• Title/Summary/Keyword: electrochemical methods

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In-Situ Generation of Nanostructured Au Surfaces by Anodic Dissolution Followed by Cathodic Deposition (산화 용해에 연이은 환원 석출을 통한 나노구조 금 표면 형성)

  • Kweon, Suji;Choi, Suhee;Kim, Jongwon
    • Journal of the Korean Electrochemical Society
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    • v.18 no.3
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    • pp.107-114
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    • 2015
  • Electrochemical fabrication of nanostructured Au surfaces has received increased attention. In the present work, electrochemical modification of Au surfaces for fabricating nanostructured Au surfaces in the absence of externally added precursors is presented, which is different to the previous methods utilizing electrochemical deposition of externally added precursors. Application of anodic potential at Au surfaces in phosphate buffers containing $Br^-$ resulted in the anodic dissolution of Au, which produced Au precursors at the electrode surfaces. The resulting Au precursors were further reduced at the surface to produce nanostructured Au structures. The effects of applied potential and time on the morphology of Au nanostructures were systematically examined, from which a unique backbone type Au nanostructures was produced. The backbone type Au nanostructures exhibited high surface-enhanced Raman activity. The present work would give insights into the formation of electrochemical fabrication of nanostructured Au surfaces.

Lab scale electrochemical codeposition experiments for comparison to computational predictions

  • Lafreniere, Philip;Zhang, Chao;Simpson, Michael;Blandford, Edward D.
    • Nuclear Engineering and Technology
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    • v.52 no.9
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    • pp.2025-2033
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    • 2020
  • Signature-based safeguards (SBS) is being developed to assist tradition nuclear material accountancy methods in tracking material in pyroprocessing facilities. SBS involves identifying off-normal scenarios that would result in improper movement of material in a pyroprocessing facilities and determining associated sensor response signatures. SBS investigations are undertaken in the computational space utilizing an electrochemical transport code known as enhanced REFIN with anodic dissolution (ERAD) to calculate the affect of off-normal conditions in the electrorefiner (ER) on material movement. Work is undertaken to experimentally validate the predictions and assumptions made by ERAD for off-normal occurrences. These experiments were undertaken on a benchtop scale and involved operating an electrochemical cell at 10 separate current densities for constant current operations to deposit U and Gd at a W cathode. These experiments were then modeled using ERAD to compare calculated predictions versus analytical experimental results it was found. It was discovered both the experimental and calculated results reflect a trend of increased codeposition of U and Gd with increasing current density. ERAD was thus demonstrated to be useful for predicting trends from anomalous operation but will require further optimization to be utilized as a quantitative design tool.

Synthesis and Electrochemical Properties of Nanocrystalline LiFePO4 Obtained by Different Methods

  • Son, C.G.;Chang, D.R.;Kim, H.S.;Lee, Y.S.
    • Journal of Electrochemical Science and Technology
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    • v.2 no.2
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    • pp.103-109
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    • 2011
  • Nanocrystalline $LiFePO_4$ powders were prepared at 660-$670^{\circ}C$ in an Ar atmosphere using two different synthetic routes, solid-state and sol-gel. Both materials showed well-developed XRD patterns without any impurity peaks. Particles composed in the range of 200-300 nm from the solid-state method, and 50-100 nm from the sol-gel method, were confirmed through scanning electron microscopy and dynamic light scattering. The $LiFePO_4$ obtained by the sol-gel method offered a high discharge capacity (153 mAh/g) and stable discharge behavior, even at elevated temperatures (50 and $60^{\circ}C$), whereas poor electrochemical performance was observed from the solid-state method. Rate capability studies for sol gel-derived $LiFePO_4$ ranged from 0.2 to 30 C, which revealed excellent retention over 70 cycles with a 99.9% capacity.

The Inhibitor Effect of (E)-5-[(4-(benzyl(methyl)amino)phenyl)diazenyl]-1,4-dimethyl-1H-1,2,4-triazol-4-ium zinc(II) Chloride, an Industrial Cationic Azo Dye, onto Reducing Acidic Corrosion Rate of Mild Steel

  • Ozkir, Demet;Kayakirilmaz, Kadriye
    • Journal of Electrochemical Science and Technology
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    • v.11 no.3
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    • pp.257-272
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    • 2020
  • This study covers the stages of testing whether the azo dye with chemical name (E)-5-[(4-(benzyl(methyl)amino)phenyl)diazenyl]-1,4-dimethyl-1H-1,2,4-triazol-4-ium zinc (II) chloride (DMT), known as Maxilon Red GRL in the dye industry, can be used as an anticorrosive feasible inhibitory agent, especially in industrial areas other than carpet, yarn and fibre dyeing. These test stages consist of the electrochemical measurement techniques such as potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) and linear polarization resistance (LPR) for diverse concentrations and durations. The adsorption of the viewed DMT molecule on the mild steel surface obeyed the Langmuir isotherm. The zero charge potential (PZC) of mild steel was also found to assess the inhibition mechanism in containing DMT solution. The inhibition performance of DMT on the mild steel in a 1.0 M HCl solution was also investigated using methods such as metal microscope, atomic force microscope (AFM) and field emission scanning electron microscope (FE-SEM).

