Directly growth of highly uniform MnS–MoS2 on carbon cloth for advanced H2 evolution electrocatalyst in different pH electrolytes

The activation energy barrier of the H–O bond of water molecules is high, and thus the rate of H₂ evolution reaction (HER) via water splitting is very slow. Hence, chemists are committed to finding high-performance, cheap and stable catalysts for realizing efficient H₂ production. The molybdenum disulfide (MoS₂)-based bimetallic sulfide electrocatalysts are favored by researchers because of their particular structures and properties. Herein, the Waugh type polyoxometalate (POM) is used as raw materials. A series of MnS–MoS₂ electrocatalysts are in-situ coupled on carbon cloth (CC) substrate by a hydrothermal sulfidation method. The catalyst MnS-MoS₂-CC possesses high catalytic activity for HER in a alkaline electrolyte, showing a low overpotential of 54 mV at a current density of 10 mA cm^?2, which is very close to 35 mV of the 20% Pt/C electrode. Meanwhile, under a current density of over 50 mA cm^?2, the overpotential of MnS-MoS₂-CC is less than that of the 20% Pt/C electrode. Moreover, the electrocatalysts show overpotentials of 141 mV and 201 mV at a current density of 10 mA cm^?2 in 0.5 M H₂SO₄ and 1.0 M phosphate buffer solution (PBS), respectively. Besides the high catalytic activity, the MnS-MoS₂-CC electrode shows long-term durability in a wide pH range, which is confirmed by several methods including the tests of linear sweep voltammetry (LSV) curve, current density vs. time (I-t) curve, and scanning electron microscopy (SEM). This work provides a feasible route for the preparation of HER electrocatalysts applied in broad pH conditions, especially for alkaline solutions.     

Open and porous NiS2 nanowrinkles grown on non-stoichiometric MoOx nanorods for high-performance alkaline water electrolysis and supercapacitor

Hierarchical hybrid heterostructures are regarded to be promising materials for highly efficient bifunctional electrocatalysts and high-performance supercapacitors due to their intriguing morphological features and remarkable electrochemical properties. Herein, we demonstrate the rational construct of cost-effective MoO_x@NiS₂ hybrid nanostructures as bifunctional electrocatalysts and the electrode material of supercapacitor. Microstructural analysis shows that the hybrid is a kind of hierarchical heterostructure composed of open and porous NiS₂ nanowrinkles in situ grown on non-stoichiometric MoO_x nanorods, which greatly improves the conductivity, and effectively maximized the electrochemical surface area. As expected, the MoO_x@NiS₂ hybrid show remarkable electrocatalytic performance in alkaline media, such as overpotentials of 101 mV at 10 mA cm^?2 for hydrogen evolution reaction (HER) and 278 mV at 20 mA cm^?2 for oxygen evolution reaction (OER), and a low cell voltage of 1.62 V to deliver a current density of 10 mA cm^?2. Moreover, the hybrid nanostructures present a high specific capacitance 1050 A/g at 1 A/g with ultra-long stability in 6 M KOH. The strategy proposed here introduces a new perspective about the development of efficient earth-abundant bifunctional elecrocatalysts and electrode materials for superior energy conversion and storage devices.     

Metal-organic frameworks derived self-supported Ni2P nanorod arrays for electrocatalytic hydrogen evolution

The development of efficient and low-cost electrocatalysts for hydrogen evolution reaction (HER) is of importance. Herein, we demonstrate a self-supported Ni₂P nanostructure with nanorod arrays morphology, fabricated by directly growing metal-organic frameworks (MOFs) on the commercial nickel foam prior to phosphorization treatment, as an electrocatalyst for HER. This electrocatalyst exhibits remarkable electrocatalytic HER activity in an alkaline electrolyte, affording current densities of 10 and 100 mA cm^?2 at the overpotentials of 120 and 168 mV, respectively, accompanied with a low Tafel slope of 37 mV dec^?1. Furthermore, this electrocatalyst shows a current density of 105 mA cm^?2, and this current density can be retained for more than 20 h, suggesting its superior stability. This remarkable HER performance is believed a result of superiority for its structural integrality and mechanical stability.     

