• Title/Summary/Keyword: EXAFS

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Lead Stabilization in Soil Amended with Lime Waste: An Extended X-ray Absorption Fine Structure (EXAFS) Investigation

  • Lim, Jung Eun;Lee, Sang Soo;Yang, Jae E.;Ok, Yong Sik
    • Korean Journal of Soil Science and Fertilizer
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    • v.47 no.6
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    • pp.443-450
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    • 2014
  • To determine Pb species in soils following the immobilization process, sequential extraction has been used despite the possibility of overestimating Pb species from unintended reactions during chemical extraction. Meanwhile, the application of extended X-ray absorption fine structure (EXAFS) has been shown to provide a more precise result than chemical extraction. In this study, the immobilization of Pb in contaminated soils treated with liming materials such as oyster shell (OS) or eggshell (ES) was evaluated with thermodynamic modelling and EXAFS analysis. Thermodynamic modelling by visual MINTEQ predicted the precipitation of $Pb(OH)_2$ in OS and ES treated soils. In particular, the values of saturation index (SI) for $Pb(OH)_2$ in OS (SI=0.286) and ES (SI=0.453) treated soils were greater than in the control soil (SI=0.281). Linear combination fitting (LCF) analysis confirmed the presence of $C_{12}H_{10}O_{14}Pb_3$ (lead citrate, 44.7%) by citric acid from plant root, Pb-gibbsite (Pb adsorbed gibbsite, 26.4%), and Pb-kaolinite (Pb adsorbed kaolinite, 20.3%) in the control soil. On the other hand, $Pb(OH)_2$ (16.8%), Pb-gibbsite (39.3%), and Pb-kaolinite (25.6%) were observed in the OS treated soil and $Pb(OH)_2$ (55.2%) and Pb-gibbsite (33.8%) were also confirmed in the ES treated soil. Our results indicate that the treatment with OS and ES immobilizes Pb by adsorption of Pb onto the soil minerals as a result of the increase in soil negative charge and the formation of stable $Pb(OH)_2$ under high pH condition of soils.

The Effect of the Oxygen Flow Rate on the Electronic Properties and the Local Structure of Amorphous Tantalum Oxide Thin Films

  • Denny, Yus Rama;Lee, Sunyoung;Lee, Kangil;Kang, Hee Jae;Yang, Dong-Seok;Heo, Sung;Chung, Jae Gwan;Lee, Jae Cheol
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.398-398
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    • 2013
  • The electronic properties and the local structure of tantalum oxide thin film with variation of oxygen flow rate ranging from 9.5 to 16 sccm (standard cubic centimeters per minute) have been investigated by X-ray photoelectron spectroscopy (XPS), Reflection Electron Energy Loss Spectroscopy (REELS), and X-ray absorption spectroscopy (XAS). The XPS results show that the Ta4f spectrum for all films consist of the strong spin-orbit doublet $Ta4f_{7/2}$ and $Ta4f_{5/2}$ with splitting of 1.9 eV. The oxygen flow rate of the film results in the appearance of new features in the Ta4f at binding energies of 23.2 eV, 24.4 eV, 25.8, and 27.3 eV, these peaks attribute to $Ta^{1+}$, $Ta^{2+}$, $Ta^{4+}$/$Ta^{2+}$, and $Ta^{5+}$, respectively. Thus, the presence of non-stoichiometric state from tantalum oxide ($TaO_x$) thin films could be generated by the oxygen vacancies. The REELS spectra suggest the decrease of band gap for tantalum oxide thin films with increasing the oxygen flow rate. The absorption coefficient ${\mu}$ and its fine structure were extracted from the fluorescence mode of extended X-ray absorption fine structure (EXAFS) spectra. In addition, bond distances (r), coordination numbers (N) and Debye-Waller factors (${\sigma}^2$) each film were determined by a detailed of EXAFS data analysis. EXAFS spectrapresent both the increase of coordination number of the first Ta-O shell and a considerable reduction of the Ta-O bond distance with the increase of oxygen flow rate.

