• Title/Summary/Keyword: Aqueous route

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Interaction Metal Ions with NADH Model Compounds. Cupric Ion Oxidation of Dihydronicotinamides

  • Park, Joon-Woo;Yun, Sung-Hoe;Koh Park, Kwang-Hee
    • Bulletin of the Korean Chemical Society
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    • v.9 no.5
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    • pp.298-303
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    • 1988
  • Kinetic studies on cupric ion ($Cu^{2+}$) oxidation of 1-benzyl- and 1-aryl-1,4-dihydronicotinamides (XNAH) in aqueous solution were performed. In the presence of dioxygen ($O_2$), the reaction followed first order kinetics with respect to both XNAH and $Cu^{2+}$. The oxidation reaction was found to be independent and parallel to the acid-catalyzed hydration reaction of XNAH. The catalytic role of $Cu^{2+}$ for the oxidation of XNAH in the presence of $O_2$ was attributed to $Cu^{2+}/Cu^+$ redox cycle by the reactions with XNAH and $O_2$. The second order rate constants of the Cu2+ oxidation reaction kCu, and acid-catalyzed hydration reaction $k_H$ were strongly dependent on the nature of the substituents in 1-aryl moiety. The slopes of log $k_{Cu}$ vs log $K_H$ and log $k_{Cu}$ vs ${\sigma}_p$ of the substituents plots were 1.64 and -2.2, respectively. This revealed the greater sensitivity of the oxidation reaction rate to the electron density on the ring nitrogen than the hydration reaction rate. A concerted two-electron transfer route involving XNAH-$Cu^{2+}$ complex was proposed for mechanism of the oxidation reaction.

Facile Electrodeposition Technique for the Fabrication of MoP Cathode for Supercapacitor Application

  • Samanta, Prakas;Ghosh, Souvik;Murmu, Naresh Chandra;Lee, Joong Hee;Kuila, Tapas
    • Composites Research
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    • v.34 no.6
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    • pp.345-349
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    • 2021
  • The continued environmental pollution caused by fossil fuel consumption has prompted researchers around the world to develop environmentally friendly energy technologies. Electrochemical energy storage is the significant area of research in this development process, and the research significance of supercapacitors in this field is increasing. Herein, a simple electrodeposition synthetic route was explored to develop the MoP layered cathode material. The layered structure provided a highly ion-accessible surface for smooth and faster ion adsorption/desorption. After Fe was doped into MoP, the morphology of MoP changes and the electrochemical performance was significantly improved. Specific capacitance value of the binder-free FeMoP electrode was found to be 269 F g-1 at 2 A g-1 current density in 6 M aqueous KOH electrolyte. After adding Fe to MoP, an additional redox contribution was observed in the redox conversion from Fe3+ to Fe2+ redox pair, and the charge transfer kinetics of MoP was effectively improved. This research can provide guidance for the development of supercapacitor electrode materials through simple electrodeposition technology.

Comparative Study of Undoped and Nickel-Doped Molybdenum Oxide Photoanodes for PEC Water Splitting

  • Garcia-Garcia, Matias
    • Journal of Electrochemical Science and Technology
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    • v.13 no.3
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    • pp.377-389
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    • 2022
  • The current global energy supply depends heavily on fossil fuels. This makes technology such as direct water splitting from harvesting solar energy in photoelectrochemical (PEC) systems potentially attractive due to its a promising route for environmentally benign hydrogen production. In this study, undoped and nickel-doped molybdenum oxide photoanodes (called photoanodes S1 and S2 respectively) were synthesized through electrodeposition by applying -1.377 V vs Ag/AgCl (3 M KCl) for 3 hours on an FTO-coated glass substrate immersed in molibdatecitrate aqueous solutions at pH 9. Scanning electron microscopy (SEM), atomic force microscopy (AFM), energy-dispersive X-ray spectroscopy (EDS), and X-ray photoelectron spectroscopy (XPS) were used for microstructural and compositional characterizations of the photoanodes. In addition, the optical and photoelectrochemical characterizations of these photoanodes were performed by UV-Visible spectroscopy, and linear scanning voltammetry (LSV) respectively. The results showed that all the photoanodes produced exhibit conductivity and catalytic properties that make them attractive for water splitting application in a photoelectrochemical cell. In this context, the photoanode S2 exhibited better photocatalytic activity than the photoanode S1. In addition, photoanode S2 had the lowest optical band-gap energy value (2.58 eV), which would allow better utilization of the solar spectrum.

