• 제목/요약/키워드: x-ray absorption spectroscopy

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비소 및 중금속 오염토양 안정화 분야에서의 X선 흡수분광법(XAS) 활용 (Application of X-ray Absorption Spectroscopy (XAS) in the Field of Stabilization of As and Heavy Metal Contaminated Soil)

  • 임정은;문덕현;김권래;옥용식
    • Journal of Applied Biological Chemistry
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    • 제58권1호
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    • pp.65-74
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    • 2015
  • X선 흡수분광법(X-ray absorption spectroscopy, XAS)을 이용하는 X선 흡수미세구조(X-ray absorption fine structure, XAFS)의 분석은 다양한 학문분야에서 적용되고 있다. 본 연구에서는 XAFS 분석을 위한 토양 시료의 준비에서부터 XAFS 측정 후 X선 흡수 끝머리 부근 미세구조(X-ray absorption near edge structure, XANES) 및 광범위 X선 흡수 미세구조(extended Xray absorption fine structure, EXAFS) 데이터를 추출하여 연구에 활용하는 것에 대해 간략하게 소개하였다. 특히 토양환경 분야에서 XANES 및 EXAFS 분석을 활용한 선행연구들에 대해 비소(As) 및 중금속 주요 원소(Cd, Cu, Ni, Pb, Zn)별로 그 내용을 정리하였다. 토양환경 분야에서 XAFS의 응용은 납(Pb)의 화학종 규명에 관한 연구가 가장 많은 것으로 나타났다. 이와 함께 대부분의 연구들은 오염토양 내 중금속 화학종의 규명을 통해 중금속의 유입 원인 등에 대해 기술하고 있으며, 이를 정화하기 위한 다양한 방법들(개량제 처리, 식물정화)을 적용한 후, 안정화된 중금속 화학종을 XANES 및 EXAFS 분석을 통해 규명하여 정화 방법들의 효율성과 안정성에 대해 보고하였다.

In Situ X-ray Absorption Spectroscopic Study for α-MoO3 Electrode upon Discharge/Charge Reaction in Lithium Secondary Batteries

  • Kang, Joo-Hee;Paek, Seung-Min;Choy, Jin-Ho
    • Bulletin of the Korean Chemical Society
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    • 제31권12호
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    • pp.3675-3678
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    • 2010
  • In-situ X-ray absorption spectroscopy (XAS) was used to elucidate the structural variation of $\alpha-MoO_3$ electrode upon discharge/charge reaction in a lithium ion battery. According to the XAS analysis, hexavalent Mo atoms in $\alpha-MoO_3$ framework are reduced as the amount of intercalated lithium ions increases. As lithium de-intercalation proceeds, most of pre-edge peaks are restored again. However, according to the Fourier transforms of the extended X-ray absorption fine structure (EXAFS) spectra, lithium de-intercalation reaction is partially irreversible upon the charge reaction, which is one of the main reasons why the capacity of $\alpha-MoO_3$ electrode decreases upon successive discharge/charge cycles.

Absorption Spectroscopy of Biological Specimens Near X-ray Absorption Edges of Constituent Elements

  • Ito, Atsushi;Shinohara, Kunio
    • Journal of Photoscience
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    • 제9권2호
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    • pp.460-462
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    • 2002
  • Absorption spectra of biological specimens in the soft X-ray region have been presented with special reference to the XANES (X-ray absorption Near Edge Structure) of constituent elements. Absorption spectrum in this wavelength region is characterized by the absorption edges from which elemental content could be derived. In addition, XANES has a characteristic profile for chemical environment around the element such as chemical bond. Using the specific absorption peak we can assign not only the chemical bond but also molecules having such a chemical bond. In the present paper, absorption spectrum of DNA was measured in the wavelength range from 1.5nm to 5nm. Spectrum of Chinese Hamster Ovary (CHO) cells was compared with the DNA spectrum. XANES were distinct at the K absorption edges of major elements, C, N and O. In the spectrum of the cells prominent peaks at the L absorption edge of minor element Ca were also detectable. XANES profiles in small local areas in a cell could also be measured in combination with X-ray microscopy. These give information about local chemical environment in a cell. XANES at the phosphorus K absorption edge in a human HeLa cell was successfully obtained corresponding to a sharp and intensive XANES peak of DNA.

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A Practical Method to Correct the Saturation Effect in XMCD Spectra

  • Kim, J.Y.
    • Journal of Magnetics
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    • 제13권3호
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    • pp.85-87
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    • 2008
  • I report a simple method to correct the saturation effect in absorption spectra measured in total electron yield (TEY) mode. It does not require additional measurements of the X-ray penetration depth. In order to check the reliability of the method, X-ray magnetic circular dichroism (XMCD) spectra for polycrystalline Fe were measured at two different incident angles, and then processed with the method. The two resultant XMCD spectra were identical, and their sum rule analysis produced the ratios of orbital magnetic moment to spin magnetic moment, which were very close to the well-known value.

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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X-Ray Absorption Spectroscopy: A Complementary Tool for Structural and Electronic Characterization of Solids

  • Jean Etourneau
    • Bulletin of the Korean Chemical Society
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    • 제19권1호
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    • pp.5-21
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    • 1998
  • The purpose of this paper is to show that X-ray absorption spectroscopy (XANES and EXAFS) is a powerful technique for characterizing both crystalline and amorphous solids from structural (local order) and electronic point of view. The principle of this technique is briefly described by showing the main factors which must be considered for recording and fitting the experimental results. Some non-trivial examples have been selected for demonstrating that XAS spectroscopy is the only technique for bringing a definitive answer as for example: the determination of the local distortion of the $NiO_6$ octahedra in the $Li_{1-z}Ni_{1+z}O_2$ layered oxides and the evidence of the presence of copper pairs in the NASICON-type phosphate $CuZr_2 (PO_4)_3$. Are also reported some significant examples for which XAS spectroscopy is decisive with other characterization methods as (i) Raman spectroscopy for glasses (ii) Mossbauer spectroscopy for $LiNi_{1+z-t}Fe_To_2$ oxides (iii) magnetic measurements for Ce-based intermetallic compounds.

