• Title/Summary/Keyword: high pressure synthesis

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AlN preparation by Self-propagation High-temperature Synthesis (SHS) in Al-N2 and Al-N2-AIN system (Al-N2와 Al-N2-AlN계에서 고온자전연소법에 의한 AlN 합성)

  • 이재령;이익규;안종관;김동진;안양규;정헌생
    • Journal of Powder Materials
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    • v.11 no.4
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    • pp.294-300
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    • 2004
  • This study for preparation of aluminum nitride (AlN) with high purity was carried out by self-propagating high-temperature synthesis method in two different systems, $Al-N_{2}$ and $Al-N_{2}$-AlN, with the change of nitrogen gas pressure and dilution factor. On the occasion of $Al-N_{2}$ system, unreacted aluminum was detected in the product in spite of high nitrogen pressure, 10 MPa, This may be caused by obstructing nitrogen gas flow to inner part of molten and agglomerate of aluminum, formed in pre-heating zone. In $Al-N_{2}$-AlN system, AlN with a purity of 95% or ever can be prepared in the condition of $f_{Dil}\geq0.5$, $P_{N_{2}}\geq$ 1 MPa, and the purity can be elevated to 98% over in the condition of $f_{Dil}$ = 0.7 and $P_{N_{2}}$ = 10 MPa.

Synthesis of TiO2 Nanowires by Thermal Oxidation of Titanium Alloy Powder (타이타늄 합금 분말의 열적산화를 통한 TiO2 나노와이어의 합성)

  • Kim, Yoo-Young;Cho, Kwon-Koo
    • Journal of Powder Materials
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    • v.25 no.1
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    • pp.48-53
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    • 2018
  • One-dimensional rutile $TiO_2$ is an important inorganic compound with applicability in sensors, solar cells, and Li-based batteries. However, conventional synthesis methods for $TiO_2$ nanowires are complicated and entail risks of environmental contamination. In this work, we report the growth of $TiO_2$ nanowires on a Ti alloy powder (Ti-6wt%Al-4wt%V, Ti64) using simple thermal oxidation under a limited supply of $O_2$. The optimum condition for $TiO_2$ nanowire synthesis is studied for variables including temperature, time, and pressure. $TiO_2$ nanowires of ${\sim}5{\mu}m$ in length and 100 nm in thickness are richly synthesized under the optimum condition with single-crystalline rutile phases. The formation of $TiO_2$ nanowires is greatly influenced by synthesis temperature and pressure. The synthesized $TiO_2$ nanowires are characterized using field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), and high-resolution transmission electron microscopy (HR-TEM).

A Study on Synthesis and Characterization of $Ti_xZr_{1-x}C$ Solid-Solution by Self-propagation High Temperature Synthesis Method (SHS법에 의한 $Ti_xZr_{1-x}C$ 고용체의 합성 및 특성 연구)

  • 이형복;오유근;이성민
    • Journal of the Korean Ceramic Society
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    • v.34 no.7
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    • pp.731-737
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    • 1997
  • TixZr1-xC(0$0^{\circ}C$, 5.1 mm/sec respectively. The relative density, three point flexural strength, and the hardness of composites, which was sintered at 190$0^{\circ}C$ for 60 min by using hot-pressing under a pressure of 30 MPa, were 99%, 525 MPa and 24 GPa respectively.

