Search Results (112)

A natural deep eutectic solvent (NADES)-based electropolymerization strategy was developed to deposit polypyrrole (PPy) and Naproxen-doped PPy films onto a biomedical Ti–20Zr–5Ta–2Ag high-entropy alloy. Using cyclic voltammetry, chronoamperometry, and chronopotentiometry, coatings were grown potentiostatically (1.2–1.6 V) or galvanostatically (0.5–1 mA) to fixed charge values (1.6–2.2 C). Surface morphology and composition were assessed by optical microscopy, SEM and FTIR, while wettability was quantified via static contact-angle measurements in simulated body fluid (SBF). Electrochemical performance in SBF was evaluated through open-circuit potential monitoring, potentiodynamic polarization, and electrochemical impedance spectroscopy. Drug-release kinetics were determined by UV–Vis spectrophotometry and analyzed using mathematical modelling. Compared to uncoated alloy, PPy and PPy–Naproxen coatings increased hydrophilicity (contact angles reduced from ~31° to <10°), and reduced corrosion current densities from 754 µA/cm² to below 5.5 µA/cm², with polarization resistances rising from 0.06 to up to 37.8 kΩ·cm². Naproxen incorporation further enhanced barrier integrity (R_coat up to 1.4 × 10¹¹ Ω·cm²) and enabled sustained drug release (>90% over 8 days), with diffusion exponents indicating Fickian (n ≈ 0.51) and anomalous (n ≈ 0.67) transport for potentiostatic and galvanostatic coatings, respectively. These multifunctional PPy–Naproxen films combine robust corrosion protection with controlled therapeutic delivery, supporting their potential biomimetic role as smart coatings for next-generation implantable devices. Full article

Hydrogen energy is a pivotal carrier for achieving carbon neutrality, requiring green and efficient production via water electrolysis. However, the anodic oxygen evolution reaction (OER) involves a sluggish four-electron transfer process, resulting in high overpotentials, while the prohibitive cost and complex preparation of precious metal catalysts impede large-scale commercialization. In this study, we develop a FeCo-based bimetallic deep eutectic solvent (FeCo-DES) as a multifunctional reaction medium for engineering a three-dimensional (3D) coral-like FeOOH-Co₂(OH)₃Cl/NF composite via a mild one-step impregnation approach (70 °C, ambient pressure). The FeCo-DES simultaneously serves as the solvent, metal source, and redox agent, driving the controlled in situ assembly of FeOOH-Co₂(OH)₃Cl hybrids on Ni(OH)₂/NiOOH-coated nickel foam (NF). This hierarchical architecture induces synergistic enhancement through geometric structural effects combined with multi-component electronic interactions. Consequently, the FeOOH-Co₂(OH)₃Cl/NF catalyst achieves a remarkably low overpotential of 197 mV at 100 mA cm⁻² and a Tafel slope of 65.9 mV dec⁻¹, along with 98% current retention over 24 h chronopotentiometry. This study pioneers a DES-mediated strategy for designing robust composite catalysts, establishing a scalable blueprint for high-performance and low-cost OER systems. Full article

Efficient and low-cost electrocatalysts for the hydrogen evolution reaction (HER) in alkaline media are essential for sustainable hydrogen production. In this study, Ni electrocatalysts were deposited on pencil graphite using a simple one-step pulsed current electrodeposition method, from both acidic Watts and alkaline citrate baths. The influence of bath type and electrodeposition parameters—current density and temperature—on catalyst morphology and performance for HER was systematically investigated by scanning electron microscopy and electrochemical methods. Linear sweep voltammetry, chronopotentiometry, and electrochemical impedance spectroscopy (EIS) were used to evaluate the electrocatalytic activity, stability, and HER mechanism. The best catalytic performance was achieved for the Ni electrocatalyst deposited from the citrate bath at 50 mA cm⁻² and 40 °C, showing an exchange current density of 0.93 mA cm⁻², a Tafel slope of −208 mV dec⁻¹, and overpotentials of −210 mV and −386 mV at 10 and 100 mA cm⁻², respectively, in 1 M KOH solution. Chronopotentiometry confirmed improved stability and an overpotential reduction of approximately 92 mV as compared to pure Ni, while EIS revealed the lowest charge transfer resistance. It was shown that the electrocatalysts deposited from the citrate bath outperform those from the Watts bath, and electrodeposition at 40 °C is optimal for achieving the highest electrocatalytic activity for HER. Full article

