One-step Electrochemical Synthesis Research Articles

One-Step Electrochemical Synthesis of Molybdenum-Disulfide-Based Materials for Enhanced Supercapacitor Performance

Molybdenum disulfide (MoS2)-based two-dimensional materials were produced in one-step at room temperature using cyclic voltammetry technique. These materials were then used as electrode materials in supercapacitors. Concentration of supporting electrolyte, precursor, and cycle number parameters, which were the factors affecting the success of the synthesis, were optimized as 0.5 M, 0.15 M,and 10 cycles, respectively. The produced MoS2-coated electrodes were characterized using spectroscopic and microscopic methods. The chemical characterizations of the produced materials were examined by X-ray photoelectron spectroscopy, X-ray diffraction diffractometry, and scanning electron microscopy-energy-dispersive X-ray analysis. Surface morphologies of the composite materials were investigated using scanning electron microscopy. Finally, the produced MoS2-based materials were used as electrode materials in supercapacitors. The produced supercapacitors were characterized using cyclic voltammetry and electrochemical impedance spectroscopy methods, and the changes in the capacitive behavior of these systems over cycles were investigated using the cyclic charge-discharge technique. The highest areal capacitance value was determined as 251 mF.cm−2 at 0.2 mA.cm−2 charge-discharge current rates in 1.0 M H2SO4 by using of MoS-AD1 as the electrode material. Capacitance retention of this electrode was over 100% after 4000 cycles.

One-Step Electrochemical Synthesis of Multiyolk-Shell Nanocoils for Exceptional Photocatalytic Performance.

Multiyolk-shell (mYS)nanostructures have garnered significant interest in various photocatalysis applications such as water splitting and waste treatment. Nonetheless, the complexity and rigorous conditions for the synthesis have hindered their widespread implementation. This study presents a one-step electrochemical strategy for synthesizing multiyolk-shell nanocoils (mYSNC), wherein multiple cores of noble metal nanoparticles, such as Au, are embedded within the hollow coil-shaped FePO4 shell structures, mitigating the challenges posed by conventional methods. By capitalizing on the dissimilar dissolution rates of bimetallic alloy nanocoils in an electrochemically programmed solution, nanocoils of different shapes and materials, including two variations of mYSNCs are successfully fabricated. The resulting Au-FePO4 mYSNCs exhibit exceptional photocatalytic performance for environmental remediation, demonstrating up to 99% degradation of methylene blue molecules within 50min and 95% degradation of tetracycline within 100min under ultraviolet-visible (UV-vis) light source. This remarkable performance can be attributed to the abundant electrochemical active sites, internal voids facilitating efficient light harvesting with coil morphology, amplified localized surface plasmon resonance (LSPR) at the plasmonic nanoparticle-semiconductor interface, and effective band engineering. The innovative approach utilizing bimetallic alloys demonstrates precise geometric control and design of intricate multicomponent hybrid composites, showcasing the potential for developing versatile hollow nanomaterials for catalytic applications.

Single step synthesis of β- and γ- aryl-substituted ß- and γ-amino acid derivatives by electrochemistry

Electrochemical transformations are a subject of increasing interest in early drug discovery due to its ability to assemble complex scaffolds under rather mild reaction conditions. In this context, we became interested in electrochemical decarboxylative cross-coupling (DCC) protocols of redox-active esters (RAEs) and halo(hetero)arenes. Starting with the one-step electrochemical synthesis of novel methylamino-substituted heterocycles we recognized the potential of this methodology to deliver a novel approach to β- and γ- amino acids by starting from the corresponding RAEs. Our work finally resulted in the delivery of novel and highly valuable trifunctional building blocks based on ß- and γ-amino-acid scaffolds.

Mg Electrodes Coiled with Cu Wires Promoted Formation of Diphenylacetylene from Tetrachloroethylene and Bromobenzene: One-step Electrochemical Synthesis without Pd Catalyst

Mg Electrodes Coiled with Cu Wires Promoted Formation of Diphenylacetylene from Tetrachloroethylene and Bromobenzene: One-step Electrochemical Synthesis without Pd Catalyst

One-step electrochemical synthesis of FTO/MnO2-graphene composite for electrochemical energy storage

