• Title/Summary/Keyword: 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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Optical Transparency and Microstructure of $TiO_2-SiO_2$ Binary Aerogels ($TiO_2-SiO_2$ 이성분계 Aerogel의 광학적 투명성과 미세구조)

  • 이종혁;최수영;김창은;김구대;이해욱
    • Journal of the Korean Ceramic Society
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    • v.32 no.3
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    • pp.321-330
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    • 1995
  • Homogeneous and monolithic TiO2-SiO2 binary aerogels were prepared by supercritical drying. Optical transparency was increased with adding acid catalyst during two step hydrolysis and with decreasing water content. These differences in optical transparency were related to microstructures of gel network formed through polycondensation reaction during supercritical drying process, rather than the final composition of aerogel.

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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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Optimum process conditions for supercritical fluid and co-solvents process for the etching, rinsing and drying of MEMS-wafers (초임계 유체와 공용매를 이용한 미세전자기계시스템 웨이퍼의 식각, 세정을 위한 최적공정조건)

  • Noh, Seong Rae;You, Seong-sik
    • Journal of the Semiconductor & Display Technology
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    • v.16 no.3
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    • pp.41-46
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    • 2017
  • This study aims to select suitable co-solvents and to obtain optimal process conditions in order to improve process efficiency and productivity through experimental results obtained under various experimental conditions for the etching and rinsing process using liquid carbon dioxide and supercritical carbon dioxide. Acetone was confirmed to be effective through basic experiments and used as the etching solution for MEMS-wafer etching in this study. In the case of using liquid carbon dioxide as the solvent and acetone as the etching solution, these two components were not mixed well and showed a phase separation. Liquid carbon dioxide in the lower layer interfered with contact between acetone and Mems-wafer during etching, and the results after rinsing and drying were not good. Based on the results obtained under various experimental conditions, the optimum process for treating MEMS-wafer using supercritical CO2 as the solvent, acetone as the etching solution, and methanol as the rinsing solution was set up, and MEMS-wafer without stiction can be obtained by continuous etching, rinsing and drying process. In addition, the amount of the etching solution (acetone) and the cleaning liquid (methanol) compared to the initial experimental values can be greatly reduced through optimization of process conditions.

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A Study on the Preparation and Characterization of $TiO_2-SiO_2$ Aerogels by Supercritical Drying (Supercritical Drying에 의한 $TiO_2-SiO_2$ 이성분계 Aerogel의 제조 및 그 특성분석)

  • 김창은;이종혁;김구대;이해욱
    • Journal of the Korean Ceramic Society
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    • v.31 no.6
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    • pp.623-628
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    • 1994
  • TiO2-SiO2 homogeneous sol was prepared by means of complexing titanium iso-propoxide with acetylacetone. Crack-free, monolithic binary TiO2-SiO2 aerogels were obtained by evacuating the solvent under the pressure of 2,200 psi at 28$0^{\circ}C$, which was determined as a supercritical condition. The microstructure of the binary aerogels was observed to be finer and more homogeneous as the Ti content decreased. The microstructure was related to the optical transition of aerogels from opaque to transluscent.

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Preparation of Alumina Powders Using Supercritical Drying and Fluid Method (초임계 건조 및 유체법에 의해 알루미나 분말의 제조)

  • Lim, Dae-Young;Hong, Seok-Hyoung;Jung, Yong-Jin;Park, Sang-Jun;Cho, Seung-Beom
    • The Journal of Engineering Research
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    • v.4 no.1
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    • pp.87-91
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    • 2002
  • Nano-size Alumina powders were prepared by heat treatments which were products obtained using supercritical drying and fluid method. Al-isopropoxide dispersed in ethylene glycol as solvents were used as starting materials. The alumina powders were made by supercritical drying fluid method at Autoclave, those were characterize examined closely by XRD, SEM and TG-DTA. The powders were transformed $\alpha-A12O3$ in new route after heat treatment.

