• Title/Summary/Keyword: Electrochemical Characterization

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Preparation and Characterization of Dimeric Molybdenum(Ⅴ) Complexes with Bis(hydroxyethyl)dithiocarbamate (Bis(Hydroxyethyl)dithiocarbamate 의 이핵 몰리브덴 (Ⅴ) 착물 합성과 그 성질)

  • Yeh Gyung-Hak;Koo Bon-Kweon
    • Journal of the Korean Chemical Society
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    • v.34 no.5
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    • pp.452-459
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    • 1990
  • A series of oxo-and sulfido-bridged molybdenum (V) complexes, Mo$_2$O$_4$L$_2$, Mo$_2$O$_3$L$_4$, Mo$_2$O$_2$S$_2$L$_2$, and Mo$_2$OS$_3$L$_2$ [L = bis(hydroxyethyl)dithiocarbamate] have been prepared. The complexes with bridging and terminal oxo groups have been synthesized by the reactions of (PyH)$_2$MoOCl$_5$ or MoCl$_5$ and ligand in water. One of the rest two complexes, in which bridging and terminal oxo groups have been replaced by sulfido in Mo$_2$O$_4^{2+}$ core, Mo$_2$O$_2$S$_2$L$_2$ have been prepared by addition of triphenylphosphine to a chloroform solution of Mo$_2$OS$_3$L$_2$. While, Mo$_2$OS$_3$L$_2$ is obtained from aqueous solution of (NH$_4$)$_2$MoS$_4$ and ligand in the presence of sodium dithionite. The complexes are identified by elemental analysis, and spectral data of IR, UV-vis, nmr, and mass. Also, the electrochemical behaviour for the complexes in dimethylsulfoxide has been investigated by the cyclic voltammograms.

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Characterization of manganese oxide supercapacitors using carbon cloth (Carbon Cloth을 이용한 이산화망간 슈퍼커패시터 특성 연구)

  • Lee, Seung Jin;Kim, Chihoon;Ji, Taeksoo
    • Journal of Digital Contents Society
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    • v.18 no.6
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    • pp.1199-1205
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    • 2017
  • Global energy consumption is rapidly increasing yearly due to drastic industrial advances, requiring the development of new energy storage devices. For this reason, supercapacitors with fast charge-discharge, long life cycle and high power density is getting attention, and have been considered as one of the potential energy storage systems. In this research, we developed a supercapacitor that consists of amorphous manganese oxide($MnO_2$) electrodes deposited onto carbon cloth substrates using the hydrothermal method. The Fe-doped amorphous $MnO_2$ samples were characterized by X-ray diffraction(XRD), Energy Dispersive X-ray spectroscopy(EDX), as well as scanning electron microscopy(SEM). The electrochemical analysis of the prepared samples were performed using cyclic voltammetry and galvanostatic charge-discharge measurements in 1M $Na_2SO_4$ electrolyte. The test results demonstrate that the supercapacitor based on the Fe-doped amorphous $MnO_2$ electrodes has a specific capacitance as high as 163F/g at 1A/g current density, and good cycling stability of 87.34% capacitance retention up to 1000 cycles.

Synthesis and Characterization of The Electrolessly Deposited Co(Re,P) Film for Cu Capping Layer (무전해 도금법으로 제조된 Co(Re,P) capping layer제조 및 특성 평가)

  • Han, Won-Kyu;Kim, So-Jin;Ju, Jeong-Woon;Cho, Jin-Ki;Kim, Jae-Hong;Yeom, Seung-Jin;Kwak, Noh-Jung;Kim, Jin-Woong;Kang, Sung-Goon
    • Korean Journal of Materials Research
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    • v.19 no.2
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    • pp.61-67
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    • 2009
  • Electrolessly deposited Co (Re,P) was investigated as a possible capping layer for Cu wires. 50 nm Co (Re,P) films were deposited on Cu/Ti-coated silicon wafers which acted as a catalytic seed and an adhesion layer, respectively. To obtain the optimized bath composition, electroless deposition was studied through an electrochemical approach via a linear sweep voltammetry analysis. The results of using this method showed that the best deposition conditions were a $CoSO_4$ concentration of 0.082 mol/l, a solution pH of 9, a $KReO_4$ concentration of 0.0003 mol/l and sodium hypophosphite concentration of 0.1 mol/L at $80^{\circ}C$. The thermal stability of the Co (Re,P) layer as a barrier preventing Cu was evaluated using Auger electron spectroscopy and a Scanning calorimeter. The measurement results showed that Re impurities stabilized the h.c.p. phase up to $550^{\circ}C$ and that the Co (Re,P) film efficiently blocked Cu diffusion under an annealing temperature of $400^{\circ}C$ for 1hr. The good barrier properties that were observed can be explained by the nano-sized grains along with the blocking effect of the impurities at the fast diffusion path of the grain boundaries. The transformation temperature from the amorphous to crystal structure is increased by doping the Re.