Copper niobate (CuNb₂O₆) is an important compound due to its low cost and polymorphism, presenting monoclinic and orthorhombic phases, which leads to unique physical–chemical properties. The electrochemical performance of efficient electrocatalysts for the oxygen evolution reaction (OER) is of importance in order to produce hydrogen gas from water. In this context, this work reports the synthesis of CuNb₂O₆ particles by high-energy milling for 5 and 10 h, and subsequent thermal treatment at 900 °C for 3 h. The samples were characterized by XRD, XRF, FESEM, RAMAN, UV–Vis, and FT-IR techniques, and were applied as electrocatalysts for the OER. The samples had both monoclinic and orthorhombic crystalline phases. The band gaps were in the range of 1.92 to 2.06 eV. In the application for the OER, the particles obtained by 5 and 10 h of milling exhibited overpotentials of 476 and 347 mV vs. RHE at 10 mA cm⁻², respectively. In chronopotentiometry experiments for 15 h, the samples exhibited excellent chemical stability. The electrochemical performance of the sample milled for 10 h showed superior performance (347 mV vs. RHE) when compared with electrocatalysts of the same type, demonstrating that the methodology used to synthesize the samples is promising for energy applications. Full article

The electrochemical water splitting method is widely regarded as an efficient and sustainable approach for producing high-purity hydrogen in an environmentally friendly manner. Cost-effective and efficient electrocatalysts are essential for augmenting the electrocatalytic water oxidation reaction. Herein, the PEG-WO₃-NiO electrocatalyst is acknowledged for attaining efficient oxygen evolution reaction (OER) performances in alkaline conditions. The NiO nanoparticles anchored themselves to the PEG-WO₃‘s surface and produced an effective interfacial contact between the electrocatalyst materials. Among various compositions, the optimized ratio of the PEG-WO₃-NiO electrocatalyst exhibits a low overpotential of 349.7 mV at a current density of 10 mA cm⁻² and a Tafel slope of 71.22 mV dec⁻¹ for the OER in 1 M KOH. Additionally, the electrocatalyst demonstrates excellent stability, maintaining its performance even after 5000 cyclic voltammetry (CV) cycles and chronopotentiometry analysis. Given its durability and high electrochemically active surface area, the PEG-WO₃-NiO electrocatalyst contributes to the advancement of cost-effective and scalable solutions for water oxidation applications. Full article

Cobalt electrochemical deposition, with its bottom–up growth properties, is a core technology for creating metal interconnects. Additives are crucial during electrodeposition to control the quality of deposits by adsorbing onto the Co surface. The functional groups of additive molecules are the key to tailoring the adsorption behavior. This study focuses on heteroaromatic thiol additives, including 2-mercaptobenzimidazole (MBI), 2-mercapto-5-benzimidazolesulfonic acid sodium salt dehydrate (MBIS), and 2-mercaptobenzoxazole (MBO). Cyclic voltammetry, chronopotentiometry, quantum chemical calculations, and characterization tests were employed to investigate the adsorption behavior of additive molecules with different functional groups on cobalt. The results indicate that the inhibitory strength of the three additives on electrodeposition follows the following order: MBI > MBIS > MBO. The strong inhibitory effect of MBI primarily stems from the adsorption of the thiol group, the pyridine-like nitrogen in the heterocycle, and the benzene ring. MBIS exhibits reduced inhibitory capability due to the combined effects of the sulfonic acid group and hydrolysis ionization. MBO, with the introduction of an oxygen atom in the heterocycle, shows the weakest adsorption and inhibitory capability among the three. Full article

Water electrolysis for hydrogen production is of great importance for the reliable use of renewable energy sources to have a clean environment. Electrolyzers play a key role in achieving the carbon-neutral target of 2050. Among the different types of water electrolyzers, proton exchange membrane water electrolyzers (PEMWEs) represent a well-developed technology that can be easily integrated into the smart grid for efficient energy management. In this study, a discrete dynamic mathematical model of a PEMWE was developed in MATLAB/Simulink to simulate cell performance under various operating conditions such as temperature, inlet flow rate, and current density loads. A lab-scale test bench was designed and set up, and a 5 cm² PEMWE was tested at different temperatures (40–80 °C) and flow rates (3–12 mL/min), obtaining Linear Sweep Voltammetry (LSV), Cyclic Voltammetry (CV), Chrono-potentiometry (CP), and Electrochemical Impedance Spectroscopy (EIS) results for comparison and adjustment of the dynamic model. Sensitivity analysis of different operating variables confirmed that current density and temperature are the most influential factors affecting cell voltage. The parametric sensitivity of various chemical–physical and electrochemical parameters was also investigated. The most significant ones were estimated via non-linear least squares optimization to fine-tune the model. Additionally, strong correlations between these parameters and temperature were identified through regression analysis, enabling accurate performance prediction across the studied temperature range. Full article

