Search results for: electrochemical properties

Authors: Maria Sofia Palagonia, Doriano Brogioli, Fabio La Mantia

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In the last decade, lithium has become an important raw material in various sectors, in particular for rechargeable batteries. Its production is expected to grow more and more in the future, especially for mobile energy storage and electromobility. Until now it is mostly produced by the evaporation of water from salt lakes, which led to a huge water consumption, a large amount of waste produced and a strong environmental impact. A new, clean and faster electrochemical technique to recover lithium has been recently proposed: electrochemical ion pumping. It consists in capturing lithium ions from a feed solution by intercalation in a lithium-selective material, followed by releasing them into a recovery solution; both steps are driven by the passage of a current. In this work, a new configuration of the electrochemical cell is presented, used to study and optimize the process of the intercalation of lithium ions through the hydrodynamic condition. Lithium Manganese Oxide (LiMn₂O₄) was used as a cathode to intercalate lithium ions selectively during the reduction, while Nickel Hexacyano Ferrate (NiHCF), used as an anode, releases positive ion. The effect of hydrodynamics on the process has been studied by conducting the experiments at various fluxes of the electrolyte through the electrodes, in terms of charge circulated through the cell, captured lithium per unit mass of material and overvoltage. The result shows that flowing the electrolyte inside the cell improves the lithium capture, in particular at low lithium concentration. Indeed, in Atacama feed solution, at 40 mM of lithium, the amount of lithium captured does not increase considerably with the flux of the electrolyte. Instead, when the concentration of the lithium ions is 5 mM, the amount of captured lithium in a single capture cycle increases by increasing the flux, thus leading to the conclusion that the slowest step in the process is the transport of the lithium ion in the liquid phase. Furthermore, an influence of the concentration of other cations in solution on the process performance was observed. In particular, the capturing of the lithium using a different concentration of NaCl together with 5 mM of LiCl was performed, and the results show that the presence of NaCl limits the amount of the captured lithium. Further studies can be performed in order to understand why the full capacity of the material is not reached at the highest flow rate. This is probably due to the porous structure of the material since the liquid phase is likely not affected by the convection flow inside the pores. This work proves that electrochemical ion pumping, with a suitable hydrodynamic design, enables the recovery of lithium from feed solutions at the lower concentration than the sources that are currently exploited, down to 1 mM.

Keywords: desalination battery, electrochemical ion pumping, hydrodynamic, lithium

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Authors: Chetna Tyagi. G. B. V. S. Lakshmi, Ambuj Tripathi, D. K. Avasthi

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Graphene oxide provides a good host matrix for preparing nanocomposites due to the different functional groups attached to its edges and planes. Being biocompatible, it is used in therapeutic applications. As enzyme-based biosensor requires complicated enzyme purification procedure, high fabrication cost and special storage conditions, we need enzyme-less biosensors for use even in a harsh environment like high temperature, varying pH, etc. In this work, we have prepared both enzyme-based and enzyme-less graphene oxide-based biosensors for glucose detection using glucose-oxidase as enzyme and gold nanoparticles, respectively. These samples were characterized using X-ray diffraction, UV-visible spectroscopy, scanning electron microscopy, and transmission electron microscopy to confirm the successful synthesis of the working electrodes. Electrochemical measurements were performed for both the working electrodes using a 3-electrode electrochemical cell. Cyclic voltammetry curves showed the homogeneous transfer of electron on the electrodes in the scan range between -0.2V to 0.6V. The sensing measurements were performed using differential pulse voltammetry for the glucose concentration varying from 0.01 mM to 20 mM, and sensing was improved towards glucose in the presence of gold nanoparticles. Gold nanoparticles in graphene oxide nanocomposite played an important role in sensing glucose in the absence of enzyme, glucose oxidase, as evident from these measurements. The selectivity was tested by measuring the current response of the working electrode towards glucose in the presence of the other common interfering agents like cholesterol, ascorbic acid, citric acid, and urea. The enzyme-less working electrode also showed storage stability for up to 15 weeks, making it a suitable glucose biosensor.

Keywords: electrochemical, enzyme-less, glucose, gold nanoparticles, graphene oxide, nanocomposite

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Authors: Barzin Rajabloo, Martin Desilets

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First, an electrochemical model for the reduction of CO₂ into CH₃OH is developed in which mass and charge transfer, reactions at the surface of the electrodes and fluid flow of the electrolyte are considered. This mathematical model is developed in COMSOL Multiphysics® where both secondary and tertiary current distribution interfaces are coupled to consider concentrations and potentials inside different parts of the cell. Constant reaction rates are assumed as the fitted parameters to minimize the error between experimental data and modeling results. The model is validated through a comparison with experimental data in terms of faradaic efficiency for production of CH₃OH, the current density in different applied cathode potentials as well as current density in different electrolyte flow rates. The comparison between model outputs and experimental measurements shows a good agreement. The model indicates the higher hydrogen evolution in comparison with CH₃OH production as well as mass transfer limitation caused by CO₂ concentration, which are consistent with findings in the literature. After validating the model, in the second part of the study, some design parameters of the cell, such as cathode geometry and catholyte/anolyte channel widths, are modified to reach better performance and higher faradaic efficiency of methanol production.

