Catalytic Reaction Research Articles

Activating the Mn Single Atomic Center for an Efficient Actual Active Site of the Oxygen Reduction Reaction by Spin-State Regulation.

The ligand engineering for single-atom catalysts (SACs) is considered a cutting-edge strategy to tailor their electrocatalytic activity. However, the fundamental reasons underlying the reaction mechanism and the contemplation for which the actual active site for the catalytic reaction depends on the pyrrolic and pyridinic N ligand structure remain to be fully understood. Herein, we first reveal the relationship between the oxygen reduction reaction (ORR) activity and the N ligand structure for the manganese (Mn) single atomic site by the precisely regulated pyrrolic and pyridinic N4 coordination environment. Experimental and theoretical analyses reveal that the long Mn-N distance in Mn-pyrrolic N4 enables a high spin state of the Mn center, which is beneficial to reduce the adsorption strength of oxygen intermediates by the high filling state in antibond orbitals, thereby activating the Mn single atomic site to achieve a half-wave potential of 0.896 V vs RHE with outstanding stability in acidic media. This work provides a new fundamental insight into understanding the ORR catalytic origin of Mn SACs and the rational design strategy of SACs for various electrocatalytic reactions.

Catalytic Biomaterials-Activated In Situ Chemical Reactions: Strategic Modulation and Enhanced Disease Treatment.

Chemical reactions underpin biological processes, and imbalances in critical biochemical pathways within organisms can lead to the onset of severe diseases. Within this context, the emerging field of "Nanocatalytic Medicine" leverages nanomaterials as catalysts to modulate fundamental chemical reactions specific to the microenvironments of diseases. This approach is designed to facilitate the targeted synthesis and localized accumulation of therapeutic agents, thus enhancing treatment efficacy and precision while simultaneously reducing systemic side effects. The effectiveness of these nanocatalytic strategies critically hinges on a profound understanding of chemical kinetics and the intricate interplay of reactions within particular pathological microenvironments to ensure targeted and effective catalytic actions. This review methodically explores in situ catalytic reactions and their associated biomaterials, emphasizing regulatory strategies that control therapeutic responses. Furthermore, the discussion encapsulates the crucial elements-reactants, catalysts, and reaction conditions/environments-necessary for optimizing the thermodynamics and kinetics of these reactions, while rigorously addressing both the biochemical and biophysical dimensions of the disease microenvironments to enhance therapeutic outcomes. It seeks to clarify the mechanisms underpinning catalytic biomaterials and evaluate their potential to revolutionize treatment strategies across various pathological conditions.

Monitoring C–C coupling in catalytic reactions via machine-learned infrared spectroscopy

Abstract Tracking atomic structural evolution along chemical transformation pathways is essential for optimizing chemical transitions and enhancing control. However, molecule-level knowledge of structural rearrangements during chemical processes remains a great challenge. Here, we couple infrared spectroscopy as a non-invasive method to probe molecular transformations, with a machine-learned protocol to immediately map the spectroscopic fingerprints to atomistic structures. From the theoretical perspective, we demonstrate it here with the example of C–C coupling in catalytic reactions, elucidating various structural conformations along dynamic trajectories. Within the transferable application to the specific CO–CO dimerization reaction, the structural and energetic variations of the critical chemical species could be identified via infrared spectroscopy. This approach extends the power of spectroscopy from fingerprinting chemical configurations to using them for assigning dynamic structural information.

Mn−Ce Symbiosis: Nanozymes with Multiple Active Sites Facilitate Scavenging of Reactive Oxygen Species (ROS) Based on Electron Transfer and Confinement Anchoring

AbstractRegulating appropriate valence states of metal active centers, such as Ce3+/Ce4+ and Mn3+/Mn2+, as well as surface vacancy defects, is crucial for enhancing the catalytic activity of cerium‐based and manganese‐based nanozymes. Drawing inspiration from the efficient substance exchange in rhizobia‐colonized root cells of legumes, we developed a symbiosis nanozyme system with rhizobia‐like CeOx nanoclusters robustly anchored onto root‐like Mn3O4 nanosupports (CeOx/Mn3O4). The process of “substance exchange” between Ce and Mn atoms—reminiscent of electron transfer—not only fine‐tunes the metal active sites to achieve optimal Ce3+/Ce4+ and Mn3+/Mn2+ ratios but also enhances the vacancy ratio through interface defect engineering. Additionally, the confinement anchoring of CeOx on Mn3O4 ensures efficient electron transfer in catalytic reactions. The final CeOx/Mn3O4 nanozyme demonstrates potent catalase‐like (CAT‐like) and superoxide dismutase‐like (SOD‐like) activities, excelling in both chemical settings and cellular environments with high reactive oxygen species (ROS) levels. This research not only unveils a novel material adept at effectively eliminating ROS but also presents an innovative approach for amplifying the efficacy of nanozymes.

