• Title/Summary/Keyword: ceramic precursor

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Hydrothermal Synthesis of Li-Mn Spinel Nanoparticle from K-Birnessite and Its Electrochemical Characteristics (K-Birnessite를 이용한 Li-Mn Spinel 나노입자 합성 및 전기화학적 특성 평가)

  • Kim, Jun-Il;Lee, Jae-Won;Park, Sun-Min;Roh, Kwang-Chul;Sun, Yang-Kook
    • Applied Chemistry for Engineering
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    • v.21 no.5
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    • pp.590-592
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    • 2010
  • Li-Mn spinel ($LiMn_2O_4$) is prepared by a hydrothermal process with K-Birnessite ($KMnO_4{\cdot}yH_2O$) as a precursor. The K-Birnessite obtained via a hydrothermal process with potassium permanganate [$KMnO_4$] and urea [$CO(NH_2)_2$] as starting materials are converted to Li-Mn spinel nanoparticles reacting with LiOH. The molar ratio of LiOH/K-Birnessite is adjusted in order to find the effect of the ratio on the structural, morphological and electrochemical performances of the Li-Mn spinel. X-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDS), and thermogravimetry (TG) are used to investigate the crystal structure and morphology of the samples. Galvanostatic charge and discharge are carried out to measure the capacity and rate capability of the Li-Mn spinel. The capacity shows a maximum value of $117\;mAhg^{-1}$ when the molar ratio of LiOH/K-Birnessite is 0.8 and decreases with the increase of the ratio. However the rate capability is improved with the increase of the ratio due to the reduction of the particle size.

Synthesis and Characteristics of Zirconium Hybridized Polycarbosilane (지르코늄 혼성 폴리카르보실란의 합성 및 특성)

  • Kang, Phil-Hyun;Yang, Hyun-Soo
    • Applied Chemistry for Engineering
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    • v.9 no.6
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    • pp.791-797
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    • 1998
  • As organosilicon based preceramic polymer, new zirconium hybridized polycarbosilane having a good thermal stability and forming stage was synthesized. Oxidative stability(infusibility) and mechanical property of this polymer during the thermal curing process and heat treatment were examined. Prepared zirconium hybridized polycarbisilane (PZC) was spun into fiber at $250{\sim}270^{\circ}C$. Spinnability of PZC polymer having a molecular weight of 1000 to 1400 and having a dispersity<2 was good. The thermal curing process of the PZC fiber was done at 140 to $200^{\circ}C$. The mechanical properties of PZC ceramic fiber depend on curing temperature of PZC as precursor of PZC ceramic fiber. It was found that the optimum curing temperature was variable with the molecular weight of PZC. The cured PZC fiber need constant gel fraction to have good tensile strength.

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Characteristics of Polyimide-silica Hybrid Materials Prepared from Alkoxide Precursor Using Sol-gel Process (졸-겔법을 이용하여 알콕사이드 전구체로부터 합성된 Polyimide-silica 혼성체의 특성)

  • Kim, Byoung-Woo;Lee, Sung-Hwan;Kim, Sung-Wan;Park, Jae-Hyun;Kim, Jun-Ho;Park, Seong-Soo;Park, Hee-Chan
    • Journal of the Korean Ceramic Society
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    • v.39 no.11
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    • pp.1063-1068
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    • 2002
  • Polyimide/silica(PI/silica) hybrid materials having physical or chemical bonds between the PI and silica network were prepared using sol-gel process through hydrolysis and polycondensation of tetraethoxysilane with the polyamic Acid(PAA) or end-capped PAA solution. PAA solution was synthesized by ring opening reaction of pyromellitic dianhydride and oxydianiline monomers in dimethyl acetamide solution. End-capped PAA solution was synthesized by the addition of 3-aminopropyltriethoxysilane in PAA solution. PI/silica hybrid samples were characterized by infrared spectroscopy, differential thermogravimetry, X-ray diffractometry, scanning electron microscopy, and tensile tester. It has been demonstrated that the properties of hybrid samples were affected by the silica content and the bond type between PI and silica.

Synthesis of Aluminum Nitride Powers and Whiskers from a (NH4)[Al(edta)]·2H2O Complex under a Flow of Nitrogen (질소 분위기에서 (NH4)[Al(edta)]·2H2O 착물으로부터 질화알루미늄 분말 및 휘스커의 합성)