Keywords: carbon dioxide, electrochemical reduction, methanol, modeling

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Authors: Shyam Ranjan Kumar, Shashikant Rajpal

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Zinc Telluride (ZnTe) is a binary II-VI direct band gap semiconducting material. This semiconducting material has several applications in sensors, photo-electrochemical devices and photovoltaic solar cell. In this study, Zinc telluride (ZnTe) thin films were deposited on nickel substrate by electrodeposition technique using potentiostat/galvanostat at -0.85 V using AR grade of Zinc Chloride (ZnCl2), Tellurium Tetrachloride (TeCl4) in non-aqueous bath. The developed films were physically stable and showed good adhesion. The as deposited ZnTe films were annealed at 400ºC in air. The solid state properties and optical properties of the as deposited and annealed films were carried out by XRD, EDS, SEM, AFM, UV–Visible spectrophotometer, and photoluminescence spectrophotometer. The diffraction peak observed at 2θ = 49.58° with (111) plane indicate the crystalline nature of ZnTe film. Annealing improves the crystalline nature of the film. Compositional analysis reveals the presence of Zn and Te with tellurium rich ZnTe film. SEM photograph at 10000X shows that grains of film are spherical in nature and densely distributed over the surface. The average roughness of the film is measured by atomic force microscopy and it is nearly equal to 60 nm. The direct wide band gap of 2.12 eV is observed by UV-Vis spectroscopy. Luminescence peak of the ZnTe films are also observed in as deposited and annealed case.

Keywords: annealing, electrodeposition, optical properties, thin film, XRD, ZnTe

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Authors: Charmaine Lamiel, Van Hoa Nguyen, Marjorie Baynosa, Jae-Jin Shim

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The depletion of non-renewable sources had led to the continuous development of various energy storage systems in order to cope with the world’s demand in energy. Supercapacitors have attracted considerable attention because they can store more energy than conventional capacitors and have higher power density than batteries. The combination of carbon-based material and metal chalcogenides are now being considered in response to the search for active electrode materials exhibiting high electrochemical performance. In this study, a hierarchical mesoporous carbon sphere@nickel cobalt sulfide (CS@Ni-Co-S) core-shell was synthesized using a simple hydrothermal method. The CS@Ni-Co-S core-shell microstructures exhibited a high capacitance of 724.4 F g−1 at 2 A g−1 in a 6 M KOH electrolyte. Good specific retention of 86.1% and high Coulombic efficiency of 97.9% was obtained after 2000 charge-discharge cycles. The electrode exhibited a high energy density of 58.0 Wh kg−1 (1440 W kg−1) and high power density of 7200 W kg−1 (34.2 Wh kg−1). The reaction involved green synthesis without further sulfurization or post-heat treatment. Through this study, a cost-effective and facile synthesis of CS@Ni-Co-S as an active electrode showed favorable electrochemical performance.

Keywords: carbon sphere, electrochemical, hydrothermal, nickel cobalt sulfide, supercapacitor

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Authors: Asiful Hossain Seikh, Mohammad Asif Alam, Ubair Abdus Samad, Jabair A. Mohammed, S. M. Al-Zahrani, El-Sayed M. Sherif

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In this current investigation, aliphatic amine-cured diglycidyl ether of bisphenol-A (DGEBA) based epoxy coating was mixed with certain weight % hardener polyaminoamide (1:2) and was coated on carbon steel panels with and without 1% nano crystalline Al powder. The corrosion behavior of the coated samples were investigated by exposing them in the salt spray chamber, for 500 hours. According to ASTM-B-117, the bath was kept at 35 °C and 5% NaCl containing mist was sprayed at 1.3 bars pressure. Composition of coatings was confirmed using Fourier-transform infrared spectroscopy (FTIR). Electrochemical characterization of the coated samples was also performed using potentiodynamic polarization technique and electrochemical impedance spectroscopy (EIS) technique. All the experiments were done in 3.5% NaCl solution. The nano Al coated sample shows good corrosion resistance property compared to bare Al sample. In fact after salt spray exposure no pitting or local damage was observed for nano coated sample and the coating gloss was negligibly affected. The surface morphology of coated and corroded samples was studied using scanning electron microscopy (SEM).

Keywords: epoxy, nano aluminium, potentiodynamic polarization, salt spray, electrochemical impedence spectroscopy

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Authors: Şeyma Dombaycıoğlu, Hilal Köse, Ali Osman Aydın, Hatem Akbulut

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Rechargeable lithium ion batteries (LIBs) have been considered as one of the most attractive energy storage choices for laptop computers, electric vehicles and cellular phones owing to their high energy and power density. Compared with conventional carbonaceous materials, transition metal oxides (TMOs) have attracted great interests and stand out among versatile novel anode materials due to their high theoretical specific capacity, wide availability and good safety performance. ZnO, as an anode material for LIBs, has a high theoretical capacity of 978 mAh g-1, much higher than that of the conventional graphite anode (∼370 mAhg-1). However, several major problems such as poor cycleability, resulting from the severe volume expansion and contraction during the alloying-dealloying cycles with Li+ ions and the associated charge transfer process, the pulverization and the agglomeration of individual particles, which drastically reduces the total entrance/exit sites available for Li+ ions still hinder the practical use of ZnO powders as an anode material for LIBs. Therefore, a great deal of effort has been devoted to overcome these problems, and many methods have been developed. In most of these methods, it is claimed that carbon nanotubes (CNTs) will radically improve the performance of batteries, because their unique structure may especially enhance the kinetic properties of the electrodes and result in an extremely high specific charge compared with the theoretical limits of graphitic carbon. Due to outstanding properties of CNTs, MWCNT buckypaper substrate is considered a buffer material to prevent mechanical disintegration of anode material during the battery applications. As the bridge connecting the positive and negative electrodes, the electrolyte plays a critical role affecting the overall electrochemical performance of the cell including rate, capacity, durability and safety. Commercial electrolytes for Li-ion batteries normally consist of certain lithium salts and mixed organic linear and cyclic carbonate solvents. Most commonly, LiPF6 is attributed to its remarkable features including high solubility, good ionic conductivity, high dissociation constant and satisfactory electrochemical stability for commercial fabrication. Besides LiPF6, LiBF4 is well known as a conducting salt for LIBs. LiBF4 shows a better temperature stability in organic carbonate based solutions and less moisture sensitivity compared to LiPF6. In this work, free standing zinc oxide (ZnO) and multiwalled carbon nanotube (MWCNT) nanocomposite materials were prepared by a sol gel technique giving a high capacity anode material for lithium ion batteries. Electrolyte solutions (including 1 m Li+ ion) were prepared with different Li salts in glove box. For this purpose, LiPF6 and LiBF4 salts and also mixed of these salts were solved in EC:DMC solvents (1:1, w/w). CR2016 cells were assembled by using these prepared electrolyte solutions, the ZnO/MWCNT buckypaper nanocomposites as working electrodes, metallic lithium as cathode and polypropylene (PP) as separator. For investigating the effect of different Li salts on the electrochemical performance of ZnO/MWCNT nanocomposite anode material electrochemical tests were performed at room temperature.