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Drying Characteristics of Apple Slabs after Pretreatment with Supercritical CO2

  • Lee, Bo-Su;Choi, Yong-Hee;Lee, Won-Young
    • Preventive Nutrition and Food Science
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    • v.16 no.3
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    • pp.261-266
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    • 2011
  • Supercritical $CO_2$ pretreatment before dehydration leads to a faster dehydration rate. The best supercritical $CO_2$ pretreatment conditions for the most effective dehydration were $45^{\circ}C$, 25 MPa and $55^{\circ}C$, 25 MPa. Increasing pressure of the supercritical $CO_2$ pretreatment system tended to accelerate the dehydration rate more than increasing temperature did. Samples pretreated at higher temperatures and pressures showed greater shrinking and pore distribution on scanning electron microscopy. Control samples maintained their cell walls, whereas samples pretreated at higher temperatures and pressures showed more cell disruption, and more pores were observed. Pore sizes of control and pretreated samples were about 100 and $70{\sim}80\;{\mu}m$, respectively. Samples pretreated at higher temperatures and pressures had smaller pores and a denser distribution.

Enhancement in the Textural Properties and Hydrophobicity of Tetraethoxysilane-based Silica Aerogels by Phenyl Surface Modification

  • Dhavale, Rushikesh P.;Parale, Vinayak G.;Kim, Taehee;Choi, Haryeong;Kim, Younghun;Lee, Kyu-Yeon;Jung, Hae-Noo-Ree;Park, Hyung-Ho
    • Journal of the Microelectronics and Packaging Society
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    • v.27 no.2
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    • pp.27-32
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    • 2020
  • Robust and hydrophobic tetraethoxysilane (TEOS) based silica aerogel was synthesized by supercritical alcohol drying with surface modification using the phenyl based silica co-precursor (PTMS). The aerogels were synthesized by hydrolysis and polycondensation reaction in which TEOS and PTMS in methanol were reacted together in presence of oxalic acid and ammonium hydroxide as the catalysts. Supercritical alcohol dried PTMS/TEOS composite silica aerogel were examined for the hydrophobicity, chemical interaction, surface morphology, and textural characteristics. The hydrophobic silica-based aerogels were characterized by Fourier transform infrared spectroscopy to investigate the presence of functional groups and chemical bonds. The prepared silica demonstrates hydrophobicity (76°-149°), a high specific surface area (398 ㎡/g to 739 ㎡/g). The present investigation provides a simple approach to synthesize hydrophobic and thermally stable silica aerogels.

Capsule Free Hot Isostatic Pressing of Ceria-Doped Tetragonal Zirconia Powder Crystallized in Supercritical Methanol

  • Shu Yin;Satoshi Uehida;Yoshinobu Fujishiro;Mamoru Ohmori;Tsugio Sato
    • The Korean Journal of Ceramics
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    • v.5 no.1
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    • pp.73-77
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    • 1999
  • Capsule free hot isostatic pressing (HIPing) of 12 mol% $CeO_2-88 mo% ZrO_2 (12CeO_2-88ZrO_2)$ powder was conducted at 1100~$1200^{\circ}C$ using the powder crystallized in supercritical methanol followed by supercritical drying. Porous $12CeO_2-88ZrO_2$ ceramics with ~35% open porosity, micropore diameter of ~23 nm and a narrow pore size distribution were fabricated by capsule free hot isostatic pressing at $1100^{\circ}C$. The porosity increased with decrease in HIPing temperature and was accompanied by a steady decrease in fracture strength.

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Preparation and Characterization of Opacified Silica Aerogels Doped by TiO$_2$ (TiO$_2$ 첨가에 의한 불투명한 실리카 에어로겔의 합성 및 특성화)

  • 손봉희;현상훈
    • Journal of the Korean Ceramic Society
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    • v.36 no.2
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    • pp.159-166
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    • 1999
  • The physical properties and microstructural changes with heat-treatment of opacified silica aerogels doped by TiO2 were investigated. Monolithic SiO2-TiO2 aerogels were prepared by supercritical drying (25$0^{\circ}C$, 1250 psig) of wet gel obtained by adding titanium isopropoxide to prehydrolyzed TEOS-isopropanol solutions. The density and the porosity of SiO2-10 mol% TiO2 aerogels were 0.23 g/㎤ and 90%, respectively. During supercritical drying, the linear shrinkage of aerogels increased with increase in the titanium content an TiO2 was transformed to the anatase phase as well as particls agglomerates led to TiO2 clusters of 100~800 nm dispersed homogeneoulsy in the silica matrix. The IR transmittance of opacified silica aerogels was very low in the region of wavelengths below 8 ${\mu}{\textrm}{m}$ compared with pure silica aerogels and SiO2-TiO2 aerogels showed the high thermal stability of microstructures up to $600^{\circ}C$.

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