• Title/Summary/Keyword: Hydrothermal synthesis

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Impregnation of Ibuprofen on MCM-41 using Supercritical Carbon Dioxide (초임계 이산화탄소를 이용한 MCM-41에의 Ibuprofen 함침)

  • Kim, Hong-Lyong;Kim, Jung-Teag;Chun, Jae Kee;Lee, Seok Hee;Hong, Seong-Soo;Ju, Chang-Sik
    • Korean Chemical Engineering Research
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    • v.44 no.3
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    • pp.248-253
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    • 2006
  • In order to develope an efficient drug delivery system, experimental researches on the supercritical impregnation of ibuprofen onto mesoporous silica, MCM-41,and its drug release characteristics were performed. Supercritical carbon dioxide was adapted as an alternative solvent as it is harmless and able to avoid defects of organic solvents in drug manufacturing processes. The procedure was composed of three steps, that is, as hydrothermal synthesis of MCM-41, supercritical impregnation of ibuprofen onto MCM-41 and release of impregnated ibuprofen. Supercritical impregnation reached equilibrium within 2 h for all cases of this research and the amount of equilibrium impregnation increased with solubility of ibuprofen in supercritical carbon dioxide. Release profiles of impregnated ibuprofen showed a similar behavior for all MCM-41 with different impregnated ibuprofen.

Two 3D CdII and ZnII Complexes Based on Flexible Dicarboxylate Ligand and Nitrogen-containing Pillar: Synthesis, Structure, and Luminescent Properties

  • Liu, Liu;Fan, Yan-Hua;Wu, Lan-Zhi;Zhang, Huai-Min;Yang, Li-Rong
    • Bulletin of the Korean Chemical Society
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    • v.34 no.12
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    • pp.3749-3754
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    • 2013
  • Two 3D isomorphous and isostructural complexes, namely, $[Zn(BDOA)(bpy)(H_2O)_2]_n$ (1) and $[Cd(BDOA)-(bpy)(H_2O)_2]_n$ (2); (BDOA = Benzene-1,4-dioxyacetic acid, bpy = 4,4'-bipyridine) were synthesized under hydrothermal conditions and characterized by means of elemental analyses, thermogravimetric (TG), infrared spectrometry, and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in the triclinic system, space group P-1 and each metal ion in the complexes are six-coordinated with the same coordination environment. In the as-synthesized complexes, $BDOA^{2-}$ anions link central metal ions to form a 1D zigzag chain $[-BDOA^{2-}-Zn(Cd)-BDOA^{2-}-Zn(Cd)-]_{\infty}$, whereas bpy pillars connect metal ions to generate a 1D linear chain $[-bpy-Zn(Cd)-bpy-Zn(Cd)-]_{\infty}$. Both infinite chains are interweaved into 2D grid-like layers which are further constructed into a 3D open framework, where hydrogen bonds play as the bridges between the adjacent 2D layers. Luminescent properties of complex 1 showed selectivity for $Hg^{2+}$ ion.

Fabrication of M-Doped TiO2 (M=Co, Cr, Fe) : Its Electronic Band Structure-(1) (M-Doped TiO2 (M=Co, Cr, Fe)의 제조 : 전자 밴드구조-(1))

  • Bae, Sang-Won;Kim, Hyun-Gyu;Ji, Sang-Min;Jang, Jum-Suk;Jeong, Euh-Duck;Hong, Suk-Joon;Lee, Jae-Sung
    • Journal of the Korean Ceramic Society
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    • v.43 no.1 s.284
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    • pp.22-27
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    • 2006
  • The electronic band structures of Metal-doped titanium dioxide, M-doped $TiO_2$ (M=Co, Cr, Fe), have been studied by using XRD, UV-vis diffuse reflectance spectrometer and FP-LAPW (Full-Potential Linearized Augmented-Plane-Wave) method. The UV-vis of M-doped $TiO_2$ (M=Co, Cr, Fe) showed two absorption edges; the main edge due to the titanium dioxide at 387 nm and a shoulder due to the doped metals at around 560 nm. The band gap energies of Co, Cr and Fe-doped $TiO_2$ calculated by FP-LAPW method were 2.6, 2.0, and 2.5 eV, respectively. The theoretically calculated band gap energy of $TiO_2$ by using FP-LAPW method was the same as experimental results. FP-LAPW method will be useful for fabrication and development of photo catalysts working under visible light.

