• Title/Summary/Keyword: Solid-phase syntheses

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Hydrothermal Synthesis of PZT Powders. (수열법에 의한 PZT분말 합성 연구)

  • 최승도;박병규
    • Korean Journal of Crystallography
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    • v.8 no.2
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    • pp.97-104
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    • 1997
  • Hydrothermal synthesis of PbZ1-xTixO3 has been investigated. Syntheses were performed using lead acetate triphdrate as Pb source, Ti/Zr gel by hydrolizing Ti-isopropoxide as Tiand Zr source and Zr-propoxide and KOH (0.5m, 1m, 2m) as mineralizer. The hydrothermal synthesis has been examined at 140℃, 150℃ and 160℃. Synthesized PZT powders showed a rectangular shape and were agglomerate. At 1m and 2m KOH concentrations PZT powders were synthesized the respective time of 8 hrs and 1hr but at 0.5m KOH concentration phase pure PZT powders were not synthesized for 5days reaction. At the conditions of low temperature and low KOH concentration unreacted Ti/Zr gel remained although synthesized powders were almost PZT. The size of PZT powders increased with KOH concentrations. PbO solid solutions were formed as intermediate phases and these were classified to PbO-10%TiO2 solid solution and PbO-3% TiO-3% TiO2 solid solution.

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A Study on the Synthesis and Consolidation of Ti3Al by Electro-Discharge (전기방전에 의한 Ti3Al의 합성 및 소결 특성 연구)

  • Jang, Hyungsun;Cho, Yujung;Kang, Taeju;Kim, Kibeom;Lee, Wonhee
    • Korean Journal of Metals and Materials
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    • v.47 no.8
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    • pp.488-493
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    • 2009
  • Direct syntheses of bulk $Ti_3Al$ via electro-discharge-sintering (EDS) of a stoichiometric elemental powder mixture were investigated. A capacitor bank of $450{\mu}F$ was charged with three input energies, 0.5, 1.0, and 1.5 kJ. The charged capacitor bank was then instantaneously discharged through 0.3 g of a Ti-25.0 at.%Al powder mixture for consolidation. Complete phase transformation occurred in less than $200{\mu}sec$ by the discharge and a bulk $Ti_3Al$ compact was obtained. Compared with consolidated samples fabricated by conventional methods such as high vacuum sintering and casting, the electro-discharge-sintered $Ti_3Al$ compact shows a very fine microstructure with a hardness value of 425 Hv. Electro-discharge-sintering under a $N_2$ atmosphere successfully modified the surface Ti oxide of the $Ti_3Al$ compact into Ti nitride, which concurred with the synthesis and consolidation of $Ti_3Al$. Complete conversion yielding a single phase $Ti_3Al$ is primarily dominated by the fast solid state diffusion reaction.

mPW1PW91 Calculated and Experimental UV/IR Spectra of Unsymmetrical trans-Stilbenes

  • Choe, Jong-In;Park, Seong-Jun;Cho, Chul-Hee;Kim, Chul-Bae;Park, Kwang-Yong
    • Bulletin of the Korean Chemical Society
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    • v.31 no.8
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    • pp.2175-2179
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    • 2010
  • Quantum mechanical properties of unsymmetrical and unfunctionalized trans-stilbene derivatives 1-3, which had been prepared by solid-phase parallel syntheses, were characterized using mPW1PW91/6-311G(d,p) (hybrid HF-DF) calculations. The total electronic energies, normal vibrational modes, Gibbs free energies, and HOMOs and LUMOs of sixteen different structures from three different groups were analyzed. The energy differences between the HOMOs and LUMOs of the various unsymmetrical trans-stilbenes are in accord with the maximum absorption peaks of the experimental UV spectra of 1-3. The calculated normal vibrational modes of 21 were comparable with its experimental IR spectrum. The $\pi$-conjugation in the para-connected biphenyl group of 2 is better than the one in the metaconnected biphenyl group on the shorter side of 3.

Syntheses and Arene Transport Studies of Water Soluble Aminomethylcalixarene (수용성 아미노메틸칼릭스아렌의 합성 및 방향족 물질의 통과실험 연구)

  • Kye Chung Nam;Dae Soon Kim
    • Journal of the Korean Chemical Society
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    • v.36 no.6
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    • pp.933-940
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    • 1992
  • Calix[6]arene react with formaldehyde and secondary amines to yields water soluble Mannich bases which can be converted to the corresponding quaternary salts. Treatment of the quaternary salts with a nucleophile such as cyano, ethoxy, and hydride yields p-substituted calix[6]arenes. Calix[8]arene too react with formaldehyde and diallyl amine to yield a water soluble Mannich base. The transport of neutral arenes through an aqueous phase along a concentration gradient mediated by those of water soluble calixarenes as molecular carrier was studied in a U-type cell. Naphthalene, anthracene, pyrene, and fluoranthene are tested as a neutral solid guest compounds for the transport experiment.

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Syntheses, Dielectric Properties and Ordering Structures of $Pb(Fe _{1/2}Ta_{1/2})O_3$ ($Pb(Fe _{1/2}Ta_{1/2})O_3$의 합성, 유전특성 및 질서배열구조)

  • 우병철;김병국;김병호
    • Korean Journal of Crystallography
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    • v.13 no.3_4
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    • pp.165-171
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    • 2002
  • Single phase $Pb(Fe_{1/2}Ta_{1/2})O_3$, ceramics were successfully synthesized from the powders prepared by solid state reaction (sintering temperature: $1100^{\circ}C$, density: $9.3g/cm^3$, average grain size: $5.1{\pm}1.2mm$, space group: Pm3m). Their dielectric properties measured at $-150{\sim}50^{\circ}C$ showed the maximum relative dielectric constant of 31000 at $-41^{\circ}C$. 1 kHz, and typical relaxor ferroelectrics characteristics such as diffuse phase transition and dielectric relaxation phenomena. However, the diffuseness of phase transition decreased and the dielectric properties became more normal ferroelectrics as the time of annealing at $1000^{\circ}C$ increased. By using Raman spectroscopy, it was revealed that the $Fe^{3+}$ and $Ta^{5+}$ ions in the as-sintered $Pb(Fe_{1/2}Ta_{1/2})O_3$, are stoichiometrically 1 : 1 ordered within the short-range that can not be probed even by transmission electron microscopy, and this stoichiometric 1 : 1 ordering is enhanced by the annealing. The relaxor ferroelectric characteristics in the as-sintered $Pb(Fe_{1/2}Ta_{1/2})O_3$, could be correlated with the stoichiometric 1 : 1 short-range ordering of B-site cations, and the decrease of relaxor ferroelectric characteristics in the annealed $Pb(Fe_{1/2}Ta_{1/2})O_3$ could be correlated with the enhanced stoichiometric 1 : 1 short-range ordering of B-site cations.