• Title/Summary/Keyword: Sol-Gel Method

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A Study on Characteristics of HI Decomposition Using Pt Catalysts on ZrO2-SiO2 Mixed Oxide (ZrO2-SiO2 복합산화물에 담지된 백금 촉매의 요오드화수소 분해 특성 연구)

  • Ko, Yunki;Park, Eunjung;Bae, Kikwang;Park, Chusik;Kang, Kyoungsoo;Cho, Wonchul;Jeong, Seonguk;Kim, Changhee;Kim, Young Ho
    • Transactions of the Korean hydrogen and new energy society
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    • v.24 no.5
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    • pp.359-366
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    • 2013
  • This work is investigated for the catalytic decomposition of hydrogen iodide (HI). Platinum was used as active material by loading on $ZrO_2-SiO_2$ mixed oxide in HI decomposition reaction. To obtain high and stable conversion of hydrogen iodide in severe condition, it was required to improve catalytic activity. For this reason, a method increasing dispersion of platinum was proposed in this study. In order to get high dispersion of platinum, zirconia was incorporated in silica by sol-gel synthesis. Incorporating zirconia influence increasing platinum dispersion and BET surface area as well as decreasing deactivation of catalysts. It should be able to stably product hydrogen for a long time because of inhibitive deactivation. HI decomposition reaction was carried out under the condition of $450^{\circ}C$ and 1 atm in a fixed bed reactor. Catalysts analysis methods such as $N_2$ adsorption/desorption analysis, X-ray diffraction, X-ray fluorescence, ICP-AES and CO gas chemisorption were used to measurement of their physico-chemical properties.

A Solid-State NMR Study of Coordination Transformation in Amorphous Aluminum Oxide: Implication for Crystallization of Magma Ocean (고상 NMR을 이용한 비정질 알루미나의 상전이 연구: 마그마 바다 구성 용융체의 결정화 과정의 의의)

  • Ryu, Saebom;Lee, Sung Keun
    • Journal of the Mineralogical Society of Korea
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    • v.25 no.4
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    • pp.283-293
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    • 2012
  • In order to have better insights into the chemical differentiation of Earth from its magma ocean phase to the current stratified structure, detailed information of crystallization kinetics of silicate melts consisting of the magma ocean is essential. The structural transitions in oxide glasses and melts upon crystallization provide improved prospects for a systematic and quantitative understanding of the crystallization processes. Here, we report the $^{27}Al$ 3QMAS NMR spectra for sol-gel synthesized $Al_2O_3$ glass with varying temperature and annealing time. The NMR spectra for the amorphous $Al_2O_3$ show well-resolved Al coordination environments, characterized with mostly $^{[4,5]}Al$ and a minor fraction of $^{[6]}Al$. The fraction of $^{[5]}Al$ in the alumina phase decreases with increasing annealing time at constant temperature. The NMR results of $Al_2O_3$ phases also imply that multiple processes (e.g., crystallization and/or changes in structural disorder within glasses) could involve upon its phase transition. The current results and method can be useful to understand crystallization kinetics of diverse natural and multi-component silicate glasses and melts. The potential result may yield atomic-level understanding of Earth's chemical evolution and differentiation from the magma ocean.

Magnetic Properties of Mn-substituted Magnetite Thin Films (망간 치환된 마그네타이트 박막의 자기적 특성 연구)

  • Lee, Hee-Jung;Kim, Kwang-Joo
    • Journal of the Korean Vacuum Society
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    • v.16 no.4
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    • pp.262-266
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    • 2007
  • Polycrystalline $Mn_xFe_{3-x}O_4$ thin films were synthesized on Si(100) substrates using sol-gel method and the effects of Mn substitution on the structural, magnetic, and magnetotransport properties were analyzed. X-ray diffraction revealed that cubic structure is maintained up to x = 1.78 with increasing lattice constant for increasing x. Such increase of the lattice constant is attributable to the substitution of $Mn^{2+}$ (with larger ionic radius) ions into tetrahedral $Fe^{3+}$(with smaller ionic radius) sites. VSM measurements revealed that $M_s$ does not vary significantly with x, qualitatively explainable by comparing spin magnetic moments of Mn and Fe ions. On the other hand, $H_c$ was found to decrease with increasing x, attributable to the decrease of magnetic anisotropy due to the decrease of $Fe^{2+}$ density through $Mn^{2+}$ substitution. Magnetoresistance (MR) of the $Mn_xFe_{3-x}O_4$ films was found to decrease with increasing x. Analysis of the MR data in comparison with the VSM results gives an indication of the tunneling of spin-polarized carriers through the grain boundaries of the polycrystalline samples at low external field and spin-flip of the carriers at high external field.