Well-dispersed Pt nanodots interfaced with Ni(OH)2 on anodized nickel foam for efficient hydrogen evolution reaction

Hindered by price and scarcity, the exploitation of supported Pt-based electrocatalysts with Pt single atoms or Pt nanoclusters is an alternative way to decrease the dosage of Pt and improve the electrocatalytic performance for hydrogen evolution reaction (HER) of water splitting. The anodization technology is used to modify the surface of nickel foam (NF) to form the porous NiF₂ network structure. Then Pt nanodots interfaced with Ni(OH)₂ (Pt/Ni(OH)₂) hybrid on the anodized NF has been in-situ synthesized by a simple hydrothermal decomposition method. Results show that Pt nanodots on the substrate have good dispersion with the average size of 3 nm, and the Pt loading is only 0.229 mg cm⁻². The prepared electrode exhibits the low overpotentials of 25.9 mV and 211 mV at the current densities of 10 and 100 mA cm⁻², respectively, a small Tafel slope of 37.6 mV dec⁻¹, and the excellent durability for HER. The porous network nanostructure of Pt/Ni(OH)₂ hybrid, the large electrochemical surface area, the fast facilitated electron transport capability, and the firm adhesion of Pt nanodots with the anodized NF substrate contribute to the remarkable performance towards HER.     

Ni(OH)2/ NiSe2 hybrid nanosheet arrays for enhanced alkaline hydrogen evolution reaction

Developing efficient, non-noble electrocatalysts toward hydrogen evolution reaction (HER) in alkaline electrolytes is of important significance for future energy supplement but still a challenge. Recently, pyrite-type NiSe₂ nanomaterial has been considered as an idea HER electrocatalyst due to its high conductivity, strong corrosion resistance and low cost. However, the HER performance of NiSe₂ in alkaline electrolytes is still unsatisfactory, which is possibly limited to the activate water dissociation in alkaline media. Herein, a novel hybrid electrocatalyst of Ni(OH)₂/NiSe₂ nanosheet arrays on carbon cloth (Ni(OH)₂/NiSe₂/CC) is fabricated, exhibiting excellent HER catalytic activity with a low overpotential of 82 mV to drive a current density of 10 mAcm⁻² as well as maintaining a long-term durability for 12 h in 1.0 M KOH, which is 77 mV less than that of NiSe₂/CC and superior to most recently reported non-noble HER electrocatalysts. In addition, the Tafel slope of Ni(OH)₂/NiSe₂/CC (60 mV dec ⁻¹) is also much smaller than that of NiSe₂/CC (112 mV dec ⁻¹), suggesting a promotion kinetics of HER process for Ni(OH)₂/NiSe₂/CC. Our further experimental results show that the significantly improved activity of Ni(OH)₂/NiSe₂/CC electrode should ascribe to its enlarged active surface, good conductivity and interfacial synergy between Ni(OH)₂ and NiSe₂. The synergetic strategy may provide an efficient way to promote the HER activity of other non-noble transition metal selenides in alkaline electrolyte.     

Interfacing perovskite strontium molybdate to molybdenum disulfide nanoplatelts for boosting HER from water

Due to low hydrogen adsorption free energy at the edges of 2D-MoS₂ layered sheets, nanostructured MoS₂ materials recently are assigned to prospective electrocatalysts for hydrogen evolution reaction (HER) from water. However, the efficiency and stability of HER onto the MoS₂ designed on the conductive substrates are poor. To significantly increase the number of active sites and achieve a long-time working stability, the design of hybrid-type electrodes is crucial. Here, we report the synthesis of a new hybrid material composed of molybdenum disulfide and molybdenum oxides heterostructured with strontium molybdate. For this, a facile one-pot hydrothermal process was developed directly onto the TiO₂ nanotube carpet substrate. The interfacing of strontium molybdate at the electrode substrate verified by X-ray photoelectron spectroscopy and Time of flight secondary ions mass spectrometry (ToF SIMS) techniques. Considerable higher catalytic activity at the surface of this hybrid film, with the onset potential of 190 mV vs RHE and a Tafel slope of 66 mV dec^?1 attaining ~80 mA cm^?2 at 0.35 V overvoltage was ascertained. Exciting HER stability in comparison with the pure synthetic MoS₂ was verified by a prolonged potential cycling from 0.05 to ?0.35 V versus RHE potential and 45 h continuous HER processing at a constant current density.     

