• Title/Summary/Keyword: Precursor Solution

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Fabrication and Characterization of Porous TiO2 Powder by Aerosol Process (에어로졸공정에 의한 다공성 TiO2분말의 제조 및 공극특성)

  • Chang, Han Kwon;Jang, Hee Dong;Park, Jin Ho;Cho, Kuk;Kil, Dae Sup
    • Korean Chemical Engineering Research
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    • v.46 no.3
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    • pp.479-485
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    • 2008
  • Porous $TiO_2$ nanostructured particles containing both mesopores and macropores were fabricated by utilizing an aerosol templating method from two kinds of starting materials (colloidal mixture of $TiO_2$ nanoparticles and PS particles, and that of TTIP solution and PS particles). The effects of mixing ratio of PS to $TiO_2$ and reactor temperature on the particle properties were investigated. When $TiO_2$ nanoparticles were used as starting materials, the increase of macropores number was observed by SEM and the specific surface area and total pore volume were increased from $31.6m^2/g$ to $39.1m^2/g$ and $0.068cm^3/g$ to $0.089cm^3/g$, respectively, by increasing the weight mixing ratio of $PS/TiO_2$ from 0.79 to 1.31. When TTIP was used as precursor, the specific surface area and mesopore volume of particles prepared at same condition decreased by 67% and 75%, respectively.

Fabrication of Al2O3/ZrO2Ceramics by the Polymerization Dispersion Process (ZrO2의 고분자화 분산법을 이용한 Al2O3/ZrO2요업체의 제조)

  • Cho, Myung-Je;Hwang, Kyu-Hong;Lee, Jong-Kook
    • Journal of the Korean Ceramic Society
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    • v.41 no.4
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    • pp.284-288
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    • 2004
  • To improve mechanical properties of $Al_2$O$_3$/ZrO$_2$composites have been controlled dispersion of ultra low size ZrO$_2$ particles in $Al_2$O$_3$ ceramics by polymeric precursor method (Pechini process). In case of coprecipitation or mechanical mixing of ZrO$_2$ powders with $Al_2$O$_3$, homogeneous dispersion and controlling the ZrO$_2$ size were relatively difficult due to high sintering temperature. So the polyesterization process of Zr/Y(NO$_3$)$_3$-citric acid solution in ethylene glycol with the commercial sub-micron sized o(-alumina powder (Sumitomo AES-11(0.4 ${\mu}{\textrm}{m}$)) was adopted in order to obtain homogeneous dispersion of ZrO$_2$ in A1203. By this partial polyesterization process, the homogeneous dispersion of relatively low sized ZrO$_2$in $Al_2$O$_3$/ZrO$_2$composites was achieved at 1450∼1$600^{\circ}C$ of sintering temperature range and their mechanical properties were measured.

Solvothermal Synthesis and Characterization of Cu3(BTC)2 Tubular Membranes Using Surface Modified Supports (표면 개질된 지지체를 이용한 Cu3(BTC)2 튜브형 분리막의 용매열 합성 및 특성분석)

  • Noh, Seung-Jun;Kim, Jinsoo
    • Korean Chemical Engineering Research
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    • v.52 no.2
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    • pp.214-218
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    • 2014
  • In this study, nanoporous $Cu_3(BTC)_2$ membranes were synthesized on macroporous alumina tube supports by solvothermal method. It is very difficult to prepare uniform and crack-free $Cu_3(BTC)_2$ layer on macroporous alumina support by in situ solvothermal method. In this study, continuous and crack-free $Cu_3(BTC)_2$ tubular membranes could be obtained by in situ solvothermal process after surface modification of alumina support. The surface modification was conducted by spraying Cu precursor solution on the alumina support heated at $200^{\circ}C$. The prepared $Cu_3(BTC)_2$ tubular membranes were characterized by XRD, FE-SEM and gas permeation experiments. $H_2$ permeance through $5{\mu}m$ thick $Cu_3(BTC)_2$ tubular membrane was calculated to be $7.8{\times}10^{-7}mol/s{\cdot}m^2{\cdot}Pa$ by single gas permeation test, with the ideal selectivities of $H_2/N_2=11.94$, and $H_2/CO_2=12.82$.

