• Title/Summary/Keyword: crystal transition

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Structural Characteristics and Physical Properties of Wild Silk Fibres; Antheraea pernyi and Antheraea yamamai (야잠사의 구조특성 및 물리적 성질)

  • 권해용;박영환
    • Journal of Sericultural and Entomological Science
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    • v.36 no.2
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    • pp.138-146
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    • 1994
  • The structural characteristics of Antheraea yamamai and Antheraea pernyi silk were investigated by using x-ray diffraction method, IR spectroscopy and polarizing microscopy. The amino acid composition, fiber density, thermal decomposition temperature and glass transition temperature were also measured for relating these physical properties to the structure in comparison with those of Bombyx mori silk fiber. There was no significant structural difference between A. yamamai and A. pernyi silk fiber on an examination of x-ray diffraction curve and IR spectrum. Both of these wild silk fibers showed double diffraction peaks at the Bragg angle 2Θ16.7˚ and 20.5˚by x-ray diffraction analysis as well as IR absorption peaks for the bending vibration of specific groups related to ala-ala amino acid sequence. On the other hand, the x-ray diffraction curve and IR spectrum of Bombyx mori silk fiber are different from those of wild silk fibers, indicating different crystal structure as well as amino acid sequences. It showed under the polarizing microscope examination that the birefringence and optical orientation factor of wild silk fibers are much lower than those of B. mori silk. Also, the surface of degummed wild silk fibers was characterized by the longitudinal stripes of microfibrils in the direction of fiber axies. The amino acid composition, which is strongly related to the fine structure and properties, was not significantly different between these two wild silk fibers. However, the alanine content was somewhat less and polar amino acid content more for A. yamamai. As a result of fiber density measurement, the specific gravities of B. mori, A. pernyi and A. yamamai were 1.355~1.356, 1.308~1.311, 1.265~1.301g/㎤ in the order, respectively. The calculated crystallinity(%) was 64% for B. mori and 51~52% for wild silk fibers, which showed same trend by IR method in spite of somewhat higher value. The thermal decomposition behaviour was examined by DSC and TGA, showing that the degradation temperature was in the order of B mori, A. prernyi and A. yamamai at around 350$^{\circ}C$. It was also observed by TGA that the decomposition seems to proceed step by step according to their specific regions in the fiber structure, resulting the difference in their thermal stabilities. The glass transition temperature was turned out to be 220$^{\circ}C$ for B. mori, 240$^{\circ}C$ A. yamamai and 255$^{\circ}C$ A. pernyi by the dynamic mechanical analysis. It is expected that the chemical properties are affected by the dynamic mechanical behavior in accordance with their structural characters.

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Nonstoichiometry and Magnetic Properties of the $Eu_{1-x}Sr_xCoO_{3-y}$ System ($Eu_{1-x}Sr_xCoO_{3-y}$계의 비화학량론과 자기적 특성)

  • Ryu, Kwang Hyun;Min, Ji Young;Yo, Chul Hyun
    • Journal of the Korean Chemical Society
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    • v.39 no.7
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    • pp.508-512
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    • 1995
  • A series of samples in the $Eu_{1-x}Sr_xCoO_{3-y}$ system has been prepared by heating the proper amount of reactant mixture to 1150$^{\circ}C$ under an ambient atmosphere, and the solid solutions are identified by X-ray powder diffraction analysis. The crystal system of samples for the compositions of x=0.00 and 0.25 are found to be orthorhombic whose local symmetry is similiar to the distorted octahedra with orthoferrite type one, whereas those of x=0.50 and 0.75 to be the cubic system, and that of x=1.00 to the orthorhombic similiar to be the brownmillerite type. The amount of $Co^{4+}$ ion (${\tau}$ value) is maximized at the composition of x=0.50, and the oxygen vacancies increase with the x value. The nonstoichiometric chemical formula of each compound could be determined from the mole ratio of $Co^{4+}$ ion and oxygen vacancies. The $Co^{3+}$ ion located in octahedral site has spin transition from low spin to high spin states with increasing temperature. Therefore, the effective magnetic moment of each samples obtained from the magnetic measurement is increased with the increasing temperature. The $EuCoO_{3.00}$ has strong antiferromagnetic interaction between the neighboring $Co^{3+}$ ions through the intermediate oxygen ions. With the increasing ${\tau}$ value, the absolute {\theta}_p$ value is decreased by the ferromagnetic interaction of $Co^{3+}-O^2-Co^{4+}$ and thus the {\theta}_p$ has positive value at x=0.50.

