WorldWideScience

Sample records for high-precision x-ray spectroscopy

  1. High precision X-ray spectroscopy in hydrogen-like fermionic and bosonic atomic systems

    Energy Technology Data Exchange (ETDEWEB)

    Borchert, G.L.; Anagnostopoulos, D.; Augsburger, M.; Belmiloud, D.; Castelli, C.; Chatellard, D.; Daum, M.; Egger, J.P.; El-Khoury, P.; Elble, M.; Frosch, R.; Gorke, H.; Gotta, D.; Hauser, P.; Indelicato, P.; Kirch, K.; Lenz, S.; Nelms, N.; Rashid, K.; Schult, O.W.B. (and others)

    1998-11-15

    Some time after its formation an exotic atom may be considered a hydrogen-like system consisting of a nucleus and an exotic particle in a bound state. In this situation it is an ideal tool to study cascade properties, while for the innermost orbits it can be used to probe the interaction with the nucleus. From an extended series of experiments using high resolution X-ray spectroscopy for both aspects typical examples are reported and preliminary results are given: 1. To determine the complex scattering length in p-barH the 3D{yields}2P hyperfine transitions have been measured. 2. To determine the pion mass the 5 {yields} 4 transitions in {pi}{sup 14}N have been studied. In all cases a major contribution to the uncertainty originates from the calibration. Therefore a new method is proposed that will establish a universal set of high precision calibration lines for pionic, muonic and electronic systems.

  2. High precision x ray lithographic masks

    Science.gov (United States)

    Pease, R. F.; Browning, R.

    1992-09-01

    This contract period was first concerned with winding up the projects on the embedded X-ray Mask structure and on the 'quantum lithography' idea. As a result of developments elsewhere it became clear that among the most critical issues in achieving high precision X-ray masks were those associated with achieving high precision in both feature size and feature placement in electron beam lithography. Most of the effort in this reporting period was aimed at achieving precision in feature size; notably an attack on the problem of proximity effects. There were two approaches: (1) A short term approach aimed at correcting effects in existing electron beam pattern generators (notably the ETEC MEBES 3 and 4) for feature sizes down 500 nm; and (2) A long term approach aimed at avoiding proximity effects by employing low energy electron exposure for feature size below 500 nm.

  3. Probing the Impact of Solvation on Photoexcited Spin Crossover Complexes with High-Precision X-ray Transient Absorption Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Cunming; Zhang, Jianxin [State; Lawson Daku, Latévi M. [Département; Gosztola, David; Canton, Sophie E. [ELI-ALPS, ELI-HU Non-Profit Ltd., Dugonics ter 13, Szeged 6720, Hungary; Attosecond; Zhang, Xiaoyi

    2017-11-17

    Investigating the photoinduced electronic and structural response of bistable molecular building blocks incorporating transition metals in solution phase constitutes a necessary stepping stone for steering their properties towards applications and perfomance optimizations. This work presents a detailed X-ray transient absorption (XTA) spectroscopy study of a prototypical spin crossover (SCO) complex [FeII(mbpy)3]2+ (where mbpy=4,4’-dimethyl-2,2’-bipyridine) with a [FeIIN6] first coordination shell in water (H2O) and acetonitrile (CH3CN). The unprecedented data quality of the XTA spectra together with the direct fitting of the difference spectra in k space using a large number of scattering paths enables resolving the subtle difference in the photoexcited structures of an FeII complex in two solvents for the first time. Compared to the low spin (LS) 1A1 state, the average Fe-N bond elongations for the photoinduced high spin (HS) 5T2 state are found to be 0.181 . 0.003 Å in H2O and 0.199 . 0.003 Å in CH3CN. This difference in structural response is attributed to ligand-solvent interactions that are stronger in H2O than in CH3CN for the HS excited state. Our studies demonstrate that, although the metal center of [FeII(mbpy)3]2+ could have been expected to be rather shielded by the three bidentate ligands with quasi-octahedral-coordination, the ligand field strength in the HS excited state is nevertheless indirectly affected by solvation that modifies the charge distribution within the Fe-N covalent bonds. More generally, this work highlights the importance of including solvation effects in order to develop a generalized understanding of the spin-state switching at the atomic level.

  4. X-ray Absorption Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Yano, Junko; Yachandra, Vittal K.

    2009-07-09

    This review gives a brief description of the theory and application of X-ray absorption spectroscopy, both X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS), especially, pertaining to photosynthesis. The advantages and limitations of the methods are discussed. Recent advances in extended EXAFS and polarized EXAFS using oriented membranes and single crystals are explained. Developments in theory in understanding the XANES spectra are described. The application of X-ray absorption spectroscopy to the study of the Mn4Ca cluster in Photosystem II is presented.

  5. High Precision Assembly of Thin Mirror X-ray Telescopes

    Science.gov (United States)

    Schattenburg, Mark

    Lightweight high resolution x-ray telescope optics are one of the key technologies under development for next-generation x-ray telescopes. The ultimate goal of this effort is to realize optics with spatial resolution rivaling Chandra (glass mirrors which were epoxied into place around a spindle structure. While very light weight, this process resulted in ~1 arc min resolution. We want to achieve ~100 times better with similar mass. A group at NASA GSFC has recently demonstrated an alternative thin-glass assembly procedure that has achieved ~7 arc sec resolution with x-ray tests. Further progress towards 1 arc-sec will require mirrors with improved figure, lower stress coatings, improved alignment, better metrology, and low stress bonding. Many of the difficulties with current mirror assembly practice stem from the use of epoxy as a bonding agent. Epoxy has many disadvantages, including high shrinkage, large CTE and creep, resin aging effects, water absorption, outgassing, low tensile strength, exothermicity, and requiring large amounts of time and/or heat to cure. These effects can cause errors that become â€oefrozen in― to the bond with no possibility of correction. We propose to investigate replacing epoxy with low temperature, low shrinkage solder alloys. We use these solders in conjunction with high power, millisec-long pulses from a fiber IR laser to deliver controlled amounts of heat into the bond area. We have demonstrated that laser pulses can be used to actuate carefully designed bonds by permanently compressing or expanding a very thin and brief surface melt in the solder by amounts controlled in the nanoscale range, allowing post assembly correction of the mirror mount points. We believe this technology will be one of the keys to realize a sub-1 arc-sec thin-glass x-ray telescope.

  6. High-Resolution X-ray Emission and X-ray Absorption Spectroscopy

    NARCIS (Netherlands)

    Groot, F.M.F. de

    2000-01-01

    In this review, high-resolution X-ray emission and X-ray absorption spectroscopy will be discussed. The focus is on the 3d transition-metal systems. To understand high-resolution X-ray emission and reso-nant X-ray emission, it is first necessary to spend some time discussing the X-ray absorption

  7. X-ray spectroscopy an introduction

    CERN Document Server

    Agarwal, Bipin K

    1979-01-01

    Rontgen's discovery of X-rays in 1895 launched a subject which became central to the development of modern physics. The verification of many of the predic­ tions of quantum theory by X-ray spectroscopy in the early part of the twen­ tieth century stimulated great interest in thi's area, which has subsequently influenced fields as diverse as chemical physics, nuclear physics, and the study of the electronic properties of solids, and led to the development of techniques such as Auger, Raman, and X-ray photoelectron spectroscopy. The improvement of the theoretical understanding of the physics underlying X-ray spectroscopy has been accompanied by advances in experimental techniques, and the subject provides an instructive example of how progress on both these fronts can be mutually beneficial. This book strikes a balance between his­ torical description, which illustrates this symbiosis, and the discussion of new developments. The application of X-ray spectroscopic methods to the in­ vestigation of chemical b...

  8. High-precision soft x-ray polarimeter at Diamond Light Source.

    Science.gov (United States)

    Wang, H; Dhesi, S S; Maccherozzi, F; Cavill, S; Shepherd, E; Yuan, F; Deshmukh, R; Scott, S; van der Laan, G; Sawhney, K J S

    2011-12-01

    The development and performance of a high-precision polarimeter for the polarization analysis in the soft x-ray region is presented. This versatile, high-vacuum compatible instrument is supported on a hexapod to simplify the alignment with a resolution less than 5 μrad, and can be moved with its own independent control system easily between different beamlines and synchrotron facilities. The polarimeter can also be used for the characterization of reflection and transmission properties of optical elements. A W/B(4)C multilayer phase retarder was used to characterize the polarization state up to 1200 eV. A fast and accurate alignment procedure was developed, and complete polarization analysis of the APPLE II undulator at 712 eV has been performed.

  9. High-precision soft x-ray polarimeter at Diamond Light Source

    Science.gov (United States)

    Wang, H.; Dhesi, S. S.; Maccherozzi, F.; Cavill, S.; Shepherd, E.; Yuan, F.; Deshmukh, R.; Scott, S.; van der Laan, G.; Sawhney, K. J. S.

    2011-12-01

    The development and performance of a high-precision polarimeter for the polarization analysis in the soft x-ray region is presented. This versatile, high-vacuum compatible instrument is supported on a hexapod to simplify the alignment with a resolution less than 5 μrad, and can be moved with its own independent control system easily between different beamlines and synchrotron facilities. The polarimeter can also be used for the characterization of reflection and transmission properties of optical elements. A W/B4C multilayer phase retarder was used to characterize the polarization state up to 1200 eV. A fast and accurate alignment procedure was developed, and complete polarization analysis of the APPLE II undulator at 712 eV has been performed.

  10. High-precision measurement of the x-ray Cu Kα spectrum

    Science.gov (United States)

    Mendenhall, Marcus H.; Henins, Albert; Hudson, Lawrence T.; Szabo, Csilla I.; Windover, Donald; Cline, James P.

