Search Results (105)

This work deals with the comparative analysis of fluoride coatings, i.e., 5 wt.% AlF₃ and LiF, applied as surface layer of Li-rich Li_1.2Ni_0.13Co_0.13Mn_0.54O₂ (LNCM) layered oxides synthesized via facile and cost-effective sol–gel route. The detailed structural and morphological characterizations demonstrate that AlF₃ and LiF deposits have a pivotal role in enhancing the electrochemical properties of LNCM. These electrochemical properties include galvanostatic charge–discharge (GCD), differential capacity (dQ/dV), electrochemical impedance spectroscopy (EIS), and area-specific impedance (ASI). A much lower decay of the discharge capacity of 0.22 and 0.25 mAh g⁻¹ per cycle was obtained for AlF₃- and LiF-coated LMNC, respectively, after 100 charge/discharge cycles at 0.1 C compared with 0.42 mAh g⁻¹ per cycle for pristine LNCM. Results evidence the non-evolution of the charge transfer resistance, enhanced lithium-ion kinetics and stabilization of electrode/electrolyte interface during cycling. Full article

Tungsten oxide (WO₃) nanostructures have emerged as promising electroactive materials due to their high pseudocapacitance, structural versatility, and chemical stability, while reduced graphene oxide (rGO) provides excellent electrical conductivity and surface area. The strategic combination of these nanomaterials in hybrid electrodes has gained attention for enhancing the energy storage performance of supercapacitors. In this work, we report the fabrication and electrochemical performance of nanostructured multilayer films based on the electrostatic Layer-by-Layer (LbL) self-assembly of poly (amidoamine) (PAMAM) dendrimers alternated with tungsten oxide (WO₃) nanofibers dispersed in reduced graphene oxide (rGO). The films were deposited onto indium tin oxide (ITO) substrates and subsequently subjected to electrochemical reduction. UV-Vis spectroscopy confirmed the linear growth of the multilayers, while atomic force microscopy (AFM) revealed homogeneous surface morphology and thickness control. Electrochemical characterization by cyclic voltammetry (CV) and galvanostatic charge–discharge (GCD) revealed a predominantly electrical double-layer capacitive (EDLC) behavior. From the GCD measurements (PAMAM/rGO-WO₃)₂₀ films achieved an areal capacitance of ≈2.20 mF·cm⁻², delivering an areal energy density of ≈0.17 µWh·cm⁻² and an areal power density of ≈2.10 µW·cm⁻², demonstrating efficient charge storage in an ultrathin electrode architecture. These results show that the synergistic integration of PAMAM dendrimers, reduced graphene oxide, and WO₃ nanofibers yields a promising strategy for designing high-performance electrode materials for next-generation supercapacitors. Full article

A novel process for the synthesis of binder-free, porous nickel/polythiophene-functionalized sulfur (Ni/S-PTh) composite cathodes for lithium–sulfur (Li–S) batteries is introduced in this paper. Initially, a polyvinyl butyl polymer scaffold is 3D printed, then coated with a graphite-based conducting layer, and, finally, it is pulse-plated for nickel deposition to produce a high-surface-area, mechanically stable current collector. S-PTh particles are afterwards co-deposited into the Ni matrix through composite electrodeposition. After the dissolution of the polymer template, the resulting self-standing electrodes still maintain porous structure with uniform sulfur distribution and a distinct transition between the dense Ni layer and the Ni/S-PTh composite layer. Electrochemical characterization of the Ni/S-PTh composite cathodes by galvanostatic cycling at C/10 rate results in an initial specific discharge capacity of ~1120 mAh·g⁻¹ and a specific capacity of ~910 mAh·g⁻¹ after 200 cycles, resulting in a high capacity retention of ~81 %. For our novel approach, no steps at high temperatures or toxic solvents are involved and the need for polymer binders and conductive additives is avoided. These results demonstrate the potential of composite electrodeposition in combination with 3D printing for producing sustainable, high-performance sulfur cathodes with tunable architecture. Full article

