• Title/Summary/Keyword: Solid-phase reaction

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Synthesis of $WS_2$ Solid Lubricant ($WS_2$ 고체 윤활제의 합성)

  • 신동우;윤대현;황영주;김성진;김인섭
    • Tribology and Lubricants
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    • v.13 no.4
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    • pp.60-65
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    • 1997
  • The tungsten disulfide $(WS_2)$ solid lubricant was synthesized by two different reaction processes, i.e., the reaction between $CS_2$ gas phase and solid $WO_3$powder, and the vapour phase transport method of tungsten and sulfur in a high vacuum. The chemical and physical characteristics of synthesized $WS_2$powder were analyzed in terms of the average particle size, morphology, crystalline phase etc. in comparison with those of commercial $WS_2$powder. The solid $WO_3$ powder with the average size of 0.2 ${\mu}{\textrm}{m}$ was reacted with $CS_2$gas flowed with$N_2$or 96%$N_2{\times}4%H_2$forming gas for 36 h and 24 h at 90$0^{\circ}C$ respectively. $WS_2$ crystalline phase was then formed through the intermediate phase of .$W_{20}O_{58}$ In the case of vapour phase transport method, the 3.5 wt% iodine was added as a vapour transport reagent into the composition of tungsten and sulfur powders maintaining a constant molar ratio of W:S=1:2.2. The mixture was then heat treated at 85$0^{\circ}C$ for 2 weeks in vacuum. The reaction product obtained showed the average size of 12 ${\mu}{\textrm}{m}$ and the hexagonal plate shape of typical solid lubricant with 2H-$WS_2$crystalline phase.

Characterization of Synthesized WS$_2$ Solid Lubricant (합성 WS$_2$ 고체윤활제의 특성 분석)

  • 신동우;윤대현;최인혁;김인섭
    • Proceedings of the Korean Society of Tribologists and Lubrication Engineers Conference
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    • 1997.10a
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    • pp.211-216
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    • 1997
  • The tungsten disulfide (WS$_2$) solid lubricant was synthesized by two different reaction processes, and the chemical and physical characteristics of synthesized WS$_2$ powder were analyzed in terms of the average particle size, morphology, crystalline phase. The solid WO$_3$ powder with the average size of 0.2 $\mu$m was reacted with CS$_2$ gas flowed with N$_2$ or 96% N$_2$ + 4% H$_2$ forming gas for 36 h and 24 h at 900$\circ$C respectively. In the case of vapour phase transport method, the 3.5 wt% iodine was added as a vapour transport reagent into the composition of tungsten and sulfur powders maintaining a constant molar ratio of W : S = 1 : 2.2. The mixture was then heat treated at 850$\circ$C for 2 weeks in vacuum The reaction product obtained showed the average size of 12 $\mu$m and the hexagonal plate shape of typical solid lubricant with 2H-WS$_2$ crystalline phase.

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Solid-liquid phase equilibria on the GdBa2Cu3O7-δ stability phase diagram in low oxygen pressures (1 - 100 mTorr)

  • Lee, J.W.;Lee, J.H.;Moon, S.H.;Yoo, S.I.
    • Progress in Superconductivity and Cryogenics
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    • v.14 no.4
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    • pp.28-31
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    • 2012
  • We report the solid-liquid phase equilibria on the $GdBa_2Cu_3O_{7-{\delta}}$ (GdBCO) stability phase diagram in low oxygen pressures ($PO_2$) ranging from 1 to 100 mTorr. On the basis of the GdBCO stability phase diagram experimentally determined in low oxygen pressures, the isothermal sections of three different phase fields on log $PO_2$ vs. 1/T diagram were schematically constructed within the $Gd_2O_3-Ba_2CuO_y-Cu_2O$ ternary system, and the solid-liquid phase equilibria in each phase field were described. The invariant points on the phase boundaries include the following three reactions; a pseudobinary peritectic reaction of $GdBCO{\leftrightarrow}Gd_2O_3$ + liquid ($L_1$), a ternary peritectic reaction of $GdBCO{\leftrightarrow}Gd_2O_3+GdBa_6Cu_3O_y$ + liquid ($L_2$), and a monotectic reaction of $L_1{\leftrightarrow}GdBa_6Cu_3O_y+L_2$. A conspicuous feature of the solid-liquid phase equilibria in low $PO_2$ regime (1 - 100 mTorr) is that the GdBCO phase is decomposed into $Gd_2O_3+L_1$ or $Gd_2O_3+GdBa_6Cu_3O_y+L_2$ rather than $Gd_2BaCuO_5+L$ well-known in high $PO_2$ like air.

