• Title/Summary/Keyword: electrochemical reduction

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Preparation of Conducting Polymer PEDiTT Thin Film Using SAM Method (자기조립법을 이용한 전도성고분자 PEDiTT박막의 제조)

  • 손용근;강규식;심창용;최정식;이두연
    • Polymer(Korea)
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    • v.26 no.5
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    • pp.589-598
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    • 2002
  • thiathlophene (EDiTT) was synthesized. The yield of the synthesis was about 29%. The monomer was identified by using NMR, IR and UV/Vis spectroscopic methods. Poly (3,4-ethylenedithiathiophene) (PEDiTT) was prepared using this monomer and FeCl$_3$. The deep blue green color of the product was changed into brown color by the reduction with $N_2$H$_4$. This was soluble to common organic solvents. Spectroelectrochemistry was used to characterize the PEDiTT. NMP was the best solvent for PEDiTT. PEDiTT/NMP solution was used for making SAM type thin film of the polymer on gold electrode. Electrochemical and IR spectroscopic methods were used to identify the thin film.

Anodic Reactions at a Pb-Ag Anode in Sulfuric Acid Solutions Containing Manganese(II) (망간(II)을 함유한 황산용액에서 Pb-Ag 양극의 산화반응)

  • Lee, Man-Seung;Nicol, M.J.
    • Resources Recycling
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    • v.26 no.4
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    • pp.34-41
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    • 2017
  • The effect of Mn(II) concentration on the anodic reactions occurring on a Pb-Ag electrode in sulfuric acid solutions has been studied by potentiostatic oxidation in the potential range of 1.8 to 2.0 V. High oxidation potentials and low initial concentrations of Mn(II) resulted in higher concentrations of soluble Mn(III) ions which were obtained from spectrophotometric analysis of the solution after oxidation. $MnO_2$ was deposited on the electrode by electrochemical oxidation of Mn(II) at 1.8 and 1.9 V, while it was formed by disproportionation of Mn(III) at 2.0 V. No $PbO_2$ was formed in the presence of Mn(II) during potentiostatic oxidation treatment for two hours at 1.8 V. Chemical reduction of $PbO_2$ with Mn(II) led to a decrease in the amount of $PbO_2$ as Mn(II) concentration increased at 1.9 and 2.0 V.

Synthesis of Pentadentate Schiff Base Molybdenum(Ⅴ) Complexes and Their Electrochemical Properties in Aprotic Solvents (다섯자리 Schiff Base Molybdenum(Ⅴ) 착물들의 합성과 비수용매에서의 전기화학적 성질)

  • Kim, Seon Suk;Choe, Ju Hyeong;Choe, Yong Guk;Jeong, Byeong Gu
    • Journal of the Korean Chemical Society
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    • v.38 no.2
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    • pp.160-168
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    • 1994
  • Pentadentate Schiff base molybdenum(Ⅴ) complexes such as [Mo(Ⅴ)O(Sal-DET)(NCS)] and [Mo(Ⅴ)O(Sal-DPT)(NCS)] were synthesized by Sabat method. The structure of these complexes were identified by elemental analysis, spectroscopy, and thermogravimetric analysis(T.G.A.). It was found that the mole ratio of Schiff base ligand to the complexes was found to be 1 : 1. The redox processes of the complexes were investigated by cyclic voltammetric and differential pulse polarographic technique in nonaqueous solvent containing 0. 1 M tetraethyl ammonium perchlorate(TEAP) as supporting electrolyte at glassy carbon electrode. It was found that diffusion controlled reduction processes of four steps with one electron were 2Mo(Ⅴ)$\rightleftarrow^{e-}$ Mo(Ⅴ)Mo(Ⅳ) $\longrightarrow^{e-}$ 2Mo(Ⅳ), Mo(Ⅳ) $\longrightarrow^{e-}$ Mo(Ⅲ) $\longrightarrow^{e-}$ Mo(Ⅱ)

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In situ Structural Investigation of Iron Phthalocyanine Monolayer Adsorbed on Electrode Surface by X-ray Absorption Fine Structure

