• Title/Summary/Keyword: tetraethoxysilane

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Novel Silica Nanotubes Using a Library of Carbohydrate Gel Assemblies as Templates for Sol-Gel Transcription in Binary Systems

  • Jung, Jong-Hwa;Lee, Shim-Sung;Shinkai, Seiji;Iwaura, Rika;Shimizu, Toshimi
    • Bulletin of the Korean Chemical Society
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    • v.25 no.1
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    • pp.63-68
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    • 2004
  • Sugar-based gelator p-dodecanoyl-aminophenyl- ${\beta}$-D-aldopyranosides (1-3) have been shown to self-assemble in the presence of p-aminophenyl aldopyranosides. The hydrogel 1+4 showed the double-helical structure with 3-25 nm outer diameters, which is quite different from that of 1. The gel 2+5 revealed twisted ribbon structure with 30-50 nm in widths and a few micrometers of length whereas the gel 3+4 revealed the single and the bundled fiber structures. The difference in these gel supramolecular structures has successfully been transcribed into silica structures by sol-gel polymerization of tetraethoxysilane (TEOS), resulting in the doublehelical, the twisted-ribbon, the single and the multiple (lotus-shaped) hollow fiber structures. These results indicate that novel silica structures can be created by transcription of various superstructures formed in binary gels through the hydrogen-bonding interaction, and the amino group of the p-aminophenyl aldopyranosides acts as an efficient driving force to create novel silica nanotubes. Furthermore, electron energy-loss spectroscopy (ELLS) provided strong evidence for the inner hollow structure of the double-helical silica nanotube. This is a novel and successful example that a variety of new silica structures can be created using a library of carbohydrate gel fibers as their templates.

Properties of Zeolite Nanopowder Coated with Titanium Dioxide by Atomic Layer Deposition

  • Lee, Bo Kyung;Ok, Hae Ryul;Bae, Hye Jin;Kim, Hyug Jong;Choi, Byung Ho
    • Korean Journal of Materials Research
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    • v.26 no.3
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    • pp.149-153
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    • 2016
  • Nanosized zeolites were prepared in an autoclave using tetraethoxysilane (TEOS), tetrapropylammonium hydroxide (TPAOH), and $H_2O$, at various hydrothermal synthesis temperatures. Using transmission electron microscopy and particle size analysis, the nanopowder particulate sizes were revealed to be 10-300 nm. X-ray diffraction analysis confirmed that the synthesized nanopowder was silicalite-1 zeolite. Using atomic layer deposition, the fabricated zeolite nanopowder particles were coated with nanoscale $TiO_2$ films. The $TiO_2$ films were prepared at $300^{\circ}C$ by using $Ti[N(CH_3)_2]_4$ and $H_2O$ as precursor and reactant gas, respectively. In the TEM analysis, the growth rate was ${\sim}0.7{\AA}/cycle$. Zeta potential and sedimentation test results indicated that, owing to the electrostatic repulsion between $TiO_2$-coated layers on the surface of the zeolite nanoparticles, the dispersibility of the coated nanoparticles was higher than that of the uncoated nanoparticles. In addition, the effect of the coated nanoparticles on the photodecomposition was studied for the irradiation time of 240 min; the concentration of methylene blue was found to decrease to 48%.

Preparation and Gas Permeation Properties of Polyimide-Silica Hybric Memberanes (폴리이미드-실리카 하이브리드막의 제조와 기체투과특성)

