• Title/Summary/Keyword: TEOS

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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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Step-Coverage Consideration of Inter Metal Dielectrics in DLM Processing : PECVD and $O_3$ ThCVD Oxides (이층 배선공정에서 층간 절연막의 층덮힘성 연구 : PECVD와 $O_3$ThCVD 산화막)

  • Park, Dae-Gyu;Kim, Chung-Tae;Go, Cheol-Gi
    • Korean Journal of Materials Research
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    • v.2 no.3
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    • pp.228-238
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    • 1992
  • An investigation on the step-coverage of PECVD and $O_3$ ThCVD oxides was undertaken to implement into the void-free inter metal dielectric planarization using multi-chamber system for the submicron double level metallization. At various initial aspect ratios the instantaneous aspect ratios were measured through modelling and experiment by depositing the oxides up to $0.9{\mu}m$ in thickness in order to monitor the onset of void formation. The modelling was found to be in a good agreement with the observed instantaneous aspect ratio of TEOS-based PECVD oxide whose re-entrant angle was less than $5^{\circ}$. It is demonstrated that either keeping the instantaneous aspect ratio of PECVD oxide as a first layer less than a factor of 0.8 or employing Ar sputter etch to create sloped oxide edge ensures the void-free planarization after$O_3$ ThCVD oxide deposition whose step-coverage is superior to PECVD oxide. It has been observed that $O_3$ ThCVD oxide etchback scheme has shown higher yield of via contact chain than non etchback process, with resistance per via contact of $0.1~0.3{\Omega}/{\mu}m^2$.

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A Study on the Monodispersed Silica Fine Particles Prepared by Using Batch-Semibatch Mixed Process (회분과 반회분의 혼합형 공정에 의해 생성된 단분산 실리카 미립자에 관한 연구)

  • Kim, Ki Do;Kim, Hee Taik
    • Applied Chemistry for Engineering
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    • v.10 no.8
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    • pp.1180-1185
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    • 1999
  • Modispersed silica fine particles were produced from the hydrolysis of $Si(OC_2H_5)_4$ by using batch-semibatch mixed systems. Four types of mixed process, i.e., batch-batch, batch-semibatch, semibatch-batch, semibatch-semibatch, were used in order to measure mean particle size, particle size distribution, yield, and packing density. As a result of the test, silica particles prepared by semibatch-semibatch process were larger than those prodeced from any other systems in particle size and yield. On the other hand, silica particles prepared by batch-semibatch process were better than those produced from any other systems in particle size distribution and packing density. Especially, it was found that particle size of $SiO_2$ prepared by semibatch-batch process decreased with increasing the reaction time. Therefore, batch-semibatch process was a successful method for controlling the size, i.e., a narrow distribution of a particle size which ranges to several microns.

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Bioactivity behavior of Si and Mg ion-substituted biphasic calcium phosphate powders (Si 및 Mg 이온이 교환된 biphasic calcium phosphate 분말의 생체활성 거동)

  • Kim, Tae-Wan;Kim, Dong-Hyun;Jin, Hyeong-Ho;Lee, Heon-Soo;Park, Hong-Chae;Yoon, Seog-Young
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.22 no.2
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    • pp.92-98
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    • 2012
  • The co-precipitation technique has been applied to synthesize biphasic calcium phosphate (BCP). $Ca(NO_3)_2{\cdot}4H_2O$, $(NH_4)_2HPO_4$, TEOS and $Mg(NO_3)_2{\cdot}6H_2O$ as the starting materials was used. After the heat treatment of powder crystalline phases HAp and ${\beta}$-TCP analysis showed a mixed phase. The overall spectra appear to have mainly two modes corresponding to characteristic $PO^{3-}_4$ and $OH^-$ groups. After immersion in Hanks' Balanced Salt Solution (HBSS) for 1 week a precipitation started to be formed with individual small granules on the specimen surface. An MTT assay indicated that ionic substituted BCP powders had no cytotoxic effects on MG-63 cells, and that they have good biocompatibility.