Preparation of Ferroelectric (YbxY1-x)MnO3 Thin Film by Sol-Gel Method (졸-겔법에 의한 (YbxY1-x)MnO3강유전체 박막제조)

  • 강승구;이기호
    • Journal of the Korean Ceramic Society
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    • v.41 no.2
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    • pp.170-175
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    • 2004
  • The ferroelectric (Y $b_{x}$ $Y_{1-x}$)Mn $O_3$ thin films were fabricated by sol-gel method using Y-acetate, Yb-acetate, and Mn-acetate as raw materials. The stable (Y $b_{x}$ $Y_{1-x}$)Mn $O_3$ precursor solution (sol) was prepared through the reflux process with acetylaceton as a catalyst and coated on Si(100) substrate by spin coating. The heat treatment temperature and, Rw ($H_2O$/alkoxide moi ratio) dependence on crystallinity of thin films were studied. The lowest temperature for obtaining YbMn $O_3$phase and the optimum heat-treatment conditions were proved as at 7$50^{\circ}C$ and 80$0^{\circ}C$, respectively. The hexagonal YbMn $O_3$with c-axis preferred orientation could be obtained at Rw=1 condition. The remanent polarization for the thin films of x=0 or 1 was about 200 nC/㎤ while, for the specimens ot 0< x< 1, were 50∼100 nC/$\textrm{cm}^2$.

Synthesis of Protoberberine Derivatives and Their Biological Activities (Protoberberine의 고급지방산 유도체합성 및 활성연구(V))

  • Kim, Sin-Kyu;Kwon, Chang-Ho;Yook, Chang-Soo;Rho, Young-Soo;Seo, Seong-Hoon;Choung, Se-Young;Chung, Sung-Hyun;Kim, Dong-Hyun;Hwang, Soon-Ho
    • YAKHAK HOEJI
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    • v.36 no.1
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    • pp.1-6
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    • 1992
  • Irradiation of phenolbetaine in a stream of nitrogen produced 8,14-cycioberbine[1]. Compound[1] was treated with 10% HCl solution to give the 8-hydroxycycloberbine[2] in 67.7% yield. Subsequently addition of ethylchloroformate to the compound[2] gave rise to the 8-hydroxy-7-ethylcarboxy-9, 10-dimethoxy-2, 3-methylenelioxy-13-oxo-norochotensane[3] in 78% yield. Treatment of the compound[3] with bis-(2-chloroethyl)amine then lead to the 7-bis(2-chloroethyl)carbamyl-norochoteneare[4]. On the other hand the compound[5], which is the 8-methoxynorochotensane, was derived when compound[1] was treated with methanol in a few drops of BF. Treatment of the compound[6], and the compound[7], 7-bis(2-chloroethyl)-carbanyl-8-methoxy-norocheyensane, was then synthesized by reaction of the compound[6] with bis(2-chloroethyl) amine. In the other synthetic pathway when compound[5] was treated with $POCl_3$ in dried benzene, 13-chloro-6-ene-norochetensane[8] with 42% yield was formed. Finally the 13-bis-(2-chloroethyl) amino-8-methoxy-norochotensane[9] was produced when we treated the compound[8] with bis-(2-chloroethyl) amine. In another pathway, reaction between phenolbetaine which is the precursor of the compound[1] and benzoylchloride in dried chloroform gave us the 5,6,7 trihydro-2, 3-methylene-dioxy-9-chloromethyl-10, 11-dimethoxyphenylisoquinoline-8-benzoate[10] in 73% yield. The results of biological activities for these compounds are also presented in Table I and II.