  • 염승호;정용수;이우태;김선일;김진환
    • Membrane Journal
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    • v.11 no.3
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    • pp.116-123
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    • 2001
  • Polyimide-silica hybrid membranes were prepared and the effect of silica content on the structural properties and the gas transport properties was studied. The hybrid membranes were obtained by the sol-gel process starting from 1,2,4,5-benzenetetracarboxylic dianhydride(PMDA), 4,4`-diamino- diphenyl oxide(ODA) and tetraethoxysilane(TEOS) in N,N` dimethylacetatmide (DMAc) solvent. The structural characterizations of the membrane were performed by FT-IR, EDX, TGA and SEM. The gas permeation experiments with ${N_2}, {O_2}, {H_2}, {CO_2}and ${CH_4}$ were carried out at the temperature of $25^{\circ}C$ and in the range of pressure from 3atm to 7atm. the hybrid membranes showed higher thermal stability than PI membranes. The silica patricles were uniformly embedded in the polyimide matrix and the size of silica particles increased with increasing silica content. The permeability coefficients of ${N_2}, {O_2}, {H_2}, {CO_2}and ${CH_4}$ increased with increasing silica content but the diffusion coefficients might appear to be a result of a solubility enhancement. In spite of the permeability enhancement, an increase in the selectivities of ${H_2}/{N_2}, ${H_2}/{O_2} and ${H_2}/{CO_2} was observed.

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BPSG 및 PSG CVD 공정 중 발생하는 오염입자 발생특성

  • Na, Jeong-Gil;Mun, Ji-Hun;Choe, Hu-Mi;Kim, Tae-Seong;Choe, Jae-Bung;Im, Seong-Gyu;Park, Sang-Hyeon;Lee, Heon-Jeong;Go, Yong-Gyun;Lee, Sang-Mi;Yun, Ju-Yeong;Gang, Sang-U
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.261-261
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    • 2010
  • 본 연구에서는 PBMS (Particle Beam Mass Spectrometer)와 ISPM (In-Situ Particle Monitor)을 연계하여 BPSG (Borophosphosilicate Glass) 및 PSG (Phosphosilicate Glass) 박막 증착을 위한 CVD (chemical vapor deposition) 공정 중 발생하는 오염입자 발생특성에 대해 비교 평가하였다. 소스는 TEB (Triethylborate), TEPO (Triethylphosphate) 및 TEOS (Tetraethoxysilane)를 사용하였고, 운반가스 및 반응가스로 He과 $O_2$$O_3$를 사용하였다. 증착온도와 압력은 각각 $450^{\circ}C$, 200 Torr 이었다. 반응기의 배기라인에 PBMS와 ISPM을 설치하고 500 nm 이하의 입자에 대해 공정단계별 시간에 따른 모니터링 결과 전 공정에 걸쳐 동일한 패턴의 입자발생분포를 보였으며, 특히 PBMS의 경우 ISPM의 입자측정한계인 260 nm 이하의 입자크기도 측정할 수 있었다. 입자발생이 안정적으로 일어나는 증착공정 중 PBMS를 통하여 입자크기를 측정한 결과 BPSG의 경우 약 110 nm, PSG의 경우 약 80 nm의 분포를 나타내었다. 이를 통해 TEB 소스가 배제된 PSG의 경우 BPSG의 경우보다 입자의 성장이 지체됨을 확인하였다. 측정에 대한 신뢰성을 확보하기 위해 PBMS 내의 TEM (Transmission Electron Microscopy) grid를 이용하여 입자를 샘플링 하였고, TEM 분석을 실시한 결과 PBMS 측정결과와 잘 일치하였다. 또한 EDS (Energy Dispersive Spectroscopy) 분석을 통하여 입자성분에 대해 검증하였다.

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Synthesis of Imogolite by a Hydrothemal Method (이모골라이트의 합성)

  • Jang, Young-Nam;Ryu, Gyoung-Won;Suh, Yong-Jae;Chae, Soo-Chun;Bae, In-Kook
    • Journal of the Mineralogical Society of Korea
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    • v.21 no.3
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    • pp.283-287
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    • 2008
  • The imogolite synthesis wore performed by using tetraethoxysilane (TEOS) and aluminium-sec-butoxide (ASB) at < $100^{\circ}C$. A mixure of TEOS and ASB in a molar ratio of 1:2 was prepared under vigorous stirring and the experiments were performed under the hydrothemal refluxing condition. When the concentration of TEOS and ASB in solution was 0.5 M, a well-crystallized imogolite was synthesized, and the reflections wore shown at d = 22.4, $9.5\;\AA$ etc., after XRD analysis. DTA analysis shows 2 exothemal peaks at 68 and $249^{\circ}C$, suggesting the dehydration and the dehyroxylation reaction, respectively. The result of TG indicates 41% weight loss. And the weak and unsymmetrical peaks by the Si-O-Al stretching vibrations at 953 and $993cm^{-1}$ and by O-Si-O bending vibration at $562cm^{-1}$ were observed after IR analysis. The synthetic imogolite was fibrous and shows a spiders web like network structure.