Formation of Ti-B-N-C Ceramic Composite Materials via a Gas-Solid Phase Reaction

  • Yoon, Su-Jong
    • Korean Journal of Materials Research
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    • v.16 no.1
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    • pp.50-57
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    • 2006
  • Phase mixtures of Titanium boride, nitride, and carbide powder were produced by the reduction of a mixture of titanium and boron oxides with carbon via a gas-solid phase reaction. Boron oxides produce a vapour phase or decompose to a metal sub-oxide gaseous species when reduced at elevated temperature. The mechanism of BO sub-oxide gas formation from $B_2O_3$ and its subsequent reduction to titanium diboride for the production of uniform size hexagonal platelets is explained. These gaseous phases are critical for the formation of boride, nitride and carbide ceramics. For the production of ceramic phase composite microstructures, the nitrogen partial pressure was the most critical factor. Some calculated equilibrium phase fields has been verified experimentally. The theoretical approach therefore identifies conditions for the formation of phase mixtures. The thermodynamic and kinetic factors that govern the phase constituents are also discussed.

Efficient Macrocyclization for Cyclicpeptide Using Solid-Phase Reaction

  • Kim, Joong-Hup;Hong, Il-Khee;Kim, Hyo-Jeong;Jeong, Hyeh-Jean;Choi, Moon-Jeong;Yoon, Chang-No;Jeong, Jin-Hyun
    • Archives of Pharmacal Research
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    • v.25 no.6
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    • pp.801-806
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    • 2002
  • Cyclicpeptides are important targets in peptide synthesis because of their interesting biological properties. Constraining highly flexible linear peptides by cyclization is one of the mostly widely used approaches to define the bioactive conformation of peptides. Cyclic peptides often have increased receptor affinity and metabolic stability over their linear counterparts. We carried out virtual screening experiment via docking in order to understand the interaction between HLE-Human Leukocyte Elastase and ligand peptide and to identify the sequence that can be a target in various ligand peptides. We made cyclic peptides as a target base on Metlle-Phe sequence having affinity for ligand and receptor active site docking. There are three ways to cyclize certain sequences of amino acids such as Met-lie-Phe-Gly-Ile. First is head-to-tail cyclization method, linking between N-terminal and C-terminal. Second method utilizes amino acid side chain such as thiol functional group in Cys, making a thioether bond. The last one includes an application of resin-substituted amino acids in solid phase reaction. Among the three methods, solid phase reaction showed the greatest yield. Macrocyclization of Fmoc-Met-Ile-Phe-Gly-Ile-OBn after cleavage of Fmoc protection in solution phase was carried out to give macrocyclic compound 5 in about 7% yield. In the contrast with solution phase reaction, solid phase reaction for macrocyclization of Met-Ile-Phe-Gly-Ile-Asp-Tentagel in normal concentrated condition gave macrocyclic compound 7 in more than 35% yield.