This study presents a comprehensive electrochemical characterization and simulation of anion exchange membranes (AEMs) for water treatment applications, focusing on ion transport behavior. Experimental techniques, including chronopotentiometry, current–voltage (I–V) curve measurements, and electrochemical impedance spectroscopy (EIS), were employed to investigate the kinetics and dynamics of ion transport at the membrane interface. The results were validated and further explored through finite element method (FEM) simulations using COMSOL Multiphysics. The study revealed key insights into the role of membrane resistance, ion diffusion, and capacitive effects on overall membrane performance. Parametric analyses of electrolyte layer thickness, bulk solution concentration, and membrane porosity provided guidelines for optimizing membrane design. The findings highlight the importance of considering these factors in enhancing the efficiency and applicability of AEMs in water treatment processes. Future work will focus on refining simulation models and exploring advanced materials to further improve membrane performance. Full article

The use of a novel chrono-potentiometry method (abbreviated as “CP”) in the determination of the moisture content in wood (abbreviated as “MC”) above the FSP is a practical application of the electrical charging effect (or ECE). In the specific case of this CP method, the ECE consists of an electrical charging phase for the wood and a discharge phase following the interruption of the charging current. The electrical resistance, R, and the electrical chargeability, Cha(E), of three hardwood species were determined from the final potential, E1, of the charging phase and the initial potential, E2, of the discharge phase, with the three hardwood species being birch (Betula spp.), aspen (Populus spp.), and black alder (Alnus glutinosa (L.) Gaertn). An auxiliary variable in the form of U (E1; E2) was defined as a function of E1 and E2. This was used as an independent electrical variable in the calibration model for a CP moisture meter for the three tree species when it came to the moisture content (MC) region above the FSP (fibre saturation point). It was found that upon a determination of the MC in the wood, the traditional calibration model (the R-model), which uses the electrical resistance of wood, was able to predict a single-measurement precision level of +/−10% for the MC while the U-model predicted a precision level of +/−1.75% for the MC over a single MC measurement in the wood. Full article

This paper presents the application of a multi-sensor with a renewable surface based on a carbon black paste modified with ruthenium dioxide hydrate for monitoring the concentration changes of four ionic compounds (nitrate, ammonium, sodium, and calcium). By combining these into one sensor body, analyses can be performed simultaneously, based on a single standard curve, on a small number of available samples. The multi-sensor electrodes were characterized by determining both their electrical parameters, using methods such as chronopotentiometry and electrochemical impedance spectroscopy, and analytical parameters, through a series of potentiometric tests. The electrodes were characterized by high electric charge capacities ranging from 80 µF for the sodium electrode to 257 µF for the nitrate electrode. The tested electrodes showed calibration curve slopes of −51.1 mV/dec for the nitrate electrode, 59.3 mV/dec for the ammonium electrode, 57.0 mV/dec for the sodium electrode, and 26.0 mV/dec for the calcium electrode. The multi-sensor parameters allow for free determination of ions of biological significance in river water samples, soil samples, and plant substrates. The multi-sensor presented in this work can be successfully used to analyze water or plant substrates at home or among commercial crops. Full article

The corrosion of low-alloy steel in ethanolamine solution, simulating steam generator chemistry, is studied by in situ chronopotentiometry and electrochemical impedance spectroscopy combined with ex situ analysis of the obtained oxide films and model calculations. Hydrodynamic calculations of the proposed setup to study flow-assisted corrosion demonstrate that turbulent conditions are achieved. Quantum chemical calculations indicate the adsorption orientation of ethanolamine on the oxide surface. Interpretation of impedance spectra with a kinetic approach based on the mixed-conduction model enabled estimating the rate constants of oxidation at the alloy–oxide interface, as well as charge transfer and ionic transport resistances of the corrosion process. In turbulent conditions, the dissolution of Fe oxide and ejection of Fe cations are enhanced, leading to Cr enrichment in the oxide and alteration of its electronic and electrochemical properties that influence the corrosion rate. Full article

