Efficient Hydrogen Production Research Articles

High transmittance BiVO4 thin-film photoanodes by reactive magnetron sputtering for a photovoltaic-photoelectrocatalysis water splitting system

As the system with the highest solar hydrogen conversion efficiency, the further improvement of photovoltaic-photoelectrocatalysis (PV-PEC) efficiency is dependent on the light transmittance, activity and stability of the photoanode. Here, a highly permeable BiVO4 thin film was fabricated through controlled magnetron sputtering. The thickness of the thin film was merely 345 nm, while its transmittance in the visible light range reached as high as 70%. Moreover, large-scale production of such films could be achieved. By incorporating NiFeOx oxygen extraction cocatalyst, under AM 1.5G illumination, the photocurrent density at 1.23 V on reversible hydrogen electrode (RHE) increased to 4.2 mA cm–2 and the incident photon-current conversion efficiency reached 70%. A PV-PEC system was designed to efficiently harness sunlight by integrating the photoanode with a solar photovoltaic panel. Upon connection with the solar photovoltaic panel (with an efficiency of only 7%), spontaneous water decomposition could be achieved, resulting in a solar-to-hydrogen conversion efficiency (ηSTH) of 4.2% for the series system. This study contributes to the realization of cost-effective and highly efficient PV-PEC hydrogen production.

Effect of Pretreatment of Anaerobic Acid Fermentation Sludge from Mixed Swine Wastewater and Food Waste Leachate on Biohydrogen Generation

Objectives:This study aims to investigate the effects of heat shock and 2-bromoethanesulfonate (2-BES) injection on hydrogen production and methanogens inhibition in anaerobic acid fermenter sludge and methane fermenter sludge using mixed swine wastewater and food waste leachate as substrates. Additionally, the analysis of biogas, fermentation products such as volatile fatty acids (VFAs) and alcohols, and microbial community changes were conducted to derive efficient pretreatment conditions for anaerobic hydrogen generation.Methods:Sludge samples were collected from two-phase anaerobic digesters treating swine wastewater and food waste leachate. Heat shock (90°C, 15 min) and 2-BES injection (1, 5, 10, 50, and 100 mmol/L) pretreatments were applied to the each sludge, along with control reactor without pretreatment before anaerobic digestion. Batch experiments were conducted at 30°C to assess biogas, organic compounds (COD, VS, VFAs, and alcohols), and microbial community composition.Results and Discussion:In methanogenic sludge, hydrogen gas was not produced under all conditions, but heat shock method inhibited methane production more effectively than 2-BES injection method. As the concentration of 2-BES increased, methane production decreased. Conversely, hydrogen was produced from the all acid fermentation sludges, mainly attributed to the butyric acid production by dominant Clostridium spp., but the pattern of biogas production varied over time. In the experimental group injected with 2-BES, even at a low concentration of 1 mmol/L, methane gas did not produce due to the inhibition of methanogens. However, in the control group, produced hydrogen was entirely converted to methane by hydrogenotrophic methanogens such as Methanobrevibacter and Methanosphaera. The heat shock group showed delayed hydrogen production due to prolonged lag phase of hydrogen-producing bacteria, with hydrogenotrophic methanogen metabolism starting after 12 days. Heat shock and 2-BES injection reduced bacterial diversity in the acid fermentation process compared to the initial stage.Conclusion:For efficient anaerobic hydrogen production from swine wastewater and food waste leachate, 2-BES injection into the acid fermentation sludge was found to be a preferable method over heat shock, considering hydrogen production efficiency and sustained methanogen inhibition. Further research is needed to find more economical and efficient pretreatment methods and operational strategies considering subsequent methane production processes for practical application in the field.

Vertically aligned ReS2 on MOF deorived CoS2–C hybrid as core-shell catalyst for promoting overall water splitting

The rational design of a core-shell structured electrocatalyst is important to improve the efficiency of electrocatalytic hydrogen production through water splitting. Herein, the catalyst is composed of rhenium disulfides (ReS2) vertically grown on cobalt sulfides/carbon hybrid by hydrothermal and activation treatment (CoS2–C@ReS2/CFP). The core-shell structure is constructed by sulfurizing the cobalt-based metal-organic framework, preventing the restacking of the ReS2 nanosheet, exposing more active sites, and facilitate electrolyte ion diffusion. Moreover, the CoS2–C@ReS2/CFP catalyst shows exceptional performance during the hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) process in an alkaline electrolyte. At ·10 mA cm−2, the overpotentials of the CoS2–C@ReS2/CFP catalyst are 85 and 257 mV during the HER and OER processes with the small Tafel slope, low charge transfer resistance and exceptional catalytic stability. The combination of the CoS2 core and ReS2 shell is designed to adjust the adsorption energy of water molecules, promoting water dissociation, and enhancing the catalytic activity of CoS2–C@ReS2/CFP catalyst. This work provides an efficient strategy for developing the core-shell structured catalysts, potentially advancing the practical application into water splitting for hydrogen production.

