• Title/Summary/Keyword: Sol-gel supercritical drying

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Low Pressure Synthesis of Silica Aerogels by Supercritical Drying (초임계 건조에 의한 실리카 에어로겔의 저압 합성)

  • 김동준;현상훈
    • Journal of the Korean Ceramic Society
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    • v.33 no.5
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    • pp.485-494
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    • 1996
  • Silica Aerogels with the density and porosity of 0.1g/cm3 and 96% were synthesized by two different supercri-tical drying processes (i.e additional solvent and intial pressure methods) Isoptopanol was chosen as sol-gel and supercritical drying solvents in order to synthesize aerogels at the lower temperature and pressure because the critical values of isopropanol are lower than those of methanol and ethanol commonly used. The P-V-T relationship of isopropanol was experimentally described for optimizing supercritical drying conditions such as the amount of extra solvent and supercritical drying temperature and pressure. In the addional solvent method monolithic and transparent aerogels were obtained by supercritical drying at 25$0^{\circ}C$ and 900 psing after 40% of the reactor volume was filled with isopropanol. Crack-free aerogels were synthesized at 25$0^{\circ}C$ and 1100~1200 psig by the initial pressure method with an intial nitrogen gas pressure of 400 psig and the isopropanol amount of 5% of the reactor volume.

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Surface Modification of Silica Aerogels (실리카 에어로겔의 표면 개질)

  • 현상훈;이찬호;김동준
    • Journal of the Korean Ceramic Society
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    • v.33 no.12
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    • pp.1319-1324
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    • 1996
  • Silica aerogels were synthesis by the sol-gel-supercritical drying process using isopropanol as a solvent. Effets of the heat-treatment and the surface modification through propoxylation on the structural reinforcement as well as the surface hydrophobic/hydrophilic characteristics of aerogels were investigated. Silica aerogels synthesized by supercritical drying were hydrophobic but aerogels heat-treated above 20$0^{\circ}C$ were transformed to be hydrophilic. In particular it was found that the skeletal structure of aerogels heat-treated at 50$0^{\circ}C$ was strong enough not to crack after adsorbing a large amount of water vapor. Hydrophilic aerogels modified by propoxylation at 28$0^{\circ}C$ for 20 h were reversed to the hydrophobic form. Transition between hydrophobicity and hydrophilicity was reversible. The hydrophobicvity and the hydrophilicity of silica aerogels were attributed to the Si-Oh bond and the nonpolar C-H bond groups of orgainc species respectively.

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The Synthesis of Silica Aerogel in the Macroporous Ceramic Structure by Sono-gel Process and Supercritical Drying Process (초음파 겔화 공정과 초임계 건조 공정을 이용한 다공성 세라믹스 구조체 내부에 실리카 에어로겔 합성)

  • Hong, Sun-Wook;Song, In-Hyuck;Park, Young-Jo;Yun, Hui-Suk;Hwang, Ki-Young;Rhee, Young-Woo
    • Journal of the Korean Ceramic Society
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    • v.47 no.6
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    • pp.553-559
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    • 2010
  • The synthesis behavior of nanoporous silica aerogel in the macroporous ceramic structure was observed using TEOS as a source material and glycerol as a DCCA(dry control chemical additive). Silica aerogel in the macroporous ceramic structure were synthesized through a sono-gel process. The wet gel in the macroporous ceramic structure were aged in ethanol for 72 h at $50^{\circ}C$. The aged wet gel was dried under supercritical drying condition. The addition of glycerol has a role of giving the uniform pore size distribution. The reproducibility of aerogel in the macroporous ceramic was improved in the glycerol(0.05 mol%) added to the silica sol and TEOS : $H_2O$=1 : 12.

Synthesis and Characterization of Type-VI Silica by Sol-Gel Method (졸-겔법을 이용한 Tape-VI형 실리카 에어로겔의 제조 및 특성분석)

  • 김성철;최대원;최용수;이종혁;이해욱;김창은
    • Journal of the Korean Ceramic Society
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    • v.35 no.3
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    • pp.264-272
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    • 1998
  • The effect of catalytic condition on the properties of SiO2 aerogels has been investigated and then the dri-ed aerogels were partially densified to induce mechanical strength by heat treatment in order to prepare Type-VI silica by Sol-Gel method. Aerogel made by 1-step base process had the highest skeletal density lowest shrinkage and the smallest particle size. But in case of using acid catalyst in both 1st and 2nd step had the lowest skeletal density highest shrinkage and the largest particle size The aerogel synthesized by 1-step base process was most transparent because of its homogeneous microstructure. During heat treatments cracks occurred below 200$^{\circ}C$ for aerogel with the skeletal density lower than 1.9 g/cm3 but the with the higher skeletal density did not cracked up to 800$^{\circ}C$ shrinkage and skeletal density increased as heating temperature increased due to condensation and viscous sintering mechanism.

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Elastic and Superhydrophobic Monolithic Methyltrimethoxysilane-based Silica Aerogels by Two-step Sol-gel Process

  • Mahadik, D.B.;Jung, Hae-Noo-Ree;Lee, Yoon Kwang;Lee, Kyu-Yeon;Park, Hyung-Ho
    • Journal of the Microelectronics and Packaging Society
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    • v.23 no.1
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    • pp.35-39
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    • 2016
  • The flexible and superhydrophobic properties of silica aerogels are extremely important material for thermal insulation and oil spill cleanup applications for their long-term use. Flexible silica aerogels were synthesized by using a two-step sol-gel process with precursors, methyltrimethoxysilane (MTMS) followed by supercritical drying. Silica aerogels were prepared at different molar ratio of methanol to MTMS (M). It was observed that the silica aerogels prepared at M=28 were monolithic but inelastic in nature, however, for M=35, the obtained aerogels were monolithic, elastic in nature with less shrinkage. The microstructural studies were carried out using scanning electron microscopy and surface area measurements. The hydrophobicity was confirmed by Fourier transform Infrared spectroscopy and water contact angle measurements. The detailed insight mechanism for flexible nature of silica aerogels and hydrophobic behavior were studied.

