whereas experimental observations inevitably involve kinetic influences. A linear relationship between the change of free energy and activation energy, named Brønsted (Bell)–Evans–Polanyi (BEP) relationship, was established based on pure thermodynamic considerations.^99–101 The BEP principle believes that the free-energy-activation energy is linearly correlated with the reaction free energy.¹⁰² In other words, ΔE = aΔG, where ΔE represents the activation energy, ΔG is the reaction free energy, and A denotes the BEP coefficient (0 < a < 1).¹⁰³ In general, the positive value of a indicates that a thermodynamically unfavorable step tends to correspond with unfavorable kinetics, revealing that the thermodynamically ideal catalyst should also be the kinetically optimum catalyst. In combination of the discussion, this also implies that the electrocatalyst with proper binding energy can also offer favorable kinetic reaction conditions. Although the BEP principle establishes a linear relationship between thermodynamic and kinetic parameters, it may not accurately depict the free energy in some cases. A Marcus theory presents a quadratic relationship between the change of free energy and activation energy , where ΔE represents the activation energy, ΔG is the reaction free energy, and β denotes the Marcus coefficient.¹⁰⁴ For these two principles, the disparity is less conspicuous when closer to equilibrium. Nonetheless, the predictions from the two principles deviate as the overpotential is heightened. Once the overpotential exceeds a certain point, the activation energy begins to rise, indicating a negative BEP coefficient, which is contrary to the assumption of 0 < a < 1.

With the development of computational theories, DFT calculations serve as a powerful tool in comprehending the Sabatier principle.⁹⁹ By accurately predicting the microscopic physical quantities such as surface energy, adsorption energy, and activation energy. DFT enables researchers to ascertain the optimal binding strengths required for efficient electrocatalytic activity. Combining DFT calculations with the BEP principle can significantly reduce theoretical calculation time and expedite electrocatalyst screening processes. Additionally, DFT calculations elucidate the detailed reaction mechanisms occurring on the catalyst surface, offering insights into reaction pathways, transition states, and reaction intermediates. This understanding is crucial for designing catalyst materials that adhere to the Sabatier principle, striking the delicate balance between the adsorption strength and the desorption kinetics.

From traditional materials science to the forefront of machine learning research, there is a unanimous acknowledgment that the binding energy of reaction intermediates serves as a pivotal parameter in forecasting electrocatalytic activity. The concepts of Sabatier principle and the binding energy theory are central to contemporary electrocatalysis and are recognized as useful tools to predict the intrinsic activity of electrocatalysts. In the field of electrodegradation of nitrogenous pollutants, the Sabatier principle serves as an efficient tool to analyze the reactive activity and targeted product selectivity. The bond strength between reactants such as NO₃*, NH₃*, N₂H₄*, and CO(NH₂)₂* and the electrocatalyst surface greatly affects the catalytic performance. Appropriate bond strengths redound to the capture and activation of nitrogenous pollutants, whereas the high bond strength impairs the desorption of products (N₂*, CO₂*, or NH₃*) and the conversion of intermediates (NH_x* and NO_x*). In a typical case, the poisonous effect of N* on noble metals severely limits the applications of noble metals in the electrodegradation of nitrogenous pollutants (especially the AOR processes), due to the strong bond strengths between N* and noble metal sites. It is essential to not only underscore its utility but also to critically address its challenges and limitations, so that this approach not only helps prevent misleading analyses but also provides clarity on the necessary further exploration.

3.3 d-band theory

The Sabatier principle's reliance on a simplistic balance of adsorption and desorption energies, without considering complex reaction mechanisms or other critical factors such as the electronic effects, limits its ability to provide comprehensive and advanced guidance for catalyst design. The electronic structure of the electrocatalyst greatly affects catalytic properties such as the adsorption behavior and electronic cooperativity. The adsorption of adsorbates onto electrocatalyst surfaces can be understood as the interaction between the orbitals of the adsorbates and those of the electrocatalysts from an orbital perspective. The electronic states on transition metal surfaces have been widely investigated. In transition metals, the s- and p-orbitals display a broad overlapping shape, while the d-orbital is localized and narrow. Given the similarity between the s-band and the d-band of most transition metals, the adsorption behavior is predominantly associated with the d-band. Thus, the well-known d-band theory was proposed in 1995 by Nørskov to describe how the electronic structure of transition metal surface, especially the d-orbital, influences the catalytic activity.¹⁰⁵