Characterized on hydrogen properties and mechanism of Al–Sn–Bi composite powder in salt solutions

Using low-melting point elements to promote the Al/H2O reaction has garnered considerable attention because it is an economical approach to hydrogen supply. Herein, .Al–Sn–Bi composite powder was prepared through milling. The Al–Sn–Bi composite powder and the hydrolysate were investigated using X-ray diffraction (XRD) and scanning electron microscope (SEM). The results show that the hydrolysis products is primarily AlOOH. The properties of the Al/H2O reaction were systematically characterized in salt solutions. Results show that the presence of Sn and Bi is beneficial to achieve short introduction times and large Al/H2O reaction rates. The hydrogen generation rate of the Al–Sn–Bi composite is 4566 mL min−1 g−1 and 3600 mL min−1·g−1 with NaCl and Na2SO4 solutions, respectively and the hydrogen production efficiency can reach 100% in 1 min. Additionally, the mechanism of Sn and Bi promoting Al/H2O reaction was characterized by density functional theory (DFT) calculations. The DFT calculations show that Sn and Bi replace 1/8 ML, 1/4 ML and 1/2 ML surface atoms of Al (111), the surface chemical potential increases with increasing doping concentration, and the electrode potential decreases with increasing doping concentration. The presence of Sn and Bi increases the surface chemical potential and reduces the electrode potential, this is conducive to the microcell reaction and promotes the Al/H2O reaction.

Edge-Rich 3D Structuring of Metal Chalcogenide/Graphene with Vertical Nanosheets for Efficient Photocatalytic Hydrogen Production.

Constructing pertinent nanoarchitecture with abundant exposed active sites is a valid strategy for boosting photocatalytic hydrogen generation. However, the controllable approach of an ideal architecture comprising vertically standing transition metal chalcogenides (TMDs) nanosheets on a 3D graphene network remains challenging despite the potential for efficient photocatalytic hydrogen production. In this study, we fabricated edge-rich 3D structuring photocatalysts involving vertically grown TMDs nanosheets on a 3D porous graphene framework (referred to as 3D Gr). 2D TMDs (MoS2 and WS2)/3D Gr heterostructures were produced by location-specific photon-pen writing and metal-organic chemical vapor deposition for maximum edge site exposure enabling efficient photocatalytic reactivity. Vertically aligned 2D Mo(W)S2/3D Gr heterostructures exhibited distinctly boosted hydrogen production because of the 3D Gr caused by synergetic impacts associated with the large specific surface area and improved density of exposed active sites in vertically standing Mo(W)S2. The heterostructure involving graphene and TMDs corroborates an optimum charge transport pathway to rapidly separate the photogenerated electron-hole pairs, allowing more electrons to contribute to the photocatalytic hydrogen generation reaction. Consequently, the size-tailored heterostructure showed a superior hydrogen generation rate of 6.51 mmol g-1 h-1 for MoS2/3D graphene and 7.26 mmol g-1 h-1 for WS2/3D graphene, respectively, which were 3.59 and 3.76 times greater than that of MoS2 and WS2 samples. This study offers a promising path for the potential of 3D structuring of vertical TMDs/graphene heterostructure with edge-rich nanosheets for photocatalytic applications.