    2017-06-01

    The structure of the x-ray emission lines of the Cu {{K}}{α } complex has been remeasured on a newly commissioned instrument, in a manner directly traceable to the Système Internationale definition of the meter. In this measurement, the region from 8000 to 8100 eV has been covered with a highly precise angular scale, and well-defined system efficiency, providing accurate wavelengths and relative intensities. This measurement updates the standard multi-Lorentzian-fit parameters from Härtwig, Hölzer, et al, and is in modest disagreement with their results for the wavelength of the {{K}}{α }1 line when compared via quadratic fitting of the peak top; the intensity ratio of {{K}}{α }1 to {{K}}{α }2 agrees within the combined error bounds. However, the position of the fitted top of {{K}}{α }1 is very sensitive to the fit parameters, so it is not believed to be a robust value to quote without further qualification. We also provide accurate intensity and wavelength information for the so-called {{K}}{α }{3,4} ‘satellite’ complex. Supplementary data, available online at stacks.iop.org/JPB/50/115004/mmedia, is provided which gives the entire shape of the spectrum in this region, allowing it to be used directly in cases where simplified, multi-Lorentzian fits to it are not sufficiently accurate.

  11. Neutron and X-ray Spectroscopy

    CERN Document Server

    Hippert, Françoise; Hodeau, Jean Louis; Lelièvre-Berna, Eddy; Regnard, Jean-René

    2006-01-01

    Neutron and X-Ray Spectroscopy delivers an up-to-date account of the principles and practice of inelastic and spectroscopic methods available at neutron and synchrotron sources, including recent developments. The chapters are based on a course of lectures and practicals (the HERCULES course) delivered to young scientists who require these methods in their professional careers. Each chapter, written by a leading specialist in the field, introduces the basic concepts of the technique and provides an overview of recent work. This volume, which focuses on spectroscopic techniques in synchrotron radiation and inelastic neutron scattering, will be a primary source of information for physicists, chemists and materials scientists who wish to acquire a basic understanding of these techniques and to discover the possibilities offered by them. Emphasizing the complementarity of the neutron and X-ray methods, this tutorial will also be invaluable to scientists already working in neighboring fields who seek to extend thei...

  12. Femtosecond X-ray Absorption Spectroscopy at a Hard X-ray Free Electron Laser

    DEFF Research Database (Denmark)

    Lemke, Henrik T.; Bressler, Christian; Chen, Lin X.

    2013-01-01

    X-ray free electron lasers (XFELs) deliver short (hard X-rays, making them excellent sources for time-resolved studies. Here we show that, despite the inherent instabilities of current (SASE based) XFELs, they can be used for measuring high......-quality X-ray absorption data and we report femtosecond time-resolved X-ray absorption near-edge spectroscopy (XANES) measurements of a spin-crossover system, iron(II) tris(2,2'-bipyridine) in water. The data indicate that the low-spin to high-spin transition can be modeled by single-exponential kinetics...

  13. Review of X-ray Tomography and X-ray Fluorescence Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Shear, Trevor A. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-03-16

    This literature review will focus on both laboratory and synchrotron based X-ray tomography of materials and highlight the inner workings of these instruments. X-ray fluorescence spectroscopy will also be reviewed and applications of the tandem use of these techniques will be explored. The real world application of these techniques during the internship will also be discussed.

  14. X-ray Spectroscopy of Cooling Cluster

    Energy Technology Data Exchange (ETDEWEB)

    Peterson, J.R.; /SLAC; Fabian, A.C.; /Cambridge U., Inst. of Astron.

    2006-01-17

    We review the X-ray spectra of the cores of clusters of galaxies. Recent high resolution X-ray spectroscopic observations have demonstrated a severe deficit of emission at the lowest X-ray temperatures as compared to that expected from simple radiative cooling models. The same observations have provided compelling evidence that the gas in the cores is cooling below half the maximum temperature. We review these results, discuss physical models of cooling clusters, and describe the X-ray instrumentation and analysis techniques used to make these observations. We discuss several viable mechanisms designed to cancel or distort the expected process of X-ray cluster cooling.

  15. X-ray absorption spectroscopy of semiconductors

    CERN Document Server

    Ridgway, Mark

    2015-01-01

    X-ray Absorption Spectroscopy (XAS) is a powerful technique with which to probe the properties of matter, equally applicable to the solid, liquid and gas phases. Semiconductors are arguably our most technologically-relevant group of materials given they form the basis of the electronic and photonic devices that now so widely permeate almost every aspect of our society. The most effective utilisation of these materials today and tomorrow necessitates a detailed knowledge of their structural and vibrational properties. Through a series of comprehensive reviews, this book demonstrates the versatility of XAS for semiconductor materials analysis and presents important research activities in this ever growing field. A short introduction of the technique, aimed primarily at XAS newcomers, is followed by twenty independent chapters dedicated to distinct groups of materials. Topics span dopants in crystalline semiconductors and disorder in amorphous semiconductors to alloys and nanometric material as well as in-sit...

  16. Technology development for soft X-ray spectroscopy

    Science.gov (United States)

    Törmä, P. T.; Sipilä, H. J.; Koskinen, T.; Mattila, M.

    2016-05-01

    X-ray spectroscopy instruments lose part of their performance due to the lack of suitable components for soft X-ray region below 1 keV. Therefore, in the analysis of low atomic number elements including lithium, beryllium, boron and carbon instrument sensitivity is often limited. In this work we describe how the performance of the spectroscopy of soft X-rays is significantly improved when all devices integrated in the spectroscopic instrument are suitable for both soft and hard X-rays. This concept is based on utilizing ultra-thin SiN X-ray windows with proven performance not only as a detector window but also as an X-ray source window. By including a soft-X-ray-sensitive silicon drift detector with efficient surface charge collection in this concept the sensitivity and performance of the instrument is significantly increased.

  17. High energy resolution off-resonant X-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Wojciech, Blachucki [Univ. of Fribourg (Switzerland). Dept. of Physics

    2015-10-16

    This work treats of the high energy resolution off-resonant X-ray spectroscopy (HEROS) method of determining the density of unoccupied electronic states in the vicinity of the absorption edge. HEROS is an alternative to the existing X-ray absorption spectroscopy (XAS) methods and opens the way for new studies not achievable before.

  18. X-ray absorption near-edge structure (XANES) spectroscopy

    NARCIS (Netherlands)

    Henderson, Grant S.; De Groot, Frank M F; Moulton, Benjamin J A

    2014-01-01

    The previous Reviews in Mineralogy volume on spectroscopic methods (Vol. 18 Spectroscopic Methods in Mineralogy and Geology, Frank C. Hawthorne, ed. 1988), contained a single chapter on X-ray absorption spectroscopy which reviewed aspects of both EXAFS (Extended X-ray Absorption Fine Structure) and

  19. X-ray spectroscopy of manganese clusters

    Energy Technology Data Exchange (ETDEWEB)

    Grush, M.M. [Univ. of California, Davis, CA (United States). Dept. of Applied Science]|[Lawrence Berkeley National Lab., CA (United States). Energy and Environment Div.

    1996-06-01

    Much of this thesis represents the groundwork necessary in order to probe Mn clusters more productively than with conventional Mn K-edge XAS and is presented in Part 1. Part 2 contains the application of x-ray techniques to Mn metalloproteins and includes a prognosis at the end of each chapter. Individual Mn oxidation states are more readily distinguishable in Mn L-edge spectra. An empirical mixed valence simulation routine for determining the average Mn oxidation state has been developed. The first Mn L-edge spectra of a metalloprotein were measured and interpreted. The energy of Mn K{beta} emission is strongly correlated with average Mn oxidation state. K{beta} results support oxidation states of Mn(III){sub 2}(IV){sub 2} for the S{sub 1} state of Photosystem II chemical chemically reduced preparations contain predominantly Mn(II). A strength and limitation of XAS is that it probes all of the species of a particular element in a sample. It would often be advantageous to selectively probe different forms of the same element. The first demonstration that chemical shifts in x-ray fluorescence energies can be used to obtain oxidation state-selective x-ray absorption spectra is presented. Spin-dependent spectra can also be used to obtain a more simplified picture of local structure. The first spin-polarized extended x-ray absorption fine structure using Mn K{beta} fluorescence detection is shown.

  20. Observing Solvation Dynamics with Simultaneous Femtosecond X-ray Emission Spectroscopy and X-ray Scattering

    DEFF Research Database (Denmark)

    Haldrup, Kristoffer; Gawelda, Wojciech; Abela, Rafael

    2016-01-01

    In liquid phase chemistry dynamic solute solvent interactions often govern the path, ultimate outcome, and efficiency of chemical reactions. These steps involve many-body movements on subpicosecond time scales and thus ultrafast structural tools capable of capturing both intramolecular electronic......, confirming previous ab initio molecular dynamics simulations. Structural changes in the aqueous solvent associated with density and temperature changes occur with similar to 1 ps time constants, characteristic for structural dynamics in water. This slower time scale of the solvent response allows us...... rearrangement of the solute with X-ray emission spectroscopy, thus establishing time zero for the ensuing X-ray diffuse scattering analysis. The simultaneously recorded X-ray diffuse scattering atterns reveal slower subpicosecond dynamics triggered by the intramolecular structural dynamics of the photoexcited...

  1. Femtosecond X-ray magnetic circular dichroism absorption spectroscopy at an X-ray free electron laser

    Science.gov (United States)

    Higley, Daniel J.; Hirsch, Konstantin; Dakovski, Georgi L.; Jal, Emmanuelle; Yuan, Edwin; Liu, Tianmin; Lutman, Alberto A.; MacArthur, James P.; Arenholz, Elke; Chen, Zhao; Coslovich, Giacomo; Denes, Peter; Granitzka, Patrick W.; Hart, Philip; Hoffmann, Matthias C.; Joseph, John; Le Guyader, Loïc; Mitra, Ankush; Moeller, Stefan; Ohldag, Hendrik; Seaberg, Matthew; Shafer, Padraic; Stöhr, Joachim; Tsukamoto, Arata; Nuhn, Heinz-Dieter; Reid, Alex H.; Dürr, Hermann A.; Schlotter, William F.

