• Title/Summary/Keyword: Sol-gel preparation

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Preparation of Zirconium Nitride by Nitridation of Zirconia and its Physical Characteristics (Zirconia로부터 Zr 질화물의 합성 및 물리화학적 특성)

  • Ahn, Beom-Shu;Sung, Ki-Chun
    • Journal of the Korean Applied Science and Technology
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    • v.20 no.4
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    • pp.358-365
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    • 2003
  • Zirconium nitride powders were synthesized at a relatively lower temperature using methane as a reducing agent in the nitridation of zircoia. $ZrO_2$ powder was prepared by a sol-gel technique. The resulting sol-gel was centrifuged, and the gel was washed with deionized water. Anhydrous ammonia was used as the nitrogen source and methane was used as the reducing agent. Conversion diagrams show the equilibrium solid phase as a function of reagent concentrations for a specific temperature and gas pressure for the reagent system $NH_3-ZrO_2-CH_4$. The reagent concentration ranges within which pure ZrN is formed increase with increasing reaction temperature. Low pressure with an excess of hydrogen decreases the reaction temperature at which pure ZrN is formed. Low pressure together with the introduction of excess hydrogen into the reaction system increases Zr and N conversion efficiency and retards C deposition.

Preparation of $10TiO_2$.$90SiO_2$ Glass by Sol-Gel Process (졸-겔법에 의한 $10TiO_2$.$90SiO_2$ 유리의 제조)

  • Rhee, Jhun;Chi, Ung-Up;Kang, Tae-Soo;Jo, Dong-Soo;Ko, Sung-Kwan
    • Journal of the Korean Ceramic Society
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    • v.23 no.4
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    • pp.27-34
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    • 1986
  • In the present study an attempt was made to synthesize $10TiO_2$.$90SiO_2$ glass by Sol-Gel process. Tetra-ethyl-ortho-silane and titanium-iso-propoxide were used as precursors. As the mutual solvent ethanol and iso-propanol were used. TEOS was partially hydrolyzed with one-fold mole of $H_2O$ prior to the reaction with titanium-iso-propoxide to control the difference of hydrolysis rate of the two metal alkoxides. At gelling temperature higher than 6$0^{\circ}C$ it was difficult to obtain monolithic gels. At such a low temperature as 85$0^{\circ}C$ clear amorphous gel derived glass with Si-O-Ti bonding was obtained.

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Adhesion improvement between metal and ceramic substrate by using ISG process (ISG법에 의한 금속과 세라믹기판과의 밀착력 향상)

  • 김동규;이홍로;추현식
    • Journal of the Korean institute of surface engineering
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    • v.32 no.6
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    • pp.709-716
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    • 1999
  • Ceramic is select for an alternative substrate material for high-speed circuits due to its low-thermal expansion. As, in this study, ceramic was prepared by ISG (interlayer sol-gel) process using metal salts and a metal alkoxide as the starting materials. Generally ceramic substrate is used electroless copper plating for the metallization. But it has been indicate weakely the adhesion strength between the substrate and copper layer. Therefore, this research, using the ISG process on the preparation of homogeneous and possible preparation at law temperature fabricated sol solution. Using of the dip coating method was coated for the purpose of giving the anchoring effect on the coating layer and enhancing the adhesion strength between the $Al_2$O$_3$ substrate and copper layer. This study examined primary the characteristic of the sol making condition and differential thermal analysis (DTA) X-ray diffraction (XRD) were mearsured to identify the crystal phase of heat treatment specimens. The morphology of the coated films were studied by scanning electron microscopy(SEM). As a resurt, XRD analysis was obtained patterns of $\alpha$-cordierite after heat-treatment about 2 hours at $1000^{\circ}C$. SEM analysis could have seen a large number of voids on coated film. The more contants of$ Al_2$$O_3$ Wt% was increased the more voids was advanced. Peel adhesion strength has a maximum in the contants of the TEOS:ANE of 1:0.7 mole%. In this case, adhesion strength has been measured 1150gf, peel adhesion strength were about 10 times more than uncoated of the ceramics film.

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Glass Preparation of$ZrO_2$-$SiO_2$ System by the Sol-Gel Method (졸-겔법에 의한 $ZrO_2$-$SiO_2$계 유리 제조)

  • 신대용;한상목;소명기;이풍헌
    • Journal of the Korean Ceramic Society
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    • v.27 no.5
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    • pp.668-676
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    • 1990
  • Glass in the ZrO2-SiO2 system containing up to 30mol% ZrO2 were prepared by heating the gel made from the mixed solutions of Zr(OC3H7)4 and partial hydrolysed Si(OC2H5)4. As a result, the monolith gel was made from the HCl and water content as 2.7$\times$10-3 and 8 molar ratio to alkoxide and drying temoperature as 4$0^{\circ}C$. Heating rate of dry gel maintained under 0.5$^{\circ}C$/min and heating at a temperature as 90$0^{\circ}C$ was found to be for making the transparent glass.