Keywords: anode, electrolyte, Li-ion battery, ZnO/MWCNT

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Authors: Shiying Fan, Xinyong Li

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The development of highly efficient multifunctional catalytic materials towards HER, ORR and Photo-fuel cell applications in terms of combined electrochemical and photo-electrochemical principles have currently confronted with dire challenges. In this study, novel palladium (Pd) and ruthenium (Ru) Bimetal Quantum Dots (BQDs) co-anchored on Titania nanotube (NTs) arrays electrodes have been successfully constructed by facial two-step electrochemical strategy. Double Schottky junctions with superior performance in electrocatalytic (EC) hydrogen generations and solar fuel cell energy conversions (PE) have been found. Various physicochemical techniques including UV-vis spectroscopy, TEM/EDX/HRTEM, SPV/TRV and electro-chemical strategy including EIS, C-V, I-V, and I-T, etc. were chronically utilized to systematically characterize the crystal-, electronic and micro-interfacial structures of the composites with double Schottky junction, respectively. The characterizations have implied that the marvelous enhancement of separation efficiency of electron-hole pairs generations is mainly caused by the Schottky-barriers within the nanocomposites, which would greatly facilitate the interfacial charge transfer for H₂ generations and solar fuel cell energy conversions. Moreover, the DFT calculations clearly indicated that the oriented growth of Ru and Pd bimetal atoms at the anatase (101) surface is mainly driven by the interaction between Ru/Pd and surface atoms, and the most active site for bimetal Ru and Pd adatoms on the perfect TiO₂ (101) surface is the 2cO-6cTi-3cO bridge sites and the 2cO-bridge sites with the highest adsorption energy of 9.17 eV. Furthermore, the electronic calculations show that in the nanocomposites, the number of impurity (i.e., co-anchored Ru-Pd BQDs) energy levels near Fermi surface increased and some were overlapped with original energy level, promoting electron energy transition and reduces the band gap. Therefore, this work shall provide a deeper insight for the molecular design of Bimetal Quantum Dots (BQDs) assembled onto Tatiana NTs composites with superior performance for electrocatalytic hydrogen productions and solar fuel cell energy conversions (PE) simultaneously.

Keywords: eletrocatalytic, Ru-Pd bimetallic quantum dots, titania nanotube arrays, double Schottky junctions, hydrogen production

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Authors: Boriana Karamanova, Svetlana Veleva, Luybomir Soserov, Ana Arenillas, Francesco Lufrano, Antonia Stoyanova

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Supercapacitors have received a lot of research attention and are promising energy storage devices due to their high power and long cycle life. In order to developed an advanced device with significant capacity for storing charge and cheap carbon materials, efforts must focus not only on improving synthesis by controlling the morphology and pore size but also on improving electrode-electrolyte compatibility of the resulting systems. The present study examines the relationship between the surface chemistry of two activated carbon xerogels, the electrolyte type, and the electrochemical properties of supercapacitors. Activated carbon xerogels were prepared by varying the initial pH of the resorcinol-formaldehyde aqueous solution. The materials produced are physicochemical characterized by DTA/TGA, porous characterization, and SEM analysis. The carbon xerogel based electrodes were prepared by spreading over glass plate a slurry containing the carbon gel, graphite, and poly vinylidene difluoride (PVDF) binder. The layer formed was dried consecutively at different temperatures and then detached by water. After, the layer was dried again to improve its mechanical stability. The developed electrode materials and the Aquivion® E87-05S membrane (Solvay Specialty Polymers), socked in Na2SO4 as a polymer electrolyte, were used to assembly the solid-state supercapacitor. Symmetric supercapacitor cells composed by same electrodes and 1 M KOH electrolytes are also assembled and tested for comparison. The supercapacitor performances are verified by different electrochemical methods - cyclic voltammetry, galvanostatic charge/discharge measurements, electrochemical impedance spectroscopy, and long-term durability tests in neutral and alkaline electrolytes. Specific capacitances, energy, and power density, energy efficiencies, and durability were compared into studied supercapacitors. Ex-situ physicochemical analyses on the synthesized materials have also been performed, which provide information about chemical and structural changes in the electrode morphology during charge / discharge durability tests. They are discussed on the basis of electrode-electrolyte interaction. The obtained correlations could be of significance in order to design sustainable solid-state supercapacitors with high power and energy density. Acknowledgement: This research is funded by the Ministry of Education and Science of Bulgaria under the National Program "European Scientific Networks" (Agreement D01-286 / 07.10.2020, D01-78/30.03.2021). Authors gratefully acknowledge.

