Search Results (526)

Films of a Ni/Al-layered double hydroxide intercalated with reduced graphene oxide were deposited, by means of a simple and rapid electrochemical synthesis, on Pt electrodes previously submitted to a special cleaning procedure. The aim of the research was to determine whether the better electrocatalytic properties of the Ni(III)/Ni(II) couple, due to the presence of the carbon nanomaterial, as compared to the Ni/Al-LDH alone, could allow glucose detection at physiological pHs, as normally LDHs work as redox mediators in basic solutions. Chronoamperometric experiments were carried out by applying a potential of 1.0 V vs. SCE to the electrode soaked in solutions buffered at pHs from 5.0 to 9.0 to which glucose was continuously added. The steady-state currents increased as the pH solution increased, but at pH = 7.0 the modified electrode exhibited a fast and rather sensitive response, which was linear up to 10.0 mM glucose, with a sensitivity of 0.56 A M⁻¹ cm⁻² and a limit of detection of 0.05 mM. Our results suggest the potential application of Ni/Al-LDH(ERGO) composite for the non-enzymatic detection of glucose or other oxidizable analytes under biological conditions. Full article

The oxygen evolution reaction (OER) plays a central role as an anode in electrocatalytic processes such as energy conversion and storage and the generation of molecular oxygen from the electrolysis of water. Currently, precious metal oxides such as IrO₂ and RuO₂ are recognized as reference OER electrocatalysts with reasonably high activity; however, their widespread use in practical devices has been severely hindered by their high cost and scarcity. It is essential to design alternative OER electrocatalysts made of low-cost and abundant earth elements with significant activity and robustness. We report four new nanocellulose-derived Fe–zeolite nanocomposites, namely Fe/Zeolite@CCNC (1), Fe/Zeolite@CCNF (2), Fe/Zeolite/CNT@CCNC (3), and Fe/Zeolite/CNT@CCNF (4). Two different types of nanocellulose were investigated: nanocellulose nanofibrils and nanocellulose nanocrystals. Characterization with TEM, SEM-EDS, PXRD, and XPS is reported. The nanocomposites exhibited electrocatalytic activity for OER that varies based on the origin of biocarbon and the composition content. The effect of adding carbon nanotubes to the nanocomposites was studied, and an improvement in OER catalysis was observed. The electrochemical double-layer capacitance and electrochemical impedance spectroscopy of the nanocomposites are reported. The nanocomposite 3 exhibited the highest performance, with an onset potential value of 1.654 V and an overpotential of 551 mV, which exceeds the activity of RuO₂ for OER catalysis at 10 mA/cm² in the glassy carbon electrode. A 24 h chronoamperometry study revealed that the catalyst is active for ~2 h under continuous operating conditions. BET surface analysis showed that the crystalline nanocellulose-derived composite exhibited 301.47 m²/g, and the fibril nanocellulose-derived composite exhibited 120.39 m²/g, indicating that the increased nanoporosity of the former contributes to the increase in OER catalysis. Full article

This review article compiled previous reports in the fabrication of hydroquinone (HQ) electrochemical sensors using differently modified electrodes. The electrode materials, which are also called electrocatalysts, play a crucial role in electrochemical detection of biomolecules and toxic substances. Metal oxides, MXenes, carbon-based materials such as reduced graphene oxide (rGO), carbon nanotubes (CNTs), layered double hydroxides (LDH), metal sulfides, and hybrid composites were extensively utilized in the fabrication of HQ sensors. The electrochemical performance, including limit of detection, linearity, sensitivity, selectivity, stability, reproducibility, repeatability, and recovery for real-time sensing of the HQ sensors have been discussed. The limitations, challenges, and future directions are also discussed in the conclusion section. It is believed that the present review article may benefit researchers who are involved in the development of HQ sensors and catalyst preparation for electrochemical sensing of other toxic substances. Full article