Studies on the Electrochemical Behaviors, Spectrophotometric Determination of Heavy Lanthanide Ions and Heavy Metal Chelate Complexes with Bidentate Ligands(III) -Synthesis and Characterization of the Tetrakis(5,7-dichloro-8-quinolinato)(2-mercaptopyrimidinato) molybdenum(IV) Complex- (무거운 란탄이온의 전기화학적 거동, 분광학적 정량 및 중금속 이온과 두 자리 리간드 착물에 관한 연구(제 3 보): -테트라키스(5,7-디클로로-8-퀴놀리나토)(2-메르캅토피리미디나토) 몰리브데늄(IV) 착물의 합성 및 특성-)

  • Chang, Choo Hwan;Choi, Won Jong;Park, Keun Su;Son, Pyung Su;Suh, Moo Yul
    • Analytical Science and Technology
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    • v.6 no.5
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    • pp.417-424
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    • 1993
  • Eight-coordinate tetrakis molybdenum(IV) complexes containing 5,7-dichloro-8-hydroxyquinolinol(Hdcq) and 2-mercaptopyrimidine(Hmpd) has been prepared. $Mo(mpd)_4$, $Mo(dcq)(mpd)_3$, $Mo(dcq)_2(mpd)_2$, $Mo(dcq)_3(mpd)$ and $Mo(dcq)_4$ complexes have been isolated by thin-layer chromatography on silicagel plates. These complexes have been charaterized by $^1H-nmr$ spectrum and UV-Vis. spectrum. The chemical shift values of the protons ${\alpha}$ to the nitrogen in the ligands are shifted to down field. The relative intensities of the peaks which are positioned at the same proton of $Mo(dcq)(mpd)_3$ and $Mo(dcq)_3(mpd)$ are observed in 2:1 ratio, in case of $Mo(dcq)_2(mpd)_2$ appears in approximately a 1:1 ratio. The stereochemistry of the complexes in discussed in terms of their nmr spectrum and Orgel's rule. By vertue of the intensities (${\varepsilon}$>10,000~25,000) the low energy($16,600{\sim}19,800cm^{-1}$) bands are observed for the electronic spectra of the complexes are assigned as charge transfer bands.

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Structural and electrochemical characterization of K2NiF4 type layered perovskite as cathode for SOFCs (K2NiF4 type 층상 페롭스카이트 구조 La(Ca)2Ni(Cu)O4-δ의 SOFC 양극 특성 및 결정구조 평가)

  • Myung, Jae-ha;Hong, Youn-Woo;Lee, Mi Jai;Jeon, Dae-Woo;Lee, Young-Jin;Hwang, Jonghee;Shin, Tae Ho;Paik, Jong Hoo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.25 no.3
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    • pp.116-120
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    • 2015
  • $La_2NiO_{4+{\delta}}$ based oxides, a mixed electronic-ionic conductors (MIECs) with $K_2NiF_4$ type structure, have been considerably investigated in recent decades as electrode materials for advanced solid oxide fuel cells (SOFCs) due to their high electrical conductivity, and oxidation reduction reaction (ORR). In this study, structure properties of $La(Ca)_2Ni(Cu)O_{4+{\delta}}$ were studied as a potential cathode for intermediate temperature SOFCs (IT-SOFCs).

Artificial Control of ZnO Nanorods via Manipulation of ZnO Nanoparticle Seeds (산화아연 나노핵의 조작을 통한 산화아연 나노로드의 제어)