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Preparation of Silica Sol by Partial Hydrolysis of TEOS and High Purity Silica Glass Fiber (TEOS의 부분가수분해에 의한 실리카 졸의 합성과 유리섬유 제조)

  • Yang, Hyun S.;Kwon, Oh H.;Lee, Jae D.;Rho, Jae S.;Kim, Young H.
    • Applied Chemistry for Engineering
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    • v.7 no.5
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    • pp.823-831
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    • 1996
  • At the ratio [$H_2O$]/[TEOS]=1.7, the silica sol was synthesized by partial hydrolysis in the presence of acid catalyst. After stabilizing the silica sol by trimethylsilylation, the molecular weight and viscosity of the sol obtained at various reaction times were examined to determine a best spinnability of the sol. Gel fibers were prepared from the sol solution after removing solvent in the solution, and the gel fibers were heated at $1,000^{\circ}C$. The prepared silica fibers were in the shape of circular cross-section and their tensile strength and $SiO_2$ purity were $83{\pm}20kg/mm^2$ and about 99.997%, respectively.

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Preparation and Gas Permeation Properties of Silica Membranes on Porous Stainless Steel-Tube Supports (다공성 금속 지지체에 제조된 실리카 분리막의 기체 투과 특성)

  • Lee, Hye Ryeon;Seo, Bongkuk
    • Membrane Journal
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    • v.24 no.3
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    • pp.177-184
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    • 2014
  • Silica membranes with high permeability were prepared using colloidal and polymeric silica sols on a porous stainless steel-tube support by a DRFF and SRFF method. Silica sols were derived with tetraethylorthosilicate (TEOS) by sol-gel method and analyzed with DLS, FE-SEM, and $N_2$ adsorption. The coating of the intermediate layer with colloidal silica sol on the stainless steel-tube support led to a denser surface morphology of the membrane along with a considerable reduction in the number of surface defect. As the polymeric silica sol enclosed the colloidal silica sol with spherical particles during the SRFF method, the separation-layer-coated silica membrane showed a denser surface than the intermediate layer. Moreover, the silica membranes showed high hydrogen gas permeability of $(6.63-9.21){\times}10^{-5}mol{\cdot}m^{-2}{\cdot}s^{-1}{\cdot}Pa^{-1}$ with low $H_2/N_2$ perm-selectivity (2.9-3.1) at room temperatures.

Preparation of Thin Film Electrolyte for Solid Oxide Fuel Cell by Sol-Gel Method and Its Gas Permeability (졸-겔법을 이용한 고체산화물연료전지의 전해질 박막 제조 및 가스 투과도)

  • Son, Hui-Jeong;Lee, Hye-Jong;Lim, Tak-Hyoung;Song, Rak-Hyun;Peck, Dong-Hyun;Shin, Dong-Ryul;Hyun, Sang-Hoon;Kilner, John
    • Journal of the Korean Ceramic Society
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    • v.42 no.12 s.283
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    • pp.827-832
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    • 2005
  • In this study, thin electrolyte layer was prepared by 8YSZ ($8mol\%$ Yttria-Stabilized Zirconia) slurry dip and sol coating onto the porous anode support in order to reduce ohmic resistance. 8YSZ polymeric sol was prepared from inorganic salt of nitrate and XRF results of xerogel powder exhibited similar results $(99.2\pm1wt\%)$ compared with standard sample (TZ-8YS, Tosoh Co.). The dense and thin YSZ film with $1{\mu}m$ thickness was synthesized by coating of 0.7M YSZ sol followed by heat-treatment at $600^{\circ}C$ for 1 h. Thin film electrolyte sintered at $1400^{\circ}C$ showed no gas leakage at the differential pressure condition of 3 atm.

