• Title/Summary/Keyword: TEOS $SiO_2$

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Fabrication of Uniform Hollow Silica Nanospheres using a Cationic Polystyrene Core

  • Yun, Dong-Shin;Jang, Ho-Gyeom;Yoo, Jung-Whan
    • Bulletin of the Korean Chemical Society
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    • v.32 no.5
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    • pp.1534-1538
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    • 2011
  • Uniform, hollow nanosilica spheres were prepared by the chemical coating of cationic polystyrene (cPS) with tetraethylorthosilicate (TEOS), followed by calcination at 600 $^{\circ}C$ under air. cPS was synthesized by surfactant-free emulsion polymerization using 2,2'-azobis (2-methyl propionamidine) dihydrochloride as the cationic initiator, and poly(vinyl pyrrolidone) as a stabilizer. The resulting cPS spheres were 280 nm in diameter, and showed monodispersion. After coating, the hollow silica product was spherically shaped, and 330 nm in diameter, with a narrow distribution of sizes. Dispersion was uniform. Wall thickness was 25 nm, and surface area was 96.4 $m^2/g$, as determined by BET. The uniformity of the wall thickness was strongly dependent upon the cPS surface charge. The effects of TEOS and ammonia concentrations on shape, size, wall thickness, and surface roughness of hollow $SiO_2$ spheres were investigated. We observed that the wall thicknesses of hollow $SiO_2$ spheres increased and that silica size was simultaneously enhanced with increases in TEOS concentrations. When ammonia concentrations were increased, the irregularity of rough surfaces and aggregation of spherical particles were more severe because higher concentrations of ammonia result in faster hydrolysis and condensation of TEOS. These changes caused the silica to grow faster, resulting in hollow $SiO_2$ spheres with irregular, rough surfaces.

Fabrication and Characterization of LPCVD $P_2O_5-SiO_2$ Films for Inegrated Optics (1) -LPCVD of TEOS and TMPite (LPCVD $P_2O_5-SiO_2$ 집적광학박막의 제작 및 특성 연구(1) -TEOS와 TMPite의 LPCVD-)

  • 정환재
    • Korean Journal of Optics and Photonics
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    • v.4 no.3
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    • pp.266-275
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    • 1993
  • We made $P_2O_5-SiO_2$ films on silicon for integrated optics application by low pressure chemical vapor deposition using TEOS (tetraethylorthosilicate) and TMPite (trimethylphosphite) and studied the deposition characteristics. The activation energy of the reaction was changed from 54.6 kcal/mole to 39.2 kcal/mole by incorporating the TMPite into the reaction of TEOS. The deposition rate and the P concentration of films increased in proportion to the flow of TMPite. As the deposition temperature increased, the deposition rate of the films increased but the P concentration decreased. The fabricated films showed the increase of refractive index of 0.0019 per 1 wt% of P concentration. The nonuniformity of films was ${\pm}$7% in thickness and ${\pm}$0.5wt% in P concentration and we showed this'nonuniformity is due to the nonuniform transport of TMPite. The films of more than 10wt% P concentration developed phosphoric acid on its surface when exposed to air for long time.

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An Experimental Study on Composition Characteristics of SiO$_2$/TiO$_2$/Multicomponent Particle Generated in a Coflow Diffusion Flame (화염중 발생하는 SiO$_2$/TiO$_2$/다성분입자의 조성특성에 관한 실험적 연구)

  • Kim, Tae-O;Seo, Jeong-Su;Choe, Man-Su
    • Transactions of the Korean Society of Mechanical Engineers B
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    • v.25 no.9
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    • pp.1175-1182
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    • 2001
  • Chemical compositions of polydisperse SiO$_2$/TiO$_2$multicomponent aggregates were measured for different heights from the burner surface and different mobility diameters of aggregates. SiO$_2$/TiO$_2$multicomponent particles were generated in a hydrogen/oxygen coflow diffusion flame from two sets of precursors: TTIP(titanium tetraisopropoxide), TEOS(tetraethylorthosilicate). To maintain 1:1 mole ratio of TTIP:TEOS vapor, flow rate of carrier gas $N_2$was fixed at 0.6lpm for TTIP, at 0.1lpm for TEOS. In-situ sampling probe was used to supply particles into DMA(differential mobility analyzer) which was calibrated with using commercial DMA(TSI, model 3071A) and classifying monodisperse multicomponent particles. Classified monodisperse particles were collected with electrophoretic collector. The distributions of composition from particles to particle were determined using EDS(energy dispersive spectrometry) coupled with TEM(transmission electron microscope). The chemical(atomic) compositions of classified monodisperse particle were obtained for different heights; z=40mm, 60mm, 80mm. The results suggested that the chemical(atomic) composition of SiO$_2$decreased with the height from burner surface and the composition of SiO$_2$and TiO$_2$approached to the value of 1 to 1 fat downstream. It is also found that the composition of SiO$_2$decreases as the mobility diameter of aggregate increases.