Facile Chemical Growth of Cu(OH)2 Thin Film Electrodes for High Performance Supercapacitors (간단한 화학적 합성을 통한 고성능 슈퍼캐패시터용 수산화 구리 전극)

  • Patil, U.M.;Nam, Min Sik;Shinde, N.M.;Jun, Seong Chan
    • KEPCO Journal on Electric Power and Energy
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    • v.1 no.1
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    • pp.175-180
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    • 2015
  • A facile soft chemical synthesis route is used to grow nano-buds of copper hydroxide [$Cu(OH)_2$] thin films on stainless steel substrate[SS]. Besides different chemical methods for synthesis of $Cu(OH)_2$ nanostructure, the chemical bath deposition (CBD) is attractive for its simplicity and environment friendly condition. The structural, morphological, and electro-chemical properties of $Cu(OH)_2$ thin films are studied by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), cyclic voltammetry (CV) and galvanostatic charge-discharge (GCD) measurement techniques. The results showed that, facile chemical synthesis route allows to form the polycrystalline, granular nano-buds of $Cu(OH)_2$ thin films. The electrochemical properties of $Cu(OH)_2$ thin films are studied in an aqueous 1 M KOH electrolyte using cyclic voltammetry. The sample exhibited supercapacitive behavior with $340Fg^{-1}$ specific capacitance. Moreover, electrochemical capacitive measurements of $Cu(OH)_2/SS$ electrode exhibit a high specific energy and power density about ${\sim}83Wh\;kg^{-1}$ and ${\sim}3.1kW\;kg^{-1}$, respectively, at $1mA\;cm^{-2}$ current density. The superior electrochemical properties of copper hydroxide ($Cu(OH)_2/SS$) electrode with nano-buds like structure mutually improves pseudocapacitive performance. This work evokes scalable chemical synthesis with the enhanced supercapacitive performance of $Cu(OH)_2/SS$ electrode in energy storage devices.

Synthesis parameters of hydroxyapatite preparation by a precipitation process (합성조건이 침전법에 의한 Hydroxyapatite 제조에 미치는 영향)

  • Moon, Sung Wook;Lee, Byeong Woo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.32 no.3
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    • pp.96-102
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    • 2022
  • Hydroxyapatite (HAp) was synthesized from calcium hydroxide (Ca(OH)2) reacting with phosphoric acid (H3PO4) in aqueous solution. HAp powders were synthesized from extremely high concentration of precursor solutions over 3 M of Ca(OH)2 aqueous suspension using modified process parameters such as phosphoric acid (H3PO4) pouring rate, aging time and post ball milling process. Regardless of phosphoric acid pouring rate, the DCPD (dicalcium phosphate dihydrate) was formed at room temperature and when heated above 700℃, β-TCP (tricalcium phosphate) was synthesized and the amount reached its maximum at 900℃. When the synthesized powder was sintered at 1150℃, β-TCP, a high temperature impurity phase, remained. The single HAp phase without DCPD was obtained from post ball-milled precipitates followed by 3 day aging. For the ball-milled precipitates even without the aging process, the desired single HAp phase without β-TCP could be obtained by heat treatment above 500℃. The post ball milling process provided a convenient route for HAp synthesis.