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Variation of Band Gap Energy upon Structural Distortion for Nb-containing Oxyfluorides (Nb를 포함하는 불소산화물에서 구조적 뒤틀림에 따른 에너지 띠 간격의 변화)

  • Kim, Hyun-Jun;Kim, Seung-Joo
    • Journal of the Korean Chemical Society
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    • v.51 no.3
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    • pp.265-269
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    • 2007
  • A comparative study on crystal structures and UV-visible diffuse reflectance spectra for Nb-containing oxyfluorides was performed to probe the relationship between energy band gap and local structure. The oxyfluorides, RbSrNb2O6F, RbCaNb2O6F and RbNb2O5F are commonly composed of the corner-sharing NbO5F octahedra as structural building units. The average Nb-O(F)-Nb bond angles, which can be a measure of the structural distortion, are 158.6° for RbSrNb2O6F, 149.6° for RbCaNb2O6F and 139.5° for RbNb2O5F. As the bond angle decreases, the band gap increases: 3.48eV for RbSrNb2O6F, 3.75eV for RbCaNb2O6F and 4.03 eV for RbNb2O5F. This experimental result implies that the band gap can be controlled with a range of 0.6 eV through a variation of local structure for the Nb-containing oxyfluorides.

A facile synthesis of transfer-free graphene by Ni-C co-deposition

  • An, Sehoon;Lee, Geun-Hyuk;Jang, Seong Woo;Hwang, Sehoon;Yoon, Jung Hyeon;Lim, Sang-Ho;Han, Seunghee
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.129-129
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    • 2016
  • Graphene, as a single layer of $sp^2$-bonded carbon atoms packed into a 2D honeycomb crystal lattice, has attracted much attention due to its outstanding properties. In order to synthesize high quality graphene, transition metals, such as nickel and copper, have been widely employed as catalysts, which needs transfer to desired substrates for various applications. However, the transfer steps are not only complicated but also inevitably induce defects, impurities, wrinkles, and cracks of graphene. Furthermore, the direct synthesis of graphene on dielectric surfaces has still been a premature field for practical applications. Therefore, cost effective and concise methods for transfer-free graphene are essentially required for commercialization. Here, we report a facile transfer-free graphene synthesis method through nickel and carbon co-deposited layer. In order to fabricate 100 nm thick NiC layer on the top of $SiO_2/Si$ substrates, DC reactive magnetron sputtering was performed at a gas pressure of 2 mTorr with various Ar : $CH_4$ gas flow ratio and the 200 W DC input power was applied to a Ni target at room temperature. Then, the sample was annealed under 200 sccm Ar flow and pressure of 1 Torr at $1000^{\circ}C$ for 4 min employing a rapid thermal annealing (RTA) equipment. During the RTA process, the carbon atoms diffused through the NiC layer and deposited on both sides of the NiC layer to form graphene upon cooling. The remained NiC layer was removed by using a 0.5 M $FeCl_3$ aqueous solution, and graphene was then directly obtained on $SiO_2/Si$ without any transfer process. In order to confirm the quality of resulted graphene layer, Raman spectroscopy was implemented. Raman mapping revealed that the resulted graphene was at high quality with low degree of $sp^3$-type structural defects. Additionally, sheet resistance and transmittance of the produced graphene were analyzed by a four-point probe method and UV-vis spectroscopy, respectively. This facile non-transfer process would consequently facilitate the future graphene research and industrial applications.

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Fabrication and Characterization of Si Quantum Dots in a Superlattice by Si/C Co-Sputtering (실리콘과 탄소 동시 스퍼터링에 의한 실리콘 양자점 초격자 박막 제조 및 특성 분석)

  • Kim, Hyun-Jong;Moon, Ji-Hyun;Cho, Jun-Sik;Park, Sang-Hyun;Yoon, Kyung-Hoon;Song, Jin-Soo;O, Byung-Sung;Lee, Jeong-Chul
    • Korean Journal of Materials Research
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    • v.20 no.6
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    • pp.289-293
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    • 2010
  • Silicon quantum dots (Si QDs) in a superlattice for high efficiency tandem solar cells were fabricated by magnetron rf sputtering and their characteristics were investigated. SiC/$Si_{1-x}C_x$ superlattices were deposited by co-sputtering of Si and C targets and annealed at $1000^{\circ}C$ for 20 minutes in a nitrogen atmosphere. The Si QDs in Si-rich layers were verified by transmission electron microscopy (TEM) and X-ray diffraction. The size of the QDs was observed to be 3-6 nm through high resolution TEM. Some crystal Si and -SiC peaks were clearly observed in the grazing incident X-ray diffractogram. Raman spectroscopy in the annealed sample showed a sharp peak at $516\;cm^{-1}$ which is an indication of Si QDs. Based on the Raman shift the size of the QD was estimated to be 4-6 nm. The volume fraction of Si crystals was calculated to be about 33%. The change of the FT-IR absorption spectrum from a Gaussian shape to a Lorentzian shape also confirmed the phase transition from an amorphous phase before annealing to a crystalline phase after annealing. The optical absorption coefficient also decreased, but the optical band gap increased from 1.5 eV to 2.1 eV after annealing. Therefore, it is expected that the optical energy gap of the QDs can be controlled with growth and annealing conditions.