Recently, it has been found that electrochemical sensing technology is one of the significant approaches for the monitoring of toxic and hazardous substances in food and the environment. Nitrofurazone (NFZ) and nitrofurantoin (NFT) possess a hazardous influence on the environment, aquatic life, and human health. Thus, various advanced materials such as graphene, carbon nanotubes, metal oxides, MXenes, layered double hydroxides (LDHs), polymers, metal–organic frameworks (MOFs), metal-based composites, etc. are widely used for the development of nitrofurazone and nitrofurantoin sensors. This review article summarizes the progress in the fabrication of electrode materials for nitrofurazone and nitrofurantoin sensing applications. The performance of the various electrode materials for nitrofurazone and nitrofurantoin monitoring are discussed. Various electrochemical sensing techniques such as square wave voltammetry (SWV), differential pulse voltammetry (DPV), linear sweep voltammetry (LSV), amperometry (AMP), cyclic voltammetry (CV), and chronoamperometry (CA) are discussed for the determination of NFZ and NFT. It is observed that DPV, SWV, and AMP/CA are more sensitive techniques compared to LSV and CV. The challenges, future perspectives, and limitations of NFZ and NFT sensors are also discussed. It is believed that present article may be useful for electrochemists as well materials scientists who are working to design electrode materials for electrochemical sensing applications. Full article

In this investigation, a hierarchical FeCo-layered double hydroxide (FeCo-LDH) electrochemical membrane material was prepared by a simple in situ hydrothermal method. The prepared material formed a 3D honeycomb-structured FeCo-LDH-modified carbon felt (FeCo-LDH/CF) catalytic layer with uniform open pores on a CF substrate with excellent catalytic activity and was served as the cathode in a flow-through electro-Fenton (FTEF) reactor. The electrocatalyst demonstrated excellent treatment performance (99%) in phenol simulated wastewater (30 mg L⁻¹) under the optimized operating conditions (applied voltage = 3.5 V, pH = 6, influent flow rate = 15 mL min⁻¹) of the FTEF system. The high removal rate could be attributed to (i) the excellent electrocatalytic oxidation performance and low interfacial charge transfer resistance of the FeCo-LDH/CF electrode as the cathode, (ii) the ability of the synthesized FeCo-LDH to effectively promote the conversion of H₂O₂ to •OH under certain conditions, and (iii) the flow-through system improving the mass transfer efficiency. In addition, the degradation process of pollutants within the FTEF system was additionally illustrated by the •OH dominant ROS pathway based on free radical burst experiments and electron paramagnetic resonance tests. This study may provide new insights to explore reaction mechanisms in FTEF systems. Full article

Electrocatalytic urea oxidation reaction (UOR) is a promising dual-purpose approach for hydrogen production and wastewater treatment, addressing critical energy and environmental challenges. However, conventional anode materials often suffer from limited active sites and high charge transfer resistance, restricting UOR efficiency. To overcome these issues, a novel NiP@PNC/NF electrocatalyst was developed via a one-step thermal annealing process under nitrogen, integrating nickel phosphide (NiP) with phosphorus and nitrogen co-doped carbon nanotubes (PNCs) on a nickel foam (NF) substrate. This design enhances catalytic activity and charge transfer, achieving current densities of 50 mA cm⁻² at 1.34 V and 100 mA cm⁻² at 1.43 V versus the reversible hydrogen electrode (RHE). The electrode’s high electrochemical surface area (235 cm²) and double-layer capacitance (94.1 mF) reflect abundant active sites, far surpassing NiP/NF (48 cm², 15.8 mF) and PNC/NF (39.5 cm², 12.9 mF). It maintains exceptional stability, with only a 16.3% performance loss after 35 h, as confirmed by HR-TEM showing an intact nanostructure. Our single-step annealing technique provides simplicity, scalability, and efficient integration of NiP nanoparticles inside a PNC matrix on nickel foam. This method enables consistent distribution and robust substrate adhesion, which are difficult to attain with multi-step or more intricate techniques. Full article

