• Title/Summary/Keyword: In Situ Composite

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Structural Behavior of Mixed $LiMn_2O_4-LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ Cathode in Li-ion Cells during Electrochemical Cycling

  • Yun, Won-Seop;Lee, Sang-U
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.05a
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    • pp.5-5
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    • 2011
  • The research and development of hybrid electric vehicle (HEV), plug-in hybrid electric vehicle (PHEV) and electric vehicle (EV) are intensified due to the energy crisis and environmental concerns. In order to meet the challenging requirements of powering HEV, PHEV and EV, the current lithium battery technology needs to be significantly improved in terms of the cost, safety, power and energy density, as well as the calendar and cycle life. One new technology being developed is the utilization of composite cathode by mixing two different types of insertion compounds [e.g., spinel $LiMn_2O_4$ and layered $LiMO_2$ (M=Ni, Co, and Mn)]. Recently, some studies on mixing two different types of cathode materials to make a composite cathode have been reported, which were aimed at reducing cost and improving self-discharge. Numata et al. reported that when stored in a sealed can together with electrolyte at $80^{\circ}C$ for 10 days, the concentrations of both HF and $Mn^{2+}$ were lower in the can containing $LiMn_2O_4$ blended with $LiNi_{0.8}Co_{0.2}O_2$ than that containing $LiMn_2O_4$ only. That reports clearly showed that this blending technique can prevent the decline in capacity caused by cycling or storage at elevated temperatures. However, not much work has been reported on the charge-discharge characteristics and related structural phase transitions for these composite cathodes. In this presentation, we will report our in situ x-ray diffraction studies on this mixed composite cathode material during charge-discharge cycling. The mixed cathodes were incorporated into in situ XRD cells with a Li foil anode, a Celgard separator, and a 1M $LiPF_6$ electrolyte in a 1 : 1 EC : DMC solvent (LP 30 from EM Industries, Inc.). For in situ XRD cell, Mylar windows were used as has been described in detail elsewhere. All of these in situ XRD spectra were collected on beam line X18A at National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory using two different detectors. One is a conventional scintillation detector with data collection at 0.02 degree in two theta angle for each step. The other is a wide angle position sensitive detector (PSD). The wavelengths used were 1.1950 ${\AA}$ for the scintillation detector and 0.9999 A for the PSD. The newly installed PSD at beam line X18A of NSLS can collect XRD patterns as short as a few minutes covering $90^{\circ}$ of two theta angles simultaneously with good signal to noise ratio. It significantly reduced the data collection time for each scan, giving us a great advantage in studying the phase transition in real time. The two theta angles of all the XRD spectra presented in this paper have been recalculated and converted to corresponding angles for ${\lambda}=1.54\;{\AA}$, which is the wavelength of conventional x-ray tube source with Cu-$k{\alpha}$ radiation, for easy comparison with data in other literatures. The structural changes of the composite cathode made by mixing spinel $LiMn_2O_4$ and layered $Li-Ni_{1/3}Co_{1/3}Mn_{1/3}O_2$ in 1 : 1 wt% in both Li-half and Li-ion cells during charge/discharge are studied by in situ XRD. During the first charge up to ~5.2 V vs. $Li/Li^+$, the in situ XRD spectra for the composite cathode in the Li-half cell track the structural changes of each component. At the early stage of charge, the lithium extraction takes place in the $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ component only. When the cell voltage reaches at ~4.0 V vs. $Li/Li^+$, lithium extraction from the spinel $LiMn_2O_4$ component starts and becomes the major contributor for the cell capacity due to the higher rate capability of $LiMn_2O_4$. When the voltage passed 4.3 V, the major structural changes are from the $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ component, while the $LiMn_2O_4$ component is almost unchanged. In the Li-ion cell using a MCMB anode and a composite cathode cycled between 2.5 V and 4.2 V, the structural changes are dominated by the spinel $LiMn_2O_4$ component, with much less changes in the layered $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ component, comparing with the Li-half cell results. These results give us valuable information about the structural changes relating to the contributions of each individual component to the cell capacity at certain charge/discharge state, which are helpful in designing and optimizing the composite cathode using spinel- and layered-type materials for Li-ion battery research. More detailed discussion will be presented at the meeting.