  • Shin, Kyung-Sik;Lee, Sam-Dong;Kim, Sang-Woo
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.11a
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    • pp.399-399
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    • 2008
  • Synthesis and characterization of ZnO structure such as nanowires, nanorods, nanotube, nanowall, etc. have been studied to multifunctional application such as optical, nanoscale electronic and chemical devices because it has a room-temperature wide band gap of 3.37eV, large exiton binding energy(60meV) and various properties. Various synthesis methods including chemical vapor deposition (CVD), physical vapor deposition, electrochemical deposition, micro-emulsion, and hydrothermal approach have been reported to fabricate various kinds of ZnO nanostructures. But some of these synthesis methods are expensive and difficult of mass production. Wet chemical method has several advantage such as simple process, mass production, low temperature process, and low cost. In the present work, ZnO nanorods are deposited on ITO/glass substrate by simple wet chemical method. The process is perfomed by two steps. One-step is deposition of ZnO seeds and two-step is growth of ZnO nanorods on substrates. In order to form ZnO seeds on substrates, mixture solution of Zn acetate and Methanol was prepared.(one-step) Seed layers were deposited for control of morpholgy of ZnO seed layers by spin coating process because ZnO seeds is deposited uniformly by centrifugal force of spin coating. The seed-deposited samples were pre-annealed for 30min at $180^{\circ}C$ to enhance adhesion and crystallinnity of ZnO seed layer on substrate. Vertically well-aligned ZnO nanorods were grown by the "dipping-and-holding" process of the substrates into the mixture solution consisting of the mixture solution of DI water, Zinc nitrate and hexamethylenetetramine for 4 hours at $90^{\circ}C$.(two-step) It was found that density and morphology of ZnO nanorods were controlled by manipulation of ZnO seeds through rpm of spin coating. The morphology, crystallinity, optical properties of the grown ZnO nanostructures were carried out by field-emission scanning electron microscopy, high-resolution electron microscopy, photoluminescence, respectively. We are convinced that this method is complementing problems of main techniques of existing reports.

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Synthesis and Characterization of Power Conversion Efficiency of D/A Structure Conjugated Polymer Based on Benzothiadiazole-Benzodithiophene (Benzothiadiazole-benzodithiophene을 기반으로 한 D/A구조의 공액 고분자 합성 및 광전변환 효율 특성 개선 연구)

  • Seong, Ki-Ho;Yun, Dae-Hee;Woo, Je-Wan
    • Applied Chemistry for Engineering
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    • v.24 no.5
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    • pp.537-543
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    • 2013
  • In this study, the push-pull structure polymer for organic photo voHaics (OPVs) was synthesized and characterized. The poly{4,8-didodecyloxybenzo[1,2-b;3,4-b]dithiophene-alt-5,6-bis(octyloxy)-4,7-di(thiophen-2-yl)benzo[c][1,2,5]-thiadiazole} (PDBDT-TBTD) was synthesized by Stille coupling reaction using the benzothiadiazole (BTD) derivative as an electron acceptor and benzodithiophene (BDT) derivative as an electron donor. The structure of monomers and polymers was identified by $^1H-NMR$ and GC-MS. The optical, physical and electrochemical properties of the conjugated polymer were identified by GPC, TGA, UV-Vis and cyclic voltammetry. The number average molecular weight ($M_n$) and initial decomposition temperature (5% weight loss temperature, $T_d$) of PDBDT-TBTD were 6200 and $323^{\circ}C$, respectively. The absorption maxima on the film was about 599 nm and the optical band gap was about 1.70 eV. The structure of device was ITO/PEDOT : PSS/PDBDT-TBTD : $PC_{71}BM/BaF_2/Ba/Al$. PDBDT-TBTD and $PC_{71}BM$ were blended with the weight ratio of 1:2 which were then used as an optical active layer. The power conversion efficiency (PCE) of fabricated device was measured by solar simulator and the best PCE was 2.1%.

Synthesis and Characterization of Quinoxaline-Based Thiophene Copolymers as Photoactive Layers in Organic Photovoltaic Cells

  • Choi, Yoon-Suk;Lee, Woo-Hyung;Kim, Jae-Ryoung;Lee, Sang-Kyu;Shin, Won-Suk;Moon, Sang-Jin;Park, Jong-Wook;Kang, In-Nam
    • Bulletin of the Korean Chemical Society
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    • v.32 no.2
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    • pp.417-423
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    • 2011
  • A series of new quinoxaline-based thiophene copolymers (PQx2T, PQx4T, and PQx6T) was synthesized via Yamamoto and Stille coupling reactions. The $M_ws$ of PQx2T, PQx4T, and PQx6T were found to be 20,000, 12,000, and 29,000, with polydispersity indices of 2.0, 1.2, and 1.1, respectively. The UV-visible absorption spectra of the polymers showed two distinct absorption peaks in the ranges 350 - 460 nm and 560 - 600 nm, which arose from the ${\pi}-{\pi}^*$ transition of oligothiophene units and intramolecular charge transfer (ICT) between a quinoxaline acceptor and thiophene donor. The HOMO levels of the polymer ranged from -5.37 to -5.17 eV and the LUMO levels ranged from -3.67 to -3.45 eV. The electrochemical bandgaps of PQx2T, PQx4T, and PQx6T were 1.70, 1.71, and 1.72 eV, respectively, thus yielding low bandgap behavior. PQx2T, PQx4T, and PQx6T had open circuit voltages of 0.58, 0.42, and 0.47 V, and short circuit current densities of 2.9, 5.29 and 9.05 mA/$cm^2$, respectively, when $PC_{71}BM$ was used as an acceptor. For the solar cells with PQx2T-PQx6T:$PC_{71}BM$ (1:3) blends, an increase in performance was observed in going from PQx2T to PQx6T. The power conversion efficiencies of PQx2T, PQx4T, and PQx6T devices were found to be 0.69%, 0.73%, and 1.80% under AM 1.5 G (100 mW/$cm^2$) illumination.