  • Kim, Seong Hyeon;Toshiaki Ohta;Gang, Gwang Hun
    • Bulletin of the Korean Chemical Society
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    • v.21 no.6
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    • pp.588-594
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    • 2000
  • Structural changes of an iron phthalocyanine (FePC) monolayer induced by adsorption and externally applied potential on high area carbon surface have been investigated in situ by iron K-edge X-ray absorption fine structure (XAFS) in 0.5 M $H_2S0_4.$ Fine structures shown in the X-ray absorption near edge structure (XANES) for microcrystalline FePC decreased upon adsorption and further diminished under electrochemical conditions. Fe(II)PC(-2) showed a 1s ${\rightarrow}$ 4p transition as poorly resolved shoulder to the main absorption edge rather than a distinct peak and a weak 1s ${\rightarrow}$ 3d transition. The absorption edge position measured at half maximum was shifted from 7121.8 eV for Fe(lI)PC(-2) to 7124.8 eV for $[Fe(III)PC(-2)]^+$ as well as the 1s ${\rightarrow}$ 3d pre-edge peak being slightly enhanced. However, essentially no absorption edge shift was observed by the 1-electron reduction of Fe(Il)PC(-2), indicating that the species formed is $[Fe(II)PC(-3)]^-$. Structural parameters were obtained by analyzing extended X-ray absorption fine structure (EXAFS) oscillations with theoretical phases and amplitudes calculated from FEFF 6.01 using multiple-scattering theory. When applied to the powder FePC, the average iron-to-phthalocyanine nitrogen distance, d(Fe-$N_p$) and the coordination number were found to be 1.933 $\AA$ and 3.2, respectively, and these values are the same, within experimental error, as those reported ( $1.927\AA$ and 4). Virtually no structural changes were found upon adsorption except for the increased Debye-Wailer factor of $0.005\AA^2$ from $0.003\AA^2.$ Oxidation of Fe(II)PC(-2) to $[Fe(III)PC(-2)]^+$ yielded an increased d(Fe-Np) (1 $.98\AA)$ and Debye-Wailer factor $(0.005\AA^2).$ The formation of $[Fe(II)PC(-3)]^-$, however, produced a shorter d(Fe-$N_p$) of $1.91\AA$ the same as that of crystalline FePC within experimental error, and about the same DebyeWaller $factor(0.006\AA^2)$.

Improved structures of stainless steel current collector increase power generation of microbial fuel cells by decreasing cathodic charge transfer impedance

  • Nam, Taehui;Son, Sunghoon;Kim, Eojn;Tran, Huong Viet Hoa;Koo, Bonyoung;Chai, Hyungwon;Kim, Junhyuk;Pandit, Soumya;Gurung, Anup;Oh, Sang-Eun;Kim, Eun Jung;Choi, Yonghoon;Jung, Sokhee P.
    • Environmental Engineering Research
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    • v.23 no.4
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    • pp.383-389
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    • 2018
  • Microbial fuel cell (MFC) is an innovative environmental and energy system that converts organic wastewater into electrical energy. For practical implementation of MFC as a wastewater treatment process, a number of limitations need to be overcome. Improving cathodic performance is one of major challenges, and introduction of a current collector can be an easy and practical solution. In this study, three types of current collectors made of stainless steel (SS) were tested in a single-chamber cubic MFC. The three current collectors had different contact areas to the cathode (P $1.0cm^2$; PC $4.3cm^2$; PM $6.5cm^2$) and increasing the contacting area enhanced the power and current generations and coulombic and energy recoveries by mainly decreasing cathodic charge transfer impedance. Application of the SS mesh to the cathode (PM) improved maximum power density, optimum current density and maximum current density by 8.8%, 3.6% and 6.7%, respectively, comparing with P of no SS mesh. The SS mesh decreased cathodic polarization resistance by up to 16%, and cathodic charge transfer impedance by up to 39%, possibly because the SS mesh enhanced electron transport and oxygen reduction reaction. However, application of the SS mesh had little effect on ohmic impedance.

