• Title/Summary/Keyword: X-ray absorption near edge structure

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Chemisorption and orientation of Selenopheneon Si(100)-$2{\times}1$

  • Lee, Han-Koo;Kim, Ki-Jeong;Kim, Hyeong-Do;Shin, Hyun-Joon;Kim, Bong-Soo
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.372-372
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    • 2010
  • We have investigated adsorption of selenophene on Si(100) at room temperature using high resolution photoemission spectroscopy (HRPES) and near edge X-ray absorption fine structure (NEXAFS) in the partial electron yield (PEY) mode. The Si 2p, C 1s, Se 3d spectra of selenophene on Si(100) show that selenophene is nondissociatively chemisorbed on Si(100)-$2{\times}1$ through [2+2] cycloaddition. NEXAFS has been conducted to characterize the adsorption geometry of selenophene on Si(100). Since the $\pi^*$ orbital of C=C bond show good angular dependence in carbon K-edge NEXAFS spectra, the angle $53{\pm}5^{\circ}$ determined from NEXAFS spectra. This majority structure is consistent with the [2+2] cycloaddition of selenophene to the dimer of the Si(100)-$2{\times}1$ surface.

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Spatial Pattern of Copper Phosphate Precipitation Involves in Copper Accumulation and Resistance of Unsaturated Pseudomonas putida CZ1 Biofilm

  • Chen, Guangcun;Lin, Huirong;Chen, Xincai
    • Journal of Microbiology and Biotechnology
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    • v.26 no.12
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    • pp.2116-2126
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    • 2016
  • Bacterial biofilms are spatially structured communities that contain bacterial cells with a wide range of physiological states. The spatial distribution and speciation of copper in unsaturated Pseudomonas putida CZ1 biofilms that accumulated 147.0 mg copper per g dry weight were determined by transmission electron microscopy coupled with energy dispersive X-ray analysis, and micro-X-ray fluorescence microscopy coupled with micro-X-ray absorption near edge structure (micro-XANES) analysis. It was found that copper was mainly precipitated in a $75{\mu}m$ thick layer as copper phosphate in the middle of the biofilm, while there were two living cell layers in the air-biofilm and biofilm-medium interfaces, respectively, distinguished from the copper precipitation layer by two interfaces. The X-ray absorption fine structure analysis of biofilm revealed that species resembling $Cu_3(PO_4)_2$ predominated in biofilm, followed by Cu-Citrate- and Cu-Glutathione-like species. Further analysis by micro-XANES revealed that 94.4% of copper were $Cu_3(PO_4)_2$-like species in the layer next to the air interface, whereas the copper species of the layer next to the medium interface were composed by 75.4% $Cu_3(PO_4)_2$, 10.9% Cu-Citrate-like species, and 11.2% Cu-Glutathione-like species. Thereby, it was suggested that copper was initially acquired by cells in the biofilm-air interface as a citrate complex, and then transported out and bound by out membranes of cells, released from the copper-bound membranes, and finally precipitated with phosphate in the extracellular matrix of the biofilm. These results revealed a clear spatial pattern of copper precipitation in unsaturated biofilm, which was responsible for the high copper tolerance and accumulation of the biofilm.

Advanced Nanoscale Characterization of Cement Based Materials Using X-Ray Synchrotron Radiation: A Review

  • Chae, Sejung R.;Moon, Juhyuk;Yoon, Seyoon;Bae, Sungchul;Levitz, Pierre;Winarski, Robert;Monteiro, Paulo J.M.
    • International Journal of Concrete Structures and Materials
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    • v.7 no.2
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    • pp.95-110
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    • 2013
  • We report various synchrotron radiation laboratory based techniques used to characterize cement based materials in nanometer scale. High resolution X-ray transmission imaging combined with a rotational axis allows for rendering of samples in three dimensions revealing volumetric details. Scanning transmission X-ray microscope combines high spatial resolution imaging with high spectral resolution of the incident beam to reveal X-ray absorption near edge structure variations in the material nanostructure. Microdiffraction scans the surface of a sample to map its high order reflection or crystallographic variations with a micron-sized incident beam. High pressure X-ray diffraction measures compressibility of pure phase materials. Unique results of studies using the above tools are discussed-a study of pores, connectivity, and morphology of a 2,000 year old concrete using nanotomography; detection of localized and varying silicate chain depolymerization in Al-substituted tobermorite, and quantification of monosulfate distribution in tricalcium aluminate hydration using scanning transmission X-ray microscopy; detection and mapping of hydration products in high volume fly ash paste using microdiffraction; and determination of mechanical properties of various AFm phases using high pressure X-ray diffraction.