  • Jung, Woo-Sik
    • Journal of the Korean Ceramic Society
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    • v.39 no.3
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    • pp.272-277
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    • 2002
  • Aluminum nitride (AlN) powders and whiskers were synthesized by a modified carbothermal reduction and nitridation where a ($NH_4)[Al(ethylenediaminetetraacetate)]{\cdot}2H_2O$ complex is used as precursor. The AlN powders were obtained by calcining the complex without mixing any carbon source under a flow of nitrogen in the temperature range 1200∼1500$^{\circ}$C and then burning out the residual carbon. The nitridation process was investigated by $^{27}Al$ magic-angle spinning (MAS) unclear magnetic resonance, infrared spectroscopy and X-ray diffraction. The complex is pyrolyzed, converted to ${\rho}$- and ${\gamma}$- alumina and then nitridated to AlN without ${\gamma}-{\alpha}$ alumina transition. The morphology of ${\gamma}$-alumina, when it was converted to AlN, was retained, strongly indicating that ${\gamma}$-alumina is converted to AlN through solid-state $AlO_xN_y$, not through gaseous intermediates such as aluminum and aluminaum suboxides. AlN whiskers were obtained, when a (0001) sapphire was used as a catalyst.

Pressureless Infiltration Processing of B4C/Al Composite by Surface Modification (표면 개질에 의한 상압에서의 B4C/Al복합체 제조 방법)

  • 임경란;강덕일;김창삼
    • Journal of the Korean Ceramic Society
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    • v.40 no.2
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    • pp.128-131
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    • 2003
  • Formation of$B_4C/Al$composite by pressureless infiltration was investigated by lowering wetting angle via surface modification of $B_4C$powder with alumina precursor. Surface modification was confirmed by zeta potential analysis. The$B_4C/Al$composite was prepared by placing an Al 6061 disk on the$B_4C$preform and heating at $1030{\circ}C$/20 min under a flowing argon, but no infiltration took place for a bare $B_4C$ preform even at$1250{\circ}C$/30 min. Analysis of XRD and SEM showed the $Al_3BC$phase besides$B_4C$and Al, but no trace of deteriorative$A1_4C_3$.

Preparation and characterization of inexpensive submicron range inorganic microfiltration membranes

  • Nandi, B.K.;Das, B.;Uppaluri, R.;Purkait, M.K.
    • Membrane and Water Treatment
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    • v.1 no.2
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    • pp.121-137
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    • 2010
  • This work presents inexpensive inorganic precursor formulations to yield submicron range symmetric ceramic microfiltration (MF) membranes whose average pore sizes were between 0.1 and $0.4{\mu}m$. Incidentally, the sintering temperature used in this work was about 800 to $950^{\circ}C$ instead of higher sintering temperatures ($1100^{\circ}C$) that are usually deployed for membrane fabrication. Thermogravimetric (TGA) and X-Ray diffraction (XRD) analysis were carried out to evaluate the effect of temperature on various phase transformations during sintering process. The effect of sintering temperature on structural integrity of the membrane as well as pore size distribution and average pore size were evaluated using scanning electron microscopy (SEM) analysis. The average pore sizes of the membranes were increased from 0.185 to $0.332{\mu}m$ with an increase in sintering temperature from 800 to $950^{\circ}C$. However, a subsequent reduction in membrane porosity (from 34.4 to 19.6%) was observed for these membranes. Permeation experiments with both water and air were carried out to evaluate various membrane morphological parameters such as hydraulic pore diameter, hydraulic permeability, air permeance and effective porosity. Later, the membrane prepared with a sintering temperature of $950^{\circ}C$ was tested for the treatment of synthetic oily waste water to verify its real time applicability. The membrane exhibited 98.8% oil rejection efficiency and $5.36{\times}10^{-6}\;m^3/m^2.s$ permeate flux after 60 minutes of experimental run at 68.95 kPa trans-membrane pressure and 250 mg/L oil concentration. Based on retail and bulk prices of the inorganic precursors, the membrane cost was estimated to be $220 /$m^2$ and $1.53 /$m^2$, respectively.

Cathode Materials LaNi1−xCuxO3 for Low Temperature Solid Oxide Fuel Cells

  • Sun, Juncai;Wang, Chengli;Li, Song;Ji, Shijun
    • Journal of the Korean Ceramic Society
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    • v.45 no.12
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    • pp.755-759
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    • 2008
  • New cathode materials $LaNi_{1-x}{Cu_x}{O_3}$ (typically $LaNi_{0.8}Cu_{0.2}O_3$) were synthesized using a co-precipitation method. The structure and morphology of the powders were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The composite material [$Ce_{0.8}Sm_{0.2}O_{2-\ddot{a}}$(SDC) and carbonate (${Na_2}{CO_3},{Li_2}{CO_3}$)], NiO and $LaNi_{1-x}{Cu_x}{O_3}$ were used as the electrolyte, anode and cathode, respectively. The electrochemical performance of La-Ni-Cu-O perovskite oxide at low temperatures ($400{\sim}550^{\circ}C$) was studied. The results showed that $LaNi_{0.8}Cu_{0.2}O_3$ precursor powder prepared through a co-precipitation method and calcined at $860^{\circ}C$ for 2 h formed uniform grains with diameters in the range of $400{\sim}500\;nm$. The maximum power density and the short circuit current density of the single cell unit at $550^{\circ}C$ were found to be $390\;mW/cm^2$ and $968\;mA/cm^2$, respectively.

