• 제목/요약/키워드: oxidation characterization

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Synthetic, Characterization, Biological, Electrical and Catalytic Studies of Some Transition Metal Complexes of Unsymmetrical Quadridentate Schiff Base Ligand

  • Maldhure, A. K.;Pethe, G. B.;Yaul, A. R.;Aswar, A. S.
    • 대한화학회지
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    • 제59권3호
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    • pp.215-224
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    • 2015
  • Unsymmetrical tetradentate Schiff base N-(2-hydroxy-5-methylacetophenone)-N'-(2-hydroxy acetophenone) ethylene diamine (H2L) and its complexes with Cr(III), Mn(II), Fe(III), Co(II), Ni(II) and Cu(II) have been synthesized and characterized by elemental analyses, magnetic susceptibility measurements, IR, electronic spectra and thermogravimetric analyses. 1H, 13C-NMR and FAB Mass spectra of ligand clearly indicate the presence of OH and azomethine groups. Elemental analyses of the complexes indicate that the metal to ligand ratio is 1:1 in all complexes. Infrared spectra of complexes indicate a dibasic quadridentate nature of the ligand and its coordination to metal ions through phenolic oxygen and azomethine nitrogen atoms. The thermal behavior of these complexes showed the loss of lattice water in the first step followed by decomposition of the ligand in subsequent steps. The thermal data have also been analyzed for the kinetic parameters by using Horowitz-Metzger method. The dependence of the electrical conductivity on the temperature has been studied over the temperature range 313-403 K and the complexes are found to show semiconducting behavior. XRD and SEM images of some representative complexes have been recorded. The antimicrobial activity of the ligand and its complexes has been screened against various microorganisms and all of them were found to be active against the test organisms. The Fe(III) and Ni(II) complex have been tested for the catalytic oxidation of styrene.

V2O5가 고용된 Karrooite계의 Brown색 안료합성과 특성 (Synthesis and Characterization of V2O - Doped Karrooite Brown Pigments)

  • 김금선;이병하
    • 한국세라믹학회지
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    • 제48권4호
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    • pp.303-306
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    • 2011
  • [ $V_2O_5$ ]doped Karrooite pigments were synthesized by the solid state method to get stabilized brown pigment in oxidation and reduction atmosphere. Optimum substitution condition and limited dopant with $V_2O_5$ for Karrooite pigment was investigated. With calcination at $1250^{\circ}C{\sim}1400^{\circ}C$, compositions were designed varying $V_2O_5$ molar ratio by increasing 0.02mole to the formula $Mg_1-xTi_2-xM_{2x}O_5$(x = 0.01~0.09 mole). Synthesized pigments were analyzed by XRD, Raman spectroscopy and UV-vis. When $V_2O_5$ was doped from 0.01 to 0.05 mole, single phase of Karrooite was observed at temperature $1300^{\circ}C$ and soaking time 4h by Raman spectroscopy. However, it was found that excess $VO_2$ peak appeared with 0.07 and 0.09 mole of $V_2O_5$ doped to $MgTi_2O_5$. This result indicated that the maximum limit of solid solution is 0.05 mole $V_2O_5$. Karrooite pigments were applied as a ceramic pigment to achieve brown colors in lime magnesia glaze and lime barium graze at both of oxidation and reduction atmosphere. CIE color coordinates are $L^*$ = 40.34, $a^*$ = 9.94, $b^*$ = 21.40 in lime magnesia glaze.

Synthesis and Characterization of CrZr-O-N Films Using Cr-Zr Segment Targets by Unbalanced Magnetron Sputtering

  • Kim, Dong Jun;La, Joung Hyun;Ki, Sung Min;Lee, Sang Yul
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제44회 동계 정기학술대회 초록집
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    • pp.94-94
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    • 2013
  • The Cr-Zr-N films have much improved mechanical properties and very smooth surface roughness. However, in spite of their outstanding properties, the Cr-Zr-N coatings revealed their mechanical properties deteriorated severely with increasing Zr content at $500^{\circ}C$ ecause of very rapid oxidation. Recently oxynitride films have been widely studied due to their excellent unique mechanical properties and oxidation resistance. In this work, CrZr-O-N films with various O contents were synthesized by unbalanced magnetron sputtering with Cr-Zr segment targets (Cr:Zr volume ratios is 1:1) and all films were prepared in a nitrogen rich mixture of N2 and O2. Characteristics such as crystalline structure, hardness and chemical composition as a function of the O content were investigated by X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM), microhardness testing system and energy dispersive spectroscopy (EDS). Results showed that the thin films had dense and compact microstructure as O content in the films increases. The microstructure of the thin films consisted of mainly crystalline Cr (Zr)N phase and Cr2O3 phase. The maximum hardness and elastic modulus of the films was measured to be approximately 33.2 GPa and 280.6 GPa from the films with low content of O elements. Detailed experimental results will be presented.