    2016-03-01

    X-ray magnetic circular dichroism spectroscopy using an X-ray free electron laser is demonstrated with spectra over the Fe L3,2-edges. The high brightness of the X-ray free electron laser combined with high accuracy detection of incident and transmitted X-rays enables ultrafast X-ray magnetic circular dichroism studies of unprecedented sensitivity. This new capability is applied to a study of all-optical magnetic switching dynamics of Fe and Gd magnetic sublattices in a GdFeCo thin film above its magnetization compensation temperature.

  2. Femtosecond X-ray magnetic circular dichroism absorption spectroscopy at an X-ray free electron laser.

    Science.gov (United States)

    Higley, Daniel J; Hirsch, Konstantin; Dakovski, Georgi L; Jal, Emmanuelle; Yuan, Edwin; Liu, Tianmin; Lutman, Alberto A; MacArthur, James P; Arenholz, Elke; Chen, Zhao; Coslovich, Giacomo; Denes, Peter; Granitzka, Patrick W; Hart, Philip; Hoffmann, Matthias C; Joseph, John; Le Guyader, Loïc; Mitra, Ankush; Moeller, Stefan; Ohldag, Hendrik; Seaberg, Matthew; Shafer, Padraic; Stöhr, Joachim; Tsukamoto, Arata; Nuhn, Heinz-Dieter; Reid, Alex H; Dürr, Hermann A; Schlotter, William F

    2016-03-01

    X-ray magnetic circular dichroism spectroscopy using an X-ray free electron laser is demonstrated with spectra over the Fe L(3,2)-edges. The high brightness of the X-ray free electron laser combined with high accuracy detection of incident and transmitted X-rays enables ultrafast X-ray magnetic circular dichroism studies of unprecedented sensitivity. This new capability is applied to a study of all-optical magnetic switching dynamics of Fe and Gd magnetic sublattices in a GdFeCo thin film above its magnetization compensation temperature.

  3. Femtosecond X-ray magnetic circular dichroism absorption spectroscopy at an X-ray free electron laser

    Energy Technology Data Exchange (ETDEWEB)

    Higley, Daniel J., E-mail: dhigley@stanford.edu; Yuan, Edwin [SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, California 94025 (United States); Department of Applied Physics, Stanford University, Stanford, California 94305 (United States); Hirsch, Konstantin; Dakovski, Georgi L.; Jal, Emmanuelle; Lutman, Alberto A.; Coslovich, Giacomo; Hart, Philip; Hoffmann, Matthias C.; Mitra, Ankush; Moeller, Stefan; Ohldag, Hendrik; Seaberg, Matthew; Stöhr, Joachim; Nuhn, Heinz-Dieter; Reid, Alex H.; Dürr, Hermann A.; Schlotter, William F. [SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, California 94025 (United States); Liu, Tianmin; MacArthur, James P. [SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, California 94025 (United States); Department of Physics, Stanford University, Stanford, California 94305 (United States); and others

    2016-03-15

    X-ray magnetic circular dichroism spectroscopy using an X-ray free electron laser is demonstrated with spectra over the Fe L{sub 3,2}-edges. The high brightness of the X-ray free electron laser combined with high accuracy detection of incident and transmitted X-rays enables ultrafast X-ray magnetic circular dichroism studies of unprecedented sensitivity. This new capability is applied to a study of all-optical magnetic switching dynamics of Fe and Gd magnetic sublattices in a GdFeCo thin film above its magnetization compensation temperature.

  4. Soft X-Ray and Vacuum Ultraviolet Based Spectroscopy of the Actinides

    Energy Technology Data Exchange (ETDEWEB)

    Tobin, J G

    2011-03-17

    The subjects of discussion included: VUV photoelectron spectroscopy, X-ray photoelectron spectroscopy, Synchrotron-radiation-based photoelectron spectroscopy, Soft x-ray absorption spectroscopy, Soft x-ray emission spectroscopy, Inverse photoelectron spectroscopy, Bremstrahlung Isochromat Spectroscopy, Low energy IPES, Resonant inverse photoelectron spectroscopy.

  5. Future projects of light kaonic atom X-ray spectroscopy

    Directory of Open Access Journals (Sweden)

    Tatsuno H.

    2016-01-01

    Full Text Available X-ray spectroscopy of light kaonic atoms is a unique tool to provide precise information on the fundamental K̄N interaction at the low-energy limit and the in-medium nuclear interaction of K−. The future experiments of kaonic deuterium strong-interaction shift and width (SIDDHARTA-2 and J-PARC E57 can extract the isospin dependent K−N interaction at threshold. The high-resolution X-ray spectroscopy of kaonic helium with microcalorimeters (J-PARC E62 has the possibility to solve the long-standing potential-strength problem of the attractive K−-nucleus interaction. Here, the recent experimental results and the future projects of X-ray spectroscopy of light kaonic atoms are presented.

  6. Single atom identification by energy dispersive x-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Lovejoy, T. C.; Dellby, N.; Krivanek, O. L. [Nion, 1102 8th St., Kirkland, Washington 98033 (United States); Ramasse, Q. M. [SuperSTEM Laboratory, STFC Daresbury, Keckwick Lane, Daresbury WA4 4AD (United Kingdom); Falke, M.; Kaeppel, A.; Terborg, R. [Bruker Nano GmbH, Schwarzschildstr. 12, 12489 Berlin (Germany); Zan, R. [School of Physics and Astronomy, University of Manchester, Manchester M13 9PL (United Kingdom)

    2012-04-09

    Using aberration-corrected scanning transmission electron microscope and energy dispersive x-ray spectroscopy, single, isolated impurity atoms of silicon and platinum in monolayer and multilayer graphene are identified. Simultaneously acquired electron energy loss spectra confirm the elemental identification. Contamination difficulties are overcome by employing near-UHV sample conditions. Signal intensities agree within a factor of two with standardless estimates.

  7. Nanosecond X-Ray Photon Correlation Spectroscopy on Magnetic Skyrmions

    Science.gov (United States)

    Seaberg, M. H.; Holladay, B.; Lee, J. C. T.; Sikorski, M.; Reid, A. H.; Montoya, S. A.; Dakovski, G. L.; Koralek, J. D.; Coslovich, G.; Moeller, S.; Schlotter, W. F.; Streubel, R.; Kevan, S. D.; Fischer, P.; Fullerton, E. E.; Turner, J. L.; Decker, F.-J.; Sinha, S. K.; Roy, S.; Turner, J. J.

    2017-08-01

    We report an x-ray photon correlation spectroscopy method that exploits the recent development of the two-pulse mode at the Linac Coherent Light Source. By using coherent resonant x-ray magnetic scattering, we studied spontaneous fluctuations on nanosecond time scales in thin films of multilayered Fe/Gd that exhibit ordered stripe and Skyrmion lattice phases. The correlation time of the fluctuations was found to differ between the Skyrmion phase and near the stripe-Skyrmion boundary. This technique will enable a significant new area of research on the study of equilibrium fluctuations in condensed matter.

  8. Nanosecond X-Ray Photon Correlation Spectroscopy on Magnetic Skyrmions.

    Science.gov (United States)

    Seaberg, M H; Holladay, B; Lee, J C T; Sikorski, M; Reid, A H; Montoya, S A; Dakovski, G L; Koralek, J D; Coslovich, G; Moeller, S; Schlotter, W F; Streubel, R; Kevan, S D; Fischer, P; Fullerton, E E; Turner, J L; Decker, F-J; Sinha, S K; Roy, S; Turner, J J

    2017-08-11

    We report an x-ray photon correlation spectroscopy method that exploits the recent development of the two-pulse mode at the Linac Coherent Light Source. By using coherent resonant x-ray magnetic scattering, we studied spontaneous fluctuations on nanosecond time scales in thin films of multilayered Fe/Gd that exhibit ordered stripe and Skyrmion lattice phases. The correlation time of the fluctuations was found to differ between the Skyrmion phase and near the stripe-Skyrmion boundary. This technique will enable a significant new area of research on the study of equilibrium fluctuations in condensed matter.

  9. X-Ray and Near-Infrared Spectroscopy of Dim X-Ray Point Sources Constituting the Galactic Ridge X-Ray Emission

    Directory of Open Access Journals (Sweden)

    Kumiko Morihana

    2014-12-01

    Full Text Available We present the results of X-ray and Near-Infrared observations of the Galactic Ridge X-ray Emission (GRXE. We extracted 2,002 X-ray point sources in the Chandra Bulge Field (l =0°.113, b = 1°.424 down to ~10-14.8 ergscm-2s-1 in 2-8 keV band with the longest observation (900 ks of the GRXE. Based on X-ray brightness and hardness, we classied the X-ray point sources into three groups: A (hard, B (soft and broad spectrum, and C (soft and peaked spectrum. In order to know populations of the X-ray point sources, we carried out NIR imaging and spectroscopy observation. We identied 11% of X-ray point sources with NIR and extracted NIR spectra for some of them. Based on X-ray and NIR properties, we concluded that non-thermal sources in the group A are mostly active galactic nuclei and the thermal sources are mostly white dwarf binaries such as cataclysmic variables (CVs and Pre-CVs. We concluded that the group B and C sources are X-ray active stars in flare and quiescence, respectively.