Electrosorption Behavior of $TiO_2$/Activated Carbon Composite for Capacitive Deionization (축전식 이온제거에 대한 $TiO_2$/Activated Carbon 화합물의 전기흡착 거동)

  • Lee, Jeong-Won;Kim, Hong-Il;Kim, Han-Joo;Park, Soo-Gil
    • Applied Chemistry for Engineering
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    • v.21 no.3
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    • pp.265-271
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    • 2010
  • Desalination effects of capacitive deionization (CDI) process was studied using $TiO_2$/activated carbon electrode. In order to enhance the wettability of electrode and decrease a electrode resistance, $TiO_2$ was coated on activated carbon. By means of $TiO_2$ coating on activated carbon, electric double layer to adsorption content in CDI process was increased. It was identified from TEM, XRD, and XPS that the activated carbon based on $TiO_2$ composite was fabricated successfully by means of sol-gel method. As a results of cyclic voltammetry and impedance, it was identified that $TiO_2$/activated carbon electrode has more electric double later capacitance and less diffusion resistance than activated carbon. Also charge-discharge and ion conductivity profiles showed that the ion removal ratios of $TiO_2$/activated carbon electrode in NaCl electrolyte of $1000\;{\mu}S/cm$ more increased about 39% than that of activated carbon. In conclusion it was possible to identify that the carbon electrode coated $TiO_2$ as electrode material was more effective than raw carbon electrode.

Optical Properties and Phenol Destruction Performance of Pd-inserted TiO2 Photocatalysts (Pd이 삽입된 TiO2 광촉매의 광학 특성 및 페놀 분해 성능 평가)

  • Do, Jeong Yeon;Kim, Teho;Sim, Hwanseok;Jeong, Hamin;Choi, Jae Hoon;Kang, Misook
    • Applied Chemistry for Engineering
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    • v.28 no.5
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    • pp.547-553
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    • 2017
  • This study focused on the difference of photocatalytic performance by the incorporation of Pd into the $TiO_2$ framework and suggested five different catalysts composed of $TiO_2$ and x mol% $Pd-TiO_2$ (x = 0.25, 0.5, 0.75, and 1.0). A typical sol-gel method was used to synthesize catalysts, and the phenol photodegradation performance of each catalysts was evaluated. The physicochemical and optical properties of catalysts were confirmed by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy/energy dispersive spectrometer (SEM/EDS), ultraviolet/visible spectroscopy (UV/Vis), photoluminescence spectroscopy (PL), and photocurrent measurements. With the addition of Pd ions, the band gap of catalysts was shortened and the charge separation between photogenerated electrons and holes easily also occurred. As a result, the phenol photo-destruction performance over 0.75 mol% $Pd-TiO_2$ catalyst was 3 times higher than that of pure $TiO_2$. This is believed to be due to Pd ions acted as an electron capturing function during photocatalysis.

Disinfection of E.coli in Drinking Water by TiO2 Photocatalytic System (TiO2 광촉매 시스템을 이용한 음용수 중의 대장균 살균연구)

  • Jung, Jin-Ah;Kwak, Do Hwan;Oh, Dae Woong;Park, Dong Min;Yang, O-Bong
    • Korean Chemical Engineering Research
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    • v.50 no.1
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    • pp.11-17
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    • 2012
  • Disinfection of Escherichia coli (E. coli) in drinking water was investigated by using $TiO_2$ and $TiO_2-SiO_2$ based photocatalyst prepared by sol-gel method. The disinfection test was carried out in an annular flow reactor with circulating sterile water containing the photocatalysts powder under UV-A irradiation. The disinfection activity was proportional to the anatase`s intensity of crystalline peak of the $TiO_2$ photocatalysts. 100% disinfection of E.coli without endotoxin was achieved with $TiO_2$ coated photocatalytic system under UV-A irradiation within 2 h. However, toxic endotoxine was exist in the disinfection of E.colithe under UV-C irradiation even though 100% disinfection of E.colithe within 30 min, which suggest that $TiO_2$ coated photocatalytic system with UV-A is useful tool for the disinfection of E.coli in drinking water.

