Search results for: electrochemical etching

Authors: Md. Abdul Aziz

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Sulfide ion is water soluble, highly corrosive, toxic and harmful to the human beings. As a result, knowing the exact concentration of sulfide in water is very important. However, the existing detection and quantification methods have several shortcomings, such as high cost, low sensitivity, and massive instrumentation. Consequently, the development of novel sulfide sensor is relevant. Nevertheless, electrochemical methods gained enormous popularity due to a vast improvement in the technique and instrumentation, portability, low cost, rapid analysis and simplicity of design. Successful field application of electrochemical devices still requires vast improvement, which depends on the physical, chemical and electrochemical aspects of the working electrode. The working electrode made of bulk gold (Au) and platinum (Pt) are quite common, being very robust and endowed with good electrocatalytic properties. High cost, and electrode poisoning, however, have so far hindered their practical application in many industries. To overcome these obstacles, we developed a sulfide sensor based on an indium tin oxide nanoparticle (ITONP)-modified ITO electrode. To prepare ITONP-modified ITO, various methods were tested. Drop-drying of ITONPs (aq.) on aminopropyltrimethoxysilane-functionalized ITO (APTMS/ITO) was found to be the best method on the basis of voltammetric analysis of the sulfide ion. ITONP-modified APTMS/ITO (ITONP/APTMS/ITO) yielded much better electrocatalytic properties toward sulfide electro-οxidation than did bare or APTMS/ITO electrodes. The ITONPs and ITONP-modified ITO were also characterized using transmission electron microscopy and field emission scanning electron microscopy, respectively. Optimization of the type of inert electrolyte and pH yielded an ITONP/APTMS/ITO detector whose amperometrically and chronocoulοmetrically determined limits of detection for sulfide in aqueous solution were 3.0 µM and 0.90 µM, respectively. ITONP/APTMS/ITO electrodes which displayed reproducible performances were highly stable and were not susceptible to interference by common contaminants. Thus, the developed electrode can be considered as a promising tool for sensing sulfide.

Keywords: amperometry, chronocoulometry, electrocatalytic properties, ITO-nanoparticle-modified ITO, sulfide sensor

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Authors: Atef Youssef, Marwa Mostafa Moharam

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The effects of poly pyrrole (PP) addition on LiFePO4 have been studied by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and galvanostatic measurements. PP was prepared with LiFePO₄ in different ways, such as chemically dispersion, insinuation polymerization, and electrochemically polymerization. The EIS results showed that the charge transfer resistance (Rct) of LiFePO₄ was decreased by adding 10% PP polymerized in a situation to 153 vs. 1660  for bare LiFePO₄. The CV curves show that 10% PP added LiFePO₄ had higher electrochemical reactivity for lithium insertion and extraction than the un-doped material. The mean redox potential is E1/2 = 3.45 V vs. Li+/Li. The first discharge curve of the 10% poly pyrrole doped LiFePO₄ showed a mainly flat voltage plateau over the 3.45–3.5 V range, indicating the lithium extraction and insertion reactions between LiFePO₄ and FePO₄. A specific discharge capacity of cells prepared from in-situ 10% PP added LiFePO4to was about 210 vs. 65 mAhg-1 for bare LiFePO₄.

Keywords: liFePO₄, poly pyrrole addition, positive electrode, lithium battery

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Authors: Yumei Wang, Xiaoyu Xu, Li Lu

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Solid-state battery adopts solid-state electrolyte such as oxide- and composite-based solid electrolytes. With the adaption of nonflammable or less flammable solid electrolytes, the safety of solid-state batteries can be largely increased. NASICON (Na₃Zr₂Si₂PO₁₂, NZSP) is one of the sodium ion conductors that possess relatively high ionic conductivity, wide electrochemical stable range and good chemical stability. Therefore, it has received increased attention. We report the development of high-density NZSP through liquid phase sintering and its organic-inorganic composite electrolyte. Through reactive liquid phase sintering, the grain boundary conductivity can be largely enhanced while using an organic-inorganic composite electrolyte, interfacial wetting and impedance can be largely reduced hence being possible to fabricate scalable solid-state batteries.

Keywords: solid-state electrolyte, composite electrolyte, electrochemical performance, conductivity

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Authors: Ruey-Chi Wang, Po-Hsiang Huang, Ping-Chang Chuang, Shu-Jen Chen

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High-performance Li: CuO/reduced graphene oxide (RGO) flexible electrodes for supercapacitors were fabricated via a low-temperature and low-cost route. To increase energy density while maintaining high power density and long-term cyclability, Li was doped to increase the electrical conductivity of CuO particles between RGO flakes. Electrochemical measurements show that the electrical conductivity, specific capacitance, energy density, and rate capability were all enhanced by Li incorporation. The optimized Li:CuO/RGO electrodes show a high energy density of 179.9 Wh/kg and a power density of 900.0 W/kg at a current density of 1 A/g. Cyclic life tests show excellent stability over 10,000 cycles with a capacitance retention of 93.2%. Li doping improves the electrochemical performance of CuO, making CuO a promising pseudocapacitive material for fabricating low-cost excellent supercapacitors.

