Simple Electrodeposition Research Articles

One-step electrodeposition synthesis of NiFePS on carbon cloth as self-supported electrodes for electrochemical overall water splitting

Electrocatalytic water splitting (EWS) for hydrogen production is considered an ideal strategy for utilizing renewable energy, reducing fossil fuel consumption, and addressing environmental pollution issues. Traditional noble metal electrocatalysts have excellent performance, but their cost is high. Developing efficient, stable, and relatively inexpensive dual functional electrocatalysts is crucial for promoting large-scale EWS hydrogen production processes. Herein, a simple one-step electrodeposition method was used to grow nickel–iron phosphorus-sulfides (NiFePS) on the surface of hydrophilic treated carbon cloth (CC). The resultant NiFePS/CC with a phosphorus to sulfur ratio of 1:4 exhibited the best electrocatalytic performance, requiring only −91 mV and 216 mV overpotentials to generate the current densities of 10 mA·cm−2 in hydrogen evolution reaction (HER) and oxygen evolution reaction (OER), respectively. When it was used as a bifunctional electrocatalyst to overall water splitting (OWS), a voltage of 1.536 V can generate a current density of 10 mA·cm−2. The excellent electrocatalytic performance can be ascribed to two factors: 1) the CC with excellent conductivity serves as a growth substrate, reducing the impedance of charge transfer from the electrode to the electrolyte and accelerating the electron transfer rate; 2) The large number of ultra-thin nanosheets formed on the surface of the catalyst increase the electrochemical specific surface area, expose more reaction sites, and thus improve the electrocatalytic reaction performance. This work provides a new approach for designing efficient non-noble metal electrocatalysts for water splitting.

Sn-doped cobalt–iron hydroxide nanoarrays for enhanced electrocatalytic oxygen evolution in oilfield wastewater systems

Developing efficient electrocatalysts suitable for oilfield wastewater is considered the most crucial aspect of advancing photoelectrochemical water splitting for hydrogen production in arid regions. In this work, Sn-doped cobalt iron hydroxide (SnCoFe-LDH/NF) with a nanoarray structure was successfully prepared in situ on nickel foam using a simple electrodeposition method. The catalyst exhibits high oxygen evolution reaction (OER) activity in 1.0 mol L−1 KOH, requiring only an overpotential of 239 mV to provide a current density of 10 mA cm−2, with a Tafel slope as low as 37.8 mV dec−1. More importantly, it also maintains excellent electrocatalytic activity in 1.0 mol L−1 KOH+oilfield wastewater. The enhancement of electrocatalysis performance can be attributed to the incorporation of Sn ions and layered structure of hydroxide, which increases the inherent activity of the materials, speeds up the kinetics, and improves the synergy between the hydroxides. This study proposes a simple and efficient strategy to prepare cheap and efficient electrocatalysts operating in complex water systems.

Industrial-Si-based photoanode for highly efficient and stable water splitting

Photoelectrochemical (PEC) water splitting is an effective and sustainable method for solar energy harvesting. However, the technology is still far away from practical application because of the high cost and low efficiency. Here, we report a low-cost, stable and high-performing industrial-Si-based photoanode (n-Indus-Si/Co-2mA-xs) that is fabricated by simple electrodeposition. Systematic characterizations such as scanning electron microscopy, X-ray photoelectron spectroscopy have been employed to characterize and understand the working mechanisms of this photoanode. The uniform and adherent dispersion of co-catalyst particles result in high built-in electric field, reduced charge transfer resistance, and abundant active sites. The core–shell structure of co-catalyst particles is formed after the activation process. The reconstructed morphology and modified chemical states of the surface co-catalyst particles improve the separation and transfer of charges, and the reaction kinetics for water oxidation greatly. Our work demonstrates that large-scale PEC water splitting can be achieved by engineering the industrial-Si-based photoelectrode, which shall guide the development of solar energy conversion in the industry.