Monitoring of pH and dissolved oxygen in microorganism fermentation processes using a 24-well microplate (24-웰 마이크로 플레이트를 이용한 미생물 발효공정에서 pH 및 용존산소의 모니터링)

  • Kim, Sun-Yong;Kim, Chun-Kwang;Sohn, Ok-Jae;Rhee, Jong-Il
    • KSBB Journal
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    • v.24 no.2
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    • pp.207-211
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    • 2009
  • In this study, the sensing membranes for detection of pH and dissolved oxygen(DO) were prepared by immobilizing 6-aminofluorescein or ruthenium complex onto the sol-gel matrixes of GPTMS, MTMS, and TEOS and then recoated with the mixture of hydrophobic sol-gel and graphite for light insulation. The pH and DO sensing membranes recoated with the light insulation layer showed a higher sensitivity than those without light insulation layer. The sensing membranes were immobilized on the wells of 24-well microplate and used to monitor the fluorescence intensity for pH and DO in E.coli JM109 and P.pastoris X-33 fermentation processes. The change of the fluorescence intensity in the DO sensing membrane agreed with the growth patterns of microorganisms, that the membranes are valuable to monitor the DO in fermentation processes. In the case of pH monitoring, the fluorescence intensity has showed good correlation to the off-line pH data, that the pH membranes are valuable to monitor pH values in fermentations.

Study on the Improved Abrasion Resistance of Polycarbonate Substrate by UV-curable Organic/Inorganic Hybrid Coatings (자외선 경화형 유기/무기 복합코팅에 의한 폴리카보네이트의 내마모성 향상 연구)

  • 윤석은;우희권;김동표
    • Polymer(Korea)
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    • v.24 no.3
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    • pp.389-398
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    • 2000
  • Transparent, abrasion resistant coatings with 4~13 ${\mu}{\textrm}{m}$ thickness were prepared by spin-coating on polycarbonates with organic/inorganic hybrid solutions, followed by UV curing and heat treatment at 12$0^{\circ}C$ for 12 hours. The coating solutions were composed of inorganic phase and organic phase in 0:100, 20:80, 30:70, 50:50, 80:20 wt% ratios, respectively, mixed with photoinitiator, senaitizer and surfactant. The inorganic phase was formed by sol-gel reaction of TEOS and silane coupling agent MPTMS in 1 : 2 or 2 : 1 molar ratios, the organic phase consisted of difunctional urethane acrylate oligomeric resin, multifunctional acrylate TMPTA and HDDA in 4 : 3 : 3 wt% ratio. The coating systems were investigated by FT-IR, $^{29}$ Si-NMR spectra. In addition, TGA/DSC for thermal analysis and SEM, AFM observation for coated surface were examined. Gererally, the homogeneity of phases, the surface smoothness of coating and abrasion resistance were improved with the higher content of inorganic component. Namely, coating system with below 10 $\AA$ surface roughness and T$_{g}$ of 15$0^{\circ}C$ showed only 10% decrease in light transmittance after abrasion test, whereas uncoated polycarbonate substrate exhibited 46% decrease..

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Stabilizing Properties of SiOF Film with Low Dielectric Constant by $N_2O$ Plasma Annealing ($N_2O$ 플라즈마 열처리에 의한 저유전율 SiOF 박막의 물성 안정화)

  • Kim, Yoon-Hae;Lee, Seok-Kiu;Kim, Sun-Oo;Kim, Hyeong-Joon
    • Korean Journal of Materials Research
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    • v.8 no.4
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    • pp.317-322
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    • 1998
  • The stabilization of low dielectric constant SiOF films prepared by conventional PECVD using TEOS and $C_2F_6$ was evaluated by the $N_2O$-plasma post-deposition annealing. Properties of SiOF film became unstable when it was air-exposed or heat-treated. Water absorption of SiOF films was increased as F content was increased due to the for¬mation of F -Si- F bonds. Also F content of SiOF films decreased after heat treatment. $N_2O$-plasma post-deposition annealing was proved to be effective on stabilizing SiOF films. which was mainly due to the formation of thin SiON layer near the top surface of films. However. the value of dielectric constant was greatly increased again when $N_2O$-plasma post-deposition annealing was done for a long time. To stabilize the SiOF films without an increase of dielec¬tric constant by $N_2O$- plasma post-deposition annealing. the annealing time should be kept the minimum value. to which stabilizing effects against air environment and heat treatment were preserved.