Keywords: supercapacitor, CuO, RGO, lithium

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Authors: Liyew Yizengaw Yitayih

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This nanotechnology study focuses on how potassium ions (K+) affect lithium-ion (Li-ion) battery performance. By adding potassium ions (K+) to the lithium tin oxide (LiSnO) anode and employing styrene-butadiene rubber (SBR) as a binder, the doping of K+ was specifically studied. The methods employed in this study include computer modeling and simulation, material fabrication, and electrochemical characterization. The potassium ions (Li+) were successfully doped into the LiSnO lattice during charge/discharge cycles, which increased the lithium-ion diffusivity and electrical conductivity within the anode. However, it was found that internal doping of potassium ions (K+) into the LiSnO lattice occurred at high potassium ion concentrations (>16.6%), which hampered lithium ion transfer because of repulsion and physical blockage. The electrochemical efficiency of lithium-ion batteries was improved by this comprehensive study's presentation of potassium ions' (K+) potential advantages when present in the appropriate concentrations in electrode materials.

Keywords: lithium-ion battery, LiSnO anode, potassium doping, lithium-ion diffusivity, electronic conductivity

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Authors: A. Masek, M. Zaborski

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Electrochemical oxidation of dodecyl gallate (lauryl gallate), the main monomer flavanol found in green tea, was investigated on platinum electrodes using cyclic voltammetry (CV) and differential pulse (DPV) methods. The rate constant, electron transfer coefficient and diffusion coefficients were determined for dodecyl gallate electrochemical oxidation. The oxidation mechanism proceeds in sequential steps related to the hydroxyl groups in the aromatic ring of dodecyl gallate. Confirmed antioxidant activity of lauryl gallate verified its use in polymers as an environment-friendly stabiliser to improve the resistance to aging of the elastomeric materials. Based on the energy change of the deformation, cross-linking density and time of the oxygen induction with the TG method, we confirmed the high antioxidant activity of lauryl gallate in polymers. Moreover, the research on biodegradation confirmed the environment-friendly influence of the antioxidant by increasing the susceptibility of the elastomeric materials to disintegration by mildew mushrooms.

Keywords: polymers, flavonoids, stabilization, ageing

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Authors: Juan Patricio Ibáñez, Exequiel López

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A method for synthesizing copper nanoparticles through an electrochemical approach is proposed, employing surfactants to stabilize the size of the newly formed nanoparticles. The electrolyte was made up of a matrix of H₂SO₄ (190 g/L) having Cu²⁺ (from 3.2 to 9.5 g/L), sodium dodecyl sulfate -SDS- (from 0.5 to 1.0 g/L) and Tween 80 (from 0 to 7.5 mL/L). Tween 80 was used in a molar relation of 1 to 1 with SDS. A glass cell was used, which was in a thermostatic water bath to keep the system temperature, and the electrodes were cathodic copper as an anode and stainless steel 316-L as a cathode. This process was influenced by the control exerted through the initial copper concentration in the electrolyte and the applied current density. Copper nanoparticles of electrolytic purity, exhibiting a spherical morphology of varying sizes with low dispersion, were successfully produced, contingent upon the chemical composition of the electrolyte and current density. The minimum size achieved was 3.0 nm ± 0.9 nm, with an average standard deviation of 2.2 nm throughout the entire process. The deposited copper mass ranged from 0.394 g to 1.848 g per hour (over an area of 25 cm²), accompanied by an average Faradaic efficiency of 30.8% and an average specific energy consumption of 4.4 kWh/kg. The chemical analysis of the product employed X-ray powder diffraction (XRD), while physical characteristics such as size and morphology were assessed using atomic force microscopy (AFM). It was identified that the initial concentration of copper and the current density are the variables defining the size and dispersion of the nanoparticles, as they serve as reactants in the cathodic half-reaction. The presence of surfactants stabilizes the nanoparticle size as their molecules adsorb onto the nanoparticle surface, forming a thick barrier that prevents mass transfer with the exterior and halts further growth.

Keywords: copper nanopowder, electrochemical synthesis, current density, surfactant stabilizer

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Authors: Si Yin Tee

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Bimetallic nanostructures have received tremendous interests as a new class of nanomaterials which may have better technological usefulness with distinct properties from those of individual atoms and molecules or bulk matter. They excelled over the monometallic counterparts because of their improved electronic, optical and catalytic performances. The properties and the applicability of these bimetallic nanostructures not only depend on their size and shape, but also on the composition and their fine structure. These bimetallic nanostructures are potential candidates for bio-applications such as biosensing, bioimaging, biodiagnostics, drug delivery, targeted therapeutics, and tissue engineering. Herein, gold-incorporated copper (Cu/Au) nanostructures were synthesized through the controlled disproportionation of Cu⁺-oleylamine complex at 220 ºC to form copper nanowires and the subsequent reaction with Au³⁺ at different temperatures of 140, 220 and 300 ºC. This is to achieve their synergistic effect through the combined use of the merits of low-cost transition and high-stability noble metals. Of these Cu/Au nanostructures, Cu/Au nanotubes display the best performance towards electrochemical non-enzymatic glucose sensing, originating from the high conductivity of gold and the high aspect ratio copper nanotubes with high surface area so as to optimise the electroactive sites and facilitate mass transport. In addition to high sensitivity and fast response, the Cu/Au nanotubes possess high selectivity against interferences from other potential interfering species and excellent reproducibility with long-term stability. By introducing gold into copper nanostructures at a low level of 3, 1 and 0.1 mol% relative to initial copper precursor, a significant electrocatalytic enhancement of the resulting bimetallic Cu/Au nanostructures starts to occur at 1 mol%. Overall, the present fabrication of stable Cu/Au nanostructures offers a promising low-cost platform for sensitive, selective, reproducible and reusable electrochemical sensing of glucose.