The FTO/MnO2-Graphene composite was prepared using a one-step electrochemical approach employing chronoamperometry. Graphene was synthesized via electrochemical exfoliation and characterized using Raman spectroscopy and transmission electron microscopy (TEM).The prepared composite film exhibiting an extraordinary structure offers a large surface area provided with several channels to enhance the rapid diffusion of ions and electron transport owing to the grapheme sheets content. Various characteristics of the composite films have been investigated through X ray diffraction (XRD). Fourier transform infrared spectroscopy (FTIR), Field emission scanning electron microscopy (FESEM) and UV–Vis spectroscopy. To evaluate the electrochemical performance of the FTO/MnO2 and FTO/MnO2-GR films, cyclic voltammetry, electrochemical impedance spectroscopy (EIS), and galvanostatic charge-discharge tests were conducted. The specific capacitance was found at 5 mV·s−1, to be 192.3 F g−1 with graphene and 73.5 F g−1 without. This increase in capacitance upon incorporating grapheme sheets suggests that FTO/MnO2-GR composite film would have many potential applications as suitable materials for supercapacitor electrodes and energy storage devices. The FTO/MnO2-GR in a asymmetric supercapacitor demonstrated an excellent reversible operation, delivering an energy density of 3 W h kg−1 at a specific power of 25 W/ kg. Furthermore, even after 1000 cycles, the FTO/MnO2-GR asymmetric supercapacitor retains an impressive 99 % of its capacitance.

A Universal Electrochemical Synthetic Strategy for the Direct Assembly of Single-Atom Catalysts.

Single-atom catalysts (SACs) have been one of the frontiers in the field of catalysis in recent years owing to their high atomic utilization and unique electronic structure. To facilitate the practical application of single-atom, it is vital to develop a sustainable, facile single-atom preparation method with mass production potential. Herein, a universal one-step electrochemical synthesis strategy is proposed, and various metal-organic framework-supported SACs (including Pt, Au, Ir, Pd, Ru, Mo, Rh, and W) are straightforwardly obtained by simply replacing the guest metal precursors. As a proof-of-concept, the electrosynthetic Pt-based catalysts exhibit outstanding activity and stability in the electrocatalytic hydrogen evolution reaction (HER). This study not only enriches the single-atom synthesis methodology, but also extends the scenario of electrochemical synthesis, opening up new avenues for the design of advanced electro-synthesized catalysts.

One-Step Plasma-Assisted Electrochemical Synthesis of Nanocomposites of Few-Layer Graphene Structures with Manganese Oxides as Electrocatalysts for Oxygen Reduction Reaction

Using the method of plasma-assisted electrochemical exfoliation of graphite, a nanocomposite, which consists of few-layer graphene structures with surface decorated with manganese oxides nanoparticles, is synthesized in one-step process. It is found that this material exhibits a high electrocatalytic activity towards the oxygen reduction reaction due to the presence of manganese in the +2 and +3 oxidation states, and also carbonyl (quinone) functional groups on the surface of graphene structures.

One-Step Plasma-Assisted Electrochemical Synthesis of Nanocomposites of Few-Layer Graphene Structures with Manganese Oxides as Electrocatalysts for Oxygen Reduction Reaction

One-Step Plasma-Assisted Electrochemical Synthesis of Nanocomposites of Few-Layer Graphene Structures with Manganese Oxides as Electrocatalysts for Oxygen Reduction Reaction

One-Step Electrochemical Synthesis of AlO x -Passivated Twisted-Phosphorene Nanosheets for Potentially Stable Energy Storage Devices.

Black phosphorus (BP), a promising 2D material for electronics, energy storage, catalysis, and sensing, has sparked a research boom. However, exfoliated thin-layered BP is unstable and can easily be degraded under environmental conditions, severely limiting its practical applications. In this context, a simple and cost-effective method has been proposed that involves electrochemically exfoliating BP and simultaneously electrochemically depositing aluminum oxide (AlO x ) for passivation of the exfoliated BP. The ambient stability of the exfoliated BP is studied using a time-dependent atomic force microscope (AFM). The AlO x capping layer significantly improves the environmental stability of BP compared to uncapped BP. The thermal stability of the resulting BP is evaluated using power-dependent Raman spectroscopy. The results show that the AlO x -passivated BP has increased thermal stability, with only a slight shift in peak position toward higher Raman power intensity. These properties can make the material suitable for stable energy storage devices. Interestingly, the electrochemical exfoliation and passivation processes resulted in the BP with a twist angle (9.86°), which is expected to exhibit unique electronic properties similar to those of graphene with a twist angle.

