Gel combustion synthesized NiMoO4 anchored polymer nanocomposites as a flexible electrode material for solid state asymmetric supercapacitors

Recent research has focused on the search for new electrode materials to improve the specific capacitance of supercapacitors. Conductive polymers and metal oxides have been extensively tested as electrode materials for supercapacitors. Incorporating both conductive polymers and metal oxides into a composite provides excellent results for the electrochemical performance of supercapacitors. In this present work, we have fabricated the nanoscale α-NiMoO₄ particles that enwrapped on electronically conducting polymer nanocomposites (PNCs) based on Polyvinyl alcohol (PVA)/Poly(vinyl) pyrrolidone (PVP) for supercapacitor applications. The different concentrations of PVA/PVP with α-NiMoO₄ loaded polymer nanocomposites were developed by using a solution casting method. All the polymer nanocomposites have been subjected to Scanning Electron Microscopy (SEM), Fourier Transforms Infrared (FTIR), X-ray diffraction (XRD), and electrochemical studies. The prepared PNCs surface morphology has been acquired as a non-uniform rod-like structure. The electrochemical performances of the prepared PNCs have been investigated and the resultant value of the maximum specific capacitance is 15.56 F g⁻¹ for 1 wt % of α-NiMoO₄ nanoparticles(NPs) loaded polymer blended electrode at a scan rate of 5 mVs⁻¹. The prepared PNCs exhibit 97.12% of columbic efficiency studied by using two electrode systems at room temperature in an aqueous electrolyte solution of 3 M KOH. From these investigation, it has been revealed that the PVA/PVP/α-NiMoO₄ composites could be portable and flexible electrodes for energy storage applications.     

Ni3Mo3N coupled with nitrogen-rich carbon microspheres as an efficient hydrogen evolution reaction catalyst and electrochemical sensor for H2O2 detection

Hydrogen evolution reaction (HER) and electrochemical analysis are two important fields of electrochemical research at present. We found that both HER and some electrochemical analytical reactions relied on the concentration of hydrogen ions (H⁺) in solution, so we intended to develop an electrode material that is sensitive to H⁺ and can be used for both HER and some electrochemical analyses. In this work, we synthesized Ni₃Mo₃N coupled with nitrogen-rich carbon microspheres (Ni₃Mo₃N@NC MSs) as highly efficient electrode material for HER and detection of Hydrogen peroxide (H₂O₂), which plays an important role in physiological processes. Here the aniline was used as the nitrogen and carbon sources to synthesize Ni₃Mo₃N@NC. The Ni₃Mo₃N@NC MSs showed high performance for HER in 1 M KOH solution with a small overpotential of 51 mV at 10 mA cm^?2 and superior stability. For H₂O₂ detection, a detection limit of 1 μM (S/N = 3), sensitivity of 120.3 μA·mM^?1 cm^?2 and linear range of 5 μM–40 mM can be achieved, respectively. This work will open up a low-cost and easy avenue to synthesize transition metal nitrides coupled with N-doped carbon as bifunctional electrode material for HER and electrochemical detection.     

Insight into effects of graphene and zinc oxide in Li4Ti5O12 as anode materials for Li-ion full-cell battery

Programmable design of nanocomposites of Li₄Ti₅O₁₂ (LTO) conducted through hydrothermal route in the presence of ethylenediamine as basic and capping agent. In this work, effect of ZnO and Graphene on the Li₄Ti₅O₁₂ based nanocomposites as anode materials investigated for Li-Ion battery performances. The full cells battery assembled with LTO based nanocomposites on Cu foil as the anode electrode and commercial LMO (LiMn₂O₄) on aluminum foil as cathode electrode. X-Ray diffraction (XRD), Energy-dispersive X-ray spectroscopy (EDS), Fourier-transform infrared spectroscopy (FT-IR), along with Field Emission Scanning Electron Microscopy (FE-SEM) and Transmission electron microscopy (TEM) images was applied for study the composition and structure of as-prepared samples. The electrochemical lithium storage capacity of prepared nanocomposites was compared with pristine LTO via chronopotentiometry charge-discharge techniques at 1.5–4.0 V and current rate of 100 mA/g. As a result, the electrode which is provided by LTO/TiO₂/ZnO and LTO/TiO₂/graphene nanocomposites provided 765 and 670 mAh/g discharge capacity compared with pristine LTO/TiO₂ (550 mAh/g) after 15 cycles. Based on the obtained results, fabricated nanocomposites can be promising compounds to improve the electrochemical performance of lithium storage.     

