• Title/Summary/Keyword: X-선 구조분석

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In situ Synchrotron X-ray Techniques for Structural Investigation of Electrode Materials for Li-ion Battery (방사광 X-선을 이용한 리튬이온전지 소재의 실시간 구조 분석 연구)

  • Han, Daseul;Nam, Kyung-Wan
    • Ceramist
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    • v.22 no.4
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    • pp.402-416
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    • 2019
  • The development of next-generation secondary batteries, including lithium-ion batteries (LIB), requires performance enhancements such as high energy/high power density, low cost, long life, and excellent safety. The discovery of new materials with such requirements is a challenging and time-consuming process with great difficulty. To pursue this challenging endeavor, it is pivotal to understand the structure and interface of electrode materials in a multiscale level at the atomic, molecular, macro-scale during charging / discharging. In this regard, various advanced material characterization tools, including the first-principle calculation, high-resolution electron microscopy, and synchrotron-based X-ray techniques, have been actively employed to understand the charge storage- and degradation-mechanisms of various electrode materials. In this article, we introduce and review recent advances in in-situ synchrotron-based x-ray techniques to study electrode materials for LIBs during thermal degradation and charging/discharging. We show that the fundamental understanding of the structure and interface of the battery materials gained through these advanced in-situ investigations provides valuable insight into designing next-generation electrode materials with significantly improved performance in terms of high energy/high power density, low cost, long life, and excellent safety.

Mn K-Edge XAS Analyses of $Zn_{2-x}Mn_xSiO_4$ Phosphors ($Zn_{2-x}Mn_xSiO_4$ 형광체의 망간 K 흡수단 엑스선 흡수 분광 분석)

  • Choi, Yong Gyu;Lim, Dong Sung;Kim, Kyong Hon;Sohn, Kee Sun;Park, Hee Dong
    • Journal of the Korean Chemical Society
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    • v.43 no.6
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    • pp.636-643
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    • 1999
  • Green-emission intensity of a $Zn_{2-x}Mn_xSiO_4$ phosphor, which is a potential candidate as a green component in PDP device, significantly increases provided that the compound is additionally heat treated at 900$^{\circ}C$ after solid state reaction at 1300$^{\circ}C$. In order to verify origin of such an intensity enhancement after the additional heat treatment in association with the electronic and local structural change at around Mn ions, the Mn K-edge X-ray absorption spectra were recorded. From the analyses of the preedge peak corresponding to $1s{\rightarrow}3d$ bound state transition and XANES spectrum, it is known that most Mn ions are in +2 oxidation state and substitute Zn ion site regardless of the thermal treatment. In addition, EXAFS analyses revealed that Mn ions formed $MnO_4$ tetrahedra with the Mn-O bond length shortened by 0.01${\AA}$ and with reduced Debye-Waller factor in the thermally treated sample.

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Synthesis and Characterization of Tetradentate N2O2 Schiff Base Ligand and its Rare Earth Metal Complexes (사배위 N2O2 Schiff 염기 리간드와 그 희토류 금속착물의 합성 및 특성)

  • Shelke, Vinod A.;Jadhav, Sarika M.;Shankarwar, Sunil G.;Munde, chut S.;Chondhekar, Trimbak K.
    • Journal of the Korean Chemical Society
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    • v.55 no.3
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    • pp.436-443
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    • 2011
  • The solid complexes of La(III), Ce(III), Pr(III), Nd(III), Sm(III) and Gd(III) with 4-hydroxy-3-(1-{2-(2,4-dihydroxy-benzylidene)-amino phenylimino}-ethyl)-6-methyl-pyran-2-one ($H_2$L) derived from o-phenylenediamine, 3-acetyl-6-methyl-(2H)pyran,2,4(3H)-dione (dehydroacetic acid or DHA) and 2, 4-dihydroxy benzaldehyde have been synthesized and characterized by elemental analysis, conductometry, magnetic susceptibility, UV-visible, FT-IR, $^1H$-NMR, X-ray diffraction, thermal analysis study, and screened for antimicrobial activity. The FT-IR spectral data suggest that the ligand behaves as a dibasic tetradentate ligand with ONNO donor atoms sequence towards central metal ion. From the microanalytical data, the stoichiometry of the complexes has been found to be 1:1 (metal: ligand). The physico-chemical data suggests distorted octahedral geometry for La(III), Ce(III), Pr(III), Nd(III), Sm(III) and Gd(III) complexes. The X-ray diffraction data suggests monoclinic crystal system for La(III) and Ce(III) and orthorombic crystal system for Pr(III) and Nd(III) complexes. Thermal behavior (TG/DTA) of the complexes was studied and kinetic parameters were determined by Horowitz-Metzger and Coats-Redfern methods. The ligand and its metal complexes were screened for antibacterial activity against Staphylococcus aureus, Escherichia coli, Bacillus Sp. and fungicidal activity against Aspergillus Niger, Trichoderma and Fusarium oxysporum.