Interfacing Silicate Layer Between MoO3 Ribbon and Pt Metaldots Boosts Methanol Oxidation Reaction

  • Lee, Dohun;Jeong, Juwon;Manivannan, Shanmugam;Kim, Kyuwon
    • Journal of Electrochemical Science and Technology
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    • v.11 no.3
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    • pp.273-281
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    • 2020
  • Constructing and making highly active and stable nanostructured Pt-based catalysts with ultralow Pt loading are still electrifying for electrochemical applications such as water electrolysis and fuel cells. In this study, MoO3 ribbons (RBs) of few micrometer in length is successfully synthesized via hydrothermal synthesis. Subsequently, 3-dimentional (3D)-silicate layer for about 10 to 15 nm is introduced via chemical deposition onto the pre-formed MoO3 RBs; to setup the platform for Pt metaldots (MDs) deposition. In comparison with the bare MoO3 RBs, the MoO3-Si has served as a efficient solid-support for stabilizing and accommodating the uniform deposition of sub-2 nm Pt MDs. Such a structural design would effectively assist in improving the electronic conductivity of a fabricated MoO3-Si-Pt catalyst towards MOR; the interfaced, porous and 3D silicate layer has assisted in an efficient mass transport and quenching the poisonous COads species leading to a significant electrocatalytic performance for MOR in alkaline medium. Uniformly decorated, sub-2 nm sized Pt MDs has synergistically oxidized the MeOH in association with the MoO3-Si solid-support hence, synergistic catalytic activity has been achieved. Present facile approach can be extended for fabricating variety of highly efficient Metal Oxide-Metal Nanocomposite for energy harvesting applications.

High-Temperature Behavior of Ba-Doped Boehmite Hydrothermally Prepared from $Al(OH)_3$ and $Ba(OH)_2$

  • Fujiyohi, Kaichi;Ishida, Shingo
    • The Korean Journal of Ceramics
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    • v.5 no.4
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    • pp.379-385
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    • 1999
  • Minute boehmite crystals with high aspect rations, which were hydrothermally synthesized from gibbsite in $Ba(OH)_2$ solution, occluded Ba with the Ba/Al molar ratio of about 0.03 in their interlayers. Their surface areas were about 14$\m^2$/g. The Ba-intercalated bohemite samples were partly used for producing $BaAl_{12}O){19}$ with low sinterability by externally supplementing $Ba(OH)_2$, and for forming transient aluminas. The surface area of $BaAl_{12}O){19}$ obtained by firing at $1500^{\circ}C$ for 3 h was 5.3$\m^2$/g, which was significantly lower than 12$\m^2$/g of the sol-gel origin. While a mixture ${\gamma}$-alumina and BaO is known to from $BaAl_{12}O){19}$ at $1200^{\circ}C$, solid state reaction between η-alumina transformed from the Ba-intercalated boehmite and BaO formed from $Ba(OH)_2$ deposited on the boehmite started above $1300^{\circ}C$. This suggests that large sized $Ba^{2+}$ ion occluded in η-alumina considerably suppresses the diffusion of $Al^{3+}$ ion. The surface area of the Ba-intercalated boehmite fired at $1400^{\circ}C$ for 3h was as high as 14$\m^2$/g indicative of its potential applicability to combustion catalysts. But it was decreased to 5.0$\m^2$/g after firing at $1500^{\circ}C$ for 3 h, accompanied by abrupt formations of $\alpha$-alumina and $BaAl_{12}O){19}$ as main products. The suppression of $\alpha$-alumina formation up to $1400^{\circ}C$ also suggests the significant blocking effect of $Ba^{2+}$ ion on the diffusion of the component ions.

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Preparation of Co3O4/NF Anode for Lithium-ion Batteries