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Study on crystallization of $PbTiO_3$ thin films by the Sol-Gel method (Sol-Gel법을 이용한 $PbTiO_3$ 박막의 결정화에 관한 연구)

  • Kyu Seog Hwang;Byung Wan Yoo;Byung Hoon Kim
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.4 no.2
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    • pp.199-209
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    • 1994
  • $PbTiO_3$ thin films were prepared on soda-lime-silica slide glasses, Si-wafer and sapphire substrate by the dip-coating of precursor solution. As starting materials, titanium tetra iso-propoxide and lead acetate trihydrate were used. Then acetylacetone was added to prepare stable sol. The effect of the parameters such as viscosity and composition of sol were investigated. The optical transmittance at visible range, refractive index, IR spectra were measured in varying compositions, thickness and heat treatment temperature. The crystallization of $PbTiO_3$ films were measured by using XRD and SEM. Diffusion of compositions from slide glass to thin film were investigated by using EDX, too. These sols not precipitated for 20 days. Transmittance of $PbTiO_3$ films at visible range were decreased with the increase of thickness and heat treatment temperatures, and were exhibited flat spectra. Pyrochlore type appeared in the films on slide glass and perovskite type appeared in the films on Si-wafer or sapphire at $600^{\circ}C$. Perovskite crystals transformed to $PbTi_3O_7$ phase at $800^{\circ}C$.

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Synthesis of Lithium Manganese Oxide by a Sol-Gel Method and Its Electrochemical Behaviors (졸-겔 방법에 의한 LiMn2O4의 합성 및 전기화학적 거동)

  • Jeong, Euh-Duck;Moon, Sung-Wook;Lee, Hak-Myoung;Won, Mi-Sook;Yoon, Jang-Hee;Park, Deog-Su;Shim, Yoon-Bo
    • Journal of the Korean Electrochemical Society
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    • v.6 no.4
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    • pp.229-235
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    • 2003
  • A precursor of lithium manganese oxide was synthesized by mixing $(CH_3)_2CHOLi\;with\;Mn(CH_3COO)_2{\cdot}4H_2O$ in ethanol using a sol-gel method, then heat-treated at $400^{\circ}C\;and\;800^{\circ}C$ in air atmosphere. The condition of heat treatment was determined by thermogravimetric analysis/differential thermogravimetric analysis (TGA/DTA). The characterization of the lithium manganese oxide was done by X-ray diffraction (XRD) spectra and scanning electron microscopy (SEM). The electrochemical characteristics of lithium manganese oxide electrode for lithium ion battery were measured by cyclic voltammetry (CV), chronoamperometry and AC impedance method using constant charge/discharge process. The electrochemical behaviors of the electrode have been investigated in a 1.0M $LiClO_4/propylene$ carbonate electrolyte solution. The diffusivity of lithium ions, $D^+\;_{Li}\;^+$, as determined by AC impedance technique was $6.2\times10^{-10}cm^2s^{-1}$.

Influence of Addition Amount of CaCO3on the Synthesizing behavior and Microstructural Evolution of CaZrO3 and m-ZrO2 in 5ZrSiO4-xCaCO3 Mixture System (5ZrSiO4-xCaCO3 혼합계에서 CaCO3첨가량이 CaZrO3와 m-ZrO2의 합성 및 미세구조변화에 미치는 영향)

  • Kim, Jae-Won;Lee, Jae-Ean;Jo, Chang-Yong;Lee, Je-hyun;Jung, Yeon-Gil
    • Korean Journal of Materials Research
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    • v.13 no.9
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    • pp.572-580
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    • 2003
  • Synthesizing behavior and microstructural evolution of $CaZrO_3$and $m-ZrO_2$in a thermal reaction process of $ZrSiO_4$-$xCaCO_3$mixtures, where x is 7 and 19, were investigated to determine the addition amount of CaO in CaO:$ZrO_2$:$SiO_2$ternary composition. CaZrO$_3$-Ca$_2$SiO$_4$precursor prepared by the mixture of $ZrSiO_4$and CaCO$_3$in aqueous suspending media was controlled to the acidic (pH=4.0) condition with HCI solution to enhance the thermal reaction. The addition amount of dispersant into the $ZrSiO_4$-$xCaCO_3$slip increased with increasing mole ratio of $CaCO_3$, which was associated with the viscosity of slip. Decarbonation reaction was activated with an increase of the addition amount of $CaCO_3$, showing different final temperatures in $ZrSiO_4$-$7CaCO_3$and $ZrSiO_4$-$19CaCO_3$mixtures as about 980 and 116$0^{\circ}C$, respectively, for finishing decarbonation reaction. The grain morphology was changed to spherical shape for all samples with an increase of sintering temperature. The grain size and phase composition of the synthesized composites depended on the mixture ratio of Zrsi04 and CacO3 powders, indicating that the main crystals were m-ZrO2 ($\leq$3 $\mu\textrm{m}$) and $CaZrO_3$ ($\leq$ 7 $\mu\textrm{m}$) in $ZrSiO_4$$>-7CaCO_3$and $ZrSiO_4$-$19CaCO_3$mixtures, respectively.

