OER Activity Research Articles

Deciphering the energy storage and electro‐catalytic potential of the BaLa2MnS5 ternary metallic sulfide prepared via single source precursor route

AbstractThe present work elucidates the first report on the synthesis and energy applications of the novel BaLa2MnS5 prepared from single source precursor route. This metal chalcogenide expressed a tuned band gap of 3.84 eV and an average crystallite size of 20.52 nm. Functional groups explored for BaLa2MnS5 expressed strong signals for presence of the metal sulfide bonds. The thermal decomposition pattern of BaLa2MnS5 followed a two‐phased mechanism. Synthesized metal sulfide possessed an irregular morphology with particles arranged in random manner. An assessment of the chalcogenide BaLa2MnS5 for energy applications has been carried out. When employed as an electrode material in 1 M KOH, which acted as the background electrolyte, BaLa2MnS5 chalcogenide showed a specific capacitance of 597 F g−1. Furthermore, this BaLa2MnS5 chalcogenide decorated electrode has a low resistance, as shown by the Rs of 1.35 Ω, and a specific power density of 7366 W kg−1, according to the impedance investigations. The electrochemical results for the OER activity are indicative of the OER overpotential and Tafel slope values as 388 mV and 108 mV/dec. This electrode achieved the HER overpotential value of 241 mV while the obtained Tafel slope was 194 mV/dec.

Synthesis and characterization of (Ni, Mn)-ZnO/g-C3N4 nanocomposite for efficient electrochemical water splitting: The role of electrocatalyst for OER

The scarcity of non-renewable energy sources and rising worldwide temperatures are significant challenges. Electrochemical water splitting using low-cost materials (metals and their oxides) is a highly efficient and cost-effective method of producing both hydrogen and oxygen. Apart from precious metals, carbon-based materials have also shown effectiveness in catalyzing these reactions. To minimize overpotentials and enable practical applications, metal oxide encapsulation in graphite layers has demonstrated significant activity for both HER and OER. Metal oxides are known for their high conductivity and mechanical strength, making them suitable candidates for this task. In the present research, we report the design of a composite (Ni, Mn)-ZnO/g-C3N4 ((Ni, Mn)-CNZ) electrocatalyst with improved electrocatalytic performance. The coprecipitation of (Ni, Mn)-ZnO with graphitic carbon nitride (g-C3N4) produced the composite material. The structure of the electrocatalyst was analyzed using characteristic techniques such as FTIR, EDX, SEM, and XRD. Electrodeposition on FTO glass is employed to facilitate studies of water distribution. The (Ni, Mn)-CNZ composite exhibits excellent electrochemical water-splitting behavior, with low overpotentials, 380 mV (OER) and 288 mV (HER), reaching a current density of 10 mA cm−2 compared to Ni-CNZ and Mn-CNZ. This highlights the potential of (Ni, Mn)-CNZ as a highly effective electrocatalyst for water splitting.

Optimization of light response and electron redistribution of active sites by structuring CoS2/MoS2/Ni3S2 heterojunction for highly efficient photo-assisted oxygen evolution

Highly efficient photoelectrocatalysts become one of the current research hotspots for overall water splitting, the design of heterojunctions with a wide response range to sunlight and efficient separation and migration of photo-generated carriers is challenging. Herein, a nanorod CoS2/MoS2/Ni3S2 photoelectrocatalyst with heterojunction is prepared by a one-step hydrothermal method. Under simulated solar irradiation, CoS2/MoS2/Ni3S2 exhibits excellent photoelectrocatalytic activity for OER, with overpotential of 166 mV and the cell voltage of 1.464 V at 10 mA cm−2, and the catalytic performance exhibited a slight decline after 12 hours of stable operation. In addition the STH efficiency reaches 6.6 %. Experiments and DFT calculations demonstrate that CoS2 as a photoactive layer optimizes the light absorption properties of catalyst. Additionally, MoS2 as a co-catalyst modulates the d-band centers and the electronic structure of Co active site, reducing the energy barrier of the rate-determining step. Meanwhile, the II-type heterojunction formed by CoS2 and MoS2 can effectively promote the separation and migration of photo-generated carriers, which further enhances the photoelectrocatalytic OER performance. This work provides a novel insight to design photoelectrocatalysts with transition metal sulfide heterojunction for overall water splitting.