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Simultaneous Synthesis and Sintering of Titanium Carbide by HPCS(High Pressure-Self Combustion Sintering) (고압연소 소결(HPCS)법에 의한 탄화티타늄(TiC)의 합성 및 소결)

  • 김지헌;최상욱;조원승;조동수;오장환
    • Journal of the Korean Ceramic Society
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    • v.34 no.5
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    • pp.473-482
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    • 1997
  • Titanium carbide(TiC) has a poor sinterability due to the strong covalent bond. Thus, it is generally fabricated by either hot pressing or pressureless-sintering at elevated temperature by the addition of sintering aids such as nickel(Ni), molybdenum(Mo) and cobalt(Co). However, these sintering methods have the following disadvantages; (1) the complicated process, (2) the high energy consumption, and (3) the possibility of leaving inevitable impurities in the product, etc. In order to reduce above disadvantages, we investigated the optimum conditions under which dense titanium carbide bodies could be synthesized and sintered simultaneously by high pressure self-combustion sintering(HPCS) method. This method makes good use of the explosive high energy from spontaneous exothermic reaction between titanium and carbon. The optimum conditions for the nearly full-densification were as follows; (1) The densification of sintered body becomes high by increasing the pressing pressure from 400kgf/$\textrm{cm}^2$ upto 1200 kgf/$\textrm{cm}^2$. (2) Instead of adding the coarse graphite or activated carbon, the fine particles of carbon black should be added as a carbon source. (3) The optimum molar ratio of carbon to titanium (C/Ti) was unity. In reality, titanium carbide body which were prepared under optimum conditions had relatively dense textures with the apparent porosity of 0.5% and the relative density of 98%.

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Magnetic Properties of Micron Sized Fe3O4 Crystals Synthesized by Hydrothermal Methods (수열합성을 이용하여 제작한 Fe3O4 결정입자의 자기적 특성)

  • Lee, Ki-Bum;Nam, Chunghee
    • Journal of Powder Materials
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    • v.26 no.6
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    • pp.481-486
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    • 2019
  • Iron oxides currently attract considerable attention due to their potential applications in the fields of lithiumion batteries, bio-medical sensors, and hyperthermia therapy materials. Magnetite (Fe3O4) is a particularly interesting research target due to its low cost, good biocompatibility, outstanding stability in physiological conditions. Hydrothermal synthesis is one of several liquid-phase synthesis methods with water or an aqueous solution under high pressure and high temperature. This paper reports the growth of magnetic Fe3O4 particles from iron powder (spherical, <10 ㎛) through an alkaline hydrothermal process under the following conditions: (1) Different KOH molar concentrations and (2) different synthesis time for each KOH molar concentrations. The optimal condition for the synthesis of Fe3O4 using Fe powders is hydrothermal oxidation with 6.25 M KOH for 48 h, resulting in 89.2 emu/g of saturation magnetization at room temperature. The structure and morphologies of the synthesized particles are characterized by X-ray diffraction (XRD, 2θ = 20°-80°) with Cu-kα radiation and field emission scanning electron microscopy (FE-SEM), respectively. The magnetic properties of magnetite samples are investigated using a vibrating sample magnetometer (VSM). The role of KOH in the formation of magnetite octahedron is observed.

High Pressure Effects on 1,3-Dipolar Cycloaddition of Azides with Alkynes (아자이드와 알킨의 1,3-쌍극자 고리첨가반응에서 고압이 반응속도에 미치는 영향에 대한 연구)

  • Kwon, Jinju
    • Journal of the Korea Institute of Military Science and Technology
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    • v.18 no.6
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    • pp.736-742
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    • 2015
  • The effect of pressure on 1,3-dipolar cycloaddtion has been studied by means of FT-IR and NMR spectroscopy. Pressure accelerates 1,3-dipolar cycloaddition without solvent or catalyst. This simple and inexpensive method eliminates the need for work-up or purification. The method is expected to be applied to the synthesis of binders for solid rocket propellants.

SPUTTER-DEPOSITION OF CARBON NITRIDE FILMS WITH HIGH NITROGEN CONCENTRATION

  • Taki, Yusuke;Takai, Osamu
    • Journal of the Korean institute of surface engineering
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    • v.29 no.5
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    • pp.498-504
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    • 1996
  • The synthesis of carbon nitride thin films with high nitrgen concentration was accomplished by reactive supttering at relatively high working pressure. In conventional reactive sputter-deposition of carbon nitride films, working pressure was 0.3-5Pa and the ratio of nitrogen to carbon(N/C ratio) in the films was less than 0.5. In this study, amorphous carbon nitride films with the N/C ratio $\tickapprox$ 1.0 were prepared on Si(100). substrates at higher pressure, 20-60 Pa. Structural analyses with Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy revealed that the films prepared consisted of triazine-like plain network.