Long‐Lasting Hybrid Seawater Electrolysis Enabled by Anodic Mass Transport Intensification for Energy‐Saving Hydrogen Production

AbstractHybrid water electrolysis offers a groundbreaking approach to energy‐saving hydrogen production by utilizing thermodynamically favorable and value‐added reactions to replace sluggish anodic oxygen evolution in overall water splitting. However, numerous anodic processes generate intermediates or products incompatible with aqueous environments, thereby degrading anodic performance to limit the efficiency and durability of hybrid water electrolysis. Herein, this difficulty is addressed by applying anodic mass transport intensification in conjunction with catalyst engineering, realizing a long‐lasting hybrid seawater electrolysis coupling sulfion oxidation reaction (SOR) for efficient hydrogen production below 1.2 V at an industrial‐level current density of 500 mA cm−2. An exceptional longevity of 2000 h is achieved for the electrolysis by eliminating anode passivation by sulfur deposition during SOR, a general concern in the sulfur‐involved industrial sector. This technology cut the electricity expense of hydrogen production to 2.80 kWh m−3 H2, undercutting alkaline water electrolysis by 34.9–51.1%. Simultaneously, fast upcycling of sulfion pollutants to value‐added sulfur is achieved to add additional economic and environmental profits, enabling hydrogen production at a midpoint expense ($ 0.93) of the United States Department of Energy's 2026 target ($ 2.0) for the cost per gallon of gasoline‐equivalent.

Nanoscale-Confined Synthesis of 2D Metal Compounds for Electrochemical Applications.

2D metal compounds, such as transition metal dichalcogenides (TMDs), layered double hydroxides (LDHs), and MXenes, are emerging as important electrocatalyst materials in the transition to a sustainable energy future. Aided by their high surface area, electrical conductivity, and tunable electronic properties, these materials have provided a crucial research thrust in enhancing the efficiency of green hydrogen production, fuel cells, and carbon reduction processes. Most importantly, the synthesis of nanostructured 2D compounds, while challenging, is the key to optimizing their catalytic performance. Recent advancements in this field have highlighted the potential of 2D metal compounds in revolutionizing energy conversion technologies, which entails the discovery of new material compositions, the development of novel synthetic routes, and the integration of these materials into practical energy conversion systems. This review presents an overview of the distinctive characteristics of nanoscale-confined 2D metal compounds, the challenges encountered in their synthesis, and electrochemical applications.

Boosting 5-Hydroxymethylfurfural Electrooxidation by Porous Biochar via Loading Numerous Surface-Exposed Cobalt Phosphonates.

The electrooxidation of 5-hydroxymethylfurfural (HMF) into 2,5-furandicarboxylic acid (FDCA) demonstrated its unique superiority, not only in reducing overpotential and improving energy conversion efficiency for green hydrogen production but also in utilizing abundant biomass resources and producing high-value-added chemicals. However, designing highly efficient electrocatalysts for HMF electrooxidation (HMF-EOR) with low cost and high performance for large-scale production remained a huge challenge. Herein, we introduced an easy one-step activation process to produce P-doped porous biochar loaded with multiple crystal surfaces exposed to CoP2O6 catalysts (CoP2O6@PC), which exhibited outstanding electrooxidation performance. To achieve a current density of 50 mA cm-2, only a low overpotential of 200 mV was needed for the electrooxidation of HMF in 1.0 M KOH + 10 mM HMF. This performance far surpassed that of other similar materials. CoP2O6@PC exhibited outstanding HMF-EOR performance with high conversion (nearly 100%), selectivity (97.1%), faradaic efficiency (95.3%), and robust stability. This work represents a promising strategy to fabricate macroscale and low-cost HMF-EOR electrocatalysts and achieve potential industrial applications of HMF-EOR.

Oxide-modified HZSM-5 for efficient production of hydrogen via steam reforming of dimethyl ether

Oxide-modified HZSM-5 for efficient production of hydrogen via steam reforming of dimethyl ether

Heterojunction engineering via in-situ electrochemical reconstruction for boosting electrocatalytic biomass upgrading-coupled hydrogen production