Keywords: carbon xerogel, electrochemical tests, neutral and alkaline electrolytes, supercapacitors

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Authors: A. Mohamed, A. El-Aziz

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The pH of the body plays a great role in the degradation kinetics of biodegradable Mg-Ca orthopedic implants. At the location of fracture, the pH of the body becomes no longer neutral which draws the attention towards studying a range of different pH values of the body fluid. In this study, the pH of Hank’s balanced salt solution (HBSS) was modified by phosphate buffers into an aggressive acidic pH 1.8, a slightly acidic pH 5.3 and an alkaline pH 8.1. The biodegradation of Mg-0.8Ca implant was tested in those three different media using immersion test and electrochemical polarization means. It was proposed that the degradation rate has increased with decreasing the pH of HBSS. The immersion test revealed weight gain for all the samples followed by weight loss as the immersion time increased. The highest weight gain was pronounced for the acidic pH 1.8 and the least weight gain was observed for the alkaline pH 8.1. This was in agreement with the electrochemical polarization test results where the degradation rate was found to be high (7.29 ± 2.2 mm/year) in the aggressive acidic solution of pH 1.8 and relatively minimum (0.31 ± 0.06 mm/year) in the alkaline medium of pH 8.1. Furthermore, it was confirmed that the pH of HBSS has reached a steady state of an alkaline pH (~pH 11) at the end of the two-month immersion period regardless of the initial pH of the solution. Finally, the corrosion products formed on the samples’ surface were investigated by SEM, EDX and XRD analyses that revealed the formation of magnesium and calcium phosphates with different morphologies according to the pH.

Keywords: biodegradable, electrochemical polarization means, orthopedics, immersion test, simulated body fluid

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Authors: Issam Lakdhar, Akram Alhussein, Juan Creus

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With the huge increase in world energy consumption, researchers are working to find other alternative sources of energy instead of fossil fuel one causing many environmental problems as the production of greenhouse effect gases. Hydrogen is considered a green energy source, which its combustion does not cause environmental pollution. The transport and the storage of the gas molecules or the other products containing this smallest chemical element in metallic structures (pipelines, tanks) are crucial issues. The dissolve and the permeation of hydrogen into the metal lattice lead to the formation of hydride phases and the embrittlement of structures. To protect the metallic structures, a surface treatment could be a good solution. Among the different techniques, magnetron sputtering is used to elaborate micrometric coatings capable of slowing down or stop hydrogen permeation. In the plasma environment, the deposition parameters of new thin-film metallic glasses Al-Ti-W were optimized and controlled in order to obtain, hydrogen barrier. Many characterizations were carried out (SEM, XRD and Nano-indentation…) to control the composition and understand the influence of film microstructure and chemical composition on the hydrogen permeation through the coatings. The coating performance was evaluated under two hydrogen production methods: chemical and electrochemical (cathodic protection) techniques. The hydrogen quantity absorbed was experimentally determined using the Thermal-Desorption Spectroscopy method (TDS)). An ideal ATW thin film was developed and showed excellent behavior against the diffusion of hydrogen.

Keywords: thin films, hydrogen, PVD, plasma technology, electrochemical properties

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Authors: Meriem Hamla, Mohamed Benaicha, Sabrine Derbal

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In the present work, several materials such as M/glass (M = Pt, Mo) were investigated to test their suitability for studying the early nucleation stages and growth of copper-tin clusters. It was found that most of these materials stand as good substrates to be used in the study of the nucleation and growth of electrodeposited Cu-Sn alloys from aqueous solution containing CuCl2, SnCl2 as electroactive species and Na3C6H5O7 as complexing agent. Among these substrates, Pt shows instantaneous models followed by 3D diffusion-limited growth. On the other hand, the electrodeposited copper-tin thin films onto Mo substrate followed progressive nucleation. The deposition mechanism of the Cu-Sn films has been studied using stationary electrochemical techniques (cyclic voltammetery (CV) and chronoamperometry (CA). The structural, morphological and compositional of characterization have been studied using X-ray diffraction (XRD), scanning electron microscopy (SEM) and EDAX techniques respectively.

Keywords: electrodeposition, CuSn, nucleation, mechanism

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Authors: Priyal Chikhaliwala, Sudeshna Chandra

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Liver cancer is one of the most common malignant tumors with poor prognosis. This is because liver cancer does not exhibit any symptoms in early stage of disease. Increased serum level of AFP is clinically considered as a diagnostic marker for liver malignancy. The present diagnostic modalities include various types of immunoassays, radiological studies, and biopsy. However, these tests undergo slow response times, require significant sample volumes, achieve limited sensitivity and ultimately become expensive and burdensome to patients. Considering all these aspects, electrochemical biosensors based on dendrimer-magnetic nanoparticles (MNPs) was designed. Dendrimers are novel nano-sized, three-dimensional molecules with monodispersed structures. Poly-amidoamine (PAMAM) dendrimers with eight –NH₂ groups using ethylenediamine as a core molecule were synthesized using Michael addition reaction. Dendrimers provide added the advantage of not only stabilizing Fe₃O₄ NPs but also displays capability of performing multiple electron redox events and binding multiple biological ligands to its dendritic end-surface. Fe₃O₄ NPs due to its superparamagnetic behavior can be exploited for magneto-separation process. Fe₃O₄ NPs were stabilized with PAMAM dendrimer by in situ co-precipitation method. The surface coating was examined by FT-IR, XRD, VSM, and TGA analysis. Electrochemical behavior and kinetic studies were evaluated using CV which revealed that the dendrimer-Fe₃O₄ NPs can be looked upon as electrochemically active materials. Electrochemical immunosensor was designed by immobilizing anti-AFP onto dendrimer-MNPs by gluteraldehyde conjugation reaction. The bioconjugates were then incubated with AFP antigen. The immunosensor was characterized electrochemically indicating successful immuno-binding events. The binding events were also further studied using magnetic particle imaging (MPI) which is a novel imaging modality in which Fe₃O₄ NPs are used as tracer molecules with positive contrast. Multicolor MPI was able to clearly localize AFP antigen and antibody and its binding successfully. Results demonstrate immense potential in terms of biosensing and enabling MPI of AFP in clinical diagnosis.