Mechanical Strength and Thermal Conductivity of Silica Aerogels Opacified by Adding Oxides (산화물 첨가에 의한 불투명화 실리카 에어로겔의 기계작 강도 및 열전도도)

  • 손봉희;김계태;현상훈;성대진
    • Journal of the Korean Ceramic Society
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    • v.36 no.8
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    • pp.829-834
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    • 1999
  • The silica aerogels opacified via adding oxides were prepared by the sol-gel supercritical drying technique and their characteristics of mechanical strength and thermal conduction were investigated. The compressive strength of SiO2-10 mol% TiO2 and SiO2-10mol% Fe2O3 aerogels were 0.11 and 0.047 MP a respectively much higher than 0.025 MPa of pure silica aerogels. The thermal conductivity of silica aerogels opacified by TiO2 was as low as 0.02505 W/m${\cdot}$K at $400^{\circ}C$ It was found that the TiO2 -opacifier for improving mechanical strength and suppressing high temperature conduction of pure silica aerogels was more effective than the Fe2O3 -opacifier

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Mechanical Strength and Thermal Conductivity of Pure/Opacified Silica Aerogels (순수/불투명화 실리카 에어로겔의 기계적 강도 및 열전도도)

  • 현상훈;이찬호;김동준;성대진
    • Journal of the Korean Ceramic Society
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    • v.34 no.9
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    • pp.969-978
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    • 1997
  • The properties of microstructure, hydrophobicity/hydrophilicity, mechanical strength, and thermal conduction of pure/opacified silica aerogels synthesized by the sol-gel supercritical drying technique were investigated. The hydrophobic surface of opacified silica aerogels doped with carbon (0.13 g/cm3 density, 94% porosity, 580 m2/g specific surface area) transformed to hydrophilic surface after heat-treated above 30$0^{\circ}C$. The values of compressive modulus (1.85 MPa) and strength (0.5 MPa) of opacfied silica aerogels were about 20 times higher than those of pure silica aerogels. The mechanical properties of pure silica aerogels heat-treated at $700^{\circ}C$ were also considerably improved without changing their porosity and density. Particularly, compressive modulus and compressive strength of pure silica aerogels GPSed under 100$0^{\circ}C$ and 80 bar were improved 140 and 37 times, respectively. Thermal conductivities of pure/opacified silica aerogels measured at room temperature and 227$^{\circ}C$ were about 0.013 and 0.019 W/m.K, respectively, and were to be found very low value of 0.004 W/m.K below 10 torr pressure at room temperature.

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Ultralow Dielectric Properties of $SiO_2$ Aerogel Thin Films (실리카 에어로겔 박막의 극저 유전특성)

  • 현상훈;김중정;김동준;조문호;박형호
    • Journal of the Korean Ceramic Society
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    • v.34 no.3
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    • pp.314-322
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    • 1997
  • The thin film processing and the applicability as a IMD material of SiO2 aerogels providing ultralow dielec-tric properties were studied. The SiO2 aerogel films with 0.5g/㎤ density (78% porosity) and 4000~21000$\AA$ thickness could be prepared at 25$0^{\circ}C$ and 1160 psig by supercritical drying of wet-gel films, which were spin-coated at the spin rate of 1000~7000 rpm on p-Si(111) wafer under the isopropanol atmosphere. The optimum viscosity of polymeric SiO2 sols for spin coating was in the range of 10~14 cP. The main fac-tors being able to control the film thickness and microstructures were found to be sol concentration, spin rpm, and aging time of wet-gel films. The dielectric constant of the SiO2 aerogel thin film was around 2.0 low enough to be applied to the next generation semiconductor device beyond the giga level.

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Performance Test of $TiO_2$ Catalyst in VOCs Photocatalytic Degradation (VOCs 광촉매 분해용 $TiO_2$촉매제조 및 성능평가)

  • Lee Seung-Bum;Lee Jae-Dong;Park Yoon-Shin
    • Journal of environmental and Sanitary engineering
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    • v.20 no.4 s.58
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    • pp.45-50
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    • 2005
  • Titania gel formations were prepared by sol-gel method using titanium(IV) chloride $(TiCl_4)$, and its characteristics were analyzed by varying the $epoxide/TiCl_4$ ratio and the amount of water In the end, titania $(TiO_2)$ aerogel were prepared using supercritical drying process. VOCs such as benzene, toluene, and m-xylene (BTX) were oxidized using prepared titania aerogel and commercially available $TiO_2$, and its performance was compared. The surface area, pore volume, and average pore diameter of 1,2-epoxybutane are significantly smaller than the propylene oxide. And the titania aerogels with 6 moi of epoxides have high surface areas, pore volumes, and average pore diameters. As a result of photo-oxidation, conversion of benzene was reached about $70\%$, and other reactants were reached about $60\%$ similarly. The conversion of BTX was increased as inlet concentration decreased. The reactivity of titania calcined at $600^{\circ}C$ was greater than $400^{\circ}C$ and $800^{\circ}C$. Water is required as a reactants for the oxidation of VOCs, and the continuous consumption of hydroxyl radicals required replenishments to maintain catalyst activity. The activity ratio increased with increasing reaction time when enough amount of water was present in the reactor.