Keywords: bimetallic, electrochemical sensing, glucose oxidation, gold-incorporated copper nanostructures

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Authors: L. Mentar, O. Baka, A. Azizi

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Zinc oxide as a wide band semiconductor materials, especially nanostructured materials, have potential applications in large-area such as electronics, sensors, photovoltaic cells, photonics, optical devices and optoelectronics due to their unique electrical and optical properties and surface properties. The feasibility of ZnO for these applications is due to the successful synthesis of diverse ZnO nanostructures, including nanorings, nanobows, nanohelixes, nanosprings, nanobelts, nanotubes, nanopropellers, nanodisks, and nanocombs, by different method. Among various synthesis methods, electrochemical deposition represents a simple and inexpensive solution based method for synthesis of semiconductor nanostructures. In this study, the electrodeposition method was used to produce zinc oxide (ZnO) nanostructures on fluorine-doped tin oxide (FTO)-coated conducting glass substrate as TCO from chloride bath. We present a systematic study on the effects of the concentration of chloride anion on the properties of ZnO. The influence of KCl concentrations on the electrodeposition process, morphological, structural and optical properties of ZnO nanostructures was examined. In this research electrochemical deposition of ZnO nanostructures is investigated using conventional electrochemical measurements (cyclic voltammetry and Mott-Schottky), scanning electron microscopy (SEM), and X-ray diffraction (XRD) techniques. The potentials of electrodeposition of ZnO were determined using the cyclic voltammetry. From the Mott-Schottky measurements, the flat-band potential and the donor density for the ZnO nanostructure are determined. SEM images shows different size and morphology of the nanostructures and depends greatly on the KCl concentrations. The morphology of ZnO nanostructures is determined by the corporated action between [Zn(NO3)2] and [Cl-].Very netted hexagonal grains are observed for the nanostructures deposited at 0.1M of KCl. XRD studies revealed that the all deposited films were polycrystalline in nature with wurtzite phase. The electrodeposited thin films are found to have preferred oriented along (002) plane of the wurtzite structure of ZnO with c-axis normal to the substrate surface for sample at different concentrations of KCl. UV-Visible spectra showed a significant optical transmission (~80%), which decreased with low Cl-1 concentrations. The energy band gap values have been estimated to be between 3.52 and 3.80 eV.

Keywords: electrodeposition, ZnO, chloride ions, Mott-Schottky, SEM, XRD

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Authors: Mohamed A. Baba, Gazy Rodowan, Brigita Abakevičienė, Sigitas Tamulevičius, Bartlomiej Lemieszek, Sebastian Molin, Tomas Tamulevičius

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Solid oxide fuel cells (SOFC) efficiently convert hydrogen to energy without producing any disturbances or contaminants. The core of the cell is electrolyte. For improving the performance of electrolyte-supported cells, it is desirable to extend the available exchange surface area by micro-structuring of the electrolyte with laser-based micromachining. This study investigated the electrochemical performance of cells micro machined using a femtosecond laser. Commercial ceramic SOFC (Elcogen, AS) with a total thickness of 400 μm was structured by 1030 nm wavelength Yb: KGW fs-laser Pharos (Light Conversion) using 100 kHz repetition frequency and 290 fs pulse length light by scanning with the galvanometer scanner (ScanLab) and focused with a f-Theta telecentric lens (SillOptics). The sample height was positioned using a motorized z-stage. The microstructures were formed using a laser spiral trepanning in Ni/YSZ anode supported membrane at the central part of the ceramic piece of 5.5 mm diameter at active area of the cell. All surface was drilled with 275 µm diameter holes spaced by 275 µm. The machining processes were carried out under ambient conditions. The microstructural effects of the femtosecond laser treatment on the electrolyte surface were investigated prior to the electrochemical characterisation using a scanning electron microscope (SEM) Quanta 200 FEG (FEI). The Novo control Alpha-A was used for electrochemical impedance spectroscopy on a symmetrical cell configuration with an excitation amplitude of 25 mV and a frequency range of 1 MHz to 0.1 Hz. The fuel cell characterization of the cell was examined on open flanges test setup by Fiaxell. Using nickel mesh on the anode side and au mesh on the cathode side, the cell was electrically linked. The cell was placed in a Kittec furnace with a Process IDentifier temperature controller. The wires were connected to a Solartron 1260/1287 frequency analyzer for the impedance and current-voltage characterization. In order to determine the impact of the anode's microstructure on the performance of the commercial cells, the acquired results were compared to cells with unstructured anode. Geometrical studies verified that the depth of the -holes increased linearly according to laser energy and scanning times. On the other hand, it reduced as the scanning speed increased. The electrochemical analysis demonstrates that the open circuit voltage OCV values of the two cells are equal. Further, the modified cell's initial slope reduces to 0.209 from 0.253 of the unmodified cell, revealing that the surface modification considerably decreases energy loss. Plus, the maximum power density for the cell with the microstructure and the reference cell respectively, are 1.45 and 1.16 Wcm⁻².

Keywords: electrochemical performance, electrolyte-supported cells, laser micro-structuring, solid oxide fuel cells

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Authors: O. Çomaklı, M. Yazıcı, T. Yetim, A. F. Yetim, A. Çelik

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In this work, TiO₂ films were deposited on Cp-Ti substrates by thermal oxidation, DC plasma oxidation, and by the sol-gel method. Microstructures of uncoated and TiO₂ film coated samples were examined by X-ray diffraction and SEM. Thin oxide film consisting of anatase (A) and rutile (R) TiO₂ structures was observed on the surface of CP-Ti by under three different treatments. Also, the more intense anatase and rutile peaks appeared at samples plasma oxidized at 700˚C. The thicknesses of films were about 1.8 μm at the TiO₂ film coated samples by sol-gel and about 2.7 μm at thermal oxidated samples, while it was measured as 3.9 μm at the plasma oxidated samples. Electrochemical corrosion behaviour of uncoated and coated specimens was mainly carried out by potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) in simulated body fluid (SBF) solution. Results showed that at the plasma oxidated samples exhibited a better resistance property to corrosion than that of other treatments.