Selective Oxidation of Acrolein over Cupric Salt of 12-Molybdophosphoric Acid (12-몰리브도 인산 동염 촉매상에서 아크롤레인의 선택 산화반응)

  • Kim, Kyung-Hoon;Na, Suk-Eun;Park, Dae-Won
    • Applied Chemistry for Engineering
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    • v.4 no.4
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    • pp.721-730
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    • 1993
  • Various catalysts of $Cu_xH_3-{_{2x}}PMo_{12}O_{40}{\cdot}_nH_2O$ with different x-values have been prepared and characterized by thermal analysis, X-ray powder diffraction, infrared spectroscopy, BET surface-area measurement, electron microscopy, and temperature programmed desorption of ammonia. The properties of these catalysts in acrolein oxidation have been investigated in a continuous-flow fixed-bed reactor. The catalysts lost their water of crystallization at about $200^{\circ}C$ and their constitutional water between 300 and $400^{\circ}C$. The Keggin structure of the catalysts was identified by infrared spectroscopy. The decomposition of Keggin anion, $(PMo_{12}O_{40})^{3-}$, was increased with the increase of substituted copper content and identifiable $MoO_3$ and $P_2O_5$ as decomposition products were observed. The conversion of acrolein decreased with the increase of x probably due to the decrease of specific surface area and of total amount of acid sites. But specific reaction rate and selectivity to acrylic acid were maximized at x=1.0, and it showed specific acid site distributions.

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Study on the Structural and Transporting Property of Sr2Ru1-xCuxO4-y(0.0≤x≤0.5) (Sr2Ru1-xCuxO4-y(0.0≤x≤0.5) 화합물의 구조 및 전달 특성에 대한 연구)

  • Park, Jung-Chul
    • Journal of the Korean Chemical Society
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    • v.47 no.6
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    • pp.614-618
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    • 2003
  • $Sr_2Ru_{1-x}Cu_xO_{4-y}(0.0{\le}x{\le}0.5)$ compounds were prepared using a conventional solid state reaction. Based on the Rietveld refinements of X-ray diffraction results, it is revealed that $Sr_2Ru_{1-x}Cu_xO_{4-y}$ compounds are the single phases with K2NiF4 type tetragonal system in the range of 0=x=0.3, while the mixed phases of$Sr_2RuO_4$ and $Sr_2CuO_3$ in the range of $0.4{\le}x{\le}0.5$. By means of X-ray photoelectron spectroscopy, the valence states of Ru and Cu in $Sr_2Ru_{1-x}Cu_xO_{4-y}$, have been confirmed to 4+ and 2+, respectively. The bond length difference between $Ru-O_1 ({\times}4)\;and\;Ru-O_2 ({\times}2)\;in\;RuO_6$ octahedron is gradually decreased with increasing Cu content in $Sr_2Ru_{1-x}Cu_xO_{4-y}$, which results in the lower c/a ratio. So, it might be assured that the variation of local symmetry of $RuO_6$ octahedron is very closely related to the transporting property of $Sr_2Ru_{1-x}Cu_xO_{4-y}$ compounds. The behavior of resistivity discloses that the metallic property in $Sr_2RuO_4$ changes into the semiconducting one in proportion to the Cu content in $Sr_2Ru_{1-x}Cu_xO_{4-y}$.

Quantitative Analysis of Eupatilin and Jaceosidin in Artemisia herba (약쑥 함유 Eupatilin과 Jaceosidin 성분의 분석)

  • Ryu Su-Noh;Kang Sam Sik;Kim Ju Sun;Ku Bon Il
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.49 no.6
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    • pp.452-456
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    • 2004
  • Artemisia Herb is the dry aboveground part of Artemisia asiatica (Compositae). This is listed officially in the Korean Herbal Pharmacopoeia and used mainly in stopping all kinds of bleeding, regulating menses and curing menstrual disorders as well as in alleviating pain. Eupatilin and jaceosidin were isolated from Sazabalsuk and Sajuarisuk. and identified by means of spectral methods $(UV,\;^1H\;and\;^{13}C-NMR,\;MS) $ and quantitative analysis using HPLC. Regression equations for two flavonoid component standards obtained from Artemisia asiatica were $y=76069_x\;+\;107329\;(r=0.9999^{**})$ for eupatilin, $y=76651_x\;+\;77399\;(r=0.9996^{**})$ for jaceosidin. The eupatilin content of Sazabalsuk was 240mg, jaceosidin was 10mg in 100 g dry leaves. The Sajuarisuk were 330mg, 123mg in 100g dry leaves, respectively.

