• Title/Summary/Keyword: Thermal dehydration

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Fabrication of High Tc Superconductor Using Thermal Pyrolysis (열분해법에 의한 고온 초전도 합성)

  • Lee, Sang-Heon
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2006.06a
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    • pp.85-86
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    • 2006
  • A high Tc superconducting with a nominal composition of $Bi_2Sr_2Ca_2Cu_3O_y$ was prepared by the citarte method. The solid precursor produced by the dehydration of the gel at $120^{\circ}C$ for 12h is not in the amorphous state as expected but in a crystalline state. X-ray diffraction peaks of nearly the same angular position as the peaks of high Tc phase were observed in the precursor. After pyrolysis at $400^{\circ}C$ and calcination at $840^{\circ}C$ for 4h, the (001)peak of the high Tc phase was cleary observed. Experimental results suggest that the intermediate phase formed before the formation of the superconducting phase may be the most important factro in determining whether it is easy to form the high Tc phase or not, because the nucleation barriers of the two superconducting phase may be altered by the variation of the crystal structures of those intermediate phase.

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Novel Syntheses of Isomers of Damascenone from Ethyl 2,6,6-Trimethyl-4-oxo-2-cyclohexene-1-carboxylate

  • Lee, Woo-Young;Jang, Se-Young;Lee, Jun-Gu;Chae, Woo-Ki
    • Bulletin of the Korean Chemical Society
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    • v.12 no.1
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    • pp.31-35
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    • 1991
  • Three isomers of damascenone, odorous terpenic ketones, have been synthesized conveniently from a same starting material, ethyl 2,6,6-trimethyl-4-oxo-2-cyclohexene-1-carboxylate(1), which was easily available by the acid-catalyzed condensation of mesityl oxide or acetone with ethyl acetoacetate. ${\alpha}$-Damascenone(7) was prepared by converting the enone ester 1 into the corresponding tosylhydrazone(4), followed by treating with 4 molar equiv of allyllithium. ${\beta}$-Damascenone(12) was synthesized by chemoselective reduction of 1 with sodium borohydride/cerium chloride to give corresponding allylic alcohol 8, conversion of 8 into acetate 9, and thermal decomposition of 9 with DBU to afford ethyl ${\beta}$-safranate(10), followed by reaction with an excess amount of allyllithium. ${\gamma}$-Damascenone(15) was obtained by dehydration of 8 with boric acid to furnish ${\gamma}$-safranate(13), followed by treatment with 2 molar equiv of allyllithium.

A Facile Method for the Synthesis of Freestanding CuO Nanoleaf and Nanowire Films

  • Zhao, Wei;Jung, Hyunsung
    • Journal of the Korean institute of surface engineering
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    • v.51 no.6
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    • pp.360-364
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    • 2018
  • A facile method to fabricate freestanding CuO nanoleaves and CuO nanowires-based films was demonstrated. $Cu(OH)_2$ nanoleaves and nanowires were prepared by a hydrolysis reaction in aqueous solution including pyridine and NaOH with the tailored concentrations at room temperature. The films of freestanding CuO nanoleaves and CuO nanowires can be successfully obtained via the simple vacuum infiltration following a thermal dehydration reaction. The morphologies and crystallinity of the $Cu(OH)_2$ nanoleaves/nanowires and CuO nanoleaves/nanowires were characterized by XRD, SEM, TEM and FT-IR. The films fabricated with freestanding CuO nanoleaves and nanowires in this study may be applicable for building high-efficiency organic binder-free devices, such as gas sensors, batteries, photoelectrodes for water splitting and so on.

Lanthanide Complexes of Some High Energetic Compounds (II), Crystal Structures and Thermal Properties of Picrate Complexes