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Controlled Growth of Large-area Mono-, Bi-, and Few-layer Graphene by Chemical Vapor Deposition on Copper Substrate

  • Kim, Yooseok;Lee, Su-il;Jung, Dae Sung;Cha, Myoung-Jun;Kim, Ji Sun;Park, Seung-Ho;Park, Chong-Yun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.380.2-380.2
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    • 2014
  • Direct synthesis of graphene using a chemical vapor deposition (CVD) has been considered a facile way to produce large-area and uniform graphene film, which is an accessible method from an application standpoint. Hence, their fundamental understanding is highly required. Unfortunately, the CVD growth mechanism of graphene on Cu remains elusive and controversial. Here, we present the effect of graphene growth parameters on the number of graphene layers were systematically studied and growth mechanism on copper substrate was proposed. Parameters that could affect the thickness of graphene growth include the pressure in the system, gas flow rate, growth pressure, growth temperature, and cooling rate. We hypothesis that the partial pressure of both the carbon sources and hydrogen gas in the growth process, which is set by the total pressure and the mole fraction of the feedstock, could be the factor that controls the thickness of the graphene. The graphene on Cu was grown by the diffusion and precipitation mode not by the surface adsorption mode, because similar results were observed in graphene/Ni system. The carbon-diffused Cu layer was also observed after graphene growth under high CH4 pressure. Our findings may facilitate both the large-area synthesis of well-controlled graphene features and wide range of applications of graphene.

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Effect of Zine Oxide Size and Oxygen Pressure on the Magnetic Properties of (Ni, Zn) Ferrite Powders Prepared by Self-propagating High Temperature Synthesis (ZnO의 입도와 산소압이 고온연소합성법으로 제조된 Ni-Zn Ferrite 분말의 자기적 특성에 미치는 영향)

  • Choi, Yong;Cho, Nam-Ihn;Hahn, Y.D.
    • Journal of the Korean Magnetics Society
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    • v.9 no.2
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    • pp.78-84
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    • 1999
  • $(Ni, Zn)Fe_2O_4$ powders were prepared through self-propagating high temperature synthesis reaction and the effects of initial zinc oxide powder size and oxygen pressure on the magnetic properties of the final combustion products were studied. The ferrite powders were combustion synthesized with iron, iron oxide, nickel oxide, and zinc oxide powders under various oxygen pressures of 0.5~10 atmosphere after blended in n-hexane solution for 5 minutes with a spex mill, followed by dried at 120 $^{\circ}C$ in vacuum for 24 hours. The maximum combustion temperature and propagating rate were about 1250 $^{\circ}C$ and 9.8 mm/sec under the tap density, which were decreased with decreasing ZnO size and oxygen pressure. The final product had porous microstructure with spinel peaks in X-ray spectra. As the ZnO particle size in the reactant powders and oxygen pressure during the combustion reaction increase, coercive force, maximum magnetization, residual magnetization, squareness ratio were changed from 1324 Oe, 43.88 emu/g, 1.27 emu/g, 0.00034 emu/gOe, 37.8$^{\circ}C$ to 11.83 Oe, 68.87 emu/g, 1.23 emu/g, 0.00280 emu/gOe, 43.9 $^{\circ}C$ and 7.99 Oe, 75.84 emu/g, 0.791 emu/g, 0.001937 emu/gOe, 53.8 $^{\circ}C$ respectively. Considering the apparent activation energy changes with oxygen pressure, the combustion reaction significantly depended on initial oxygen pressure and ZnO particle size.

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