Hydrogen Production from Photocatalytic Splitting of Water/Methanol Solution over a Mixture of P25-TiO2 and AgxO (산화은/이산화티타늄 혼합물을 광촉매로 활용한 물/메탄올 분해 수소제조)

  • Kim, Kang Min;Jeong, Kyung Mi;Park, No-Kuk;Lee, Tae Jin;Kang, Misook
    • Clean Technology
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    • v.21 no.4
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    • pp.271-277
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    • 2015
  • A photocatalyst which mixed by the commercialized P25-TiO2 and a synthesized AgxO was used in an appropriate weight ratio to effectively produce hydrogen gas in this study. The AgxOs were synthesized with the conventional sol-gel method, and tetramethylammonium hydroxides were added at the synthesis process in order to stabilize the solutions, and then the solutions were heat-treated at the temperatures of -5, 25, and 50 ℃, resulted to obtain the three types of silver oxides. Physicochemical properties of the synthesized AgxOs were identified through X-ray diffraction analysis (XRD), scanning emission microscopy (SEM), ultraviolet-visible spectroscopy, and X-ray photoelectron spectroscopy (XPS). In the photolysis results of water/methanol (weight ratio 1:1) solution, the mixture of P25-TiO2/AgxO exhibited a significantly higher hydrogen gases evolution, compared to that of pure P25-TiO2. Additionally, the addition of H2O2 as an supplement oxidant and in AgxO synthesized at 50 ℃ improved the hydrogen production efficiency. In particular, the emitted hydrogen gases reached to 13,000 μmol during 8 hours when a mixed catalyst, AgxO of 0.1 g and P25-TiO2 of 0.9 g, were used.

Structural and Magnetic Properties of Fe Doped CuO (Fe 첨가된 CuO의 구조적, 자기적 특성)

  • Park, Young-Ran;Kim, Kwang-Joo;Park, Jae-Yun;Ahn, Geun-Young;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.16 no.1
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    • pp.34-39
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    • 2006
  • Pure and Fe-doped CuO thin-film and powder samples were prepared using a sol-gel method. Undoped CuO films exhibited monoclinic structure and p-type electrical conductivity $(\~10^{-2}\;{\Omega^{-1}\;cm^{-1}$ due to copper deficiency. On the other hand, CuO: Fe films were found to be insulating and Li doping on the films led to a restoration of p-type conductivity and a ferromagnetic hysteresis behaviour at room temperature. The observed properties far the CuO : Fe, Li films can be explained in terms of hole creation by substitution of $Li^+$ for $Cu^{2+}$ sites and mediation of long-range interactions between $Fe^{3+}$ ions by the $Li^+$-induced defect states. CuO: Fe powders exhibited a ferromagnetism at room temperature with its strength being dependent on post-annealing temperature. Mossbauer measurements on the CuO: Fe films and powders revealed that the octahedral $Cu^{2+}$ sites are mostly substituted by $Fe^{3+}$ ions.

Fabrication of Ba-, Pb-electronic ceramics by powder prepartion of wet chemical method (습식화학적 분말합성법에 의한 Ba-, Pb-계 전자세라믹스의 제조)