Hydrothermal preparation of MoX2 (X = S,Se, Te)/TaS2 hybrid materials on carbon cloth as efficient electrocatalyst for hydrogen evolution reaction

The prominent features-based two-dimensional (2D) materials have proven themselves as efficient as well as robust electrocatalysts for the hydrogen evolution reaction (HER) owing to their low-cost, abundance and predominant conductivity. In this work, we report the synthesis of series of molybdenum chalcogenide nanostructures MoX₂ (X = S, Se, Te), hybridized with TaS₂ nanosheets, via a facile hydrothermal method, on self-supported carbon cloth electrode. Used as an electrocatalyst for HER, hybrid phase MoSe₂/TaS₂/CC electrode with a Mo/Se ratio of 1:1.5 exhibits the best HER performance, which could afford the benchmark current densities of 10 mA/cm² at the overpotentials of 75 mV with the measured Tafel slope values of 54.7 mV/dec. In addition, the presented molybdenum dichalcogenides in this work are also complimented with robustness as determined from durability and air stability measurements. The unique aspects of these unique hybrids, such as 1T and 2H phases hybridized MoS₂ and MoSe₂, semimetallic nature 1T′-MoTe₂ petal clusters and strong interface interaction between MoX₂ (X = S, Se, Te) and conductive TaS₂ nanosheets, cause superior HER catalytic performance.     

Superhydrophilic 3D peony flower-like Mo-doped Ni2S3@NiFe LDH heterostructure electrocatalyst for accelerating water splitting

Constructing highly efficient nonprecious electrocatalysts for oxygen evolution reaction (OER) and hydrogen evolution reaction (HER) is essential to improve the efficiency of overall water splitting, but still remains lots of obstacles. Herein, a novel 3D peony flower-like electrocatalyst was synthesized by employing Mo–Ni₂S₃/NF nanorod arrays as scaffolds to in situ growth ultrathin NiFe LDH nanosheets (Mo-Ni₂S₃@NiFe LDH). As expected, the novel peony flower-like Mo–Ni₂S₃@NiFe LDH displays superior electrocatalytic activity and stability for both OER and HER in alkaline media. Low overpotentials of only 228 mV and 109 mV are required to achieve the current densities of 50 mA cm^?2 and 10 mA cm^?2 for OER and HER, respectively. Additionally, the material remarkably accelerates water splitting with a low voltage of 1.54 V at 10 mA cm^?2, which outperforms most transition metal electrodes. The outstanding electrocatalytic activity benefits from the following these features: 3D peony flower-like structure with rough surface provides more accessible active sites; superhydrophilic surfaces lead to the tight affinity between electrode with electrolyte; metallic Ni substrate and highly conductive Mo–Ni₂S₃ nanorods scaffold together with offer fast electron transfer; the nanorod arrays and porous Ni foam accelerate gas bubble release and ions transmission; the strong interfacial effect between Mo-doped Ni₃S₂ and NiFe LDH shortens transport pathway, which are benefit for electrocatalytic performance enhancement. This work paves a new avenue for construction and fabrication the 3D porous structure to boost the intrinsic catalytic activities for energy conversion and storage applications.     

Nanostructure and stoichiometry tailoring of CoS2 for high performance hydrogen evolution reaction

Developing efficient and low-cost electrocatalysts for hydrogen evolution reaction (HER) is important for hydrogen fuel production. In this study, we synthesized two different types of CoS₂ under low sulfur (LS) and high sulfur concentration (HS) conditions. Structural analysis results show that CoS impurity phase forms easily when the concentration of sulfur is low, while at high sulfur concentration the growth of CoS impurity phase is inhibited and leads to phase-pure CoS₂. Electrochemical investigation of HER performance reveals that the onset potential of CoS₂ (HS) electrode (ca. − 0.11 V vs. the reversible hydrogen electrode, RHE) is 30 mV anodic of the CoS₂ (LS) one (ca. − 0.14 V vs. RHE). At a specific current density of 10 mA cm⁻² the required overpotential on CoS₂ (HS) electrode is only 163 mV, which is 40 mV less than the CoS₂ (LS) electrode. Electrochemical impedance spectroscopy (EIS) data further demonstrate that the charge transfer rate of CoS₂ (HS) electrode is faster than that of CoS₂ (LS) electrode towards HER.     