Modulation of electronic structure of Ni3S2 via Fe and Mo co-doping to enhance the bifunctional electrocatalytic activities for HER and OER

Heazlewoodite nickel sulfide (Ni3S2) is advocated as a promising nonnoble catalyst for electrochemical water splitting because of its unique structure configuration and high conductivity. However, the low active sites and strong sulfur–hydrogen bonds (S–Hads) formed on Ni3S2 surface greatly inhibit the desorption of Hads and reduce the hydrogen and oxygen evolution reaction (HER and OER) activity. Doping is a valid strategy to stimulate the intrinsic catalytic activity of pristine Ni3S2 via modifying the active site. Herein, the Ni foam supported Fe and Mo co-doped Ni3S2 electrocatalysts (Fe-MoS2/Ni3S2@NF) have been constructed using Keplerate polyoxomolybdate {Mo72F30} as precursor through a facile hydrothermal process. Experimental results certificate that Fe and Mo co-doping can effectively tune the local electronic structure, facilitate the interfacial electron transfer, and improve the intrinsic activity. Consequently, the Fe-MoS2/Ni3S2@NF display more excellent HER and OER activity than MoS2/Ni3S2@NF and bare Ni3S2@NF by delivering the 10 and 50 mA cm−2 current densities at ultra-low overpotentials of 74/175 and 80/160 mV for HER and OER. Moreover, when coupled in an alkaline electrolyzer, Fe-MoS2/Ni3S2@NF approached the current of 10 mA cm−2 under a cell voltage of 1.60 V and exhibit excellent stability. The strategy to realize tunable catalytic behaviors via foreign metal doping provides a new avenue to optimize the water splitting catalysts.

Sulfurization of bimetallic (Co and Fe) oxide and alloy decorated on multi-walled carbon nanotubes as efficient bifunctional electrocatalyst for water splitting

The advancement in electrocatalysis, particularly in the development of efficient catalysts for hydrogen and oxygen evolution reactions (HER and OER), is crucial for sustainable energy generation through processes like overall water splitting. A notable bifunctional electrocatalyst, CoFe2O4/Co7Fe3, has been engineered to facilitate both OER and HER concurrently, aiming to reduce overpotentials. In the pursuit of further enhancing catalytic efficiency, a morphological transformation has been achieved by introducing a sulphur source and multi-walled carbon nanotubes (MWCNTs) into the catalyst system, resulting in S–CoFe2O4/Co7Fe3/MWCNTs. This modification has significantly improved the activity for both OER and HER. An onset overpotential of 250 mV@10 mAcm−2 for the OER and 270 mV@50 mAcm−2 for the HER, indicating efficient catalytic activity at relatively low overpotentials. S–CoFe2O4/Co7Fe3/MWCNTs display an outstanding long-term stability in alkaline electrolytes, with minimal Tafel slopes of 77 mV/dec for the OER and 70 mV/dec for the HER, suggesting sustained catalytic performance over extended periods. Furthermore, when employed as both the cathode and anode in the context of complete water splitting, S–CoFe2O4/Co7Fe3/MWCNTs demonstrate an impressive cell voltage of 1.52 V at a current density of 10 mA cm−2 in a 1 M KOH solution, showcasing its viability for practical applications. Given its cost-effectiveness and superior activity, S–CoFe2O4/Co7Fe3/MWCNTs hold significant promise for widespread applications in overall water splitting electrocatalysis, contributing to the advancement of cleaner and sustainable fuel generation technologies.

Anion-modulated HER and OER activity of 1D Co-Mo based interstitial compound heterojunctions for the effective overall water splitting

Anion-modulated HER and OER activity of 1D Co-Mo based interstitial compound heterojunctions for the effective overall water splitting

Three-dimensional Cobalt-MOF/ CNF microstructured assembly as a bifunctional electrocatalyst for effective overall water-splitting in alkaline media

The electrocatalyst Co-MOF/CNF microstructure exhibits excellent stability and charge transfer efficiency synthesized via ultrasonication technique. The composite has a lower Rct value of 2 Ω. The larger Cdl value of Co-MOF/CNF (12.3 mF/dec) is responsible for the high catalytic activity for both HER and OER reactions. The composite has strong catalytic activity in HER and OER, with low overpotentials of 193 mV and 250 mV at 10 mA/cm2. Furthermore, excellent water electrolyzer activity was achieved by Co-MOF/CNF||Co-MOF/CNF with a cell voltage of 1.49 V at 10 mA/cm2 and is stable over 24 h, proving the long-term efficacy in sustainable energy systems.