  • 이병우;오근호
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1996.06b
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    • pp.259-279
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    • 1996
  • 최근 정보·전자산업의 발전으로 고 신뢰성 전자재료에 대한 수요가 증대되고 있으며 이러한 첨단산업의 기반의 될 신소재 중 전자세라믹스가 차지하는 비중이 그 대부분을 차지하고 있으며 이에 대한 수요와 기대가 점점 커지고 있다. 이러한 전자세라믹스는 유전재료, 자성재료, 압전재료, 도전성 재료 등으로 나뉘게 된다. 어떠한 분류에 들어가든 그 조성은 금속의 산화물 형태가 일반적이며 미세한 분말의 성형체를 소결(sintering) 함으로써 최종제품으로 완성된다. 이러한 전잣라믹스가 최근 요구되는 고 신뢰성, 고 밀도화를 달성하기 위해선 원료 분말 제조단계부터 제어가 필요하다. 원료분말의 균일·균질성과 그 입도는 소결특성 뿐만아니라 전기적 특성에도 큰 영향을 미치기 때문이다. 세라믹스의 분말제조 방법 중 일반적으로 사용되는 방법으로는 고상 산화물을 혼합하여 하소(calcination)한 후 분쇄하는 '고상합성법'과 금속의 염 또는 alkoxide 용액을 이용하여 화학적으로 제조하는 '습식 화학적 합성법'이 있다. 고상합성법은 합성온도가 높고 기계적 분쇄와 혼합에 의존하므로 균일·균질성이 떨어지고 분말크기를 1㎛ 이하로 만들기 힘들다. 반면에 습식화학적 합성법은 기계적인 분쇄와 혼합에선 얻을 수 없는 원자 혹은 분자단위의 균일한 혼합과 submicron 이하의 미세한 분말을 얻을 수 있다. 따라서 이러한 습식 화학적 합성으로 얻은 분말을 사용하면 미세한 입자의 특성으로 인해 소결온도를 낮출 수 있으며 균일한 미세구조와 균질한 조성을 갖게되어 기계적·전기적 물성증진도 가져올 수 있게 된다. 습식 화학적 분말합성법은 전술하였듯이 alkoxide의 가수분해를 이용하는 sol-gel 법과 금속의 염(salt) 용액을 이용하여, 화학적으로 화합물 침전을 얻거나 또는 공침전물(coprecipitate) 형태의 분말을 얻는, 침전법으로 나뉠 수 있다. 침전법의 근본원리는 pH 및 pCO3 등에 따른 이온종의 용해도 차이를 이용하는 것으로써 각 이온종에 따른 solubility product(ksp)를 이용하여 설명된다. 본 연구에서는 침전법을 사용한 Ba-, Pb-계 전자세라믹스의 분말합성에 대한 이론적 고찰과 공정개발 및 실험을 통한 물성증진 효과에 대해 알아보았다. 본 실험상의 전자세라믹스 조성은 강유전체, 세라믹반도체, 압효과에 대해 알아보았다. 본 실험상의 전자세라믹스 조성은 강유전체, 세라믹 반도체, 압전재료로 널리 사용되는 BaTiO3, PZT(PbZrO3-PbTiO3)와 수직 자기기록매체로 큰 가능성이 있으며 hard ferrite로 널리쓰이는 Ba-feerite(BaFe12O19)로써 수산화물 형태의 침전에 대한 기구(mechanism)와 물성에 대해 살펴보았다. 이러한 침전법에 의한 분말합성 과정에는 소결체의 물성에 영향을 미치는 pH 조절제나 원료에서 혼입될 수 있는 Na+, K+, Cl-, SO4- 등의 제거(washing 혹은 filtering)가 필수적이다. 그러나 침전법에서 얻게 되는 분말은 매우 미세하여 colloid를 형성하게 되며, 이러한 colloid 상태의 미세한 침전입자가 filtering media에 끼이게 되어 견고하면서도 상당한 부피를 가지는 filter cake을 형성하기 때문에 filtering에 많은 시간과 다량의 filtering agent (본 실험의 경우엔 증류수)가 필요하게 된다. 따라서 이러한 문제점을 해결하기 위하여 colloid 상태의 침전물을 얼렸다 녹이는 freezing process를 개발, 적용하여 그 원리 및 효과, 그로인한 분말형태를 관찰하여 보았다.

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Weatherability of Organic-Inorganic Hybrid Coating Agents with N-Triethoxy silyl propyl quinine urethane (N-Triethoxy silyl propyl quinine urethane을 도입한 유-무기 복합 코팅제의 내후성)

  • Lee, Man Sung;Jo, Nam-Ju
    • Journal of Adhesion and Interface
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    • v.2 no.2
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    • pp.20-27
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    • 2001
  • Recently polycarbonate material has been utilized as windows in aircraft, buildings, and optical lens. However, while polycarbonate has excellent optical transparency, impact strength and many beneficial mechanical properties, it possesses poor abrasion resistance and weatherability. Then, there is a need for developing optically clear, anti-abrasive and weather resistant hard coating agents for polycarbonate. In this study, N-triethoxy silyl propyl quinine urethane(TESPQU) was synthesized with quinine and 3-isocyanato propyl triethoxy silane(3-IPTES). In order to introduce optically active silane in the main siloxane network, TESPQU was co-hydrolysed and co-condensed with methyl triethoxy silane(MTES) under acidic conditions. Polycarbonate sheets were coated with silica coating agents by the sol-gel method, and their abrasion resistance, ability of UV absorption and weatherability were evaluated. Coating agents containing hydroxybenzophenone as a UV absorber were also prepared to compare weatherability with TESPQU containing coating agent. TESPQU containing coating agent had good weatherability in accelerated QUV test.

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