Ring Formation of Furan on Epitaxial Graphene

  • Kim, Ki-Jeong;Yang, Sena;Lee, Han-Koo;Kim, Bong-Soo;Lee, Hang-Il
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.02a
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    • pp.315-315
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    • 2011
  • The ring formation and electronic properties of furan adsorbed on graphene layers grown on 6H-SiC(0001) has been investigated using atomic force microscopy (AFM), near edge X-ray absorption fine structure (NEXAFS) spectra for the C K-edge, and high resolution photoemission spectroscopy (HRPES). Moreover, we observed that furan molecules adsorbed on graphene could be used for chemical functionalization via the lone pair of electrons on the oxygen group, allowing chemical doping. We also found that furan spontaneously formed rings with one of three different bonding configurations and the electronic properties of the ring formed by furan on graphene can be described using by AFM, NEXAFS and HRPES, respectively.

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Influence of sputtering parameter on the properties of silver-doped zinc oxide sputtered films

  • S. H. Jeong;Lee, S. B.;J.H. Boo
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2003.10a
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    • pp.58-58
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    • 2003
  • Silver doped ZnO (SZO) films were prepared by rf magnetron sputtering on glass substrates with extraordinary designed ZnO target. With the doping source for target, use AgNO$_3$ powder on a various rate (0, 2, and 4 wt.%). We investigated dependence of coating parameter such as dopant content in target and substrate temperature in the SZO films. The SZO films have a preferred orientation in the (002) direction. As amounts of the Ag dopant in the target were increased, the crystallinity and the transmittance and optical band gap were decreased. And the substrate temperature were increased, the crystallinity and the transmittance were increased. But the crystallinity and the transmittance of SZO films were retrograde at 200$^{\circ}C$. Upside facts were related with composition. In addition, the Oxygen K-edge features of the SZO films were investigated by using near edge X-ray absorption fine structure (NEXAFS) spectroscopy. Changes of optical band gap of the SZO films were explained compared with XRD, XPS and NEXAFS spectra.

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Interaction of Oxygen and $CH_4$ with Molybdenum Oxide Catalysts

  • Kim, C. M.
    • Bulletin of the Korean Chemical Society
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    • v.18 no.10
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    • pp.1082-1085
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    • 1997
  • The Near-Edge X-ray Absorption Fine Structure (NEXAFS) technique and Differential Scanning Calorimetry (DSC) were utilized to investigate the reaction of CH4 and O2 on the MoO3/SiO2 catalyst. The NEXAFS results showed that the stoichiometry of the molybdenum oxide catalyst supported on silica was MoO3. MoO3 was reduced to MoO2 when the catalyst was exposed to CH4 at 773 K. NEXAFS results confirm that lattice oxygen is directly related to the process of CH4 oxidation which takes place on the surface of MoO3/SiO2 catalysts. DSC results show that the structure of MoO3 changes around 573 K and this structural change seems to improve the migration of oxygen in the lattice.

Fabrication, temperature-dependent local structural and electrical properties of VO2 thin films

  • Jin, Zhenlan;Hwang, In-Hui;Park, Chang-In;Han, Sang-Wook
    • Proceedings of the Korean Vacuum Society Conference
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    • 2015.08a
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    • pp.169.2-169.2
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    • 2015
  • $VO_2$ is a well-known a metal-to-insulator-transition (MIT) material, accompanied with a first order structural phase transition near room temperature. Because of the structural phase transition and the MIT occur near a same temperature, there is an ongoing argument whether the MIT is induced by the structural phase transition. $VO_2$ exhibits a relatively weak anti-oxidization ability and can be oxidized to higher-valence oxides (e.g., $V_4$ $O_7$ or $V_2$ $O_5$) when annealed at a high temperature in an oxygen-rich atmosphere. We fabricated $VO_2$ films on $Al_2$ $O_3$ (0001) substrates using a DC magnetron sputtering deposition process with carefully control the $O_2$ percentage in an atmosphere. X-ray diffraction measurements from the films showed only (0l0) peaks with no extra peaks, indicating b-oriented films. The temperature-dependent local structural properties of $VO_2$ films were investigated by using in-situ X-ray absorption fine structure (XAFS) measurements at the V K edge. XAFS revealed that the structural phase transition was occurred nearly $70^{\circ}C$ for heating process and reproducible. Resistance measurements as a function of temperature (R-T) demonstrated that the resistance of $VO_2$ films was changed by a factor of 4 near $75^{\circ}C$ which was higher than $68^{\circ}C$ reported from a $VO_2$ bulk. We will discuss the MIT of $VO_2$ films, comparing with the local structural properties determined by XAFS measurements.