Defects engineering of nickel tellurium electrocatalyst to boost urea oxidation reaction: Electrodeposition mechanism and performance

The urea oxidation reaction (UOR) offers an attractive strategy to replace the oxygen evolution reaction (OER) for energy-saving hydrogen production due to its favorable thermodynamic property, but its development is hindered by the lack of efficient and cost-effective electrocatalysts. In this study, nickel-tellurium (Ni-Te) grown on 3D nickel foam was successfully synthesized using a simple and facile electrodeposition method. The electrodeposition process of Ni-Te follows the three-dimensional instantaneous nucleation/growth mechanism controlled by diffusion. The apparent activation energy (Ea) of Ni-Te in the electrodeposition process is as low as 36.5 kJ∙mol-1. Lattice distortion structure obtained by electrodeposition modifies the intrinsic electronic structure and optimizes the adsorption energy of intermediates. Thanks to the synergistic effects of fast electron transport, superhydrophilic surface and nanoflake structure, the prepared Ni-Te electrocatalyst shows excellent activity toward UOR with a low potential of 1.503 V vs. RHE at 100 mA·cm-2 and a small Tafel slope (63.6 mV·dec-1) in 1.0 M KOH containing 0.33 M urea solution.

Experimental investigation on the electrodeposited nickel-based dichalcogenides for the efficient overall water splitting

Layered transition metal dichalcogenides are effective electrocatalysts for water splitting due to their unique properties such as high electrical conductivity, active site density, and catalytic properties. This study focused on the deposition of Ni-based dichalcogenides (NiX2, where X = S, Se, Te) onto a carbon cloth substrate using a simple one-step electrodeposition method at room temperature with different deposition times (10, 15, and 20 min). The optimized NiS2-15, NiSe2-15, and NiTe2-15 electrocatalysts showed excellent bifunctional electrocatalytic activity for both hydrogen evolution reaction and oxygen evolution reaction in alkaline media. The overpotential values for hydrogen evolution were ∼56 mV, ∼37 mV, and ∼75 mV for NiS2-15, NiSe2-15, and NiTe2-15, respectively, while the overpotential values for oxygen evolution were ∼220 mV, ∼170 mV, and ∼210 mV, respectively. The electrocatalysts maintained stability for 24 h during the evolution reactions. The density functional theory calculations suggested that NiSe2 had a lower ΔGH* value due to its smaller bandgap and inherent metallic characteristics, which is consistent with the experimental results. These findings provide a new direction for designing NiX2 (X = S, Se, Te) nanosheets for electrocatalysis applications.

Rational design of multi-component Fe(OH)3/Ni-NiO heterostructures bifunctional catalyst for electrochemical water splitting

Exploring economic-efficient bifunctional catalysts is critical for the production of green hydrogen through water splitting. Herein, we fabricate a novel hybrid catalyst with three-phase heterojunction (Fe(OH)3/Ni-NiO) via a simple electrodeposition and chemical precipitation method. Benefiting from the desirable amorphous-crystal interfaces, the electronic structure of Ni, NiO and Fe(OH)3 is regulated, which will optimize the adsorption of H intermediates (H*) and also reduce the kinetic barrier for the hydrogen evolution reaction (HER). The optimal Fe(OH)3–3/Ni-NiO/CC shows superior bifunctional activity with low overpotentials of 66 mV for HER and 220 mV for OER at 10 mA cm−2 in alkaline solution, respectively, as well as remarkable durability over a period of 40 h. Besides, Fe(OH)3–3/Ni-NiO/CC requires 1.52 and 1.72 V to deliver 10 and 100 mA cm−2 and shows no obvious increase in current within 40 h toward overall water splitting. Experimental and theoretical results show that the HER process is promoted by the synergistic effect of electronic redistribution between Ni, NiO and Fe(OH)3 due to the construction of three phase crystalline-amorphous heterogeneous interface. Meanwhile, Fe(OH)3 and NiO appeared reconstruction, transforming into FeOOH and NiOOH during OER process, respectively. This work offers a simple synthesis method for designing bifunctional catalysts for water splitting.

Effective photoabsorption and band-structural engineering in CuxO/NiO interfacial photosensor for improved ultraviolet response

Energy bands modulations in thin films heterostructure has offered exceptional leads towards the development of photosensing material. In this work, nanostructured metal oxides interfacial electrode structure has been employed to fabricate a highly sensitive ultraviolet (UV) sensor with high responsivity and detectivity. A unique, simple and cost-effective electrodeposition approach was adopted for the growth of the film samples. The interfacial structural effect and optical energy band modulations on the photo-electronic structure and UV detector performance of the structure have been examined. The films had fair transmissions of the visible light spectrum with CuxO dominance in the resulting bilayer structure and a high absorption peak in the ultraviolet (UV) region. The energy band gap redshifted towards the bilayer structure from 3.74 to 2.67 eV. Charge carriers trapping through surface recombination has been found to reduce from the assistance of ohmic contact formation of the heterostructure. The bilayer film-based photodetector demonstrated enhanced performance with photodetectivity (1.6⨯1011 Jones at 0.068 mWcm−2 power density), attributable to the existence of lower recombination state in the structure, according to the UV sensing study. The study showed that tailoring dissimilar metal oxide semiconducting films to the bilayer (CuxO/NiO) structure can provide excellent UV photodetector performance over single-layer of NiO and CuxO.