Maize-like CoP nanorod arrays as an efficient and robust electrocatalyst for superior hydrogen generation

High-performance, low-cost and robust electrocatalysts for the hydrogen evolution reaction (HER) play a critical role in large-scale hydrogen production via water splitting. Herein, we proposed a synthesis strategy for the self-assembly of maize-like CoP nanorod arrays with abundant active sites via a combination of conventional hydrothermal reaction and low-temperature phosphorization. This unique architecture exhibited remarkable catalytic performance for the HER, with a low overpotential of 130 mV at a current density of 10 mA cm^?2 and a small Tafel slope of 59 mV dec^?1 in 1.0 M KOH electrolyte, as well as good stability as verified by chronoamperometry measurement for 10 h. Density functional theory calculations further revealed that these maize-like CoP nanorod arrays with dense active sites and a high phosphorization degree could boost the HER performance in terms of low adsorption energy and free energy. This work provided a facile strategy towards manipulating morphology engineering to enhance the HER activity of CoP-based catalysts.     

Ni activated Mo2C nanoparticles supported on stereotaxically-constructed graphene for efficient overall water splitting

Exploring cost-effective, high-efficiency and stable electrocatalysts for overall water splitting is greatly desirable and challenging for sustainable energy. Herein, a novel designed Ni activated molybdenum carbide nanoparticle loaded on stereotaxically-constructed graphene (SCG) using two steps facile strategy (hydrothermal and carbonization) as a bifunctional electrocatalyst for overall water splitting. The optimized Ni/Mo₂C(1:20)-SCG composites exhibit excellent performance with a low overpotential of 150 mV and 330 mV for hydrogen evolution reaction (HER) and oxygen evolution reaction (OER), respectively to obtain a current density of 10 mA cm^?2 in 1.0 M KOH solution. In addition, when the optimized Ni/Mo₂C(1:20)-SCG composite is used as a bifunctional electrode for overall water splitting, the electrochemical cell required a low cell voltage of 1.68 V at a current density of 10 mA cm^?2 and long-term stability of 24 h. More significantly, the synergetic effects between Ni-activated Mo₂C nanoparticles and SCG are regarded as a significant contributor to accelerate charge transfer and promote electrocatalytic performance in hybrid electrocatalysts. Our works introduce a novel approach to design advanced bifunctional electrodes for overall water splitting.     

Hexagonal CoSe2 nanosheets stabilized by nitrogen-doped reduced graphene oxide for efficient hydrogen evolution reaction

CoSe₂ is considered as a promising candidate among non-noble metal electrocatalysts for the hydrogen evolution reaction (HER) due to its intrinsic metallicity and low Gibbs free energy for hydrogen adsorption. Recently, the hexagonal CoSe₂ becoming increasingly popular owing to its chemically favorable basal plane, which provides more active sites, but remains limited by the poor stability. In this study, we design a small-molecule-amine-assisted hydrothermal method to in situ anchor the hexagonal CoSe₂ nanosheets (NSs) on nitrogen-doped reduced graphene oxides (RGO) as an advanced electrode material for HER. Due to the existence of abundant functional groups and high specific surface area of RGO, the hexagonal CoSe₂ NSs could be stably formed on RGO. As a result, only a small overpotential of 172 mV is needed for the optimized sample to drive a current density of 10 mA cm⁻² in 0.5 M H₂SO₄ and the Tafel slope is 35.2 mV dec⁻¹, which is comparable with the state-of-the-art Pt catalyst (32.3 mV dec⁻¹). Therefore, the facile and low-cost method for synthesizing hexagonal TMDs with robust electrical and chemical coupling developed in this work is promising in promoting the large-scale application of non-precious electrocatalysts.     

Facile construction of porous and heterostructured molybdenum nitride/carbide nanobelt arrays for large current hydrogen evolution reaction

The development of cost-effective, highly efficient and stable electrocatalysts for alkaline water electrolysis at a large current density has attracted considerable attention. Herein, we reported a one-dimensional (1D) porous Mo₂C/Mo₂N heterostructured electrocatalyst on carbon cloth as robust electrode for large current hydrogen evolution reaction (HER). The MoO₃ nanobelt arrays and urea were used as the metal and non-metal sources to fabricate the electrocatalyst by one-step thermal reaction. Due to the in-situ formed abundant high active interfaces and porous structure, the Mo₂C/Mo₂N electrocatalyst shows enhanced HER activity and kinetics, as exemplified by low overpotentials of 54, 73, and 96 mV at a current density of 10 mA cm^?2 and small Tafel slopes of 48, 59 and 60 mV dec^?1 in alkaline, neutral and acid media, respectively. Furthermore, the optimal Mo₂C/Mo₂N catalyst only requires a low overpotential of 290 mV to reach a large current density of 500 mA cm^?2 in alkaline media, which is superior to commercial Pt/C catalyst (368 mV) and better than those of recently reported Mo-based electrocatalysts. This work paves a facile strategy to construct highly efficient and low-cost electrocatalyst for water splitting, which could be extended to fabricate other heterostructured electrocatalyst for electrocatalysis and energy conversion.     