In this work, a comparative study of the corrosion resistance and microstructural characteristics of oxide coatings based on TiO₂ and TiO₂ + Cr₂ + Cr₂O₃ both deposited onto and without a tantalum sublayer has been carried out. The coatings were formed through thermal spraying, and their corrosion behaviour was evaluated through potentiodynamic polarisation in 3.5% NaCl solution using a potentiostat–galvanostat in a three-electrode cell. The TiO₂ + Cr₂O₃ composite coating, applied with a tantalum sublayer, had the lowest corrosion current density and the most positive corrosion potential, indicating its high corrosion resistance. The morphology and elemental composition of the coatings were analysed using scanning electron microscopy (SEM) and energy-dispersive analysis (EDX). The microstructural analysis revealed that the coatings with Cr₂O₃ added were characterised by an increased density, a more uniform phase distribution, and improved adhesion to the substrate. The obtained results confirm that combined TiO₂ + Cr₂O₃ coatings with a tantalum sublayer are promising for use in aggressive environments due to their high corrosion resistance and structural stability. Full article

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

TiO₂ composites with polypyrrole have gained attention for various applications; however, some reported results on the suitability of this heterojunction for photoelectrochemical water oxidation do not agree. In this sense, it is relevant to further study this material to clarify the role of polypyrrole in this system. Here, TiO₂ nanorods were grown on fluorine-doped tin oxide (FTO) substrates by a hydrothermal route; then, polypyrrole coatings were electrochemically synthetized on TiO₂ nanorods using a galvanostatic signal. The heterojunctions were characterized by different spectroscopic, microscopic, and electrochemical techniques. As a result, it was found that the polypyrrole underwent a rapid degradation process and that this process occurred independently of the amount of polymer deposited on the TiO₂, the illumination direction (back and front of the photoanode), and the type of light used (UV-Vis and Vis). In addition, from the measurements of the band positions of TiO₂ and the HOMO level of polypyrrole, it was shown that the TiO₂–polypyrrole heterojunction is not suitable for achieving the transfer of photogenerated holes to the electrolyte. These findings contribute to understanding the properties and interaction of two components of wide interest in materials science. Full article

In our study, supercapacitor electrodes were prepared by depositing electroless Ni-B coating on copper plates, followed by nitric acid etching. The composition and the micro- and phase structure of the coatings were investigated by ICP-OES, PFIB-SEM, and XRD techniques. The original pebble-like structure of the coating consists of 0.8–10 µm particles, with an X-ray amorphous phase structure. The surface morphology and porosity of the coating can be tuned simply by changing the etching time. The supercapacitive performance of the electrodes was evaluated by means of cyclic voltammetry, galvanostatic charge–discharge, and electrochemical impedance spectroscopy measurements. The capacitance of the coating was found to vary on the etching time according to a maximum function, allowing for the determination of an optimal duration to obtain a specific capacitance of 157 mF/cm² (at 0.5 A/g). An excellent charge storage retention of 178% was found after 5000 CV cycles at a scan rate of 50 mV/s owing to the evolved electrochemically active network on the surface of the electrode, indicating a long-term stable and reliable electrode. Full article

The galvanostatic electrodeposition of zinc on carbon paper from mildly acidic solutions (ZnCl₂: 0.05–0.1 M; H₃BO₃: 0.05 M) was investigated. The deposits’ growth mechanisms were analyzed through the study of the electrodeposition potential transients and the physical characterization of the electrodes synthesized by varying the current density, transferred charge, and zinc precursor concentration. The analysis reveals that the transition from crystalline to amorphous mossy deposits takes place via the electrodeposition of metallic zinc followed by the formation of oxidized zinc structures. The time required for this transition can be controlled by varying the zinc precursor concentration and electrodeposition current density, allowing for the synthesis of composite zinc/oxidized zinc electrodes with varying ratios of the oxidized to underlying metallic phases. The impact of this ratio on the electrode activity for CO₂ electroreduction is analyzed, highlighting that composite zinc/oxidized zinc electrodes can achieve a faradaic efficiency to CO equal to 82% at −1.8 V vs. Ag/AgCl. The mechanisms behind the variations in the catalytic activity with varying morphologies and structures are discussed, providing guidelines for the synthesis of composite zinc/oxidized zinc electrodes for CO₂ electroreduction. Full article

