• 제목/요약/키워드: XAFS

검색결과 26건 처리시간 0.026초

Distribution of Co Ions in Ferromagnetic Zn (1-x) Co (x)O Films

  • 박창인;서수영;김정란;한상욱
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2012년도 제43회 하계 정기 학술대회 초록집
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    • pp.166-166
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    • 2012
  • We examined the distribution of Co ions of ferromagnetic n-type Zn(1-x)Co(x)O semiconducting films with the Co concentrations of 0.03~0.07 using x-ray absorption fine structure (XAFS) measurements at the Co and Zn K edges. Extended XAFS (EXAFS) revealed that Co ions mainly occupied the zinc sites of the films. X-ray absorption near edge structure (XANES) spectra demonstrated that the pre-edge peak of the Co K edge was substantially affected by the second neighboring Co ions at the zinc sites due to hybridizing of the Co 4p conduction electrons with the Co 3d bounded electrons. From XANES and EXAFS analysis using ab initio calculations, we found that Co ions uniformly occupied the zinc sites of the Zn (0.93) Co (0.07)O film, whereas the Co ions of the Zn (0.97) Co (0.03)O and Zn (0.95) Co (0.05)O films were substituted at localized zinc sites. The ferromagnetic properties of the Zn (0.93) Co(0.07)O film could be induced by direct interaction between the magnetic dipoles of the Co ions with a mean distance of 4.3 A or by Co 4p electron mediation.

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A Complexation Study of Novel Triaza and Hexaaza Macrocycles for the Use of Analytical Reagents

  • Wakita, Hisanobu;Yamaguchi, Toshio;Matsuki, Yuuichi;Kurisaki, Tsutomu
    • 분석과학
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    • 제8권4호
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    • pp.449-456
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    • 1995
  • Novel macrocyclic ligands modified with pendant arms, N, N', N'', N''', N'''', N'''''-hexakis(2-aminoethyl)-1, 4, 7, 10, 13, 16-hexaazacyclootadecane [$L_3$, Fig.1] and 1, 4, 7-tris(3-(o-hydroxyphenyl)propyl)-1, 4, 7-triazacyclononane [$L_4$, Fig.1] have been synthesized, and the protonation of $L_3$ and $L_4$ and stability constants of $L_3$ with bivalent transition metal ions and rare earth metal ions were determined by a potentiometry. The obtained results show that the complex formation of $L_3$ depends on the metal ligand ratios, and the stability of the metal complexes does not depend on the sizes of the metal ions, but on the nature of the metal ions. The structures of the rare earth complexes for $L_4$ were characterized by an X-ray absorption spectrometry(XAFS).

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Synthesis and Structural Properties of $VO_2$ Thin Films

  • Jin, Zhenlan;Park, Changin;Hwang, Inhui;Han, S.W.
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제45회 하계 정기학술대회 초록집
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    • pp.190.2-190.2
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    • 2013
  • Vanadium dioxide ($VO_2$) has been widely attracted for academic research and industrial applications due to its metal-insulator transition (MIT) temperature close to room temperature. We synthesized VOx film on (0001) sapphire substrate with vanadium target (purity: 99.9%) using DC magnetron sputtering in Ar ambience at a pressure of $10^{-3}$ Torr at $400{\sim}700^{\circ}C$. The VOx film subsequently was annealed at difference temperatures in ambience of Ar and $O_2$ gas mixture at $60{\sim}800^{\circ}C$. The structural properties of the films were investigated using scanning electron microscopic (SEM), x-ray diffraction (XRD) and x-ray absorption fine structure (XAFS) measurements. SEM reveal that small grains formed on the substrates with a roughness surface. XRD shows oriented $VO_2$(020) crystals was deposited on the $Al_2O_3$(006) substrate. From I-V measurements, the electric resistance near its MIT temperature were dramatically changed by ${\sim}10^4$ during heating and cooling the films. We will also discuss the temperature-dependent local structural changes around vanadium atoms using XAFS measurements.