Electrochemical Growth of Palladium Nanowire for Highly Sensitive Hydrogen Sensor (고감도 수소센서를 위한 팔라듐 나노선의 전기화학적인 성장)

  • Jo, S.Y.;Kang, B.R.;Im, Y.H.
    • Journal of Energy Engineering
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    • v.19 no.1
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    • pp.21-24
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    • 2010
  • We present a novel electrochemical method to fabricate a single Pd nanowire based on direct current assisted dielectropheresis (DEP) process between two predefined metal electrodes. The electrochemical methods was investigated as functions of frequency and voltage for optimal growth conditions of Pd nanowire. The synthesized Pd nanowire have a good resistance of $1\;k{\Omega}$, diameters of several hundred nanometers on average and lengths of $8\;{\mu}m$. Finally, the single Pd nanowire was capable of detecting hydrogen in the concentration range from 100 to 2500 ppm with high sensitivity and response time, thus demonstrating its suitability for use as a hydrogen sensor.

Simple Preparation of Diaphorase/Polysiloxane Viologen Polymer Modified Electrode for Sensing NAD and NADH

  • Song, Ji-Eun;Hong, Zhenyu;Nagarale, Rajaram Krishna;Shin, Woon-Sup
    • Journal of Electrochemical Science and Technology
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    • v.2 no.3
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    • pp.163-167
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    • 2011
  • Nicotinamide adenine dinucleotide, $NAD^+$, and its reduced form, NADH, play important roles as coenzymes in many enzymatic reactions. Electrochemical methods for $NAD^+$ or NADH detection or generation are drawn attention because it can provide the simple and low cost platform with fairly good sensitivity. In this study, the polysiloxane viologen polymer/diaphorase/hydrophilic polyurethane (PSV/DI/HPU) modified electrodes were simply prepared and demonstrated for bio-electrocatalytic $NAD^+$ sensors. The electrodes were co-immobilized with diaphorase and polysiloxane viologen polymer as an electron mediator followed by the overcoating with HPU membrane. The mixture of the enzyme and the electron mediator was well stabilized within HPU membrane and exhibited good reversibility and stability. The sensitivity was 0.2 $nA{\cdot}{\mu}M^{-1}$ and the detection limit was 28 ${\mu}M$ with a response time of 50 s ($t_{90%}$). The capability for NADH sensor was also observed on the PSV/DI/HPU electrode.

Concurrent Electrocatalysis and Sensing of Hydrazine and Sulfite and Nitrite Ions using Electrodeposited Gold Nanostructure-Modified Electrode

  • Seo, Yeji;Manivannan, Shanmugam;Kang, Inhak;Shin, Woo-Seung;Kim, Kyuwon
    • Journal of Electrochemical Science and Technology
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    • v.8 no.1
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    • pp.25-34
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    • 2017
  • Concurrent electrocatalysis and sensing of hydrazine, sulfite ions, and nitrite ions in a mixture were studied using electrodes modified by electrodeposited Au nanostructures (NSs). The ${\beta}$-cyclodextrin-mixed silicate sol-gel composite was drop-casted on the electrode surface and nucleation guided by ${\beta}$-cyclodextrin occurred, followed by the electrodeposition of Au NSs. The additive, ${\beta}$-cyclodextrin, played an evident role as a structure-directing agent; thus, small raspberry-like Au NSs were obtained. The modified electrodes were characterized by surface characterization techniques and electrochemical methods. The Au NSs-modified electrodes effciently electrocatalyzed the oxidation of toxic molecules such as hydrazine and sulfite and nitrite ions even in the absence of any other electron transfer mediator or enzyme immobilization. Well-resolved oxidation peaks along with decreased overpotentials were noticed during the electrooxidation process. The fabricated Au nanostructured electrode clearly distinguished the electrooxidation peaks of each of the three analytes from their mixture.

