• Title/Summary/Keyword: solid state phase synthesis

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Peculiarities of SHS and solid state synthesis of $ReBa_{2}Cu_{3}O_{7-x}$ materials

  • Sho, Dea-Wha;Li, Yingmei;Cho, Yong-Joon;Kim, Tae-Wan;Korobova, N.;Isaikina, O.;Mansurov, Z.;Baydeldinova, A.;Ksandopoulo, G.
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2001.07a
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    • pp.620-623
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    • 2001
  • The peculiarities of using Self-propagating High-temperature Synthesis (SHS) and solid state phase synthesis for production of high temperature superconductor materials are discussed. Oxide superconductors with general formula $ReBa_2$$Cu_3$$O_{7-x}$ (Re= Y, Yb, Sm, Nd) have been made with using barium oxide initial powder instead of traditional barium carbonate. X-ray powder diffraction showed a single phase orthorhombic perovskite structure was produced in all reactions. Phenomena observed during the grinding of the reactant mixture are presented. Mechano-chemical activation - as a pretreatment of the reactant mixture - strongly influences the kinetic parameters, the reaction mechanism, and the composition and structure of the final product.

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Solid Phase Synthesis of 3-(4-Hydroxyphenyl)coumarin: Preliminary Experiments for Combinatorial Synthesis of Substituted 3-Phenylcoumarin Derivatives

  • Bae, Hoon;Kim, Hak-Sung
    • Archives of Pharmacal Research
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    • v.27 no.8
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    • pp.811-815
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    • 2004
  • Coumarin and its derivatives occur widely in nature. Many attempts were made for synthesis of various coumarin derivatives because of their interesting biological activities. In this study, solid phase synthetic approach of 3-(4-hydroxyphenyl)coumarin was achieved for combinatorial synthesis of substituted 3-phenylcoumarin analogues. Starting from 4-hydroxyphenylacetic acid methyl ester, release of 3-(4-hydroxypnehyl)coumarin from polymer support was accom-plished.

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.

Synthesis of Zn4Sb3 by Solid State Reaction and Hot Pressing, and Their Thermoeletric Properties (고상 합성과 진공 압축성형에 의한 Zn4Sb3의 제조 및 열전특성)

  • Ur Soon-Chul
    • Korean Journal of Materials Research
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    • v.15 no.7
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    • pp.473-479
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    • 2005
  • Thermoelectric $Zn_4Sb_3$ alloys were synthesized by a conventional powder metallurgy process consisting of solid state reaction and hot pressing. Single phase $Zn_4Sb_3$ was successfully produced by the annealing of cold compact starting with the mixed elemental powders, and subsequent hot pressing yielded single phase bulk specimens without microcracks. Phase transformations in this alloy system during synthesis were investigated using XRD, SEM and EDS. Thermoelectric properties as a function of temperature were investigated from room temperature to 600 K and compared with results of analogue studies. Transport properties at room temperature were also evaluated. Thermoelectric properties of single phase $Zn_4Sb_3$ materials produced by this process are comparable to the published data. Synthesis by solid state reaction and hot pressing offers a potential processing route to produce a bulk $Zn_4Sb_3$

The SrLiAl3N4:Eu2+ Phosphor Synthesized by the Raw Material Model Obtained by DFT Calculations

  • Park, Woon Bae
    • Journal of the Korean Ceramic Society
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    • v.54 no.3
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    • pp.217-221
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    • 2017
  • Improvement studies of existing phosphors are needed for use in light emitting diodes (LEDs). Among the phosphors discovered recently, the SLA ($SrLiAl_3N_4:Eu^{2+}$) is a phosphor that has a narrow width. It is now known as a good red phosphor that meets the industry's needs for warm white (color temperature ranging from 2700 to 4000 K) and high CRI (> 80). However, SLA phosphors are obtained from difficult synthetic methods. All commercially available phosphors should be derived from the general solid state synthesis method. The phosphors produced by difficult synthetic methods will inevitably fall out of price competitiveness and will be scrapped. This study succeeded in synthesizing SLA ($SrLiAl_3N_4:Eu^{2+}$) phosphors by using a general solid phase synthesis method based on the reaction energy obtained from DFT calculations. As a result, we found an optimal solid state synthesis method for SLA phosphors.