Microstructural Development in Synthetic Hydroxyapatite (합성 수산화아파타이트의 미세구조 발달)

  • Kim, Jong-Hee;Park, Young-Min;Yang, Tae-Young;Yoon, Seog-Young;Park, Hong-Chae
    • Journal of the Korean Ceramic Society
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    • v.41 no.4
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    • pp.289-296
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    • 2004
  • Whisker and short rod shaped hydroxyapatite (Ca$_{10}$(PO$_4$)$_{6}$(OH)$_2$ with stoichiometric composition (Ca/P=1.62 -1.67, molar ratio) has been synthesized by hydrolysis and hydrothermal reaction of aqueous $\alpha$-Ca$_3$(PO$_4$)$_2$($\alpha$-TCP) solution (pH 11), respectively. The shape of resultant HAp was mainly dependent on synthetic route and the microstructural development was on processing condition. In hydrolysis processing, the degree of intersection of whiskerlike particles and agglomeration in the apsis line increased with increasing reaction time. In hydrothermal synthesis, the reaction product obtained under excessive reaction time ($\geq$3 h at 20$0^{\circ}C$) was severely agglomerated without further grain growth above certain critical size (0.75 ${\mu}{\textrm}{m}$ in length, 0.3${\mu}{\textrm}{m}$ 11m in diameter).

Fabrication of carbon nanotube emitters by filtration through a metal mesh

  • Choi, Ju-Sung;Lee, Han-Sung;Gwak, Jeung-Chun;Lee, Nae-Sung
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2010.06a
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    • pp.150-150
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    • 2010
  • Carbon nanotubes have drawn attention as one of the most promising emitter materials ever known not only due to their nanometer-scale radius of curvature at tip and extremely high aspect ratios but also due to their strong mechanical strength, excellent thermal conductivity, good chemical stability, etc. Some applications of CNTs as emitters, such as X-ray tubes and microwave amplifiers, require high current emission over a small emitter area. The field emission for high current density often damages CNT emitters by Joule heating, field evaporation, or electrostatic interaction. In order to endure the high current density emission, CNT emitters should be optimally fabricated in terms of material properties and morphological aspects: highly crystalline CNT materials, low gas emission during electron emission in vacuum, optimal emitter distribution density, optimal aspect ratio of emitters, uniform emitter height, strong emitter adhesion onto a substrate, etc. We attempted a novel approach to fabricate CNT emitters to meet some of requirements described above, including highly crystalline CNT materials, low gas emission, and strong emitter adhesion. In this study, CNT emitters were fabricated by filtrating an aqueous suspension of highly crystalline thin multiwalled CNTs (Hanwha Nanotech Inc.) through a metal mesh. The metal mesh served as a support and fixture frame of CNT emitters. When 5 ml of the CNT suspension was engaged in filtration through a 400 mesh, the CNT layers were formed to be as thick as the mesh at the mesh openings. The CNT emitter sample of $1{\times}1\;cm^2$ in size was characteristic of the turn-on electrical field of 2.7 V/${\mu}m$ and the current density of 14.5 mA at 5.8 V/${\mu}m$ without noticeable deterioration of emitters. This study seems to provide a novel fabrication route to simply produce small-size CNT emitters for high current emission with reliability.

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Studies of Silyl-Transfer Photochemical Reactions of N-[(Trimethylsilyl)alkyl]saccharins

  • Cho, Dae-Won;Oh, Sun-Wha;Kim, Dong-Uk;Park, Hea-Jung;Xue, Jin-Ying;Yoon, Ung-Chan;Mariano, Patrick S.
    • Bulletin of the Korean Chemical Society
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    • v.31 no.9
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    • pp.2453-2458
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    • 2010
  • Photochemical studies of N-[(trimethylsilyl)alkyl]saccharins were carried out to investigate their photochemical behavior. Depending on the nature of the substrate and the solvent system employed, reactions of these substances can take place by either SET-promoted silyl migration from carbon to either the amide carbonyl or sulfonyl oxygen or by a N-S homolysis route. The results of the current studies show that an azomethine ylide, arising from a SET-promoted silyl migration pathway, is generated in photoreactions of N-[(trimethylsilyl)methyl]saccharin and this intermediate reacts to give various photoproducts depending on the conditions employed. In addition, irradiation of N-[(trimethylsily)ethyl]saccharin produces an excited state that reacts through two pathways, the relative importance is governed by solvent polarity and protic nature. Finally, photoirradiation of N-[(trimethylsilyl)propyl]saccharin in a highly polar solvent system comprised of 35% aqueous MeOH gives rise to formation of a tricyclic pyrrolizidine and saccharin that generated via competitive SET-promoted silyl transfer and $\gamma$-hydrogen abstraction pathways.