Towards Photothermal Acid Catalysts Using Eco-Sustainable Sulfonated Carbon Nanoparticles—Part II: Thermal and Photothermal Catalysis of Biodiesel Synthesis

The main goal of this work is to evaluate the ability of sulfonated carbon nanoparticles (SCNs) to induce photothermal catalysis of the biodiesel synthesis reaction (transesterification of natural triglycerides (TGs) with alcohols). Carbon nanoparticles (CNs) are produced by the carbonization of cross-linked resin nanoparticles (RNs). The RNs are produced by condensation of a phenol (resorcinol or natural tannin) with formaldehyde under ammonia catalysis (Stober method). The method produces nanoparticles, which are carbonized into carbon nanoparticles (CNs). The illumination of CNs increases the temperature proportionally (linear) to the nanoparticle concentration and exposure time (with saturation). Solid acid catalysts are made by heating in concentrated sulfuric acid (SEAr sulfonation). The application of either light or a catalyst (SCNs) (at 25 °C) induced low conversions (<10%) for the esterification reaction of acetic acid with bioethanol. In contrast, the illumination of the reaction medium containing SCNs induced high conversions (>75%). In the case of biodiesel synthesis (transesterification of sunflower oil with bioethanol), conversions greater than 40% were observed only when light and the catalyst (SCNs) were applied simultaneously. Therefore, it is possible to use sulfonated carbon nanoparticles as photothermally activated catalysts for Fischer esterification and triglyceride transesterification (biodiesel synthesis).

A Cascade C(sp3)-H Annulation Involving C(alkyl),C(alkyl)-Palladacycle Intermediates.

C-H bond functionalization involving C,C-palladacycle intermediates provides a unique platform for developing novel reactions. However, the vast majority of studies have been limited to the transformations of C(aryl),C-palladacycles. In sharp contrast, catalytic reactions involving C(alkyl),C(alkyl)-palladacycles have rarely been reported. Herein, we disclose an unprecedented cascade C(sp3)-H annulation involving C(alkyl),C(alkyl)-palladacycles. In this protocol, alkene-tethered cycloalkenyl bromides undergo intramolecular Heck/C(sp3)-H activation to generate C(alkyl),C(alkyl)-palladacycles, which can be captured by α-bromoacrylic acids to afford tricyclic fused pyridinediones. In addition, this strategy can also be applied to indole-tethered cycloalkenyl bromides to construct pentacyclic fused pyridinediones via suquential Heck dearomatization/C(sp3)-H activation/decarboxylative cyclization. Notably, the removal of α-bromoacrylic acids in the reaction of alkene-tethered cycloalkenyl bromides can build an interesting tricyclic skeleton containing a four-membered ring. Preliminary mechanistic experiments indicate that five-membered C(alkyl),C(alkyl)-palladacycles serve as the key intermediates. Meanwhile, density functional theory (DFT) calculations have provided insights into the reaction pathway.

Supported phenylalanine on core-shell mesoporous microsphere as a catalyst for the synthesis of triazolo[1,2-a] indazole-triones and spiro triazolo[1,2-a] indazole-tetraones

In recent years, mesoporous silica materials have gained attention due to their unique properties, such as high surface area, pore volume, size, and chemical stability. These characteristics make them effective in various fields, particularly efficient supports in heterogeneous catalytic reactions. The present study developed a novel type of core-shell mesoporous microsphere material by anchoring phenylalanine on a core-shell SiO2@NiO@MS support. The catalyst support (SiO2@NiO@MS) was synthesized through homogeneous precipitation and sol-gel methods, with NiO encapsulated within the porous silica. The catalyst was characterized using various techniques, including Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Scanning electron microscopy (SEM), Energy dispersive spectroscopy (EDS), Elemental mapping analysis, N2 adsorption-desorption, Transmission electron microscopy (TEM), Vibrating sample magnetometer (VSM), and Thermogravimetric analysis (TGA). It was then employed for the synthesis of triazolo[1,2-a]indazole-trione and spiro triazolo[1,2-a]indazole-tetraones compounds from 4-phenyl urazole, dimedone, and aromatic aldehydes or isatin derivatives. This synthetic approach offers multiple advantages, including high yields, faster reaction times, low catalyst requirements, and environmentally sustainable conditions.

