• Title/Summary/Keyword: high-temperature spinning

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Thermal and Rheological Characterizations of Polycarbosilane Precursor by Solvent Treatment (폴리카보실란 전구체의 용매 처리에 따른 열적 및 유변학적 특성 분석)

  • Song, Yeeun;Joo, Young Jun;Shin, Dong Geun;Cho, Kwang Youn;Lee, Doojin
    • Composites Research
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    • v.35 no.1
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    • pp.23-30
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    • 2022
  • Polycarbosilane(PCS) is an important precursor for melt-spinning the silicon carbide(SiC) fibers and manufacturing ceramics. The PCS is a metal-organic polymer precursor capable of producing continuous SiC fibers having excellent performance such as high-temperature resistance and oxidation resistance. The SiC fibers are manufactured through melt-spinning, stabilization, and heat treatment processes using the PCS manufactured by synthesis, purification, and control of the molecular structure. In this paper, we analyzed the effect of purification of unreacted substances and low molecular weight through solvent treatment of PCS and the effect of heat treatment at various temperatures change the polymerization and network rearrangement of PCS. Especially, we investigated the complex viscosity and structural arrangement of PCS precursors according to solvent treatment and heat treatment through the rheological properties.

The Effect of the Te on the Microstructure of Rapidly Solidification Ag-Sn-In Contact Material (급속응고한 Ag-Sn-In계 접점재료의 미세조직에 미치는 Te 의 영향)

  • Chang, Dae-Jung;Kwon, Gi-Bong;Kim, Young-Ju;Cho, Dae-Hyoung;Nam, Tae-Woon
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.20 no.1
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    • pp.86-91
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    • 2007
  • Contact material is widely used as electrical parts. Ag-CdO has a good wear resistance and stable contact resistance. But the disadvantages of Ag-Cd alloy are coarse Cd oxides and harmful metal, Cd. Then Ag-Sn alloy that has stable and fine Sn oxide at high temperature has been developed. In order to investigate the effect of Te additional that affects the formation of the oxide layer on the surface and the formation of oxide in matrix Ag, we studied the microstructures and properties of Ag-Sn-In(-Te) material fabricated by rapid solidification process. The experimental procedure were melting using high frequency induction, melt spinning, and internal oxidation. Specimens were examined and analyzed by Transmission electron microscopy(TEM), energy dispersive X-ray spectroscopy(EDS) and Vickers hardness. As a result, internal oxidation was completed even at $600^{\circ}C$. Te forms coarse $In_{2}TeO_{6}$ phase and makes fine and well dispersed $SnO_{2}$ Phase. 0.3 wt% Te shows favorable properties.

The Effect of Misch Metal on the Microstructure of Rapidly solidified Ag-Sn-In Alloys (급속응고한 Ag-Sn-In 합금의 미세조직에 미치는 Misch Metal의 영향)

  • Chang, Dae-Jung;Nam, Tae-Woon
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.20 no.6
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    • pp.561-565
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    • 2007
  • Because of a good wear resistance and a stable contact resistance, Ag-CdO is widely used as electrical contact material. But, the Cd-oxide mainly exists as a coarse particle and adversely affected to environment. As a reason, $Ag-SnO_2$ alloy has been developed. The Sn-oxide maintains stable and fine particle even at high temperature. In order to investigate the effect of Misch metal (Mm) additional that affects the formation of the oxide and the formation of fine matrix Ag, we studied the microstructures and properties of Ag-Sn-In(-Mm) material fabricated by rapid solidification process. The experimental procedure were melting using high frequency induction, melt spinning, and internal oxidation. The Mm addition makes Ag matrix more fine than no Mm addition. The reason is that the addition of Misch metal decreased a latent heat of fusion of alloy, as a result the rapid solidification effect of alloy is increased. The maximum hardness shows at 0.3 wt%Mm. after that the hardness is decreased until 0.4 wt% Mm, but still larger than no Mm addition alloy. At 0.5 wt% Mm alloy, the precipitation of Misch metal causes a decrease of hardness than no Mm addition alloy.

7Li MAS NMR studies of Li4P2O7 and LiFePO4 materials (LiFePO4와 Li4P2O77Li MAS NMR 특성 연구)

  • Han, Doug-Young;Park, Nam-Sin;Lee, Sang-Hyuk;Lee, Hak-Man;Kim, Chang-Sam
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.21 no.1
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    • pp.15-20
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    • 2011
  • [ $^7Li$ ]Magic Angle Spinning (MAS) NMR spectroscopy has been used to study the lithium local environments in $Li_4P_2O_7$ and$LiFePO_4$ materials. The purpose of this study was to know the structure of the solid electrolyte interphase (SEI) in lithium ion cells composed of $LiFePO_4$ as cathode material. $Li_4P_2O_7$ and $LiFePO_4$ were prepared by a solid-state reaction. The $^7Li$ MAS NMR experiments were carried out at variable temperatures in order to observe the local structure changes at the temperatures in $Li_4P_2O_7$ system. The $^7Li$ MAS NMR spectra of in $Li_4P_2O_7$ indicate that the lithium local environments in $Li_4P_2O_7$ were not changed in the temperature range between $27^{\circ}C$ and $97^{\circ}C$ Through this work, we confirmed that the small amount of $Li_4P_2O_7$ less than 5.0 wt% in $LiFePO_4$ could be clearly measured by the $^7Li$ MAS NMR spectroscopy at high spinning rate over than 11 kHz.