In-situ “encapsulation” of Mo:Mo2C with nano-mosaic structure on wood-derived carbon for hydrogen evolution reaction

Coupling metallic and Mo₂C phases uniformly on conductive matrix at nanoscale is a promising route to solve the poor electrical conductivity and aggregation problems of nano-Mo₂C. In this work, a 3D self-supporting carbonized wood (CW) electrode encapsulation with mosaic structure Mo:Mo₂C for hydrogen evolution reaction was fabricated successfully by a facile annealing treatment and a gas-solid reaction. The presence of Mo phase accelerated the transfer rate of electrons and provided heterogeneous interface. The obtained electrode shows abundant catalytic active sites and low electrochemical impedance, thus improving the catalytic process of splitting water for HER. The Mo:Mo₂C-775 electrode requires an overpotential of 73.5 mV and 117 mV to achieve the current density of 10 mA cm^?2 in 0.5 M H₂SO₄ and 1.0 M KOH, respectively. Moreover, Mo:Mo₂C-775 electrode displayed excellent stability performance, which almost maintained a constant current density for 12 h (at ?100 mV vs RHE) in 0.5 M H₂SO₄ and 1.0 M KOH, respectively. This study provides a new idea for preparation of efficient 3D self-supporting electro-catalyst for HER.     

Improved energy conversion and storage performance enabled by hierarchical zigzag-like P-doped CuCo2O4 nanosheets based 3D electrode materials

Developing a bi-functional material which can meet both electrochemical water splitting and supercapacitors (SCs) is a hot spot in current research. In this study, hierarchical zigzag-like phosphorus doped CuCo₂O₄ nanosheets based 3D electrode materials were successfully synthesized via a hydrothermal method and followed by thermal treatment. Since the unique morphology of 2D nanosheets with zigzag-like edges could provide more reactive sites, which is not only conducive to the hydrogen evolution reaction (HER), but also conducive to the electrochemical energy storage. Meanwhile, the doping of phosphorus was adopted to improve the conductivity, which would further enhance the electrochemical properties of CuCo₂O₄. Thereafter, its performance for HER and SCs in 1 M KOH were systematically investigated. As an electrode for HER, it only required a low overpotential of 152 mV to reach 10 mA cm^?2 with a Tafel slope of 115.7 mV dec^?1. Furthermore, I-t test result showed an excellent stability. As an electrode for SCs, it exhibited a high specific capacity of 896.9C g^?1 at 1 A g^?1 in three-electrode system. All in all, the obtained hierarchical zigzag-like phosphorus doped CuCo₂O₄ nanosheets provided a feasible route for the design of bi-functional electrode materials both for energy conversion and storage.     

Self-standing Co decorated Cu2O/CuS-based porous electrocatalyst for effective hydrogen evolution reaction in basic media

The self-standing Co decorated Cu₂O/CuS-based porous electrocatalyst was prepared with the help of simple electrodeposition and hydrothermal method. The structural characterizations of fabricated samples were performed with X-Ray diffraction spectroscopy and X-Ray photoelectron spectroscopy, while the morphology of catalysts was studied with the help of Field-Emission Spectroscopy and Transmission Electron Spectroscopy. The electrochemical performance of the hydrogen evolution reaction was checked in a basic electrolyte. The gradual increment in the electrochemical performance of Cu₂O was observed when it underwent sulfurization without and with Co precursor respectively. The best electrochemical performance for hydrogen evolution reaction with an overpotential of 150.29 mV to achieve a geometric current density of 10 mA/cm² was observed for the Cu₂O sample sulfurized with Co precursor. The results of different characterizations suggested that the improved electrochemical performance could be attributed to the increased intrinsic activity and surface porosity of the electrocatalyst after sulfurization.     