Conductive Additives for Improving the Rate Capability of Cathode Materials in Secondary Lithium Batteries

Conductive additive, one of the most important components of a battery, is an indispensable key material in the high-current charging and discharging processes of lithium-ion batteries. The most fundamental reason for adding appropriate conductive additives in the electrode is to improve the poor conductive performance of the electrode-active material, reduce the internal resistance and polarization of the electrode, and improve the comprehensive performance of the battery. Herein, a graphene-like material with a unique two-dimensional morphology was proposed, as obtained by an efficient one-step electrochemical synthesis, which can provide a flexible plane-to-point conducting network to improve the electronic conductivity of cathode materials. Compared with the commercial conductive additive Super P, the NCM811 cathode material with ECGO can deliver a capacity of 147.3 mAh g–1 at a high rate of 2 C, and sulfur cathode retains 620 mAh g–1 after 200 cycles, corresponding to the capacity retention of 74%. Also, due to the presence of oxygen groups, ECGO is proposed as an effective conductive additive in Li-ion cathodes prepared by water-based processing. Therefore, the cathode materials with the ECGO conductive additive can contribute to reduce the interfacial resistance and increase the capability, showing great advantages compared to the commercial conductive additives.

One-Step Electrochemical Synthesis and Surface Reconstruction of NiCoP as an Electrocatalyst for Bifunctional Water Splitting.

We adopted a simple one-step electrochemical deposition to acquire an efficient nickel cobalt phosphorus (NiCoP) catalyst, which avoided the high temperature phosphatization engineering involved in the traditional synthesis method. The effects of electrolyte composition and deposition time on electrocatalytic performance were studied systematically. The as-prepared NiCoP achieved the lowest overpotential (η10 = 111 mV in the acidic condition and η10 = 120 mV in the alkaline condition) for the hydrogen evolution reaction (HER). Under 1 M KOH conditions, optimal oxygen evolution reaction (OER) activity (η10 = 276 mV) was also observed. Furthermore, the bifunctional NiCoP catalyst enabled a high-efficiency overall water-splitting by applying an external potential of 1.69 V. The surface valence and structural evolution of NiCoP samples with slowly decaying stability under alkaline conditions are revealed by XPS. The NiCoP is reconstructed into the Ni(Co)(OH)2 (for HER) and Ni(Co)OOH (for OER) on the surface with P element loss, acting as real "active sites".

One-step synthesis of PtNi anchored on TiO2 nanotube arrays for methanol oxidation

Highly active, stable, economic friendly electrocatalysts play a crucial role for the commercialization of direct methanol fuel cells (DMFCs). One kind of flower-like PtNi bimetallic particle anchored on TiO2 nanotube arrays (PtNi/TNTs/Ti) had been synthesized by one-step electrochemical synthesis as anode catalysts for methanol oxidation reaction (MOR) in this study. The PtNi/TNTs/Ti electrode demonstrated high electrocatalytic activity and durability significantly for MOR. In addition, PtNi100/TNTs/Ti possessed a mass activity of 409.8 mA/mgpt, which was four times greater than that of Pt100/TNTs/Ti electrodes. According to further structure analysis, the improvement in catalytic activity was attributed to lattice compression when Ni atoms entered the Pt lattice accompanied by a 1.02 eV positive shift in Pt 4 f7/2 binding energy, and density functional theory (DFT) calculations indicated that the remarkably enhanced catalytic performance on PtNi through lattice compression arising from the enhanced OH adsorption. It appears promising that this simple method could be adopted to prepare an integrated electrode used as energy and environmental applications.

A facile one-step electrosynthesis of polypyrrole/nano-SbOx composite for supercapacitors