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Temperature-dependent Structural and Magnetic Properties of Diamagnetic $HgI_2$

  • Park, C.I.;Jin, Zhenlan;Hwang, I.H.;Yeo, S.M.;Han, S.W.
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제45회 하계 정기학술대회 초록집
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    • pp.291.1-291.1
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    • 2013
  • We examined the temperature-dependent structural and magnetic properties of HgI2 in the temperature range of 300~400 K. HgI2 is a diamagnetic material and can be used for X-ray or γ-ray detectors. DCmagnetization measurements on HgI2 showed that there is a small but distinguishable change in its diamagnetic properties near 375 K. The magnetic property change is not expected because Hg and I are known as nonmagnetic elements. X-ray diffraction (XRD) measurements revealed a structural transition in the temperature of 350~400 K. Temperature-dependent x-ray absorption fine structure (XAFS) demonstrated that the chemical valence states of both Hg and I did not changed in the temperature range of 300~400 K. However, XAFS revealed that the bond-length disorder was slightly increased in the temperature range, particularly, near Hg atoms. The structural changes of HgI2 are likely related to its diamagnetic property change. We will discuss the relation between the diamagnetic properties and local structural properties of HgI2 in detail.

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Synthesis and Temperature-Dependent Local Structural Properties of Ti2O3

  • Hwang, Inhui;Jin, Zhenlan;Park, Changin;Jiang, Bingzhi;Han, S.W.
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제45회 하계 정기학술대회 초록집
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    • pp.202.2-202.2
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    • 2013
  • Ti2O3 is known as a typical Mott insulator with a transition temperature of near $200^{\circ}C$. Unlike VO2, Ti2O3 does not have a structural phase transition near the metal-insulator-transition (MIT) temperature. We investigated the temperature-dependent thermal vibration change using temperature-dependent x-ray absorption fine structure (XAFS) at Ti K-edge in the temperature range of 300~600 K. Ti2O3 powder and films were synthesized using thermal chemical vapor deposition (CVD) at $800{\sim}900^{\circ}C$. X-ray diffraction measurements show a single phased Ti2O3 at room temperature. XAFS confirmed no structural phase transition in the temperature of 300~600 K. A small but distinguishable structural disorder change was observed near the transition temperature. We will discuss the MIT behavior with the change of structural disorder.

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이차전지 양극활물질의 chemical state 측정을 위한 X0ray Induced Electron Emission Spectroscopy (XIEES)의 활용

  • 이재철;송세안;임창빈
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2000년도 제18회 학술발표회 논문개요집
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    • pp.167-167
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    • 2000
  • 전지 재료의 충방전 과정 연구에는 X-선 분말회절(x-ray powder diffraction techniques)과 중성자회절을 많이 사용하였다. 하지만 이러한 분석기술은 long-range order의 구조에 관한 정보를 제공하는데 유용하지만 atomic scale의 구조에 관한 정보를 얻기에는 한계가 있다. Li 전지에서의 전기화학적 반응에서는 cathode 물질에 포함된 전이금속의 산화, 환원 반응에 의한 Li 이온의 intercalation (charge process)과 deintercalation (discharge process) 현상이 일어난다. 이러한 충방전 과정은 알려지지 않은 다양한 형태의 위상 변화를 동반하게 되는데 x-선 이나 중성자를 이용한 powder diffraction techniques 로는 단지 정성적인 결정학적 정보를 얻을 수 있다. 따라서 최근에 원자 단위의 local structure에 관한 정보와 electrochemical state에 관한 정보를 동시에 얻을 수 있는 X-ray Absorption Fine Structure (XAFS) 분석기술을 Li 전지분석에 활용하기 시작하였다. XAFS는 하나의 x-ray 흡수원자에 대해서 주변원자들의 원자구조에 관한 정보와 구성 원소의 electrochemical state에 관한 정보를 얻을 수 있는 분석방법이다. X-ray Induced Electron Emission Spectroscopy (XIEES)는 x-ray에 의해서 방출된 전자를 검출하여 스펙트럼을 얻는 기능을 함축적으로 나타낸 것으로, x-ray를 물질 표면에 조사하여 발생하는 광전자, Auger 전자, 이차전자 등을 전자검출기(Channel Electron Multiplier: CEM)로 검출하는 기능과, 시료를 투과한 x-ray와 시료에서 발생하는 형광 x-ray를 비례계수기로 검출하는 기능을 가지고 있다. 이러한 검출 능력을 바탕으로 EXAFS, XANES, Standing Wave Technique, Elemental Composition Analysis, DXRD, Total Reflection Technique 등을 이용하여 물질을 구성하고 있는 원소의 성분, 미세원자구조, 전자구조에 관한 정보를 얻을 수 있는 새로운 spectrometer이다. 본 연구에서는 자체 개발한 XIEES의 XAFS 기능을 이용하여 여러 가지 방법으로 제조한 LiMn2-xO4와 LiMnO2, MnO2에서 Mn K-absorption edge에 대한 chemical state 변화를 측정하였다. Absorption edge에서 chemical shift를 측정하기 위해서는 방사광 가속기 수준의 에너지 분해능(~0.3eV)이 필요하다. 이번 연구에서는 SiO2(3140) monochromator를 사용하고 여기에 맞는 적절한 parameter를 적용하여 x-ray 에너지 분해능을 포항방사광가속기 수준으로 개선하였다. XIEES에서 얻은 스펙트럼과 포항방사광가속기에서 얻은 스펙트럼을 비교하였다. Chemical shift가 일어나는 경향은 두 실험 결과가 잘 일치하였다.