Size and strain dependent activity of Ni nano and micro particles for hydrogen evolution reaction

In the context of constant research for the improvement of alkaline water electrolysis process using advanced electrocatalytic materials for the hydrogen evolution reaction (HER), various nickel particle based electrode materials were prepared and characterized. The synthesis of nickel hydroxide nanoparticles was performed in water in presence of three different stabilizers (CTAB, PVP and KBr). A thermal treatment at 400 °C under 5% H₂/Ar atmosphere led to nickel nanoparticles. Mechanically milled commercial micrometric particles and nanoparticles synthesised by a polyol route completed a series of Ni powders showing broad ranges of size (5 nm–73 μm) and strain (6 ppm–0.7%). The electrocatalytic activity of the resulting electrode materials was evaluated versus powder morphology. Their apparent and intrinsic activity and the mechanism of the HER were studied by electrochemical impedance spectroscopy (EIS) and steady-state polarisation. A change in the HER mechanism is observed depending on particle size. This first systematic study demonstrates that the smaller the size and the more defective the particles, the greater the electrocatalytic activity. As a matter of fact, appreciable cathodic current densities of 100 mA cm⁻² at ∼ −300 mV of overpotential were obtained for nickel nanoparticles with 5 nm size and 0.7% strain.     

On the thermodynamic stability of La2Mo2O9−δ oxide-ion conductor

The stability of La₂Mo₂O_9−δ oxide-ion conductor was studied under Ar–H₂ and controlled oxygen partial pressure (pO₂) atmospheres within the range 608 ≤ T ≤ 1000 °C, by thermogravimetry (TG), X-ray Diffraction (XRD), Temperature Controlled X-ray Diffraction (TCXRD) and Scanning Electron Microscopy (SEM).     

Surface controlled synthesis of Cu2FeSnS4 particles for enhanced hydrogen evolution reaction

Cu₂FeSnS₄ (CFTS) particles are synthesized using different surfactants such as thioglycolic acid (TGA), polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA) via the solution process. The effect of surfactants on crystal structure, morphology, elemental composition, and electrocatalytic properties of CFTS particles are investigated. CFTS particles with a better crystalline phase are obtained in PVP (surfactant), while impurity phases are observed in TGA and PVA (surfactants). The morphology of CFTS is significantly changed when a different surfactant is used in the synthesis process. The mixture of aggregate and porous (1 μm) particles is observed when PVA is used as a surfactant to synthesize CFTS particles. At the same time, highly porous particles having nanosheets and nanoparticles at the surface are obtained in the case of PVP. In the TGA case, spherical particles with 1 μm size are observed. The electrocatalytic ability of all CFTS particles toward hydrogen evolution reactions (HER) is studied in 0.5 M H₂SO₄ electrolyte. The overpotential of PVP-based CFTS particles is the lowest as ƞ = 421 mV at 10 mA/cm² compared to the other two samples. CFTS particles synthesized using PVP exhibit enhanced electro-catalytic performance due to higher surface area.     

Electrochemical performance of La2Cu1−xCoxO4 cathode materials for intermediate-temperature SOFCs

K₂NiF₄-type structure oxides La₂Cu_1−xCo_xO₄ (x = 0.1, 0.2, 0.3) are synthesized and evaluated as cathode materials for intermediate temperature solid oxide fuel cells (IT-SOFCs). The materials are characterized by XRD, SEM and electrochemical impedance spectrum (EIS), respectively. The results show that no reaction occurs between La₂Cu_1−xCo_xO₄ electrode and Ce_0.9Gd_0.1O_1.95 (CGO) electrolyte at 1000 °C. The electrode forms good contact with the electrolyte after sintering at 800 °C for 4 h in air. The electrode properties of La₂Cu_1−xCo_xO₄ are studied under various temperatures and oxygen partial pressures. The optimum composition of La₂Cu_0.8Co_0.2O₄ results in 0.51 Ω cm² polarization resistance (R_p) at 700 °C in air. The rate limiting step for oxygen reduction reaction (ORR) is the charge transfer process. La₂Cu_0.8Co_0.2O₄ cathode exhibits the lowest overpotential of about 50 mV at a current density of 48 mA cm⁻² at 700 °C in air.     

Ni doped Bi2WO6 for electrochemical OER activity

Due to over depletion of fossil fuels, researchers started to find hydrogen energy to compete with the energy demands. Bi₂WO₆ and Ni (5% and 10%) doped Bi₂WO₆ were prepared via hydrothermal route. Structural confirmation of undoped and doped Bi₂WO₆ nanostructures was estimated by using standard characterization studies. The nanoflake and nanoneedle like morphology of undoped and Ni doped Bi₂WO₆ was confirmed in nanoscale range. The highest OER activity was achieved for 10% Ni doped Bi₂WO₆ nanostructure electrode with the excellent current density of 272 mA/g with overpotential of 242 mV in the fabricated three electrode half cell set up. The higher electron transport offered by Ni ions to Bi₂WO₆ host has been reported with the electrochemical mechanism. Hence, the unusual robust electrodes for electrochemical potential applications by tuning its property via suitable foreign ion dopant could be the great beginning of this recent year research. In such a way, this work would be the better way of swapping of nobel metal catalysts for electrochemical OER activity.     