Development of Micro-Tubular Perovskite Cathode Catalyst with Bi-Functionality on ORR/OER for Metal-Air Battery Applications

  • Jeon, Yukwon;Kwon, Ohchan;Ji, Yunseong;Jeon, Ok Sung;Lee, Chanmin;Shul, Yong-Gun
    • Korean Chemical Engineering Research
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    • v.57 no.3
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    • pp.425-431
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    • 2019
  • As rechargeable metal-air batteries will be ideal energy storage devices in the future, an active cathode electrocatalyst is required with bi-functionality on both oxygen reduction reaction (ORR) and oxygen evolution reaction (OER) during discharge and charge, respectively. Here, a class of perovskite cathode catalyst with a micro-tubular structure has been developed by controlling bi-functionality from different Ru and Ni dopant ratios. A micro-tubular structure is achieved by the activated carbon fiber (ACF) templating method, which provides uniform size and shape. At the perovskite formula of $LaCrO_3$, the dual dopant system is successfully synthesized with a perfect incorporation into the single perovskite structure. The chemical oxidation states for each Ni and Ru also confirm the partial substitution to B-site of Cr without any changes in the major perovskite structure. From the electrochemical measurements, the micro-tubular feature reveals much more efficient catalytic activity on ORR and OER, comparing to the grain catalyst with same perovskite composition. By changing the Ru and Ni ratio, the $LaCr_{0.8}Ru_{0.1}Ni_{0.1}O_3$ micro-tubular catalyst exhibits great bi-functionality, especially on ORR, with low metal loading, which is comparable to the commercial catalyst of Pt and Ir. This advanced catalytic property on the micro-tubular structure and Ru/Ni synergy effect at the perovskite material may provide a new direction for the next-generation cathode catalyst in metal-air battery system.

Synthesis and Characteristics of Pd/r-TiO2 Nanotube Arrays Hetrojunction Photocatalyst (Pd/r-TiO2 나노튜브 이종결합 광촉매의 합성과 특성)

  • Lee, Jong-Ho;Lee, Young-Ki;Kim, Young-Jig;Jang, Kyung-Wook;Oh, Han-Jun
    • Korean Journal of Materials Research
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    • v.32 no.1
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    • pp.14-22
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    • 2022
  • To improve light absorption ability in the visible light region and the efficiency of the charge transfer reaction, Pd nanoparticles decorated with reduced TiO2 nanotube photocatalyst were synthesized. The reduced TiO2 nanotube photocatalyst was fabricated by anodic oxidation of Ti plate, followed by an electrochemical reduction process using applied cathodic potential. For TiO2 photocatalyst electrochemically reduced using an applied voltage of -1.3 V for 10 min, 38% of Ti4+ ions on TiO2 surface were converted to Ti3+ ion. The formation of Ti3+ species leads to the decrease in the band gap energy, resulting in an increase in the light absorption ability in the visible range. To obtain better photocatalytic efficiency, Pd nanoparticles were decorated through photoreduction process on the surface of reduced TiO2 nanotube photocatalyst (r10-TNT). The Pd nanoparticles decorated with reduced TiO2 nanotube photocatalyst exhibited enhanced photocurrent response, and high efficiency and rate constant for aniline blue degradation; these were ascribed to the synergistic effect of the new electronic state of the TiO2 band gap energy induced by formation of Ti3+ species on TiO2, and by improvement of the charge transfer reaction.

Effect of Cr and Mo Contents on Hydrogen Embrittlement of Tempered Martensitic Steels (템퍼드 마르텐사이트강의 수소취성에 미치는 Cr 및 Mo 함량의 영향)

  • Sang-Gyu, Kim;Jae-Yun, Kim;Hee-Chang, Sin;Byoungchul, Hwang
    • Korean Journal of Materials Research
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    • v.32 no.11
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    • pp.466-473
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    • 2022
  • The effect of Cr and Mo contents on the hydrogen embrittlement of tempered martensitic steels was investigated in this study. After the steels with different Cr and Mo contents were austenitized at 820 ℃ for 90 min, they were tempered at 630 ℃ for 120 min. The steels were composed of fully tempered martensite with a lath-type microstructure, but the characteristics of the carbides were dependent on the Cr and Mo contents. As the Cr and Mo contents increased, the volume fraction of film-like cementite and prior austenite grain size decreased. After hydrogen was introduced into tensile specimens by electrochemical charging, a slow strain-rate test (SSRT) was conducted to investigate hydrogen embrittlement behavior. The SSRT results revealed that the steel with lower Cr or lower Mo content showed relatively poor hydrogen embrittlement resistance. The hydrogen embrittlement resistance of the tempered martensitic steels increased with increasing Mo content, because the reduction in the film-like cementite and prior austenite grain size plays an important role in improving hydrogen embrittlement resistance. The results indicate that controlling the Cr and Mo contents is essential to achieving a tempered martensitic steel with a combination of high strength and excellent hydrogen embrittlement resistance.