The d-band theory describes a linear relationship between the adsorption energy and the d-band center (Fig. 6b).¹⁰⁶ The d orbitals of transition metals interact with the orbital of adsorbates The high binding energy between electrocatalysts and adsorbates arises from the elevated d-band center (closer to the Fermi energy level).⁹² In detail, when the d-band center shifts to a higher Fermi energy level, a higher anti-banding orbital is formed after absorbing the reactive molecule, which makes it difficult to fill the high-energy orbitals and thus induces a stable adsorbed structure. Moving across the periodic table from left to right and from top to bottom, the d-band center of transition metals decreases gradually, leading to weaker adsorption.¹⁰⁷

The d-band theory helps explain various properties of transition metal catalysts, such as their ability to activate and stabilize reactant molecules, control reaction pathways, and participate in electron transfer processes. The d-band center theory effectively describes the trend in the variation of adsorption energy for numerous systems including pure metal surfaces, stepped/stained surfaces, and alloy surfaces.¹⁰⁸ By understanding the d-band structure of these surfaces, scientists can design and optimize electrocatalysts for specific reactions and improve their efficiency and selectivity. The determination of the energy position of the d-band center involves a combination of experimental techniques and theoretical calculations including X-ray photoelectron spectroscopy (XPS), scanning tunneling microscopy/spectroscopy (STM/STS), and DFT calculations. The valence band (VB) spectra, recorded by X-ray photoelectron spectroscopy, provide concrete information about the density and occupancy of the electronic state in the valence band of electrocatalysts. The position of the d-band center relative to the Fermi energy level can be obtained by normalized integration of the VB spectra. Besides, STM/STS can provide information about the local electronic structure and density of states (DOS) near the electrocatalyst surface. The energy position of the d-band center can be inferred by analyzing the local density of states (LDOS) and differential conductance spectra. Furthermore, DFT calculation can provide the DOS information of electrocatalyst models by simulating the energy levels of d orbitals and the interaction between adsorbates. The d-band center can be directly obtained by the analysis of the projected density of states (PDOS). Adjusting the d-band center for electrocatalysis is crucial for optimizing the adsorption properties and further improving the electrocatalytic performance. Several strategies such as (1) incorporation of metals with different electronegativities or d-band filling, (2) introduction of surface ligands or functional groups to alter the coordination environment of central metals, (3) doping with elements of different electronegativities or valence states, and (4) introduction of strain effects to adjust the atomic spacing have been proposed.^109–114

The efficacy of the d-band center theory may be limited in some cases. The d-band center descriptor was found deviated when examining coinage metals. The incorporation of Ag, which has a lower d-band center, into Rh led to increased NO adsorption, challenging the predictions of the d-band center theory.¹¹⁵ Other descriptors including d-bandwidth, d-band charge, and p-band center, have been proposed to characterize the adsorption states.^116–118

The d-band center stands as a pivotal theory in electrocatalysis, offering guidance for tailoring the electronic structure and catalytic behavior of transition metal electrocatalysts. Through the precise control of the d-band center, researchers can achieve remarkable improvements in catalytic activity, selectivity, and stability, paving the way for groundbreaking applications in energy conversion, environmental remediation, and chemical synthesis. However, single d-band descriptors may be limited to describe the actual adsorption behaviors. Challenges persist in accurately characterizing the d-band center, understanding its dynamic behavior on surfaces, and integrating theoretical predictions with experimental observations. Nevertheless, the study of the d-band center still holds immense promise for driving the innovation in electrocatalysis and the preparation of efficient electrocatalysts. In the field of electrodegradation of nitrogenous pollutants, the d-band theory can provide prediction, explanation, and guidance for designing advanced electrocatalysts. The enhanced overlap between the d-band orbitals of reactive metals and the molecular orbitals of the nitrogenous pollutants facilitates the adsorption and activation processes. For instance, the high energy level of the lowest unoccupied molecular orbital (LUMO) π* of nitrate favors NtrRR catalysts with a high d-band center and d-band energy. The adsorption and desorption behaviors of NH_x and NO_x intermediates, along with the formation of by-products, can be effectively predicted through the guidance of the d-band theory, thereby leading to a significant improvement in the selectivity for the target products.