Fe-Mo-R (R = rare earth metal) crystalline alloys as a cathode material for hydrogen evolution reaction in alkaline solution

Ternary Fe-Mo-R (R = Rare Earth metal) crystalline alloys, Fe₇₅Mo₂₀Gd₅, Fe₇₅Mo₂₀Dy₅, Fe₇₅Mo₂₀Er₅ and Fe₇₅Mo₂₀MM₅ (MM = mischmetal: 50.2% Ce, 26.3% La, 17.5% Nd, 6.0% Pr, atomic %) have been characterized by means of microstructural and electrochemical techniques in view of their possible applications as electrocatalytic materials for hydrogen evolution reaction (HER). The microstructure of the alloys was examined by scanning electron microscopy coupled with electron probe microanalysis; XRD measurements were also performed. The electrochemical efficiency of the electrodes has been studied on the basis of electrochemical data obtained from steady-state polarization and electrochemical impedance spectroscopy (EIS) techniques in 1 M NaOH solution at 298 K. The results were compared with those obtained on a binary Fe-Mo commercial alloy (Fe₈₀Mo₂₀, atomic %). Moreover, literature data concerning the electrocatalytic activity of the Ni₇₅Mo₂₅ and Co₇₅Mo₂₅ crystalline alloys, which are considered good electrocatalyst materials for the HER, were also reported for comparison. The microstructural features play a fundamental role in determining the electrocatalytic activity of the investigated alloys. The overall experimental data indicate that interesting electrocatalytic performances are displayed by the Fe₇₅Mo₂₀MM₅ electrode, which exhibits the highest activity towards the HER.     

Monometallic,bimetallic, and trimetallic chalcogenide-based electrodes for electrocatalytic hydrogen evolution reaction

Cu₂CoSnS₄, Cu₂SnS₃, Cu₂CoS₄, Co₂SnS₃, Cu₂S, CoS₂, and SnS₂ were synthesized using a one-step solvent-free solid-phase approach. The surface structure, morphology, and composition were characterized using an X-ray diffractometer (XRD), Fourier-Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), and X-ray Photoelectron Spectroscopy (XPS). The characterizations reveal pure phase formation and porous morphology. Further, the Hydrogen evolution reaction was performed using Cu₂CoSnS₄, Cu₂SnS₃, Cu₂CoS₄, Co₂SnS₃, Cu₂S, CoS₂, and SnS₂-based electrodes. Amid all electrocatalysts, Cu₂CoSnS₄ shows an excellent hydrogen evolution reaction with a low overpotential of ?192.1 mV at ?10 mA/cm² in 0.5 M H₂SO₄. And higher current density. Cu₂CoSnS₄ also shows a lower Tafel slope of 98.6 mV/dec and charge transfer resistance than mono and bimetallic chalcogenide-based electrodes. The Cu₂CoSnS₄ exhibit very good stability for ～22 h at ?10 mA/cm² current density in 0.5 M H₂SO₄.     

High-efficiency Co6W6C catalyst with three-dimensional ginger-like morphology for promoting the hydrogen and oxygen evolution reactions

Development of electrocatalysts composed of low cost and abundant elements that exhibit catalytic activity comparable to noble metals is important for water splitting. As such, in this study, a catalyst material with a ginger-like morphology consisting of Co₆W₆C is synthesized via a hydrothermal reaction and pyrolysis treatment. The Co₆W₆C catalyst exhibits satisfactory electrochemical properties towards both hydrogen and oxygen evolution reactions in an alkaline electrolyte, with a low overpotential, low Tafel slope, and durable stability. Co₆W₆C possesses a high activity for the hydrogen evolution reaction in alkaline conditions, with an onset potential and overpotential of −0.024 V and 101 mV, respectively, and low Tafel slope of 80.5 mV dec⁻¹ at a current density of 10 mA cm⁻². In addition, Co₆W₆C achieves a current density of 10 mA cm⁻² for the oxygen evolution reaction at an overpotential of only 343 mV. Furthermore, electrochemical stability tests indicate that the Co₆W₆C catalyst maintains 91% of the original current after 60,000 s for the hydrogen evolution reaction and 95% of the original current after 45,000 s for the oxygen evolution reaction. Moreover, electrochemical splitting of water via a two-electrode system employing this catalyst can hold 89% of the initial current after 40,000 s in 1 M KOH.     

