• Title/Summary/Keyword: Solid-State Reaction

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Formation and Properties of Dimethylamine Complexes of Palladium(II) Having trans Phosphorus Spanning Terdentate Ligands

  • 류상열;양웅강;김훈식;박순흠
    • Bulletin of the Korean Chemical Society
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    • v.18 no.11
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    • pp.1183-1185
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    • 1997
  • Dimethylamine complexes of palladium(Ⅱ) [(PCP)Pd(NHMe2)](OTf) (PCP = 2,6-(R2PCH2)2C6H3); R = Ph (1), R = Cy (2)), have been prepared from the reaction of (PCP)Pd(OTf) and dimethylamine. The complex 1 is stable both in solution and in the solid state, while 2 is stable only in solution in the presence of dimethylamine although the formation of 2 in solution is quantitative by NMR Spectroscopy. A solution NMR spectroscopic study shows that dimethylamine favors over carbon monoxide in the coordination sphere of palladium(Ⅱ) having rigid terdentate ligands. The complexes 1 and 2 in chlorinated solvents undergo a chlorine abstract reaction yielding Pd(2,6-(R2PCH2)2C6H3)Cl in the presence of a base such as dimethylamine and DABCO (diazabicyclooctane), in which a transient dimethylamido palladium(Ⅱ) species likely involves.

Synthesis And Ionic Conductivity of Siloxane Based Polymer Electrolytes with Propyl Butyrate Pendant Groups

  • Jalagonia, Natia;Tatrishvili, Tamara;Markarashvili, Eliza;Aneli, Jimsher;Grazulevicius, Jouzas Vidas;Mukbaniani, Omar
    • Korean Chemical Engineering Research
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    • v.54 no.1
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    • pp.36-43
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    • 2016
  • Hydrosilylation reactions of 2.4.6.8-tetrahydro-2.4.6.8-tetramethylcyclotetrasiloxane with allyl butyrate catalyzed by Karstedt's, $H_2PtCl_6$ and Pt/C catalyst were studied and 2.4.6.8-tetra (propyl butyrate)-2.4.6.8-tetramethylcyclotetrasiloxane was obtained. The reaction order, activation energies and rate constants were determined. Ringopening polymerization of 2.4.6.8-tetra (propyl butyrate)-2.4.6.8-tetramethylcyclotetrasiloxane in the presence of $CaF_2$, LiF, KF and anhydrous potassium hydroxide in $60-70^{\circ}C$ temperature range was carried out and methylsiloxane oligomers with regular arrangement of propyl butyrate pendant groups were obtained. The synthesized products were studied by FTIR and NMR spectroscopy. The polysiloxanes were characterized by wide-angle X-ray, gel-permeation chromatography and DSC analyses. Via sol-gel processes of oligomers doped with lithium trifluoromethylsulfonate or lithium bis (trifluoromethylsulfonyl)imide, solid polymer electrolyte membranes were obtained. The dependences of ionic conductivity of obtained polyelectrolytes on temperature and salt concentration were investigated, and it was shown that electric conductivity of the polymer electrolyte membranes at room temperature changed in the range $3.5{\times}10^{-4}{\sim}6.4{\times}10^{-7}S/cm$.

Study on the Pyrolysis Kinetics of RDF(Refuse Derived Fuel) with Thermogravimetric Analysis (열중량 분석 기법을 통한 RDF의 열분해 특성 조사)

  • Kim, Dong-Won;Lee, Jong-Min;Kim, Jae-Sung
    • Korean Chemical Engineering Research
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    • v.47 no.6
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    • pp.676-682
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    • 2009
  • Devolatilization of the Refuse Derived Fuel(RDF) which is produced at WonJu in Korea was characterized in air atmosphere with variation of heating rate(10, 20 and $30^{\circ}C/min$) in TGA. The results of TG Analysis have shown that the pyrolysis and char combustion of the RDF occurred in the range of $350{\sim}700^{\circ}C$ depending on the heating rate. Activation energy of the RDF which was determined by using Friedman and Ozawa-Flynn-Wall method was in the range of 14.44~18.40 kcal/mol. Also, reaction order(n) and pre-exponential factors(A) were 1.219 and $3.02{\times}10^5$ by using Friedman method, respectively. In order to find out the devolatilization mechanism of the RDF, twelve solid-state mechanisms defined by Coats Redfern Method were tested. The results of the Coats Redfern Method have shown that chemical reaction is the effective mechanism by comparison with the value of the activation energy which was derived from the Friedman and Flynn-Wall-Ozawa method and correlation coefficient from twelve solid-state mechanisms of Coats Redfern Method. The solid state decomposition mechanism of the RDF was found to be a decelerated $F_1$ type, random nucleation with one nucleus on the individual particle.