An Experimental Study on Composition Characteristics of $SiO_2/TiO_2$ Multicomponent Particle in Coflow Diffusion Flame (화염중 발생하는 $SiO_2/TiO_2$ 다성분입자의 조성특성에 관한 실험적 연구)

  • Kim, Tae-Oh;Suh, Jeong-Soo;Choi, Man-Soo
    • Proceedings of the KSME Conference
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    • 2000.04b
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    • pp.441-446
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    • 2000
  • Chemical compositions of monodisperse $SiO_2/TiO_2$ multicomponent aggregates were measured for different heights from the burner surface and different mobility diameters of aggregates. $SiO_2/TiO_2$ multicomponent particles were generated in a hydrogen/oxygen coflow diffusion flame from two sets of precursors: TTIP (titanium tetraisopropoxide), TEOS(tetraethylorthosilicate). To maintain 1:1 mole ratio of TTIP:TEOS vapor theoretically, flow rate of carrier gas $N_2$ was fixed at 0.61pm for TTIP, at 0.11pm for TEOS. In situ sampling probe was used to supply particles into differential mobility analyzer(DMA) which was calibrated with using commercial DMA(TSI 3071A) and classifying monodisperse multicomponent particles. Classified particles were collected with electrophoretic collector. The distributions of composition from particle to particle were determined using EDS (energy dispersive spectrometry) coupled with TEM (transmission electron microscope). The chemical (atomic) compositions of classified monodisperse particle were obtained for different heights; z=40mm, 60mm, 80mm. The results suggested that the atomic composition of $SiO_2$ decreased with the height from burner surface and the composition of $SiO_2$ and $TiO_2$ approached to the value of 1 to 1 in far downstream. It is also found that the composition of $SiO_2$ decreases as the mobility diameter of aggregate increases.

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냉음극 변압기 플라즈마와 TEOS 소스를 이용한 $SiO_2$ 박막 증착

  • Lee, Je-Won;No, Gang-Hyeon;Song, Hyo-Seop;Kim, Seong-Ik;Lee, Eun-Ji;Lee, Se-Hui;Jo, Gwan-Sik
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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    • pp.164-164
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    • 2012
  • 저진공 (>100 mTorr)에서 냉음극 변압기 전원 소스를 이용하여 플라즈마를 발생시키는 시스템을 개발하였다. 또한 이 장치를 이용하여 Tetraethylorthosilicate (TEOS)를 기화시켜 이산화규소 ($SiO_2$) 박막 증착 기술을 연구하였다. 공정 압력은 400~1,000 mT이었다. 증착된 박막의 박막 두께, 굴절률 등의 측정을 실시하였다. 결과를 요약하면, 플라즈마 공정 압력이 증가함에 따라 박막 증착 속도는 약 200~300 A/min이었다. 또한 전압이 1,100에서 2,100 V로 증가함에 따라 산화막의 증착 속도는 약 300에서 40 nm/min으로 증가하였다. TEOS만을 사용하였을 때 굴절률은 약 1.5~1.6정도였다. 그러나 TEOS에 산소를 추가하면 자연 산화막의 굴절률인 1.46을 쉽게 얻을 수 있었다. 초기 연구 결과를 정리하면 냉음극 변압기 플라즈마 장치는 향후 실용적인 산화막 플라즈마 증착 연구 장치로 사용될 수 있을 것으로 생각된다.