  10. Vanadium Oxidation State Determination by X-Ray Absorption Spectroscopy

    Science.gov (United States)

    Duchesne, Marc A.; Nakano, Jinichiro; Hu, Yongfeng; MacLennan, Aimee; Hughes, Robin W.; Bennett, James; Nakano, Anna

    Vanadium is found in slags produced during metal refinement and fossil fuel combustion/gasification. The oxidation state of vanadium in slag has technological and environmental implications. For example, it may affect slag flow and refractory wear inside reactors, as well as leachability and toxicity of industrial by-products. Determination of vanadium's oxidation state in crystalline phases can be achieved via the widely adopted X-ray diffraction (XRD) technique. However, this technique does not provide information on vanadium in amorphous phases. The objective of this research is to determine the oxidation state of vanadium in petroleum coke gasification samples and laboratory samples using X-ray absorption spectroscopy (XAS) with Canadian Light Source's soft X-ray micro-characterization beamline (SXRMB). Linear combination fitting of XAS spectra with reference samples allowed quantitative determination of vanadium speciation.

  11. Tracking of azobenzene isomerization by X-ray emission spectroscopy.

    Science.gov (United States)

    Ebadi, H

    2014-09-11

    Cis-trans isomerizations are among the fundamental processes in photochemistry. In azobenzene or its derivatives this dynamics is, due to its reversibility, one of the reactions widely used in photostimulation of molecular motors or in molecular electronics. Though intensively investigated in the optical regime, no detailed study exists in the X-ray regime so far. Because the X-ray emission spectroscopy echoes the electronic structure sensitive to the geometry, this theoretical report based on the density functional theory and its time-dependent version presents different nitrogen K-edge X-ray emission spectra for cis and trans isomers with close interrelation to their electron configuration. Considering the spectrum along the isomerization path, these structural signatures can be utilized to probe the isomerization dynamics in the excited molecule. The scheme can further be generalized to the element specific photoreactions.

  12. Hard X-rays in–soft X-rays out: An operando piggyback view deep into a charging lithium ion battery with X-ray Raman spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Braun, Artur, E-mail: artur.braun@alumni.ethz.ch [Laboratory for High Performance Ceramics. Empa, Swiss Federal Laboratories for Materials Science and Technology, CH-8600 Dübendorf (Switzerland); Nordlund, Dennis [Stanford Synchrotron Radiation Lightsource, SLAC National Accelerator Laboratory, Menlo Park, CA 94720 (United States); Song, Seung-Wan [Department of Fine Chemical Engineering & Applied Chemistry, Chungnam National University, Daejeon 305-764 (Korea, Republic of); Huang, Tzu-Wen [Laboratory for High Performance Ceramics. Empa, Swiss Federal Laboratories for Materials Science and Technology, CH-8600 Dübendorf (Switzerland); Sokaras, Dimosthenis [Stanford Synchrotron Radiation Lightsource, SLAC National Accelerator Laboratory, Menlo Park, CA 94720 (United States); Liu, Xiasong; Yang, Wanli [Advanced Light Source, Ernest Orlando Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Weng, Tsu-Chien [Stanford Synchrotron Radiation Lightsource, SLAC National Accelerator Laboratory, Menlo Park, CA 94720 (United States); Liu, Zhi [Advanced Light Source, Ernest Orlando Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States)

    2015-04-15

    Graphical abstract: - Abstract: For lithium intercalation battery electrodes, understanding of the electronic structure of bulk and surface is essential for their operation and functionality. Soft X-rays are excellent probes for such electronic structure information, but soft X-rays are predominantly surface sensitive and thus cannot probe the bulk. Moreover, soft X-rays hardly permit meaningful in situ and operando studies in battery assemblies. We show here how we penetrate with hard X-rays (>10 keV) in situ a lithium cell, containing a manganite-based cathode. Through X-ray Raman spectroscopy we extract the Mn 2p multiplet from the entire cathode material, thus obtaining bulk-sensitive electronic structure information during battery charging and discharging.

  13. Introductory overview: X-ray absorption spectroscopy and structural genomics.

    Science.gov (United States)

    Ascone, Isabella; Fourme, Roger; Hasnain, S Samar

    2003-01-01

    A special Issue of the Journal is presented, dedicated to biological applications of X-ray absorption spectroscopy (BioXAS) and examining the role of this technique in post-genomic biology. The Issue confirms that BioXAS has come of age and it can be expected to make a significant contribution in the structural genomics effort on metalloproteins, which are estimated to make up about 30% of proteins coded by genomes.

  14. Ultrafast x-ray-induced nuclear dynamics in diatomic molecules using femtosecond x-ray-pump–x-ray-probe spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Lehmann, C. S.; Picón, A.; Bostedt, C.; Rudenko, A.; Marinelli, A.; Moonshiram, D.; Osipov, T.; Rolles, D.; Berrah, N.; Bomme, C.; Bucher, M.; Doumy, G.; Erk, B.; Ferguson, K. R.; Gorkhover, T.; Ho, P. J.; Kanter, E. P.; Krässig, B.; Krzywinski, J.; Lutman, A. A.; March, A. M.; Ray, D.; Young, L.; Pratt, S. T.; Southworth, S. H.

    2016-07-01

    The availability at x-ray free electron lasers of generating two intense, femtosecond x-ray pulses with controlled time delay opens the possibility of performing time-resolved experiments for x-ray induced phenomena. We have applied this capability to molecular dynamics. In diatomic molecules composed of low-Z elements, K-shell ionization creates a core-hole state in which the main decay is an Auger process involving two electrons in the valence shell. After Auger decay, the nuclear wavepackets of the transient two-valence-hole states continue evolving on the femtosecond timescale, leading either to separated atomic ions or long-lived quasi-bound states. By using an x-ray pump and an x-ray probe pulse tuned above the K-shell ionization threshold of the nitrogen molecule, we are able to observe ion dissociation in progress by measuring the time-dependent kinetic energy releases of different breakup channels. We simulated the measurements on N2 with a molecular dynamics model that accounts for K-shell ionization, Auger decay, and time evolution of the nuclear wavepackets. In addition to explaining the time-dependent feature in the measured kinetic energy release distributions from the dissociative states, the simulation also reveals the contributions of quasi-bound states.

  15. Advances in X-ray spectroscopy contributions in honour of professor Y. Cauchois

    CERN Document Server

    Bonnelle, C

    1982-01-01

    Advances in X-Ray Spectroscopy covers topics relevant to the advancement of X-ray spectroscopy technology. The book is a collection of papers written by specialists in X-ray spectroscopy and pays tribute to the scientific work of Prof. Yvette Cauchois. The text is organized into four parts. Part I covers the analysis of X-ray transitions between atomic levels and relativistic theories of X-ray emission satellites and electron BremsStrahlung. Part II reviews the means provided by X-ray spectroscopy for the determination of the electronic structure of solids, while Part III discusses methods of

  16. Hard X-ray emission spectroscopy with pink beam

    Energy Technology Data Exchange (ETDEWEB)

    Kvashnina, Kristina O.; Rossberg, Andre; Exner, Joerg; Scheinost, Andreas C. [Helmholtz-Zentrum Dresden-Rossendorf e.V., Dresden (Germany). Molecular Structures

    2017-06-01

    Valence-band X-ray emission spectroscopy (XES) with a ''pink beam'', i.e. a beam with large energy bandwidth produced by a double-multilayer monochromator, is introduced here to overcome the weak count rate of monochromatic beams produced by conventional double-crystal monochromators. Our results demonstrate that - in spite of the large bandwidth in the order of 100 eV - the high spectral resolution of the Johann-type spectrometer is maintained, while the two orders of magnitude higher flux greatly reduces the required counting time. The short working distance Johann-type X-ray emission spectrometer and multilayer monochromator is available at ROBL.

  17. Valence-to-core-detected X-ray absorption spectroscopy

    DEFF Research Database (Denmark)

    Hall, Eleanor R.; Pollock, Christopher J.; Bendix, Jesper

    2014-01-01

    X-ray absorption spectroscopy (XAS) can provide detailed insight into the electronic and geometric structures of transition-metal active sites in metalloproteins and chemical catalysts. However, standard XAS spectra inherently represent an average contribution from the entire coordination...... environment with limited ligand selectivity. To address this limitation, we have investigated the enhancement of XAS features using valence-to-core (VtC)-detected XAS, whereby XAS spectra are measured by monitoring fluorescence from valence-to-core X-ray emission (VtC XES) events. VtC emission corresponds...... to transitions from filled ligand orbitals to the metal 1s core hole, with distinct energetic shifts for ligands of differing ionization potentials. VtC-detected XAS data were obtained from multiple valence emission features for a series of well-characterized Mn model compounds; taken together, these data...

  18. Arsenic speciation in solids using X-ray absorption spectroscopy

    Science.gov (United States)

    Foster, Andrea L.; Kim, Chris S.

    2014-01-01

    Synchrotron-based X-ray absorption spectroscopy (XAS) is an in situ, minimally-destructive, element-specific, molecular-scale structural probe that has been employed to study the chemical forms (species) of arsenic (As) in solid and aqueous phases (including rocks, soils, sediment, synthetic compounds, and numerous types of biota including humans) for more than 20 years. Although several excellent reviews of As geochemistry and As speciation in the environment have been published previously (including recent contributions in this volume), the explosion of As-XAS studies over the past decade (especially studies employing microfocused X-ray beams) warrants this new review of the literature and of data analysis methods.

  19. X-ray absorption spectroscopy using a self-seeded soft X-ray free-electron laser

    OpenAIRE

    Kroll, Thomas; Kern, Jan; Kubin, Markus; Ratner, Daniel; Gul, Sheraz; Fuller, Franklin D.; Löchel, Heike; Krzywinski, Jacek; Lutman, Alberto; Ding, Yuantao; Dakovski, Georgi L.; Moeller, Stefan; Turner, Joshua J.; Alonso-Mori, Roberto; Nordlund, Dennis L.