The study depicts a one-step electrochemical synthesis of composite based on polypyrrole (PPy) and SbOx (Sb2O3, Sb2O5) on the graphite surface for the supercapacitor electrode in an acetonitrile solution including pyrrole monomer and Sb(BF4)3. PPy/SbOx composite on graphite plate is characterized using XPS, XRD, TEM, BET, and FESEM by comparing it with PPy homopolymer prepared in the same way. SbOx forms in nano-size and homogeneously encapsulates in PPy due to their simultaneous synthesis. The average pore size of the composite coating is 23.9 nm. The coated PG electrodes are tested in an H2SO4 electrolyte using CV, EIS, and GCD methods. SbOx nanoparticles enhance the capacitive performance of PPy due to the contribution of its catalytic and pseudocapacitive properties. The specific capacitance of the PPy/SbOx-coated PG electrode is 389.5 F g−1 at 5 A g−1 for 1.0 mg cm−2 loading. PPy/SbOx is synthesized in the presence of carboxymethyl cellulose (CMC) to provide stability to the coating. An asymmetric supercapacitor cell is fabricated by assembling the PPy/SbOx/CMC-coated and activated carbon-based graphite paper electrodes (10 mg cm−2 loading). While the potential window expands to 1.4 V, it delivers an energy density of 8.3 Wh kg−1, a power density of 3.5 kW kg−1, and a coulombic efficiency of 90% at 5 A g−1. Post-mortem analysis reveals that structural degradation of PPy in the composite limits long-term stability.

Facile fabrication of superhydrophobic coatings with superior corrosion resistance on LA103Z alloy by one-step electrochemical synthesis

Superhydrophobic coatings are effective in avoiding corrosion of substrates due to their special wetting properties. The present work dispenses with the need for complex pre-treatments and post-modification with low surface energy substances. A facile and rapid one-step electrochemical synthesis method was used to prepare a superhydrophobic coating of [CH3(CH2)12COO]2Ca with excellent corrosion resistance on the surface of LA103Z alloy. The corrosion behavior of the coated alloy in 3.5 wt% NaCl solution was investigated using electrochemical techniques. The results show that a uniform and relatively thick surface is an effective barrier to the penetration of corrosive liquids. The best corrosion resistance of the coated samples was achieved at an electrochemical synthesis time of 30 min, with a positive shift in corrosion potential and a significant reduction in corrosion current density.

One-step electrochemical synthesis and optimization of Sb-Co-P alloy anode for sodium ion battery

The Sb-Co-P anode prepared successfully through the low-cost electrodeposition method was examined to be a feasible and effective anode for sodium ion batteries. Under specified conditions, Sb21.0Co46.9P32.1 showed a high reversible charging capacity of 586.3 mAh∙g−1, with an initial coulombic efficiency of 84.4% and a capacity retention rate of 77.6% after 100 cycles. The improved electrochemical performance of the optimized Sb21.0Co46.9P32.1 anode is mainly due to the "active-inactive-active" matrix and its unique leaf-shaped cluster structure. Furthermore, the reaction mechanism of sodium storage was revealed by in situ X-ray diffraction. This work provides a potential opportunity for the scalable fabrication of Sb-based alloys for high-performance sodium-ion batteries.

One-Step Regio- and Stereoselective Electrochemical Synthesis of Orexin Receptor Antagonist Oxidative Metabolites.

Synthesis of drug metabolites, which often have complex structures, is an integral step in the evaluation of drug candidate metabolism, pharmacokinetic (PK) properties, and safety profiles. Frequently, such synthetic endeavors entail arduous, multiple-step de novo synthetic routes. Herein, we present the one-step Shono-type electrochemical synthesis of milligrams of chiral α-hydroxyl amide metabolites of two orexin receptor antagonists, MK-8133 and MK-6096, as revealed by a small-scale (pico- to nano-mole level) reaction screening using a lab-built online electrochemistry (EC)/mass spectrometry (MS) (EC/MS) platform. The electrochemical oxidation of MK-8133 and MK-6096 was conducted in aqueous media and found to produce the corresponding α-piperidinols with exclusive regio- and stereoselectivity, as confirmed by high-resolution nuclear magnetic resonance (NMR) characterization of products. Based on density functional theory (DFT) calculations, the exceptional regio- and stereoselectivity for this electrochemical oxidation are governed by more favorable energetics of the transition state, leading to the preferred secondary carbon radical α to the amide group and subsequent steric hindrance associated with the U-shaped conformation of the cation derived from the secondary α-carbon radical, respectively.