Three-dimensional Ni2P–MoP2 mesoporous nanorods array as self-standing electrocatalyst for highly efficient hydrogen evolution

Electrochemical hydrogen evolution reaction (HER) via the splitting of water has required electrocatalysts with cost-effectiveness, environmentally friendliness, high catalytic activity, and superior stability to meet the hydrogen economy in future. In this context, we report the successful synthesis of self-standing mesoporous Ni₂P–MoP₂ nanorod arrays on nickel foam (Ni₂P–MoP₂ NRs/3D-NF) through an effective phosphidization of the corresponding NiMoO₄ NRs/3D-NF. The as-synthesis Ni₂P–MoP₂ NRs/3D-NF, as an efficient HER electrocatalyst, exhibits small overpotential of 82.2 and 124.7 mV to reach current density of 10 and 50 mA cm⁻², a low Tafel slope of 52.9 mV dec⁻¹ and it retains its catalytic performance for at least 20 h in alkaline condition. Our work also offers a new strategy in designing and using transition metal phosphide-based 3D nanoarrays catalysts with enhanced catalytic efficiency for mass production of hydrogen fuels.     

Aqueous substitution synthesis of platinum modified amorphous nickel hydroxide on nickel foam composite electrode for efficient and stable hydrogen evolution

Exploring highly active and stable electrocatalysts toward hydrogen evolution reaction (HER) is vital for the production of green energy and storage of intermittently renewable electrical energy. In this study, we fabricate Pt-modified Ni(OH)₂ on 3D nickel foam (Pt content: 1.5 wt %) via a one-step galvanic replacement reaction in aqueous solution to achieve a top performance of HER under alkaline conditions. It exhibits a negligible onset potential, a Tafel slope of 17 mV dec⁻¹, and overpotentials of 38, 114, and 203 mV to deliver 10, 50, and 100 mA cm⁻² current densities, respectively, which outperforms the commercial Pt/C and Pt sheet. Moreover, this catalyst shows enhanced durability towards HER, sustaining electrolysis at −20 mA cm⁻² for 4, 500 min in 1 M KOH with little degradation. Its good performances come from the synergism of flake-like Pt and amorphous Ni(OH)₂. This work provides not only a facile and easy scale-up approach to fabricate Pt−modified electrocatalysts with improved HER performance but also a new strategy to design self-supported high-performance hybrid materials of noble-metal and amorphous transitional metal hydroxides for sustainable energy conversion and storage.     

Ultrathin MoS2 nanosheets in situ grown on rich defective Ni0.96S as heterojunction bifunctional electrocatalysts for alkaline water electrolysis

Developing earth-abundant and highly active bifunctional electrocatalysts are critical to advance sustainable hydrogen production via alkaline water electrolysis but still challenging. Herein, heterojunction hybrid of ultrathin molybdenum disulfide (MoS₂) nanosheets and non-stoichiometric nickel sulfide (Ni_0.96S) is in situ prepared via a facile one-step hydrothermal strategy, followed by annealing at 400 °C for 1 h. Microstructural analysis shows that the hybrid is composed of intimate heterojunction interfaces between Ni_0.96S and MoS₂ with exposed active edges provided by ultrathin MoS₂ nanosheets and rich defects provided by non-stoichiometric Ni_0.96S nanocrystals. As expected, it is evaluated as bifunctional electrocatalysts to produce both hydrogen and oxygen via water electrolysis with a hydrogen evolution reaction (HER) overpotential of 104 mV at 10 mA cm⁻² and an oxygen evolution reaction (OER) overpotential of 266 mV at 20 mA cm⁻² under alkaline conditions, outperforming most current noble-metal-free electrocatalysts. This work provides a simple strategy toward the rational design of novel heterojunction electrocatalysts which would be a promising candidate for electrochemical overall water splitting.     