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Synthesis of Graphene Oxide Based CuOx Nanocomposites and Application for C-N Cross Coupling Reaction

  • Choi, Jong Hoon;Park, Joon B.
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2014년도 제46회 동계 정기학술대회 초록집
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    • pp.176.1-176.1
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    • 2014
  • Graphene has attracted an increasing attention due to its extraordinary electronic, mechanical, and thermal properties. Especially, the two dimensional (2D) sheet of graphene with an extremely high surface to volume ratio has a great potential in the preparation of multifunctional nanomaterials, as 2D supports to host metal nanoparticles (NPs). Copper oxide is widely used in various areas as antifouling paint, p-type semiconductor, dry cell batteries, and catalysts. Although the copper oxide(II) has been well known for efficient catalyst in C-N cross-coupling reaction, copper oxide(I) has not been highlighted. In this research, CuO and Cu2O nanoparticles (NPs) dispersed on the surface of grapehene oxide (GO) have been synthesized by impregnation method and their morphological and electronic structures have been systemically investigated using TEM, XRD, and XAFS. We demonstrate that both CuO and Cu2O on graphene presents efficient catalytic performance toward C-N cross coupling reaction. The detailed structural difference between CuO and Cu2O NPs and their effect on catalytic performance are discussed.

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2015년 연료전지 자동차 판매를 눈앞에 둔 기술동향과 과제 (Review of commercial Fuel Cell Vehicle for 2015years)

  • 김유상
    • 한국표면공학회:학술대회논문집
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    • 한국표면공학회 2014년도 추계학술대회 논문집
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    • pp.149-149
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    • 2014
  • 연료전지의 성능향상을 가속하기 위해서는 연료전지 작동조건에서의 화학 상태를 직접 해석한 연후에 반응 기구를 결정하고, 활성지배 인자, 열화지배 인자를 명확히 하는 것이 중요하다. X-선 흡수 미세구조(XAFS; X-ray Absorption Fine Structure) 해석은 연료전지 작동조건에서 촉매의 전자상태, 국소구조를 직접 관측 가능한 유효한 도구이다. 2015년 일본에서는 연로전지 자동차 판매를 눈앞에 두고 있다. 이에 연료전지 성능평가도 중요하다. 본고에서는 X-선 흡수 미세구조 해석의 원리에 관하여 해설한 후, X-선 흡수기법을 코어 셀 촉매의 영역 해석에 적용한 사례에 관하여 기술하였다.

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High Catalytic Activity and Recyclability of Graphene Oxide Based Palladium Nanocomposites in Sonogashira Reaction

  • Kim, Bo Hyun;Park, Joon B.
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제45회 하계 정기학술대회 초록집
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    • pp.139.1-139.1
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    • 2013
  • Graphene and graphene oxide (GO) have been modified with palladium nanoparticles (Pd NPs) to develop high performance catalysts for the Sonogashira cross coupling reaction. To understand catalytic performance of Pd NPs on graphene (Pd/G) and Pd NPs on GO (Pd/GO), we monitored their morphological and electronic structural changes before/after Sonogashira reaction using FT-IR, XRD, XPS, and XAFS. Here, we demonstrate that both Pd/G and Pd/GO show high catalytic efficiency toward the Sonogashira reaction, but only Pd/GO revealed excellent recyclability. The remarkable catalytic efficiency of both catalysts is attributed to the high degree of the Pd NP dispersions on supports and thus smaller Pd NPs can provide highly reactive low coordinated Pd atoms. However, we attributed the excellent recyclability of Pd/GO to the presence of oxygen functionalities on GO, which can provide nucleation sites for the detached Pd atoms during the Sonogashira reaction and prevent agglomeration of the Pd NPs since the oxygen functional groups are very reactive to mobile Pd adatoms.

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