  • Yun, Sock-Sung;Kang, Sung-Kwon;Suh, Hong-Ryol;Suh, Hyung-Sock;Lee, Eun-Kwang;Kim, Jae-Kyung;Kim, Chong-Hyeak
    • Bulletin of the Korean Chemical Society
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    • v.26 no.8
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    • pp.1197-1202
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    • 2005
  • The Ln(III) complexes with picrate ligand, $[Sm(Pic)_2(H_2O)_6]Pic{\cdot}6H_2O$, 1, and $[Ho(Pic)(H_2O)_7](Pic)_2{\cdot}3H_2O$, 2, have been synthesized and their crystal structures are analyzed by X-ray diffraction methods. Complex 1, crystallizes in the monoclinic $P2_1/n$ space group and complex 2 in the triclinic P-1 space group. In complex 1, two picrate ligands coordinate to the Sm(III) ion, one of them in the bidentate fashion. There are one picrate anion and six water molecules in the crystal lattice. The nine-coordinated Sm(III) ion forms a slightly distorted tricapped trigonal prism. In complex 2, only one picrate ligand coordinates to the metal ion as a monodentate. There are two picrate anions and three water molecules in the crystal lattice. The eight-coordinated Ho(III) ion forms a distorted bicapped trigonal prism. Based on the results of the TG-DTG and DSC thermal analysis, it was analyzed that the lanthanide picrate complexes 1 and 2 are thermally decomposed in three distinctive stages, the dehydration, the picrate decomposition, and the formation of the metal oxide.

Synthesis of 6-Alkyl-3-Chromonealdehyde(2,2-dialkyl)hydrazone Derivatives for Green Light Emitting Materials (녹색발광 6-알킬-3-크로몬알데히드(2,2-디알킬)하이드라존 유도체의 합성)

  • Chung, Pyung-Jin;Chang, Hong-Joon
    • Applied Chemistry for Engineering
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    • v.21 no.4
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    • pp.424-429
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    • 2010
  • 6-Alkyl-3-chromonealdehyde (2,2-dialkyl)hydrazone derivatives were synthesized by dehydration condensation. They are green-emitting materials for organic light emitting device (OLED) composed of electron acceptor of 6-alkyl-3-chromonealdehydes and electron donor of 2,2-dialkylhydrazones in a conjugated structure. The structural properties of reaction products were analyzed by FT-IR and $^1H$-NMR spectroscopy. The thermal stabilities and reactivities were measured by melting points and yields. The UV-visibles and PL properties were also determined by excitation spectra and emission spectra, respectively.

CHANGES IN SOME PHYSIOLOGICAL PARAMETERS OF ALBINO RATS AT DIFFERENT AMBIENT TEMPERATURES

  • Hassanin, S.H.;Khali, F.A.;Abd-Elaziz, A.M.S.;EL-Sobhy, H.E.
    • Asian-Australasian Journal of Animal Sciences
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    • v.7 no.4
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    • pp.471-474
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    • 1994
  • Five experimental groups with five adult male rats in each, were exposed to 20, 35, 40 and $45^{\circ}C$ air temperature for 50-70 minutes, and to $50^{\circ}C$ for 30-50 minutes, respectively. Food and drinking water were not permitted during the exposure. Blood samples were obtained by heart puncture immediately after the thermal treatment. All the rats were hyperthermic (p<0.01) as compared to the controls ($20^{\circ}C$). Hyperthermia was associated with hypoglycemia which was significant (p<0.01) at 45 and $50^{\circ}C$ exposures. Plasma levels of GOT and GPT declined at 35 and $40^{\circ}C$ reaching the lowest (p<0.05) level at $45^{\circ}C$, while at $50^{\circ}C$ GOT level was elevated by 45% but GPT was normal as compared to the controls. Differences between groups were significant (p<0.01) for GOT and insignificant for GPT. Hematocrit value increased significantly (p<0.01) at 45 and $50^{\circ}C$, indicating hemoconcentration. It could be concluded that severe heat stress (45 and $50^{\circ}C$) resulted in critical hyperthermia, hypoglycemia, disturbed liver function, body dehydration, and hemoconcentration leading to death.