Keywords: TiO₂, CP-Ti, corrosion properties, thermal oxidation, plasma oxidation, sol-gel

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Authors: Jafar Khan Kasi, Ajab Khan Kasi, Muzamil Bokhari

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Carbon nanotube is one of the most attractive materials for the potential applications of nanotechnology due to its excellent mechanical, thermal, electrical and optical properties. In this paper we report a supercapacitor made of nickel foil electrodes, coated with multiwall carbon nanotubes (MWCNTs) thin film using electrophoretic deposition (EPD) method. Chemical vapor deposition method was used for the growth of MWCNTs and ethanol was used as a hydrocarbon source. High graphitic multiwall carbon nanotube was found at 750 C analyzing by Raman spectroscopy. We observed the electrochemical performance of supercapacitor by cyclic voltammetry. The electrodes of supercapacitor fabricated from MWCNTs exhibit considerably small equivalent series resistance (ESR), and a high specific power density. Electrophoretic deposition is an easy method in fabricating MWCNT electrodes for high performance supercapacitor.

Keywords: carbon nanotube, chemical vapor deposition, catalyst, charge, cyclic voltammetry

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Authors: Ramon Alberto Paredes Camacho, Li Lu

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Sustainable batteries are possible through the development of cheaper and greener alternatives whose most feasible option is epitomized by Sodium-Ion Batteries (SIB). Na₃V₂(PO₄)₂F₃ (NVPF) an important member of the Na-superionic-conductor (NASICON) materials, has recently been in the spotlight due to its interesting electrochemical properties when used as cathode namely, high specific capacity of 128 mA h g-¹, high energy density of 507 W h Kg-¹, increased working potential at which vanadium redox couples can be activated (with an average value around 3.9 V), and small volume variation of less than 2%. These traits grant NVPF an excellent perspective as a cathode material for the next generation of sodium batteries. Unfortunately, because of its low inherent electrical conductivity and a high energy barrier that impedes the mobilization of all the available Na ions per formula, the overall electrochemical performance suffers substantial degradation, finally obstructing its industrial use. Many approaches have been developed to remediate these issues where nanostructural design, carbon coating, and ion doping are the most effective ones. This investigation is focused on enhancing the electrochemical response of NVPF by doping metal ions in the crystal lattice, substituting vanadium atoms. A facile sol-gel process is employed, with citric acid as the chelator and the carbon source. The optimized conditions circumvent fluorine sublimation, ratifying the material’s purity. One of the reasons behind the large ionic improvement is the attraction of extra Na ions into the crystalline structure due to a charge imbalance produced by the valence of the doped ions (+2), which is lower than the one of vanadium (+3). Superior stability (higher than 90% at a current density of 20C) and capacity retention at an extremely high current density of 50C are demonstrated by our doped NVPF. This material continues to retain high capacity values at low and high temperatures. In addition, full cell NVPF//Hard Carbon shows capacity values and high stability at -20 and 60ºC. Our doping strategy proves to significantly increase the ionic and electronic conductivity of NVPF even at extreme conditions, delivering outstanding electrochemical performance and paving the way for advanced high-potential cathode materials.

Keywords: sodium-ion batteries, cathode materials, NASICON, Na3V2(PO4)2F3, Ion doping

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Authors: Sujit Kumar Guchhait, Subir Paul

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One of the major research areas is to find an alternative source of energy to fulfill the energy crisis and environmental problems. The Fuel cell is such kind of energy producing unit. Use of fuel cell to produce renewable energy for commercial purpose is limited by the high cost of Pt based electrode material. Development of high energetic, as well as inexpensive fuel cell electrode materials, is needs of hour to produce clean energy using derive bio-fuel. In this present investigation, inexpensive Cu-Ni-CeO2 electrode material has been synthesized by using pulse current. The surface morphology of the electrode materials is controlled by several deposition parameters to increase the rate of electrochemical oxidation of alcoholic fuel, ethanol. The electrochemical characterization of the developed material was done by Cyclic Voltammetry (CV) and Chronoamperometry (CA) and Electrochemical Impedance Spectroscopy test. It is interesting to find that both these materials have shown high electrocatalytic properties in terms of high exchange current density (I0), low polarization resistance (Rp) and low impedance. It is seen that the addition of CeO2 to Ni-Cu has outperformed Pt as far as high electrocatalytic properties are concerned. The exchange current density on the Cu-Ni-CeO2 electrode surface for ethanol oxidation is about eight times higher than the same on the Pt surface with much lower polarization resistance than the later. The surface morphology of the electrode materials has been revealed by Field Effect Scanning Electron Microscope (FESEM). It is seen that grains are narrow and subspherical with 3D surface containing pores in between two elongated grains. XRD study exhibits the presence of Ni and CeO2 on the Cu surface.