Exploration of carbon additives to the synthesis of Cu2Mo6S8 structures and their electrocatalytic activity in oxygen reduction reaction

Catalytic processes are contemplated as break point in generating alternative and sustainable energy platforms. The cathodic oxygen reduction reaction (ORR) is an important catalytic system, mainly finding practice in fuel cell and metal-air battery technologies. This work presents the synthesis, structural characterization and electrocatalytic properties of three different Cu₂Mo₆S₈ structures as alternative ORR electrocatalysts. The effect of different carbon additives during synthesis was studied and no positive influence of the carbon addition was indicated. Our findings show that only the bare Cu₂Mo₆S₈ enhances the ORR electro-performance to class with the state-of-the-art ORR catalysts. Excellent stability of 10,000 consecutive ORR cycles, a superior onset potential of 0.894 V and half-wave (E_1/2) potential of 0.641 V vs. reversible hydrogen electrode (RHE) increase the noteworthiness of the Cu₂Mo₆S₈ electrodes. Aside from experimental investigations, density functional theory calculations deliver profound knowledge on the structural and electronic properties (electronic band structure, partial density of states and electron density) of Cu₂Mo₆S₈.     

Highly stable La0.5Sr0.5Fe0.9Mo0.1O3-δ electrode for reversible symmetric solid oxide cells

Reversible solid oxide cells (RSOCs) using identical material as both fuel electrode and air electrode have received extensive attentions due to their simplified fabrication process, increased compatibility between electrolyte and electrode. In this work, Molybdenum doped La_0.5Sr_0.5Fe_0.9Mo_0.1O_3-δ (LSFMo) symmetric electrode based on RSOCs is firstly designed and synthesized via sol-gel method. The effect of Molybdenum substitution at Fe-site on crystal structure, chemical stability, conductivity and electrochemical performance of La_0.5Sr_0.5FeO_3-δ oxide is thoroughly investigated. The structural stability of La_0.5Sr_0.5FeO_3-δ (LSF) in reducing condition is significantly enhanced after the incorporation of Mo^5+/6+ and the conductivity in 5% H₂ for LSFMo is ~7 times higher than that of undoped LSF. In addition, the polarization resistance value at 850 °C based on LSFMo/LSGM/LSFMo is 0.08 and 0.09 Ω cm² in air and wet H₂, respectively. At 850 °C and 20%H₂O–H₂, a peak power density of 640 mW cm⁻² is obtained in fuel cell mode, while a current density of −1000 mA cm⁻² is attained at 1.3 V in electrolysis mode. Finally, the symmetric cell exhibits an excellent cycling reversible operation in both SOFCs mode and SOECs mode without detectable degradation.     

Facile process to utilize carbonaceous waste as a carbon source for the synthesis of low cost electrocatalyst for hydrogen production

Low cost non-noble metal electrocatalysts are highly desirable for the sustainable production of hydrogen as a renewable energy source. Molybdenum carbide (Mo₂C) has been considered as the promising non-noble metal electrocatalyst for the hydrogen production via hydrogen evolution reaction (HER) through water splitting. The nanostructured nitrogen (N) incorporated carbon (C) coupled with Mo₂C is the potential candidate to boost the HER activity and electrode material for the energy conversion applications. In this work, nitrogen incorporated carbon coated Mo₂C (Mo₂C@C/N) has been synthesized in an eco-friendly way using waste plastic as the carbon source. The pure phase Mo₂C@C/N has been synthesized at 700 and 800 °C for 10 h. The relatively higher temperature synthesized phase shows enhanced HER activity with lower Tafel slope (72.9 mVdec⁻¹) and overpotential of 186.6 mV to drive current density of 10 mAcm⁻². It also exhibits stability up to 2000 cyclic voltammetry (CV) cycles and retains the current density with negligible loss for 10 h. The higher temperature synthesized phase exhibits higher electrochemical active surface area (ECSA) and enhanced HER kinetics.     