    2016-01-01

    X-ray free electron lasers (XFELs) enable unprecedented new ways to study the electronic structure and dynamics of transition metal systems. L-edge absorption spectroscopy is a powerful technique for such studies and the feasibility of this method at XFELs for solutions and solids has been demonstrated. However, the required x-ray bandwidth is an order of magnitude narrower than that of self-amplified spontaneous emission (SASE), and additional monochromatization is needed. Here we compare L-...

  20. X-ray absorption spectroscopy using a self-seeded soft X-ray free-electron laser

    OpenAIRE

    Kroll, T.; J. Kern; Kubin, M; Ratner, D.; Gul, S.; Fuller, FD; Löchel, H.; Krzywinski, J.; A. Lutman; Ding, Y.; Dakovski, GL; Moeller, S.; Turner, JJ; Alonso-Mori, R.; Nordlund, DL

    2016-01-01

    © 2016 Optical Society of America. X-ray free electron lasers (XFELs) enable unprecedented new ways to study the electronic structure and dynamics of transition metal systems. L-edge absorption spectroscopy is a powerful technique for such studies and the feasibility of this method at XFELs for solutions and solids has been demonstrated. However, the required x-ray bandwidth is an order of magnitude narrower than that of self-amplified spontaneous emission (SASE), and additional monochromatiz...

  1. X-ray photoelectron spectroscopy, high-resolution X-ray diffraction ...

    Indian Academy of Sciences (India)

    Powder X-ray diffraction studies were carried out on doped lithium niobate for phase identification. High-resolution X-ray diffraction technique was used to study the crystalline quality through full-width at half-maximum values. The refractive index values are more for doped samples than for pure sample as determined by ...

  2. Metallic magnetic calorimeters for high resolution X-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Krantz, M.; Hengstler, D.; Geist, J.; Schoetz, C.; Hassel, K.; Hendricks, S.; Keller, M.; Kempf, S.; Gastaldo, L.; Fleischmann, A.; Enss, C. [Heidelberg Univ. (Germany). KIP

    2015-07-01

    We develop microfabricated, energy dispersive particle detector arrays based on metallic magnetic calorimeters (MMCs) for high resolution X-ray spectroscopy to challenge bound-state QED calculations. Our MMCs are operated at about T=30 mK and use a paramagnetic temperature sensor, read-out by a SQUID, to measure the energy deposited by single X-ray photons. We discuss the physics of MMCs, the detector performance and the cryogenic setups for two different detector arrays. We present their microfabrication layouts with focus on challenges like the heatsinking of each pixel of the detector and the overhanging absorbers. The maXs-20 detector is a linear 1x8-pixel array with excellent linearity in its designated energy range up to 20 keV and unsurpassed energy resolution of 1.6 eV for 6 keV x-rays. MaXs-20 operated in a highly portable pulse tube cooled ADR setup has already been used at the EBIT facilities of the MPI-K for new reference measurements of V-like and Ti-like tungsten. The maXs-30 detector currently in development is a 8x8-pixel 2d-array with an active detection area of 16 mm{sup 2} and is designed to detect X-rays up to 50 keV with a designated energy resolution below 5 eV. MaXs-30 will be operated in a cryogen free 3He/4He-dilution refrigerator at the tip of a 40 cm long cold finger at T=20 mK.

  3. High-Precision Spectroscopy with Counterpropagating Femtosecond Pulses

    Science.gov (United States)

    Barmes, Itan; Witte, Stefan; Eikema, Kjeld S. E.

    2013-07-01

    An experimental realization of high-precision direct frequency comb spectroscopy using counterpropagating femtosecond pulses on two-photon atomic transitions is presented. The Doppler broadened background signal, hampering precision spectroscopy with ultrashort pulses, is effectively eliminated with a simple pulse shaping method. As a result, all four 5S-7S two-photon transitions in a rubidium vapor are determined with both statistical and systematic uncertainties below 10-11, which is an order of magnitude better than previous experiments on these transitions.

  4. Hubbard Model Approach to X-ray Spectroscopy

    Science.gov (United States)

    Ahmed, Towfiq

    We have implemented a Hubbard model based first-principles approach for real-space calculations of x-ray spectroscopy, which allows one to study excited state electronic structure of correlated systems. Theoretical understanding of many electronic features in d and f electron systems remains beyond the scope of conventional density functional theory (DFT). In this work our main effort is to go beyond the local density approximation (LDA) by incorporating the Hubbard model within the real-space multiple-scattering Green's function (RSGF) formalism. Historically, the first theoretical description of correlated systems was published by Sir Neville Mott and others in 1937. They realized that the insulating gap and antiferromagnetism in the transition metal oxides are mainly caused by the strong on-site Coulomb interaction of the localized unfilled 3d orbitals. Even with the recent progress of first principles methods (e.g. DFT) and model Hamiltonian approaches (e.g., Hubbard-Anderson model), the electronic description of many of these systems remains a non-trivial combination of both. X-ray absorption near edge spectra (XANES) and x-ray emission spectra (XES) are very powerful spectroscopic probes for many electronic features near Fermi energy (EF), which are caused by the on-site Coulomb interaction of localized electrons. In this work we focus on three different cases of many-body effects due to the interaction of localized d electrons. Here, for the first time, we have applied the Hubbard model in the real-space multiple scattering (RSGF) formalism for the calculation of x-ray spectra of Mott insulators (e.g., NiO and MnO). Secondly, we have implemented in our RSGF approach a doping dependent self-energy that was constructed from a single-band Hubbard model for the over doped high-T c cuprate La2-xSrxCuO4. Finally our RSGF calculation of XANES is calculated with the spectral function from Lee and Hedin's charge transfer satellite model. For all these cases our

  5. Individual heteroatom identification with X-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Stroud, R. M., E-mail: rhonda.stroud@nrl.navy.mil; Bassim, N. D. [Materials Science and Technology Division, Naval Research Laboratory, 4555 Overlook Ave. South West, Washington, District of Columbia 20375 (United States); Lovejoy, T. C.; Corbin, G. J.; Dellby, N.; Hrncirik, P.; Krivanek, O. L. [Nion Co., 11511 NE 118th St., Kirkland, Washington 98034 (United States); Falke, M.; Kaeppel, A.; Noack, M.; Hahn, W.; Rohde, M. [Bruker Nano GmbH, Am Studio 2D, 12489 Berlin (Germany)

    2016-04-18

    Individual heteroatoms in nanoscale materials often play a pivotal role in materials properties. To obtain maximum control over materials properties, researchers must be able to detect and identify diverse heteroatoms in samples with varying thickness and composition. Here, we demonstrate the identification of individual Si, S, P, and Ca heteroatoms in two-phase carbonaceous nanoscale mixtures with energy dispersive X-ray spectroscopy in a scanning transmission electron microscope. In order to fully demonstrate the robustness of the technique and the potential advantages over electron energy loss spectroscopy for single-atom speciation, no a priori constraint was placed on the sample thickness or types of heteroatom species. The various heteroatoms were identified with X-ray spectrum collection times ranging from 8 to 57 s, and normalized count rates of 0.096–0.007 counts s{sup −1} pA{sup −1}. The lowest times/highest effective count rates were achieved by maximizing the effective dwell time on the atom, through minimizing the oversampling area of the electron beam raster.

  6. The high-precision x-ray tomograph for quality control of the ATLAS MDT muon spectrometer

    CERN Document Server

    Drakoulakos, D G; Maugain, J M; Rohrbach, F; Sedykh, Yu

    1997-01-01

    For the Large Hadron Collider (LHC) of the next millennium, a large general-purpose high-energy physics experiment, the ATLAS project, is being designed by a world-wide collaboration. One of its detectors, the ATLAS muon tracking detector, the MDT project, is on the scale of a very large industrial project: the design, the construction and assembly of twelve hundred large muon drift chambers are aimed at producing an exceptional quality in terms of accuracy, material reliability, assembly, and monitoring. This detector, based on the concept of very high mechanical precision required by the physics goals, will use tomography as a quality control platform. An X-ray tomograph prototype, monitored by a set of interferometers, has been developed at CERN to provide high-quality control of the MDT chambers which will be built in the collaborating institutes of the ATLAS project. First results have been obtained on MDT prototypes showing the validity of the X-ray tomograph approach for mechanical control of the detec...

  7. X-ray magneto-optical polarization spectroscopy: an analysis from the visible region to the x-ray regime.

    Science.gov (United States)

    Tesch, M F; Gilbert, M C; Mertins, H-Ch; Bürgler, D E; Berges, U; Schneider, C M

    2013-06-20

    An ultra-high vacuum compatible multipurpose chamber for magneto-optical reflection and transmission experiments with polarization analysis on magnetic systems is introduced. It is applicable in a broad photon energy range from the visible to the soft x-ray regime and for a wide angular range from grazing to normal incidence. It exploits a novel magnetization device based on rotating permanent magnets, which generates tuneable magnetic fields up to 570 mT in longitudinal, transverse and polar geometry. The unique combination of these features enables the feasibility of all typical magneto-optical spectroscopy techniques as T-MOKE, L-MOKE, P-MOKE, x-ray magneto optical linear dichroism, x-ray magnetic circular dichroism in reflection and Kerr polarization-spectroscopy, which is demonstrated for Co with focus on the Co 3p edges.

  8. Characterization of Metalloproteins and Biomaterials by X-ray Absorption Spectroscopy and X-ray Diffraction

    DEFF Research Database (Denmark)

    Frankær, Christian Grundahl

    This thesis presents thework on combining complementary X-rays techniques for studying the structures of proteins and other biomaterials, and consists of three different projects: (i) Characterization of protein powders with X-ray powder diffraction (XRPD). (ii) The combination of X-ray crystallo......This thesis presents thework on combining complementary X-rays techniques for studying the structures of proteins and other biomaterials, and consists of three different projects: (i) Characterization of protein powders with X-ray powder diffraction (XRPD). (ii) The combination of X......, nickel and copper, and their XRD crystal structures were solved to 1.90 Å, 1.50 Å and 1.45 Å resolution, respectively. As the affinity to iron is low, iron insulin crystals were grown in presence of small amounts of zinc. The two metal sites in the XRD structure thus contained respectively one Fe2......+ and one Zn2+ ion, with respectively tetrahedral and octahedral coordination geometry. The metal sites in nickel and copper insulin were studied by XAS. Coordination distances were refined from EXAFS showing a very regular octahedral coordination of Ni2+, which was further verified by calculated XANES...