Keywords: electro-catalyst, alcoholic fuel, cyclic voltammetry, potentiodynamic polarization, EIS, XRD, SEM

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Authors: Navpreet Kaur, Himkusha Thakur, Nirmal Prabhakar

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One of the most publicized and controversial issue in crop production is the use of agrichemicals- also known as pesticides. This is evident in many reports that Organophosphate (OP) insecticides, among the broad range of pesticides are mainly involved in acute and chronic poisoning cases. Therefore, detection of OPs is very necessary for health protection, food and environmental safety. In our study, a nanocomposite of poly (3,4 ethylenedioxythiophene) (PEDOT) and multi-walled carbon nanotubes (MWCNTs) has been deposited electrochemically onto the surface of fluorine doped tin oxide sheets (FTO) for the analysis of malathion OP. The -COOH functionalization of MWCNTs has been done for the covalent binding with amino groups of AChE enzyme. The use of PEDOT-MWCNT films exhibited an excellent conductivity, enables fast transfer kinetics and provided a favourable biocompatible microenvironment for AChE, for the significant malathion OP detection. The prepared PEDOT-MWCNT/FTO and AChE/PEDOT-MWCNT/FTO nano-biosensors were characterized by Fourier transform infrared spectrometry (FTIR), Field emission-scanning electron microscopy (FE-SEM) and electrochemical studies. Electrochemical studies were done using Cyclic Voltammetry (CV) or Differential Pulse Voltammetry (DPV) and Electrochemical Impedance Spectroscopy (EIS). Various optimization studies were done for different parameters including pH (7.5), AChE concentration (50 mU), substrate concentration (0.3 mM) and inhibition time (10 min). The detection limit for malathion OP was calculated to be 1 fM within the linear range 1 fM to 1 µM. The activity of inhibited AChE enzyme was restored to 98% of its original value by 2-pyridine aldoxime methiodide (2-PAM) (5 mM) treatment for 11 min. The oxime 2-PAM is able to remove malathion from the active site of AChE by means of trans-esterification reaction. The storage stability and reusability of the prepared nano-biosensor is observed to be 30 days and seven times, respectively. The application of the developed nano-biosensor has also been evaluated for spiked lettuce sample. Recoveries of malathion from the spiked lettuce sample ranged between 96-98%. The low detection limit obtained by the developed nano-biosensor made them reliable, sensitive and a low cost process.

Keywords: PEDOT-MWCNT, malathion, organophosphates, acetylcholinesterase, nano-biosensor, oxime (2-PAM)

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Authors: Maxim Panov, Evgenia Khairullina, Sergey Ermakov, Oleg Gundobin, Vladimir Kochemirovsky

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The continuous in situ laser-induced catalysis proceeding via generation and growth of nano-sized copper particles was discussed. Also, the simple and lost-cost method for manufacturing of microstructural copper electrodes was proposed. The electrochemical properties of these electrodes were studied by cyclic voltammetry and impedance spectroscopy. The surface of the deposited copper structures (electrodes) was investigated by X-ray photoelectron spectroscopy and atomic force microscopy. These microstructures are highly conductive and porous with a dispersion of pore size ranging from 50 nm to 50 μm. An analytical response of the fabricated copper electrode is 30 times higher than those observed for a pure bulk copper with similar geometric parameters. A study of sensory characteristics for hydrogen peroxide determination showed that the value of Faraday current at the fabricated copper electrode is 2-2.5 orders of magnitude higher than for etalon one.

Keywords: laser-induced deposition, electrochemical electrodes, non-enzymatic sensors, copper

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Authors: Mohamed Ben Rabha

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In this paper, we report on the effect of porous silicon (PS) treatment on the surface passivation of monocrystalline silicon (c-Si). PS film with a thickness of 80 nm was deposited by stain etching. It was demonstrated that PS coating is a very interesting solution for surface passivation. The level of surface passivation is determined by techniques based on photoconductance and FTIR. As a results, the effective minority carrier lifetime increase from 2 µs to 7 µs at ∆n=1015 cm-3 and the reflectivity reduce from 28 % to about 7 % after PS coating.

Keywords: porous silicon, effective minority carrier lifetime, reflectivity

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Authors: Anju Joshi, C. N. Tharamani

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Diabetes is one of the leading cause of death at present and remains an important concern as the prevalence of the disease is increasing at an alarming rate. Therefore, it is crucial to diagnose the accurate levels of glucose for developing an efficient therapeutic for diabetes. Due to the availability of convenient and compact self-testing, continuous monitoring of glucose is feasible nowadays. Enzyme based electrochemical sensing of glucose is quite popular because of its high selectivity but suffers from drawbacks like complicated purification and immobilization procedures, denaturation, high cost, and low sensitivity due to indirect electron transfer. Hence, designing a robust enzyme free platform using transition metal oxides remains crucial for the efficient and sensitive determination of glucose. In the present work, manganese doped nickel oxide nanoparticles (Mn-NiO) has been synthesized onto the surface of multiwalled carbon nanotubes using a simple microwave assisted approach for non-enzymatic electrochemical sensing of glucose. The morphology and structure of the synthesized nanostructures were characterized using scanning electron microscopy (SEM) and X-Ray diffraction (XRD). We demonstrate that the synthesized nanostructures show enormous potential for electrocatalytic oxidation of glucose with high sensitivity and selectivity. Cyclic voltammetry and square wave voltammetry studies suggest superior sensitivity and selectivity of Mn-NiO decorated carbon nanotubes towards the non-enzymatic determination of glucose. A linear response between the peak current and the concentration of glucose has been found to be in the concentration range of 0.01 μM- 10000 μM which suggests the potential efficacy of Mn-NiO decorated carbon nanotubes for sensitive determination of glucose.