3.4 Other descriptors

Additional activity descriptors have also been proposed to elucidate the catalytic behaviors of electrocatalysts such as metal oxides and metal-free catalysts, and serve as supplementary tools for the forementioned principles, which have been extensively utilized in metal electrocatalysts. For instance, the d-band theory primarily aims to characterize the average state of d-orbital electrons and thus face limitations when applied to magnetic materials such as transition metal oxides containing a significant number of unpaired electrons. The spin state is essential for the precise description of the d orbital's electronic state, impacting the strength of metal–ligand bonds and the adsorption behavior of the intermediates.¹¹⁹ Influenced by the splitting energy and electron pairing energy, electrons can adopt high spin, intermediate spin, and low spin states, each of which affects the charge transfer and adsorption behavior differently. High spin states typically result in the generation of more unpaired electrons, consequently boosting the electrical conductivity. The efficiency of electrocatalytic reactions can be inferred from surface structure parameters. The surface coordination number (CN) directly reflects the atomic environment surrounding the active site and exhibits a linear relationship with adsorption energy.¹²⁰

4. Advanced electrocatalysts

The complex mechanisms and reaction paths of the electrodegradation reactions necessitate the advanced electrocatalyst design. Based on the aforementioned theoretical principles and descriptors, the selection criteria for high-performance electrocatalysts have been widely investigated. In this section, the option criteria for the relevant electrocatalysts, coupled with the representative and advanced catalyst design, are elaborately discussed.

4.1 NtrRR electrocatalysts

4.2 AOR electrocatalysts

4.3 HzOR electrocatalysts

4.4 UOR electrocatalysts

5. Electrochemical devices for energy valorization

Based on the related contaminated substrates and their corresponding electrochemical reactions, sound integration of specific reactions with tailored energy devices holds exceptional promise for achieving valorization in electrochemical degradation processes. The chemical energy released during electrochemical redox processes can be harnessed for the generation of added values. The electro-oxidation of nucleophilic N-containing pollutants, including ammonia nitrogen, hydrazine, and urea, has the potential to release tremendous energy due to their high hydrogen content and energy density. Constructing equipment akin to fuel cells in wastewater treatment can efficiently degrade these low-valence nitrogen-containing species while concurrently producing electricity. Besides, electro-reduction reactions such as NtrRRs can analogously be incorporated into electricity generation via peculiar electronic devices, such as metal-nitrate batteries. Furthermore, electro-degradation of nitrogen-containing pollutants offers the potential to directly or indirectly produce high-value chemicals. For instance, the selective reduction of nitrate and nitrite to produce ammonia is recognized as a promising route satisfying value generation and simultaneous pollutant degradation as a promising alternative to the Haber process. Moreover, the electrochemical degradation reactions offer a strategic pathway to support the production of clean energy, hydrogen via innovative hybrid water splitting systems. Hence in this section, the application of efficient energy conversion devices targeted for the output of additional values is elaborately discussed, in tandem with the highlighting of reported driving electrodes and cell design.

5.1 Electricity and ammonia production with Zn-nitrate/nitrite batteries

Nitrate, one of the most widespread water pollutants, greatly ruins the natural ecology and the health of creatures. Electrolysis provides a promising and substantial approach to accomplish nitrate degradation. The Zn-nitrate batteries with the NtrRR cathode and the Zn anode enable the denitration of sewage and valuable chemical NH₃ generation at the cathode, and simultaneous electricity output during the discharge process, offering notable advantages including high energy density, flat discharge voltage, extended shelf life, innate safety, low cost, and environmental friendliness.^355,356 Despite the relatively low theoretical voltage of Zn-nitrate batteries, Zn-nitrate batteries possess a high theoretical energy density compared with Zn–air/oxygen batteries. The typical cell reactions within Zn-nitrate batteries are shown as follows:

Cathode: NO3− + 6H2O + 8e− → NH3 + 9OH−

Anode: Zn + 4OH− → Zn(OH)42− + 2e−

An initial demonstration on the feasibility of Zn-nitrate batteries for electricity production and NH₃ generation was performed using a Pd-doped TiO₂ nanorod array as the cathode and presented passable energy supplement ability (peak power density (PPD) of 0.87 mW cm⁻² and open cell voltage (OCV) of 0.81, and capacity to produce NH₃, 0.03 mmol h⁻¹ cm⁻² yield rate with ∼87% FE).³⁵⁷ Nonetheless, the reported cell performance cannot conform to the requirement of practical application. The NtrRR to NH₃ is a sluggish eight-electron transfer reaction involving multiple intermediates, leading to inevitable byproducts such as N₂, NO_x, and N₂H₄. The generation of these byproducts in Zn-nitrate batteries might lower the batteries’ efficiency, thus propelling the exploration of high-performance cathodic catalysts. Metal-based cathodic materials (Fe, Cu, Ni, Cu, Mo, and Ce), as well as their alloys, oxides/hydroxides, phosphides, and sulfides, have been intensively reported and are discussed in Section 4.1.^358–360 For instance, a Zn-nitrate battery (Fig. 14a) with a Cu nanowire array cathode was reported, and it exhibited high cell performance with an OCV of 0.943 V and a PPD of 14.09 mW cm⁻² (Fig. 14b and c).³⁶⁰ A thermodynamically preferable [2+6]-electron pathway (Convert all nitrate into nitrite and then convert nitrite into NH₃) (Fig. 14d) distinguished from the 8 proton–electron transfer pathway for the NtrRR to NH₃ was detected, meaning that the visible increase in NH₃ production could only be observed when the majority of nitrate had been converted into nitrite. The 2D Cu plate catalyst with a uniform sheet-like morphology and nanosized thickness was also synthesized as the cathode for a Zn-nitrate battery.³⁶¹ Similarly, by constructing the 2D structure of Cu NtrRR electrocatalysts with a smooth fluid field, the assembled Zn-nitrate battery presented an OCV of 1.4 V and an enhanced PPD of 12.09 mW cm⁻², along with an NH₃ FE of 85.4%. The complexity of the NtrRR to NH₃, involving 8-electron and 9-proton transfer, usually poses challenges for single-compound catalysts to retain advantages throughout the entire process. Hence, multi-metallic cathodes have also attracted substantial attention and development.^362–364 For instance, the spinel oxides with flexible ion arrangement, admirable conductivity, and multi-valence structure have been widely studied for electrocatalysis.³⁶⁵ A spinel Zn-nitrate battery with a NiCo₂O₄ nanowire array on carbon cloth, named NiCo₂O₄/CC, as the cathode was reported.³⁶⁶ This assembled Zn-nitrate battery enabled a PPD of 3.94 mW cm⁻² and an NH₃ production rate of 48.5 μmol h⁻¹ cm⁻² in a 0.1 M nitrate solution on account of the synergistic effects between Ni and Co atoms in NiCo₂O₄. Other spinel-based electrodes such as ZnCo₂O₄ NSA/CC,³⁶⁷ Co₂AlO₄/CC³⁶⁸ were also reported. Besides, alloy cathodes have been widely employed in Zn-nitrate batteries, showing advantages in the electronic interaction between metal elements and/or tandem site configurations. For example, a Zn-nitrate battery with a CuNi alloy on a Cu foil, denoted as CuNi NPs/CF, was designed as an electrode, achieving efficient power output and NH₃ production ability with a PPD of 70.7 mW cm⁻² and an NH₃ yield rate of 18.1 mg h⁻¹ cm⁻².³⁶⁹ Parallelly, a Zn-nitrate battery with a tandem Ag/Co₃O₄/CoOOH NW catalyst as the cathode was prepared.³⁷⁰ While the Ag phases catalyzed the conversion of NO₃* into NO₂*, the Co₃O₄ phases preferentially catalyzed the reduction of NO* into NO*, and the subsequent reaction of NO* hydrogenation to NH₃* was mainly catalyzed by CoOOH phases. This Zn-nitrate battery demonstrated a PPD of 2.56 mW cm⁻² and an OCV of 1.32 V with high electrochemical stability. Further, heterostructures and/or heterointerface-based materials with accelerated mass transfer ability and enhanced exposed catalytic sites are deemed as promising cathodic candidates for Zn-nitrate cathodes.^371,372 For example, a hybrid nanoarray catalyst, replete with abundant heterointerfaces, was devised using a dual-template to engineer the interface between hydrogen-substituted graphdiyne (HsGDY) and NiCoBDC (a NiCo-MOF) for the NrtRR process.³⁷³ This prepared NiCoBDC@HsGDY electrode exhibited an outstanding NtrRR catalytic performance, originating from i) the electronic effects between Ni and Co, which promoted the removal of O on NO₃* and water dissociation into H and ii) the HsGDY boosted the adsorption of nitrate and promoted the reduction of NO₃* into NO₂*. Thus, the NiCoBDC@HsGDY endowed the assembled Zn-Nitrate battery with an outstanding cell performance. Analogously, a Zn-nitrate battery assembled with Ru-doped Co nanosheets, which could be reconstructed into Ru/β-Co(OH)₂ heterostructures in situ during the NtrRR process, as a cathode was reported, which exhibited a PPD of 29.97 mW cm⁻² and an NH₃ production rate of 0.38 mmol h⁻¹ cm⁻².³⁷⁴