The Effects of Post-Treatments for Wet Spun PVDF on the Piezoelectric Property (습식방사 된 PVDF 섬유의 후 처리를 통한 결정구조의 변화)

  • Yu, Seung Mi;Oh, Hyun Ju;Hwang, Sang-Kyun;Chung, Yong Sik;Hwang, Hui Yun;Kim, Seong Su
    • Composites Research
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    • v.26 no.2
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    • pp.123-128
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    • 2013
  • The PVDF (polyvinylidene fluoride) fibers were prepared using the wet spinning processing. To improve ${\beta}$-phase crystalline which closely related piezoelectric property PVDF wet spun fibers conducted post treatment. Post treatment is consisted of heat stretching and annealing process. The heat stretching and annealing conditions were controlled by changing temperature between glass transition temperature and melting temperature. From these experimental data, the resulting crystal structure of the ${\beta}$-phase crystalline was confirmed by FT-IR and XRD experiments. From these analysis results, optimum stretching and annealing conditions of the wet spun PVDF fibers were founded to increase high ${\beta}$-phase crystalline. Furthermore results showed that thermal processing had a direct effect on modifying the crystalline microstructure and also confirmed that heat stretching and annealing could increase the degree of crystallinity and ${\beta}$-phase crystalline. Finally, piezoelectric constant ($d_{11}$) of the post heat treated PVDF fibers reinforced composite were measured to investigate the feasibility for the sensing materials.

Hydrogen Permeation Properties of $(Ni_{60}-Nb_{40})_{95}-Pd_5$ Amorphous Metallic Membrane ($(Ni_{60}-Nb_{40})_{95}-Pd_5$ 비정질 금속막의 수소투과 특성)

  • Lee, Dock-Young;Kim, Yoon-Bae
    • Transactions of the Korean hydrogen and new energy society
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    • v.19 no.4
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    • pp.359-366
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    • 2008
  • Hydrogen as a high-quality and clean energy carrier has attracted renewed and ever-increasing attention around the world in recent years, mainly due to developments in fuel cells and environmental pressures including climate change issues. In this processes for hydrogen production from fossil fuels, separation and purification is a critical technology. $(Ni_{60}-Nb_{40})_{95}-Pd_5$ alloy ingots were prepared by arc-melting the mixture of pure metals in an Ar atmosphere. Melt-spun ribbons were produced by the single-roller melt-spinning technique in an Ar atmosphere. Amorphous structure and thermal behavior were characterized by XRD and DSC. The permeability of the $(Ni_{60}-Nb_{40})_{95}-Pd_5$ amorphous alloy membrane was characterized by hydrogen permeation experiments in the temperature range 623 to 773 K and pressure of 2 bars. The maximum hydrogen permeability was $3.54{\times}10^{-9}[mol{\cdot}m^{-1}s^{-1}{\cdot}pa^{-1/2}]$ at 773 K for the $(Ni_{60}-Nb_{40})_{95}-Pd_5$ amorphous alloy.

Effects of the Substitution of Mischmetal for PrNd on the Microstructures and Magnetic Properties of Rapidly Quenched (MM)PrNd-Fe-B Nanocrystalline Magnets

  • Zhao, Zeng-ru;Wang, Xin;Zhang, Xue-feng;Ma, Qiang;Liu, Yan-li;Li, Yong-feng;Liu, Fei;Wang, Gao-feng
    • Journal of Magnetics
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    • v.22 no.1
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    • pp.60-64
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    • 2017
  • Mischmetal of Bayan Obo ore was utilized to prepare the high performance $(Pr_{7.34}Nd_{21.86})_{1-x}MM_xFe_{68.7}Al_{0.1}Cu_{0.12}Co_{0.88}B$ ribbons using melt-spinning method. Phase composition and magnetic properties were investigated at room temperature. The ribbons mainly consist of $R_2Fe_{14}B$ phase in isotropic nanostructure. Both coercivity and maximum energy product decrease with the increase of MM content. The magnetic parameters of the ribbons with MM = 20 % in mass are $B_r=7.38kGs$, $H_{cj}=13.66kOe$, $(BH)_{max}=11.81MGOe$. Henkel plots were applied to demonstrate the exchange coupling interaction between grains.