Rationally designing and constructing high-performance electrocatalysts is critical for environmental and sustainable electrocatalytic biomass upgrading coupled with hydrogen evolution. Herein, we developed a novel in-situ electrochemical reconstruction strategy to fabricate heterostructured electrocatalysts for efficient biomass upgrading-coupled hydrogen production. Through in-situ anodic and cathodic electrochemical reconstructions, Ni(OH)2-CuO nanorods assembled by nanosheets with abundant low-crystalline Ni(OH)2/crystalline CuO heterojunctions on Cu foam (Ni(OH)2-CuO/CF) and S-doped Ni(OH)2-Cu2O nanofoam formed by cross-linked nanoparticles on CF (Ni(OH)2-Cu2O(S)/CF) were respectively constructed for electrocatalytic 5-hydroxymethylfurfural oxidation reaction (HMFOR) and hydrogen evolution reaction (HER). For the Ni(OH)2-CuO/CF, the overall configuration of nanorods assembled by self-standing nanosheets ensures good conductivity, full exposure of active sites, and fast mass/electron transfer. The abundant Ni(OH)2/CuO heterojunctions provide dual active sites of Ni and Cu to simultaneously adsorb and activate hydroxyl and aldehyde groups in HMF. The electronic interaction between Ni(OH)2 and CuO accelerates the reversible conversion of Ni2+↔Ni3+ to generate more Ni3+ active species and enhances the intrinsic activity of dual active sites to reduce the reaction energy barrier of the rate-determining step. As a result, the Ni(OH)2-CuO/CF shows superior HMFOR performance, with a HMF conversion of 99.3%, a FDCA yield of 98.1%, and stability for 50 cycles in 10 mM HMF+1.0 M KOH medium. Meanwhile, the Ni(OH)2-Cu2O(S)/CF also exhibits remarkable HER activity with an overpotential of only 64.7 mV at 10 mA cm−2 in 1.0 M KOH solution due to its unique structure and composition. When coupling a two-electrode system, the HMFOR-HER system achieves a current density of 10 mA cm−2 at 1.44 V, 221 mV lower than that of the OER-HER system. This work provides an in-situ electrochemical reconstruction strategy for designing advanced heterojunction-rich electrocatalysts for various electrocatalytic applications.

Sulfonated graphene oxide linked with alkali metal ions membranes for proton conductivity in hydrogen production from water electrolysis

Amid technological advances, rising energy demand, and environmental concerns, countries endorse green energy solutions. Prominent among them is hydrogen production via clean water electrolysis, a key strategy for sustainable development. Herein, to address the limitations of expensive and potentially harmful Nafion membranes, we have developed a new graphene oxide (GO) series membranes (hydrophilic sulfonated GO (GO-SO3H) linked with monovalent alkali metal ions were synthesized to fabricate the membranes) to be used in water electrolysis for hydrogen production by introducing the iodide oxidation reaction (IOR) as an alternative to the traditional oxygen evolution reaction (OER). Various modifications by sulfuric acid, methanol, and different alkali metal hydroxides (LiOH, NaOH, KOH) result in membranes with distinct properties. Characterization techniques, including ATR-FTIR, SEM, AFM, XRD, water contact angle (WCA), and electrochemical impedance spectroscopy (EIS), validated the modifications, assessed membrane morphology, interlayer spacing, hydrophilicity, and electrical properties. Among the membranes, GO-SO3K stood out, exhibiting the highest proton conductivity (119.16 mS) and superior potassium ion permeability (20.382 cm/s). Importantly, all GO series membranes demonstrate excellent stability in the electrochemical system. The findings suggested that GO-SO3K holds promise as a potassium ion-conductive membrane for efficient and sustainable hydrogen production, offering a viable alternative to conventional Nafion membranes in water electrolysis applications.

ZnO/TiO2 heterojunction nanorod array for efficient photoelectrochemical water splitting

This study presents a novel approach utilizing a simple, stable, reproducible CV (Cyclic Voltammetry) electrodeposition method to deposit varying amounts of ZnO onto ordered TiO2 (Rutile) nanorod arrays. Comprehensive investigations were conducted on the morphology, semiconductor band-gap structure of different ZnO/Rutile composites, and their performance in photocatalytic (PC) and photoelectrochemical (PEC) hydrogen production. Results demonstrate that the ZnO/TiO2 photoanodes fabricated in this manner exhibit outstanding PC/PEC hydrogen production capabilities. Particularly noteworthy is the Z/R-15 photoanode, showcasing superior PEC performance with a photocurrent density 3.5 times higher than that of the pristine TiO2 photoanode under equivalent conditions. Furthermore, it was observed that depositing ZnO onto highly crystalline, annealed TiO2 nanorods yields optimal photoelectrical properties. Incorporating oxygen-rich vacancies in ZnO significantly enhances the photoelectrocatalytic performance of TiO2 photoanodes. The CV electrodeposition method offers valuable insights for developing efficient photocatalytic hydrogen production catalysts.

Full-Space Electric Field in Mo-Decorated Zn2In2S5 Polarization Photocatalyst for Oriented Charge Flow and Efficient Hydrogen Production.