Preparation of $LaAlO_3$ thin Films by Sol-gel Method (Sol-gel 방법에 의한 $LaAlO_3$ 박막의 제조)

  • Kim, H.J.;Kim, B.J.;Lee, H.G.;Hong, G.W.
    • Progress in Superconductivity
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    • v.9 no.1
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    • pp.85-90
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    • 2007
  • Lanthanum aluminate($LaAlO_3$) film has been prepared on single crystal and metal substrates by dip coating method. Lanthanum acetate and aluminum were prepared via ligand exchange starting from lanthanum nitrate hexahydrate and aluminum nitrate hexahydrate in acetate glacial acetic acid solution after being refluxed. Coating solution was obtained by diluting the gel with methanol and 2-methoxyethanol to adjust the total cation concentration to 0.67 M. Precursor coated film was prepared by dip-coating with a speed of 25 mm/min on various substrates such as $LaAlO_3$ (001), MgO(001), $SrTiO_3$(001) single crystal, LMO/MgO/Ni-alloy. Thin films have been obtained by heat treating the precursor film at various temperatures from $600^{\circ}C{\sim}900^{\circ}C$ and various heating rate from $0.83^{\circ}C/min{\sim}1.25^{\circ}C/min$ under $Ar/O_2$ mixture containing 1000ppm oxygen. The films have been characterized by scanning electronic microscopy (SEM) and X-ray diffraction (XRD). XRD analysis for the prepared film showed that $LaAlO_3$ thin films with a preferred orientation of (100) plane parallel to substrate surface were obtained at $800^{\circ}C(1.11\;^{\circ}C/min)$ on LMO/MgO/Ni-alloy substrate, but the intensity decreased with the increase of heat treatment temperature.

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Preparation of NASIglasses by Sol-Gel Process (솔-젤법에 의한 NASIglass의 제조)

  • 김희주;강은태;김종옥
    • Journal of the Korean Ceramic Society
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    • v.32 no.12
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    • pp.1357-1368
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    • 1995
  • Nasigels of composition Na0.75Zr2PSi2O12 and Na3Zr2PSi2O12 have been synthesized by the sol-gel technique using metal alkoxide precursors. The monolithic dry gels of Na0.75Zr2PSi2O12 with no crack have been prepared by the control of the shrinkage rte, but gels of Na3Zr2PSi2O12 were impossible to prepare without cracking. The gels treated up to 80$0^{\circ}C$ led to the formtion of glass but the glasses were converted to the crystalline phases at above this temperature. Crystaline phases precipitated from the Na0.75Zr2PSi2O12 glass were NASICON-like phase, Na2Si2O5, and free Zirconia. Phase that precipitated from the Na3Zr2PSi2O12 was only rhombohedral NASICON. For Na0.75Zr2PSi2O12 gels, framework of PO4 tetrahedra and SiO4(PO4) tetrahedra formed at low temperature but changed to that of SiO4 and SiO4(PO4) tetrahedras as it were crystallized. In the case of Na3Zr2PSi2O12 gel, framework of isolated PO4 and SiO4 tetrahedras formed at low temperature but changed to SiO4(PO4) tetrahedra framework which usually formed in the NASICON crystal after crystallization at high temperature. The gels treated up to 80$0^{\circ}C$ contained the residual water. The ionic conduction was attributed to the motion of proton and Na+ ion at low (up to 150~20$0^{\circ}C$) and high temperatures, respectively. As the temperature of heat treatment increased, ionic conductivity gradaully increased with the extent of precipitation of crystalline phase.

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Preparation of an Intermediate and Particle Characteristics for HTGR Nuclear Fuel (고온가스로 핵연료 중간물질 제조와 분말특성)

  • Jeong, Kyung-Chai;Kim, Yeon-Ku;Oh, Seung-Chul;Lee, Young-Woo
    • Journal of the Korean Ceramic Society
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    • v.44 no.2 s.297
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    • pp.124-131
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    • 2007
  • In this study, first the ADU gel particle, an intermediate for final $UO_2$ kernel of a HTGR nuclear fuel, was prepared from sol-gel method using the broth solution which was made by mixing of the uranyl nitrate, poly vinyl alcohol and tetra-hydrofurfuryl alcohol. The prepared dried-ADU gel particles were converted to the $UO_2\;via\;UO_3$ from thermal treatment with the 4% $H_2$ atmosphere. The sizes of the spherical liquid droplets appeared $1900{\sim}2100{\mu}m$, and the harmony between the flow rate of the broth solution and the frequency and the amplitude of a vibrating system are important factors for the spherical ADU gel particles via the mono size spherical droplets. From the XRD and FT-IR analyses, the prepared ADU gel particles were judged to be a $UO_3{\cdot}xNH_3{\cdot}yH_2O$ form, and the most important factor during the thermal treatment of the dried-ADU gel particle must be avoided a rapidly heating rate in the range of $180{\sim}400^{\circ}C$, and the heating rate should be kept below $5^{\circ}C/min$.