• Title/Summary/Keyword: 졸-겔 공정

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Particle Size Control by the Addition of PVA and HNO3 in γ-Al2O3 Synthesis Using by Sol-Gel Method (졸-겔법을 이용한 γ-Al2O3 합성 시 PVA와 HNO3 첨가에 따른 입자크기 제어)

  • Um, Myeong-Heon;Kim, Na-Eun;Ha, Beom-Yong
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.11
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    • pp.537-543
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    • 2019
  • Alumina(Al2O3) is a ceramic material used in industry with a range of particle sizes and characteristics. In this study, a boehmite sol was prepared by a hydrolysis and peptizing process using the Sol-Gel method from aluminum isopropoxide (AIP). γ-Al2O3 was prepared by drying and calcining. To prevent particle agglomeration during the manufacturing process, four kinds of polyvinyl alcohol (PVA) with molecular weights of 9,000~10,000, 31,000~50,000, 89,000~98,000, and 130,000 were added and three concentrations of HNO3 (0.1, 0.3, 0.5 molar ratio) were added to determine their effects on the particles. The crystal structure, composition, particle size and shape of the prepared γ-Al2O3 were confirmed through x-ray diffraction (XRD), x-ray fluorescence analyzer (XRF), particle size analyzer (PSA), and field emission scanning electron microscopy (FE-SEM). As a result, γ-Al2O3 with a purity of approximately 98.2% was synthesized, and the particle size decreased and the uniformity increased with increasing ratio of HNO3 addition and PVA molecular weight. From these results, the particle size can be controlled during the manufacturing process of γ-Al2O3 by controlling the addition ratio of PVA and HNO3.

광전자소자의 응용을 위한 산화아연 나노로드의 패터닝 형성방법

  • Go, Yeong-Hwan;Yu, Jae-Su
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.02a
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    • pp.97-97
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    • 2011
  • 산화아연 (ZnO)은 넓은 에너지 밴드갭 (~3.37 eV), 큰 엑시톤 결합 에너지 (~60 meV) 그리고 높은 전자 이동도 (bulk~300 $cm^2Vs^{-1}$, single nanowire~1000 $cm^2Vs^{-1}$)를 갖고 있어, 광전자 소자 및 반도체소자 응용에 매우 널리 사용되고 있다. 특히, 산화아연 나노로드(ZnO nanorod)는 1차원 나노구조로써 더욱 향상된 전자 이동도와 캐리어의 direct path way를 제공하여 차세대 광전자소자 및 태양광 소자의 응용에 대한 연구가 매우 활발하게 이루어지고 있다. 한편, 이러한 산화아연 나노로드를 성장시키기 위하여 VLS (vapor-liquid-solid), 졸-겔 공정(sol-gel process), 수열합성(hydrothermal synthesis), 전기증착(electrodeposition)등 다양한 방법이 보고되었지만, 이러한 산화아연 나노로드의 성장방법은 실제적인 소자응용을 위한 패터닝 형성에 대하여 제약을 받는 문제점이 있다. 이들 중에서 수열합성법과 전극증착법은 ZnO 또는 AZO (Al doped ZnO) seed 층 표면과 성장용액의 화학반응에 의해서 선택적으로 산화아연 나노로드를 성장시킬 수 있다. 이에 본 연구에서는, 광전자소자의 응용을 위한 간단한 패터닝 공정을 위해, 산화인듐주석(ITO) 박막이 증착된 유리기판(glass substrate)위에 수열합성법과 전극증착법을 이용하여 산화아연 나노로드를 선택적으로 성장시켰다. 실험을 위해, ITO glass 위에 RF magnetron 스퍼터를 사용하여 AZO seed 층을 metal shadow mask를 이용하여 패터닝을 형성한 후, 질산아연과 헥사메틸렌테트라아민으로 혼합된 용액에 $85^{\circ}C$ 온도를 유지하여, 패터닝이 형성된 샘플에 전압을 인가하여 성장시켰다. 나노구조 분석을 위해, 전계주사현미경을 이용하여 수열합성법과 전기증착법에 의한 패터닝된 산화아연 나노로드를 비교하여 관찰하였다.