Stacked High‐Entropy Hydroxides Promote Charge Transfer Kinetics for Photoelectrochemical Water Splitting

AbstractAlthough various kinds of cocatalyst are developed and decorated on the bismuth vanadate (BiVO4) photoanode, its photoelectrochemical (PEC) water splitting performance is limited owing to severe charge recombination and sluggish oxygen evolution reaction (OER). Herein, a high‐entropy hydroxide electrocatalyst (FeCoNiMoCrOOH) is constructed as a co‐catalyst deposited on BiVO4 with a good PEC activity and stability in potassium borate buffer, addressing substantial charge recombination and poor surface oxygen evolution reaction of the material. FeCoNiMoCrOOH synthesized by a simple electrodeposition stacking strategy, delivers an overpotential of 172 mV at 10 mA cm−2 with a stability of 600 h under alkaline conditions, representing one of the best performances on high‐entropy‐based catalysts. The FeCoNiMoCrOOH/BiVO4 photoanode shows a photocurrent density of 5.23 mA cm−2 at 1.23 VRHE with 100 h durability in potassium borate buffer. Experimental investigations and theoretical calculations demonstrate that the synergistic effect of Mo and Cr in FeCoNi catalyst effectively decreases the dissolution Fe, Co, and Ni after long‐term operation, increases the charge transfer kinetics, and promotes OER and PEC performances, therefore enhancing the photocorrosion resistance of BiVO4. This work provides a new avenue to design high entropy‐based electrocatalysts boosting solar water splitting activity and stability.

Electrodeposited three-dimensional hierarchical architecture of MgO anchored with Ag nanoparticles for high-performance symmetric supercapacitors

A blossom-like, three-dimensional (3D) hierarchical architecture of MgO anchored with silver nanoparticles (Ag NPs) is developed using a simple galvanostatic electrodeposition method. This study shows how electrochemical performance is improved by the incorporation of Ag NPs within a 3D framework. The 3D blossom-like scaffold comprises thin 2D petals, whose porous lace-like patterns provide a large surface area and many channels for the rapid diffusion of electrolyte ions. The anchored Ag NPs increase the electrical conductivity of the MgO structure and enhance redox reactions. An optimum Ag loading of 10 vol% on MgO (MgO@Ag-10) affords a 100-fold enhancement in specific capacitance over that of MgO. This hybrid MgO@Ag-10 electrode on a stainless-steel substrate yields a specific capacitance of 388.6 F.g−1 (134.85 mF.cm−2) at a current density (CD) of 1 mA.cm−2, whereas pure MgO delivers only 3.72 F.g−1 (3.1 mF.cm−2) at the same CD in a three-electrode system. The MgO@Ag-10 electrode also exhibits 88.6 % capacitance retention over 5000 charge–discharge cycles. A symmetric supercapacitor device comprising two MgO@Ag-10 electrodes exhibits a specific capacitance of 42 F.g−1, an energy density of 23.33 Wh.kg−1, and a power density of 8000 W.kg−1 at 4 mA.cm−2 in aqueous KOH.

Electrodeposition of Fractal Structured Nickel for Hydrogen Evolution Reaction in Alkaline

AbstractTo accelerate the practical application of water splitting in alkaline media, it is imperative to enhance the electrocatalytic performance for the Hydrogen Evolution Reaction (HER). In this context, we demonstrate that a simple (one‐pot, one‐step) electrodeposition process of nickel (Ni) in the presence of 3,5‐diamino1,2,4‐triazole (DAT) results in the formation of fractally structured Ni films with a significantly increased surface area. The Electrochemically active surface area (ECSA) increases with the electrodeposition charge passed, with the film electrodeposited at 14 C cm−2 achieving a reduction in overpotential at −10 mA cm−2 (η10) to 65.7 mV, coupled with a remarkable increase in ECSA (114‐fold greater than that of Ni‐foil). Additionally, nickel deposited in the presence of DAT effectively mitigates deactivation during electrolysis, exhibiting a 3.6‐fold lower overpotential degradation compared to that of the smooth Ni foil. This simple electrodeposition technique, applicable to a variety of conductive substrates, is distinguished by its high catalytic performance in the HER, a feature of considerable significance.