The above-discussed Zn-nitrate batteries primarily center on the discharge process, involving the continuous degradation of nitrate and consumption of Zn electrode. Rechargeable Zn-nitrate batteries, which necessitate cathodes with bifunctional catalytic abilities for redox couples, are still in their developing stage.³⁷⁷ For instance, an aqueous rechargeable Zn-nitrate battery using the redox couple OER at the anode and NtrRR at the cathode was designed (Fig. 14e).³⁷⁵ A dense membranous Co nanomaterial, named DM-Co, was synthesized as a bifunctional electrode by coupling chemical and electrochemical deposition to promote both the reduction of nitrate into NH₃ and the oxidation of OH⁻ into O₂. The DM-Co catalysts exhibited high catalytic activity toward the NtrRR and OER, granting the rechargeable Zn-nitrate battery an outstanding cell performance of an excellent discharge–charge cyclic durability with obvious degradation after 76 cycles at 12.5 mA cm⁻² (Fig. 14f and g). Similarly, a Fe-doped nickel phosphide catalyst, denoted as Fe/Ni₂P, was reported as the cathode for rechargeable Zn-nitrate batteries.³⁷⁸ The Fe/Ni₂P demonstrated high NtrRR catalytic performance, attributed to the regulated electronic configuration through Fe doping, leading to the downshift of the d-band center of Ni atoms. This catalyst granted the Zn-nitrate battery an admirable cell performance (OCV of 1.22 V; PPD of 3.25 mW cm⁻²; NH₃ yield of 0.03 mmol h⁻¹ cm⁻²) and adequate cycling ability. Rechargeable Zn-nitrate actuated by the Mott–Schottky heterojunction structured electrode was also reported.³⁷⁹ The Co-B@CoO_x Mott–Schottky cathode formed nucleophilic/electrophilic regions, thus optimizing not only the nitrate affinity but also the H₂O decomposition behavior to produce active H. The rechargeable cell not only enabled a PPD of 4.78 mW cm⁻² and an NH₃ yield rate of 0.89 mg h⁻¹ cm⁻², but also presented a high cycling stability with a negligible change in charge/discharge voltage gaps after 8 h charge/discharge cycles at a current density of 2 mA cm⁻².

Given the instability of the Zn plate under acidic conditions, the alkaline-acidic hybrid Zn-nitrate batteries have been devised to obtain electro-degradation of nitrates in acidic electrolytes. The alkaline-acidic Zn-nitrate composed an alkaline anode electrolyte and an acidic cathode electrolyte, separated by a bipolar membrane. Ultrathin RhNi bimetallenes with an Rh-skin-type structure, denoted as RhNi@Rh BMLs, were synthesized for acidic NtrRRs and served as the cathode for alkaline-acidic hybrid Zn-nitrate batteries.³⁸⁰ The presence of Rh-skin atoms can prevent Rh dissolution induced by NO₂*/NH₂* adsorption, thereby enhancing the exceptional electrocatalytic durability during the acidic NtrRR process. The RhNi@Rh BMLs allowed the alkaline-acidic Zn-nitrate battery an OCV of 1.39 V and a PPD of 10.5 mW cm⁻². Similarly, the use of Fe phthalocyanine/TiO₂ (FePc/TiO₂) as the cathode for alkaline-acidic Zn-nitrite batteries was reported.³⁸¹ FePc/TiO₂ exhibits poor HER activity and enhanced nitrate adsorption, thus fascinating the selective NtrRR to NH₃. The assembled Zn-nitrate battery presented a high OCV of 1.99 V and a PPD of 91.4 mW cm⁻².

