• Title/Summary/Keyword: anodic oxidation

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Electrolytic Synthesis of 9-Methyl-2,3,6,7-tetramethoxyfluorene with Carbon Electrodes (카본전극을 이용한 9-Methyl-2,3,6,7-tetramethoxyfluorene의 합성)

  • Kim, Duk-Hyun
    • Applied Chemistry for Engineering
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    • v.8 no.1
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    • pp.39-48
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    • 1997
  • The intramolecular cyclization of 1,1-bis-(3,4-dimethoxyphenyl)ethane was shown to take place upon anodic oxidation at carbon electrodes in acetonitrile or in a solvent-mixture containing dichloromethane, trifluoroacetic acid(TFA). Yields are low in the former solvent due to the fact that the cyclized product (9-methyl-2,3,6,7-tetramethoxyfluorene) is more easily oxidized than it's precursor and the oxidation product is not stable. In the presence of TFA, the cation radical derived from the oxidation of the cyclized product is stabilized thus, after reduction may be isolated with better yields.

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Electro-oxidation of Cyclohexanol on a Copper Electrode Modified by Copper-dimethylglyoxime Complex Formed by Electrochemical Synthesis

  • Hasanzadeh, Mohammad.;Shadjou, Nasrin.;Saghatforoush, Lotfali.;Khalilzadeh, Balal.;Kazeman, Isa.
    • Bulletin of the Korean Chemical Society
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    • v.30 no.12
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    • pp.2943-2948
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    • 2009
  • Copper-dimethylglyoxime complex (CuDMG) modified Copper electrode (Cu/CuDMG) showed a catalytic activity towards cyclohexanol oxidation in NaOH solution. The modified electrode prepared by the dimethylglyoxime anodic deposition on Cu electrode in the solution contained 0.20 M $NH_4Cl\;+\;NH_4OH\;(pH\;9.50)\;and\;1\;{\times}\;10^{-4}$ M dimethylglyoxime. The modified electrode conditioned by potential recycling in a potential range of -900${\sim}$900 mV vs. Ag/AgCl by cyclic voltammetry in alkaline medium (1 M NaOH). The results show that the CuDMG film on the electrode behaves as an efficient catalyst for the electro-oxidation of cyclohexanol in alkaline medium via Cu (III) species formed on the electrode.

Fabrication of Plasma Electrolytic Oxidation Coatings on Magnesium AZ91D Casting Alloys

  • Lee, Sung-Hyung;Yashiro, Hitoshi;Kure-Chu, Song-Zhu
    • Journal of the Korean institute of surface engineering
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    • v.50 no.6
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    • pp.432-438
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    • 2017
  • AZ91D casting alloy requires an advanced plasma anodizing processing because large amount of defects are liable to generate during anodization. In this study, plasma electrolytic oxidation (PEO) of AZ91D Mg alloy was conducted by the application of either constant voltage or current using a pulse mode and its effects on pore formation, surface roughness and corrosion resistance were investigated. The PEO films showed a three-layer structure. The PEO film thickness was found to increase linearly with voltage. The surface roughness, Ra, ranged between $0.2{\mu}m$ and $0.3{\mu}m$. The corrosion resistance increased from RN 3.5 to 9.5 by the PEO treatment when evaluated according to the 72 hour salt spray test. The PEO-treated surface exhibited higher pitting potential than the raw material.

Detection of Trace Copper Metal at Carbon Nanotube Based Electrodes Using Squarewave Anodic Stripping Voltammetry