Keywords: alpha-fetoprotein, dendrimers, electrochemical biosensors, magnetic nanoparticles

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Authors: J. Tirano, H. Zea, C. Luhrs

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It is well known that titanium dioxide is a semiconductor with several applications in photocatalytic process. Its band gap makes it very interesting in the photoelectrodes manufacturing used in photoelectrochemical cells for hydrogen production, a clean and environmentally friendly fuel. The synthesis of 1D titanium dioxide nanostructures, such as nanotubes, makes possible to produce more efficient photoelectrodes for solar energy to hydrogen conversion. In essence, this is because it increases the charge transport rate, decreasing recombination options. However, its principal constraint is to be mainly sensitive to UV range, which represents a very low percentage of solar radiation that reaches earth's surface. One of the alternatives to modifying the TiO2’s band gap and improving its photoactivity under visible light irradiation is to dope the nanotubes with transition metals. This option requires fabricating efficient nanostructured photoelectrodes with controlled morphology and specific properties able to offer a suitable surface area for metallic doping. Hence, currently one of the central challenges in photoelectrochemical cells is the construction of nanomaterials with a proper band position for driving the reaction while absorbing energy over the VIS spectrum. This research focuses on the synthesis and characterization of Nidoped TiO2 nanotubes for improving its photocatalytic activity in solar energy conversion applications. Initially, titanium dioxide nanotubes (TNTs) with controlled morphology were synthesized by two-step potentiostatic anodization of titanium foil. The anodization was carried out at room temperature in an electrolyte composed of ammonium fluoride, deionized water and ethylene glycol. Consequent thermal annealing of as-prepared TNTs was conducted in the air between 450 °C - 550 °C. Afterwards, the nanotubes were superficially modified by nickel deposition. Morphology and crystalline phase of the samples were carried out by SEM, EDS and XRD analysis before and after nickel deposition. Determining the photoelectrochemical performance of photoelectrodes is based on typical electrochemical characterization techniques. Also, the morphological characterization associated electrochemical behavior analysis were discussed to establish the effect of nickel nanoparticles modification on the TiO2 nanotubes. The methodology proposed in this research allows using other transition metal for nanotube surface modification.

Keywords: dimensionally stable electrode, nickel nanoparticles, photo-electrode, TiO₂ nanotubes

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Authors: Hamad Almohamadi, Nabeel H. Alharthi, Abdulrahman Aljabri

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In this study, two-dimensional CuFeOx is deposited on nickel foam for the fabrication of electrocatalyst for oxygen evolution reaction (OER). The in-situ hydrothermal synthesis of CuFeOx in presence of aloe vera extract was found to yield unique nano-rose-like morphology which aided to improve the electrochemical surface area of the electrode. The phytochemical assisted synthesis of CuFeOx using 75% aloe vera extract resulted in improved OER electrocatalytic performance by attaining the overpotential of 310 mV for 50 mA cm−2 and 410 mV for 100 mA cm−2. The electrode also sustained robust stability throughout the 50 h of chronopotentiometry studies under alkaline electrolyte conditions, thus proving to be prospective electrode material for efficient OER in electrochemical water splitting.

Keywords: water splitting, phytochemicals, oxygen evaluation reaction, Tafel's slope, stability

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Authors: Garzon V., Bustos R., Salvador J. P., Marco M. P., Pinacho D. G.

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Bacterial resistance to antimicrobial treatment has increased significantly in recent years, making it a public health problem. Large numbers of bacteria are resistant to all or nearly all known antimicrobials, creating the need for the development of new types of antimicrobials or the use of “last line” antimicrobial drug therapies for the treatment of multi-resistant bacteria. Some of the chemical groups of antimicrobials most used for the treatment of infections caused by multiresistant bacteria in the clinic are Glycopeptide (Vancomycin), Polymyxin (Colistin), Lipopeptide (Daptomycin) and Carbapenem (Meropenem). Molecules that require therapeutic drug monitoring (TDM). Due to the above, a methodology based on nanobiotechnology based on an optical and electrochemical biosensor is being developed, which allows the evaluation of the plasmatic levels of some antimicrobials such as glycopeptide, polymyxin, lipopeptide and carbapenem quickly, at a low cost, with a high specificity and sensitivity and that can be implemented in the future in public and private health hospitals. For this, the project was divided into five steps i) Design of specific anti-drug antibodies, produced in rabbits for each of the types of antimicrobials, evaluating the results by means of an immunoassay analysis (ELISA); ii) quantification by means of an electrochemical biosensor that allows quantification with high sensitivity and selectivity of the reference antimicrobials; iii) Comparison of antimicrobial quantification with an optical type biosensor; iv) Validation of the methodologies used with biosensor by means of an immunoassay. Finding as a result that it is possible to quantify antibiotics by means of the optical and electrochemical biosensor at concentrations on average of 1,000ng/mL, the antibodies being sensitive and specific for each of the antibiotic molecules, results that were compared with immunoassays and HPLC chromatography. Thus, contributing to the safe use of these drugs commonly used in clinical practice and new antimicrobial drugs.

Keywords: antibiotics, electrochemical biosensor, optical biosensor, therapeutic drug monitoring

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Authors: Zahrah Thamer Althagafi, Mohamed I. Awad

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A simple method for the fabrication of Au (111)-like electrode via controlled reductive desorption of a pre-adsorbed cysteine monolayer onto polycrystalline gold (poly-Au) electrode is introduced. Then, the voltammetric behaviour of dopamine (DA) and ascorbic acid (AA) on the thus modified electrode is investigated. Electrochemical characterization of the modified electrode is achieved using cyclic voltammetry and square wave voltammetry. For the binary mixture of DA and AA, the results showed that Au (111)-like electrode exhibits excellent electrocatalytic activity towards the oxidation of DA and AA. This allows highly selective and simultaneous determination of DA and AA. The effect of various experimental parameters on the voltammetric responses of DA and AA was investigated. The enrichment of the Au (111) facet of the poly-Au electrode is thought to be behind the electrocatalytic activity.