  9. A high-precision X-ray tomograph for quality control of the ATLAS Muon Monitored Drift Tube Chambers

    CERN Document Server

    Schuh, S; Banhidi, Z; Fabjan, Christian Wolfgang; Lampl, W; Marchesotti, M; Rangod, Stephane; Sbrissa, E; Smirnov, Y; Voss, Rüdiger; Woudstra, M; Zhuravlov, V

    2004-01-01

    A dedicated X-ray tomograph has been developed at CERN to control the required wire placement accuracy of better than 20mum of the 1200 Monitored Drift Tube Chambers which make up most of the precision chamber part of the ATLAS Muon Spectrometer. The tomograph allows the chamber wire positions to be measured with a 2mum statistical and 2mum systematic uncertainty over the full chamber cross-section of 2.2 multiplied by 0.6m**2. Consistent chamber production quality over the 4-year construction phase is ensured with a similar to 15% sampling rate. Measurements of about 70 of the 650 MDT chambers so far produced have been essential in assessing the validity and consistency of the various construction procedures.

  10. Experimental characterization of hohlraum conditions by X-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Back, C.A.; Hsieh, E.J.; Kauffman, R.L. [and others

    1996-06-01

    Spectroscopy is a powerful technique used to measure the plasma parameters relevant to Inertial Confinement Fusion (ICF) plasmas. For instance, the onset of spectral signals from multilayer targets have been used to determine ablation rate scalings. Temperature and density measurements in coronal plasmas have enabled the study of laser coupling efficiency as a function of the laser wavelengths. More recently, dopants have been successfully used to determine capsule conditions of ICF targets. However, few spectroscopic studies have been performed to diagnose plasma conditions of the hohlraum itself. Several laboratories have studied enclosed cavities, previously concentrating on measurements of the radiative heat wave, the x-ray conversion efficiency, and temporal evolution of Au x rays. Measurements of electron temperature T{sub e} and electron densities n{sub e} are difficult because many physical processes occur and each diagnostic`s line-of-sight is restricted by the hohlraum wall. However, they are worth pursuing because they can provide critical information on the target energetics and the evolution of plasma parameters important to achieving fusion. Here the authors discuss spectroscopic tracers to diagnose plasma conditions in the hohlraum, using time- and space-resolved measurements. The tracers are typically mid-Z elements which are placed on the hohlraum wall or supended in the hohlraum volume. To demonstrate the breadth of measurements that can be performed, three types of experiments are presented.

  11. X-ray spectroscopy of chemical systems in liquids phase

    Energy Technology Data Exchange (ETDEWEB)

    Yin, Zhong; Kubicek, Katharina [Max Planck Institute for Biophysical Chemistry, Goettingen (Germany); Deutsches Elektronen Synchrotron DESY, Hamburg (Germany); Techert, Simone; Rajkovic, Ivan [Max Planck Institute for Biophysical Chemistry, Goettingen (Germany); Foehlisch, Alexander [Helmholtz Zentrum Berlin, Berlin (Germany); University of Potsdam (Germany); Wernet, Philippe; Quevedo, Wilson [Helmholtz Zentrum Berlin, Berlin (Germany)

    2013-07-01

    Based on their ability to salt in or salt out macromolecules salt ions are classified according to the Hofmeister series. While the macroscopic effect is known for over 100 years, the origin of the effect on the molecular level is still not understood. We present X-ray emission spectroscopy (XES) on the oxygen K-edge of water in aqueous solutions of inorganic salts using BESSY II synchrotron (Berlin, Germany) X-rays. The FlexRIXS end station utilized a liquid micro jet for sample delivery. The element- and site-specific XES method contains information about occupied and unoccupied molecular orbitals and is therefore sensitive to the chemical environment. The aim of our measurements was to reveal the influence of the water-ion interactions on the local water structure further elucidating the understanding of the structure maker and structure breaker concept. Structural changes while utilizing different salts were expected to show as spectral changes in the oxygen K-edge spectra, e.g. of peak shapes or intensities.

  12. Application of X-ray Optics to Energy-Dispersive Spectroscopy.

    Science.gov (United States)

    McCarthy; McMillan

    1998-11-01

    : X-ray optics have been used in X-ray analytical instruments for several years. Applications of X-ray optics have been reported in X-ray diffraction, X-ray fluorescence, and wavelength dispersive spectroscopy. X-ray optics have been used to increase the X-ray flux incident on the sample or to direct and focus emitted X-rays from a sample. We report here the use of a grazing incidence optic (GIO) as a flux-enhancing collimator for use with an energy-dispersive (ED) detector used to perform electron beam microanalysis. We found that the GIO in combination with an ED spectrometer (EDS) provides substantial intensity gain for X-ray lines with energy below 1 keV. The GIO is also found to provide a modest focus effect, and introduces minimal spectral artifacts.

  13. X-ray photoelectron spectroscopy of FeP phosphide

    Energy Technology Data Exchange (ETDEWEB)

    Teterin, Yu. A.; Sobolev, A. V., E-mail: salex12@rambler.ru, E-mail: alex@radio.chem.msu.ru; Presnyakov, I. A.; Maslakov, K. I. [Moscow State University (Russian Federation); Teterin, A. Yu. [National Research Center “Kurchatov Institute,” (Russian Federation); Morozov, I. V.; Chernyavskii, I. O. [Moscow State University (Russian Federation); Ivanov, K. E. [National Research Center “Kurchatov Institute,” (Russian Federation); Shevel’kov, A. V. [Moscow State University (Russian Federation)

    2017-02-15

    The structure of the outer and inner electron spectra of iron (2p, 3p, 3s, and 3d) and phosphorus (3s and 3p) atoms in FeP monophosphide is studied in detail by the X-ray photoelectron spectroscopy (XPS) method. On the basis of the analysis of the binding energy of electrons, as well as the parameters characterizing the structure of experimental spectra, a conclusion is made that Fe{sup 3+} (d{sup 5}) cations in FeP are stabilized in a state with intermediate value of the total spin (IS, S = 3/2). The range of values of intra-atomic parameters (10Dq, J{sub H}) is established in which the consideration of the high degree of covalence of Fe–P bonds may lead to the stabilization of (FeP{sub 6}){sup 15–} clusters in the IS state.

  14. X-ray absorption spectroscopy using a self-seeded soft X-ray free-electron laser.

    Science.gov (United States)

    Kroll, Thomas; Kern, Jan; Kubin, Markus; Ratner, Daniel; Gul, Sheraz; Fuller, Franklin D; Löchel, Heike; Krzywinski, Jacek; Lutman, Alberto; Ding, Yuantao; Dakovski, Georgi L; Moeller, Stefan; Turner, Joshua J; Alonso-Mori, Roberto; Nordlund, Dennis L; Rehanek, Jens; Weniger, Christian; Firsov, Alexander; Brzhezinskaya, Maria; Chatterjee, Ruchira; Lassalle-Kaiser, Benedikt; Sierra, Raymond G; Laksmono, Hartawan; Hill, Ethan; Borovik, Andrew; Erko, Alexei; Föhlisch, Alexander; Mitzner, Rolf; Yachandra, Vittal K; Yano, Junko; Wernet, Philippe; Bergmann, Uwe

    2016-10-03

    X-ray free electron lasers (XFELs) enable unprecedented new ways to study the electronic structure and dynamics of transition metal systems. L-edge absorption spectroscopy is a powerful technique for such studies and the feasibility of this method at XFELs for solutions and solids has been demonstrated. However, the required x-ray bandwidth is an order of magnitude narrower than that of self-amplified spontaneous emission (SASE), and additional monochromatization is needed. Here we compare L-edge x-ray absorption spectroscopy (XAS) of a prototypical transition metal system based on monochromatizing the SASE radiation of the linac coherent light source (LCLS) with a new technique based on self-seeding of LCLS. We demonstrate how L-edge XAS can be performed using the self-seeding scheme without the need of an additional beam line monochromator. We show how the spectral shape and pulse energy depend on the undulator setup and how this affects the x-ray spectroscopy measurements.

  15. STROBE-X: X-ray timing and spectroscopy on dynamical timescales from microseconds to years

    Directory of Open Access Journals (Sweden)

    Colleen A. Wilson-Hodge

    Full Text Available The Spectroscopic Time-Resolving Observatory for Broadband Energy X-rays (STROBE-X probes strong gravity for stellar mass to supermassive black holes and ultradense matter with unprecedented effective area, high time-resolution, and good spectral resolution, while providing a powerful time-domain X-ray observatory. Keywords: Missions, X-ray timing, X-ray spectroscopy, Compact objects

  16. New developments in high pressure x-ray spectroscopy beamline at High Pressure Collaborative Access Team.

    Science.gov (United States)

    Xiao, Y M; Chow, P; Boman, G; Bai, L G; Rod, E; Bommannavar, A; Kenney-Benson, C; Sinogeikin, S; Shen, G Y

    2015-07-01

    The 16 ID-D (Insertion Device - D station) beamline of the High Pressure Collaborative Access Team at the Advanced Photon Source is dedicated to high pressure research using X-ray spectroscopy techniques typically integrated with diamond anvil cells. The beamline provides X-rays of 4.5-37 keV, and current available techniques include X-ray emission spectroscopy, inelastic X-ray scattering, and nuclear resonant scattering. The recent developments include a canted undulator upgrade, 17-element analyzer array for inelastic X-ray scattering, and an emission spectrometer using a polycapillary half-lens. Recent development projects and future prospects are also discussed.