Controlled synthesis of self-supportive hydrangea shaped Ni based hydroxide/phosphide for efficient overall water splitting and full pH hydrogen evolution

The exploration of efficient, robust and nonprecious transition metal electrocatalysts for electrochemical hydrolysis is urgently needed. Herein, we developed Ni(OH)2 with 3D nanoflower structure on the titanium mesh by a simple electrodeposition method. The Ni(OH)2/Ti exhibited excellent oxygen evolution reaction performance and achieved 10 mA cm−2 at 190 mV with fast kinetics in alkaline conditions. Ni2P, NiS2 and NiSe2 were prepared by solid-phase reaction, and the 3D nanoflower increased the open structure and greatly enhanced catalytic activity. The Ni2P/Ti electrode required an overpotential of 52, 88 and 109 mV to reach 10 mA cm−2 for hydrogen evolution reaction in acidic, alkaline and neutral media, respectively. The results of electrochemical measurements and mechanistic studies showed that the catalytic activity of HER: Ni2P > NiS2 > NiSe2 > Ni(OH)2. The Ni2P/Ti and Ni(OH)2/Ti electrodes were assembled into an integrated water splitting electrolytic cell. The water electrolysis device assembled with the Ni2P/Ti and Ni(OH)2/Ti electrodes only needed a low potential of 1.608 V to achieve 50 mA cm−2 in alkaline environment and was operated stably for 50 h.

ECL cytosensor for sensitive and label-free detection of circulating tumor cells based on hierarchical flower-like gold microstructures

The development of sensitive and efficient cell sensing strategies to detect circulating tumor cells (CTCs) in peripheral blood is crucial for the early diagnosis and prognostic assessment of cancer clinical treatment. Herein, an array of hierarchical flower-like gold microstructures (HFGMs) with anisotropic nanotips was synthesized by a simple electrodeposition method and used as a capture substrate to construct an ECL cytosensor based on the specific recognition of target cells by aptamers. The complex topography of the HFGMs array not only catalyzed the enhancement of ECL signals, but also induced the cells to generate more filopodia, improving the capture efficiency and shortening the capture time. The effect of topographic roughness on cell growth and adhesion propensity was also investigated, while the cell capture efficiency was proposed to be an important indicator affecting the accuracy of the ECL cytosensor. In addition, the capture of cells on the electrode surface increased the steric hindrance, which caused ECL signal changes in the Ru(bpy)32+ and TPrA system, realizing the quantitative detection of MCF-7 cells. The detection range of the sensor was from 102 to 106 cells mL−1 and the detection limit was 18 cells mL−1. The proposed detection method avoids the process of separation, labeling and counting, which has great potential for sensitive detection in clinical applications.

CoNiO2/Co3O4 Nanosheets on Boron Doped Diamond for Supercapacitor Electrodes.

Developing novel supercapacitor electrodes with high energy density and good cycle stability has aroused great interest. Herein, the vertically aligned CoNiO2/Co3O4 nanosheet arrays anchored on boron doped diamond (BDD) films are designed and fabricated by a simple one-step electrodeposition method. The CoNiO2/Co3O4/BDD electrode possesses a large specific capacitance (214 mF cm-2) and a long-term capacitance retention (85.9% after 10,000 cycles), which is attributed to the unique two-dimensional nanosheet architecture, high conductivity of CoNiO2/Co3O4 and the wide potential window of diamond. Nanosheet materials with an ultrathin thickness can decrease the diffusion length of ions, increase the contact area with electrolyte, as well as improve active material utilization, which leads to an enhanced electrochemical performance. Additionally, CoNiO2/Co3O4/BDD is fabricated as the positive electrode with activated carbon as the negative electrode, this assembled asymmetric supercapacitor exhibits an energy density of 7.5 W h kg-1 at a power density of 330.5 W kg-1 and capacity retention rate of 97.4% after 10,000 cycles in 6 M KOH. This work would provide insights into the design of advanced electrode materials for high-performance supercapacitors.