Determination of optimum protection potential for cathodic protection of offshore wind-turbine-tower steel substructure by using potentiostatic method (정전위법에 의한 해상풍력 타워 구조물용 강재의 음극방식을 위한 최적방식전위 결정)

  • Lee, Jung-Hyung;Jung, Kwang-hu;Park, Jae-Cheul;Kim, Seong-Jong
    • Journal of Advanced Marine Engineering and Technology
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    • v.41 no.3
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    • pp.230-237
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    • 2017
  • In this study, electrochemical methods were used to determine the optimum protection potential of S355ML steel for the cathodic protection of offshore wind-turbine-tower substructures. The results of potentiodynamic polarization experiments indicated that the anodic polarization curve did not represent a passivation behavior, while under the cathodic polarization concentration, polarization was observed due to the reduction of dissolved oxygen, followed by activation polarization by hydrogen evolution as the potential shifted towards the active direction. The concentration polarization region was found to be located between approximately -0.72 V and -1.0 V, and this potential range is considered to be the potential range for cathodic protection using the impressed current cathodic protection method. The results of the potentiostatic experiments at various potentials revealed that varying current density tended to become stable with time. Surface characterization after the potentiostatic experiment for 1200 s, by using a scanning electron microscope and a 3D analysis microscope confirmed that corrosion damage occurred as a result of anodic dissolution under an anodic polarization potential range of 0 to -0.50 V, which corresponds to anodic polarization. Under potentials corresponding to cathodic polarization, however, a relatively intact surface was observed with the formation of calcareous deposits. As a result, the potential range between -0.8 V and -1.0 V, which corresponds to the concentration polarization region, was determined to be the optimum potential region for impressed current cathodic protection of S355ML steel.

Synthesis and Characterization of Octamethylenethiafulvalene Compounds with Osmium, Iridium, Platinium and Gold Chloride (Octamethylenethiafulvalene과 염화오스뮴, 이리듐, 백금 및 금 화합물의 합성과 특성에 관한 연구)

  • Jeong, Chan Kyou;Lee, Hong Woo;Kim, Young Jin;Choi, Sung Nak;Kim, Young Inn
    • Journal of the Korean Chemical Society
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    • v.45 no.5
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    • pp.442-447
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    • 2001
  • The charge-transfer compound (OMTTF)AuCl$_4$ was prepared from the direct reaction of octamethylenethiafulvalene (OMTTF) with HAuCl$_4{\cdot}xH_2$O in THF. (OMTTF)$_2PtCl_4$, (OMTTF)_2IrCl_6{\cdot}2H_2$O, and (OMTTF)Os$Cl_5{\cdot}THF$ were also formed using $H_2PtCl_6{\cdot}xH_2O$, $H_2IrCl_6{\cdot}xH_2O$ and $H_2OsCl_6$, respectively. The prepared compounds were characterized by magnetic (EPR, magnetic susceptibility), spectroscopic (IR, UV-Vis), electrochemical (CV) methods, and the powdered electrical conductivity measurement. The powdered electrical conductivities at room temperature were ~$10^{-7}S{\cdot}cm^{-1}$. The experimental results show that $OMTTF^+$ monocation radicals exist in all of the prepared compounds. The redox potential of OMTTF supports that $OMTTF^+$ is relatively stable. The magnetic properties indicate that there are significant magnetic interactions between the localized odd electrons on the central metal (Ir and Os) ions and the odd electrons resided on $OMTTF^+$ cation radicals in both (OMTTF) $_2IrCl_6{\cdot}2H_2O$ and (OMTTF)$OsCl_5{\cdot}THF$.

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