Carbon-coated ZnS as a high-performance ORR/OER bifunctional cathode catalyst for zinc-air batteries

The commercial application of zinc-air batteries (ZABs) is hindered by the high cost and scarcity of precious metal catalysts. In this paper, we prepared high-performance ORR/OER bifunctional catalysts with a carbon-coated ZnS spherical structure (ZnS@C) through a hydrothermal method followed by a carbonization process. Characterized by their unique spherical coated pore structure, exhibit impressive electrocatalytic activity. Specifically, ZnS@C-2, produced by a secondary carbonization process demonstrates an ORR half-wave potential of 0.82 V (relative to RHE) and an OER overpotential of 377 mV at 10 mA cm−2. When employed in a ZAB, it achieves a maximum power density of 120.4 mW cm−2, a specific capacity of 836 mAh gZn−1, and maintains cycle stabilization for up to 165 h at 10 mA cm−2. The research results demonstrate that the unique carbon-coated internal porous structure not only significantly enhances the stability of the catalyst but also increases the number of active sites, thereby providing more abundant activation energy for the catalytic reaction and facilitating its efficient progress. This underscores the catalyst's excellent ORR and OER properties, suggesting promising practical application potential.

Influence of Annealing Temperature on the OER Activity of NiO(111) Nanosheets Prepared via Microwave and Solvothermal Synthesis Approaches.

Earth-abundant transition metal oxides are promising alternatives to precious metal oxides as electrocatalysts for the oxygen evolution reaction (OER) and are intensively investigated for alkaline water electrolysis. OER electrocatalysis, like most other catalytic reactions, is surface-initiated, and the catalyst performance is fundamentally determined by the surface properties. Most transition metal oxide catalysts show OER activities that depend on the predominantly exposed crystal facets/surface structure. Therefore, the design of synthetic strategies to obtain the most active crystal facets is of significant research interest. In this work, rock salt NiO OER catalysts with (111) predominantly exposed facets were synthesized by a solvothermal (ST) method either heated under supercritical or microwave-assisted (MW) conditions. Particular emphasis was placed on the influence of the post annealing temperature on the structural configuration and OER activity to compare their catalytic performances. The as-prepared electrocatalysts are pure α-Ni hydroxides which were converted to rock salt NiO (111) nanosheets with hexagonal pores after heat treatment at different temperatures. The OER activity of the electrodes has been evaluated in 0.1 M KOH using geometric and intrinsic current densities via normalization by the disk area and BET area, respectively. The lowest overpotential at a geometric current density of 10 mA/cm2 is found for samples pretreated by heating between 400 and 500 °C with a catalyst loading of 115 μg/cm2. Despite the very similar nature of the catalysts obtained from the two methods, the ST electrodes show a higher geometric and intrinsic current density for 500 °C pretreatment. The MW electrodes, however, achieve an optimal geometric current density for 400 °C pretreatment, while their intrinsic current density requires pretreatment over 600 °C. Interestingly, pretreated electrodes show consistently higher OER activity as compared to the poorly crystalline/less ordered hydroxide as-prepared electrocatalysts. Thus, our study highlights the importance of the synthesis method and pretreatment at an optimal temperature.

Magnetic MgFeO@BC Derived from Rice Husk as Peroxymonosulfate Activator for Sulfamethoxazole Degradation: Performance and Reaction Mechanism.

Heterogeneous Mg-Fe oxide/biochar (MgFeO@BC) nanocomposites were synthesized by a co-precipitation method and used as biochar-based catalysts to activate peroxymonosulfate (PMS) for sulfamethoxazole (SMX) removal. The optimal conditions for SMX degradation were examined as follows: pH 7.0, MgFeO@BC of 0.4 g/L, PMS concentration of 0.6 mM and SMX concentration of 10.0 mg/L at 25 ℃. In the MgFeO@BC/PMS system, the removal efficiency of SMX was 99.0% in water within 40 min under optimal conditions. In the MgFeO@BC/PMS system, the removal efficiencies of tetracycline (TC), cephalexin (CEX), ciprofloxacin (CIP), 4-chloro-3-methyl phenol (CMP) and SMX within 40 min are 95.3%, 98.4%, 98.2%, 97.5% and 99.0%, respectively. The radical quenching experiments and electron spin resonance (ESR) analysis suggested that both non-radical pathway and radical pathway advanced SMX degradation. SMX was oxidized by sulfate radicals (SO4•-), hydroxyl radicals (•OH) and singlet oxygen (1O2), and SO4•- acted as the main active species. MgFeO@BC exhibits a higher current density, and therefore, a higher electron migration rate and redox capacity. Due to the large number of available binding sites on the surface of MgFeO@BC and the low amount of ion leaching during the catalytic reaction, the system has good anti-interference ability and stability. Finally, the intermediates of SMX were detected.