Dispersion Characteristics of α-Fe2O3 Nanopowders Coated with Titanium Dioxide by Atomic Layer Deposition

  • Ok, Hae Ryul;Lee, Bo Kyung;Bae, Hye Jin;Kim, Hyug Jong;Choi, Byung Ho
    • Journal of the Korean Ceramic Society
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    • v.54 no.2
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    • pp.137-140
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    • 2017
  • A $TiO_2$ nanofilm was deposited on ${\alpha}-Fe_2O_3$ nanopowders using the atomic layer deposition method. The $TiO_2$ film was prepared at $300^{\circ}C$ using $Ti(N(CH_3)_2)_4$ and $H_2O$ as the precursor and reactant gas, respectively. The thickness and composition of the $TiO_2$ surface were characterized by TEM and EDS measurements. The TEM results showed that the growth rate of the film was about $0.12{\AA}/cycle$. The EDS and SAED analyses showed the presence of titanium oxide on the surface of the ${\alpha}-Fe_2O_3$ nanopowders, confirming the deposition of the $TiO_2$ nanofilm. The Zeta potential and sedimentation test results showed that the dispersibility of the coated nanopowders was higher than that of the uncoated nanopowders. This is attributed to the electrostatic repulsion between the $TiO_2$-coated layers on the surface of the ${\alpha}-Fe_2O_3$ nanopowders. The results revealed that the $TiO_2$-coated layers modified the surface characteristics of the ${\alpha}-Fe_2O_3$ nanopowders and improved their dispersibility.

A Study on the Synthesis of Gd-doped $CeO_2$ and Sr-doped $LaMnO_3$ Powders and Phase Stability in Their Interface (Gd-doped $CeO_2$ 와 Sr-doped $LaMnO_3$ 분말의 합성 및 그 계면에서의 상 안정성 연구)

  • 정승훈;김남진;이덕열
    • Journal of the Korean Ceramic Society
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    • v.34 no.6
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    • pp.652-658
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    • 1997
  • The phase stability in the interface of Sr-doped LaMnO3(LSM)/Gd-doped CeO2(CGO) was examined in this study in order to check the feasibility of using LSM as the cathode material in a low-temperature SOFC(solid oxide fuel cell) using CGO as the electrolyte. For the purpose, CGO powders of Ce0.82Gd0.18O0.91 and two LSM powders having different compositions, La0.9Sr0.1MnO3(LSM10) and La0.5Sr0.5MnO3(LSM50), were synthesized using Pechini method. Then, specimens having the LSM/CGO interface were prepared, heat-treated at 130$0^{\circ}C$ for up to 3 days, and analyzed by XRD and STEM/EDX. Face-centered cubic CGO powders of less than 10 nm size were obtained by calcination of polymeric precursor formed in the process at 45$0^{\circ}C$. Higher calcination temperature of $700^{\circ}C$ was necessary for monoclinic LSM10 and cubic LSM50 powders. LSM powders were coarser than CGO and observed to be in the range of 50~100 nm. No trace of LSM-CGO interaction product was found in the XRD pattern. Also it was known from the concentration profile in the vicinity of the interface that interdiffusion was occurred over only a small penetration depth of ~100 nm order.

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A Study on the Preparation of Tungsten Oxide powders Using Emulsion Evaporation Methods (에멀젼 증발법에 의한 산화텅스텐 분말의 제조에 관한 연구)

  • 신창훈;안종관;이응조
    • Journal of the Korean Ceramic Society
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    • v.35 no.6
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    • pp.543-550
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    • 1998
  • A process for the preparation of spherical tungsten oxide powders by the emulsion evaporation method was developed. The characteristics of the powders thus prepared were examined by means of TGA X-ray diffraction SEM and image analysis. The emulsion was prepared by fast mixing of tungsten containing aque-ous phase and the organic phase which contained kerosene surfactant and paraffin oil. The precursor was made by evaporating the emulsion in the kerosene bath at $160^{\circ}C$ and then calcined at $650^{\circ}C$ in order to pro-duce tungsten oxide powders. The average particle size of the tungsten oxide powders was $0.5\;\mu\textrm{m}$ and their shapes were spherical. Water-in-oil type emulsion wasmore advantageous to make less agglmerated. $W_{3}$ powders than the oil-in-water type emulsion for the emulsion evaporation experiments. As the HLB value of the surfactant increased and the concentration of tungsten ions in the aqueous phase decreased the mean particle size of tungsten oxide powders decreased whereas agglomeration increased. The optimum con-centration of Span 80 was 8 percent by volume and the optimum stirring speed in the emulsion formation was 5000 rpm in order to obtain find less agglomerated $W_{3}$ powders.

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