Magnesium alloys are lightweight metals but suffer from high corrosion susceptibility due to their chemical reactivity, limiting their large-scale applications. To enhance corrosion resistance, this work combines Li–Al layered double hydroxides (LDHs) with triethylenetetramine (TETA) inhibitors to form an efficient corrosion protection system. Electrochemical tests, SEM, FT-IR, XPS, and 3D depth-of-field microscopy were employed to evaluate TETA-modified Li–Al LDH coatings at varying concentrations. Among them, the Li–Al LDHs without the addition of a TETA corrosion inhibitor decreased significantly at |Z|_{0.01 Hz} after immersion for 4 h. However, the Li–Al LDHs coating of 23.5 mM TETA experienced a sudden drop at |Z|_{0.01 Hz} after holding for about 60 h, and the Li–Al LDHs coating of 70.5 mM TETA also experienced a sudden drop at |Z|_{0.01 Hz} after holding for about 132 h. By contrast, at the optimal concentration (47 mM), after 24 h of immersion, the maximum |Z|_{0.01 Hz} reached 7.56 × 10⁵ Ω∙cm²—three orders of magnitude higher than pure Li–Al LDH coated AZ31 (2.55 × 10² Ω∙cm²). After 300 h of immersion, the low-frequency impedance remained above 10⁵ Ω∙cm², demonstrating superior long-term protection. TETA modification significantly improved the durability of Li–Al LDHs coatings, addressing the short-term protection limitation of standalone Li–Al LDHs. Li–Al LDHs themselves have a layered structure and effectively capture corrosive Cl⁻ ions in the environment through ion exchange capacity, reducing the corrosion of the interface. Furthermore, TETA exhibits strong adsorption on Li–Al LDHs layers, particularly at coating defects, enabling rapid barrier formation. This inorganic–organic hybrid design achieves defect compensation and enhanced protective barriers. Full article

The oxygen-evolving IrO₂-Ta₂O₅/Ti anode (OEA), primarily used in electrolyzers for plating, metal powder production, electrowinning (EW), and water electrolysis, is analyzed. This study focuses on the distribution of oxygen evolution reaction (OER) activity and the associated operational loss over the randomized OEA texture. The OER activity and its distribution across the IrO₂-Ta₂O₅ coating surface are key factors that influence EW operational challenges and the lifecycle of OEA in EW processes. To understand the OER activity distribution over the coating’s randomized texture, we performed analyses using anode polarization in acid solution at both low and high (EW operation relevant) overpotentials and electrochemical impedance spectroscopy (EIS) during the OER. These measurements were conducted on anodes in both their as-prepared and deactivated states. The as-prepared anode was deactivated using an accelerated stability test in an acid solution, the EW simulating electrolyte. The obtained data are correlated with fundamental electrochemical properties of OEA, such as structure-related pseudocapacitive responses at open circuit potential in the same operating environment. OER and Ir dissolution kinetics, along with the physicochemical anode state upon deactivation, are clearly characterized based on current and potential dependent charge transfer resistances and associated double layer capacitances obtained by EIS. This approach presents a useful tool for elucidating, and consequently tailoring and predicting, anode OER activity and electrolytic operational stability in industrial electrochemical applications. Full article

Transition metal oxides (TMOs) are considered to be highly promising materials for supercapacitor electrodes due to their low cost, multiple convertible valence states, and excellent electrochemical properties. However, inherent limitations, including restricted specific surface area and low electrical conductivity, have largely restricted their application in supercapacitors. In this paper, core–shell heterostructures of nickel–iron layered double hydroxide (NiFe-LDH) nanosheets uniformly grown on CuCo₂O₄ nanoneedles were synthesized by hydrothermal and calcination methods. It is found that the novel core–shell structure of CuCo₂O₄@NiFe-LDH improves the electrical conductivity of the electrode materials and optimizes the charge transport path. Under the synergistic effect of the two components and the core–shell heterostructure, the CuCo₂O₄@NiFe-LDH electrode achieves an ultra-high specific capacity of 323.4 mAh g⁻¹ at 1 A g⁻¹. And the capacity retention after 10,000 cycles at 10 A g⁻¹ is 90.66%. In addition, the assembled CuCo₂O₄@NiFe-LDH//RGO asymmetric supercapacitor device achieved a considerable energy density (68.7 Wh kg⁻¹ at 856.3 W kg⁻¹). It also has 89.36% capacity retention after 10,000 cycles at 10 A g⁻¹. These properties indicate the great potential application of CuCo₂O₄@NiFe-LDH in the field of high-performance supercapacitors. Full article