Machine learning-assisted screening of efficient ionic liquids for catalyzing CO2 cycloaddition reaction

The catalysis of CO2 cycloaddition reactions by ionic liquids holds significant promise in addressing environmental and chemical synthesis challenges. However, the design of effective ionic liquid catalysts is hindered by the sheer diversity of cation-anion combinations, leading to challenges in targeted catalyst development. This study addresses these issues by utilizing experimental data collected from literature on reactions involving epoxy compounds as substrates, conducted without solvents or co-catalysts, to establish a database for machine learning (ML). Simple descriptors derived from the ion pair structures of ionic liquids are employed as inputs for five ML classification algorithms to predict the yield of CO2 cycloaddition reactions. Subsequently, the highly accurate ML models are applied to forecast the catalytic performance of 1344 ionic liquids under ambient conditions. This approach identifies 13 cation structures and 8 anion structures that exhibit superior catalytic properties. Further refinement through density functional theory (DFT) calculations selects ion pair structures capable of catalyzing CO2 cycloaddition reactions at ambient temperature and pressure, demonstrating the efficacy of this method in guiding the design and development of ionic liquid catalysts for CO2 conversion reactions involving epoxy compounds.

Piezo-modulated interface field facilitating hydroxyl radical formation of SrTiO3/ZnO heterojunction for water purification

Piezo-modulated interface engineering is an effective method for tuning the charge transfer process to enhance piezocatalytic dynamics. In this study, SrTiO3/ZnO heterojunctions were successfully synthesized via hydrothermal methods to degrade carbamazepine in water. The optimal SrTiO3/ZnO-5 % sample exhibited a remarkable 99.9 % degradation efficiency of carbamazepine within 60 min under ultrasonic vibration. The piezocatalytic reaction rate (k value = 0.0746 min−1) was 4.63 times and 10.97 times higher than that of pure SrTiO3 and pure ZnO, respectively. Reactive species scavenger tests, electron paramagnetic resonance techniques, and bands gap analysis revealed that the enhanced activity can be attributed to the construction of an interfacial electric field in SrTiO3/ZnO heterojunctions and the modification of an internal piezoelectric polarized field. This allowed charge redistribution and transport across the SrTiO3/ZnO heterojunction interface, and facilitated the generation of hydroxyl radicals (HO•) through simultaneous hole oxidation and electron reduction. This study provides a comprehensive mechanistic understanding about piezoelectric heterojunctions in the catalytic redox reactions, and offers valuable insights for designing more effective piezoelectric heterojunctions for the degradation of pharmaceutical organic pollutants.

Heat transport regimes in structured reactors: CFD analysis and influence of reactor diameter and length

Temperature control in catalytic reactors is critical to ensure high yields and a stable process for highly exothermic reactions. To better understand the processes within structured reactors, it has already been shown that heat source based Computational Fluid Dynamics (CFD) is a simple and valid way to mimic the heat intake of catalytic surface reactions and to capture general heat transport properties. In case of structured reactors, the heat transport is highly dominated by thermal conduction. Building on these achievements, this work systematically investigates the influence of the reactor diameter and length on heat transfer and temperature distribution in a Periodic Open Cell Structure (POCS) reactor. It is found that the typically high percentage of thermal conductivity is reduced by up to 50% if the reactor diameter changes from 20 mm to 50 mm. Furthermore, heat transport regimes are introduced along the reactor axis separating reactor parts with different predominant heat transfer mechanisms. This provides a fundamental comprehension of heat transfer in structured reactors and highlights the necessity to consider a sufficient reactor length. Lastly, the influence of thermal radiation is isolated. In addition to lowering the temperature increase significantly (from 1,300 K to 500 K in a specific case), it can also enhance the heat conduction through the solid by increasing the solid's temperature close to the reactor wall. Although the heat source simulations are a simplification, they are ideal to understand the reactor systems from a heat transport perspective.