Alongside the advancements in Zn-nitrate batteries, Zn-nitrite batteries have also been developed to decontaminate the nitrite in sewage and achieve simultaneous NH₃ and power output. The cell reactions are shown as follows:^{376,382–386}

Cathode: NO2− + 5H2O + 6e− → NH3 + 7OH−

Anode: Zn + 4OH− = Zn(OH)42− + 2e−

For the first time, electricity generation and NH₃ production were achieved in a Zn-nitrite battery using nanoparticle-assembled carbon-doped Co oxide nanotubes (C/Co₃O₄) as the electrode to boost the electro-reduction of nitrites.³⁷⁶ The presence of interstitial C dopants induced a localized electric field which effectively enhanced charge transfer during the nitrite degradation process, significantly reducing the energy barrier for the hydrogenation of N* (Fig. 14h). The Zn-Nitrite battery (Fig. 14i) assembled with C/Co₃O₄ as the cathode displayed a PPD of 6.03 mW cm⁻² (Fig. 14j) and an NH₃ yield of 47.16 μmol h⁻¹ cm⁻² at 8 mA cm⁻² with a high FE of 95.1% at 12 mA cm⁻² (Fig. 14k). Dual-atom catalysts with Fe-Cu atomic pair sites, named FeCu DAC, were synthesized by introducing Cu to tune the electronic configuration of the single Fe atom center as the electrode for the Zn-nitrite battery.³⁸⁷ The Zn-based battery with an OCV of 1.463 V achieved a high NH₃ FE of 89.27% and a high NH₃ yield of 9435 μg h⁻¹ mg_catal⁻¹ at 20 mA cm⁻². Other cathodic electrodes such as TiO₂ nanoarrays,³⁸² WO₂/W,³⁸³ and FeCu SAC,³⁸⁴ Cu₃Ni/Mxene,³⁸⁸ and CuFe-P/IF,³⁸⁶ for Zn-nitrite batteries have also been explored, which exhibited admirable cell performance.

The reported works for Zn-nitrate/nitrite batteries are listed in Table 6, with detailed parameters for the discussed cells as a supplement. Zn-nitrate/nitrite batteries have emerged as promising techniques to realize nitrate/nitrite degradation and energy output along with NH₃ production. Noble-free metal-based catalysts as effective cathodes for Zn-nitrate batteries have been intensively designed and attained passable cell performance. Although the Zn-nitrate batteries offer the potential for “kill three birds with one stone”, the gap between experimental trial and practical application still needs to be abridged. The sluggish cathodic reaction in Zn-nitrate/nitrite batteries still propels the exploration of efficient catalysts with qualities to activate the nitrate/nitrite and elevate the catalytic selectivity toward NH₃. Besides, given the high-concentration nitrate in neutral and alkaline electrolytes required to achieve a high cell performance, more investigations are required to promote the Zn-nitrate/nitrite batteries conducted under acidic conditions with low-concentration nitrates. Furthermore, albeit the valuable NH₃ is generated on the cathode, the timely NH₃ collection is highly needed to avert the secondary pollution induced by NH₃, driving the development of the Zn-battery cell devices.

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5.2 Electricity production with hybrid direct fuel cells

Direct fuel cells represent an advanced means to facilitate the direct conversion of chemical energy from fuel sources into electrical energy and possess a broad spectrum of mobile and transportation applications, showing advantages in their superior efficiency, convenient operation, cost-effectiveness, and environmental sustainability.³⁸⁹ Although fuel cells using hydrogen as clean and renewable energy exhibit high energy density, zero emissions, and zero noise, the challenges associated with hydrogen storage and transport issues remain hurdles. The utilization of nucleophilic N-pollutants with high energy density in sewage, along with their corresponding electro-oxidation reactions, presents a promising avenue for developing direct fuel cells while simultaneously addressing contaminant removal.

5.3 Hydrogen production with water electrolysis devices

Hydrogen has emerged as a promising fuel with unique advantages, encompassing high energy density, recyclability, and zero-CO₂ emission.⁴⁶¹ Although traditional techniques for hydrogen production, including steam reforming and coal gasification, currently account for over 95% of the H₂ output, their further application is hampered by induced environmental concerns.⁴⁶² Water splitting system represents an efficient method for producing high-purity hydrogen fuel utilizing available clean energy sources, such as wind and solar energy.⁴⁶³ However, the sluggish kinetics of anodic OER, involving a four-electron transfer process, necessitates high energy consumption to overcome the substantial energy barrier.⁴⁶⁴ Alternative strategy is essential to minimize the required energy input. Hybrid water electrolysis, involving the electrocatalytic oxidation of low reaction energy barrier small molecules, presents an effective approach to circumvent the drawbacks in conventional water splitting systems.^35,465,466 In our previous review, we conducted a comprehensive and elaborate analysis of the selection criteria for appropriate anodic reactions, electrocatalysts, and reaction parameters involved in hybrid water electrolysis, guiding the direction of investigation on hybrid electrolysis.⁴⁶⁷ The electro-oxidation of N-containing pollutants in sewage including urea, hydrazine, and ammonia possess a lower potential and more rapid reaction kinetics than OERs (1.23 V vs. RHE), as shown in Fig. 2b. Hybrid water splitting using these sewage as anodic electrolytes allows more efficient hydrogen production at the cathode and simultaneous water decontamination at the anode.⁴⁶⁸ In this section, the latest N-containing pollutant-assisted water electrolysis systems are discussed from the perspective of both pollutant degradation and hydrogen output.