Efficient synthesis strategy and synergistic effect of Ni-Fe-Ru electrode for boosting alkaline water electrolysis

Hydrogen production from alkaline water electrolysis (AWE) has promising potential in energy storage due to the advantages of low cost and large scale, but its bottleneck is the low current density and poor durability of non-precious metal electrodes. Although numerous electrode designs with superior activity have been reported, the complicated synthesis process and refined microstructure have not changed the high preparation cost, high resistance, and poor durability of conventional AWE electrodes. Here, we report an efficient synthesis strategy of high-density Ni-Fe-Ru electrode (particle size < 5 nm) and explore the synergistic effect between Ni-Fe-Ru elements at different potentials. The electrode exhibits excellent OER activity (264 mV@100 mA cm−2, Tafel slope = 49 mV dec−1) and AWE performance (400 mA cm−2@1.89 V), it can work stably for 300 h at 500 mA cm−2, with potential for industrial applications.

In-situ stabilization of metal-nitride sites in sprouted 2D cMOF@LDHs hetero-nano petals on metaloxynitrides nanostems for enhanced water splitting

Addressing the challenges of enhancing water-splitting efficiency necessitates the exploration and rational design of high-performance and durable electrocatalysts with appealing nanoarchitectures. In this study, we present the design and fabrication of conjugated cMOF/LDH hetero-nano petals decorated with monodispersed Metal-N sites, which are uniformly shelled over tungsten oxynitride (WNO) nanowire arrays to form a unique core–shell architecture. For this rational engineering, WNO nanowire arrays were grown on carbon cloth. Then, a thin-layered Ru-Co-Fe layered double hydroxide (RuCoFe/LDH) was deposited around these wires, resulting in a highly porous three-dimensional array of hierarchical hetero RuCoFe-LDHs@WNO-NWs core–shell nanowires (RuCoFe-NSs@WNO-NWs). Subsequently, the linkers coordinated with the RuCoFe-LDH nanosheets and transformed them in-situ into the RuCoFe-cMOF nano petals (RuCoFe-NPs@WNO-NWs). Notably, the linker’s amino groups functioned as hooks for precisely anchoring and stabilizing metal sites, forming the metal nitride (M-N) moieties. Interestingly, the designed bi-functional catalyst exhibited superior catalytic activities for both OER (230 mV @ 10 mAcm−2) and HER (49 mV @ 10 mAcm−2) in an alkaline medium. Additionally, an electrolyzer cell employing Ru-CoFe-NPs@WNO-NWs as a bi-functional electrocatalyst required 1.49V to reach a current density of 10 mA cm−2. These remarkable catalytic performances can be attributed to several key factors, including opulent exposed active sites, an efficient charge/mass transport pathway, an optimized electronic structure, and an interfacial synergy effect. Hence, this study provides a new perspective for the design of efficient bi-functional electrocatalysts for use in the energy related electrochemical devices.

Hierarchical mesh-type oxygen electrode using carbon nanotube framework for anion-exchange membrane-based unitized regenerative fuel cells

Developing three-dimensional porous oxygen electrodes (OE) is crucial for enhancing round-trip efficiency (RTE) of anion-exchange membrane-based unitized regenerative fuel cells (AEM_URFCs). Herein, a novel OE design of AEM_URFCs is presented based on a hierarchical mesh electrode (HME) with a porous carbon nanotube (CNT) framework. The HME, featuring square-shaped macropores achieved by dispersing catalyst nanoparticles on the CNT framework enhances surface area, mass transport, and electron transport. Half-cell test demonstrated superior oxygen reduction reaction and oxygen evolution reaction activity compared to conventional electrodes. Moreover, the HME maintained stable ORR and OER activity during the stability test. In single-cell tests, the AEM_URFCs with the HME exhibited higher RTE (55% at 20 mA cm−2), surpassing the conventional electrode (52%). Furthermore, RTE was maintained at a remarkable 41% under ultrahigh current density (250 mA cm−2), which is unprecedented in the literature. The AEM_URFCs featuring the HME displayed superior cyclability over 5 cycles and durable performances under both fuel cell and water electrolysis modes.