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 $Zn_4Sb_3$

Reaction of Gae-Phase Atomic Hydrogen with Chemisorbed Hydrogen Atoms on an Iron Surface

  • Kim, M. S.;Ree, J.
    • Bulletin of the Korean Chemical Society
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    • v.18 no.9
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    • pp.985-994
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    • 1997
  • The reaction of gas-phase atomic hydrogen with hydrogen atoms chemisorbed on Fe(110) surface is studied by use of classical trajectory procedures. Flow of energy between the reaction zone and bulk solid phase has been treated in the generalized Langevin equation approach. A London-Eyring-Polanyi-Sato energy surface is used for the reaction zone interaction. Most reactive events are found to occur in strong single-impact collisions on a subpicosecond scale via the Eley-Rideal mechanism. The extent of reaction is large and a major fraction of the available energy goes into the vibrational excitation of H2, exhibiting a vibrational population inversion. Dissipation of reaction energy to the heat bath can be adequately described using a seven-atom chain with the chain end bound to the rest of solid. The extent of reaction is not sensitive to the variation of surface temperature in the range of Ts=0-300 K in the fixed gas temperature, but it shows a minimum near 1000 K over the Tg=300-2500 K.

Synthesis of Silicon Tracelsss Linker for Solid-Phase Reaction

  • Mun Han-Seo;Seong Jin-Hyun
    • Archives of Pharmacal Research
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    • v.27 no.4
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    • pp.371-375
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    • 2004
  • The silicon linker is the foremost traceless linker used in solid-phase reactions. Hydrogen fluo-ride (HF) or trifluoroacetic aicd (TFA) can remove the silicon linker with the silicon atom being replaced by a hydrogen atom. In this experiment, the linkers 1c and 2d, which are the most useful in solid-phase reactions, were synthesized, Linker 1c is composed of seven linearly linked carbons and linker 2d includes an oxygen atom in the linear carbon chain to increase the solvation capacity. The carboxylic acid component of linker 1c and 2d forms an amide or ester bond with resin. The synthesized linkers 1c and 2d could be utilized in constructing a chemical compound library that includes indole, benzodiazepine and phenothiazine (aromatic ring compounds).

Dynamics of Gas-phase Hydrogen Atom Reaction with Chemisorbed Hydrogen Atoms on a Silicon Surface

  • 임선희;이종백;김유항
    • Bulletin of the Korean Chemical Society
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    • v.20 no.10
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    • pp.1136-1144
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    • 1999
  • The collision-induced reaction of gas-phase atomic hydrogen with hydrogen atoms chemisorbed on a silicon (001)-(2×1) surface is studied by use of the classical trajectory approach. The model is based on reaction zone atoms interacting with a finite number of primary system silicon atoms, which then are coupled to the heat bath, i.e., the bulk solid phase. The potential energy of the Hads‥Hgas interaction is the primary driver of the reaction, and in all reactive collisions, there is an efficient flow of energy from this interaction to the Hads-Si bond. All reactive events occur on a subpicosecond scale, following the Eley-Rideal mechanism. These events occur in a localized region around the adatom site on the surface. The reaction probability shows the maximum near 700K as the gas temperature increases, but it is nearly independent of the surface temperature up to 700 K. Over the surface temperature range of 0-700 K and gas temperature range of 300 to 2500 K, the reaction probability lies at about 0.1. The reaction energy available for the product states is small, and most of this energy is carried away by the desorbing H2 in its translational and vibrational motions. The Langevin equation is used to consider energy exchange between the reaction zone and the bulk solid phase.

Synthesis of Mullite Whiskers by Vapor-Solid Reaction in the System of Al(OH)3-SiO2-AlF3 (Al(OH)3-SiO2-AlF3계에서 기상-고상반응에 의한 뮬라이트 휘스커 합성)

  • Lee, Hong-Lim;Kang, Jong-Bong
    • Journal of the Korean Ceramic Society
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    • v.43 no.6 s.289
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    • pp.376-382
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    • 2006
  • In the $Al(OH)_3-SiO_2-AlF_3$ system, leaf-shaped fluorotopaz was first formed at $800^{\circ}C$ and mullite whisker was formed at $1,100^{\circ}C$. The mass transportation of Al and Si as gas phase, the fast reaction and growth, and the absence of liquid phase existence in mullite whisker showed that the formation and growth of mullite was from the solid-vapor reaction.