5.4 Practical feasibility analysis

Adequate added values achieved with the aforementioned devices, for instance electricity, hydrogen, and other valuable chemical outputs, usually lie on high-concentration pollutant sewage.²³ The discussed works are usually over-ideal and relied on modeled electrolytes. Given the diverse scales, characteristics, and different nitrogenous pollutants content of the available sewage streams, a practical analysis on real wastewater is essential to promote the practical applications.

6. Conclusions and prospects

The N-containing pollutants in water bodies greatly perturb the natural nitrogen cycle and induce severe health issues. Different from the conventional methods for water decontamination, electrolysis is a promising approach to remove the nitrogenous pollutants in sewage. Reasonable integration of the electro-degradation processes with tailored energy conversion device can boost the realization of added values. In this review, we start with a brief introduction to the reaction mechanism of the involved electrochemical reactions such as NtrRRs, AORs, HzORs, and UORs, along with the selection criterion of high-performance catalysts. Then, the valorization strategies by resorting to energy storage and conversion devices has been scientifically and comprehensively discussed, including the NH₃ and power output through Zn-nitrate/nitrite batteries, electricity generation through direct fuel cells, and hydrogen production through hybrid water electrolyzers. The advances in the development of highly efficient electrodes to actuate these devices have been emphatically underlined. A practical discussion on the different sewage sources, pollutant enrichment methods, and electrolyte effects, is appropriately discussed. Albeit abundant progress has been made, several issues remain yet to be addressed to abridge the gap between experimental tests and practical applications. Herein, the challenges and prospects are proposed (Fig. 20) and we hope this article can provide a guidance to further researches.

In-depth investigating the reaction mechanism

The complexity of the N-containing pollutants, along with the numerous and complicated intermediates during the electro-degradation processes, poses a challenge to the exploration of reaction pathways critical for advancing the development of corresponding catalysts. Though several widely accepted reaction paths have been proposed, the degradation reactions involved multi-electron transfers, such as the 6-electron transfer UOR process and 8-electron transfer NtrRR process to NH₃, may offer alternative mechanisms beyond the reported mechanisms. For instance, the 8-electron proton-coupled electron transfer reaction path for NtrRR to NH₃, mediated by active H, is generally acknowledged. A different [2+6]-electron NtrRR pathway was proposed and achieved on a Cu-nanowire-array.³⁶⁰ The whole NtrRR process is separated into two stages and the generation of NH₃ can be observed when the nitrate is completely consumed. Likewise, the “E-C” UOR mechanism on NiOOH surface has been widely investigated on account of the accelerated kinetic. A novel and energetically favorable UOR pathway was proposed and triggered by a nickel ferrocyanide catalyst.³¹² Distinct from the currently understood mechanism, the proposed UOR mechanism involved a chemical process from urea to NH₃ and an electrochemical process from NH₃ to N₂ on the catalysts surface. Thus, in-depth investigations on the involved reaction mechanisms are still required. In situ and operando characterization techniques including in situ X-ray absorption spectrum, in situ X-ray photoelectron spectrum, in situ Raman spectrum, and in situ transmission electron microscopy are efficient approaches to identify the intermediates, structural evolution, and real catalytic species in the actual reaction processes. Besides, DFT calculation is deemed as a potent tool to predict and probe the structure of reaction energy barrier, reaction intermediates and electronic states. These tools can help advance cognition on the reaction paths and mechanisms at multiple scales. It is noteworthy that there is a gap between the performance of practical catalysts in practical reaction processes and the idealized model surfaces. Conducting microkinetic analysis of reactions is imperative for faithfully capturing experimental conditions and gaining deep insights into pivotal industrial reactions.