Dehydration Behavior of Water-butanol Solutions through Asymmetric Sulfonated Po.ysulfone Membrane (술폰화된 polysulfone 비대칭막의 제조와 이를 이용한 물-부탄올 수용액의 탈수거동)

  • 변인섭;백귀찬;차시환;권창오;서종원;김용욱
    • Membrane Journal
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    • v.9 no.3
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    • pp.170-177
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    • 1999
  • Asymmetric membranes for pervaporation were prepared with poly sulfone and sulfonated poly sulfone in order to separate water from 90% by weight butanol solution. Chlorosulfonic acid was reacted with trimethylchlorosilane for using as a sulfonating agent. The prepared polymers were characterized with FT-IR and $^1H$-NMR. The thermal properties of the polymers were examined with DSC and TGA. Back titration method was used for the evaluation of the degree of sulfonation or the ion ex¬change capacity. N-methyl-2-pyrrolidone (NMP) and diethyleneglycol dimethyl ether (DGDE) cosolvent were used for the preparation of asymmetric membranes. The cross section and skin layer of the mem¬branes were examined with scanning electron michroscopy to investigate membrane structure formed with cosolvent composition in the casting solution. In this article, the selectivity of the dense films were not different from each other so much. However, the permeation rates were significantly increased as much as 80 times compared to that of dense film.

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Selective Laser Sintering of Alumina Using an Inorganic Binder Monoclinic $HBO_2$ and Post-Processing

  • 이인섭
    • Journal of Powder Materials
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    • v.5 no.3
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    • pp.199-209
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    • 1998
  • A new low melting inorganic binder, monoclinic $HBO_2$, has been developed for Selective Laser Sintering (SLS) of alumina powder by dehydration process of boron oxide powder in a vacuum oven at $120^{\circ}C$. It led to better green SLS parts and higher bend strength far green and fired parts compared to other inorganic binders such as aluminum and ammmonium phosphate. This appeared to be due to its low viscosity and better wettability of the alumina particle surface. A low density single phase ceramic, aluminum borate ($Al_{18}B_4O_{33}$), and multiphase ceramic composites, $A_{12}O_3-A_{14}B_2O_9$, were successfully developed by laser processing of alumina-monoclinic $HBO_2$ powder blends followed by post-thermal processing; both $Al_{18}B_4O_{33}$ and $A_{14}B_2O_9$ have whisker-like grains. The physical and mechanical properties of these SLS-processed ceramic parts were correlated to the materials and processing parameters. Further densification of the $A_{12}O_3-A_{14}B_2O_9$ ceramic composites was carried out by infiltration of colloidal silica, and chromic acid into these porous SLS parts followed by heat-treatment at high temperature ($1600^{\circ}C$). The densities obtained after infiltration and subsequent firing were between 75 and 80% of the theoretical densities. The bend strengths are between 15 and 33 MPa.

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Synthesis of 3-Chromonealdehyde(2,2-disubstituted)hydrazone Derivatives for Green Light Emitting Materials (녹색발광 3-크로몬알데히드(2,2-이치환)하이드라존 유도체의 합성)

  • Chung, Pyung Jin;Chang, Hong Joon
    • Applied Chemistry for Engineering
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    • v.20 no.6
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    • pp.670-674
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    • 2009
  • 3-Chromonealdehyde(2,2-disubstituted)hydrazone derivatives were synthesized by dehydration condensation. They are green-emitting materials for organic light emitting device (OLED) composed of electron acceptor of 3-chromonealdehydes and electron donor of 2,2-disubstituted hydrazones by a conjugated structure. The structural properties of reaction products were analyzed FT-IR and $^1H-NMR$ spectroscopy. The thermal stabilities and reactivities were measured by melting points and yields. The UV-visibles and PL properties can be determined by excitation spectra and emission spectra, respectively.

Facile Fabrication and Characterization of In2O3 Nanorods on Carbon Fibers

  • Nagaraju, Goli;Ko, Yeong Hwan;Yu, Jae Su
    • Applied Science and Convergence Technology
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    • v.23 no.4
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    • pp.187-191
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    • 2014
  • Indium oxide ($In_2O_3$) nanorods (NRs) which can be expected to increase the device performance in various electronic and electrochemical applications were prepared on carbon fibers via an electrochemical deposition (ED) method. During the ED, the indium hydroxide ($In(OH)_3$) NRs were well grown and firmly attached onto the carbon fibers. After that, they were changed into $In_2O_3$ by dehydration through a thermal annealing. The morphological and structural properties were investigated using field-emission scanning electron microscope images. The crystallinity of as-prepared sample was evaluated by X-ray diffraction. The Fourier transform infrared results confirm that the functional groups are present in the $In_2O_3$ NRs. This facile process of metal oxide nanostructures on carbon fiber can be utilized for flexible electronic and energy related applications.