Herein, this work elucidates the synthesis of the Pd-MoS₂ catalyst for application in methanol-mediated overall water splitting. The scanning electron microscope (SEM) and transmission electron microscope (TEM) pictures offer an exciting nanostructured shape of the Pd-MoS₂, depicting a high surface area. Further, high-resolution TEM (HRTEM) pictures confirm the lattice plane (100), lattice spacing (0.26 nm), and hexagonal crystal structure of the Pd-MoS₂. Moreover, high-angle annular dark-field (HAADF) images and related color maps disclose the Mo, S, and Pd elements of the Pd-MoS₂. The Pd-MoS₂ catalyst exhibits lower overpotentials of 224.6 mV [methanol-mediated hydrogen evolution reaction (MM-HER)] at −10 mA cm⁻² and 133 mV [methanol-mediated oxygen evolution reaction (MM-OER)] at 10 mA cm⁻². Further, the Pd-MoS₂ illustrates noteworthy stability for 15.5 h for MM-HER and 18 h for MM-OER by chronopotentiometry test. Excitingly, the Pd-MoS₂∥Pd-MoS₂ cell reveals a small potential of 1.581 V compared to the MoS₂∥MoS₂ cell (1.648 V) in methanol-mediated overall water splitting. In addition, the Pd-MoS₂∥Pd-MoS₂ combination reveals brilliant durability over 18 h at 10 mA cm⁻². Full article

Mixed-metal nickel-iron, Ni_xFe materials draw attention as affordable earth-abundant electrocatalysts for the oxygen evolution reaction (OER). Here, nickel and mixed-metal nickel-iron metal–organic framework (MOF) composites with the carbon materials ketjenblack (KB) or carbon nanotubes (CNT) were synthesized in situ in a one-pot solvothermal reaction. As a direct comparison to these in situ synthesized composites, the neat MOFs were postsynthetically mixed by grinding with KB or CNT, to generate physical mixture composites. The in situ and postsynthetic MOF/carbon samples were comparatively tested as (pre-)catalysts for the OER, and most of them outperformed the RuO₂ benchmark. Depending on the carbon material and metal ratio, the in situ or postsynthetic composites performed better, showing that the method to generate the composite can influence the OER activity. The best material Ni₅Fe-CNT was synthesized in situ and achieved an overpotential (η) of 301 mV (RuO₂ η = 354 mV), a Tafel slope (b) of 58 mV/dec (RuO₂ b = 91 mV/dec), a charge transfer resistance (R_ct) of 7 Ω (RuO₂ R_ct = 39 Ω), and a faradaic efficiency (FE) of 95% (RuO₂ FE = 91%). Structural changes in the materials could be seen through a stability test in the alkaline electrolyte, and chronopotentiometry over 12 h showed that the derived electrocatalysts and RuO₂ have good stability. Full article

In this work, the possibilities of introducing nitric acid molecules with a solution concentration of 75–98% into graphite matrices in the form of synthetic quasi-monocrystal graphite and natural graphite of four different farcical compositions were determined in order to identify factors of the acid concentration and graphite size on the production process and properties of graphite foil. The actual stage of graphite intercalation in the resulting compound was determined by X-ray diffraction analysis (XRD). The differences in the temporal patterns of the intercalation process for different intercalation stages (from 2 to 5) are demonstrated. The obtained acid solutions were used in the manufacturing of flexible graphite foil from natural graphite of four different particle size distributions. The mass characteristics of the intermediate and final products were determined as the graphite was treated with these solutions. The actual difference in the characteristics of the raw materials and intermediate synthetic products was recorded by measuring the electrical conductivity of the final material, graphite foil. Analysis of the results has shown that a decrease in the acid concentration of a solution leads to an increase in the intercalation stage. Weight gains due to the formation of oxygen-containing groups and the introduction of water and acid were reduced by this effect, whereas the yield of the final product (thermally expanded graphite) increased. Foil made of thermally expanded graphite obtained from intercalated compounds of high stages had greater electrical conductivity. An improvement in the conductive properties of the material implies that there should be fewer defects in its structure. Full article

In green hydrogen production via water electrolysis, catalysts with multiscale nanostructures synthesized by compositing micro-heterojunctions and nanoporous structures exhibit excellent electrocatalytic oxygen evolution reaction (OER) performance. Moreover, they are the most promising non-noble metal catalysts. Herein, FeNi-based aerogels with a three-dimensional nanoporous structure and amorphous matrix embedded with FeNi₃ nanoclusters were synthesized via wet chemical reduction coprecipitation. The FeNi₃ nanoclusters and the FeNi-based amorphous matrix formed a crystalline–amorphous heterojunction. These aerogels exhibited excellent OER performance and electrocatalytic stability in alkaline electrolytes. In 1 mol/L of KOH electrolyte, the as-synthesized aerogel exhibited an overpotential of 262 mV at a current density of 20 mA cm⁻² with a Tafel slope of only 46 mV dec⁻¹. It also demonstrated excellent stability during a 12 h chronopotentiometry test. Full article