Elucidating the construction and modulation of built-in electric field in the oxygen evolution reaction

The construction of a built-in electric field (BIEF) is considered to be an effective strategy for enhancing catalyst performance due to its critical role in optimizing adsorption of reactants and key intermediates, as well as its positive impact on interface behavior. Herein, a strategy is developed to elucidate the correlation between oxygen evolution reaction activity and the BIEF and its strength by constructing and enhancing the BIEF through incorporating manganese into Co3O4@NiFe-LDH p-n heterojunction. This Co3O4@NiFe-LDH p-n heterojunction generates a BIEF that effectively regulates electronic structure, facilitates rapid electron transfer, induces alterations in the chemical microenvironment, and modulates intermediate adsorption energy. Notably, when hetoroatomic Mn is incorporated into the p-n heterojunction, particularly encapsulated within NiFe-LDH, a more pronounced enhancement for BIEF is observed. Benefiting from this strong BIEF, Co3O4@Mn/NiFe-LDH exhibits excellent OER activity and stability with an overpotential of only 209 mV at 50 mA cm−2, a Tafel slope of 57 mV dec−1, and stable operation for 110 h at approximately 10 mA cm−2. Moreover, density functional theory (DFT) calculations further confirms that the construction and reinforcement of the BIEF can effectively accelerate the electron transfer rates, adjust the metal d-band center, optimize intermediates adsorption properties, and reduce the reaction energy barriers.

Heterogeneous Ni-Boride/Phosphide Anchored Amorphous B-C Layer for Overall Water Electrocatalysis.

The rational design of efficient and economical bifunctional electrocatalysts remained a challenge for overall water electrolysis. In this work, the Ni-boride/ phosphide particles anchored amorphous B-doped carbon layer with hierarchical porous characteristics in Ni foam (Ni3P/Ni3B/B-C/NF) was fabricated for overall water splitting. The Boroncarbide (B4C) power was filled and fixed in the NF interspace through the electroplating and electroless plating, and then annealed in vacuum high temperature. The amorphous B-C layer derived from the B4 C not only speeded up the electron transport, but also cooperate with Ni-boride/phosphide to enhance the electrocatalytic activity for HER and OER synergistically. Furthermore, the hierarchical porous architecture of Ni3P/Ni3B/B-C/NF increased space utilization to load more active materials. The self-supported Ni3P/Ni3B/B-C/NF electrode possessed a low overpotential of 212 and 280 mV to deliver 100 mA cm-2 for HER and OER, respectively, and high stability for 48 h. In particular, the electrolyzer constituted with the Ni3P/Ni3B/B-C/NF bifunctional electrocatalyst only required a voltage of 1.59 V at 50 mA cm-2 for water electrocatalysis under alkaline medium, and demonstrated long-term stability for 48 h. This study provides a new technical path for the development of bifunctional of transition metal borides to promote the application of hydrogen production from water splitting.

Electron Manipulation and Surface Reconstruction of Bimetallic Iron-Nickel Phosphide Nanotubes for Enhanced Alkaline Water Electrolysis.

Developing high-efficiency and stable bifunctional electrocatalysts for water splitting remains a great challenge. Herein, NiMoO4 nanowires as sacrificial templates to synthesize Mo-doped NiFe Prussian blue analogs are employed, which can be easily phosphorized to Mo-doped Fe2xNi2(1-x)P nanotubes (Mo-FeNiP NTs). This synthesis method enables the controlled etching of NiMoO4 nanowires that results in a unique hollow nanotube architecture. As a bifunctional catalyst, the Mo-FeNiP NTs present lower overpotential and Tafel slope of 151.3 (232.6) mV at 100 mA cm-2 and 76.2 (64.7) mV dec-1 for HER (OER), respectively. Additionally, it only requires an ultralow cell voltage of 1.47 V to achieve 10 mA cm-2 for overall water splitting and can steadily operate for 200 h at 100 mA cm-2. First-principles calculations demonstrate that Mo doping can effectively adjust the electron redistribution of the Ni hollow sites to optimize the hydrogen adsorption-free energy for HER. Besides, in situ Raman characterization reveals the dissolving of doped Mo can promote a rapid surface reconstruction on Mo-FeNiP NTs to dynamically stable (Fe)Ni-oxyhydroxide layers, serving as the actual active species for OER. The work proposes a rational approach addressed by electron manipulation and surface reconstruction of bimetallic phosphides to regulate both the HER and OER activity.

Chemical etching to boost medium-entropy metal oxide for oxygen evolution reaction in alkaline

It is crucial to improve the catalytic activity of medium-entropy materials by adjusting the surface electronic structure of medium-entropy materials. In this research, we utilize a chemical etching method for synthesizing a medium-entropy metal oxide E-FeCoNiZn with abundant defects. Owing to the etching of Zn, a special form of electron-transfer by means of electron-accepting-donating is introduced, which greatly optimizes OER activity. The E-FeCoNiZn displays a superior OER activity with a low overpotential of 259 mV at 10 mA cm−2 and a small Tafel slope of 37.1 mV dec-1 in 1 M KOH solution, outperformingtheperformanceofFeCoNiZn and Ni-foam,whilemaintainingexcellentstabilityover48 h. Theoretical calculations demonstrate that the introduction of defects regulates the surface electronic structure of the E-FeCoNiZn via modifying the number of electrons transferred and then optimize the OER activity. Thisworkprovidesa newstrategyfordesigning medium-entropy materials possessing high catalytic activity.