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Preparation and characterization of nanoporous monolith with high thermal insulation performance (나노 기공성 단열 실리카 모노리스 제조 및 특성 연구)

  • Choi, Hyun-Muk;Kim, Seong-Woo
    • Journal of the Korean Applied Science and Technology
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    • v.31 no.1
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    • pp.83-91
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    • 2014
  • In this study, we synthesized two different silica monoliths by using sol-gel, solvent exchange, surface modification, ambient pressure drying processes, and surfactant-based templating technique followed by calcination process. All of the prepared two silica monoliths showed crack-free appearance with fairly good transparency, and furthermore were confirmed to have extremely high porosity, specific surface area, and mean pore size below 30 nm. The silica aerogel sample exhibited finer and more homogeneous nano-sized pore structure due to spring back effect caused by surface modification, which resulted in better thermal insulation performance. Based on measured thermal conductivities and theoretical relationship, multi-layered glass window system in which silica monolith prepared in this study was inserted as a middle layer was revealed to have superior thermal insulation performance compared to conventional air-inserted glass window system.

Ternary Phased Graphene/Silica/EVOH Nanocomposites Coating Films (삼성분계 그래핀/실리카/EVOH 나노 복합 코팅 필름)

  • Kim, Seong Woo
    • Journal of Adhesion and Interface
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    • v.23 no.3
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    • pp.94-99
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    • 2022
  • Ternary phased graphene/silica/EVOH nanocomposite coating materials were prepared via sol-gel process and solution blending process. From both SEM observations and XRD analysis, the exfoliated structure and dispersion state of graphene nanosheets and silica particles in the nanocomposites as well as the intercalated and exfoliated structure of the prepared graphene oxide were confirmed. The incorporation of GrO and silica at appropriate content resulted in remarkable improvement in oxygen barrier property of the ternary phased nanocompoiste-coated BOPP films, compared with that of binary(silica/EVOH) phased nanocomposite coating films, however, at excess amount of GrO and silica, very slight variation was observed due to incomplete exfoliation, dispersion of graphene tactoids, and formation of micro cracks in the silica clusters. In addition, the transparency of nanocomposite-coated film was investigated by measuring the light transmittance as a function of GrO contents, suggesting the possibility for the application of food packaging films.

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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A study on the calcination process of synthetic silica powder for quartz glass crucibles (석영유리 도가니용 합성 실리카 분말의 하소공정에 관한 연구)

  • Yang, Jae-Kyo;Jin, Yun-Ho
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.32 no.4
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    • pp.128-135
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    • 2022
  • The inside of a quartz glass crucible for semiconductor processing, called a transparent layer, is manufactured using synthetic silica powder. Bubbles existing in the transparent layer of the crucible cause a problem of reducing the quality of the crucible as well as the yield of the silicon ingot. Therefore, the main goal of the synthetic silica powder, which is the raw material of the transparent layer, is to minimize the bubble generation factor. For this purpose, in the case of synthetic silica powder, it is necessary to minimize silanol groups, carbon and pores. In this study, synthetic silica gel was prepared using the sol-gel method, and changes in carbon content and specific surface area were investigated according to calcination temperature and dwelled time in a two-stage calcination process. The first-stage calcination process was performed between 500℃ and 600℃ and the second-stage calcination process was performed between 1000℃ and 1100℃. The dwelled time was carried out from 10 minutes to a maximum of 12 hours. The carbon content of the powder calcined at 1000℃ for 1 hour was 0.0031 wt.%, and the specific surface area of the powder calcined at 1100℃ for 12 hours was 16.6 m2/g.

Synthesis and characterization of LiCoO2 thin film by sol-gel process (Sol-gel법에 의한 LiCoO2 박막의 합성과 특성평가)

  • Roh, Tae-Ho;Yon, Seog-Joo;Ko, Tae-Seog
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.24 no.3
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    • pp.94-98
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    • 2014
  • $LiCoO_2$ thin film has received diverse attention as cathodes material of thin-film micro-batteries. In this study, $LiCoO_2$ thin films were synthesized on Au substrates by sol-gel spin coating method and an annealing process. Their structures were studied using X-ray diffraction and Raman Spectroscopy. The particle morphologies of these thin films were observed by Scaning electron microscope. From the results of X-ray diffractometry and Raman Spectroscopy analyses, it was found that as-grown films had the structure of spinel (LT-$LiCoO_2$) and layered-Rock-salt (HT-$LiCoO_2$) at $550^{\circ}C$ and $750^{\circ}C$ respectively. The annealed films at $650^{\circ}C$ were presumed to be the mixed state of these two types. Throlugh the scanning electron microscope, It was estimated that the particle size in as-grown films at $750^{\circ}C$, were larger crystilline particle than in those at the other lower temperature and well distributed in the film.