A Study on the Resin Finishing of Silk Fabric -Silicone Resin Finishing- (견직물의 수지가공에 관한 연구)

  • 남중희;탁태문
    • Journal of Sericultural and Entomological Science
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    • v.27 no.2
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    • pp.28-39
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    • 1985
  • The structural and useful characteristics of silk habutae treated with silicone resin by emulsion finishing method were studied. The results were obtained through crease recovery test, water repellency test, scanning micrograph observation, amino acid analysis, X-Ray diffraction analysis, and Fourier Transform Infrared Spectroscopy. The results are summarized as follows; 1) The improvement in crease recovery of silk habutae finished with silicone resin, was observed b soaping treatment and curing conditions. 2) The higher water repellency and stiffness in silk fabrics finished with silicone resin was found by the fabric inspection and the scanning electron microscopic observation. It is suggested that silicone resin impregnated into the void of silk fibroin. 3) The polar side chains of amino acid composition were decreased, when the silicone resin was treated on silk fibroin. 4) Through Amino acid analysis of silicone resin finished fibroin, the different amounts of amino acid composition was indicated due to silk fibroin silicone polymer reaction and the structural difference of its fibroin were also proved by X-ray diffractograms. 5) The functionality of the siloxane compound may be deduced from the silicone finished silk habutae by Fourier Transform Spectroscopy. It was concluded from the above results that the useful characteristics of silk fabric can be improved by silicone resin finishing.

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A Study of Oxidation Behavior on the Surface of Nd-Fe-B Ribbon Alloy by X-ray Photoelectron Spectroscopy (X-선 광전자 분광법에 의한 Nd-Fe-B 리본합금으 표면 산화거동 연구)

  • Chung, Kang-Sup;Sung, Hak-Je;Kim, Kun-Han;Park, Yun-Chang;Lee, Kyoung-Chul;Shu, Su-Jeong
    • Analytical Science and Technology
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    • v.8 no.3
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    • pp.351-358
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    • 1995
  • Oxidation behavior on the surface of Nd-Fe-B ribbon alloy has been studied by X-ray Photoelectron Spectroscopy. In the incipient stage of oxidation on the surface of "as-received" ribbon Nd-oxide film was formed from the fast oxidation of Nd and Fe was metal state in bulk. In process of oxidation time Fe was more abundant in the outmost surface of ribbon from the defused Fe through Nd-oxide film and layer structure of oxidation film was formed.

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Preparation of electrostatic spray pyrolysis derived nano powder and hydroxyapatite forming ability (정전분무 열분해법에 의한 나노분말의 제조 및 하이드록시 아파타이트 형성능력 평가)

  • Lee, Young-Hwan;Jeon, Kyung-Ok;Jeon, Young-Sun;Lee, Ji-Chang;Hwang, Kyu-Seog
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.16 no.6
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    • pp.244-249
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    • 2006
  • Electrostatic spray pyrolysis, a novel fabrication technique, has been used in this study to prepare calcium phosphate nano powders. Final annealing was done at $400^{\circ}C$ for 30min in air. The hydroxyapatite - forming ability of the annealed powder has been evaluated in Eagle's minimum essential medium solution (MEM). X-ray diffraction analysis, field emission - scanning electron microscope, energy dispersive X-ray spectroscope, and Fourier transform infrared spectroscope were used to characterized the annealed powders after immersion in MEM. The powder with an amorphous structure induced hydroxyapatite formation on their surfaces after immersion fer 15 days.

DC-sputtering으로 증착한 IZO 박막의 열처리 온도에 따른 구조적 특성

  • Kim, Jun-Ho;Mun, Jin-Yeong;Kim, Hyeong-Hun;Lee, Ho-Seong;Han, Won-Seok;Jo, Hyeong-Gyun;Kim, Heung-Seung
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.06a
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    • pp.468-468
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    • 2008
  • IZO(Indium zinc oxide) 박막은 화학적으로 안정하면서, 가시광 영역 (380~780 nm)에서 80% 이상의 높은 투과도와 낮은 전기비저항, 3.5 eV 이상의 넓은 밴드갭 특성을 가진다. IZO 박막의 이러한 특성 때문에 평판표시소자 (Flat Panel Display; FPD) 및 태양전지와 같은 광전소자들의 차세대 투명전도성 산화물(Transparent Conducting Oxide; TCO) 박막 재료로 주목 받고 있다. 특히 평판표시소자(FPD)들의 고해상도, 대면적화 및 경량화로 인해 투명전극용 박막의 고품위 특성이 요구되고 있다. 현재 투명 전극으로 널리 사용되고 있는 고가의 ITO(indium tin oxide)를 대체할 다성분계 산화물 투명 전극 중에서 투광성과 전기전도도가 좋은 IZO 박막에 대한 많은 연구가 진행되고 있다. 이러한 IZO 박막의 광학적, 전기적 특성은 박막 내의 조성 차이와 미세구조에 의해 결정된다. 따라서 고품위의 IZO 박막 형성을 위해서 결정구조와 미세구조에 대한 분석이 필수적이다. 본 연구에서는 Si(100) 기판 위에 DC-sputtering으로 증착한 IZO 박막의 열처리 온도에 따른 구조적 특성을 알아보기 위해 300~$600^{\circ}C$ 공기분위기에서 1시간 동안 열처리 하였다. 표면 형상(surface morphology)은 원자현미경(AFM). 결정구조는 X-선 회절(XRD)로 분석하였고, 미세구조는 투과전자현미경(TEM)으로 관찰하였다.

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