Reaction Characterization of Y2Ba1CU1O5 Oxides by Solid State Reaction Method and Pyrophoric Synthesis Method (고상반응법과 발화합성법에 의한 Y2Ba1CU1O5 산화물의 반응특성)

  • Park, Jeong-Shik
    • Applied Chemistry for Engineering
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    • v.10 no.5
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    • pp.772-777
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    • 1999
  • $Y_2Ba_1Cu_1O_5(Y211)$ powders were prepared by pyrophoric synthesis method and by solid state reaction method using $Y_2O_3(99.9%)$, $BaCO_3(99.9%)$, and CuO(99.9%) powders in both of these processes. The phase formation and reaction kinetics of $Y_2Ba_1Cu_1O_5$ powders have been studied using X-ray diffraction analysis(XRD) of samples at various heat treatment temperatures and reaction time. The reaction characterization suggested that the phase formation rate is mainly controlled by the particle size of Y211 powders. The activation energy(${\Delta}E_a$) of Y211 phase formation in this pyrophoric synthesis method was found to be 136.42 kJ/mol compared with 149.46 kJ/mol for that of solid state reaction method. These results data showed that the pyrophoric synthesis method is kineticaly more efficient than the solid state reaction method in this $Y_2Ba_1Cu_1O_5$ system.

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Synthesis of Decapeptide of L-Aspartic Acid and Benzyl-L-Aspartic Acid by Solid Phase Peptide Synthesis

  • Yoo, Bong-K.;Jalil Miah, M.A.;Lee, Eung-Seok;Han, Kun
    • Archives of Pharmacal Research
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    • v.28 no.7
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    • pp.756-760
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    • 2005
  • Polyene macrolide amphotericin B (AmB) is the drug of choice for the treatment of disseminated fungal infections. However, because of its pronounced side effects, the drug has limited applicability. There are few interesting reports, which state that co-administration of the drug with homo-peptide of polyaspartic acid reduces the side effects of the drug. In our present study, an approach has been made to systematically synthesize low molecular weight heteropeptides consisting of L-aspartic acid and its derivative. It was hypothesized that such heteropeptides will reduce the toxic side effects of the drug by facile hydrophobic binding between the polymer and the drug. We have employed the strategy of solid phase peptide synthesis (SPPS) to synthesize low molecular weight hetero-peptides by using L-aspartic acid and benzyl-L-aspartic acid to induce the hydrophobic binding between the peptide and the drug. In future, the proposed methodology can be employed to tailor other polypeptides substituted with benzyl groups to reduce the nephrotoxicity of AmB.

Wet Chemical Preparation of Li-rich LiMn$_2$O$_4$ Spinel by Oxalate Precipitation (Oxalate 침전을 이용한 Li-과량 LiMn$_2$O$_4$ Spinel의 습식합성가 분말 특성)

  • 이병우;김세호
    • Journal of the Korean Ceramic Society
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    • v.36 no.7
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    • pp.698-704
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    • 1999
  • Li rich Li1+xMn2-xO4(x=0.07) spinel powders were prepared by an oxalate precipitation of wet chemical methods at temperature lower than $600^{\circ}C$. The FTIR results showed that the powders prepared at $600^{\circ}C$ had high degree of crystal quality comparing with the spinel powders prepared by solid state reaction at 75$0^{\circ}C$ which was the lowest synthesis temperature of the solid state reaction method. The particle size of powders prepared by the oxalate precipitation at $600^{\circ}C$ was smaller than 0.2${\mu}{\textrm}{m}$ and the specific surface area was 11.01 m2/g A heat treatment over 90$0^{\circ}C$ formed second phase in the precipitates. It was shown that there were phase transitions at temperatures. T1,T2 and T2. The transitions involved weight loss and gain during heating and cooling. The low temperature synthesis below $600^{\circ}C$ avoided the second phase formation and the prepared powders showed improved compositional and physical properties for secondary lithium battery applications.

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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.

The Synthesis of Lithium Lanthanum Titanium Oxide for Solid Electrolyte via Ultrasonic Spray Pyrolysis (초음파 분무 열분해법을 이용한 고체전해질용 Lithium Lanthanum Titanium Oxide 제조)

  • Jaeseok, Roh;MinHo, Yang;Kun-Jae, Lee
    • Journal of Powder Materials
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    • v.29 no.6
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    • pp.485-491
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    • 2022
  • Lithium lanthanum titanium oxide (LLTO) is a promising ceramic electrolyte because of its high ionic conductivity at room temperature, low electrical conductivity, and outstanding physical properties. Several routes for the synthesis of bulk LLTO are known, in particular, solid-state synthesis and sol-gel method. However, the extremely low ionic conductivity of LLTO at grain boundaries is one of the major problems for practical applications. To diminish the grain boundary effect, the structure of LLTO is tuned to nanoscale morphology with structures of different dimensionalities (0D spheres, and 1D tubes and wires); this strategy has great potential to enhance the ion conduction by intensifying Li diffusion and minimizing the grain boundary resistance. Therefore, in this work, 0D spherical LLTO is synthesized using ultrasonic spray pyrolysis (USP). The USP method primarily yields spherical particles from the droplets generated by ultrasonic waves passed through several heating zones. LLTO is synthesized using USP, and the effects of each precursor and their mechanisms as well as synthesis parameters are analyzed and discussed to optimize the synthesis. The phase structure of the obtained materials is analyzed using X-ray diffraction, and their morphology and particle size are analyzed using field-emission scanning electron microscopy.