• Title/Summary/Keyword: Solid-phase syntheses

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Direct Solid State Synthesis of Zn4Sb3 by Hot Pressing and Thermoelectric Properties (열간 압축 공정에 의한 Zn4Sb3의 직접 고상 반응 합성 및 열전특성)

  • Ur Soon-Chul
    • Journal of Powder Materials
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    • v.12 no.4 s.51
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    • pp.255-260
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    • 2005
  • Direct solid state synthesis by hot pressing has been applied in order to produce high efficiency $Zn_4Sb_3$ bulk specimens. Single phase $Zn_4Sb_3$ with 98.5% of theoretical density was successfully produced by direct hot pressing of elemental powders containing 1.2 at.% excess Zn. Thermoelectric properties as a function of temperature were investigated from room temperature to 600 K and compared with results of other studies. Transport properties at room temperature were also evaluated. Thermoelectric properties of single phase $Zn_4Sb_3$ materials produced by direct synthesis were measured and are comparable to the published data. Direct solid state synthesis by hot pressing provides a promising processing route in this material.

Simple and Highly Efficient Synthesis of [$^{11}C$]methionine Using Solid-Phase Extraction Method (고정상 추출법을 이용한 효율적인 [$^{11}C$]methionine의 합성)

  • Lim, Sung-Jae;Moon, Woo-Yeon;Choi, Jae-Chil;Cho, Shee-Man;Oh, Seung-Jun
    • The Korean Journal of Nuclear Medicine Technology
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    • v.12 no.3
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    • pp.181-183
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    • 2008
  • We developed simple and highly efficient synthesis method for [$^{11}C$]methionine using solid-phase extraction method. For synthesis, we used C18 cartridge. [$^{11}C$]methionine was synthesized on C18 cartridge according to the solid-phase [$^{11}C$]methylation of precursor L-homocysteine thiolactone hydrochloride. The radiochemical yields of [$^{11}C$]methionine was $48.9{\pm}7.93%$ decay corrected (results of 30 syntheses, mean$\pm$SD), with average production higher than 180 mCi. This procedure showed high yield and simple synthesis of [$^{11}C$]methionine.

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Smart Solid State Syntheses of Well-Crystallized Phase Pure Mixed Oxides for Electroceramics

  • Sennat, Mamoru
    • Journal of the Korean Ceramic Society
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    • v.43 no.11 s.294
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    • pp.680-687
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    • 2006
  • An overview is given to optimize the solid state processes toward phase pure and well-crystallized fine particulates of mixed oxides, serving as electroceramic materials in various genres. Elevation of the reactivity and preservation of stoichiometry of the starting mixture are of universal importance. Mechanical activation is versatile for these purposes, particularly when an oxygen atom as a hinge promotes formation of hetero-bridging bonds between dissimilar cationic species prior to calcination. Case studies carried out recently in the author's laboratory are displayed and compared for ferroelectric materials, i.e. $PbMg_{1/3}Nb_{2/3}O_3$ $xPbTiO_3$(PMN-PT), $(1-y)Pb(Zn_xMg{1-x})_{1/3}$ $yNb_{2/3}O_3$ (PZN-PMN), $BaBi_2Ta_2O_9$ (BBT), $Ba(Mg_{1/3}Ta_{2/3})O_3$ (BMT), and ferromagnetics, i.e. M-, Y-, and Z-phases of Ba-hexaferrites.

Phase Transfer Catalyst (PTC) Catalyzed Alkylations of Glycinamides for Asymmetric Syntheses of $\alpha$-Amino Acid Derivatives

  • Park, Seon Yeong;Kim, Hyeon Ju;Im, Dong Yeol
    • Bulletin of the Korean Chemical Society
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    • v.22 no.9
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    • pp.958-962
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    • 2001
  • The chiral amine auxiliary mediated stereoselective alkylation reactions of glycinamides 1-6 and 15-17 using phase transfer catalyst (PTC) for liquid-solid extraction are described. The secondary N-(diphenylmethylene) glycinamides 1, 2 and 3 give better selectivities and yields than tertiary N-(diphenylmethylene) glycinamides 4, 5 and 6. Alkylation of the glycinamide 1 and 2 using 18-Crown-6 as a PTC in toluene at $-40^{\circ}C$ gives best selectivities and yields. Alkylations of N-(4-chlorophenylmethylene)glycinamides 15, 16 and 17 under same PTC conditions give $\alpha$, $\alpha-disubstituted$ amino acid derivatives 18, 19 and 20 with low diastereoselectivities.