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Porous silica ceramics prepared by sol-gel process-Effect of $H_2O/TEOS$ molar ratio- (솔-젤법에 의한 다공성 실리카 세라믹스의 제조-$H_2O/TEOS$ 몰비의 영향-)

  • Lee, Jin-Hui;Kim, Wha-Jung;Lee, Joon
    • Journal of the Korean Ceramic Society
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    • v.34 no.2
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    • pp.216-224
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    • 1997
  • Porous silica ceramics were prepared(with HCI catalyst) using H2O/TEOS molar ratios of 2.6~59.0, with the EtOH/TEOS ratio fixed. After preparing 9 kinds of sol, the followings were investigated; measurement of the gelation time, thermal analyses by TG/DTA, property analyses of the intermediates by FT-IR and X-ray diffractometry with dried samples, analyses of SiO2 polymer by FT-IR, the investigation of specific sur-face area and pore size distribution by N2-adsorption isotherm, and structural change of SiO2 polymer and pore morphology by TEM observation, with samples heat-treated to 50$0^{\circ}C$. In the concentrations of in-vestigated compositions and catalyst, gelation time showed a minimum at ca. 11 moles of water per one mole of TEOS, the highest degree of polymerization at ca. 8-18 moles, and the largest specific surface area at ca. 11 moles, which means that the polymerization proceeded fastest at ca. 11 moles of water. In con-clusion, the more water used, the faster the polymerization reaction up to ca. 11 moles, but more than ca. 11 moles of water caused retardation of gelation and resultant reduction of specific surface area.

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Synthesis of Monodispersed and Spherical $SiO_2-coated Fe_2O_3$ Nanoparticle

  • Han, Yang Su;Yun, Seon Mi;Kim, Dong Guk
    • Bulletin of the Korean Chemical Society
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    • v.21 no.12
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    • pp.1193-1198
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    • 2000
  • The preparation of nanocrystalline hematite, ${\alpha}-Fe_2O_3$, paricles and their surface coating with silica layers are described. The hematite particles with the size of 30~60 nm are firstly prepared by thermal decomposition of trinuclear acetate-hydroxo iron (III) nitrate complex, $[Fe_3$(OCOCH_3)_7$OH${\cdot}$2H_2O]NO_3$, at $400^{\circ}C$. Subsequently the hematite surfaces are coated with siliva layers by a controlled hydrolysis and condensation reaction of TEOS with varying the TEOS concentration and pH. Monodispersed and spherical $SiO_2-coatedFe_2O_3$ particles with the average particle diameter of ~90 nm and extremely narrow size distribution can be obtained at the pH of 11 and the TEOS concentration of 0.68M, which are found to be the optimum conditions in the present study in achieving the homogeneous deposition of silica layers on hematite surfaces. Diffuse reflectance UV-Vis spectra reveal that the characteristic optical reflectance of ${\alpha}-Fe_2O_3$ particles is preserved almost constant even after coating the surfaces, suggesting that the $SiO_2$ layers can be regarded as protecting layers without degrading the optical properties of hematite particles.

Effect of the C/Si Molar Ratio on the Characteristics of β-SiC Powders Synthesized from TEOS and Phenol Resin (C/Si 몰 비가 TEOS와 페놀수지를 출발원료 사용하여 합성된 β-SiC 분말의 특성에 미치는 영향)

  • Youm, Mi-Rae;Park, Sang-Whan;Kim, Young-Wook
    • Journal of the Korean Ceramic Society
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    • v.50 no.1
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    • pp.31-36
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    • 2013
  • ${\beta}$-SiC powders were synthesized by a carbothermal reduction process using $SiO_2$-C precursors fabricated by a sol-gel process using phenol resin and TEOS as starting materials for carbon and Si sources, respectively. The C/Si molar ratio was selected as an important parameter for synthesizing SiC powders using a sol-gel process, and the effects of the C/Si molar ratio (1.4-3.0) on the particle size, particle size distribution, and yield of the synthesized ${\beta}$-SiC powders were investigated. It was found that (1) the particle size of the synthesized ${\beta}$-SiC powders decreased with an increase in the C/Si molar ratio in the $SiO_2$-C hybrid precursors, (2) the particle size distribution widened with an increase in the C/Si molar ratio, and (3) the yield of the ${\beta}$-SiC powder production increased with an increase in the C/Si molar ratio.