Integration of photocatalytic hydrogen (H2) evolution with oxidative organic synthesis presents a highly attractive strategy for the simultaneous production of clean H2 fuel and high-value chemicals. However, the sluggish dynamics of photogenerated charge carriers across the photocatalysts result in low photoconversion efficiency, hindering the wide applications of such a technology. Herein, we overcome this limitation by inducing the full-space electric field via charge polarization engineering on a Mo cluster-decorated Zn2In2S5 (Mo-Zn2In2S5) photocatalyst. Specifically, this full-space electric field arises from a cascade of the bulk electric field (BEF) and local surface electric field (LSEF), triggering the oriented migration of photogenerated electrons from [Zn-S] regions to [In-S] regions and eventually to Mo cluster sites, ensuring efficient separation of bulk and surface charge carriers. Moreover, the surface Mo clusters induce a tip enhancement effect to optimize charge transfer behavior by augmenting electrons and proton concentration around the active sites on the basal plane of Zn2In2S5. Notably, the optimized Mo1.5-Zn2In2S5 catalyst achieves exceptional H2 and benzaldehyde production rates of 34.35 and 45.31mmol gcat -1 h-1, respectively, outperforming pristine ZnIn2S4 by 3.83- and 4.15-fold. Our findings mark a significant stride in steering charge flow for enhanced photocatalytic performance. This article is protected by copyright. All rights reserved.

Non-precious Electrocatalysts for the Hydrogen Evolution Reaction

The development of non-precious metal-based catalysts for the hydrogen evolution reaction (HER) is a promising research area with the potential to advance water electrolysis and enable the widespread use of hydrogen as a clean energy source. While noble metals like Pt and Pd exhibit excellent HER activity, their limited availability and high cost present significant challenges. Non-precious transition metals such as Fe, Co, and Ni have emerged as alternative catalyst materials due to their natural abundance. However, these metals often encounter obstacles related to their hydrogen adsorption behavior. This commentary highlights the various strategies employed to optimize the electronic structures of non-precious metal-based catalysts to enhance the HER performance. The outlook of non-precious metal-based catalysts is bright, with ongoing and future research activities mainly focusing on improving their properties, integrating these catalysts into commercial water electrolysis systems, and improving the scalability for large-scale hydrogen production. The development of high-performance non-precious metal-based catalysts for HER is crucial to future sustainable and efficient hydrogen production in the transition from fossil fuels to clean energy.

Thermodynamic simulation of hydrogen production from the nano-CaO reactive sorption enhanced biomass steam reforming

Based on the principles of thermodynamic reaction equilibrium, a simulation method enhanced by the nano-CaO reactive sorption CO2 for hydrogen production from biomass steam reforming has been established. MATLAB R2022b software has been utilized to calculate the composition concentration of the product gas. Detailed simulations have been conducted to understand the changes in gas component concentration and yield under various reaction conditions, includes temperatures, steam to biomass (S/B) molar ratios, and CaO to carbon (CaO/C) molar ratios. The result demonstrated that temperature plays a significant role in both the concentration and yield of hydrogen. At an optimal reaction temperature of 650 °C, the concentration of H2 in the product reaches 77% (S/B = 2 and CaO/C = 0.5). S/B molar ratio over 2 is necessary to increase the H2 concentration. The study also reveals CaO/C molar ratio 0.5 enable successful removal of CO2 generated by reaction. The application of nano-CaO notably enhanced the efficiency of hydrogen production from biomass steam reforming, leading to a 25% increase in H2 concentration and a boost in H2 yield to 50 mL/gBiomass, and reaction temperature decrease 200 °C compared to the case without CaO.

Efficient hydrogen production and electricity generation in solar-driven single-photoelectrode photocatalytic fuel cell

Efficient hydrogen production and electricity generation in solar-driven single-photoelectrode photocatalytic fuel cell

Optimizing Renewable Energy Integration for Sustainable Fuel Production: A Techno-Economic Assessment of Dimethyl Ether Synthesis via a Hybrid Microgrid-Hydrogen System

This study offers an in-depth analysis and optimization of a microgrid system powered by renewable sources, designed for the efficient production of hydrogen and dimethyl ether—key elements in the transition toward sustainable fuel alternatives. The system architecture incorporates solar photovoltaic modules, advanced battery storage solutions, and electrolytic hydrogen production units, with a targeted reduction in greenhouse gas emissions and the enhancement of overall energy efficiency. A rigorous economic analysis was conducted utilizing the HYSYS V12 software platform and encompassing capital and operational expenditures alongside profit projections to evaluate the system’s economic viability. Furthermore, thermal optimization was achieved through heat integration strategies, employing a cascade analysis methodology and optimization via the General Algebraic Modeling System (GAMS), yielding an 83% decrease in annual utility expenditures. Comparative analysis revealed that the energy requirement of the optimized system was over 50% lower than that of traditional fossil fuel-based reforming processes. A comprehensive assessment of CO2 emissions demonstrated a significant reduction, with the integration of thermal management solutions facilitating a 99.24% decrease in emissions. The outcomes of this study provide critical insights into the engineering of sustainable, low-carbon energy systems, emphasizing the role of renewable energy technologies in advancing fuel science.