Keywords: diabetes, glucose, Mn-NiO decorated carbon nanotubes, non-enzymatic

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Authors: M. Mominul Haque, Danny KY. Wong

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In this paper, we will demonstrate the feasibility of selectively removing the azo dye, Acid Red 1, in the presence of a second dye, Indigo Carmine, at conducting polypyrrole films. A long-term goal of this work is to develop an efficient and effective electrochemical treatment of textile effluents that does not yield any toxic by-products. Specifically, pyrrole was initially electrochemically oxidised in the presence of Acid Red 1 to prepare an Acid Red 1-entrapped polypyrrole film. Next, the Acid Red 1 entrapped film was electrochemically reduced to expel the dye from the film. The film was then ready for use in removing the dye in an Acid Red 1 solution. The entrapment efficiency of the film was then studied by spectroscopically determining the change in the absorbance of the dye solution. These experiments were repeated using Indigo Carmine or a mixture of Acid Red 1 and Indigo Carmine, in place of Acid Red 1. Therefore, this has given rise to an environmentally friendly treatment method for textile effluents. In our work, we have also studied the characteristics of Acid Red 1- and Indigo Carmine-entrapped polypyrrole films by scanning electron microscopy, X-ray diffraction and Fourier transfer infrared spectroscopy.

Keywords: azo dye, electrochemical treatment, polypyrrole, Acid Red 1

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Authors: Desplanches Maxime

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Accurate estimation of the remaining useful life of lithium-ion batteries for electronic devices is crucial. Data-driven methodologies encounter challenges related to data volume and acquisition protocols, particularly in capturing a comprehensive range of aging indicators. To address these limitations, we propose a hybrid approach that integrates an electrochemical model with state-of-the-art data analysis techniques, yielding a comprehensive database. Our methodology involves infusing an aging phenomenon into a Newman model, leading to the creation of an extensive database capturing various aging states based on non-destructive parameters. This database serves as a robust foundation for subsequent analysis. Leveraging advanced data analysis techniques, notably principal component analysis and t-Distributed Stochastic Neighbor Embedding, we extract pivotal information from the data. This information is harnessed to construct a regression function using either random forest or support vector machine algorithms. The resulting predictor demonstrates a 5% error margin in estimating remaining battery life, providing actionable insights for optimizing usage. Furthermore, the database was built from the Newman model calibrated for aging and performance using data from a European project called Teesmat. The model was then initialized numerous times with different aging values, for instance, with varying thicknesses of SEI (Solid Electrolyte Interphase). This comprehensive approach ensures a thorough exploration of battery aging dynamics, enhancing the accuracy and reliability of our predictive model. Of particular importance is our reliance on the database generated through the integration of the electrochemical model. This database serves as a crucial asset in advancing our understanding of aging states. Beyond its capability for precise remaining life predictions, this database-driven approach offers valuable insights for optimizing battery usage and adapting the predictor to various scenarios. This underscores the practical significance of our method in facilitating better decision-making regarding lithium-ion battery management.

Keywords: Li-ion battery, aging, diagnostics, data analysis, prediction, machine learning, electrochemical model, regression

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Authors: H. Farokhi, A. Bahadoran

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This paper is focused on the absorbance and magnetic properties of a novel nanocomposite based on conducting polymer, carbon black and barium hexaferrite in epoxy resin on the E-glass fibre substrate. The highly conductive nanocomposite was provided by in-situ polymerization of aniline in the presence of carbon black (C) and barium hexaferrite (BaFe12O19) as electromagnetic absorbance material. The structure, morphology, and magnetic properties of samples were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). SEM images showed the uniformly coated PAni on the surface of carbon black and barium hexaferrite. XRD peaks also verified the presence of carbon black and barium hexaferrite in the nanocomposite. The microwave characteristics determined from the magnetic and dielectric properties of the elastomeric composites obtained from scattering data by fitting the samples in a waveguide, where measured in the frequency in X-band frequency range, the range of 8 to 12 GHz. The reflection losses were evaluated to be less than −5dB over the whole X-band frequency (8–12 GHz) for the thickness of 1.4mm.

Keywords: conductive polymer, magnetic materials, capacitance, electrochemical cell

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Authors: Yu-Jen Shih, Juan-Zhang Lou

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Nitrogenous compounds, such as NH4+/NH3 and NO3-, have become important contaminants in water resources. Excessive concentration of NH3 leads to eutrophication, which poses a threat to aquatic organisms in the environment. Electrochemical oxidation emerged as a promising water treatment technology, offering advantages such as simplicity, small-scale operation, and minimal reliance on additional chemicals. In this study, a nickel-based metal-organic framework (Ni-MOF) was synthesized using 2-amino terephthalic acid (BDC-NH2) and nickel nitrate. The Ni-MOF was further carbonized as derived nickel oxide and nitrogen-carbon composite, Ni/NiOx/NC. The nickel oxide within the 2D porous carbon texture served as active sites for ammonia oxidation. Results of characterization showed that the Ni-MOF was a hexagonal and flaky nanoparticle. With increasing carbonization temperature, the nickel ions in the organic framework re-crystallized as NiO clusters on the surfaces of the 2D carbon. The electrochemical surface area of Ni/NiOx/NC significantly increased as to improve the efficiency of ammonia oxidation. The phase transition of Ni(OH)2⇌NiOOH at around +0.8 V was the primary mediator of electron transfer. Batch electrolysis was conducted under constant current and constant potential modes. The electrolysis parameters included pyrolysis temperatures, pH, current density, initial feed concentration, and electrode potential. The constant current batch experiments indicated that via carbonization at 800 °C, Ni/NiOx/NC(800) was able to decrease the ammonium nitrogen of 50 mg-N/L to below 1 ppm within 4 hours at a current density of 3 mA/cm2 and pH 11 with negligible oxygenated nitrogen formation. The constant potential experiments confirmed that N2 nitrogen selectivity was enhanced up to 90% at +0.8 V.