규산나트륨을 이용한 졸-겔 구형 $SiO_2$ 나노졸 합성 연구

  • Gwon, Il-Jun;Park, Seong-Min;Kim, Myeong-Sun;Sim, Ji-Hyeon;Yeom, Jeong-Hyeon
    • Proceedings of the Korean Society of Dyers and Finishers Conference
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    • 2012.03a
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    • pp.111-111
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    • 2012
  • 나노테크놀로지는 종래의 가공으로는 얻기 힘들었던 섬유가공 효과를 간단하게 할 수 있는 기술이다. 현재 각국의 기능성 나노 가공제를 섬유에 응용하는 나노 테크놀로지는 현재 공업 생산되고 있는 면, 모, 견 등의 천연섬유 및 polyester, Nylon 등의 합성섬유의 원단에 적용하는 데서 출발하고 있다. 이러한 나노기술은 기존의 설비와 물을 사용하는 것이 큰 특징이고, 특별한 기계장치가 필요하지 않으며, 소규모의 실험장비만 있어도 현장투입이 가능한 나노입자의 제조가 가능하기 때문에 대량생산이 용이하고 설비투자는 원칙적으로 필요하지 않는다. 또한, 나노입자의 분산을 제대로 시키면 그 사이즈가 빛의 가시광선 영역의 파장(400~800nm)에 비해 절반 수준이하 크기의 입자가 대부분을 차지하기 때문에 염색성, 태의 변화가 적어 앞으로 더욱더 나노테크놀로지에 의한 가공이 확대될 것이 예상된다. 특히 유 무기 하이브리드 재료는 용액상태에서 제조되기 때문에 용액 코팅공정의 적용이 가능하여 다양한 코팅에 적극적으로 활용되고 있다. 또한 코팅공정 온도가 상대적으로 낮아서, 유기물의 기능성 발현이 용이하며, 섬유가공에 그대로 적용이 가능하고, 섬유고분자와 내구성 있게 직접 결합이 되어 실용성이 높다 할 수 있다. 또한 나노졸의 형성 시, 혹은 나노졸에 기능성 물질을 첨가함으로서 나노졸과 기능성 물질을 복합화하여 섬유상에 부여하는 것도 가능하다. 최근에 실리카졸의 형성과 성장에 관한 연구는 졸-겔 기술의 발전과 해석 및 상용화에 집중되어 있다. 규산나트륨과 황산 또는 염산을 사용하여 실리카를 생성하는 공정은 tetraethoxysilane (($Si(OC_2H_5)_4$, (TEOS))를 이용하여 합성하는 방법과 달리 대량의 실리카를 경제적으로 생산하는데 방법으로 널리 연구되고 있지만, 많은 연구가 수행되었음에도 불구하고 실리카 졸의 특성, 성장, 제조에 대한 충분한 이해가 이루어 지지 않고 있어, 아직까지 나노크기의 입자를 제조하는 공정에 대해서는 경제성, 효율성, 품질의 균일성이 떨어지는 것이 현실이다. 따라서 본 연구에서는 앞서 연구된 졸-겔 합성기술과 저렴한 원료인 규산나트륨을 이용하여 보다 간단하고 경제적인 방법으로 고부가가치의 다양한 실리카 나노졸을 제조할 수 있는 연구를 하고자 하였다. 이를 위해 규산나트륨 수용액의 특성, 핵 생성에 필요한 규산나트륨 수용액의 산화반응 특성, 그리고 출발용액의 졸겔 반응을 기초로 하여 실리카 졸 형성에 대한 반응물질의 혼합방법, 반응온도, 반응물의 농도, pH등이 최종 실리카 나노졸 제품의 입자 크기와 모양 등에 미치는 영향을 조사하려고 하며 이를 토대로 다양한 크기와 특성을 가진 실리카 나노졸을 제조하였다.