Sn-based anodes for lithium-ion batteries (LIBs) offer high capacity and low cost; however, significant volume changes during lithiation/delithiation cause mechanical degradation, limiting their practical applications. Microstructural control is a key approach to mitigating these volume changes. This study reports the fabrication of core (Sn rod)-shell (mesoporous Sn-oxide layer) structures through electrodeposition followed by anodization, and their applications to anode active materials for LIBs. First, micro-Sn rods with controlled lengths and diameters were fabricated under various electrodeposition conditions. The electrodeposited Sn exhibited a dendritic structure with short secondary rods branching from a long primary rod. While the primary Sn rod diameters remained constant, the secondary rod diameters varied depending on electrodeposition parameters. Notably, rod coarsening due to secondary rod agglomeration occurred at higher currents and longer deposition durations during galvanostatic electrodeposition. In contrast, potentiostatic electrodeposition prevented agglomeration and increased the quantity of Sn rods with voltage. Subsequently, the core-shell structures were fabricated by anodizing Sn rods, forming mesoporous Sn-oxide layers with different pore sizes and pore wall thicknesses. Electrochemical characterization revealed that the core-shell anode performance for LIBs varied with the Sn-oxide shell’s microstructure. These findings provide insights into optimal core-shell structures to improve anode performance for LIBs. Full article

This work successfully prepared the Co₃O₄ NPs via simple galvanostatic deposition followed by annealing at 400 and 800 °C for two hours. The galvanostatic deposition was carried out from a modified Watts bath. We used Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), energy dispersive X-ray (EDX), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) to examine the oxide’s characterization properties. The nature of the oxide formed was strongly dependent on the annealing temperature. The powder formed at room temperature (25 °C) is a mixture of Co(OH)₂ and metallic Co. However, at 400 and 800 °C, and according to the XRD patterns, the powder consists of the Co₃O₄ phase and a slight quantity of Co(OH)₂ phase. The average particle size measured by TEM ranged from 14.85 nm at room temperature to 90.19 nm at 800 °C. Moreover, the study examined how the operating deposition parameters affected the galvanostatic deposition process. Furthermore, these baths provide NPs, that demonstrate antibacterial activity against both Gram-positive (Staphylococcus aureus) and Gram-negative (Escherichia coli) bacteria as well as antifungal activity against Aspergillus niger. Full article

The galvanostatic electrodeposition of cobalt–nickel alloy coatings performed out on a 304 stainless steel substrate. The electrolyte baths contained metals salts, along with boric acid and sodium benzene sulfonate (SBS) as an organic additive in the deposition process. Structural and topographic analyses were performed using SEM-EDS and AFM techniques, respectively. The findings confirm the formation of nanostructured coatings. The images depicting various stages of coating formation indicated the inhibitory role of the organic additive. The presence of SBS enabled the formation of a coating composed of grains with diverse geometries and significantly reduced surface roughness. Hydrogen evolution was conducted in an alkaline environment (1 M NaOH). Overpotentials for the different structures were recorded at 10 mA/cm², yielding 196 mV and 225 mV for the coatings deposited with and without SBS, respectively. Additionally, experiments were performed in a laboratory-designed electrolyzer, which allowed for the measurement of gas volumes (H₂ and O₂) generated under constant voltage and current conditions. The results demonstrated that the obtained coatings perform more effectively as hydrogen evolution cathodes than currently used materials, particularly under higher current densities. Electrolysis was conducted for 8 h, revealing improved stability of the coating deposited in the presence of SBS. Full article

Platinum exhibits essential characteristics for enhancing electrochemical processes, but the use of electrodes made entirely of Pt is not cost-effective. A more affordable alternative is electrodepositing Pt black on accessible metallic surfaces, such as brass, to ensure that the electrodes are both resistant to corrosive environments and possess catalytic capabilities. Pourbaix and kinetic analyses were performed to establish the optimal potential and current conditions for electrodepositing Pt black on brass utilizing a Pb-free Pt solution. The Pourbaix analysis indicated that Pt electrodeposition is achieved from the PtCl₆⁻ ionic species and occurs before hydrogen evolution. Kinetic studies further revealed that Pt black nanoscale deposition on a brass surface requires mechanical surface treatment and electrochemical polishing, followed by metallic Pt electrodeposition under potentiostatic control at −295 mV vs. SCE. Subsequent Pt black deposition was achieved under galvanostatic control at −500 A cm⁻². Scanning electron microscopy (SEM) and X-ray diffraction (XRD) confirmed the formation of nanostructures of metallic Pt and Pt black on brass, with the latter presenting a larger surface area to enhance the active sites for catalysis in electrochemical processes. Full article