Pd(II)‐Catalyzed Asymmetric [2+2] Annulation for the Construction of Chiral Benzocyclobutenes

Asymmetric de novo synthesis of benzocyclobutenes (BCBs) via catalytic intermolecular reaction is highly desired for efficient access to this important class of compounds, yet such a strategy remains unmet challenge. Here, we report a Pd/Pyrox‐catalyzed asymmetric [2+2] annulation between arylboronic acids and functionalized alkenes, providing an unprecedented efficient protocol to access various enantio‐enriched BCBs in a modular and versatile manner under mild conditions. A broad substrate scope with excellent enantioselectivity has been achieved under the current protocol. The isolation and characterization of the key chiral palladacycle intermediate, together with DFT calculations, provides strong evidence for the catalytic pathway including an enantiodetermining arylpalladation step.

Photothermal catalytic oxidation performance of cerium-based perovskite catalyst CeBO3 under full-spectrum: Effect of B-site elements

In this paper, a series of cerium-based perovskite catalysts were prepared by sol-gel method combined with high-temperature calcination method, and Mn, Cr and Ni were selected as B-site elements, respectively, and characterized as well as tested for the catalytic activity of toluene oxidation. The CeMnO3 catalyst has the smallest grain size (4.33 nm), the largest specific surface area (39.65 m2/g) and the largest Oads/Olatt ratio (0.65). Based on its good low-temperature reduction performance, abundant adsorbed oxygen content, higher light absorption capacity and other characteristics, CeMnO3 exhibits outstanding photothermal catalytic oxidation of toluene under full-spectrum condition of 550 mW/cm2, and its photothermal catalytic T90% is only 233 °C. The photothermal catalytic oxidation reaction of CeMnO3 follows the Mars-van Krevelen mechanism. The introduction of light in thermal catalysis produces photothermal synergy, which has a better effect than single thermal catalysis and has a positive effect on the degradation of toluene.

Pd(II)-Catalyzed Asymmetric [2+2] Annulation for the Construction of Chiral Benzocyclobutenes.

Asymmetric de novo synthesis of benzocyclobutenes (BCBs) via catalytic intermolecular reaction is highly desired for efficient access to this important class of compounds, yet such a strategy remains unmet challenge. Here, we report a Pd/Pyrox-catalyzed asymmetric [2+2] annulation between arylboronic acids and functionalized alkenes, providing an unprecedented efficient protocol to access various enantio-enriched BCBs in a modular and versatile manner under mild conditions. A broad substrate scope with excellent enantioselectivity has been achieved under the current protocol. The isolation and characterization of the key chiral palladacycle intermediate, together with DFT calculations, provides strong evidence for the catalytic pathway including an enantiodetermining arylpalladation step.

Enhancing Compatibility of Two-Step Tandem Catalytic Nitrate Reduction to Ammonia Over P-Cu/Co(OH)2.

Electrochemical nitrate reduction reaction (NO3RR) is a promising approach to realize ammonia generation and wastewater treatment. However, the transformation from NO3 - to NH3 involves multiple proton-coupled electron transfer processes and by-products (NO2 -, H2, etc.), making high ammonia selectivity a challenge. Herein, a two-phase nanoflower P-Cu/Co(OH)2 electrocatalyst consisting of P-Cu clusters and P-Co(OH)2 nanosheets is designed to match the two-step tandem process (NO3 - to NO2 - and NO2 - to NH3) more compatible, avoiding excessive NO2 - accumulation and optimizing the whole tandem reaction. Focusing on the initial 2e- process, the inhibited *NO2 desorption on Cu sites in P-Cu gives rise to the more appropriate NO2 - released in electrolyte. Subsequently, P-Co(OH)2 exhibits a superior capacity for trapping and transforming the desorbed NO2 - during the latter 6e- process due to the thermodynamic advantage and contributions of active hydrogen. In 1m KOH + 0.1m NO3 -, P-Cu/Co(OH)2 leads to superior NH3 yield rate of 42.63mgh- 1cm- 2 and NH3 Faradaic efficiency of 97.04% at -0.4V versus the reversible hydrogen electrode. Such a well-matched two-step process achieves remarkable NH3 synthesis performance from the perspective of optimizing the tandem catalytic reaction, offering a novel guideline for the design of NO3RR electrocatalysts.