Keywords: electrochemical oxidation, nickel oxyhydroxide, metal-organic framework, ammonium, nitrate

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Authors: Majid Farsadrouh Rashti, Parisa Jahani, Amir Shafiee, Mehrdad Mofidi

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The dihydroxybenzene isomers, hydroquinone (HQ), catechol (CC) and resorcinol (RS) have been widely recognized as important environmental pollutants due to their toxicity and low degradability in the ecological environment. Speciation of HQ, CC and RS is very important for environmental analysis because they co-exist of these isomers in environmental samples and are too difficult to degrade as an environmental contaminant with high toxicity. There are many analytical methods have been reported for detecting these isomers, such as spectrophotometry, fluorescence, High-performance liquid chromatography (HPLC) and electrochemical methods. These methods have attractive advantages such as simple and fast response, low maintenance costs, wide linear analysis range, high efficiency, excellent selectivity and high sensitivity. A novel modified glassy carbon electrode (GCE) with Pd@ Cu/CNTs core−shell nanowires for the simultaneous determination of hydroquinone (HQ), catechol (CC) and resorcinol (RS) is described. A detailed investigation by field emission scanning electron microscopy and electrochemistry was performed in order to elucidate the preparation process and properties of the GCE/ Pd/CuNWs-CNTs. The electrochemical response characteristic of the modified GPE/LFOR toward HQ, CC and RS were investigated by cyclic voltammetry, differential pulse voltammetry (DPV) and Chronoamperometry. Under optimum conditions, the calibrations curves were linear up to 228 µM for each with detection limits of 0.4, 0.6 and 0.8 µM for HQ, CC and RS, respectively. The diffusion coefficient for the oxidation of HQ, CC and RS at the modified electrode was calculated as 6.5×10⁻⁵, 1.6 ×10⁻⁵ and 8.5 ×10⁻⁵ cm² s⁻¹, respectively. DPV was used for the simultaneous determination of HQ, CC and RS at the modified electrode and the relative standard deviations were 2.1%, 1.9% and 1.7% for HQ, CC and RS, respectively. Moreover, GCE/Pd/CuNWs-CNTs was successfully used for determination of HQ, CC and RS in real samples.

Keywords: dihydroxybenzene isomers, galvanized copper nanowires, electrochemical sensor, Palladium, speciation

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Authors: Olfat E. El-Azabawy, Enas M. Attia, Nadia Shawky, Amira M. Hypa

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In this work, an attempt is made to study the effects of orange peel extract (OPE) as an environment-friendly corrosion inhibitor for carbon steel (CS) within a formation water solution (FW). The study was performed in different concentrations (0.5-2.5% (v/v)) of peel extracts at ambient temperatures (25oC) and (2.5% (v/v)) at temperature range (25- 55 oC) by weight loss measurements, open circuit potential, potentiodynamic polarization and electrochemical impedance. The inhibition efficiency was calculated from all measurements and confirmed by energy-dispersive X-ray spectroscopy (EDS). Inhibition was found to increase with increasing inhibitors concentration and decrease with increasing temperature. It was seen that IE% is about 92.84% in the presence of 2.5% (v/v) of orange peel inhibitor by using weight loss method. The adsorption process was of physical type and obey Langmuir adsorption isotherm. Also, adsorption, as well as the inhibition process, followed first-order kinetics at all concentrations.

Keywords: eco-friendly corrosion inhibitor, OPE, oilfield water, electrochemical impedance

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Authors: Ingy N. Bkrey, Ahmed A. Moniem

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We succeeded to produce a high performance and flexible graphene/Manganese dioxide (G/MnO2) electrode coated on flexible polyethylene terephthalate (PET) substrate. The graphene film is initially synthesized by drop-casting the graphene oxide (GO) solution on the PET substrate, followed by simultaneous reduction and patterning of the dried film using carbon dioxide (CO2) laser beam with power of 1.8 W. Potentiostatic Anodic Deposition method was used to deposit thin film of MnO2 with different loading mass 10 – 50 and 100 μg.cm-2 on the pre-prepared graphene film. The electrodes were fully characterized in terms of structure, morphology, and electrochemical performance. A maximum specific capacitance of 973 F.g-1 was attributed when depositing 50 μg.cm-2 MnO2 on the laser reduced graphene oxide rGO (or G/50MnO2) and over 92% of its initial capacitance was retained after 1000 cycles. The good electrochemical performance and long-term cycling stability make our proposed approach a promising candidate in the supercapacitor applications.

Keywords: electrode deposition, flexible, graphene oxide, graphene, high power CO2 Laser, MnO2

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Authors: Monika Sogani, Zainab Syed, Adrian C. Fisher

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Pollution of estrogenic compounds has caught the attention of researchers as the slight increase of estrogens in the water bodies has a significant impact on the aquatic system. They belong to a class of endocrine disrupting compounds (EDCs) and are able to mimic hormones or interfere with the action of endogenous hormones. The microbial electrochemical remediation system (MERS) is employed here for exploiting an electrophototrophic bacterium for evaluating the capacity of biodegradation of ethinylestradiol hormone (EE2) under anaerobic conditions with power generation. MERS using electro-phototrophic bacterium offers a tailored solution of wastewater treatment in a developing country like India which has a huge solar potential. It is a clean energy generating technology as they require only sunlight, water, nutrients, and carbon dioxide to operate. Its main feature that makes it superior over other technologies is that the main fuel for this MERS is sunlight which is indefinitely present. When grown in light with organic compounds, these photosynthetic bacteria generate ATP by cyclic photophosphorylation and use carbon compounds to make cell biomass (photoheterotrophic growth). These cells showed EE2 degradation and were able to generate hydrogen as part of the process of nitrogen fixation. The two designs of MERS were studied, and a maximum of 88.45% decrease in EE2 was seen in a total period of 14 days in the better design. This research provides a better insight into microbial electricity generation and self-sustaining wastewater treatment facilities. Such new models of waste treatment aiming waste to energy generation needs to be followed and implemented for building a resource efficient and sustainable economy.