Noise reduction is essential in analyzing electrochemical impedance spectroscopy (EIS) data for accurate parameter identification of models of electrochemical sources and interfaces. EIS is widely used to study the behavior of electrochemical systems as it provides information about the processes occurring at electrode surfaces. However, measurement noise can severely compromise the accuracy of parameter identification and the interpretation of EIS data. This paper presents methods for parameter identification of Randles (also known as R-RC or 2R-1C) equivalent electrical circuits and noise reduction in EIS data using recursive filtering. EIS data obtained at the estimated characteristic frequency is processed with three equations in the closed form for the parameter estimation of series resistance, charge transfer resistance, and double-layer capacitance. The proposed recursive filter enhances estimation accuracy in the presence of random noise. Filtering is embedded in the estimation procedure, while the optimal value of the recursive filter weighting factor is self-tuned based on the proposed search method. The distinguished feature is that the proposed method can process EIS data and perform estimation with filtering without any input from the user. Synthetic datasets and experimentally obtained impedance data of lithium-ion batteries were successfully processed using PC-based and microcontroller-based systems. Full article

To achieve efficient preparation of microfine tool electrodes with a large aspect ratio, a bipolar pulse vertical liquid membrane electrochemical etching technique was proposed. The difference in current density distribution on the surface of tungsten rods under single-ended and double-ended vertical liquid membrane methods was analyzed using COMSOL software. The effects of negative voltage and pulse width on the distribution of electrolytic products and electrode preparation were investigated. It was found that when a large number of hydrogen bubbles were generated on the surface of the electrode, the electrode lost the protection of the diffusion layer, and the length was drastically shortened. When the pulse width was large, the electrode surface was covered with a coating layer of insoluble electrolysis product, and the shortening of electrode length was suppressed. Subsequently, the effects of forward voltage and bias on electrode preparation were investigated for large pulse widths. The optimal parameters are as follows: electrolyte concentration of 0.5 M, forward voltage of 4 V, negative voltage of −2 V, pulse period of 50 microseconds, and pulse width of 40 microseconds. Finally, the tool electrode with an average diameter of about 23.8 μm and an aspect ratio of 91.2 was prepared. Full article

Carbon nanofibrous materials from electrospinning are good candidate electrode materials for supercapacitor applications due to their straightforward processability, chemical stability, high porosity, and large surface area. In this research, a straightforward and effective way was revealed to significantly enhance the electrochemical performance of carbon nanofibrous electrode material from electrospinning of polyacrylonitrile (PAN). Fluorination of the electrospun carbon nanofibers (ECNF) was studied by comparing two types of hydrofluoric acid (HF) treatment, i.e., direct HF acid treatment on ECNF (Type I) vs. HF acid treatment on the stabilized PAN (Type II) followed by carbonization. The latter was found to be an advantageous way to introduce C-F bonds in the resultant carbon nanofibrous electrode material that contributed to pseudocapacitance. Furthermore, the Type II HF acid treatment demonstrated exciting synergistic effects with ECNF aerogel formation on carbon structure and porosity development and generated a superior fluorinated electrospun carbon nanofibrous aerogel (ECNA-F) electrode material for supercapacitor uses. The resultant ECNA-F electrode material demonstrated excellent electrochemical performance with great cyclic stability due to the large improvements in both pseudocapacitance and electrical double-layer capacitance. ECNA-F achieved a specific capacitance of 372 F/g at a current density of 0.5 A/g with 1 M H₂SO₄ electrolyte, and the device with ECNA-F and 1 M Na₂SO₄ electrolyte possessed an energy density of 29.1 Wh/kg at a power density of 275 W/kg. This study provided insight into developing high-performance and stable carbon nanofibrous electrode materials for supercapacitors. Full article