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Synthesis of Nanostructured Si Coatings by Hybrid Plasma-Particle Accelerating Impact Deposition (HP-PAID) and their Characterization (하이브리드 플라즈마 입자가속 충격퇴적(Hybrid Plasma - Particle Accelerating Impact Deposition, HP-PAID) 프로세스에 의한 Si 나노구조 코팅층의 제조 및 특성평가)

  • 이형직;권혁병;정해경;장성식;윤상옥;이형복;이홍림
    • Journal of the Korean Ceramic Society
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    • v.40 no.12
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    • pp.1202-1207
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    • 2003
  • Using a recently developed Hybric Plasma-Particle Accelerating Impact Deposition (HP-PAID) process, synthesis of nanostructured silicon coatings has been investigated by injecting vapor-phase TEOS (tetraethosysilane, (C$_2$H$\_$5/O)$_4$Si) into an Ar hybrid plasma. The plasma jet with reactants was expanded through nozzle into a deposition chamber, with the pressure dropping from 700 to 10 torr. Ultrafine particles accelerated in the free jet downstream of the nozzle, deposited by an inertial impaction onto a temperature controlled substrate. By using this process, nanostructured amorphous silicon coatings with grain size smaller than 10 nm could be synthesized. These samples were annealed in an Ar and crystallized at 900$^{\circ}C$ for 30 min. TEM analysis showed that the annealed coatings were also composed of nanoparticles smaller than 10 nm, which showed a good consistency that the average grain size of 7 nm was also estimated from a peak shift of 2.39 cm$\^$-1/ and Full Width at Half Maximum (FWHM) 5.92 cm$\^$-1/ of Raman analysis. The noteworthy is that a strong PL peak at 398 nm was also obtained for this sample, which indicates that the deposited coatings also contained 3∼4 nm nanostructured grains.

Synthesis of New Black Pigment; Carbon Black Pigment Capsulated into the Meso-pore of Silica as Black Pigment in Cosmetic (새로운 Black Color의 합성;화장품에서 블랙 색소로서 Meso-pore Silca에 캡슐레이션된 Carbon-black Silica)

  • Hye-in, Jang;Kyung-chul, Lee;Hee-chang , Ryoo
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.30 no.2
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    • pp.189-195
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    • 2004
  • Carbon black have not been used as pigment material in cosmetic because of very low density and dispersity, but carbon black have applicable character as black pigment because of non-toxic, stable physico-chemical property, and black colority. In this study, mesoporous silica samples were synthesized by sol-gel reaction using surfactants-template method; TEOS (tetraethoxysilane) - a) PEO/lecithin, b) PEO/polyethylene glycol, c) lecithin/polyethylene glycol in ethanol/water solution. Synthesized organic-inorganic hybrid - silica were heat-treated in N2 condition at 500$^{\circ}C$. Mesoporous silica with black carbon in pore have the effective density and show the good dispersity in both hydrophilic and hydrophobic solvent. Properties of the samples were measured; specific surface area (750㎡/g) and pore size (4-6nm) using BET, pore structure (cylindrical type) using XRD, morphology (spherical powder with 0.1-0.5$\mu\textrm{m}$ partical size) of the samples using SEM. Carbon-silica black color applied to mascara, it shows a dark black colority and good dispersity as compared with the general black color titania pigment. Moreover, it is possible to control the density of black color pigment because it is possible to control pore volume and particle size of mesoporous silica properly. It show the good volume effects in mascara. That is why possible to apply all kinds of cosmetic products.