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나노 구조를 가지는 다공성 주석 산화물의 전기화학적 특성 (Electrochemical Characterization of Anodic Tin Oxides with Nano-Porous Structure)

  • 이재욱;박수진;신헌철
    • 한국재료학회지
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    • 제21권1호
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    • pp.21-27
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    • 2011
  • A nano-porous structure of tin oxide was prepared using an anodic oxidation process and the sample's electrochemical properties were evaluated for application as an anode in a rechargeable lithium battery. Microscopic images of the as-anodized sample indicated that it has a nano-porous structure with an average pore size of several tens of nanometers and a pore wall size of about 10 nanometers; the structural/compositional analyses proved that it is amorphous stannous oxide (SnO). The powder form of the as-anodized specimen was satisfactorily lithiated and delithiated as the anode in a lithium battery. Furthermore, it showed high initial reversible capacity and superior rate performance when compared to previous fabrication attempts. Its excellent electrode performance is probably due to the effective alleviation of strain arising from a cycling-induced large volume change and the short diffusion length of lithium through the nano-structured sample. To further enhance the rate performance, the attempt was made to create porous tin oxide film on copper substrate by anodizing the electrodeposited tin. Nevertheless, the full anodization of tin film on a copper substrate led to the mechanical disintegration of the anodic tin oxide, due most likely to the vigorous gas evolution and the surface oxidation of copper substrate. The adhesion of anodic tin oxide to the substrate, together with the initial reversibility and cycling stability, needs to be further improved for its application to high-power electrode materials in lithium batteries.

Synthesis and Electrochemical Characterization of Silica-Manganese Oxide with a Core-shell Structure and Various Oxidation States

  • Ryu, Seong-Hyeon;Hwang, Seung-Gi;Yun, Su-Ryeon;Cho, Kwon-Koo;Kim, Ki-Won;Ryu, Kwang-Sun
    • Bulletin of the Korean Chemical Society
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    • 제32권8호
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    • pp.2683-2688
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    • 2011
  • Silica-manganese oxides with a core-shell structure were synthesized via precipitation of manganese oxides on the $SiO_2$ core while varying the concentration of a precipitation agent. Elemental analysis, crystalline property investigation, and morphology observations using low- and high-resolution electron microscopes were applied to the synthesized silica-manganese oxides with the core-shell structure. As the concentration of the precipitating agent increased, the manganese oxide shells around the $SiO_2$ core sequentially appeared as $Mn_3O_4$ particles, $Mn_2O_3+Mn_3O_4$ thin layers, and ${\alpha}-MnO_2$ urchin-like phases. The prepared samples were assembled as electrodes in a supercapacitor with 0.1 M $Na_2SO_4$ electrolyte, and their electrochemical properties were examined using cyclic voltammetry and charge-discharge cycling. The maximum specific capacitance obtained was 197 F $g^{-1}$ for the $SiO_2-MnO_2$ electrode due to the higher electronic conductivity of the $MnO_2$ shell compared to those of the $Mn_2O_3$ and $Mn_3O_4$ phases.

황산화세균 Thiobacillus thiooxidans에 의한 fly ash의 중금속 제거 특성:고형물 농도의 영향 (Characterization of Heavy Metals Bioleaching from Fly Ash by a Sulfur-Oxidizing Bacterium Thiobacillus thiooxidans: Effect of Solid Concentrations)

