• Title/Summary/Keyword: Sol-gel route

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Preparation of Y3Al5O12 Nanocrystals by a Glycol Route

  • Bartwal, Kunwar Singh;Kar, Sujan;Kaithwas, Nanda;Deshmukh, Monica;Dave, Mangla;Ryu, Ho-Jin
    • Journal of the Korean Ceramic Society
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    • v.44 no.5 s.300
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    • pp.151-154
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    • 2007
  • Yttrium aluminum garnet, $Y_3Al_5O_{12}$ (YAG) is an extensively used solid-state laser host material. YAG nanocrystals were synthesized using low-temperature glycol method, a modified sol-gel method performed at low temperature that consists of a mixture of salts that are mostly nitrates in an aqueous media. Single-phase nanocrystalline YAG was obtained at $850^{\circ}C$, which is a much lower temperature than with other techniques such as a wet-chemical technique. The structural characterization is done by powder X-ray diffraction, scanning electron microscopy and transmission electron microscopy. A crystallite size range of 20-50 nm was observed for the materials prepared at $850-950^{\circ}C$.

Acridine Fluorescence Behaviors in Different Polymeric Microenvironments Directed by C2-Proton-Acidity of Imidazolium-Based Ionic Liquids

  • Ji, Myoung-Jin;Kim, Jong-Gyu;Shin, Ueon-Sang
    • Bulletin of the Korean Chemical Society
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    • v.33 no.8
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    • pp.2489-2493
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    • 2012
  • A new fluorescent system (acridine/RTIL hybrid gel) confined in the 3D micro-structure of a poly(lactic acid) membrane were prepared from 1-butyl-3-methylimidazolium-based ionic liquids ([bmim]X (X = $SbF_6$, $NTf_2$, Cl); RTILs), poly(lactic acid) (PLA), and acridine via the sol-gel route. SEM images showed that, in the presence of [bmim]$SbF_6$ and [bmim]$NTf_2$, 3D-ly paticulated structures were created inside the PLA membranes and acridine/RTIL hybrid gels were confined in gabs of particulates. However, the use of [bmim]Cl induced the formation of a 3D-ly porous structure containing the hybrid gel of acridine/[bmimCl in the micropores. The three fluorescent systems exhibited different fluorescence behaviors (fluorescence maximum and intensity) depending on the C2-H acidity scale of the RTILs (or their anion type). Acridine gels hybridized with [bmim]$SbF_6$ and [bmim]$NTf_2$ showed blue fluorescence with relative high intensity, whereas the hybrid gel with [bmim]Cl exhibited almost no fluorescence under dry conditions. However, the acridine/[bmim]Cl hybrid system in the micro-porous PLA membrane started to emit fluorescent light under humid conditions and showed a possible response, indicating that it could be applied as a humidity sensor.

Studies on the Synthesis of High Purity and Fine Mullite Powder (I) (고순도 초미립자 물라이트 분말 합성에 대한 연구 (I))

  • 김경용;김윤호;김병호;이동주
    • Journal of the Korean Ceramic Society
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    • v.26 no.5
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    • pp.682-690
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    • 1989
  • Fine mullite powder was prepared by colloidal sol-gel route. Boehmite as a starting material of Al2O3 and silica sol or fumed silica as a starting material of SiO2 were used. $\alpha$-Al2O3, TiO2 and ZrO2 were used as seeding materials. The combination of boehmite and silica was found to be the stoichiometric mullite powder. Techniques for drying used were spray drying, freeze drying, reduced pressure evaporation and drying in a oven. The gelled powder was heated at 130$0^{\circ}C$ for 100min and was attrition-milled for 1~3hrs. The mullite powder obtained was composed of submicrometer, uniform and spherical particles with a narrow size distribution. The mullite powder was characterized by BET, SEM, XRD and IR spectroscopy.

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Simple fabrication route for vertically-aligned CZTS nanorod arrays for photoelectrochemical application based on AAO template

  • Kim, Ji-Min;Yang, U-Seok;O, Yun-Jeong;Mun, Ju-Ho
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.402.2-402.2
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    • 2016
  • In photoelectrochemical (PEC) water splitting, Cu2ZnSnS4 (CZTS) compound has attracted intense attention as a photocathode due to not only large optical absorption coefficient, but also earth-abundance of constituent elements and suitable band alignment. With rapid development of nanotechnology, one-dimensional nanostructures of CZTS have been investigated as a potential form to achieve high efficiency because the nanostructures are expected to be capable of capturing more light and enhancing charge separation and transport. Here, we report a well-controlled fabrication route for vertically-aligned CZTS nanorod arrays on anodic aluminium oxide (AAO) template via simple sol-gel process followed by deposition of ZnS or CdS buffer layers on the CZTS nanorod to enhance charge separation. The structure, morphology, composition, optical absorption, and PEC properties of the resulting CZTS nanorod samples were characterized using X-ray diffraction, Raman spectroscopy, transmission electron microscopy, energy dispersive X-ray spectrometry, scanning electron microscopy, and UV-vis spectroscopy.