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X-ray Induced Electron emission Spectroscopy

  • 송세안;이재철;최진학;김준홍;이재학;임창빈
    • Proceedings of the Korean Vacuum Society Conference
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    • 1999.07a
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    • pp.191-191
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    • 1999
  • Extended X-ray Absorption Fine Structure (EXAFS)는 일반적으로 널리 사용하는 X선 회절분광기로 분석하기 힘든 chemical 또는 biological system의 structural analyses에 매우 유용한 분석방법이다. 특히 세라믹이나 유전체 비정질 재료의 미세 원자 구조에 관한 정보를 얻는데는 가장 강력한 분석방법중의 하나로 알려져 있다. 현재까지 대부분의 EXAFS 실험은 방사광 가속기를 이용하여 수행하였다. 그런데 신제품 개발의 순환주기가 급속하게 단축되는 현실적인 문제에 부응하기 위하여 실험실에서 EXAFS 실험을 수행할 수 있는 system을 개발하게 되었다. 개발한 XIEES 장비는 rotating anode 형의 18kW X-ray source, Optical system, Detection system, Stepping motor control system, vacuum system, Utility 등으로 구성하였다. Optical system에서의 6개의 Johanson type monochromator를 사용하여 분석가능한 x-ray energy range를 480eV에서 41keV까지 구현하였다. 이는 산소에서 우라늄까지 분석이 가능함을 의미하는 것으로, 산화물 연구에 많이 활용할 것으로 기대한다. XIEES는 투과 및 형광 X-ray를 검출할 수 있는 기능과 X-ray에 의해 여기 되는 모든(광전자, Aiger 전자, 이차전자)들을 검출할 수 있는 기능을 갖추고 있는데 이를 Total Electron Yield 측정이라고 한다. Total Electron Yield 측정은 박막 시료와 같이 투과가 되지 않는 시료를 분석할 뿐만 아니라, 경원소 분석, 낮은 에너지에서 흡수 edge가 나타나는 L-edge 측정을 통한 전자 구조 분석 등에 유용한다. 실험실용 XIEES 장비는 방사광가속기에 비해 x-ray flux가 크게 뒤지는 문제와 Total Electron Yield를 측정하는 데 있어서 source에서 나오는 x-ray beam이 진공용기 안에서 산란되어 이차전자를 여기하고 이 이차전자들이 전자검출기에 유입되어 측정에 영향을 미치는 background 문제 등이 있다. 이 두 가지 문제를 해결하기 위하여 Capillary tube를 사용하였다. 본 연구에서는 실험실용 XIEES 장비를 소개하고 이를 이용하여 Cu standard 시료에서 측정한 EXAFS 결과와 Capillary tube를 사용하여 얻은 x-ray flux 증진 및 background 제거 효과에 대해서 발표한다.

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$La_{0.7}Ca_{0.3-x}Ba_xMnO_3$ manganites : Local structure and transport properties

  • A.N.Ulyanov;Yang, Dong-Seok;Yu, Seong-Cho
    • Proceedings of the Korea Crystallographic Association Conference
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    • 2003.05a
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    • pp.8-8
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    • 2003
  • Electron-phonon interaction plays a significant role in forming of colossal magnetoresistance effect (CMR). Polaron formation was observed by neutron diffraction and by extended X-ray absorption fine structure (EXAFS) analysis. Local probe as given by the EXAFS is a useful method to study the polaronic charge and its dependence on temperature and ions size. Here we present the EXAFS study of polaronic charge in La/sub 0.7/Ca/sub 0.3-X/Ba/sub X/MnO₃ compositions. The single phase La/sub 0.7/Ca/sub 0.3-X/Ba/sub X/MnO₃ manganites (x=0; 0.03; 0.06, ..., 0.3) were prepared by ceramic technology [1]. The Curie temperature was determined by extrapolation of the temperature dependence of the magnetization (down to zero magnetization). EXAFS experiments were carried out at the 7C EC beam line of the Pohang Light Source (PLS) in Korea. The atomic pair distribution functions (PDF) were obtained by re-regularization method [2] from filtered spectra. The PDF for the x=0.3 sample showed a single peak function and for x=0.0, 0.03, 0.06, 0.09, 0.12 compositions were asymmetric in agreement with a small Jahn-Teller elongation of two (short and long) bonds of the MnO/sub 6/ octahedron. Dispersion, σ/sub Min-O//sup 2/, and asymmetry, σ/sub Min-O//sup 3/, of the Mn-O bond distances varied significantly with x and showed a maximums at x=0.09. The maximum of σ/sub Min-O//sup 2/ is caused by increase of dynamic rms displacements of the Mn-O distances near the T/sub C/. The observed x dependence of σ/sub Min-O//sup 3/ reflects the reduction of charge carriers mobility at approaching to T/sub C/ from low as well as high temperatures.