  • 조경숙;문희선;이인숙
    • 환경생물
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    • 제17권2호
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    • pp.183-190
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    • 1999
  • The bioleaching of heavy metals from fly ash was performed by Thiobacillus thiooxidans MET isolated from the enrichment culture of an anaerobically digested sludge. The effect of solid concentrations on the efficiency of metal leaching was studied in shaken flasks. In the range of solid concentrations 20 g.L­$^1$to 100 g.L­$^1$T. thiooxidans MET oxidized S$^{0}$ to sulfate without any lag period. The final pH of slurry solution was decreased to below pH 1, and the final oxide-redox potential (ORP) was increased to over 420 mV in the solid concentrations below 100 g.L­$^1$. However, the initial lag period of 4 to 8 days was required to obtain the pH reduction and ORP increase of the slurry solutions in the range of solid concentrations 150 g.L­$^1$to 300 g.L­$^1$. The sulfur oxidation rate of T. thiooxidans MET in 20~100 g.L­$^1$solid concentrations was 0.70~0.75 g-S.L­$^1$ㆍ d­$^1$, but its sulfur oxidation activity was remarkably inhibited with increasing solid concentration over 150 g.L­$^1$. Increasing fly ash solids concentration in the range of solids concentration 20 g.L­$^1$ to 200 g.L­$^1$decreased the removal efficiency of Zn, Cu, Mn, Cr and Pb. The solubilization of heavy metals from fly ash was strongly correlated with the pH value of slurry solution. When the pH of slurry solution was reduced to 3, the solubilization process of Zn, Cu and Mn started, and their solubilization efficiency of Zn, Cu and Mn was progressively increased below pH 2. However, the solubilization process of Cr and Pb started at pH 2.5 and 2.0, respectively.

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고체산화물 연료전지를 위한 플라즈마 용사코팅 Ni/YSZ 음극 복합체의 특성평가 (Characterization of Ni/YSZ Anode Coating for Solid Oxide Fuel Cells by Atmospheric Plasma Spray Method)

  • 박수동;윤상훈;강기철;이창희
    • Journal of Welding and Joining
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    • 제26권4호
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    • pp.50-54
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    • 2008
  • In this research, anode for SOFC has been manufactured from two different kinds of feedstock materials through thermal spraying process and the properties of the coatings were characterized and compared. One kind of feedstock was manufactured from spray drying method which includes nano-components of NiO, YSZ (300 nm) and graphite. And the other is manufactured by blending the micron size NiO coated graphite, YSZ and graphite powders as feedstock materials. Microstructure, mechanical properties and electrical conductivity of the coatings as-sprayed, after oxidation and after hydrogen reduction containing nano composite which is prepared from spray-dried powders were evaluated and compared with the same properties of the coatings prepared from blended powder feedstock. The coatings prepared from the spray dried powders has better properties as they provide larger triple phase boundaries for hydrogen oxidation reaction and is expected to have lower polarization loss for SOFC anode applications than that of the coatings prepared from blended feedstock. A maximum electrical conductivity of 651 S/cm at $800^{\circ}C$ was achieved for the coatings from spray dried powders which much more than that of the average value.

Isolation and characterization of Vitreoscilla mutant defective in catalase-peroxidase hydroperoxidase I

  • Kim, Hee-Jung;Moon, Ja-Young;Lee, John-Hwa;Park, Kie-In
    • 한국동물위생학회지
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    • 제30권3호
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    • pp.291-304
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    • 2007
  • Mutants of an obligate aerobic bacterium, Vitreoscilla, that have deficiency in heat-labile catalase-peroxidase hydroperoxidase I (HPI) were created by EMS treatment. The catalase-peroxidase HPI-deficient mutant showed substantially lower peroxidase activity in exponential and mid-stationary phase compared with the wild type strain. In late stationary phase, the mutant exhibited no peroxidase activity. Peroxidase deficiency in the mutant was revealed by polyacrylamide gels stained for peroxidase activity. Characteristically, catalase levels in the mutant increased about 14- and 8-fold during growth in the exponential and stationary phases, respectively, compared to those in the wild type, suggesting a compensatory effect for protection from $H_2O_2$ toxicity. The mutant showed differences in physiology from the wild type: retardation in growth rate and decrease in oxygen consumption. Both the wild type and the catalase-peroxidase HPI-deficient mutant of Vitreoscilla had lower growth rates in media containing increasing $H_2O_2$ concentrations. However, the mutant exhibited an additionally decreased growth rate after 6 to 8 h of growth compared to the wild type. The wild type was resistent up to 20 mM $H_2O_2$, whereas the mutant was very sensitive to high concentrations of exogenous $H_2O_2$. Although elevated catalase levels would provide protection of the bacteria from the deleterious effect of $H_2O_2$, it did not appear to be complete. Cell-free extracts of the mutant showed decreased NADH oxidation rates and higher accumulation of $H_2O_2$ during this oxidation. These results may account for the impaired growth and earlier onset of death phase by the catalase-peroxidase HPI-deficient mutant of Vitreoscilla.