Syntheses and Characteristics of $Ln_xCa_{2-x}MnO_4$ {Ln=Gd, Nd, Pr, Sm} ($Ln_xCa_{2-x}MnO_4$ 상의 합성과 특성에 관한 연구 {Ln=Gd, Nd, Pr, Sm})

  • Seo, Sang-Il;Lee, Jai-Yeoul
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2000.05b
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    • pp.196-199
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    • 2000
  • Since the reports of CMR(colossal magnetoresistance) effects in some single crystal R-P phase $La_{1+x}Sr_{2-x}Mn_2O_7$, considerable researches have been carried out to find optimum composition and to understand the role of dimensionality in the CMR mechanism of this system. In this study, layered perovskite $Ln_xCa_{1-x}MnO_{4}$ (x=0.5, Ln=Pr, Nd, Sm, Gd) phases were synthesized by solid state reaction and their structures were refined by Rietveld method. Electrical and magnetic properties were measured between room temperature and liquid helium temperature and compared with those of two dimensional $La_{1.4}Sr_{1.6}Mn_2O_7$ phase.

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Syntheses and structure refinement of $Ln_{x}MnO_{4}$ {Ln=Gd, Nd, Pr, Sm} ($Ca_{2-X}-Ln_{x}MnO_{4}$상의 합성과 결정구조 정밀화 {Ln=Gd, Nd, Pr, Sm})

  • 서상일;이재열
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2000.07a
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    • pp.726-729
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    • 2000
  • Though L $a_{1+x}$S $r_{2-x}$M $n_2$ $O_{7}$ n=2 R-P phases have been well known to have CMR effect, it was generally believed that n=1 phase was insulating. But recently monolayered perovskite $Ca_{2-x}$L $n_{x}$Mn $O_4$phase has been reported to show magnetoresistance. In this study, layered perovskite $Ca_{2-x}$L $n_{x}$Mn $O_4$ (x=0, 0.5, Ln=Pr, Nd, Sm, Gd) phases were synthesized by solid state reaction and their structures were refined by Rietveld method. The space groups of $Ca_2$Mn $O_4$, N $d_{0.5}$C $a_{1.5}$Mn $O_4$phases were refined as C2cb and Fmmm, respectively.y.ely.y.y.y.y.y.y.

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Syntheses and Characteristics of Layered Perovskite $La_{2-x}Ca_{1+x}Mn_{2}O_{7}$ (층상구조형 페롭스카이트 $La_{2-x}Ca_{1+x}Mn_{2}O_{7}$상의 합성 및 특성)

  • 서상일;이재열
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2000.11a
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    • pp.555-558
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    • 2000
  • Layered perovskite La$_{2-x}$Ca$_{l-x}$Mn$_2$O$_{7}$ phases were synthesized by solid state reaction. Single phase R-P could be obtained in the range of 0.4$_{2-x}$Ca$_{l-x}$Mn$_2$O$_{7}$. About 30% of MR ratio was obtained at 270K when 5 T of magnetic field was applied.ied.ied.ied.

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Syntheses and Characteristics of R-P Phase $Ln_{1-x}Sr_{2-x}Mn_2O_7$(Ln=La, Pr, Gd, Eu, Er, Nd, Sm) (R-P Phase $Ln_{1-x}Sr_{2-x}Mn_2O_7$(Ln=La, Pr, Gd, Eu, Er, Nd, Sm)의 합성 및 특성연구)

  • 송민석;서상일;이재열
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 1999.05a
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    • pp.337-340
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    • 1999
  • Since the first reports of CMR(colossal magnetoresistance) effects in some single crystal R-P Phase Ln$_{1-x}$ Sr$_{2-x}$Mn$_{2}$O$_{7}$ 1996. many researches have been carried out to find optimum compositions and processing conditions in this system. In this study, layered perovskite R-P Phase Ln$_{1-x}$ Sr$_{2-x}$Mn$_{2}$O$_{7}$ (x=0.4, Ln=-La, Eu, Gd, Nd, Pr, Sm) phases were synthesized by solid state reaction and their structures were refined by Rietveld method. Electrical and magnetic properties were measured drown to 20K and compare with those of R-P Phase Ln$_{1-x}$ Sr$_{2-x}$Mn$_{2}$O$_{7}$ Phases.es.es.es.es.es.

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A Solid Phase Synthesis of Dihydro-1,4-dioxin and Dihydro-1,4-oxathiin Carboxanilides Using Polymer-bound Oxime Ester (고체상에 연결된 옥심 에스테르를 이용한 다이하이드로-1,4-다이옥신 및 다이하이드로-1,4-옥사티인 카르복스아닐라이드 유도체의 고체상 합성)

  • Hahn, Hoh-Gyu;Bae, Su-Yeal;Nam, Kee-Dal
    • The Korean Journal of Pesticide Science
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    • v.10 no.1
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    • pp.1-6
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    • 2006
  • A methodology for the syntheses of carboxanilides using solid support of 4-chloro-3-nitorbenzophenone oxime resin 5 was developed. Condensation of 4-chloro-3-nitorbenzophenone resin 6 with hydroxylamine hydrochloride salt gave oxime resin 5. The reaction of oxime resin 5 with dioxin and oxathiin derivatives 7a-d afforded the corresponding polymer-bound dioxin and oxathiin derivatives 9a-d. These polymer-bound resins 9a-d were treated respectively with aniline in the presence of acetic acid resulted in the corresponding dioxin carboxanilides 10a-d (yield, 5%-quantitative).