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

  • Park, Chang-In;Seo, Su-Yeong;Kim, Jeong-Ran;Han, Sang-Uk
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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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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Chemical Properties of Mineral Surfaces and Metal Ion Sorption: A Review (광물표면의 화학적 특성과 금속이온 수착의 고찰: A Review)

  • Yoon, Soh-Joung
    • Economic and Environmental Geology
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    • v.45 no.2
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    • pp.205-215
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    • 2012
  • Metal ions, toxic or potentially toxic to biota and human beings, can be immobilized by sorption onto the mineral surfaces in soils and sediments. This article briefly explains theories regarding the chemical properties of mineral surfaces to sorb metal ions and processes of extended X-ray absorption fine structure (EXAFS) analysis for sorption study, and reviews atomic-scale findings on metal sorption on mineral surfaces. The theoretical understanding on the chemistry of mineral surfaces and metal sorption is fundamental to the proper analysis of the atomic-scale spectroscopy to determine the sorption phases. Atomic-scale findings on metal sorption phases discussed here include co-precipitation, ternary complexation, aging effects, and desorption possibilities, as well as outer-sphere complexation, inner-sphere complexation, and surface precipitation.

EXAFS study for the ordering of manganese in $La_{0.7}Ca_{0.3-x}Ba_xMnO_3$

  • 양동석
    • Proceedings of the Korea Crystallographic Association Conference
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    • 2002.11a
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    • pp.12-12
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    • 2002
  • Lanthanum manganites have been extensively studied for the application to magnetic devices since the colossal magnetoresistance of these compounds has been observed [1]. The critical temperatures, Tc, of manganites La/sub 0.7/Ca/sub 0.3-x/Ba/sub x/MnO₃ increased as the content of Ba increased except the abrupt jump near the critical concentration. The step like behavior of the critical temperature for a similar compound has been known to be related to the structural phase transition [2]. To understand the step like behavior of Tc, the EXAFS technique is applied to the La/sub 0.7/Ca/sub 0.3-x/Ba/sub x/MnO₃ compound system. The ordering between the manganese and oxygen was examined by this method. The EXAFS analysis shows that the coordination numbers were not changed before and after the phase transition, the bonding distance between manganese and oxygen is about 1.94 ± 0.02 Å, which is consistent with other work [3] and the Debye waller parameters were about σ²= 0.0037 ± 0.0005 Ų for x=0.0 and x=3.0, respectively. The value of Debye-Waller parameter for x=0.09 is about σ² = 0.0050 ± 0.0005 Ų in about phase transition concentration. Based on the Debye-Waller parameters, it is shown that the ordering between manganese and oxygen is significantly reduced near the phase transition concentration.

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Structure Study of PbO-Ga$_2$O$_3$ Glasses Using Ga K-edge EXAFS Taken at Cryogenic Temperature (갈륨 K 흡수단의 저온 EXAFS를 이용한 PbO-Ga$_2$O$_3$ 유리의 구조 해석)

  • Choi, Yong-Gyu;Kim, Kyong-Hon;Chernov, Vladimir A;Heo, Jong
    • Journal of the Korean Ceramic Society
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    • v.35 no.11
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    • pp.1148-1154
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    • 1998
  • Ga K-edge EXAFS spectra of PbO-Ga2O3 glasses were recorded at liquid nitrogen temperature and analyz-ed in order to quantitatively understand the medium-range-order arrangement around gallium in the glasses. The second peak was generated from a backscattering of the neighbor balliums and the Ga-Ga distance is ~3.13 A with Ga coordination number of ~2.7 Therefore GaO4 tetrahedra are connected through the cor-ner~sharing mode and form their own clusters made of the tetrahedra sharing more than 3 corners while some chains or rings are also present. These connection schemes of the GaO4 tetrahedra are believed to form the substantial part of the network structure.

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