• Title/Summary/Keyword: X-ray absorption spectroscopy (XAS)

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X-ray Absorption and Photoemission Spectroscopy Study of Nd1/2A1/2Mn1-yCryO3(A=Ca, Sr)

  • Kang, J.S.;Kim, J.H.;Han, S.W.;Kim, K.H.;Choi, E.J.;Sekiyama, A.;Kasai, S.;Suga, S.;Kimura, T.
    • Journal of Magnetics
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    • v.8 no.4
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    • pp.142-145
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    • 2003
  • Valence states and electronic structures of Cr-doped $Nd_{1/2}A_{1/2}Mn_{1-y}Cr_{y}O_3$(NAMO; A=Ca, Sr) manganites have been investigated using x-ray absorption spectroscopy (XAS) and high-resolution photoemission spectroscopy (PES). All the Cr-doped NAMO systems exhibit the clear metallic Fermi edges in the Mn $e_{g}$ PES spectra near $E_{F}$. The spectral intensity at $E_{F}$ is higher for Cr-doped N $d_{l}$ 2/S $r_{l}$ 2/Mn $O_3$(NSMO) than for Cr-doped N $d_{l}$ 2/C $a_{l}$ 2/Mn $O_3$ (NCMO), reflecting the stronger metallic nature for NSMO than for NCMO. The measured Cr 2p XAS spectra are found to be very similar to that of C $r_2$ $O_3$, indicating that Cr ions in Cr-doped NAMO are in the trivalent C states ( $t^3$$_{2g}$). The Cr 2p XAS data are consistent with the Cr 3d PES spectra located at ∼1.3 eV below $E_{F}$ and having no emission near $E_{F}$.

Synthesis and Characterization of New Macroporous SnO2 Foams

  • Choi, Moon-Hyung;Paek, Seung-Min
    • Bulletin of the Korean Chemical Society
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    • v.34 no.5
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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.

Soft x-ray Synchrotron Radiation Spectroscopy Study of Molecule-based Nano Bioparticles Containing Fe (철원소를 함유한 분자기반 생체물질 나노입자들의 연 x선 방사광 분광 연구)

  • Lee, Eun-Sook;Kim, D.H.;Hwang, Ji-Hoon;Lee, Ki-Ho;Kang, J.S.
    • Journal of the Korean Magnetics Society
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    • v.22 no.4
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    • pp.125-129
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    • 2012
  • By employing soft x-ray absorption spectroscopy (XAS) and soft x-ray magnetic circular dichroism (XMCD), the electronic structures of molecule-based nano bioparticles, such as Helicobacter pylori ferritin (H. pylori ferritin), Heme, $NaM[Fe(CN)_6]{\cdot}H_2O$-type Prussian Blue (M=Co, Ni) analogue, have been investigated. The measured Fe 2p XAS spectra reveal that Fe ions are trivalent ($Fe^{3+}$) in H. pylori ferritins, while they are in the $Fe^{2+}-Fe^{3+}$ mixed-valent states in $NaM[Fe(CN)_6]{\cdot}H_2O$ Prussian Blue analogues (M=Co, Ni). According to the Fe 2p XMCD spectrum of high-state H. pylori ferritin, all the $Fe^{3+}$ ions have the same local symmetry and their magnetic moments are aligned in the same direction. It is also found that the Fe 3d orbitals in $NaM[Fe(CN)_6]{\cdot}H_2O$ have a strong covalent bonding to $(CN)^-$ ligands, but with a very weak bonding to the 2p orbitals of O ligands.

XMCD and PES study of a compensated-ferrimagnetic half-metal Mn3Ga

  • Seong, Seungho;Lee, Eunsook;Kim, Hee Yeon;Kim, Younghak;Baik, Jaeyoon;Kang, J.S.
    • Current Applied Physics
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    • v.18 no.11
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    • pp.1190-1195
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    • 2018
  • By employing soft X-ray magnetic circular dichroism (XMCD), soft X-ray absorption spectroscopy (XAS), and photoemission spectroscopy (PES), we have investigated the electronic structure of the candidate zero-moment half-metallic $Mn_3Ga$. We have studied the ball-milled and annealed $Mn_3Ga$ powder samples that exhibit nearly zero magnetization. Mn 2p XAS revealed that Mn ions in $Mn_3Ga$ are nearly divalent for both of the Mn ions having the locally octahedral symmetry and those having the locally tetrahedral symmetry. The measured Mn 2p XMCD spectrum of $Mn_3Ga$ is very similar to that of ferrimagnetic $MnFe_2O_4$ having divalent Mn ions. The sum-rule analysis of the Mn 2p XMCD spectrum shows that both the spin and orbital magnetic moments of Mn ions in $Mn_3Ga$ are negligibly small, in agreement with the nearly compensated-ferrimagnetic ground state of $Mn_3Ga$. The valence-band PES spectrum of $Mn_3Ga$ agrees well with the calculated density of states, supporting the half-metallic electronic structure of $Mn_3Ga$.