Effects of Calcination Temperature on Characteristics of Electrospun TiO2 Catalyst Supports for PEMFCs (열처리 온도가 전기방사방법을 이용하여 제조한 PEMFC용 TiO2 담체의 물리적 특성에 미치는 영향)

  • Kwon, Chorong;Yoo, Sungjong;Jang, Jonghyun;Kim, Hyoungjuhn;Kim, Jihyun;Cho, Eunae
    • Transactions of the Korean hydrogen and new energy society
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    • v.24 no.3
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    • pp.223-229
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    • 2013
  • Polymer Electrolyte Membrane Fuel Cell (PEMFC) is a power generation system to convert chemical energy of fuels and oxidants to electricity directly by electrochemical reactions. As a catalyst support for PEMFCs, carbon black has been generally used due to its large surface area and high electrical conductivity. However, under certain circumstances (start up/shut down, fuel starvation, ice formation etc.), carbon supports are subjected to serve corrosion in the presence of water. Therefore, it would be desirable to switch carbon supports to corrosion-resistive support materials such as metal oxide. $TiO_2$ has been attractive as a support with its stability in fuel cell operation atmosphere, low cost, commercial availability, and the ease to control size and structure. However, low electrical conductivity of $TiO_2$ still inhibits its application to catalyst support for PEMFCs. In this paper, to explore feasibility of $TiO_2$ as a catalyst support for PEMFCs, $TiO_2$ nanofibers were synthesized by electrospinning and calcinated at 600, 700, 800 and $900^{\circ}C$. Effects of calcination temperature on crystal structure and electrical conductivity of electrospun $TiO_2$ nanofibers were examined. Electrical conductivity of $TiO_2$ nanofibers increased significantly with increasing calcination temperature from $600^{\circ}C$ to $700^{\circ}C$ and then increased gradually with increasing the calcination temperature from $700^{\circ}C$ to $900^{\circ}C$. It was revealed that the remarkable increase in electrical conductivity could be attributed to phase transition of $TiO_2$ nanofibers from anatase to rutile at the temperature range from $600^{\circ}C$ to $700^{\circ}C$.

Calcination Characteristics of High-purity Limestone from the Pungchon Limestone in the Quicklime Manufacture (생석회 제조 공정에서의 풍촌층 고품위 석회석의 소성 특성)

  • Noh, Jin-Hwan;Lee, Hyun-Chul
    • Journal of the Mineralogical Society of Korea
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    • v.21 no.2
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    • pp.209-224
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    • 2008
  • Various types of high-purity limestone, which occurred in the Pungchon Formation, are examined to understand applied-mineralogical factors controlling their calcination characters with respect to the ore characters. To do this work, systematic characterization and determination were carried out for the limestone ores and their calcination products in a fixed heating condition, and the results were correlated and discussed. During the calcination experiment, a phase transition from calcite to quicklime begins to occur selectively in the physical weak zones such as grain boundary, cleavage and twin planes. All the fabrics of original limestones are preserved in the resultant quicklime. In addition, crystallinity of the quicklime was advanced, as the aging time of calcination was increased. Major controlling factors on the calcination effects of the high-purity limestone are elucidated to be the degree of development of cleavage and twin, together with crystallinity and textures in the limestone ore. Especially, lower crystallinity and dense interlocking fabrics obviously play advantageous role in all the calcination characters. But the development of cleavage and twin affects negatively on the calcination characters on account of favoring decrepitaion of quicklime in the lime manufacturing. Thus, the high-purity limestones characteristic of marble fabrics and relatively lower crystallinity are comparatively advantageous for the uses of lime manufacture.