  • Choi, Changkun;Jeong, Youngsam;Kwon, Yongchai
    • Bulletin of the Korean Chemical Society
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    • v.34 no.3
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    • pp.801-809
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    • 2013
  • We investigate sensitivity and limit of detection (LOD) of trace copper (Cu) metal using pristine carbon nanotube (CNT) and acidified CNT (ACNT) electrodes. Squarewave based anodic stripping voltammetry (SWASV) is used to determine the stripped Cu concentration. Prior to performing the SWASV measurements, its optimal conditions are determined and with that, effects of potential scan rate and $Cu^{2+}$ concentration on stripping current are evaluated. The measurements indicate that (1) ACNT electrode shows better results than CNT electrode and (2) stripping is controlled by surface reaction. In the given $Cu^{2+}$ concentration range of 25-150 ppb, peak stripping current has linearity with $Cu^{2+}$ concentration. Quantitatively, sensitivity and LOD of Cu in ACNT electrode are 9.36 ${\mu}A\;{\mu}M^{-1}$ and 3 ppb, while their values are 3.99 ${\mu}A\;{\mu}M^{-1}$ and 3 ppb with CNT electrode. We evaluate the effect of three different water solutions (deionized water, tap water and river water) on stripping current and the confirm types of water don't affect the sensitivity of Cu. It turns out by optical inspection and cyclic voltammetry that superiority of ACNT electrode to CNT electrode is attributed to exfoliation of CNT bundles and improved interfacial adhesion occurring during oxidation of CNTs.

Fabrication of Alumina Membrane Using Anodic Oxidation Process (양극산화를 이용한 알루미나 나노세공 멤브레인의 제조)

  • Im, W.S.;Cho, K.C.;Cho, Y.S.;Choi, G.S.;Kim, D.J.
    • Korean Journal of Materials Research
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    • v.13 no.9
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    • pp.593-597
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    • 2003
  • Anodic aluminum oxide (AAO) membrane was made of aluminum sheet (99.6%, 0.2 mm thickness). The regular array of hexagonal nano pores or channels were prepared by two step anodization process. A detail description of the AAO fabrication is presented. After the 1st anodization in oxalic acid (0.3 M) at 45 V, The formed AAO was removed by etching in a solution of 6 wt% $H_3$$PO_4$+1.8 wt% $H_2$$CrO_4$. The regular arrangement of the pores was obtained by the 2nd anodization, which was carried out in the same condition as the 1st anodization. Subsequently, the alumina barrier layer at the bottom of the channel layer was removed in phosphoric acid (1M) after removing of aluminum. Pore diameter, density, and thickness could be controlled by the anodization process parameters such as applied voltage, anodizing time, pore widening time, etc. The pore diameter is proportional to the applied voltage and pore widening time. The pore density and thickness can be controlled by anodization temperature and voltage.

Integrated Microdisk Gold Electrode Modified with Metal-porphyrin and Metal-phthalocyanines for Nitric Oxide Determination in Biological Media

  • Kim, Il-Kwang;Bae, Hyun-Ok;Oh, Gi-Soo;Chung, Hun-Taeg;Kim, Young-Jin;Chun, Hyun-Ja
    • Bulletin of the Korean Chemical Society
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    • v.24 no.11
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    • pp.1579-1584
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    • 2003
  • An integrated gold microdisk electrode was constructed and modified with metal-porphyrin or metal-phthalocyanines for NO determination in biological media. Microanalysis of NO using square wave anodic stripping voltammetry in $1\;{\times}\;10^{-2}$ M $HClO_4$ was optimal when the accumulation potential was 0.1 V, frequency 100 Hz, and the scan rate was 200 mV/s. When the electrode was modified with metal-porphyrin or metal-phthalocyanines, the anodic peak currents of NO increased due to the catalytic oxidation of NO. In case of Fe(II)-phthalocyanine modified electrode, the peak currents remarkably increased and the sensitivity was high. The calibration curve had good linearity in the range from $3.6\;{\times}\;10^{-5}$ M to $7.2\;{\times}\;10^{-7}$ M, and the detection limit was $5.7\;{\times}\;10^{-7}$ M. For the structural stability and increased sensitivity, Fe(II)-phthalocyanine modified gold microdisk electrode coated with Nafion was applied to determination of NO released from cultured macrophase.

Novel Method of Poly-silicon Crystallization using Ordered Porous Anodic Alumina (정렬된 다공질 산화알루미늄을 이용한 새로운 다결정 실리콘 결정화 방법)

  • Kim, Jong-Yeon;Kim, Mi-Jung;Kim, Byoung-Yong;Oh, Byeong-Yun;Han, Jin-Woo;Han, Jeong-Min;Seo, Dae-Shik
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2007.11a
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    • pp.396-396
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    • 2007
  • Highly ordered pore structures as a template for formation of seeds have been prepared by the self-organization process of aluminum oxidation. The a-Si films were deposited on the anodic alumina films and crystallized by laser irradiation. It was found that un-melted part of fine poly-Si grain formed by explosive crystallization (EX) lead super lateral growth(SLG) and occluded with neighbor grains. The crystallized grains along the distribution of seeds were obtained. This results show a great potential for use in novel crystallization for decently uniform polycrystalline Si thin film transistors (poly-Si TFTs).