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Platinum Nano-Dispersion via In Situ Processing - Preparation and catalytic Property of Porous $CaZrO_3/MgO/Pt$ Nanocomposite

  • Yoshikazu;Hwang, Hae-Jin;Naoki Kondo;Tatsuki Ohji
    • Journal of Powder Materials
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    • v.8 no.3
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    • pp.163-167
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    • 2001
  • A bulk porous $CaZrO_3/MgO$ composite with plantinum nano-dispersion was synthesized in air atmosphere through the combination of several in situ reactions, including the pyrolysis of $PtO_2$. A mixture of $CaMg(CO_3)_2$(dolomite), $ZrO_2$, $PtO_2$ and LiF (0.5 wt%, as an additive) was cold isostatically pressed at 200 MPa and sintered at $1100^{\circ}C$ for 2 h. The porous $CaZrO_3/MgO/Pt$ composite ($CaZrO_3/MgO$ : Pt=99 : 1 in volume) had a uniformly open-porous structure (porosity: 56%) with three-dimensional (3-D) network and a narrow pore-size distribution, similarly to the porous $CaZrO_3/MgO$ composites reported before. Catalytic Properties (viz., NO direct decomposition and NO reduction by $C_2H_4$) of the $CaZrO_3/MgO/Pt$ composite were investigated up to $900^{\circ}C$. In the absence of oxygen, the NO conversion rate reached ~52% for the direct decomposition and ~100% for the reduction by $C_2H_4$, respectively. The results suggest the possibility of the porous composite as a multifunctional filter, i.e., simultaneous hot gas-filtering and $de-NO_x$ in one component.

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Preparation and Physical Properties of Conductive Poly(acrylonitrile) Fabrics Containing Polypyrrole (폴리피롤을 이용한 전도성 아크릴 직물의 제조 및 물성)

  • 이영관;조재춘
    • Polymer(Korea)
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    • v.24 no.2
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    • pp.276-280
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    • 2000
  • A conductive poly(acrylonitrile)/polypyrrole composite fabric was prepared. A conductive composite was prepared by the impregnation of PAN fabric into a mixed solution of pyrrole and oxidant in order to induce the in-situ polymerization of a conducting polymer into the matrix fabric. In the composite formation, the reaction condition was optimized to achieve the best properties, and the effect of the externally-added arylsulfonate dopants on the physical properties was examined. As a result, the best properties of electrical conductivity, thermal stability, and fastness to washing, was observed in the composite containing an antraquinonesulfonate (AQSA) dopant.

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Improved Electrical Conductivity of a Carbon Nanotube Mat Composite Prepared by In-Situ Polymerization and Compression Molding with Compression Pressure

  • Noh, Ye Ji;Kim, Han Sang;Kim, Seong Yun
    • Carbon letters
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    • v.13 no.4
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    • pp.243-247
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    • 2012
  • A fabrication method to improve the processability of thermoplastic carbon nanotube (CNT) mat composites was investigated by using in-situ polymerizable and low viscous cyclic butylene terephthalate oligomers. The electrical conductivity of the CNT mat composites strongly depended on the compression pressure, and the trend can be explained in terms of two cases, low and high compression pressure, respectively. High CNT mat content in the CNT mat composites and the surface of the CNT mat composites with fully contacted CNTs was achieved under high compression pressure, and direct contact between four probes and the surface of the CNT mat composites with fully contacted CNTs gave resistance of $2.1{\Omega}$. In this study the maximum electrical conductivity of the CNT mat composites, obtained under a maximum applied compression pressure of 27 MPa, was 11 904 S $m^{-1}$, where the weight fraction of the CNT mat was 36.5%.