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Chemical and Electronic structures of $Co_{1-x}Ga_x$ alloys by X-ray Analyses (X-선을 이용한 $Co_{1-x}Ga_x$ 합금계의 화학구조와 전자구조)

  • 유권국;이주열;지현배;이연승
    • Journal of the Korean Vacuum Society
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    • v.13 no.2
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    • pp.86-91
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    • 2004
  • Transiton-metal gallides attract wide interest as a candidate for high-temperature structural materials. In a wide composition range, in which it was known that Co-Ga alloy have CsCl (B2) crystallographic structure, a systematic study on the correlation between physical properties and electronic structures of Co-gallides was performed. $Co_{l-x}Ga$ $_{x}$ alloys ($0.35\leq$x$\leq0.55$) were prepared by arc-melting method and were annealed at $1000 ^{\circ}C$ for 48hour to increase the homogeneity. In this composition range all the prepared alloys have the CsCl (B2) structure. The chemical states and the electronic structure were studied by using x-ray photoemission spectroscopy (XPS), and x-ray absorption near-edge structure (XANES), and exhibit different physical properties depending on the composition. During the annealing, a significant oxidation has happened and all the oxygen atoms are incorporated with the Ga atoms to form a $Ga_2O_3$ phase. In a view point of electronic structure, the $Co_{l-x}Ga$ $_{x}$ alloys were formed by the Ga(p) - Co(d) hybridization.

Preparation and Cyclic Performance of Li1.2(Fe0.16Mn0.32Ni0.32)O2 Layered Cathode Material by the Mixed Hydroxide Method

  • Karthikeyan, K.;Nam, K.W.;Hu, E.Y.;Yang, X.Q.;Lee, Y.S.
    • Bulletin of the Korean Chemical Society
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    • v.34 no.7
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    • pp.1995-2000
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    • 2013
  • Layered $Li_{1.2}(Fe_{0.16}Mn_{0.32}Ni_{0.32})O_2$ was prepared by the mixed hydroxide method at various temperatures. Xray diffraction (XRD) pattern shows that this material has a ${\alpha}-NaFeO_2$ layered structure with $R{\bar{3}}m$ space group and that cation mixing is reduced with increasing synthesis temperature. Scanning electron microscopy (SEM) reveals that nano-sized $Li_{1.2}(Fe_{0.16}Mn_{0.32}Ni_{0.32})O_2$ powder has uniform particle size distribution. X-ray absorption near edge structure (XANES) analysis is used to study the local electronic structure changes around the Mn, Fe, and Ni atoms in this material. The sample prepared at $700^{\circ}C$ delivers the highest discharge capacity of 207 $mAhg^{-1}$ between 2-4.5 V at 0.1 $mAcm^{-2}$ with good capacity retention of 80% after 20 cycles.

Pile Contact Depth Effects in Rubbed Polyimide(PI) Films

  • Kim, Gi-Jeong;Gwon, Hyeok-Min;Lee, Sang-Mun;Lee, Cheol-Gu;Gwak, Mu-Seon;Kim, Bong-Su
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.398-398
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    • 2010
  • To determine the molecular directionality of PI chains depending on rubbing condition, we measured the angle resolved near edge X-ray absorption fine structure (NEXAFS) spectra at C K-edge of the rubbed PI films. Twisted nematic mode PI (PI-TN) and in plane switching mode PI (PI-IPS) were introduced to examine the effect of rubbing conditions on the chain directionality. The average tilt angle a of the PI molecules was estimated through the measured intensity change of $C=C\;{\pi}^*$ in NEXAFS C K-edge spectrum by controlling the stage speed and the pile contact depth. After rubbing, the irregular molecular direction changed to a regular direction with a molecular tilt angle of $51.2^{\circ}$ for PI-TN and $49.6^{\circ}$ for PI-IPS at the rubbing condition of the roll speed of 1000 rpm, stage speed of 50 mm/sec, and file contact depth of 0.3 mm. The molecular tilt angle $\alpha$ was linearly decreased in the PI-TN and PI-IPS samples with increasing depth of the pile contact.

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