Advanced alkaline water electrolysis (AWE) in “zero-gap” configuration is a promising approach for low-temperature hydrogen production, but its efficiency strongly depends on the design and surface chemistry of nickel-based electrodes. Here, we present a simple dip-and-drying method (DDM) to modify commercial nickel foam with a Ni–FeOOH/PTFE microporous catalytic layer and evaluate its electrochemical performance in 1 M KOH and in a laboratory zero-gap cell with a Zirfon^® Perl 500 UTP diaphragm, through circulating 25 wt.% KOH. The FeSO₄-assisted DDM treatment generates mixed Ni–Fe oxyhydroxide surface species, while PTFE imparts control hydrophobicity, enhancing both catalytic activity and gas-release behavior. Annealing the electrode (DDM-NF-CAT-A) results in a cell voltage of 2.45 V at 1 A·cm⁻² and 80 °C, demonstrating moderate performance comparable to other Ni-based electrodes prepared via low-complexity methods, though below that of optimized state-of-the-art zero-gap systems. Short-term durability tests (80 h at 0.5 A·cm⁻²) indicate stable operation, but long-term industrial performance was not assessed. These findings illustrate the potential of the DDM approach as a simple, low-cost route to structured nickel foam electrodes and provide a foundation for further optimization of catalyst loading, microstructure, and long-term stability for practical AWE applications.

This work demonstrates for the first time a cost-effective modification of stainless-steel electrodes with an Fe³⁺ precursor via the deep-and-dry method (DDM) at processing temperatures between 20 °C and 80 °C, enabling their simultaneous applicability for both OER and HER in zero-gap electrolyzers. The approach offers a durable and economical alternative to conventional nickel-based electrodes. Morphological and compositional analyses by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) demonstrated a pronounced temperature-dependent evolution of surface features. At 20 °C, the coatings exhibited high porosity and incomplete coverage, whereas treatment at 60 °C yielded a compact, uniform, and continuous layer with suppressed Fe/Ni exposure and enhanced oxygen incorporation. Electrochemical characterization in 25% KOH by cyclic voltammetry and polarization measurements confirmed reversible redox behavior and comparable electrochemically active surface areas across all samples, with the 60 °C electrodes achieving the highest catalytic activity. In electrolysis cell tests (zero gap), the optimized electrodes delivered low cell voltages, current densities up to 1.35 A cm⁻², and power outputs approaching 3.5 W cm⁻². These results establish processing temperature as a decisive factor for tailoring the morphology, composition, and performance of DDM-fabricated electrodes, underscoring the promise of 60 °C-treated electrodes for efficient hydrogen production.

This study investigates the performance of a commercial PEM (proton exchange membrane) electrolysis cell, with a working area of 16 cm2 and catalyst loading of 2 mg /cm-2 of IrRuOx on the anode, and 0.5 mg /cm-2 of 60% PtC and 0.25 mg /cm-2 of PtB on the cathode side, under constant and dynamic conditions to identify optimal operating modes for practical use. For this purpose, a custom programmable proportional-integrated (PI) direct current (DC) regulator and a pulse-width-modulation (PWM) frequency generator were developed to provide stationary and dynamic modes, functioning as a single system with integrated data logging for cell voltage, temperature, and pressure sensors via a C# program. Experiments confirmed that square wave pulse loading at 1 Hz with 50% duty cycle provides increased efficiency by reducing the cell voltage compared to a continuous DC operation.