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Preparation and Characterization of BaTiO3 Powders and Thin films (티탄산바륨 분말과 박막의 제조 및 특성 연구)

  • Jung, Miewon;Son, Hyunjin;Lee, Jiyun;Kim, Hyunjung
    • Analytical Science and Technology
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    • v.17 no.2
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    • pp.173-179
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    • 2004
  • The $BaTiO_3$ powders and thin films were prepared by an alkoxide modified sol-gel process (polymerization-complex route) using ethylene glycol. The stable starting (Ba-Ti)-mixed metal organic sol was made by addition of acetylacetone. The $BaTiO_3$ powders, which had a particle size of 40~77 nm, were crystallized from an amorphous to a tetragonal phase on annealing at 700 and $1100^{\circ}C$ for 1 h. From FT-IR, solid-state $^{13}C$ CP/MAS NMR spectroscopy and X-ray diffractometry, the trace of the Ba-Ti-oxycarbonate phase first appeared at $400^{\circ}C$. Hydrolyzed sol was spin coated on a quartz wafer at 3500 rpm for 60 s and pyrolyzed at $1100^{\circ}C$ for 1 h. After heat treatment, the coated layer became dense and smooth.

Preparation of Bi2O3-PbO-SrO-CaO Coating Sol for Wiring and Superconductivity and Its properties

  • Jung, Jee-Sung;Iwasaki, Mitusnobo;Park, Won-Kyu
    • Korean Journal of Materials Research
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    • v.17 no.3
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    • pp.147-151
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    • 2007
  • Cu-free multi-component sol, of which final oxide composition becomes $Bi_{1.9}Pb{0.35}SrCaO,\;Bi_{1.8}Pb_{0.2}SrCaO\;and\;Bi_{1.5}SrCaO$, respectively, was prepared through sol-gel route and coated on a bare Cu substrate. Starting materials were metal-alkoxides as follows.; [$Bi(OC_{2}H_{5})_{3}\;Pb(O^{1}C_{3}H_{7})_{2},\;Sr(O^{i}C_{3}H_{7})_{2},\;Ca(OC_{2}H_{5})_{2}$] as a reagent grade. Transparent light yellowish sol was obtained in the case of $Bi_{1.9}Pb_{0.35}SrCaO\;and\;Bi_{1.8}Pb_{0.2}SrCaO$ composition and $Bi_{1.5}SrCaO$ composition's sol was light greenish. Each sol was repeatedly dip-coated on Cu substrate four times and pre-heated at $400^{\circ}C$ and finally heat-treated in the range of $740{\sim}900^{\circ}C$. In the results, crystalline phases confirmed by XRD were (2201) orthorhombic and monoclinic phases. However, only $Bi_{1.9}Pb_{0.35}SrCaO_{x}$ composition showed pseudo-superconductive behavior after heat-treatment at $900^{\circ}C$ for 12 seconds and then onset temperature was 77 K, even though it did not exhibit zero resistance below Tc.

The Study on Thermal Analysis and Thermodynamic Characteristics of Spinel Compounds(ZnCo2O4, NiCo2O4) (스피넬 구조를 가지는 전이금속화합물(ZnCo2O4, NiCo2O4)의 열적 분석 및 열역학적 특성 연구)

  • Kim, Jae-Uk;Ji, Myoung-Jin;Cha, Byung-Kwan;Kim, Chul-Hyun;Jang, Won-Cheoul;Kim, Jong-Gyu
    • Journal of the Korean Chemical Society
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    • v.54 no.2
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    • pp.192-197
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    • 2010
  • The spinel compound was obtained by the thermal decomposition of Zn-Co and Zn-Ni gel prepared by sol-gel method using oxalic acid as a chelating agent. The formation of spinel compound has been comfirmed by thermogravimetric analysis (TGA), x-ray powder diffraction (XRD) and infrared spectroscopy (IR). The particle size of 13 nm~16 nm was calculated by Scherrer's equation. The sol-gel method provides a practicable and effective route for the synthesis of the spinel compound at low temperature ($350^{\circ}C$). The kinetic parameters such as activation energy (Ea) and pre-exponential factor (A) for each compound were found by means of the Kissinger method and Arrhenius equation. The decomposition of spinel compound has an activation energy about 155 kJ/mol. Finally, the thermodynamic parameters (${\Delta}G^{\varphi}$, ${\Delta}H^{\varphi}$, ${\Delta}S^{\varphi}$) for decomposition of spinel compound was determined.