Keywords: gold electrode, electroanalysis, electrocatalysis, monolayers, self-assembly, cysteine, dopamine, ascorbic acid

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Authors: Angelo Gabriel Buenaventura, Allan Christopher Yago

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A carbon paste electrode (CPE) composed of Multiwalled Carbon Nanotube (MWCNT) conducting particle and Polydimethylsiloxane (PDMS) binder was used for simultaneous detection of Dopamine (DA) and Uric Acid (UA) in the presence of Ascorbic Acid (AA) at physiological level. The MWCNT-PDMS CPE was initially activated via potentiodynamic cycling in a basic (NaOH) solution, which resulted in enhanced electrochemical properties. Electrochemical Impedance Spectroscopy measurements revealed a significantly lower charge transfer resistance (Rct) for the OH--activated MWCNT-PDMS CPE (Rct = 5.08kΩ) as compared to buffer (pH 7)-activated MWCNT-PDMS CPE (Rct = 25.9kΩ). Reversibility analysis of Fe(CN)63-/4- redox couple of both Buffer-Activated CPE and OH--Activated CPE showed that the OH—Activated CPE have peak current ratio (Ia/Ic) of 1.11 at 100mV/s while 2.12 for the Buffer-Activated CPE; this showed an electrochemically reversible behavior for Fe(CN)63-/4- redox couple even at relatively fast scan rate using the OH--activated CPE. Enhanced voltammetric signal for DA and significant peak separation between DA and UA was obtained using the OH--activated MWCNT-PDMS CPE in the presence of 50 μM AA via Differential Pulse Voltammetry technique. The anodic peak currents which appeared at 0.263V and 0.414 V were linearly increasing with increasing concentrations of DA and UA, respectively. The linear ranges were obtained at 25 μM – 100 μM for both DA and UA. The detection limit was determined to be 3.86 μM for DA and 5.61 μM for UA. These results indicate a practical approach in the simultaneous detection of important bio-organic molecules using a simple CPE composed of MWCNT and PDMS with base anodization as activation technique.

Keywords: anodization, ascorbic acid, carbon paste electrodes, dopamine, uric acid

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Authors: B. Bouadjemi, S. Bentata, A. Abbad, W.Benstaali

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The full-potential linearized augmented plane wave method (FP-LAPW) within the Generalized Gradient Approximation (GGA) is used to calculate the magnetic and optical properties of quaternary GaFeMnN. The results show that the compound becomes magnetic and half metallic and there is an apparition of peaks at low frequencies for the optical properties.

Keywords: optical properties, DFT, Spintronic, wave

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Authors: Amer Dawoud, Jesy Motchaalangaram, Arati Biswakarma, Wujan Mio, Karl Wallace

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The development of an embedded miniaturized drone-based system for remote detection of Chemical Warfare Agents (CWA) is proposed. The paper focuses on the software/hardware system design of the electrochemical Cyclic Voltammetry (CV) and Differential Pulse Voltammetry (DPV) signal processing for future deployment on drones. The paper summarizes the progress made towards hardware and electrochemical signal processing for signature detection of CWA. Also, the miniature potentiostat signal is validated by comparing it with the high-end lab potentiostat signal.

Keywords: drone-based, remote detection chemical warfare agents, miniaturized, potentiostat

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Authors: Radka Gorejova, Ivana Sisolakova, Jana Shepa, Frederika Chovancova, Renata Orinakova

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Diabetes mellitus (DM) is a serious metabolic disease characterized by chronic hyperglycemia. Often, the symptoms are not sufficiently observable at early stages, and so hyperglycemia causes pathological and functional changes before the diagnosis of the DM. Therefore, the development of an electrochemical sensor that will be fast, accurate, and instrumentally undemanding is currently needful. Screen-printed carbon electrodes (SPCEs) can be considered as the most suitable matrix material for insulin sensors because of the small size of the working electrode. It leads to the analyst's volume reduction to only 50 µl for each measurement. The surface of bare SPCE was modified by a combination of chitosan, multi-walled carbon nanotubes (MWCNTs), and zinc nanoparticles (ZnNPs) to obtain better electrocatalytic activity towards insulin oxidation. ZnNPs were electrochemically deposited on the chitosan-MWCNTs/SPCE surface using the pulse deposition method. Thereafter, insulin was determined on the prepared electrode using chronoamperometry and electrochemical impedance spectroscopy (EIS). The chronoamperometric measurement was performed by adding a constant amount of insulin in 0.1 M NaOH and PBS (2 μl) with the concentration of 2 μM, and the current response of the system was monitored after a gradual increase in concentration. Subsequently, the limit of detection (LOD) of the prepared electrode was determined via the Randles-Ševčík equation. The LOD was 0.47 µM. Prepared electrodes were studied also as the impedimetric sensors for insulin determination. Therefore, various insulin concentrations were determined via EIS. Based on the performed measurements, the ZnNPs/chitosan-MWCNTs/SPCE can be considered as a potential candidate for novel electrochemical sensor for insulin determination. Acknowledgments: This work has been supported by the projects Visegradfund project number 22020140, VEGA 1/0095/21 of the Slovak Scientific Grant Agency, and APVV-PP-COVID-20-0036 of the Slovak Research and Development Agency.

Keywords: zinc nanoparticles, insulin, chronoamperometry, electrochemical impedance spectroscopy

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Authors: H. Acar, M. Karakışla, L. Aksu, M. Saçak

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The corrosion protection effect of poly(o-toluidine) (POT) coated on steel 316 electrode was determined in corrosive media such as NaCl, H2SO4 and HCl with the use of Tafel curves and electrochemical impedance spectroscopy techniques. The POT coatings were prepared with cyclic voltammetry technique in aqueous solution of oxalic acid and they were characterized by FTIR and UV-Visible absorption spectroscopy. The Tafel curves revealed that the POT coating provides the most effective protection compared to the bare steel 316 electrode in NaCl as corrosive medium. The results were evaluated based upon data decrease of corrosion current and shift to positive potentials with the increase of number of scans. Electrochemical impedance spectroscopy measurements were found to support Tafel data of POT coating.