Theoretical screening of corrole-based covalent organic framework metal single-atom catalysts for ORR and OER

Corrole-based covalent organic frameworks (COFs) are newly developing porous crystalline materials in the catalysis field due to their thermal stability, and ease of being functionalized by high-valent metal at the corrole center. In this work, based on the monolayer TPAPC-COF (m-TPAPC-COF), a series of stable metal corrole-based 2D monolayer SACs M1@TPAPC-COFs (M = Fe, Co, Ni, Cu, Ru, Rh, Os, Ir, Pt, Au) have been obtained by screening using density functional theory (DFT) calculations. As O2 can be adsorbed and activated on M1@TPAPC-COFs (M = Fe, Co, Ru, Rh, Os, Ir), we predicted two types of non-noble metal corrole-based COFs SACs, one is a bifunctional SAC Fe1@TPAPC-COF with high electrocatalytic activity for ORR/OER and the other is a Co1@TPAPC-COF with high electrocatalytic activity for OER, respectively. This work demonstrates that corrole-based COF is a promising 2D material for constructing high-performance SACs for the ORR and OER.

Controllable boosting activity on Co4N by Fe substitution for oxygen evolution reaction and efficient 5-hydroxymethylfurfural oxidation

The design of transition metal nitrides with excellent oxygen evolution reaction and 5-hydroxymethylfurfural oxidation reaction (HMFOR) is of great significance to achieve the goal of "carbon peaking and carbon neutrality". Herein, Fe-doped bimetallic nitride FexCo1-x)4N was prepared by a simple electron regulation strategy. The introduction of Fe changes the electronic structure of Co and optimizes the adsorption energies of *OH, reduces the potential barrier for the generation of *OOH as a potential-determining step and thus increases the intrinsic OER activity of Co4N. In addition, Fe substitution of some of the Co atoms gives (FexCo1-x)4N a higher electrochemical active surface area, which accelerates the electron transfer efficiency and improves the electrical conductivity. The overpotential for (FexCo1-x)4N-0.9 to reach a current density of 10 mA cm−2 in 1 M KOH is only 271 mV. When in 1 M KOH + 50 mM HMF condition, (FexCo1-x)4N-0.9 requires only 1.37 V to reach a current density of 10 mA cm−2. This work provides practical guidance for developing bifunctional transition metal electrocatalysts with excellent OER and HMFOR activity.

Non-precious metal high-entropy electrocatalysts (Al0.5NiCoCr-X0.5) for OER application

The high entropy alloy electrocatalysts demonstrate exceptional efficiency in the production of hydrogen through water electrolysis. Consequently, the development of durable and economically efficient electrocatalysts has become an urgent objective to accomplish. In order to achieve this goal, a bulk non-precious metal high-entropy alloy, Al0.5NiCoCr-X0.5 (Mo, Mn, Cu, V, Fe), was synthesized and characterized in this study through physical phase analysis and electrochemical property test. To explore the reasons for the influence of the five added elements on the catalytic performance of high entropy alloys in this system and to find the OER electrocatalyst with the best catalytic performance. Electrochemical performance tests were performed in 1 M KOH electrolyte. At a current density of 10 mA·cm−2, the overpotential of the high-entropy alloy catalyst Al0.5NiCoCrMo0.5 was lower than that of the high-entropy alloy with the addition of the other four elements respectively, which was only 327 mV, and lower than that of the conventional noble metal catalyst RuO2, which had an overpotential of 342 mV. This is attributed to the addition of Mo element, which makes Al0.5NiCoCr produce a large number of HCP phases on top of the original FCC phase and a very small number of BCC phases, which is more conducive to the generation of active sites on the surface of the catalysts, and thus improves the OER activity, and the stability can be maintained for at least 20 hours. Therefore, Al0.5NiCoCrMo0.5 high-entropy alloy catalysts can be used in industrial hydrogen production instead of the traditional precious metal catalysts, and it has a rather broad application prospect, and at the same time, it lays a solid foundation for the application of transition metals in catalysts.