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Electrochemical Properties of Austenitic Stainless Steel with Initial Delay Time and Surface Roughness in Electropolishing Solution (전해연마 용액에서 안정화 시간과 표면 거칠기에 따른 오스테나이트 스테인리스강의 전기화학적 특성)

  • Hwang, Hyun-Kyu;Kim, Seong-Jong
    • Corrosion Science and Technology
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    • v.21 no.2
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    • pp.158-169
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    • 2022
  • The objective of this study was to investigate the electrochemical behavior and damage degree of metal surface under different conditions by performing a potentiodynamic polarization experiment using an electropolishing solution for UNS S31603 based on initial delay time and surface roughness (parameters). A second anodic peak occurred at initial delay time of 0s and 100s. However, it was not discovered at 1000s and 3600s. This research referred to an increase in current density due to hydrogen oxidation reaction among various hypotheses for the second anodic peak. After the experiment, both critical current density and corrosion current density decreased when the initial delay time (immersion time) was longer. As a result of surface analysis, characteristics of the potentiodynamic polarization behavior were similar with roughness, although the degree of damage was clearly different. With an increase in surface roughness value, the degree of surface damage was precisely observed. As such, electrochemical properties were different according to the immersion time in the electropolishing solution. To select electropolishing conditions such as applied current density, voltage, and immersion time, 1000s for initial delay time on the potentiodynamic polarization behavior was the most appropriate in this experiment.

Study on the Photocatalytic Efficiencies of $TiO_2$ ($TiO_2$의 광촉매 효율성에 관한 연구)

  • Lee, J.H.;Oh, H.J.;Jang, J.M.;Chi, C.S.
    • Analytical Science and Technology
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    • v.14 no.1
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    • pp.15-20
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    • 2001
  • Photocatalytic $TiO_2$ films were prepared by anodic oxidation at 180 V and their structural difference caused by oxidation conditions was studies. The microstructure of $TiO_2$ films in $H_2SO_4$ and $H_2SO_4/H_2O_2$ solution was mixed type of rutile and anatase. However, the $TiO_2$ layer formed in $H_2SO_4/H_3PO_4$ and $H_2SO_4/H_3PO_4/H_2O_2$ mixture was mostly anatase type. All $TiO_2$ films prepared by anodic oxidation exhibited photocatalytic properties. The photocatalytic degradation of aniline blue was first order reaction with similar rate constants at all oxidative conditions examined in this work.

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Enhanced Electrocatalytic Activity of Low Ni Content Nano Structured NiPd Electrocatalysts Prepared by Electrodeposition Method for Borohydride Oxidation

  • Zolfaghari, Mahdieh;Arab, Ali;Asghari, Alireza
    • Journal of Electrochemical Science and Technology
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    • v.11 no.3
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    • pp.238-247
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    • 2020
  • Some nano structured bimetallic NiPd electrocatalysts were electrodeposited on glassy carbon electrodes using a double potential step chronoamperometry. The morphology of the electrodeposited samples was investigated by field emission-scanning electron microscopy, while their compositions were evaluated using energy dispersive X-ray spectroscopy. It was observed that the electrodeposited samples contained a low Ni content, in the range of 0.80 - 7.10%. The electrodeposited samples were employed as the anode electro-catalysts for the oxidation of sodium borohydride in NaOH solution (1.0 M) using cyclic voltammetry, chronoamperometry, rotating disk electrode, and impedance spectroscopy. The number of exchanged electrons, charge transfer resistances, apparent rate constants, and double layer capacitances were calculated for the oxidation of borohydride on the prepared catalysts. According to the results obtained, the NiPd-2 sample with the lowest Ni content (0.80%), presented the highest catalytic activity for borohydride oxidation compared with the other NiPd samples as well as the pure Pd sample. The anodic peak current density was obtained to be about 1.3 times higher on the NiPd-2 sample compared with that for the Pd sample.