Keywords: corrosion, impedance spectroscopy, steel 316, poly(o-toluidine)

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Authors: Sonali Panigrahy, Manjunatha K., Sudip Barman

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Electrocatalytic reduction methods hold significant promise in addressing the urgent need to mitigate excessive greenhouse gas emissions, particularly carbon dioxide (CO₂). A highly effective catalyst is essential for achieving the conversion of CO₂ into valuable products due to the complex, multi-electron, and multi-product nature of the CO₂ reduction process. The electrochemical reduction of CO₂, driven by renewable energy sources, presents a valuable opportunity for simultaneously reducing CO₂ emissions while generating valuable chemicals and fuels, with syngas being a noteworthy product. Silver-based electrodes have been the focus of extensive research due to their low overpotential and remarkable selectivity in promoting the generation of carbon monoxide (CO) in the electrocatalytic carbon dioxide reduction reaction (CO₂RR). In this study, we delve into the synthesis of carbon-supported silver nanoparticles (Ag/C), which serve as efficient electrocatalysts for the reduction of CO₂. The as-prepared catalyst, Ag/C, is not only cost-effective but also highly proficient in facilitating the conversion of CO₂ and H₂O into syngas, which is a customizable mixture of hydrogen (H₂) and carbon monoxide (CO). The highest faradic efficiency for the production of CO on Ag/C was calculated to be 56.4% at -1.4 V vs Ag/AgCl. The maximum partial current density for the generation of CO was determined to be -9.4 mA cm-2 at a potential of -1.6 V vs Ag/AgCl. This research demonstrates the potential of Ag/C as an electrocatalyst to enable the sustainable production of syngas, contributing to the reduction of CO₂ emissions and the synthesis of valuable chemical precursors and fuels.

Keywords: CO₂, carbon monooxide, electrochemical, silver

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Authors: Abdelhak Nouri

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Europium doped zinc oxide nanocolumns (ZnO:Eu) were deposited on indium tin oxide (ITO) substrate from an aqueous solution of 10⁻³M Zn(NO₃)₂ and 0.5M KNO₃ with different concentration of europium ions. The deposition was performed in a classical three-electrode electrochemical cell. The structural, morphology and optical properties have been characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM). The XRD results show high quality of crystallite with preferential orientation along c-axis. SEM images speculate ZnO: Eu has nanocolumnar form with hexagonal shape. The diameter of nanocolumns is around 230 nm. Furthermore, it was found that tail of crystallite, roughness, and band gap energy is highly influenced with increasing Eu ions concentration. The average grain size is about 102 nm to 125 nm.

Keywords: deterioration lattice, doping, nanostructures, Eu:ZnO

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Authors: Nurlan Akhmetov, Abilmansur Yeshmuratov, Aliya Kurbanova, Gulnar Sugurbekova, Murat Baisariyev

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Extraction of the vanadium and nickel compounds is complex due to the high stability of porphyrin, nickel is catalytic poison which deactivates catalysis during the catalytic cracking of the oil, while vanadyl is abrasive and valuable metal. Thus, high concentration of the Ni and V in the crude oil makes their removal relevant. Two methods of the demetallization of crude oil were tested, therefore, the present research is conducted for comparative analysis of the deasphalting with organic solvents (cyclohexane, carbon tetrachloride, chloroform) and electrochemical method. Percentage of Ni extraction reached maximum of approximately 55% by using the electrochemical method in electrolysis cell, which was developed for this research and consists of three sections: oil and protonating agent (EtOH) solution between two conducting membranes which divides it from two capsules of 10% sulfuric acid and two graphite electrodes which cover all three parts in electrical circuit. Ions of metals pass through membranes and remain in acid solutions. The best result was obtained in 60 minutes with ethanol to oil ratio 25% to 75% respectively, current fits in to the range from 0.3A to 0.4A, voltage changed from 12.8V to 17.3V. Maximum efficiency of deasphalting, with cyclohexane as the solvent, in Soxhlet extractor was 66.4% for Ni and 51.2% for V. Thus, applying the voltammetry, ICP MS (Inductively coupled plasma mass spectrometry) and AAS (atomic absorption spectroscopy), these mentioned types of metal extraction methods were compared in this paper.

Keywords: electrochemistry, deasphalting of crude oil, demetallization of crude oil, petrolium engineering

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Authors: Wilson Handoko, Farshid Pahlevani, Isha Singla, Himanish Kumar, Veena Sahajwalla

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Aluminium bronze alloys are well known for their superior abrasion, tensile strength and non-magnetic properties, due to the co-presence of iron (Fe) and aluminium (Al) as alloying elements and have been commonly used in many industrial applications. However, continuous exposure to the marine environment will accelerate the risk of a tendency to Al bronze alloys parts failures. Although a higher level of corrosion resistance properties can be achieved by modifying its elemental composition, it will come at a price through the complex manufacturing process and increases the risk of reducing the ductility of Al bronze alloy. In this research, the use of ironmaking slag and waste plastic as the input source for surface modification of Al bronze alloy was implemented. Microstructural analysis conducted using polarised light microscopy and scanning electron microscopy (SEM) that is equipped with energy dispersive spectroscopy (EDS). An electrochemical corrosion test was carried out through Tafel polarisation method and calculation of protection efficiency against the base-material was determined. Results have indicated that uniform modified surface which is as the result of selective diffusion process, has enhanced corrosion resistance properties up to 12.67%. This approach has opened a new opportunity to access various industrial utilisations in commercial scale through minimising the dependency on natural resources by transforming waste sources into the protective coating in environmentally friendly and cost-effective ways.