  • Tian, Shiyi;Li, Botao;Zhang, Bochao;Wang, Yang;Yang, Xu;Ye, Han;Xia, Zhijie;Zheng, Guoxu
    • Journal of Electrochemical Science and Technology
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    • v.11 no.4
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    • pp.384-391
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    • 2020
  • Due to its characteristics of light weight, high energy density, good safety, long service life, no memory effect, and environmental friendliness, lithium-ion batteries (LIBs) are widely used in various portable electronic products. The capacity and performance of LIBs largely depend on the performance of electrode materials. Therefore, the development of better positive and negative materials is the focus of current research. The application of metal organic framework materials (MOFs) derivatives in energy storage has attracted much attention and research. Using MOFs as precursors, porous metal oxides and porous carbon materials with controllable structure can be obtained. In this paper, rod-shaped Co-MOF-74 was grown on Ni Foam (NF) by hydrothermal method, and then Co-MOF-74/NF precursor was heat-treated to obtain rodshaped Co3O4/NF. Ni Foam was skeleton structured, which effectively relieved. The change of internal stress changes and destroys the structural volume of the electrode material and reduces the capacity attenuation. Co3O4/NF composite material has a specific discharge capacity of up to 1858 mA h/g for the first time, and a reversible capacity of up to 902.4 mA h/g at a current density of 200 mA/g, and has excellent rate and impedance performance. The synthesis strategy reported in this article opens the way to design high-performance electrodes for energy storage and electrochemical catalysis.

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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Synthesis of Ti-SBA-15 Doped with Lanthanide Ion and Photocatalytic Decomposition of Methylene Blue (La 이온이 도핑된 Ti-SBA-15의 합성 및 메틸렌블루의 광촉매 분해 반응)

  • Jung, Won-Young;Hong, Seong-Soo
    • Applied Chemistry for Engineering
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    • v.21 no.3
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    • pp.323-327
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    • 2010
  • Ti-SBA-15 catalysts doped with lanthanide ion were synthesized using conventional hydrothermal method and they were characterized by XRD, FT-IR, DRS, $NH_3$-TPD and PL. We also examined the activity of these materials on the photocatalytic decomposition of methylene blue. La/Ti-SBA-15 samples with varying lanthanide ions doping maintained the mesoporous structure and the catalysts calcined at $500^{\circ}C$ for 6 h showed the highest crystallinity. With increasing the doping amount of lanthanide ion, the pore size and pore volume of La/Ti-SBA-15 materials decreased but the surface area increased. 1% La/Ti-SBA-15 catalysts showed the highest photocatalytic activity on the decomposition of methylene blue but the catalysts doped with more than 5% lanthanide ions showed lower activity compared to pure Ti-SBA-15 catalyst.

Synthesis and Photocatalytic Effect of Brookite Phase $TiO_2$ Colloidal Sol by Hydrothermal Method (수열합성법을 이용한 Brookite $TiO2$ 졸의 제조 및 광촉매 효과)

  • Yoon, Cho-Rong;Oh, Hyo-Jin;Czoska, Anna;Park, Kyung-Soon;Lee, Nae-Sung;Kim, Sun-Jae
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2006.05a
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    • pp.117-120
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    • 2006
  • $TiOCl_2$를 중화시키고 과산화수소와 반응시켜 Ti peroxo 전구체를 수열합성법을 이용하여 autoclave 반응기 내에서 가열하여 $TiO_2$ 졸을 제조하였다. Autoclave 반응기 내에 압력을 가하면 브룩카이트상 $TiO_2$졸이 형성됨을 확인하였고, 중화과정에서 NaCl을 첨가하여 Ti 수산화물 격자 내에 Na 이온을 포획되어 브룩카이트상이 나타남을 알 수 있었다. Na 이온의 첨가량에 따라 브룩카이트 결정상 함량이 달라져 광촉매 활성도 달라짐을 브룩카이트상 $TiO_2$가 코팅된 박막의 기상벤젠 광분해 실험을 통해 확인하였고 미세구조, 결정성, 광흡수도률 측정하여 특성평가를 실시하였다.

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Synthesis of Mullite and Zeolite from Fly Ash Refined by Multi-Air Classification (다중자연낙하 공기분급에 의한 정제석탄회로부터 뮬라이트 및 제올라이트의 합성)

  • Hwang, Yeon;Bae, Kwang-Hyun
    • Resources Recycling
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    • v.10 no.6
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    • pp.29-34
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    • 2001
  • Fly ash powders were refined and separated into fine and coarse size by multi-air classification, and each particle was used for synthesizing mullite and zeolite. Mullite was prepared by sintering the mixture of fine fly ash with mean size of 6.5 $\mu$m and $A1_2$$O_3$powder at above $1450^{\circ}C$. Zeolite was synthesized through hydrothermal reaction with coarse fly ash mean size of $56.3\mu$m in 3.5 M NaOH solution at $120^{\circ}C$. The whole range of particle size can be recycled through size classification into fine and coarse fractions, which are used for syntheses of inorganic materials.

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