Innovations in Photocatalytic and Photoelectrocatalytic Water Splitting: Pathways to Efficiently Convert Biomass into Renewable Energy and Chemicals

AbstractThis review comprehensively explores the integration of photocatalytic (PC) and photoelectrocatalytic (PEC) technologies for hydrogen production via water splitting, in synergy with the efficient conversion of biomass resources. This synergistic strategy significantly boosts hydrogen production rates in both PC and PEC systems and enhances solar energy conversion efficiency. Furthermore, it enables selective conversion of cost‐effective biomass via precise modulation of catalyst structures, paving a novel pathway for green hydrogen generation and synthesis of high‐value chemicals. Specifically, the manuscript highlights recent progress in the oxidation and coupling reactions of biomass derivatives, such as methanol, ethanol, glycerol, and 5‐hydroxymethylfurfural, in PC/PEC systems. It reveals their potential to enhance hydrogen production efficiency and the synthesis of high‐value organic compounds. Future research should focus on employing in‐situ characterization techniques and theoretical simulations to deeply understand reaction mechanisms, thus advancing the field of biomass conversion through photocatalytic/photoelectrocatalytic methods.

METHANOL STEAM REFORMING FOR HYDROGEN PRODUCTION OVER Ni-BASED CATALYSTS: STATE-OF-THE-ART REVIEW AND FUTURE PROSPECTS.

With increasing global emphasis on environmental sustainability, the reliance on traditional energy sources such as coal, natural gas, and oil is encountering significant challenges. H2, known for its high energy content and pollution-free usage, emerges as a promising alternative. However, despite the great potential of H2, approximately 95% of hydrogen production still depends on non-renewable resources. Hence, the shift towards producing H2 from renewable sources, particularly through methods like steam reforming of methanol - a renewable resource - represents a beacon of hope for advancing sustainable energy practices. This review comprehensively examines recent advancements in efficient H2 production using Ni-based catalysts in methanol steam reforming (MSR) and proposes the future prospects. Firstly, the fundamental principles of MSR technology and the significance in clean energy generation are elucidated. Subsequently, the design, synthesis techniques, and optimization strategies for enhancing the catalytic performance of Ni-based catalysts are discussed. Through the analysis of various catalyst compositions, structural adjustments, surface active sites, and modification methods, the review uncovers effective approaches for boosting the activity and durability of MSR reactions.By offering a comprehensive critical analysis, this review serves as a valuable reference to enhance MSR hydrogen production efficiency and catalyst performance.

Two‐Dimensional Layered Hydroxide Materials for Nucleophile Oxidation

AbstractThe global energy crisis highlights the need to transition from fossil fuels to sustainable, renewable sources of energy. Green hydrogen produced via renewable energy‐driven water electrolysis is an emerging alternative due to its zero emissions and high energy density. To address the high energy consumption of water electrolysis, innovative hybrid electrolyzers integrating nucleophile oxidation reactions (NOR) are under activity investigation, reducing energy demands and enabling valuable product synthesis and waste treatment, thereby enhancing the efficiency and economic viability of hydrogen production via electrocatalytic technologies. Recent advancements in layered hydroxide materials (LHMs) have markedly improved the efficiency of alkaline electrochemical conversion processes and are gaining prominence in NORs due to their expansive surface areas and tailorable characteristics through diverse engineering strategies. Further, their layered architecture is readily conducive to in‐situ characterization, using techniques like XAS, XRD, Raman, and IR spectroscopy, providing insights into their anodic NOR mechanisms. This review summarizes the latest developments in LHMs as electrocatalysts for NOR, discusses current design strategies of LHMs, and emphasizes the significance of operando characterization techniques in elucidating the reaction mechanisms of different LHMs. Finally, the future challenges and potential advancements in their scale‐up application in electrocatalytic NOR are put forward.