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Microstructure and Properties of Organic-Inorganic Hybrids(PDMS/SiO$_2$) Through Variations in Sol-Gel Processing (졸-겔공정의 변수조절을 통해 제조된 유기-무기복합체 (PDMS/SiO$_2$)의 미세구조와 특성)

  • Eun, Hui-Tae;Hwang, Jin-Myeong
    • Korean Journal of Materials Research
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    • v.11 no.2
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    • pp.94-103
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    • 2001
  • SiO$_2$ and PDMS/SiO$_2$ xerogels which are derived PDMS into TEOS have been synthesized by sol-gel process and controlled pore size and distribution through 2 step acid/base catalyzed processes using HCI and NH$_4$OH as a catalyst. In HCl catalyzed SiO$_2$ and PDMS/SiO$_2$ xerogels, pH and gellation time of xerogel were 2.3~2.5 and 12~13 days, respectively, and the shape of xerogel was identified to pellet type and column type. Under acidic condition of final reaction solution, the hydrolysis rate is accelerating, resulting in long gel times. The shape of xerogel is pellet type. In contrast, under less acidic condition, the condensation rate is accelerating, resulting in shorter gel times and the shape of xerogel is column type. The surface area and average Pore size were changed 400$\rightarrow$600($\m^2$/g) and 15$\rightarrow$28$\AA$, respectively, depending to the increase of the mole ratio of HCl/NH$_4$OH, and represented uniform pore size distribution. It is that all the alkoxide groups are hydrolyzed by HCl after the first step and the condensation rate is enhanced by NH$_4$OH. The regular backbone structures of silica are formed at low temperature and the uniform pores are produced by heat treatment.

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Synthesis and Characterization of Al-containing Titanium Silicalite-1 Catalysts (알루미늄 함유 티타늄 실리카라이트-1 촉매의 합성 및 특성 연구)

  • Ko, Yong Sig;Hong, Suk Bong;Kim, Geon Joong;Ahn, Wha Seung
    • Applied Chemistry for Engineering
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    • v.9 no.5
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    • pp.639-647
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    • 1998
  • Al-containing titanium silicalite-1 ([Al]-TS-1) catalyst was prepared hydrothermally, and the effects of synthesis parameters such as silica/alumina sources, $SiO_2/TiO_2$ ratio, and aging treatment were investigated. The structure, crystal size, and shape were examined by XRD and SEM, and the extent of titanium incorporation into the zeolite framework was examined using UV-vis DRS spectroscopy. For [Al]-TS-1 catalyst preparation, aging of ca. 24h was essential, and the faster crystallization rates were achieved with Cab-O-Sil than with Ludox or TEOS as a silica source. In addition, the higher crystallinity and faster crystallization rate were obtained using sodium aluminate as an aluminum source. 2-butanol oxidation using $H_2O_2$ as an oxidant was carried out to confirm the redox property of the [Al]-TS-1. Acid sites catalyzed toluene alkylation study indicated that lattice titanium species in [Al]-TS-1 weakened the acid strength, and the para-ethyltoluene selectivity was enhanced as a results.

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Electrochemical Characteristics of High Capacity Anode Composites Using Silicon and CNT for Lithium Ion Batteries (실리콘과 CNT를 사용한 리튬 이온 전지용 고용량 음극복합소재의 전기화학적 특성)

  • Lee, Tae Heon;Lee, Jong Dae
    • Korean Chemical Engineering Research
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    • v.60 no.3
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    • pp.446-451
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    • 2022
  • In this study, to improve capacity and cycle stability, the pitch coated nano silicon sheets/CNT composites were prepared through electrostatic bonding of nano silicon sheets and CNT. Silica sheets were synthesized by hydrolyzing TEOS on the crystal planes of NaCl, and then nano silicon sheets were prepared by using magnesiothermic reduction method. To fabricate the nano silicon sheets/CNT composites, the negatively charged CNT after the acid treatment was used to assemble the positively charged nano silicon sheets modified with APTES. THF as a solvent was used in the coating process of PFO pitch. The physical properties of the prepared anode composites were analysed by FE-SEM, XRD and EDS. The electrochemical performances of the synthesized anode composites were performed by current charge/discharge, rate performances, differential capacity and EIS tests in the electrolyte LiPF6 dissolve solvent (EC:DMC:EMC = 1:1:1 vol%). It was found that the anode material with high capacity and stability could be synthesized when high composition of silicon and conductivity of CNT were used. The pitch coated nano silicon sheets/CNT anode composites showed initial discharge capacity of 2344.9 mAh/g and the capacity retention ratio of 81% after 50 cycles. The electrochemical property of pitch coated anode material was more improved than that of the nano silicon sheets/CNT composites.