Keywords: aluminium bronze, waste-based surface modification, tafel polarisation, corrosion resistance

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Authors: Siti Aishah Hasbullah

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Studies on identification of pork content in food have grown rapidly to meet the Halal food standard in Malaysia. The used mitochondria DNA (mtDNA) approaches for the identification of pig species is thought to be the most precise marker due to the mtDNA genes are present in thousands of copies per cell, the large variability of mtDNA. The standard method commonly used for DNA detection is based on polymerase chain reaction (PCR) method combined with gel electrophoresis but has major drawback. Its major drawbacks are laborious, need longer time and toxic to handle. Therefore, the need for simplicity and fast assay of DNA is vital and has triggered us to develop DNA biosensors for porcine DNA detection. Therefore, the aim of this project is to develop electrochemical DNA biosensor based on ruthenium (II) complex, [Ru(bpy)2(p-PIP)]2+ as DNA hybridization label. The interaction of DNA and [Ru(bpy)2(p-HPIP)]2+ will be studied by electrochemical transduction using Gold Screen-Printed Electrode (GSPE) modified with gold nanoparticles (AuNPs) and succinimide acrylic microspheres. The electrochemical detection by redox active ruthenium (II) complex was measured by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The results indicate that the interaction of [Ru(bpy)2(PIP)]2+ with hybridization complementary DNA has higher response compared to single-stranded and mismatch complementary DNA. Under optimized condition, this porcine DNA biosensor incorporated modified GSPE shows good linear range towards porcine DNA.

Keywords: gold, screen printed electrode, ruthenium, porcine DNA

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Authors: M. F. Perez, Ysmael Verde, B. Escobar, R. Barbosa, J. C. Cruz

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Reinforced concrete is one of the most important materials in the construction industry. However, in recent years the durability of concrete structures has been a worrying problem, mainly due to corrosion of reinforcing steel; the consequences of corrosion in all cases lead to shortening of the life of the structure and decrease in quality of service. Since the emergence of this problem, they have implemented different methods or techniques to reduce damage by corrosion of reinforcing steel in concrete structures; as the use of polymeric materials as coatings for the steel rod, spiked inhibitors of concrete during mixing, among others, presenting different limitations in the application of these methods. Because of this, it has been used a method that has proved effective, cathodic protection. That is why due to the properties attributed to carbon nanotubes (CNT), these could act as cathodic corrosion protection. Mounting a three-electrode electrochemical cell, carbon steel as working electrode, saturated calomel electrode (SCE) as the reference electrode, and a graphite rod as a counter electrode to close the system is performed. Samples made were subjected to a cycling process in order to compare the results in the corrosion performance of a coating composed of CNT and the others based on an anticorrosive commercial painting. The samples were tested at room temperature using an electrolyte consisting NaCl and NaOH simulating the typical pH of concrete, ranging from 12.6 to 13.9. Three test samples were made of steel rod, white, with commercial anticorrosive paint and CNT based coating; delimiting the work area to a section of 0.71 cm2. Tests cyclic voltammetry and linear voltammetry electrochemical spectroscopy each impedance of the three samples were made with a window of potential vs SCE 0.7 -1.7 a scan rate of 50 mV / s and 100 mV / s. The impedance values were obtained by applying a sine wave of amplitude 50 mV in a frequency range of 100 kHz to 100 MHz. The results obtained in this study show that the CNT based coating applied to the steel rod considerably decreased the corrosion rate compared to the commercial coating of anticorrosive paint, because the Ecorr was passed increase as the cycling process. The samples tested in all three cases were observed by light microscopy throughout the cycling process and micrographic analysis was performed using scanning electron microscopy (SEM). Results from electrochemical measurements show that the application of the coating containing carbon nanotubes on the surface of the steel rod greatly increases the corrosion resistance, compared to commercial anticorrosive coating.

Keywords: anticorrosive, carbon nanotubes, corrosion, steel

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Authors: Yu-Kuei Hsu, Yan-Gu Lin

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A facile and simple fabrication of copper(II) oxide (CuO) nanosheet on copper foil as nanoelectrode for H2O2 sensing application was proposed in this study. The spontaneous formation of CuO nanosheets by immersing the copper foil into 0.1 M NaOH aqueous solution for 48 hrs was carried out at room temperature. The sheet-like morphology with several ten nanometers in thickness and ~500 nm in width was observed by SEM. Those nanosheets were confirmed the monoclinic-phase CuO by the structural analysis of XRD and Raman spectra. The directly grown CuO nanosheets film is mechanically stable and offers an excellent electrochemical sensing platform. The CuO nanosheets electrode shows excellent electrocatalytic response to H2O2 with significantly lower overpotentials for its oxidation and reduction and also exhibits a fast response and high sensitivity for the amperometric detection of H2O2. The novel spontaneously grown CuO nanosheets electrode is readily applicable to other analytes and has great potential applications in the electrochemical detection.

Keywords: CuO, nanosheets, H2O2 detection, Cu foil

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Authors: P. Rutkowski, G. Górny, L. Stobierski, D. Zientara, W. Piekarczyk, K. Tran

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The polycrystalline dense alumina shows thermal conductivity about 30 W/mK and very high electrical resistivity. These last two properties can be modified by introducing commercial relatively cheap graphene nanoparticles which, as two-dimensional flakes show very high thermal and electrical properties. The aim of this work is to show that it is possible to manufacture the anisotropic alumina-graphene material with directed multilayer graphene particles. Such materials can show the anisotropic properties mentioned before.

Keywords: alumina, composite, hot-pressed, graphene, properties

Procedia PDF Downloads 232