Electrochemical Behavior of Mordant Red 19 and its Complexes with Light Lanthanides

  • Sang Kwon Lee;Taek Dong Chung;Song-Ju Lee;Ki-Hyung Chjo;Young Gu Ha;Ki-Won Cha;Hasuck Kim
    • Bulletin of the Korean Chemical Society
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    • v.14 no.5
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    • pp.567-574
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    • 1993
  • Mordant Red 19(MR19) is reduced at mercury electrode at -0.67 V vs. Ag/AgCl with two electrons per molecule in pH 9.2 buffer by differential pulse polarography and linear sweep voltammetry. The peak potential is dependent on the pH of solution. The exhaustive electrolysis, however, gives 4 electrons per molecule because of the disproportionation of the unstable hydrazo intermediate. The electrochemical reduction of lanthanide-MR19 complexes is observed at more cathodic potential than that of free ligand. The difference in peak potentials between complex and free ligand varies from 75 mV for $La^{3+}$ to 165 mV for $Tb^{3+}$ and increases with increasing the atomic number of lanthanide. The electrochemical reduction of lanthanide complexes with MR19 is due to the reduction of ligand itself, and it can be potentially useful as an indirect method for the determination of lanthanides. The shape of i-E curves and the scan rate dependence indicates the presence of adsorption and the adsorption was confirmed by potential double-step chronocoulometry and the effect of standing time. Also the surface excess of the adsorbed species and diffusion coefficients are determined. The composition of the complex is determined to be 1 : 2 by spectrophotometric and electrochemical methods.

Effect of KHCO3 Concentration Using CuO Nanowire for Electrochemical CO2 Reduction Reaction

  • Kanase, Rohini Subhash;Kang, Soon Hyung
    • Journal of the Microelectronics and Packaging Society
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    • v.27 no.4
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    • pp.11-17
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    • 2020
  • Copper has been proved to be the best catalyst for electrochemical CO2 reduction reaction, however, for optimal efficiency and selectivity, its performance requires improvements. Electrochemical CO2 reduction reaction (RR) using CuO nanowire electrode was performed with different concentrations of KHCO3 electrolyte (0.1 M, 0.5 M, and 1 M). Cu(OH)2 was formed on Cu foil, followed by thermal-treatment at 200℃ under the air atmosphere for 2 hrs to transform it to the crystalline phase of CuO. We evaluated the effects of different KHCO3 electrolyte concentrations on electrochemical CO2 reduction reaction (RR) using the CuO nanowire electrode. At a constant current (5mA), low concentrated bicarbonate exhibited a more negative potential -0.77 V vs. Reversible Hydrogen Electrode (RHE) (briefly abbreviated as VRHE), while the negative potential reduced to -0.33 VRHE in the high concentration of bicarbonate solution. Production of H2 and CH4 increased with an increased concentration of electrolyte (KHCO3). CH4 production efficiency was high at low negative potential whereas HCOOH was not influenced by bicarbonate concentration. Our study provides insights into efficient, economically viable, and sustainable methods of mitigating the harmful environmental effects of CO2 emission.

Channel Electrode Voltammetric and In Situ Electrochemical ESR Studies of Comproportionation of Methyl Viologen in Acetonitrile

  • Lee, Ji U;John C. Eklund;Robert A. W. Dryfe;Richard G. Compton
    • Bulletin of the Korean Chemical Society
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    • v.17 no.2
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    • pp.162-167
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    • 1996
  • Two redox processes of methyl viologen (+2/+, +/0) in acetonitrile were investigated by using channel electrode voltammetric and in situ electrochemical ESR methods. Two separated unequal plateau currents of the first (+2/+) and second (+/0) redox processes of the viologen were observed in the channel electrode voltammograms and showed a cube-root depedndence on the electrolyte flow rate, respectively. The simple Levich analysis resulted in two different diffusion coefficients of $D_{+2}=2.2{\times}10^{-5}\;cm^2/s$ and $D_+=3.0{\times}10^{-5}cm^2/s$ from the limiting currents. In situ electrochemical ESR studies were performed for the monocation radicals generated at the potentials of the two plateau currents in the electrolyte flow range $1.3{\times}10^{-1}{\geq}v_f{\geq}2.7{\times}10^{-3}\;cm^3/s$. Backward implicitfinite difference method was employed to simulate the electrochemical kinetic problem of two sequential electron transfers ($MV^{+2}+e{\leftrightarrows}MV^+,\;MV^{+}+e{\leftrightarrows}MV^0$) coupled with reversible comproportionation ($MV^{2+}+MV^0{{\leftrightarrows}^{k_f}_{k_b}}2MV^+$). $k_f$ was found to be greater than ($10^6M^{-1}s^{-1}.