Layered double hydroxides (LDHs), notable for their unique two-dimensional layered structures, have attracted significant research attention due to their exceptional versatility and promising performance in energy storage and conversion applications. This comprehensive review systematically addresses the fundamentals and diverse synthesis strategies for LDHs, including co-precipitation, hydrothermal synthesis, electrochemical deposition, sol-gel processes, ultrasonication, and exfoliation techniques. The synthesis methods profoundly influence the physicochemical properties, morphology, and electrochemical performance of LDHs, necessitating a detailed understanding to optimize their applications. In this paper, the role of LDHs in batteries, supercapacitors, and hydrogen production is critically evaluated. We discuss their incorporation in various battery systems, such as lithium-ion, lithium–sulfur, sodium-ion, chloride-ion, zinc-ion, and zinc–air batteries, highlighting their structural and electrochemical advantages. Additionally, the superior pseudocapacitive behavior and high energy densities offered by LDHs in supercapacitors are elucidated. The effectiveness of LDHs in hydrogen production, particularly through electrocatalytic water splitting, underscores their significance in renewable energy systems. This review paper uniquely integrates these three pivotal energy technologies, outlining current innovations and challenges, thus fulfilling a critical need for the scientific community by providing consolidated insights and guiding future research directions. Full article

Developing efficient bifunctional electrocatalysts with excellent stability at high current densities for overall water splitting is a challenging yet essential objective. However, transition metal phosphides encounter issues such as poor dispersibility, low specific surface area, and limited electronic conductivity, which hinder the achievement of satisfactory performance. Therefore, this study presents the highly efficient bifunctional electrocatalyst of CeO₂-modified NiFe phosphide on nickel foam (CeO₂/Ni₂P/Fe₂P/NF). Ni₂P/Fe₂P coupled with CeO₂ was deposited on nickel foam through hydrothermal synthesis and sequential calcination processes. The electrocatalytic performance of the catalyst was evaluated in an alkaline solution, and it exhibited an HER overpotential of 87 mV at the current density of 10 mA cm⁻² and an OER overpotential of 228 mV at the current density of 150 mA cm⁻². Furthermore, the catalyst demonstrated good stability, with a retention rate of 91.2% for the HER and 97.3% for the OER after 160 h of stability tests. The excellent electrochemical performance can be attributed to the following factors: (1) The interface between Ni₂P/Fe₂P and CeO₂ facilitates electron transfer and reactant adsorption, thereby improving catalytic activity. (2) The three-dimensional porous structure of nickel foam provides an ideal substrate for the uniform distribution of Ni₂P, Fe₂P, and CeO₂ nanoparticles, while its high conductivity facilitates electron transport. (3) The incorporation of larger Ce³⁺ ions in place of smaller Fe³⁺ ions leads to lattice distortion and an increase in defects within the NiFe-layered double hydroxide structure, significantly enhancing its catalytic performance. This research finding offers an effective strategy for the design and synthesis of low-cost, high-potential catalysts for water electrolysis. Full article

Producing hydrogen by water electrolysis has attracted significant attention as a potential renewable energy solution. In this work, a catalyst with reduced graphene oxide (rGO) loaded on IrO₂/TiO₂ (called rGO/IrO₂/TiO₂) was designed for the catalytic oxygen evolution reaction (OER). The catalyst was synthesized by coating graphene oxide onto a pretreated IrO₂/TiO₂ precursor, followed by thermal treatment at 450 °C to achieve reduction and the adhesion of graphene to the substrate. The graphene support retained its intact sp² carbon framework with minor oxygen-containing functional groups, which enhanced electrical conductivity and hydrophilicity. Benefiting from the synergistic effect of an rGO, IrO₂, and TiO₂ matrix, the rGO/IrO₂/TiO₂ catalyst only needed overpotentials of 240 mV and 320 mV to reach 10 mA cm⁻² and 100 mA cm⁻² in the OER, along with excellent stability over 50 h. Its morphology and crystalline structure were characterized by SEM and XRD spectroscopy, and its electrochemical performance was tested by LSV analysis, EIS impedance spectrum, and double-layer capacitance (C_dl) measurements. This work introduces an innovative and eco-friendly strategy for constructing a high-performance, functionalized Ir-based catalyst. Full article