Fabrication of Anorthite for Low-Firing Ceramic Substrate by PVA Steric-Entrapment Route (폴리머 고착공정을 통한 저온소성기판용 Anorthite의 제조)

  • Kim, Gwang-Seok;Lee, Chung-Hyo;Lee, Sang-Jin
    • Korean Journal of Materials Research
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    • v.12 no.8
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    • pp.595-599
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    • 2002
  • A homogeneous and stable, amorphous-type, anorthite (CaO $Al_2$$O_3$ $2SiO_2$)powder was synthesized by an organic-inorganic steric entrapment route. Polyvinyl alcohol ( PVA) was used as an organic carrier for the precursor ceramic gel. The PVA content, its degree of polymerization and type of silica sol had a significant influence on the calcination and crystallization behavior of the precursors. For densifiction and crystallization at low temperature, porous and soft, amorphous-type anorthite powder was planetary milled for 20h. The milled powder crystallized to stable anorthite phase and densified to a relative density of 94% below $1000^{\circ}C$. In the development of crystalline phases of the planetary milled powder, omisteinbergite phase was unusually observed at $900^{\circ}C$, and then anorthite was observed at $950^{\circ}C$. The sintered anorthite had a thermal expansion coefficient of $4.6$\times$10^{-6}$ /$^{\circ}C$ and a dielectric constant of 7.5 at 1 MHz. Finally, the anorthite synthesized by the new process is expected to be an useful material for low-firing ceramic substrate.

Alumimium Titanate-Mullite Composites : Part1,Thermal Durability (Alumimium Titanate-Mullite 복합체: Part1, 열적 내구성)

  • Kim, Ik-Jin;Gang, Won-Ho;Go, Yeong-Sin
    • Korean Journal of Materials Research
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    • v.3 no.6
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    • pp.624-631
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    • 1993
  • The composites in the system aluminium titanate-mullite were synthesized by stepwise alkoxide hydrolysis of tetraethylorthosilicate, Si(OCLH5), and titaniumtetraethoxide, $Ti(OC_{2}H_{5})_4$ in $Al_{2}O_{3}$ ethanolic colloidal solution. All particles produced by sol-gel-process were amorphous, monodispesed and had a narrow particle size distribution. Sintered bodies at $1600 ^{\circ}C$ for 2h were subjected to prolonged durability tests-on the one hand annealing at the critical decomposition temperature of $1100 ^{\circ}C$ for lOOh and on the other cyclic thermal shock between 750 and $1400 ^{\circ}C$ for 100h. The best thermal durability was achieved by a composition containing 70 and 80 vol% aluminium titanate, which showed little change in microstructure and thermal expansion cycles during the tests. The microstructural degradation of samples studied using scanning electron microscopy, X-ray diffraction, and dilatometry, was presented here. The study was conducted in order to predict the service life of aluminium titanate-mullite ceramics formed by this processing route.

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A Synthesis of $(Ba_{1-x}Sr_x)TiO_3$ Powders by Sol-Gel Route (졸-겔법을 이용한$(Ba_{1-x}Sr_x)TiO_3$분말합성)

  • Kim, Young-Seok;Kim, Duk-Jun;Kim, Hwan
    • Korean Journal of Materials Research
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    • v.2 no.2
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    • pp.151-156
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    • 1992
  • Using $Ba(OH)_2{\cdot}8H_2O, \;Sr(OH)_2{\cdot}8H_2O$ and $Ti(i-OC_3H_7)_4$, fine $(Ba_{1-x}, \;Sr_{x})TiO_3$ powders were synthesized through sol-gel process. The particle size of the powders calcined at $700^{\cric}C$ proved to be 20-40nm by the observation of TEM micrographs and measurement of BET specific surface area. The analysis of XRD patterns showed that the phase of the powders was cubic, and it was identified with the lattice parameters determined through XRD patterns and the shift of (112) peaks that the solid solution powders were synthesized. It was expected through the analysis of relative ratio of cations and the uniformity of compositions in the powders examined by EDAX analysis and relative dielectric constant measurements for sintered body that the distribution of cations was uniform in particle unit.

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