  17. Splittings, Satellites and Fine Structure in the Soft X-ray Spectroscopy of the Actinides

    Energy Technology Data Exchange (ETDEWEB)

    Tobin, J. G.; Yu, S. -W.; Chung, B. W.

    2013-06-14

    Perhaps the most demanding and powerful actinide spectroscopy is that using soft X-ray and VUV photons. Because of the relatively low energy and fairly small sampling depths of these photons and the corresponding electrons, it is necessary to use un-encapsulated samples with highly cleaned and well-prepared surfaces. This causes a myriad of sample containment problems for these radioactive materials. Despite these hindrances and difficulties, the soft-X-ray and ultra-violet spectroscopy of the actinides can provide an amazing level of detailed information, particularly having to do with 5f electronic structure. In this paper, the splittings, satellites and fine structure of the following actinide soft X-ray spectroscopies will be discussed: X-ray photoelectron spectroscopy; X-ray absorption spectroscopy; and inverse photoelectron spectroscopy, including Bremstrahlung isochromat spectroscopy and resonant inverse photoelectron spectroscopy.

  18. X-ray absorption spectroscopy of warm dense matter with betatron x-ray radiation (Conference Presentation)

    Science.gov (United States)

    Albert, Felicie

    2017-05-01

    Betatron x-ray radiation, driven by electrons from laser-wakefield acceleration, has unique properties to probe high energy density (HED) plasmas and warm dense matter. Betatron radiation is produced when relativistic electrons oscillate in the plasma wake of a laser pulse. Its properties are similar to those of synchrotron radiation, with a 1000 fold shorter pulse. This presentation will focus on the experimental challenges and results related to the development of betatron radiation for x-ray absorption spectroscopy of HED matter at large-scale laser facilities. A detailed presentation of the source mechanisms and characteristics in the blowout regime of laser-wakefield acceleration will be followed by a description of recent experiments performed at the Linac Coherent Light Source (LCLS). At LCLS, we have recently commissioned the betatron x-ray source driven by the MEC short pulse laser (1 J, 40 fs). The source is used as a probe for investigating the X-ray absorption near edge structure (XANES) spectrum at the K- or L-edge of iron and silicon oxide driven to a warm dense matter state (temperature of a few eV and solid densities). The driver is either LCLS itself or an optical laser. These experiments demonstrate the capability to study the electron-ion equilibration mechanisms in warm dense matter with sub-picosecond resolution.

  19. Electron cyclotron resonance ion source plasma characterization by X-ray spectroscopy and X-ray imaging

    Energy Technology Data Exchange (ETDEWEB)

    Mascali, David, E-mail: davidmascali@lns.infn.it; Castro, Giuseppe; Celona, Luigi; Neri, Lorenzo; Gammino, Santo [INFN–Laboratori Nazionali del Sud, Via S. Sofia 62, 95125 Catania (Italy); Biri, Sándor; Rácz, Richárd; Pálinkás, József [Institute for Nuclear Research (Atomki), Hungarian Academy of Sciences, Bem tér 18/c, H-4026 Debrecen (Hungary); Caliri, Claudia [INFN–Laboratori Nazionali del Sud, Via S. Sofia 62, 95125 Catania (Italy); Università degli Studi di Catania, Dip.to di Fisica e Astronomia, via Santa Sofia 64, 95123 Catania (Italy); Romano, Francesco Paolo [INFN–Laboratori Nazionali del Sud, Via S. Sofia 62, 95125 Catania (Italy); CNR, Istituto per i Beni Archeologici e Monumentali, Via Biblioteca 4, 95124 Catania (Italy); Torrisi, Giuseppe [INFN–Laboratori Nazionali del Sud, Via S. Sofia 62, 95125 Catania (Italy); Università Mediterranea di Reggio Calabria, DIIES, Via Graziella, I-89100 Reggio Calabria (Italy)

    2016-02-15

    An experimental campaign aiming to investigate electron cyclotron resonance (ECR) plasma X-ray emission has been recently carried out at the ECRISs—Electron Cyclotron Resonance Ion Sources laboratory of Atomki based on a collaboration between the Debrecen and Catania ECR teams. In a first series, the X-ray spectroscopy was performed through silicon drift detectors and high purity germanium detectors, characterizing the volumetric plasma emission. The on-purpose developed collimation system was suitable for direct plasma density evaluation, performed “on-line” during beam extraction and charge state distribution characterization. A campaign for correlating the plasma density and temperature with the output charge states and the beam intensity for different pumping wave frequencies, different magnetic field profiles, and single-gas/gas-mixing configurations was carried out. The results reveal a surprisingly very good agreement between warm-electron density fluctuations, output beam currents, and the calculated electromagnetic modal density of the plasma chamber. A charge-coupled device camera coupled to a small pin-hole allowing X-ray imaging was installed and numerous X-ray photos were taken in order to study the peculiarities of the ECRIS plasma structure.

  20. Prospects for supermirrors in hard x-ray spectroscopy

    DEFF Research Database (Denmark)

    Joensen, Karsten D.; Gorenstein, Paul; Christensen, Finn Erland

    1994-01-01

    reflectivity for x rays. For hard x rays (≥ 15 keV), the absorption, however, is low enough that it is possible to design supermirrors with 10 - 70% reflectivity in a band ≈ 3 times the width of the total reflection regime. Supermirrors of W/Si and Ni/C have been successfully fabricated and characterized...... radiation, and particle filtering in plasma diagnostics....

  1. CdZnTe detector in diagnostic x-ray spectroscopy.

    Science.gov (United States)

    Miyajima, Satoshi; Imagawa, Kotaro; Matsumoto, Masao

    2002-07-01

    A method to utilize CdZnTe (CZT) detectors in diagnostic x-ray spectroscopy is described in this article. Spectral distortion due to transmission of primary x rays, the escape of cadmium- and tellurium-K fluorescent x rays, and tailing was severe in measured x-ray spectra. Therefore, correction for the distortion was performed with the stripping method using response functions. The response functions were calculated with the Monte Carlo method. The Hecht equation was employed to approximate the effects of carrier trapping in the calculations. The parameters in the Hecht equation, the mean-free path (lambda) of electrons and holes, were determined such that the tailing in calculated response functions fit that in measured gamma-ray spectra. Corrected x-ray spectra agreed well with the reference spectra measured with an HPGe detector. The results indicate that CZT detectors are suitable for diagnostic x-ray spectroscopy with appropriate corrections.

  2. Johann Spectrometer for High Resolution X-ray Spectroscopy

    Science.gov (United States)

    Machek, Pavel; Welter, Edmund; Caliebe, Wolfgang; Brüggmann, Ulf; Dräger, Günter; Fröba, Michael

    2007-01-01

    A newly designed vacuum Johann spectrometer with a large focusing analyzer crystal for inelastic x-ray scattering and high resolution fluorescence spectroscopy has been installed at the DORIS III storage ring. Spherically bent crystals with a maximum diameter of 125 mm, and cylindrically bent crystals are employed as dispersive optical elements. Standard radius of curvature of the crystals is 1000 mm, however, the design of the mechanical components also facilitates measurements with smaller and larger bending radii. Up to four crystals are mounted on a revolving crystal changer which enables crystal changes without breaking the vacuum. The spectrometer works at fixed Bragg angle. It is preferably designed for the measurements in non-scanning mode with a broad beam spot, and offers a large flexibility to set the sample to the optimum position inside the Rowland circle. A deep depletion CCD camera is employed as a position sensitive detector to collect the energy-analyzed photons on the circumference of the Rowland circle. The vacuum in the spectrometer tank is typically 10-6 mbar. The sample chamber is separated from the tank either by 25 μm thick Kapton windows, which allows samples to be measured under ambient conditions, or by two gate valves. The spectrometer is currently installed at wiggler beamline W1 whose working range is 4-10.5 keV with typical flux at the sample of 5×1010photons/s/mm2. The capabilities of the spectrometer are illustrated by resonant inelastic experiments on 3d transition metals and rare earth compounds, and by chemical shift measurements on chromium compounds.

  3. The chemical sensitivity of X-ray spectroscopy: high energy resolution XANES versus X-ray emission spectroscopy of substituted ferrocenes.

    Science.gov (United States)

    Atkins, Andrew J; Bauer, Matthias; Jacob, Christoph R

    2013-06-07

    X-ray spectroscopy at the metal K-edge is an important tool for understanding catalytic processes and provides insight into the geometric and electronic structures of transition metal complexes. In particular, X-ray emission-based methods such as high-energy resolution fluorescence detection (HERFD), X-ray absorption near-edge spectroscopy (XANES) and valence-to-core X-ray emission spectroscopy (V2C-XES) hold the promise of providing increased chemical sensitivity compared to conventional X-ray absorption spectroscopy. Here, we explore the ability of HERFD-XANES and V2C-XES spectroscopy to distinguish substitutions beyond the directly coordinated atoms for the example of ferrocene and selected ferrocene derivatives. The experimental spectra are assigned and interpreted through the use of density functional theory (DFT) calculations. We find that while the pre-edge peaks in the HERFD-XANES spectra are affected by substituents at the cyclopentadienyl ring containing π-bonds [A. J. Atkins, Ch. R. Jacob and M. Bauer, Chem.-Eur. J., 2012, 18, 7021], the V2C-XES spectra are virtually unchanged. The pre-edge in HERFD-XANES probes the weak transition to unoccupied metal d-orbitals, while the V2C-XES spectra are determined by dipole-allowed transitions from occupied ligand orbitals to the 1s core hole. The latter turn out to be less sensitive to changes beyond the first coordination shell.