Bond Strength of SrZrO3 Coatings on Ag Sheathed Bi(2223) Mono-core Tape (은이 피복된 단심 Bi(2223) 초전도 선재에 대한 SrZrO3 코팅층의 접착강도 특성)

  • Lee, Se-Jong;Ye, Kyung-Hwan;Lee, Deuk-Yong;Song, Yo-Seung
    • Journal of the Korean Ceramic Society
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    • v.39 no.10
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    • pp.1001-1006
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    • 2002
  • Bond strength of $SrZrO_3$ resistive oxide barrier on Ag sheathed Bi(2223) tapes prepared by the sol-gel and dip-coating method was evaluated with an aid of Taguchi method and $L_18(2^1{\times}3^7)$ orthogonal arrays to determine the optimal process combination of levels of factors that best satisfy the bigger is better quality characteristic. The observed optimal condition is as follows: Sr/Zr mol ratio(0.3/0.7), amount of organic vehicle(5 wt%), drying temperature and time(160${\circ}C$, 10 min), heat treatment temperature and time(500${\circ}C$, 20 min), respectively. ANOVA analysis suggested that the influence of the factors within ${\alpha}$=0.1 was significant with a 90% confidence level.

Preparation and Characterization of Graft Copolymer/$TiO_2$ Nanocomposite Polymer Electrolyte Membranes (가지형 공중합체/$TiO_2$ 나노복합 고분자 전해질막의 제조 및 분석)

  • Koh, Jong-Kwan;Roh, Dong-Kyu;Patel, Rajkumar;Shul, Yong-Gun;Kim, Jong-Hak
    • Membrane Journal
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    • v.20 no.1
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    • pp.1-7
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    • 2010
  • A graft copolymer, i.e. poly(vinylidene fluoride-co-chlorotrifluoroethylene )-g-poly(styrene sulfonic acid) (P(VDF-co-CTFE)-g-PSSA) with 47 wt% of PSSA was synthesized via atom transfer radical polymerization (ATRP). This copolymer was combined with titanium isopropoxide (TTIP) to produce graft copolymer/$TiO_2$ nanocomposite membranes via sol-gel process. $TiO_2$ precursor (TTIP) was selectively incorporated into the hydrophilic PSSA domains of the graft copolymer and grown to form $TiO_2$ nanoparticles, as confirmed by FT-IR and UV-visible spectroscopy. Water uptake and ion exchange capacity (IEC) decreased with TTIP contents due to the decrease in number of sulfonic acid in the membranes. At 5 wt% of TTIP, the mechanical properties of membranes increased while maintaining the proton conductivity.

Synthesis of Pd-decorated SiO2 layers with superhydrophobic and oleophilic micro-nano hierarchical (초소수성 및 친유성을 갖는 마이크로-나노 계층구조의 Pd 금속입자 기능화된 SiO2층 합성)

  • Kim, Jae-Hun;Lee, Jae-Hyeong;Kim, Jin-Yeong;Kim, Sang-Seop
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2017.05a
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    • pp.67.2-67.2
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    • 2017
  • 본 연구에서는 $SiO_2$ 미세구조 상에 Pd 나노입자(NPs)를 증착하여, 불소화된 마이크로-나노 계층구조를 갖는 Pd-decorated $SiO_2$($Pd/SiO_2$)를 제작하였다. 마이크로 크기의 거칠기를 갖는 $SiO_2$ 층은 졸-겔 공정을 사용해서 제조된 용액을 전기분사함으로써 제조되었다. 이어서, 자외선(UV)을 이용한 광 환원법을 이용해 Pd 나노입자를 $SiO_2$ 층에 형성했다. 생성된 표면은 마이크로-나노의 계층구조 형태를 보여주었다. 해당 시편의 불소화 처리 후, 마이크로-나노의 계층구조 표면은 $170^{\circ}$ 이상의 물 접촉각(water contact angle; WCA) 및 $5^{\circ}$ 이하의 슬라이딩 각(sliding angle)을 보여줌으로써 물에 대해 탁월한 소수성을 나타내었다. 또한, 커피($CA=161^{\circ}$), 우유($CA=162^{\circ}$), 쥬스($CA=163^{\circ}$), 그리고 글리세롤($CA=165^{\circ}$)에 대해서도 우수한 소수 특성을 보여주었다. 또한, 이들 $Pd/SiO_2$ 층은 우수한 장기내구성 및 자외선 저항성을 보여주었다. 그리고 이어진 기름에 대한 접촉각 측정을 통해 해당 시편이 소유 특성이 아닌 친유 특성을 보여준다는 것을 확인할 수 있었고, 기름에 대한 CA는 약 ${\sim}10^{\circ}$로 매우 우수한 친유 특성을 나타내었다. 이와 같은 결과는 자체세정이 가능한 표면 및 지능형 물/기름 분리 시스템과 같은 스마트 장치에서 초소수성-친유성 특성을 갖는 계층구조의 $Pd/SiO_2$ 층을 사용할 가능성을 명확하게 보여준다고 판단된다.

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