Electrochemical performance of Sr1.9La0.1Fe1.5Mo0.5O6-δ symmetric electrode for solid oxide fuel cells with carbon-based fuels

La-doped Sr_2-xLa_xFe_1.5Mo_0.5O_6-δ perovskite oxides are synthesized and used as a symmetric electrode to evaluate the effect of La on the crystal structure, conductivity, and catalytic activity for O₂ reduction and H₂ oxidation reaction. The electronic doping effect dominates the oversize effect in Sr_2-xLa_xFe_1.5Mo_0.5O_6-δ oxide, resulting in unit cell volume expansion and decreased conductivity in air. In addition, the introduction of La increases the chemical structural stability of Sr₂Fe_1.5Mo_0.5O_6-δ in reducing condition due to the higher La–O bond compared with Sr–O bond, leading to high catalytic activity for the H₂ oxidation reaction. At 800 °C, the R_p values of Sr_1.9La_0.1Fe_1.5Mo_0.5O_6-δ symmetric cell in air and wet H₂ are as low as 0.075 and 0.21 Ω cm², respectively. Moreover, the peak power densities of 769, 561, 439, and 653 mW cm^?2 at 850 °C are obtained when wet H₂, CO, CH_4, and C₃H₈ are used as fuels on Sr_1.9La_0.1Fe_1.5Mo_0.5O_6-δ/LSGM/Sr_1.9La_0.1Fe_1.5Mo_0.5O_6-δ cell. The symmetric cell also shows excellent stability (>100 h) in wet H₂/air, implying Sr_1.9La_0.1Fe_1.5Mo_0.5O_6-δ oxide is a promising symmetric electrode material.     

Catalytic characteristics of CexCu1-xO1.9 catalysts formed by solid state method for MTS and OMTS reactions

Ce_xCu_1-xO_1.9 (x = 0.3, 0.5, 0.8 and 0.9) catalysts were synthesized by solid state method, using ball mill apparatus, and evaluated in medium temperature shift (MTS), as well as oxygen assisted MTS (OMTS) reactions at temperature range of 300–390 °C. Catalysts were characterized by X-Ray Diffraction (XRD), Temperature Programmed Reduction (TPR), Scanning Electron Microscopy (SEM), and N₂ adsorption-desorption (BET) analysis. Ce_0.9Cu_0.1O_1.9 sample showed the best catalytic activity and structural properties. Decrease in proportion of Cu to Ce, leads to increase in the Cu-Ce mixed oxide formation (according to TPR analysis), significant increase in BET surface area (from 18 m²/g for Ce_0.3Cu_0.7O_1.9–48 m²/g for Ce_0.9Cu_0.1O_1.9), and decrease in CuO crystalline size (XRD). Moreover, the effect of oxygen addition to the feed (O₂/CO ratio = 0, 0.3, 0.5, 0.7 and 1), on the catalytic performance was evaluated. CO conversion was increased by enhancing the amount of oxygen (from 60% to 80% at 360 °C). CO and H₂ oxidations are occurring as competitive parallel reactions in which CO oxidation is dominant at low O₂/CO ratios (<0.5) and H₂ oxidation (undesirable for MTS reaction) at high O₂/CO ratios (>0.5). Furthermore, molar ratios of steam to CO at ranges of 2–4 were compared in OMTS reaction. According to the obtained results, the magnitudes of O₂/CO ratio and S/C ratio which were 0.5 and 4, respectively, were selected as the best values for OMTS reaction.     

Preparation of NiCo2O4 microspheres employing hydrothermal approach

In this study, nickel cobalt oxide (NiCo₂O₄) microspheres were prepared by using facile hydrothermal route. The structural confirmation of bimetal oxide formation was acquired by X-ray powder diffraction and Raman studies. The formation of microspheres combined via irregular nanosheets was confirmed by scanning electron microscopy. Highly oriented NiCo₂O₄ microspheres yielded a high current density (258 mA/g) at 10 mV/s and low overpotential (224 V). The highly active electrode showed efficient electron transportation towards oxygen evolution reaction. Long-term stability over 16 h was achieved by the fabricated high-performance NiCo₂O₄ electrode. It is recommended that NiCo₂O₄ microspheres obtained from 3:1 stoichiometry ratio of Ni and Co would lead to new electrocatalysts that give best performance than expensive catalysts used currently in the water oxidation process.