A novel and ultrasensitive non-enzymatic electrochemical glucose sensor in real human blood samples based on facile one-step electrochemical synthesis of nickel hydroxides nanoparticles onto a three-dimensional Inconel 625 foam

A novel and ultrasensitive non-enzymatic electrochemical glucose sensor in real human blood samples based on facile one-step electrochemical synthesis of nickel hydroxides nanoparticles onto a three-dimensional Inconel 625 foam

One-Step Electrochemical Synthesis of Co0.8Fe0.2Se@NiF Spheres Enclosed with Nanoparticles and Integrated Porous FeSe2@NiF as Electrode Materials for High-Performance Asymmetric Supercapacitor

Herein, we offer a new method to prepare Co0.8Fe0.2Se spheres enclosed with nanoparticles (Co0.8Fe0.2Se@NiF) as a cathode electrode and integrated porous FeSe2 (FeSe2@NiF) as an anode electrode to construct a high-performance asymmetric supercapacitor. The Co0.8Fe0.2Se@NiF electrochemical energy storage material shows a remarkable improvement of electrochemical performance containing low internal resistance, fast kinetics, good reversibility, considerable durability, and significant specific capacity (SC) of 309.31 mAh g–1. The advancement in electrochemical performance of the FeSe2@NiF subtends a good SC of 227.34 mAh g–1 and favorable durability. An asymmetric supercapacitor (ASC) device comprised of Co0.8Fe0.2Se@NiF as a cathode and FeSe2@NiF as an anode was assembled and evaluated. The assembled device shows an SC of 108.52 mAh g–1 and energy density (ED) of 89.53 Wh kg1– at a power density (PD) of 824.95 W kg1–. This improved electrochemical performance is dependent on the structural and intrinsic properties of both electrode materials, which can guarantee a hopeful potential for later generations of electronic systems.

One-step electrochemical synthesis of γ-Fe2O3@MIL-88a magnetic composite for heterogeneous Fenton-like catalysis

We report a new one-step room-temperature electrochemical synthesis of γ-Fe2O3@MIL-88a magnetic composite. Anode from metallic iron was used as Fe-source. We did not use any toxic or hazardous solvents. A careful, comprehensive characterization of the obtained material was applied, including a synchrotron experiment. The γ-Fe2O3@MIL-88a composite comprised diamond-like MIL-88a crystals of 100–300 nm covered with γ-Fe2O3 nanoparticles. This component provided a magnetic response to the synthesized material. Moreover, γ-Fe2O3 nanoparticles boosted semiconductor MOF crystals. As a result, the γ-Fe2O3@MIL-88a composite demonstrated superior photocatalytic performance toward methylene blue degradation. MIL-88a crystals acted as photo-Fenton catalysts activating H2O2 decomposition with the production of active •OH radicals. Easy magnetic separation and visible-light activated photocatalytic properties make γ-Fe2O3@MIL-88a composite a promising system for removing organic dyes from contaminated water according to the photo-Fenton process.

One-step electrochemical synthesis of tremella-like Co-MOFs/carbon nanohorns films for enhanced electrochemical sensing of carbendazim in vegetable and fruit samples

• Co-MOFs/CNHs/GCE was synthesized by one-step electrochemical co-deposition method. • Co-MOFs/CNHs/GCE was used as electrochemical sensor for sensitively detecting CBZ. • The sensor showed excellent electrocatalytic activity for CBZ oxidation. • Low detection limit of 0.2 nM and wide linear range were obtained. • The method was successfully employed for CBZ detection in real samples. Pesticides play a vital part in agricultural production, which can effectively prevent and control crop diseases and pests. However, the extensive use can impose a serious risk to human fitness and the surroundings worldwide. Herein, a novel electrochemical strategy was proposed for sensitive detection of carbendazim (CBZ) based on Co-MOFs/carbon nanohorns (Co-MOFs/CNHs, BDC stands for 1,4-benzenedi-carboxylate) sensing platform. Tremella-like Co-MOFs/CNHs films were synthesized via a facile, mild one-step electrochemical co-deposition technique. Inter-connected Co-MOFs sheets present high surface area, giant pore quantity and plentiful active sites, which exhibit high enrichment capacity for CBZ. Meanwhile, CNHs attached Co-MOFs sheets own superior electrocatalytic properties, and electronic conductivity, which could promote the electrooxidation towards the adsorbed CBZ molecules. Attributing to these impressive features, the electrochemical signals of CBZ are greatly amplified at Co-MOFs/CNHs electrode. A low limit of detection (LOD) of 0.2 nM, and wide linear range from 0.5 nM to 20.0 µM are achieved. Additionally, the prepared sensor was also utilized for the detection of CBZ in strawberries and cabbage with the recovery ranging from 97.25% to 103.5%.