Synthesis and Characterization of NiAl2O4 Inorganic Pigment Nanoparticles by a Reverse Micelle Processing (역-마이셀 공정에 의한 NiAl2O4 무기안료 나노 분말의 합성 및 특성)

  • Son, Jeong-Hun;Bae, Dong-Sik
    • Korean Journal of Materials Research
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    • v.25 no.2
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    • pp.95-99
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    • 2015
  • $NiAl_2O_4$ nanoparticle was synthesized by a reverse micelle processing for inorganic pigment. $Ni(NO_3)_2{\cdot}6H_2O$ and $Al(NO_3)_3{\cdot}9H_2O$ were used for the precursor in order to synthesize $NiAl_2O_4$ nanoparticles. The aqueous solution, which consisted of a mixing molar ratio of Ni/Al, was 1:2 and heat treated at $800{\sim}1100^{\circ}C$ for 2h. The average size and distribution of synthesized $NiAl_2O_4$ powders are in the range of 10-20 nm and narrow, respectively. The average size of the synthesized $NiAl_2O_4$ powders increased with an increasing water-to-surfactant molar ratio and heating temperature. The crystallinity of synthesized $NiAl_2O_4$ powder increased with an increasing heating temperature. The synthesized $NiAl_2O_4$ powders were characterized by X-ray diffraction analysis(XRD), a field emission scanning electron microscopy(FE-SEM), and a color spectrophotometer. The properties of synthesized powders were affected as a function such as a molar ratio and heating temperature. Results indicate that synthesis using a reverse miclle processing is a favorable process to obtain $NiAl_2O_4$ spinels at low temperatures. The procedure performed suggests that this new synthesis route for producing these oxides has the advantage of being fast and simple. Colorimetric coordinates indicate that the pigments obtained exhibit blue colors.

Synthesis of Mesoporous Carbons with Controllable N-Content and Their Supercapacitor Properties

  • Kim, Jeong-Nam;Choi, Min-Kee;Ryoo, Ryong
    • Bulletin of the Korean Chemical Society
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    • v.29 no.2
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    • pp.413-416
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    • 2008
  • A synthesis route to ordered mesoporous carbons with controllable nitrogen content has been developed for high-performance EDLC electrodes. Nitrogen-doped ordered mesoporous carbons (denoted as NMC) were prepared by carbonizing a mixture of two different carbon sources within the mesoporous silica designated by KIT-6. Furfuryl alcohol was used as a primary carbon precursor, and melamine as a nitrogen dopant. This synthesis procedure gave cubic Ia3d mesoporous carbons containing nitrogen as much as 13%. The carbon exhibited a narrow pore size distribution centered at 3-4 nm with large pore volume (0.6-1 cm3 g-1) and high specific BET surface area (700-1000 m2 g-1). Electrochemical behaviors of the NMC samples with various N-contents were investigated by a two-electrode measurement system at aqueous solutions. At low current density, the NMC exhibited markedly increasing capacitance due to the increase in the nitrogen content. This result could be attributed to the enhanced surface affinity between carbon electrode and electrolyte ions due to the hydrophilic nitrogen functional groups. At high current density conditions, the NMC samples exhibited decreasing specific capacitance against the increase in the nitrogen content. The loss of the capacitance with the N-content may be explained by high electric resistance which causes a significant IR drop at high current densities. The present results indicate that the optimal nitrogen content is required for achieving high power and high energy density simultaneously.