Maximizing TPBs through Ni-self-exsolution on GDC based composite anode in solid oxide fuel cells

  • Tan, Je-Wan;Lee, Dae-Hui;Kim, Bo-Gyeong;Kim, Ju-Seon;Mun, Ju-Ho
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.402.1-402.1
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    • 2016
  • The performance of solid oxide fuel cells (SOFCs) is directly related to the electrocatalytic activity of composite electrodes in which triple phase boundaries (TPBs) of metallic catalyst, oxygen ion conducting support, and gas should be three-dimensionally maximized. The distribution morphology of catalytic nanoparticle dispersed on external surfaces is of key importance for maximized TPBs. Herein in situ grown nickel nanoparticle onto the surface of fluorite oxide is demonstrated employing gadolium-nickel co-doped ceria ($Gd0.2-xNixCe0.8O2-{\delta}$, GNDC) by reductive annealing. GNDC powders were synthesized via a Pechini-type sol-gel process while maximum doping ratio of Ni into the cerium oxide was defined by X-ray diffraction. Subsequently, NiO-GNDC composite were screen printed on the both sides of yttrium-stabilized zirconia (YSZ) pellet to fabricate the symmetrical half cells. Electrochemical impedance spectroscopy (EIS) showed that the polarization resistance was decreased when it was compared to conventional Ni-GDC anode and this effect became greater at lower temperature. Ex situ microstructural analysis using scanning electron microscopy after the reductive annealing exhibited the exsolution of Ni nanoparticles on the fluorite phases. The influence of Ni contents in GNDC on polarization characteristics of anodes were examined by EIS under H2/H2O atmosphere. Finally, the addition of optimized GNDC into the anode functional layer (AFL) dramatically enhanced cell performance of anode-supported coin cells.

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Microstructural and Mechanical Characteristics of In Situ Synthesized Chromium-Nickel-Graphite Composites

  • Pirso, Juri;Viljus, Mart;Letunovits, Sergei;Juhani, Kristjan
    • Proceedings of the Korean Powder Metallurgy Institute Conference
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    • 2006.09a
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    • pp.631-632
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    • 2006
  • Cr-C-Ni composites were synthesized in situ from elemental powders of Cr, Ni and C by high energy milling followed by reactive sintering. The milled powders with the grain size in nano-scale were pressed to compacts and sintered. During the following thermal treatment at first the chromium carbide was formed and then the $Cr_3C_2-Ni$ cermets were sintered in one cycle. The interface between the binder phase and the carbide grains of the in situ composite has a good bonding strength as it is not contaminated with oxidation films or other detrimental surface reactions.

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Study on GO Dispersion of PC/GO Composites according to In-situ Polymerization Method (In-situ 중합방법에 따른 폴리카보네이트(PC)/그래핀 옥사이드(GO) 복합체의 GO 분산성 연구)

  • Lee, Bom Yi;Park, Ju Young;Kim, Youn Cheol
    • Applied Chemistry for Engineering
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    • v.26 no.3
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    • pp.336-340
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    • 2015
  • Three different types of polycarbonate (PC)/graphene oxide (GO) composites using diphenyl carbonate as a monomer were fabricated by melt polymerization. Those were the PC/GO composite (PC/GO) using a twin extruder, in-situ PC/GO composite (PC/GO-cat.) using a catalyst, and in-situ PC/GO composite (PC/GO-COCl) using a GO-COCl treated by -COCl, Chemical structures of the composites were confirmed by C-H and C=O stretching peak at $3000cm^{-1}$ and $1750cm^{-1}$, respectively. The slope for the storage (G') versus loss (G") modulus plot decreased with an increase in the heterogeneous property of polymer melts. So we can check the GO dispersion of the PC/GO composites using by the slop for G'-G" plot. According to the G'- G" slopes for three different types of PC/GO composites, GO was well dispersed within PC matrix in case of PC/GO and PC/GO-cat.. It was also confirmed by atomic force microscope (AFM) photos. One of the reasons for the poor GO dispersion of PC/GO-COCl is branching and crosslinking processes occurred during polymerization, which was further confirmed by a plot for the complex modulus versus phase difference.