Characteristics of $TiH_2$ under High Pressure (고압하에서 $TiH_2$의 특성화 연구)

  • Kim, Young-Ho
    • Journal of the Mineralogical Society of Korea
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    • v.5 no.2
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    • pp.72-78
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    • 1992
  • The Earth outer core accomodates moderately considerable amount of lighter elements than pure iron itself. Hydrogen is one of the possible candidates of minor constituents in the outer core. It would be worth while to extend for the pressure effect on the solubility of hydrogen in the metal-hydrides including iron hydride. In view of hydrogen being one of the potential substitutes for petroleum, searching a more efficient way for storing hydrogen in the form of hydrides is of considerable value. For two purposes, $TiH_2$was selected among lot of hydrides for its characteristics under pressure and temperature. There have been two kinds of experiment carried out on $TiH_2$ under different experimental conditions. As one of these attempts, polycrystalline $TiH_2$ was loaded up to 15 GPa stepwise at the constant temperature 500${\circ}$ using a piston-cylinder diamond anvil cell equipped with a miniature furnace of an electric power supply. The X-ra diffraction technique was employed on the quenched samples after the simultaneous high pressure and temperature treatments. During these high pressure-temperature runs, and irreversible phase of $TiH_2$ has been observed at the pressures higher than 11.3 GPa, which would be assigned to the orthorhombic crystal system as one of the new phase(s) of $TiH_2$. Molar volume change on this phase transition is ∼10%.

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Biological activities of some organometalic compounds as artificial nuclease (인공핵산 분해효소로서 몇 가지 유기금속 화합물들의 생물활성)

  • Sung, Nack-Do;Kim, Dae-Whang;Kwon, Byung-Mok;Kim, Tae-Young;Suh, Il-Hwan
    • The Korean Journal of Pesticide Science
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    • v.4 no.1
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    • pp.32-37
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    • 2000
  • A series of transition metal complexes of 3,6-bis(6'-methyl-2'-pyridyl)pyridazine ($L^{1}$) and 3,6-bis(2'-pyridyl)pyridazine ($L^{2}$) as artificial nuclease, $1{\sim}8$ were synthesized. After determining of X-ray crystal structure, hydrolysis rate constants of phosphates, as DNA model compound and biological activities were confirmed. $L^{2}$-Zn(II) complex, 8 was shown the best hydrolysis rate constant. The $L^{2}$-Ni(II) complex, 5 and $L^{2}$-Co(II) complex, 6 showed the highest herbicidal activity against SCP (Scriptus Juncoids) with excellent tolerance to rice, ORY (Oryzae sativa L.). And the $L^{1}$-Co(II) complex, 2, $L^{1}$-Zn(II) complex, 4 and ligand ($L^{1}$ amp; $L^{2}$) displayed above 90% fungicidal activity against MAG (Magnaporthe grisea).

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Observations on the Modulated Structure in Pyrochlore-type Compounds, $In_2(Ti_{1.7}Zn_{0.3})O_{0.67}$ and $In_2(Ti_{1.7}Mg_{0.3})O_{6.7}$ (Pyrochlore형 화합물 $In_2(Ti_{1.7}Zn_{0.3})O_{0.67}$$In_2(Ti_{1.7}Mg_{0.3})O_{6.7}$에서의 변조구조 관찰)

  • Lee, Hwack-Joo;Park, Hyun-Min;Cho, Yang-Koo;Ryu, Hyun;Nahm, Sahn;Bando, Y.
    • Applied Microscopy
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    • v.29 no.4
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    • pp.471-477
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    • 1999
  • Microstructural observations on the pyrochlore-type $Lu_2Ti_2O_7$ and the similar type of compounds, $In_2(Ti_{1.7}Zn_{0.3})O_{6.7}$ and $In_2(Ti_{1.7}Mg_{0.3})O_{6.7}$ which were made by the isothermal heat-treatment at 1623K for 18 days in Pt tube, were carried out using a top-entry HRTEM working at 200 kV. The modulated structures were found in both compounds, however, not in $Lu_2Ti_2O_7$. From the electron diffraction pattern analysis, the modulated superlattices are incommensurate and are 2.69 times of sublattices along (220) direction. The high resolution TEM images have shown that the superlattices consist of alternate superlattices which are composed of two or three sublattices, resulting in the average of 2.7 times of sublattices in accordance with the analysis of electron diffraction patterns. The crystal structures of both compounds are found to quite similar to those of pyrochlore, however the evidence that the cubic axes are slightly deviated from right angle. The modulated structure has gradually changed to the unmodulated structure induced by electron irradiation.

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