Advances in electrode materials

The sluggish kinetics of these electro-removal reactions impede the improvement of the efficiency of aforementioned energy storage and conversion devices that greatly relies on the catalytic activity of related electrodes. Currently, noble metal catalysts have exhibited outstanding activity in electrochemical reactions involving active hydrogen species due to their high affinity to hydrogen. However, the high production cost greatly restricts the further adoption of the noble metal in this field. Thus, given the economy principle, transition metal catalysts, spanning their alloys, nitrides, sulfides, and phosphides, have attracted much attention and undergone intensive investigation to elevate the removal efficiency of N-containing pollutants. Several design strategies, including heteroatomic doping, heterojunction establishment, confinement, and supports modification, to construct high-performance catalysts with high activity, selectivity, and durability have been reported. These strategies involve the regulation of microenvironments, fine-tuning the electronic states of active compounds, and enhancing accessibility to active sites. Nevertheless, the current-stage catalytic performance of these non-precious metal catalysts is generally unsatisfactory. In practical tests, the non-precious metal catalysts suffer from the electrode corrosion, especially in acidic solutions, and agglomeration of active species issues. Besides, it is important to enhance the ability of electrodes to capture specific pollutants for the well function in low-concentration sewage sources. Hence, there remains a pressing need to develop high-performance and cost-effective electrodes, particularly multifunctional electrodes capable of both pollutant degradation and value-added processes.

Comprehensive evaluation on electrodes

As discussed in Section 4, different from the sewage simulated in the lab, the actual sewages are complicated in pollutant concentration and substance composition. To bridge the gap between industrial application and experimental tests, a thorough evaluation of the electrodes becomes imperative. First of all, current electrochemical testing of the electrodes for NtrRRs, AORs, HzORs, and UORs is mostly conducted in alkaline aqueous solutions to obtain satisfactory results. Neutral and acidic electrolytes are usually unfavorable resulting from the electrode corrosion and repulsion issues. For instance, the reported hybrid water splitting system for pollutant removal and hydrogen production typically operates in high-concentration alkali liquors (usually pH ≥ 14), which increases the cost of devices and, to some extent, deviates from practicality. Thus, it is urgent to assess the electrodes’ performance in a universal pH range. Besides, electrochemical tests at a high current density are also significant to assess the possibility of commercial applications. Furthermore, considering the diversity and complexity of the ingredients in sewage, it is necessary to evaluate the influence of the various impure ions and molecules during the electrochemical tests, especially when the electrocatalytic reactions of impurities have the adjacent reaction potential interval compared to the targeted reactions. For instance, in our previous work, we elaborately evaluated the impact of Cl⁻ in the hybrid water splitting process and found that the existence of Cl⁻ has no adverse impact on the cell performance even at an industrial current density level.⁴⁷⁷

Translation to practical applications

To stratify industrial applications, the energy conversion devices should be constructed subtly, considering the pH and temperature tolerance of electrolyte circulation systems, electrodes, membranes, and electrochemical cells. Cells, such as the pollutant-assisted direct fuel cells, may require high temperatures to operate, in which the high temperature stability of the devices needs to be carefully considered. The optimal pH conditions for the reported electrode reactions typically fall within a strongly alkaline environment. This poses challenges for the cell materials. Besides, the post-processes for product collection should be coped properly. In particular, concerning the Zn-nitrate/nitrite batteries for NH₃ and energy output that usually operating at room temperatures, enhancing the mass transfer and achieving the separation of NH₃ from electrolytes is still a big challenge. Likewise, the design of timely hydrogen collection equipment for pollutant-assisted water splitting systems is an urgent need to promote the continuous water electrolysis. Furthermore, pre-procedures, like necessary pH control, sewage concentrate, and impurity separation of the protogenetic wastewater streams, are essential. Considering the costs associated with all of the above-mentioned procedures, demonstrating that the economic feasibility is crucial for the practical application of electrochemical systems. Practically, technoeconomic analysis can provide a comprehensive framework for assessing feasible electrochemical processes and promote the practical applications.

Data availability

The datasets used and/or analyzed during the present study are available from the corresponding author upon reasonable request.

Conflicts of interest

There are no conflicts of interest to declare.

Acknowledgements

This work was supported by the National Natural Science Foundation of China (22179065, 22105108).

Notes and references

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