Through-Silicon-Via (TSV) technology is of crucial importance in the process of defect-free copper filling in vias. In this study, the small molecule 2-mercapto-1-methylimidazole (SN2) is proposed as a new leveler. It enables bottom-up super-filling of blind vias without the need for inhibitors. Atomic force microscopy (AFM), X-ray diffraction (XRD), and XPS were employed to characterize the surface morphology, crystal structure, and adsorption properties of copper crystals in these systems. Meanwhile, by means of electrochemical measurements, the inhibitory effect of the leveler SN2 on copper ion deposition and the synergistic effect between SN2 molecules and other additives were investigated. The LSV test indicated that additive SN2 inhibited copper electrodeposition after being added to the plating solution, and this inhibitory effect enhanced with increasing SN2 concentration. In the actual plating wafer test (1 ASD plating for 1 min, 5 ASD plating for 5 min, and 10 ASD plating for 1 h), the best plating effect was achieved at 3 ppm, which verified the conjecture of the galvanostatic measurements. Moreover, XPS and computer simulations revealed that SN2 could be adsorbed onto the copper surfaces. This work will inspire the discovery of new effective levelers in the future. Full article

This study investigates the properties of LiCoO₂ coatings as cathodes for lithium-ion batteries, focusing on the effects of annealing on their structural, morphological, chemical, vibrational, and electrochemical characteristics. The LiCoO₂ coatings were deposited on silicon and glass substrates using RF magnetron sputtering at 100 W and subsequently annealed at 600 °C for 1 h. The films were characterized before and after annealing using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and electrochemical impedance spectroscopy (EIS). Annealing improved the crystallinity of LiCoO₂, which is critical for enhancing lithium-ion diffusion. Furthermore, an XPS analysis revealed a layered structure with a Li-rich outer layer and a Co-rich underlayer, indicating a more uniform distribution of Li and Co, along with increased oxygen content. Additionally, the annealing process refined the microstructure of the LiCoO₂ coating, positively impacting its electrochemical performance. A comparative analysis of cyclic voltammetry (CV) and galvanostatic charge/discharge (GCD) results demonstrated a significant improvement in the charge/discharge capacity post-annealing. This study successfully highlights the beneficial effects of annealing on LiCoO₂ thin-film cathodes, offering valuable insights for developing more efficient and sustainable lithium-ion batteries through sputter-deposition processes. Full article

Boron nitride nanostructures (BNNs), including nanotubes, nanosheets, and nanoribbons, are renowned for their exceptional thermal stability, chemical inertness, mechanical strength, and high surface area, making them suitable for advanced material applications. Metal–organic frameworks (MOFs), characterized by their porous crystalline structures, high surface area, and tunable porosity, have emerged as excellent candidates for gas adsorption and storage applications, particularly in the context of hydrogen. This paper explores the synthesis and properties of BNNs and MOFs, alongside the innovative approach of integrating BNNs within MOFs to create composite materials with synergistic properties. The integration of BNNs into MOFs enhances the overall thermal and chemical stability of the composite while improving hydrogen sensing and storage performance. Various synthesis methods for both BNNs and MOFs are discussed, including chemical vapor deposition, solvothermal synthesis, and in situ growth, with a focus on their scalability and reproducibility. Furthermore, the mechanisms underlying hydrogen sensing and storage are examined, including physisorption, chemisorption, charge transfer, and work function modulation. Electrochemical characterization techniques, such as cyclic voltammetry, electrochemical impedance spectroscopy, and galvanostatic charge–discharge, are used to analyze the performance of BNN-MOF systems in hydrogen storage and sensing applications. These methods offer insights into the material’s electrochemical behavior and its potential to store hydrogen efficiently. Potential industrial applications of BNN-MOF composites are highlighted, particularly in fuel cells, hydrogen-powered vehicles, safety monitoring in hydrogen production and distribution networks, and energy storage devices. The integration of these materials can contribute significantly to the development of more efficient hydrogen energy systems. Finally, this study outlines key recommendations for future research, which include optimizing synthesis techniques, improving the hydrogen interaction mechanisms, enhancing the stability and durability of BNN-MOF composites, and performing comprehensive economic and environmental assessments. BNN-MOF composites represent a promising direction in the advancement of hydrogen sensing and storage technologies, offering significant potential to support the transition toward sustainable energy systems and hydrogen-based economies. Full article