Upconversion luminescence from poly-crystalline Yb3+, Er3+ co-doped NaGd(MoO4)2 by simple solid state method (Er3+, Yb3+ 이온이 동시 도핑된 NaGd(MoO4)2의 업컨버젼 분석)

  • Kang, Suk Hyun;Kang, Hyo Sang;Lee, Hee Ae;Shim, Kwang Bo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.26 no.4
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    • pp.159-163
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    • 2016
  • Up-conversion (UC) luminescence properties of polycrystalline $Er^{3+}/Yb^{3+}$ doped $NaGd(MoO_4)_2$ phosphors synthesized by a simple solid-state reaction method were investigated in detail. Used to 980 nm excitation (InfraRed area), $Er^{3+}/Yb^{3+}$ co-doped $NaGd(MoO_4)_2$ exhibited very weak red emissions near 650 and 670 nm, and very strong green UC emissions at 540 and 550 nm corresponding to the infra 4f transitions of $Er^{3+}(^4F_{9/2},\;^2H_{11/2},\;^4S_{3/2}){\rightarrow}Er^{3+}(^4I_{15/2})$. The optimum doping concentration of $Er^{3+}$, $Yb^{3+}$ for highest emission intensity was determined by XRD and PL analysis. The $Er^{3+}/Yb^{3+}$ (10.0/10.0 mol%) co-doped $NaGd(MoO_4)_2$ phosphor sample exhibited very strong shiny green emission. A possible UC mechanism for $Er^{3+}/Yb^{3+}$ co-doped $NaGd(MoO_4)_2$ depending on the pump power dependence was discussed.

Solid-state synthesis of yttrium oxyfluoride powders and their application to plasma spray coating (옥시불화이트륨 분말의 고상합성 및 플라즈마 스프레이 코팅 적용)

  • Lee, Jung-Il;Kim, Young-Ju;Chae, Hui Ra;Kim, Yun Jeong;Park, Seong Ju;Sin, Gyoung Seon;Ha, Tae Bin;Kim, Ji Hyeon;Jeong, Gu Hun;Ryu, Jeong Ho
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.31 no.6
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    • pp.276-281
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    • 2021
  • In order to manufacture a semiconductor circuit, etching, cleaning, and deposition processes are repeated. During these processes, the inside of the processing chamber is exposed to corrosive plasma. Therefore, the coating of the inner wall of the semiconductor equipment with a plasma-resistant material has been attempted to minimize the etching of the coating and particle contaminant generation. In this study, we synthesized yttrium oxyfluoride (YOF) powder by a solid-state reaction using Y2O3 and YF3 as raw materials. Mixing ratio of the Y2O3 and YF3 was varied from 1.0:1.0 to 1.0:1.6. Effects of the mixing ratio on crystal structure and microstructure of the synthesized YOF powder were investigated using XRD and FE-SEM. The synthesized YOF powder was successfully applied to plasma spray coating process on Al substrate.

An Experimental Study on Catalytic Reformer with Direct Spraying of Fuel and Water for SOFC (고체산화물 연료전지용 연료.물 직접 분무식 촉매 개질기에 관한 실험적 연구)

  • Lee, Dae-Keun;Dong, Sang-Geun;Yang, Je-Bok;Kim, Hak-Joo;Jung, Heon
    • 한국연소학회:학술대회논문집
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    • 2006.10a
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    • pp.260-265
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    • 2006
  • An experimental study on the catalytic reformer adopted in the auxiliary power unit system of solid oxide fuel cell was conducted. A 3-fluid nozzle, by which liquid fuel such as diesel, water and air are sprayed and uniformed mixed, was designed and used in this study. An electrically heated monolith inserted in the reformer was used for the vaporization of fuel and water in the transient state of reformer. The reformer uses the partial oxidizing reaction at the catalyst and the supply of water prevents the flame combustion in the spraying zone and lessens the deactivation of catalyst. The result showed that the reforming of liquid fuel can be started by the electrically heated monolith and the 3-fluid nozzle can give the uniform mixing of fuel, water and air. It was also found that the reformer fueled by n-hexadecane can make the reformate, at best, containing $H_2$ at 15.5% and CO at 11.5% that are used as fuel in the solid oxide fuel cell.