Bifunctional electrocatalysts of CoFeP/rGO heterostructure for water splitting

Bifunctional non-precious electrocatalysts with high performance are highly desired for renewable energy but remain challenging. Herein, a CoFeP/rGO heterostructure was rational developed based on the synergistic effect, including superior conductivity, increased catalytic active sites of rGO support and the regulated electron distribution of bimetallic phosphide. At a current of 10 mA cm^?2, the CoFeP/rGO-2 composite exhibits excellent HER activity with low overpotentials of 101 mV and 76 mV in 1.0 M KOH and 0.5 M H₂SO₄ electrolyte, respectively. And highly active alkaline OER performance was provided with an overpotential of only 275 mV to reach a current density of 10 mA cm^?2. By the way, the CoFeP/rGO-2 electrode showed a pleasured working voltage of 1.58 V for overall water splitting in alkaline environment. More importantly, the long term durability and higher stability of the catalysts demonstrated their feasibility of bimetallic phosphide/rGO system as bifunctional electrocatalysts.     

Multi-shelled CoS2–MoS2 hollow spheres as efficient bifunctional electrocatalysts for overall water splitting

The exploration of highly efficient non-precious electrocatalysts is essential for water splitting devices. Herein, we synthesized CoS₂–MoS₂ multi-shelled hollow spheres (MSHSs) as efficient electrocatalysts both for hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) using a Schiff base coordination polymer (CP). Co-CP solid spheres were converted to Co₃O₄ MSHSs by sintering in air. CoS₂–MoS₂ MSHSs were obtained by a solvothermal reaction of Co₃O₄ MSHSs and MoS₄²⁻ anions. CoS₂–MoS₂ MSHSs have a high specific surface area of 73.5 m²g^-1. Due to the synergistic effect between the CoS₂ and MoS₂, the electrode of CoS₂–MoS₂ MSHSs shows low overpotential of 109 mV with Tafel slope of 52.0 mV dec⁻¹ for HER, as well as a low overpotential of 288 mV with Tafel slope of 62.1 mV dec⁻¹ for OER at a current density of 10 mA cm⁻² in alkaline solution. The corresponding two-electrode system needs a potential of 1.61 V (vs. RHE) to obtain anodic current density of 10 mA cm⁻² for OER and maintains excellent stability for 10 h.     

Hydrothermally/electrochemically decorated FeSe on Ni-foam electrode: An efficient bifunctional electrocatalysts for overall water splitting in an alkaline medium

A new hybrid catalyst based on Ni foam (NF) and FeSe was prepared by a facial hydrothermal method, in which Se-decorated NF was subsequently electrochemically doped by Fe. Binder-free catalyst containing electrodes were directly tested for the hydrogen and oxygen evolution reaction (HER/OER). The FeSe/NF electrode displayed an OER current density of 100 mA cm⁻² at potential of 1.42 V, and a relatively small Tafel slope of 109 mV dec⁻¹ in a 1 M KOH solution. Also, FeSe/NF electrode exhibited reasonable HER overpotential of 200 mV at 10 mAcm⁻² current density with Tafel slope of 145 mV dec⁻¹. The XRD and TEM studies revealed that the formation of heterogeneous interfaces of NiSe₂ and FeSe₂,generated more active sites that can promote better ions and electron transport in the electrode/electrolyte interfaces. Furthermore, HRTEM analysis indicates that FeSe₂ rich in Se vacancy defects can be created with suitable M − O and M − H bond for better OER and HER performance, respectively. In a-two electrode alkaline water electrolyzer, current densities of 10 mA cm⁻² and 50 mA cm⁻² were obtained at cell voltages of 1.52 V and 1.85 V, respectively, using pure FeSe–NF as both the cathode and anode.     

Quick-to-synthesize hybrid electrodes composed of activated carbon cloth with Co/Fe-based films as bifunctional electrocatalysts for water splitting

Hybrid electrodes have recently been investigated as attractive alternatives to noble-metal-based electrocatalysts for hydrogen production by water splitting. Herein, we propose an electrode composed of an oxidized carbon cloth with an electrodeposited bimetallic Co/Fe-based film. By optimizing the electrodeposition conditions and applying electrochemically activated carbon cloth as a substrate, one can prepare a free-standing noble-metal-free electrocatalytic electrode with high bifunctional electrocatalytic activity in hydrogen and oxygen evolution from alkaline solution. The developed Fe_0.25Co_0.75 electrode requires overpotentials of 245 mV for HER and 360 mV for OER at high current densities of −100 and 100 mA cm⁻², respectively. Furthermore, its overall synthesis time from commercially available raw materials is only approximately 20 min. The electrode material was used as both a cathode and an anode in the model electrolyzer, which can deliver 10 mA cm⁻² of current density at 1.66 V without loss of activity during 100 h of performance.