Preparation of Asymmetric Folyethersulfone Hollow Fiber Membranes for Flue Gas Separation (온실기체 분리용 폴리이서설폰 비대칭 중공사 막의 제조)

  • Kim Jeong-Hoon;Sohn Woo-Ik;Choi Seung-Hak;Lee Soo-Bok
    • Membrane Journal
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    • v.15 no.2
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    • pp.147-156
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    • 2005
  • It is well-known that polyethersulfone (PES) has high $CO_2$ selectivity over $N_2\;(or\;CH_4)$ and excellent pressure resistance of $CO_2$ plasticization among muy commercialized engineering plastics[1-4]. Asymmetric PES hollow fiber membranes for flue gas separation were developed by dry-wet spinning technique. The dope solution consists of PES, NMP and acetone. Water and water/NMP mixtures are used in outer and inner coagulants, respectively. Gas permeation rate (i.e., permeance) and $CO_2/N_2$ selectivity were measured with pure gas, respectively and the micro-structure of hollow fiber membranes was characterized by scanning electron microscopy. The effects of polymer concentration, ratio of NMP to acetone, length of air gap, evaporation condition and silicone coating were investigated on the $CO_2/N_2$ separation properties of the hollow fibers. Optimized PES hollow fiber membranes exhibited high permeance of $25\~50$ GPU and $CO_2/N_2$ selectivity of $30\~40$ at room temperature and have the apparent skin layer thickness of about $0.1\;{\mu}m$. The developed PES hollow fiber membranes, would be a good candidate suitable for the flue gas separation process.

Preparatoin of Precursor Pitch for Carbon Applications from Naphtha Cracking Residues (납사분해공정 잔사유로부터 탄소재료용 전구체 핏치의 제조)

  • Kim, Myung-Soe;Kim, Sang-Yeol;Hwang, Jong-Sic
    • Journal of the Korean Applied Science and Technology
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    • v.14 no.1
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    • pp.77-87
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    • 1997
  • PFO(pyrolized fuel oil) and $C_{10}^{+}$ oil, which are the residual heavy oils form a NCC(naphtha cracking center), were heat-treated to produce the precursor-pitch for carbon materials. After PFO was initially distilled near $300^{\circ}C$ to separate the volatile matters recovering as high-quality fuel oil, the residuum of nonvolatile precursor-pitch was then thermally pyrolized in the temperature ranges from $350^{\circ}C$ to $450^{\circ}C$. Spinnable isotropic pitch with the softening point of $200^{\circ}C$ and the toluene insolubles of 36wt% was obtained at $365^{\circ}C$, and then was successfully spun through a spinneret(0.5mm diameter). After spinning, an isotropic carbon fiber of $25{\mu}m$ diameter was obtained via oxidation and craboniation procedures. Mesophase spherules began to be observed from the product pitch pyrolized at $400^{\circ}C$, and bulk mesophase with a flow texture was observed above $420^{\circ}C$. In the case of $C_{10}^{+}$ was the feed was polymerized in the presence $H_2SO_4$ at room temperature to increase the molecular weight and then heat-treated gradually up to $200{\sim}250^{\circ}C$. The products obtained with the softening point of $80{\sim}190^{\circ}C$ were carbonized at 500 and $1000^{\circ}C$ to examine the morphology.

Thermal Stability, Mechanical Properties and Magnetic Properties of Fe-based Amorphous Ribbons with the Addition of Mo and Nb

  • Han, Bo-Kyeong;Jo, Hye-In;Lee, Jin Kyu;Kim, Ki Buem;Yim, Haein
    • Journal of Magnetics
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    • v.18 no.4
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    • pp.395-399
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    • 2013
  • The metallic glass ribbons of $[(Fe_xCo_{1-x})_{0.75}B_{0.2}Si_{0.05}]_{96}Mo_4$ (x = 0, 0.3, 0.6, 0.9 at.%) and $[(Fe_xCo_{1-x})_{0.75}B_{0.2}Si_{0.05}]_{96}Nb_4$ (x = 0, 0.3, 0.6, 0.9 at.%) were obtained by melt spinning with 25-30 ${\mu}m$ thickness. The thermal stability, mechanical properties and magnetic properties of Fe-Co-B-Si based systems were investigated. The values of thermal stability were measured using differential scanning calorimetry (DSC), including glass transition temperature ($T_g$), crystallization temperature ($T_x$) and supercooled liquid region (${\Delta}T_x=T_x-T_g$). These amorphous ribbons were identified as fully amorphous, using X-ray diffraction (XRD). The mechanical properties of Febased samples were measured by nano-indentation. Magnetic properties of the amorphous ribbons were measured by a vibrating sample magnetometer (VSM). The amorphous ribbons of $[(Fe_xCo_{1-x})_{0.75}B_{0.2}Si_{0.05}]_{96}Mo_4$ (x = 0, 0.3, 0.6, 0.9 at.%) and $[(Fe_xCo_{1-x})_{0.75}B_{0.2}Si_{0.05}]_{96}Nb_4$ (x = 0, 0.3, 0.6, 0.9 at.%) exhibited soft magnetic properties with low coercive force ($H_c$) and high saturation magnetization (Ms).