Study on Stabilization of Arsenic in Soil through in situ Formation of Amorphous Fe Oxides and use of X-ray Absorption Spectroscopy (비결정질철산화물 원위치 형성을 통한 비소오염토양 안정화 및 X선 분광분석법의 활용에 대한 연구)

  • Park, Jinhee;Chung, Hyeonyong;Kim, Sang Hyun;An, Jinsung;Nam, Kyoungphile
    • Journal of Soil and Groundwater Environment
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    • v.25 no.2
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    • pp.9-15
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    • 2020
  • This study was conducted to investigate the in situ formation of amorphous Fe oxides as a stabilization technology in As-contaminated soil. After addition of ferric nitrate and the neutralizing agent, most of extractable fractions of As in soil (i.e., SO42- and PO43--extractable As) was converted into As bound to amorphous Fe oxides. In addition, results of solubility bioavailability research consortium (SBRC) test indicated that a significant amount of As in untreated soil changed to a non-bioaccessible form after stabilization. The reason was attributed to the newly formed amorphous Fe oxides in the stabilized soil, which was confirmed by linear combination of fitting (LCF) using X-ray absorption spectroscopy (XAS) analysis. Interestingly, after five months of aging of the stabilized soil, ferrihydrite and schwertmannite newly formed in the soil were transformed to crystalline Fe oxides such as goethite, and further decrease in SBRC extractable fraction of As was observed. The results suggest that co-precipitated As with amorphous Fe oxides can be further immobilized with time, due to the crystallization of amorphous Fe oxides.

Generalized Two-dimensional (2D) Correlation Spectroscopy: Principle and Its Applications (일반화된 이차원 상관 분광학: 원리 및 응용)

  • Young Mee Jung;Seung Bin Kim
    • Journal of the Korean Chemical Society
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    • v.47 no.5
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    • pp.447-459
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    • 2003
  • Generalized 2D correlation spectroscopy has been applied extensively to the analysis of spectral data sets obtained during the observation of a system under some external perturbation. It is used in various fields of spectroscopy including IR, Raman, UV, fluorescence, X-ray diffraction, and X-ray absorption spectroscopy (XAS) as well as chromatography. 2D hetero-spectral correlation analysis compares two completely different types of spectra obtained for a system under the same perturbation. Because of the wide range of applications of this technique, it has become one of the standard analytical techniques for the analytical chemistry, physical chemistry, biochemistry, and so on, and for studies of polymers, biomolecules, nanomaterials, etc. In this paper, we will introduce the principle of generalized 2D correlation spectroscopy and its applications that we have studied.

Differences in the Electronic Structures of Bulk and Powder FeV2O4 Spinel Oxide Investigated by Using Synchrotron Radiation (방사광을 이용한 FeV2O4 스피넬 산화물의 덩치상태와 분말상태의 전자구조 차이 연구)

  • Hwang, Ji-Hoon;Kim, D.H.;Lee, Eun-Sook;Kang, J.S.;Kim, W.C.;Kim, C.S.;Han, S.W.;Hong, S.C.;Park, B.G.;Kim, J.Y.
    • Journal of the Korean Magnetics Society
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    • v.21 no.6
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    • pp.198-203
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    • 2011
  • The electronic structure of ferrimagnetic spinel oxide of $FeV_2O_4$ has been investigated by employing soft x-ray absorption spectroscopy (XAS) and soft x-ray magnetic circular dichroism (XMCD). The Fe 2p and V 2p XAS spectra show that the valence states of Fe and V ions are ${\sim}Fe^{2.3+}$ mixed-valent states and ${\sim}V^{3+}$ states, respectively. In Fe 2p XMCD spectra, finite XMCD signals are observed for divalent $Fe^{2+}$ states only, but not for $Fe^{3+}$ states. This finding indicates that the magnetic moments of $Fe^{2+}$ ions are ordered ferromagnetically but that those of $Fe^{3+}$ ions are cancelled, implying that $Fe^{2+}$ ions play an important role in determining magnetic properties of $FeV_2O_4$.