Communication—Texture and Bandgap Tuning of Phase Pure Cu2O Thin Films Grown by a Simple Potentiostatic Electrodeposition Technique

Highly textured phase pure Cu2O thin films have been grown by a simple electrodeposition technique with varying deposition voltages (−0.3 to −1.0 V). The surface morphology characterized by Scanning Electron Microscopy (SEM) revealed that the deposited thin films coherently carpet the underlying substrate and are composed of sharp faceted well-defined grains of 0.5–1.0 μm sizes. XRD analyses showed that all films are composed of polycrystalline cubic Cu2O phase only and have average crystalline domain size in the range of 30–73 nm. The preferred crystalline orientation of phase pure Cu2O films was found to be changing from (200) to (111) with increasing cathodic voltages and showed the highest (111) and (200) crystalline texture coefficient while growing at −1.0 and −0.8 V respectively. The optical bandgap of the as-grown samples was calculated in the range of 1.95–2.20 eV using UV–vis Transmission data. The performance of Cu2O/FTO photocathodes was tested by estimating LED “ON/OFF” modulated surface photovoltage into a photoelectrochemical cell at a zero bias.

Investigating the Role of Embedded ZnO Seed Layer Thickness in Electrodeposited Cu2O/Zn(x)Mg(1−x)O/ZnO/FTO Heterojunctions for Photovoltaic Applications

This article represents the construction of Cu2O/Zn(x)Mg(1−x)O/ZnO/FTO heterojunctions by employing a simple electrodeposition approach. The impact of inserting ZnO seed layers with different thicknesses on the various physicochemical properties of the electrodeposited films is explored by applying various techniques. The electrochemical characterization specifies high photoresponses achieving 335.42 μA cm−2 for seeded Cu2O/Zn(x)Mg(1−x)O heterojunctions by increasing the thickness of seeded ZnO layer from 25 to 100 nm. The scanning electron microscopy and atomic force microscopy techniques indicate that the surface texture and smoothness of Cu2O/ZnO heterojunctions have significantly enhanced after increasing the thickness of the ZnO layers. The synthesized ZnO nanostructures are found to be highly crystalline in nature having ZnO with hexagonal phase oriented along (002) direction and Cu2O with cubic structure oriented along (111) direction. This study shows the introduction of ZnO seed layers, enhances the I–V characteristics of Au/Cu2O/Zn(x)Mg(1−x)O/ZnO/FTO solar cells. The ideality factor shows a decreasing tendency from 5.35 to 3.93 while the photoelectric response is increased from 427% to 643% with the increase of the ZnO thickness from 25 to 100 nm, respectively, demonstrating the effectiveness of the seed layers approach.

Built-in electric field and selenium vacancies synergistically enhance NiSe2@Co0.85Se high-performance supercapacitors

Sluggish kinetics and poor cycling stability are two major obstacles limiting large-scale energy storage in battery-type supercapacitors. Herein, a novel strategy has been proposed to address these issues, which is to use a simple two-step electrodeposition technology to prepare the NiSe2@Co0.85Se/NF(denoted as NS@CS/NF) core-shell heterostructure, generate built-in electric field, and subsequently introduced anionic vacancies to successfully construct unique Se vacancies-rich composites (denoted as Sev-NS@CS/NF). Systematic characterisation analysis and density functional theory (DFT) calculations confirm that Se vacancies and heterogeneous interfaces can modulate electronic structure and promote fast reaction kinetics to achieve excellent supercapacitor performance, with a specific capacitance of 1530 C g−1 at 1 A g−1, and a capacity retention of 86.35% even after undergoing 10,000 charge-discharge cycles. Furthermore, a hybrid supercapacitor (HSC) was constructed using Sev-NS@CS/NF as the cathode and activated carbon (AC) as the anode, exhibiting an energy density of 80 Wh kg−1 at 812 W kg−1 and maintained impressive performance metrics. Notably, when two HSC units were connected in series, they successfully illuminated an LED diode for a duration of 15 min, showcasing the considerable potential of this HSC device for various energy storage applications.