Effect of ${\gamma}$-Ray Irradiation on Surface Oxidation of Ultra High Molecular Weight Polyethylene/Zirconia Composite Prepared by in situ Ziegler-Natta Polymerization

  • Kwak, Soon-Jong;Noh, Dong-Il;Chun, Heung-Jae;Lim, Youn-Mook;Nho, Young-Chang;Jang, Ju-Woong;Shim, Young-Bock
    • Macromolecular Research
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    • v.17 no.8
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    • pp.603-608
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    • 2009
  • Novel ultra-high molecular weight polyethylene (UHMWPE)/zirconia composites were previously prepared by the in situ polymerization of ethylene using a Ti-based Ziegler-Natta catalyst supported on to the surface of zirconia, as a bearing material for artificial joints. Tribological tests revealed that a uniform dispersion of zirconia in UHMWPE markedly increased the wear resistance. The effects of zirconia content on the oxidation behavior of the ${\gamma}$-ray-treated UHMWPE/zirconia composite surfaces were examined. The oxidation index that estimates the oxidation degree as the content of total carbonyl compounds was monitored using Fourier transform infrared spectroscopy-attenuated total reflectance. The changes in the surface composition due to the oxidation were confirmed by electron spectroscopy for chemical analysis. The extent of oxidation decreased with increasing zirconia content, which was attributed to the increased crystallinity as well as the decreased polymer portion of the UHMWPE/zirconia composites.

Manufacturing Fiber-Reinforced Composite Materials Based on PLA (Poly L-Lactide) Resin Using In-Situ Polymerization and Molecular Weight Measurement Using GPC (현장 중합을 이용한 PLA(Poly L-Lactide) 수지 기반 섬유 강화 복합 재료 제조 및 GPC를 이용한 분자량 측정)

  • Seon-Ju Kim;Beom-Joo Lee;Hyeong-Min Yoo
    • Design & Manufacturing
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    • v.17 no.3
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    • pp.28-33
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    • 2023
  • The conventional FRP (Fiber Reinforced Plastic) manufacturing process used thermoset resins for ease of molding but faced the issue of non-recyclability. To address these shortcomings, a new process utilizing thermal plastic resin was developed. However, due to the high viscosity of thermal plastic resin, problems such as fiber deformation and a reduced fiber volume fraction occurred during the high-temperature, high-pressure process. In this study, to overcome the limitations of the conventional process, fiber-reinforced composite materials were manufactured through in-situ polymerization using PLA (Poly L-Lactide) resin in the VA-RTM (Vacuum Assistance Resin Transfer Molding) process. The fiber volume of the produced specimens was calculated, and resin impregnation and porosity were confirmed through optical microscopy. Additionally, molecular weight analysis using GPC (Gel Permission Chromatography) demonstrated improvements over the conventional process and emphasized the essential requirement of temperature control.

A Study on the Shear Strength Characteristics of Composited Ground applying RAP Method by Large Direct Shear Test (대형직접전단시험에 의한 RAP 복합지반의 전단강도 특성 연구)

  • Chun, Byung-Sik;Seo, Deok-Dong;Kim, Jong-San
    • Proceedings of the Korean Geotechical Society Conference
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    • 2004.03b
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    • pp.82-89
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    • 2004
  • To secure stability and availability of Rammed Aggregate Pier method as the foundation of a structure, the shear strength characteristics according to the area replacement ratio of RAP and the relative density of in-situ ground was studied through soil laboratory tests and large direct shear tests in a model ground. As a result, the internal friction angle tends to increase in proportion to in-situ relative density(Very Loose, Loose, Medium) in composite ground formed by the same area replacement ratio of RAP and also increase in proportion to increasing the area replacement ratio(30, 40, 50%) of RAP in the same ground condition. Furthermore, the comparative analysis between the experimental value and theoretical value of the shear strength is carried out.

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