• 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.

• 방사성폐기물학회지
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• 제8권3호
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• pp.201-205
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• 2010

고준위방사성폐기물에서 유출되어 나오는 아이오딘의 이동을 저지하기 위하여 은을 흡착시킨 벤토나이트 블록에 NaI 용액을 흘려주었을 때 대부분의 아이오딘이 흡착되었다. 이 은이온에 의한 아이오딘의 저지 메커니즘을 상세히 조사하기 위하여 아이오딘과 접촉하기 전후의 은이 흡착된 벤토나이트의 X-ray Absorption Near Edge Structure (XANES)와 Extended X-ray Absorption Fine Structure (EXAFS) 스펙트 럼과 표준물질로서 AgO, $Ag_2O$, AgI의 스펙트럼을 비교하였다. 그 결과, 벤토나이트에 흡착되었던 은이 떨어져 나와 AgI 침전 클러스터를 형성함으로서 아이오딘의 이동이 지연되는 것으로 생각된다.

• Bulletin of the Korean Chemical Society
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• 제21권6호
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• pp.588-594
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• 2000

Structural changes of an iron phthalocyanine (FePC) monolayer induced by adsorption and externally applied potential on high area carbon surface have been investigated in situ by iron K-edge X-ray absorption fine structure (XAFS) in 0.5 M $H_2S0_4.$ Fine structures shown in the X-ray absorption near edge structure (XANES) for microcrystalline FePC decreased upon adsorption and further diminished under electrochemical conditions. Fe(II)PC(-2) showed a 1s ${\rightarrow}$ 4p transition as poorly resolved shoulder to the main absorption edge rather than a distinct peak and a weak 1s ${\rightarrow}$ 3d transition. The absorption edge position measured at half maximum was shifted from 7121.8 eV for Fe(lI)PC(-2) to 7124.8 eV for $[Fe(III)PC(-2)]^+$ as well as the 1s ${\rightarrow}$ 3d pre-edge peak being slightly enhanced. However, essentially no absorption edge shift was observed by the 1-electron reduction of Fe(Il)PC(-2), indicating that the species formed is $[Fe(II)PC(-3)]^-$. Structural parameters were obtained by analyzing extended X-ray absorption fine structure (EXAFS) oscillations with theoretical phases and amplitudes calculated from FEFF 6.01 using multiple-scattering theory. When applied to the powder FePC, the average iron-to-phthalocyanine nitrogen distance, d(Fe-$N_p$) and the coordination number were found to be 1.933 $\AA$ and 3.2, respectively, and these values are the same, within experimental error, as those reported ( $1.927\AA$ and 4). Virtually no structural changes were found upon adsorption except for the increased Debye-Wailer factor of $0.005\AA^2$ from $0.003\AA^2.$ Oxidation of Fe(II)PC(-2) to $[Fe(III)PC(-2)]^+$ yielded an increased d(Fe-Np) (1 $.98\AA)$ and Debye-Wailer factor $(0.005\AA^2).$ The formation of $[Fe(II)PC(-3)]^-$, however, produced a shorter d(Fe-$N_p$) of $1.91\AA$ the same as that of crystalline FePC within experimental error, and about the same DebyeWaller $factor(0.006\AA^2)$.

• 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.

• 한국재료학회지
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• 제4권6호
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• pp.620-625
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• 1994

자자들은 최근 비고용 Cu-Ta계의 기계적 합금화(Mechanical Alloying) 방법을 이용하여 이계에 있어서 비정질상의 형성에 대한 구조적 확인을 중성자 회절과 EXAFS(Extended X-ray Absorption Fine Structure)의 실험결과로 부터 얻었다. Cu-Ta계와 같이 혼합 엔탈피(Heat of Mixing: $\Delta$ Hmix)가 정인계에 있어서 비정질상 형성에 대한 연구는 구조적인 측면 뿐만 아니라. 시료의 전자물성에 대해서도 많은 연구가 되어야만 할 것으로 사료된다. 따라서 본 논문에서는 120시간 MA방법으로 제작한 시료에 대하여 초전도 천이온도 및 X선 광전자분광 실험에서 얻은 가전자대 구조의 전자물성을 측정하고, 그 결과로부터 이종원자 Cu와 Ta간의 결합은 화하결합에 의한 생성임을 확인하였는데, 이들 결과로부터 120시간 MA를 행하여 얻어진 시료는 확실하게 비정질 합금임을 알 수 있었다.

• 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.

• Journal of Electrochemical Science and Technology
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• 제1권1호
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• pp.31-38
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• 2010

In this study, we have demonstrated the fine structure effect of PdCo electrocatalyst on oxygen reduction reaction activity with different alloy composition and heat-treatment time. In order to identify the intrinsic factors for the electrocatalytic activity, various X-ray analyses were used, including inductively coupled plasma-atomic emission spectrometer, transmission electron microscopy, X-ray diffractometer, and X-ray Absorption Spectroscopy technique. In particular, extended X-ray absorption fine structure was employed to extract the structural parameters required for understanding the atomic distribution and alloying extent, and to identify the corresponding simulated structures by using FEFF8 code and IFEFFIT software. The electrocatalytic activity of PdCo alloy nanoparticles for the oxygen reduction reaction was evaluated by using rotating disk electrode technique and correlated to the change in structural parameters. We have found that Pd-rich surface was formed on the Co core with increasing heating time over 5 hours. Such core shell structure of PdCo/C showed that a superior oxygen reduction reaction activity than pure Pd/C or alloy phase of PdCo/C electrocatalysts, because the adsorption energy of adsorbates was apparently reduced by lowering the dband center of the Pd skin due to a combination of the compressive strain effect and ligand effect.

• 자원환경지질
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• 제45권2호
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• pp.205-215
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• 2012

금속이온은 토양이나 퇴적물 내의 광물에 수착되어 고착화될 수 있다. 여기서는 광물 표면의 화학적 특성과 금속이온의 수착에 관련된 이론 및 수착 연구를 위한 X-선 흡수 미세구조(extended X-ray absorption fine structure, EXAFS) 분석방법에 대해 알아보고 금속이온의 광물표면 수착에 관한 원자 단위 연구 결과를 정리하였다. 광물표면의 특성과 금속이온의 수착에 관한 원자 단위 이론의 이해는 원자 단위 분광법의 분석을 수행하는데 있어서 기초가 된다. 여기에 정리된 원자 단위 수착상 연구 결과는 외부권 착물, 내부권 착물, 표면침전뿐 아니라 공침전, 삼성분 착물, 수착반응 시간의 효과, 탈착가능성을 포함한다.

• 한국진공학회:학술대회논문집
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• 한국진공학회 1997년도 제12회 학술발표회 논문개요집
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• pp.178-178
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• 1997

• 한국진공학회지
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• 제6권S1호
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• pp.127-132
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• 1997

Microstructure of the Fe-Ti system by ion beam mixing of multilayers at 300 K and 77 K has been studied in a wide composition range. The ion bombardment was carried out using $Ar^+$ ions at 80 keV. Using grazing angle x-ray diffraction we find that the lattice parameters of these bcc solid solutions are very close to that of $\alpha$-Fe. Extended x-ray absorption fine-structure spectroscopy have been performed to investgate the short-range order in the ion-beam-mixed state. The structure parameters, such as the interatomic distance and the coordination number are estmated from the Fe K-edge Fourier filtered EXAFS spectra. The interatomic distance is independent of the alloy concentration and it is almost constant. The study of x-ray absorption near-edge structure gives information on the individual $\rho$components of the partial densityof states of the conduction band of the Fe and Ti We also find that a charge transfer from Ti to Fe atoms takes place.