Investigation of Electronic Structures of TCr2O4 (T = Fe, Co, Ni) Spinel Oxides by Employing Soft X ray Synchrotron Radiation Spectroscopy (연 X선 방사광 분광법을 이용한 TCr2O4(T = Fe, Co, Ni) 스피넬 산화물의 전자구조 연구)

  • Kim, Hyun Woo;Hwang, Jihoon;Kim, D.H.;Lee, Eunsook;Kang, J.S.
    • Journal of the Korean Magnetics Society
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    • v.23 no.5
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    • pp.149-153
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    • 2013
  • The electronic structures of $TCr_2O_4$ (T = Fe, Co, Ni) spinel oxides have been investigated by employing synchrotron radiation-based soft X ray absorption spectroscopy (XAS). The measured 2p XAS spectra of transition-metal ions reveal that Cr ions are trivalent ($Cr^{3+}$), and all the T (T = Fe, Co, Ni) ions are divalent ($Fe^{2+}$, $Co^{2+}$, $Ni^{2+}$). It is also found that most of T (T = Fe, Co, Ni) ions occupy the A sites under the tetrahedral symmetry, while Cr ions occupy mainly the B sites under the octahedral symmetry. These findings show that the structures of $TCr_2O_4$ (T = Fe, Co, Ni) are very close to the normal spinel structures. Based on these findings, it is expected that Jahn-Teller (JT) effects are important in $FeCr_2O_4$ and $NiCr_2O_4$. In contrast, $CoCr_2O_4$ maintains the cubic structure without having the JT distortion since both $Cr^{3+}$ and $Co^{2+}$ ions are non-JT ions. This work suggests that the antiferromagnetic interaction between $Cr^{3+}$ and $T^{2+}$ ions plays an important role in determining the magnetic properties of $TCr_2O_4$ (T = Fe, Co, Ni).

Chimie Douce Synthesis of Chalcogen-Doped Manganese Oxides (칼코겐이 도핑된 망간 산화물의 저온합성 연구)

  • Hwang, Seong-Ju;Im, Seung-Tae;Park, Dae-Hun;Yun, Yeong-Su
    • Journal of the Korean Chemical Society
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    • v.50 no.4
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    • pp.315-320
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    • 2006
  • manganese oxides have been prepared by Chimie Douce redox reaction between permanganate and chalcogen element fine powder under acidic condition (pH = 1). According to powder X-ray diffraction analyses, the S- and Se-doped manganese oxides are crystallized with layered birnessite and tunnel-type -MnO2 structures, respectively. On the contrary, Te-doped compound was found to be X-ray amorphous. According to EDS analyses, these compounds contain chalcogen dopants with the ratio of chalcogen/manganese = 4-7%. We have investigated the chemical bonding character of these materials with X-ray absorption spectroscopic (XAS) analysis. Mn K-edge XAS results clearly demonstrated that the manganese ions are stabilized in octahedral symmetry with the mixed oxidation states of +3/+4. On the other hand, according to Se K- and Te L1-edge XAS results, selenium and tellurium elements have the high oxidation states of +6, which is surely due to the oxidation of neutral chalcogen element by the strong oxidant permanganate ion. Taking into account their crystal structures and Mn oxidation states, the obtained manganese oxides are expected to be applicable as electrode materials for lithium secondary batteries.

Mechanistic Study of FeS Reacted with Arsenate under Various pH Conditions (FeS 수용액 내 pH에 따른 5가비소의 반응 메커니즘 연구)

  • Han, Young-Soo;Lee, Mu Yeol;Seong, Hye Jin
    • Journal of Soil and Groundwater Environment
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    • v.27 no.1
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    • pp.25-30
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    • 2022
  • Mackinawite (FeS), as a ubiquitous reduced iron mineral, is known as a key controller of redox reactions in anaerobic subsurface environment. The reaction of FeS with redox-sensitive toxic element such as arsenic is substantially affected by pH conditions of the given environments. In this study, the interaction of As(V) with FeS was studied under strict anaerobic conditions with various pH conditions. The pH-dependent arsenic removal tests were conducted under wide ranges of pH conditions and X-ray absorption spectroscopy (XAS) was applied to investigate the reaction mechanisms under pH 5, 7, and 9. The removal efficiency of FeS for As(V) showed the higher removal of As(V) under low pH conditions and its removal efficiency decreased with increasing pH, and no As(V) reduction was observed in 1 g/L FeS solution. However, XAS analysis indicated the reduction of As(V) to As(III) occurred during reaction between FeS and As(V). The reduced form of As(III) was particularly identified as an arsenic sulfide mineral (As2S3) in all pH conditions (pH 5, 7, and 9). As2S3 precipitation was more pronounced in pH 5 where the solubility of FeS is higher than in other pH conditions. The linear combination fitting results of XAS demonstrated that As(V) removal mechanism is concerted processes of As2S3 precipitation and surface complexation of both arsenic species.