지방산과 인지질 혼합 LB막의 전기화학적 특성 (The Electrochemical Characterization of Mixture LB Films of Fatty Acid and Phospholipids)

  • 손태철;김남석;박근호
    • 한국응용과학기술학회지
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    • 제20권2호
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    • pp.94-100
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    • 2003
  • We studied electrochemical characteristics of Langmuir-Blodgett(LB) films by using cyclic voltammetry with a three-electrode system. An Ag/AgCl as a reference electrode, a platinum wire as a counter electrode and LB film-coated indium tin oxide(ITO) as a working electrode were used to study electrochemical characteristics at a various concentration of $NaClO_4$ solution. LB films were reduced from initial potential to -1350 mV, continuously oxidized to l650mV and returned to the initial point. The scan rate was l00mV/s. The monolayer surface morphology of the LB film have been measured by Atomic Force Microscope(AFM). As a result, We comfirmed that the microscopic properties of LB film by AFM showed the good orientation of momolayer molecules and the thickness of monolayer was 3.5-4.lnm. The cyclic voltammograms(CV) of the ITO-coated glass showed the peak potentials for the reduction-oxidation reation. LB films of 4-octyl-4'-(5-carboxypentamethyleneoxy) azobenzene(8A5H) / L-${\alpha}$-phosphayidyl choline, dilauroyl(DLPC) seemed to be irreversible process caused by only the oxidation current from the cyclic voltammogram. The current of oxidatation increased at cyclic voltammogram by increasing 8A5H density in LB films. The diffusivity(D) of LB films increased with increasing of a 8A5H amount and was inversely proportional to the concentration of $NaClO_4$ solution.

Synthesis and Characterization of Tetrathiafulvalene (TTF) and 7,7,8,8-Tetracyanoquinodimethane (TCNQ) Compounds with PdX2(X=CI, NO3and Hexafluoroacetylacetonate)

  • Kim, Young-Inn;Jeong, Chan-Kyou;Lee, Yong-Min;Choi, Sung-Nak
    • Bulletin of the Korean Chemical Society
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    • 제23권12호
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    • pp.1754-1758
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    • 2002
  • Tetrathiafulvalene(TTF) reacts with $PdCl_2,Pd(NO_3)_2$ and $Pd(hfacac)_2$(hexafluoroacetylacetonate) in ethanol to give $(TTF)_{1.5}PdCl_2$ (1a), $(TTF)_3Pd(NO_3)_2$ (1b) and $(TTF)_4Pd(hfacas)_2$ nd (1c), respectively. $PdCl(TCNQ)_{2.5}{\cdot}CH_3OH(2a)$was obtained from the reaction of $PdCl_2$ with LiTCNQ in methanol via the partial replacement of $Cl^-$ in $PdCl_2$ by $TCNQ^-$anion, whereas the total substitution of the labile $NO_3^-$ in $Pd(NO_3)_2$ yielded pd(TCNQ)·$CH_3OH$ (2b). $Pd(hfacac)_2(TCNQ)_2\cdot3CH_3OH$ (2c) was obtained from $Pd(hfacac)_2$ and LiTCNQ in methanol. The prepared compounds were characterized by spectroscopic (IR, UV, XPS) methods and magnetic (EPR, magnetic susceptibility) studies. The powdered electrical conductivities (${\sigma}_{rt}$) of the prepared compounds at room temperature were about~$10^{-7}S{\cdot}cm^{-1}$. The effective magnetic moments were lass than the spin-only value of one unpaired electron and no EPR signals from Pd metal ions were observed in any of the compounds, indicating that the Pd ions were diamagnetic and the magnetic moments arose from$(TTF)_n$ or $(TCNQ)_n$ moieties. The experimental evidences revealed that the charge transfer had occurred form $(TTF)_n$ moiety to the central Pd metal ion in 1a, 1b and 1c. Thus the TTF donors were ions in 2a and 2b were diamagnetic Pd(II) oxidation state. In contrast, the Pd metal ion was oxidized to Pd(IV) state in 2c as a result of an addition of $TCNQ^-$anion to $Pd(hfacac)_2$ in methanol. The oxidation states of the Pd metal ions were confirmed using the x-ray photoelectron spectroscopy.