Three-dimensional heterostructured MnNiCoP/FeOOH cross-linked nano-flake supported by Ni Foam as a bifunctional electrocatalysts for overall water splitting

The production of three-dimensional heterogeneous structures is a vital approach for the creation of high-performance bifunctional electrocatalysts. Herein, three-dimensional heterostructure MnNiCoP/FeOOH (MNC-P/FeOOH) supported by Ni foam was prepared by simple electrodeposition and phosphorylation as a bifunctional electrocatalyst. The results showed that the required overpotential for MNC-P/FeOOH catalyst to reach 100 mA cm−2 current density was 124 mV and 251 mV in 1.0 M KOH solution, respectively. Construction of heterojunction not only improves the OER performance of MnNiCoP, but also reduces the potential required to drive the integral water splitting at 100 mA cm−2 current density. The electrocatalytic activity of MNC-P/FeOOH is greatly increased due to a distinctive interface synergy and strong electronic contacts in the MNC-P/FeOOH heterojunction. This design approach of bifunctional transition metal phosphides provides a potential route to achieve total water splitting.

Controlled doping of ultralow amounts Ru on Ni cathode for PEMWE: Experimental and theoretical elucidation of enhanced performance

Proton exchange membrane water electrolysis (PEMWE) is an environmentally benign technology for large-scale hydrogen production. Despite many catalysts being developed to replace Pt, successful development of low-cost catalysts that meet the balance of performance and durability is limited. In this work, atomically dispersed Ru on Ni catalyst-integrated porous transport electrodes were fabricated by a simple electrodeposition. With a trace amount of Ru (< 0.05 mgRu·cm−2), the Ni98.1Ru1.9 cathode catalyst exhibited an overpotential of 35 mV at –10 mA·cm−2 with excellent stability. Density functional theory calculation revealed that the high performance was driven by optimized adsorption strength and improved mobility of hydrogen on the catalyst surface. The Ni98.1Ru1.9 electrode was further verified in a PEMWE cell and resulting performance (6.0 A·cm−2 at 2.25 Vcell) and stability (0.13 mV·h−1 decay rate at 1 A·cm−2) surpassed previously reported non-Pt and even Pt electrodes, demonstrating its readiness as an advanced cathode to replace Pt.

Controllable process to construct robust superhydrophobic membrane with tunable pore size for efficient separation of oil-water mixtures and emulsions

The increase in the discharge of industrial oily wastewater poses a threat to the environment and human health. Thus, the treatment of oily wastewater has become a focus of current research. The superhydrophobic surface derived from the lotus effect provides an effective direction for oil-water separation. Based on this, the authors reported a tunable superhydrophobic stainless steel separation mesh with a water contact angle of 155° through simple electrodeposition and modification with a fluorine-free modifier. The separation mesh with different surface morphology, by controlling different electrodeposition time and current, is able to achieve oil-water separation with super flux up to 51561 L/(m2·h) in heavy oil/water mixture and high-efficiency over 99.5% in water-in-oil emulsion. This controllable process constructs superhydrophobic membrane with tunable pore size, which is capable of separating heavy oil/water mixtures and water-in-oil emulsions depending on the process. This proposal is suggestive in the field of oil-water separation.

Spinel-covered interlayer MgO enhances the performance of BiVO4 photocatalytic ammonia synthesis

In order to respond to the call for low emissions and low energy consumption, photoelectrochemical (PEC) ammonia synthesis is used to replace the Haber-Bosch method of nitrogen reduction, and highly efficient photoelectrocatalysts were used to reduce the reaction energy barrier. In this paper, the interlayer MgO and base BiVO4 were successfully compounded by a simple electrodeposition method, and the spinel MCo2O4 (M=Zn, Mn) was compounded on MgO/BiVO4 by a hydrothermal method, forming a sandwich structure of MCo2O4/MgO/BiVO4 (M=Zn, Mn). The research shows that the sandwich structure constructed by MgO as the intermediate layer can reduce the excessive surface defects of photocatalyst, effectively reduce the recombination of photogenerated charge, promote the directional migration and separation of photogenerated charge, and improve the photocurrent density and photoelectric conversion efficiency. MCo2O4 (M=Zn, Mn) is a nitrogen reduction cocatalyst, which forms a heterojunction with n-type BiVO4 and inhibits the recombination of photogenerated electrons. The synergistic effect of MCo2O4(M=Zn, Mn) and MgO accelerates the surface charge transfer efficiency and enhances the photoelectricity ammonia synthesis efficiency. The PEC ammonia synthesis efficiency reached more than 30 µmol h−1 g−1cat, and the Faradaic efficiency(FE) is over 30%.