Keywords: endocrine disrupting compounds, ethinylestradiol, microbial electrochemical remediation systems, wastewater treatment

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Authors: Abdur Rahim, Lauro Tatsuo Kubota, Yoshitaka Gushikem

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Carbon ceramic mesoporous SiO2/50wt%C (SBET= 170 m2g-1), where C is graphite, was prepared by the sol gel method. Scanning electron microscopy images and the respective element mapping showed that, within the magnification used, no phase segregation was detectable. It presented the electric conductivities of 0.49 S cm-1. This material was used to support cobalt phthalocyanine, prepared in situ, to assure a homogeneous dispersion of the electro active complex in the pores of the matrix. The surface density of cobalt phthalocyanine, on the matrix surfaces was 0.015 mol cm-2. Pressed disk, made with SiO2/50wt%C/CoPc, was used to fabricate an electrode and tested as sensors for nitrite determination by electro chemical technique. A linear response range between 0.039 and 0.42 mmol l−1,and correlation coefficient r=0.9996 was obtained. The electrode was chemically very stable and presented very high sensitivity for this analyte, with a limit of detection, LOD = 1.087 x 10-6 mol L-1.

Keywords: SiO2/C/CoPc, sol-gel method, electrochemical sensor, nitrite oxidation, carbon ceramic material, cobalt phthalocyanine

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Authors: Amandeep Singh Oberoi, John Andrews, Alan L. Chaffee, Lachlan Ciddor

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Electrochemical storage of hydrogen in activated carbon electrodes as part of a reversible fuel cell offers a potentially attractive option for storing surplus electrical energy from inherently variable solar and wind energy resources. Such a system – which we have called a proton flow battery – promises to have roundtrip energy efficiency comparable to lithium ion batteries, while having higher gravimetric and volumetric energy densities. Activated carbons with high internal surface area, high pore volume, light weight and easy availability have attracted considerable research interest as a solid-state hydrogen storage medium. This paper compares the physical characteristics and hydrogen storage capacities of four activated carbon electrodes made by different methods from brown coal. The fabrication methods for these samples are explained. Their proton conductivity was measured using electrochemical impedance spectroscopy, and their hydrogen storage capacity by galvanostatic charging and discharging in a three-electrode electrolytic cell with 1 mol sulphuric acid as electrolyte. The highest hydrogen storage capacity obtained was 1.29 wt%, which compares favourably with metal hydrides used in commercially available solid-state hydrogen storages. The hydrogen storage capacity of the samples increased monotonically with increasing BET surface area (calculated from CO2 adsorption method). The results point the way towards selecting high-performing electrodes for proton flow batteries that the competitiveness of this energy storage technology.

Keywords: activated carbon, electrochemical hydrogen storage, proton flow battery, proton conductivity

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Authors: David Polcari, Samuel C. Perry, Loredano Pollegioni, Matthias Geissler, Janine Mauzeroll

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ᴅ-serine acts as an endogenous co-agonist for N-methyl-ᴅ-aspartate receptors in neuronal synapses. This makes it a key component in the development and function of a healthy brain, especially given its role in several neurodegenerative diseases such as Alzheimer’s disease and dementia. Despite such clear research motivations, the primary site and mechanism of ᴅ-serine release is still currently unclear. For this reason, we are developing a biosensor for the detection of ᴅ-serine utilizing a microelectrode in combination with a ᴅ-amino acid oxidase enzyme, which produces stoichiometric quantities of hydrogen peroxide in response to ᴅ-serine. For the fabrication of a biosensor with good selectivity, we use a permselective poly(meta-phenylenediamine) film to ensure only the target molecule is reacted, according to the size exclusion principle. In this work, we investigated the effect of the electrodeposition conditions used on the biosensor’s response time and selectivity. Careful optimization of the fabrication process allowed for enhanced biosensor response time. This allowed for the real time sensing of ᴅ-serine in a bulk solution, and also provided in means to map the efflux of ᴅ-serine in real time. This was done using scanning electrochemical microscopy (SECM) with the optimized biosensor to measure localized release of ᴅ-serine from an agar filled glass capillary sealed in an epoxy puck, which acted as a model system. The SECM area scan simultaneously provided information regarding the rate of ᴅ-serine flux from the model substrate, as well as the size of the substrate itself. This SECM methodology, which provides high spatial and temporal resolution, could be useful to investigate the primary site and mechanism of ᴅ-serine release in other biological samples.

Keywords: ᴅ-serine, enzymatic biosensor, microelectrode, scanning electrochemical microscopy

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Authors: M.S. Ashraf, Raja Rizwan Hussain, A. M. Alhozaimy

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The effect of supplementary cementitious materials (SCMs) with concrete pore solution on the protective properties of the oxide films that form on reinforcing steel bars has been experimentally investigated using electrochemical impedance spectroscopy (EIS) and Tafel Scan. The tests were conducted on oxide films grown in saturated calcium hydroxide solutions that included different representative amounts of NaOH and KOH. In addition to that, commonly used supplementary cementitious materials (natural pozzolan and fly ash) were also added. The results of electrochemical tests show that supplementary cementitious materials do have an effect on the protective properties of the passive oxide film. In particular, natural pozzolans has been shown to have a highly positive influence on the film quality. Fly ash also increases the protective qualities of the passive film.

Keywords: supplementary cementitious materials (SCMs), passive film, EIS, Tafel scan, rebar, concrete, simulated concrete pore solution (SPS)

Procedia PDF Downloads 417