Cover Picture: Enhanced signal to noise ratio of single entity electrochemistry signal of platinum nanoparticles using passive silver ultramicroelectrode (BKCS 11/2024) Seongkyeong Yoon, Jaedo Na, Sun Gyu Moon, Heewon Kim, Ki Jun Kim, Seong Jung Kwon

The cover image depicts the Pt nanoparticles collision on an Ag ultramicroelectrode and the delicate oxide layer formed on the Ag electrode surface. When a single nanoparticle collides with the electrode surface, a current signal related to the catalytic reaction appears, and then the current returns to its original level due to the oxide layer of the electrode. More details are available in the article by Seong Jung Kwon, Seongkyeong Yoon, Jaedo Na, Sun Gyu Moon, Heewon Kim, and Ki Jun Kim. image

Neutrophil-Mimicking Nanozyme with Cascade Catalytic Releasing Nitric Oxide and Signet Oxygen Property for Synergistic Bimodal Therapy of Methicillin-Resistant Staphylococcus Aureus Infections.

Recently, chloroperoxidase (CPO)-mediated enzyme dynamic therapy (EDT) by mimicking the antipathogen function of neutrophils via generating highly active signet oxygen (1O2) has attracted great interest in biomedical applications. However, the therapeutic efficiency of EDT is largely restricted by the low CPO delivery efficiency and insufficient hydrogen peroxide (H2O2) supply. In the present work, a neutrophil-mimicking nanozyme of MGBC with high CPO delivery efficiency, H2O2 self-supply, and enzyme-cascade catalytic properties is designed for high-efficient treatment of methicillin-resistant Staphylococcus aureus (MRSA) infections. In the infection microenvironment, MGBC can effectively catalyze glucose to self-supply substantial H2O2, which enables long-lasting 1O2 generation via the CPO-mediated catalytic reaction. At the meantime, MGBC can also catalyze H2O2 to sustainably release NO for gas therapy (GT), which synergistically strengthens the therapeutic effect of EDT. As a result, MGBC displayed effective MRSA-killing and MSRA biofilms-eradicating properties, and high efficiency in treating both MRSA infected full-thickness excision wounds and subcutaneous MRSA infection by exerting the synergistic bimodal EDT/GT therapeutic effects. In-depth mechanism study revealed that the synergistic EDT/GT antibacterial effects of MGBC can attenuate the drug resistance and toxicity of MRSA by significantly downregulating quorum sensing, multidrug efflux, virulence, and biofilm formation-related genes.

The effect of different vulcanization reagents on the synthesis of NiFeS and the performance test of seawater electrolysis

Hydrogen energy, as the most promising new energy for sustainable development, has aroused wide concern of researcher in the field of energy chemical industry. Among the many hydrogen generation approaches, electric water splitting for producing H2 is considered to be a simple and environmentally friendly method. Transition metal-based catalysts have become an important field in alkaline seawater electrolysis due to their high abundance and superior catalytic performance. Therefore, NiFeS (Ni3S2@FeS) was in-situ generated on nickel foam through a simple two-step hydrothermal approach in this paper. NiFeS/NF catalysts synthesized by three vulcanization reagents (Na2S·9H2O, CH3CSNH2, CH4N2S) were characterized and compared by a series of electrochemical tests. It is worth noting that for the first time, different vulcanization reagents were used to explore the activity of the same catalyst in seawater splitting and urea splitting. It was found that the NiFeS catalyst synthesized by Na2S·9H2O (Ni3S2@FeS-1/NF) had better oxygen evolution reaction (OER) and hydrogen evolution reaction (HER) performance and good stability in alkaline seawater. The overpotential required for the OER with Ni3S2@FeS-1/NF electrode in alkaline seawater (1 M KOH + seawater electrolyte) is 290 mV at the 10 mA cm-2, and 92 mV for the hydrogen evolution reaction at the 10 mA cm-2. It is found that the NiFeS catalyst obtained by vulcanization of NiFe-LDH not only has high activity and conductivity, but also can effectively inhibit Cl- corrosion. Ni3S2@FeS-1/NF catalyst has a unique cluster rosette nanosheet array structure, which can present more catalytic reaction centres, accelerate the electron transfer rate and promote electrochemistry performance. The work proposes a novel way to explore the effect of different synthesis methods of the same composition on the performance of electrolytic seawater.