Effects of Chloride and Sulfate Ions on Corrosion Behaviors of Structural Materials Based on Design of Experiment (실험계획에 기반한 수돗물 성분(Chloride and Sulfate Ions)의 구조재료 부식 영향성 고찰)

  • Dong-In Lim;Heng-Su Noh;Hyeok-Jun Kwon;Sung-Ryul Park;Man-Sik Jo;Doo-Youl Lee
    • Corrosion Science and Technology
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    • v.22 no.3
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    • pp.201-213
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    • 2023
  • Corrosion management of an aircraft and its engine relies on rinsing and cleaning using tap water. Few studies have reported effects of tap water species on corrosion behaviors of structural materials. In this study, a series of experiments were conducted based on the design of experiment. Solutions with different levels of chloride and sulfate ions were prepared using a full factorial design. Two structural materials (aluminum alloy and steel) were used for an alternate immersion test. Weight loss was then measured. In addition, a silver specimen was utilized as a sensor for chloride deposition measurement. The silver specimen was examined using the electrochemical reduction method, XPS, and SEM-EDS. Surface analysis revealed that levels of chloride and sulfate ions were sufficient for the formation of silver chloride and silver surface. Statistical analysis of weight loss and chloride deposition rate showed significant differences in measured values. Concentration of chloride ions greatly affected corrosion behaviors of structural materials. Sulfate ion hindered the adsorption reaction. These results emphasize the importance of controlling ion concentration of tap water used for cleaning and rinsing an aircraft.

Electrochemical properties of $Gd_{0.8}Ca_{0.2}Co_{1-x}Fe_xO_3$ cathodes for medium-temperature SOFC (중간온도형 고체산화물 연료전지의 양극재료로서 $Gd_{0.8}Ca_{0.2}Co_{1-x}Fe_xO_3$의 전기화학특성)

  • Ryu Ji-H.;Jang Jong-H.;Lee Hee-Y.;Oh Seung-M.
    • Journal of the Korean Electrochemical Society
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    • v.1 no.1
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    • pp.1-7
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    • 1998
  • For the purpose of finding new cathode materials for medium-temperature $(700\~800^{\circ}C)$ solid oxide fuel cells, $Gd_{0.8}Ca_{0.2}Co_{1-x}Fe_xO_3,\;(x=0.0\~0.5)$ are prepared, and their thermal stability and conductivity characteristics are investigated. Also, the cathodic activities are measured after the cathode layer being attached on CGO (cerium-gadolinium oxide) electrolyte disk. The X-ray analyses indicate that the materials prepared by calcining the citrate-gels at $800^{\circ}C$ have the orthorhombic perovskite structure without discernible impurities. The thermal stability of the undoped Co perovskite is so poor that it is decomposed to the individual binary oxide even at $1300^{\circ}C$. But the partially Fe-doped cobaltates exhibit a better thermal stability to retain their structural integrity up to $1400^{\circ}C$. The observation whereby both the undoped and Fe-doped cobaltates melt at ca. $1300^{\circ}C$ leads us to perform the electrode adhesion at <$1300^{\circ}C$. The cathodic activity of $Gd_{0.8}Ca_{0.2}Co_{1-x}Fe_xO_3,\;(x=0.0\~0.5)$, electrodes is superior to $La_{0.9}Sr_{0.1}MnO_3$, among the samples of $x=0.0\~0.5$, the x=0.2 cathode shows the best activity for the oxygen reduction reaction. It is likely that the Fe-doping provides a better thermal stability to the materials but in turn imparts an inferior cathodic activity, such that the optimum trade-off is made at x=0.2 between the two factors. The total electrical conductivity and ion conductivity of $Gd_{0.8}Ca_{0.2}Co_{1-x}Fe_xO_3$, are measured to be 51 S/cm and $6.0\times10^{-4}S/cm\;at\;800^{\circ}C$, respectively. The conductivity values illustrate that the materials are a mixed conductor and the reaction sites can be expanded to the overall electrode surface, thereby providing a better cathodic activity than $La_{0.9}Sr_{0.1}MnO_3$.