Fabrication and Property of Ba0.5Sr0.5Co0.8Fe0.2O3-δ Hollow Fiber Membranes (Ba0.5Sr0.5Co0.8Fe0.2O3-δ 중공사 분리막의 제조 및 물성)

  • Jeon, Sung Il;Park, Jung Hoon;Kim, Jong Pyo;Sim, Woo Jong;Lee, Yong Taek
    • Korean Chemical Engineering Research
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    • v.50 no.1
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    • pp.1-5
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    • 2012
  • $Ba_{0.5}Sr_{0.5}Co_{0.8}Fe_{0.2}O_{3-{\delta}}$ hollow fiber with o.d. 1.02 mm and i.d. 0.437 mm were fabricated by a phase-inversion spinning technique.The starting $Ba_{0.5}Sr_{0.5}Co_{0.8}Fe_{0.2}O_{3-{\delta}}$ precursor was synthesized by the polymerized complex method and then calcined at $900^{\circ}C$. As-prepared powder was dispersed in a polymer solution, and extruded as form of hollow fiber through a spinneret. Finallydense $Ba_{0.5}Sr_{0.5}Co_{0.8}Fe_{0.2}O_{3-{\delta}}$ hollow fiber membrane was obtained by sintering for 2 h at $1,080^{\circ}C$ for the application of oxygen separation. In addition, despite a very thin membrane with 0.58 mm, the BSCF hollow fiber membrane possessed a proper mechanical strength of 602.5 MPa.

Hydrothermal Synthesis and Mechanical Characterization of ZrO2 by Y2O3 Stabilizer Contents (Y2O3안정화제 첨가량에 따라 수열합성법으로 제조된 ZrO2-Xmol% Y2O3분말의 합성 및 기계적 특성)

  • Lee, Hak-Joo;Kim, Taik-Nam;Bea, Sung-Chul;Go, Myung-Won;Ryu, Jae-Kyung
    • Korean Journal of Materials Research
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    • v.20 no.10
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    • pp.518-523
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    • 2010
  • In this study, partially stabilized zirconia was synthesized using a chemical $Y_2O_3$ stabilizer and hydrothermal method. First, $YCl_3-6H_2O$ and $ZrCl_2O-8H_2O$ was dissolved in distilled water. Y-TZP (a $Y_2O_3$-doped toughened zirconia polycrystalline precursor) was also prepared by conventional co-precipitates in the presence of an excess amount of $NH_4OH$ solution under a fixed pH of 12. The Y-TZP precursors were filtered and repeatedly washed with distilled water to remove $Cl^-$ ions. $ZrO_2$-Xmol%$Y_2O_3$ powder was synthesized by a hydrothermal method using Teflon Vessels at $180^{\circ}C$ for 6 h of optimized condition. The powder added with the Xmol%- $Y_2O_3$ (X = 0,1,3,5 mol%) stabilizer of the $ZrO_2$ was synthesized. The crystal phase, particle size, and morphologies were analyzed. Rectangular specimens of $33mm{\times}8mm{\times}3$ mm for three-point bend tests were used in the mechanical properties evaluation. A teragonal phase was observed in the samples, which contains more than 3 mol% $Y_2O_3$. The $3Y-ZrO_2$ agglomerated particle size was measured at $7.01{\mu}m$. The agglomerated particle was clearly observed in the sample of 5 mol % $Y_2O_3-ZrO_2$, and and the agglomerated particle size was measured at 16.4 um. However, a 20 nm particle was specifically observed by FE-SEM in the sample of 3 mol% $Y_2O_3-ZrO_2$. The highest bending fracture strength was measured as 321.3 MPa in sample of 3 mol% $Y_2O_3-ZrO_2$.