CoM-ZSM5 (M = Zn and Ni) Zeolites for an Oxygen Evolution Reaction in Alkaline Media

An ion-exchange procedure of synthetic zeolite ZSM-5 (Si/Al = 15) was used to prepare three cobalt ZSM-5 zeolites (CoM-ZSM5 (M = Zn and Ni)) that were examined for OERs in alkaline media. The structural, morphological, and surface properties of the prepared materials were studied by X-ray powder diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy with energy dispersive spectroscopy, and low-temperature nitrogen adsorption. All three electrocatalysts showed OER activity where CoNi-ZSM5 presented the highest current density (9.5 mA cm−2 at 2 V), the lowest Tafel slope (134 mV dec−1), and the lowest resistances of the charge transfer reaction (31.5 Ω). Overpotential (ηonset) at an onset potential of 410 mV for both CoNi-ZSM5 and Co-ZSM5 and 440 mV for CoZn-ZSM5 electrodes was observed. Co-ZSM5 showed somewhat lower OER catalytic activity than CoNi-ZSM5, while CoZn-ZSM5 demonstrated the lowest OER catalytic activity. The Rct of CoZn-ZSM5 is significantly higher than the Rct of CoNi-ZSM5, which could lead to their different OER activities. Good OER stability and low price are the main advantages of the synthesized CoM-ZSM5 samples in this study.

Investigating the electrochemical performance of Mn3O4/MoMn2P12 mixed-phase catalyst on MWCNT for high specific energy supercapacitors and HER/OER reactions

A versatile Mn/MoMn hybrid oxide/phosphide composite (MnO/MoMnP) supported on MWCNT is synthesized using hydrothermal method and in-situ phosphorization methods. This composite serves as a catalyst for supercapacitors and oxygen and hydrogen evolution reactions (OER/HER) in electrochemical water splitting. XRD analysis confirmed the presence of mixed-phase of Mn3O4 and MoMn2P12. Electrochemical tests revealed exceptional charge storage performance for MnO/MoMnP/MWCNT, with a high specific capacitance(436 F g−1 at 1 A g−1) and impressive capacitance retention (96.51 % for 5000 cycles at 15 A g−1). This performance surpasses that of bare MnO/MoMnP by 50 %. Furthermore, we assembled a MnO/MoMnP/MWCNT//MWCNT device, that achieved a remarkable energy density of 128.11 W h kg−1 at an ultra-high-power density of 1920 W kg−1, along with excellent cycling stability (92.5 % for 5000 cycles). Moreover, the MnO/MoMnP/MWCNT composite exhibited a remarkable bifunctional electro catalytic activity for OER and HER, with low overpotentials of 335 and 430 mV at 10 mA cm−2 in 1 M KOH solution. These results highlight MnO/MoMnP/MWCNT as a promising and efficient alternative catalyst for future applications in supercapacitors and water electrolysis.

Preparation of highly active and durable electrodes for alkaline water electrolysis by anodizing of commercial FeNi and FeNiCo alloys

Anodizing is gaining popularity as a binder-free fabrication route for obtaining catalyst materials directly on the current collector without using noble metals, binders, or conductive carbon additives. Here, we fabricate promising highly active electrodes for alkaline water electrolysis by anodizing commercial FeNi and FeNiCo alloys (%wt. Fe range between 22 and 63) in an ethylene glycol-based fluoride electrolyte. Anodizing forms metal fluoride coatings, which are converted to OER active compounds (γ-NiOOH:Fe) during potential cycling in an alkaline aqueous solution (1 mol L−1 (M) KOH at 293 K) as a result of leaching of fluoride ions. The morphology, thickness, and number of active sites are influenced by the amount of Fe in the alloy, and the electrode with the highest electrochemical active surface area (Kovar alloy with a 54 %wt. Fe) shows the largest OER activity enhancement by anodizing. The performance evaluation in practical conditions (7 mol L−1 KOH at 343 K) demonstrated a highly active performance with an OER potential as low as 1.52 V at a current density of 600 mA cm−2 even for electrodes obtained in alloys with a low amount of Fe (78-Permalloy with a 22 %wt. Fe), demonstrating that anodizing is an effective way to develop highly active OER electrodes from commercially available alloys. On the other hand, anodizing is a good fluoridation route for transition metals with good results in the formation of F-enriched precursors that efficiently promote active phase formation during the catalytic process, offering the possibility of obtaining catalysts directly on the current collector in a one-step process, easily implemented in industrial applications.