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Hydration and time-dependent rheology changes of cement paste containing ground fly ash

  • Chen, Wei;Huang, Hao
    • Computers and Concrete
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    • v.11 no.1
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    • pp.39-49
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    • 2013
  • The use of ground fly ash in concrete can increase the risk of slump loss due to the drastic surface change of the particles after the grinding treatment and the accelerated reaction compared to the untreated ash. This study is aimed at the early age hydration and time-dependent rheology changes of cement paste containing ground fly ash. An original fly ash is ground into different fineness and the hydration of cement paste containing the ground fly ash is monitored with the ultrasound propagation method. The zeta potentials of the solid particles are measured and the changes of rheological parameters of the cement pastes with time are analyzed with a rheometer. A particle packing model is used to probe packing of the solid particles. The results show that the early age hydration of the paste is strongly promoted by replacing Portland cement with fly ash up to 30 percent (by mass), causing increase of the yield stress of the paste. The viscosity of a paste containing ground fly ash is lower than that containing the untreated ash, which is explained by the denser packing of the solid particles.

Electrolyte Preparation and Characteristics of La1-xSrxMnO3 for Solid Oxide Fuel Cell (고체전해질형 연료전지용 전해질 제작 및 La1-xSrxMnO3의 특성에 관한 고찰)

  • Rim, Hyung-Ryul;Lee, Ju-Seong
    • Applied Chemistry for Engineering
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    • v.7 no.1
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    • pp.9-17
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    • 1996
  • Solid oxide electrolytes of 8mol% YSZ($Y_2O_3$ stabilized zirconia) were prepared at various sintering conditions and their ionic conductivities were measured. The highest ionic conductivity of $10^{-1}S.cm^{-1}$ was obtained when the sintering temperature was 1400oC and the sintering time was 10hr. Also the cathode material, $La_{1-x}Sr_xMnO_3$ was prepared by solid state reaction method and the overpotential, electrical conductivity, and charge transfer resistance between cathode material and YSZ electrolyte were studied. It was found that the optimum doping content of Sr for La was 50mo1%.

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Interface chemistry of SiC/Co reaction (SiC/Co 반응의 계면화학)

  • ;Hubertus Nickel
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.5 no.2
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    • pp.109-121
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    • 1995
  • Reaction coulples of SiC with cobalt were annealed in an Ar/4 vol% $H_2$ atmosphere at temperatures between $950^{\circ}C$ and $1250^{\circ}C$for various times between 4 and 100 h. At temperatures above $950^{\circ}C$, solid state reactions lead to the formation of various silicides with carbon precipitates. The typical reaction layer sequence was $SiC/CoSi + C/CozSi + C/CozSi/CozSi + C/{\cdot\cdot\}/CO_2Si/CO$ in the reaction zone. The mechanism of the periodic band structure formation with the carbon precipitation behaviour was examined and discussed in terms of reaction kinetics and thermodynamic considerations. The growth of the reaction zone has a square root of time dependence. The reaction kinetics is proposed to estimate the effective reaction constant from the parabolic gowth of the reaction zone. The mechanical properties of the reaction zones were determined by the microhardness test.

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Synthesis and Superconductivity in $(Ru_{0.8}Nb_{0.2})Sr_2(Gd_{1.5-x}Nd_xCe_{0.5})Cu_2O_z$ System ($(Ru_{0.8}Nb_{0.2})Sr_2(Gd_{1.5-x}Nd_xCe_{0.5})Cu_2O_z$ 계의 합성 및 초전도 특성)

  • Lee, H.K.;Bae, S.M.
    • Progress in Superconductivity
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    • v.10 no.2
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    • pp.128-132
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    • 2009
  • Polycrystalline samples of $(Ru_{0.8}Nb_{0.2})Sr_2(Gd_{1.5-x}Nd_xCe_{0.5})Cu_2O_z$($ 0{\leq}x{\leq}1.25$) have been synthesized by a solid-state reaction route. The X-ray diffraction data revealed that the Nd solubility limit can be placed between x=0.5 and x=0.75. The superconducting transition temperature decreased with increasing Nd content, confirming that Nd entered the lattice. Room-temperature thermoelectric power measurements showed that all the samples are in the underdoped state and the partial substitution of Nd for Gd resulted in a decrease in the carrier density on the superconducting layers.

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