Design of an Electron Ohmic-Contact to Improve the Balanced Charge Injection in OLEDs

  • 박진우;임종태;염근영
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2011년도 제40회 동계학술대회 초록집
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    • pp.283-283
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    • 2011
  • The n-doping effect by doping metal carbonate into an electron-injecting organic layer can improve the device performance by the balanced carrier injection because an electron ohmic contact between cathode and an electron-transporting layer, for example, a high current density, a high efficiency, a high luminance, and a low power consumption. In the study, first, we investigated an electron-ohmic property of electron-only device, which has a ITO/$Rb_2CO_3$-doped $C_{60}$/Al structure. Second, we examined the I-V-L characteristics of all-ohmic OLEDs, which are glass/ITO/$MoO_x$-doped NPB (25%, 5 nm)/NPB (63 nm)/$Alq_3$ (32 nm)/$Rb_2CO_3$-doped $C_{60}$(y%, 10 nm)/Al. The $MoO_x$doped NPB and $Rb_2CO_3$-doped fullerene layer were used as the hole-ohmic contact and electron-ohmic contact layer in all-ohmic OLEDs, respectively, Third, the electronic structure of the $Rb_2CO_3$-doped $C_{60}$-doped interfaces were investigated by analyzing photoemission properties, such as x-ray photoemission spectroscopy (XPS), Ultraviolet Photoemission spectroscopy (UPS), and Near-edge x-ray absorption fine structure (NEXAFS) spectroscopy, as a doping concentration at the interfaces of $Rb_2CO_3$-doped fullerene are changed. Finally, the correlation between the device performance in all ohmic devices and the interfacial property of the $Rb_2CO_3$-doped $C_{60}$ thin film was discussed with an energy band diagram.

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Local Structure Refinement of the $BaFe_{1-x}Sn_xO_{3-y}$ System with Fe K-Edge X-Ray Absorption (XANES/EXAFS) Spectroscopy

  • 김민규;곽기섭;로권선;여철현
    • Bulletin of the Korean Chemical Society
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    • 제18권7호
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    • pp.743-749
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    • 1997
  • Local structure refinement of the BaFe1-xSnxO3-y system (x=0.00-0.50) has been carried out with Fe K-edge x-ray absorpion spectroscopic studies. It is found out that the Fe ions are placed in two different symmetric sites such as tetrahedral and octahedral sites in the compounds by comparison with Fe K-edge x-ray absorption near edge structure (XANES) spectrum of the γ-Fe2O3 compound as a reference. Small absorption peaks of dipole-forbiden transitions appear at a pre-edge region of 7111 eV due to the existence of Fe ions in the tetrahedral and octahedral sites. The peak intensity decreases with the substitution amount of Sn ion. Three different absorption peaks of 1s→4p dipole-allowed transition appear on the energy region between 7123 and 7131 eV. The peaks correspond to 1s→4p main transition of Fe ions in tetrahedral and octahedral sites and 1s→4p transition followed by the shakedown process of ligand to metal charge transfer. The bond distances between Fe ions in the tetrahedral site and nearest neighboring oxygen atom (Fe-4O), and those in octahedral site (Fe-6O) are determined with the extended x-ray absorption fine structure (EXAFS) analysis. Two different interatomic distances increase with the substitution amount of Sn ion and also the bond lengths of Fe-4O are shorter than those of Fe-6O in all compounds.

Synthesis and Characterization of New Macroporous SnO2 Foams

  • Choi, Moon-Hyung;Paek, Seung-Min
    • Bulletin of the Korean Chemical Society
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    • 제34권5호
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    • pp.1388-1390
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    • 2013
  • Macroporous $SnO_2$ foam was successfully synthesized via a simple soft-chemical route by hybridization between alkylamine and tin(IV) oxide. According to X-ray diffraction (XRD) analysis, the as-prepared $SnO_2$ foam had a highly ordered lamella structure along the crystallographic c-axis, which transformed to a rutile phase after thermal treatment at $300^{\circ}C$. X-ray absorption spectroscopy (XAS) at the Sn K-edge revealed that $SnO_2$ particles in the hybrid material maintained their nanosized structure after hybridization with alkylamine. Scanning electron microscope (SEM) images clearly showed that the as-prepared $SnO_2$ foam had a macroporous structure. This synthetic route can be extended to the development of open frameworks with good electrochemical properties in battery applications.

Electronic structure studies of CoFeRO (R=Hf,La,Nb) thin films by X-ray absorption spectroscopy

  • Song, J.H.;Gautam, S.;Chae, K.H.;Asokan, K.
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2009년도 제38회 동계학술대회 초록집
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    • pp.378-378
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    • 2010
  • We report the electronic structure of CoFeO-R (R=Hf, La, Nb) thin films studied by x-ray absorption spectroscopy (XAS). These ferrites thin films were prepared by pulsed laser deposition method and characterized by XAS measurements at O K-, Co and Fe L-edges. The O K-edge spectra suggest that there is a strong hybridization between O 2p and 3d electrons of transition metal cations and Fe $L_{3,2}$-edge spectra indicate that Fe-ions exist in $Fe^{2+}$ with tetrahedral site of the spinel structure. Divalent Co ions is also distributed in tetrahedral site with rare earth ions goes to octahedral sites of spinel structure. X-ray magnetic circular dichroism (XMCD) is also used to explain the symmetry and magnetic nature dependence on rare-earth ions.

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