  4. Precision X-ray spectroscopy of kaonic atoms as a probe of low-energy kaon-nucleus interaction

    Directory of Open Access Journals (Sweden)

    Shi H.

    2016-01-01

    Full Text Available In the exotic atoms where one atomic 1s electron is replaced by a K−, the strong interaction between the K− and the nucleus introduces an energy shift and broadening of the low-lying kaonic atomic levels which are determined by only the electromagnetic interaction. By performing X-ray spectroscopy for Z = 1,2 kaonic atoms, the SIDDHARTA experiment determined with high precision the shift and width for the 1s state of K− p and the 2p state of kaonic helium-3 and kaonic helium-4. These results provided unique information of the kaon-nucleus interaction in the low energy limit.

  5. X-ray spectroscopy and dosimetry with a portable CdTe device

    Energy Technology Data Exchange (ETDEWEB)

    Abbene, Leonardo [Dipartimento di Fisica e Tecnologie Relative, Universita di Palermo, Viale delle Scienze, Edificio 18, Palermo 90128 (Italy) and INFN, Sezione di Catania, Catania (Italy)]. E-mail: abbene@difter.unipa.it; La Manna, Angelo [Dipartimento di Fisica e Tecnologie Relative, Universita di Palermo, Viale delle Scienze, Edificio 18, Palermo 90128 (Italy); INFN, Sezione di Catania, Catania (Italy); Fauci, Francesco [Dipartimento di Fisica e Tecnologie Relative, Universita di Palermo, Viale delle Scienze, Edificio 18, Palermo 90128 (Italy); INFN, Sezione di Catania, Catania (Italy); Gerardi, Gaetano [Dipartimento di Fisica e Tecnologie Relative, Universita di Palermo, Viale delle Scienze, Edificio 18, Palermo 90128 (Italy); INFN, Sezione di Catania, Catania (Italy); Stumbo, Simone [Struttura Dipartimentale di Matematica e Fisica dell' Universita degli studi di Sassari, Sassari (Italy); INFN Sezione di Cagliari, Cagliari (Italy); Raso, Giuseppe [Dipartimento di Fisica e Tecnologie Relative, Universita di Palermo, Viale delle Scienze, Edificio 18, Palermo 90128 (Italy); INFN, Sezione di Catania, Catania (Italy)

    2007-02-01

    X-ray spectra and dosimetry information are very important for quality assurance (QA) and quality control (QC) in medical diagnostic X-ray systems. An accurate knowledge of the diagnostic X-ray spectra would improve the patient dose optimization, without compromising image information. In this work, we performed direct diagnostic X-ray spectra measurements with a portable device, based on a CdTe solid-state detector. The portable device is able to directly measure X-ray spectra at high photon fluence rates, as typical of clinical radiography. We investigated on the spectral performances of the system in the mammographic energy range (up to {approx}40 keV). Good system response to monoenergetic photons was measured (energy resolution of 5% FWHM at 22.1 keV). We measured the molybdenum X-ray spectra produced by a mammographic X-ray unit (GE Senographe DMR) at 28 kV and 30 kV under clinical conditions. The results showed the good reproducibility of the system and low pile-up distortions. Preliminary dosimetric measurements have been regarded as exposure and half value layer (HVL) values obtained from direct measurements and from measured X-ray spectral data, and a good agreement between exposure attenuation curves and the HVL values was obtained. The results indicated that the portable device is suitable for mammographic X-ray spectroscopy under clinical conditions.

  6. X-ray absorption and X-ray emission spectroscopy theory and applications

    CERN Document Server

    Lamberti, Carlo

    2016-01-01

    During the last two decades, remarkable and often spectacular progress has been made in the methodological and instrumental aspects of x–ray absorption and emission spectroscopy. This progress includes considerable technological improvements in the design and production of detectors especially with the development and expansion of large-scale synchrotron reactors All this has resulted in improved analytical performance and new applications, as well as in the perspective of a dramatic enhancement in the potential of x–ray based analysis techniques for the near future. This comprehensive two-volume treatise features articles that explain the phenomena and describe examples of X–ray absorption and emission applications in several fields, including chemistry, biochemistry, catalysis, amorphous and liquid systems, synchrotron radiation, and surface phenomena. Contributors explain the underlying theory, how to set up X–ray absorption experiments, and how to analyze the details of the resulting spectra. X-R...

  7. Magnetic effects in resonant X-ray emission spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Grebennikov, V.I. E-mail: greben@imp.uran.ru

    2004-07-01

    A theoretical description for L{sub {alpha}} and L{sub {beta}} emission spectra recorded at different excitation photon energies gives the main spectral lines: a normal emission peak, with the constant energy, and a quasi-elastic peak that moves in energy scale when the incident photon energy changes. The intensity of the quasi-elastic peak is strongly controlled by valence electron excitations due to core-hole effects. Characteristic shake-up processes give rise to double lines in spectra. Applications of resonant inelastic soft X-ray scattering for studying magnetic systems are discussed. Emission spectra (as well as absorption spectra) show the magnetic dichroism when they are excited by the polarized incident X-ray radiation. But, the emission experiments contain information on the local magnetic moment values on excited atoms even in the case of depolarized incident radiation and in disordered magnetic states. The integral intensities ratio for L{sub {beta}}/L{sub {alpha}} lines in transition metal oxides are analyzed from this point of view. The similarity of experimental X-ray fluorescent spectra with emission spectra received by electron impacts allow us to conclude that in 3d-element compounds the high-energy electron impact transfers the 2p-electron into valence states with considerable probability.

  8. Femtosecond X-ray absorption and emission spectroscopy on zno nanoparticles in solution

    DEFF Research Database (Denmark)

    Penfold, Thomas J.; Szlachetko, Jakub; Gawelda, Wojciech

    2016-01-01

    We have performed femtosecond X-ray spectroscopy measurements after UV photoexcitation of a colloidal solution of ZnO nanoparticles. The results indicate sub-ps hole trapping at oxygen vacancies with shallowly-trapped electrons in the conduction band.......We have performed femtosecond X-ray spectroscopy measurements after UV photoexcitation of a colloidal solution of ZnO nanoparticles. The results indicate sub-ps hole trapping at oxygen vacancies with shallowly-trapped electrons in the conduction band....

  9. Soft x-ray pulse length measurement by pump-probe absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Tom, H.W.K. [Univ. of California, Riverside, CA (United States); Sher, M.H.; Mohideen, U.; Wood, O.R. II; Aumiller, G.D. [AT and T Bell Labs., Holmdel, NJ (United States); McIlrath, T.J. [Univ. of Maryland, College Park, MD (United States); Bokor, J.; Freeman, R.R. [AT and T Bell Labs., Murray Hill, NJ (United States); Sugar, J. [National Institute of Standards and Technology, Gaithersburg, MD (United States)

    1994-12-31

    The authors have demonstrated a system for subpicosecond, soft-x-ray continuum, pump-probe absorption spectroscopy. Using multiphoton ionization to abruptly change the x-ray absorption spectra of a gas, they have measured the temporal profile of laser-generated x-ray pulses near 90 eV. Although the x-ray pulses from a laser-generated plasma here were only as short as {approximately}20 psec, the technique is extendible to higher energy x-rays which will have pulse durations approaching 100 fsec. They also present the absorption spectrum of Kr ions produced under conditions of high intensity non-resonant multiphoton ionization. The spectra are identified with a fit to the Cowan code.

  10. Superconductive tunnel junctions for X-ray spectroscopy

    Science.gov (United States)

    de Korte, P. A. J.; van den Berg, M. L.; Bruijn, M. P.; Frericks, M.; Le Grand, J. B.; Gijsbertsen, J. G.; Houwman, E. P.; Flokstra, J.

    1992-10-01

    Superconductive tunnel junctions are under development as detectors for X-ray astronomy in the 0.5 - 10 keV energy range, because of their potentially high energy resolution in combination with high detection efficiency. Absorber-junction combinations offer the prospect of high energy resolution detectors with a high detection efficiency and a reasonable (about 1/sq cm) size. The proximity effect between the Nb absorber and the Al trapping layer plays a dominant role. A study of the proximity effect in Nb/Al/Al2O3/Al/Nb junctions with different Al-layer, the trapping layer, thicknesses is presented.

  11. Hard X-ray Spectroscopy of Obscured AGN with NuSTAR

    Science.gov (United States)

    Balokovic, Mislav; Harrison, Fiona; NuSTAR Extragalactic Surveys Team

    2017-01-01

    The Nuclear Spectroscopic Telescope Array (NuSTAR) has enabled studies of the local active galactic nuclei (AGN) to extend into the hard X-ray band, up to 79 keV, with unprecedented spatial resolution and sensitivity. As a part of its extragalactic program, NuSTAR is surveying the nearby population of AGN detected at hard X-ray energies by the Swift Burst Alert Telescope (Swift/BAT), selecting even the most obscured local AGN. I will highlight some of the results based on broadband X-ray spectroscopy of individual targets and present my work on the large representative sample of more than a hundred nearby obscured AGN, which constitutes the largest available atlas of hard X-ray spectra of obscured AGN to date. The high quality of the data allows us to probe the details of AGN structures such as the X-ray-emitting corona and the toroidal obscurer in the under-explored spectral window above 10 keV. I will present both phenomenological results important for synthesis models of the cosmic X-ray background, and a novel approach for constraining the geometry of the gas surrounding the supermassive black hole (including the accretion disk, the broad-line region, and the torus) from the hard X-ray band. Finally, I will discuss how what we learned from this survey of local AGN relates to deeper high-redshift X-ray surveys and AGN structure probes at other wavelengths.

  12. Quantitative investigation of two metallohydrolases by X-ray absorption spectroscopy near-edge spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, W. [Hefei National Laboratory for Physical Sciences at Microscale and School of Life Sciences, University of Science and Technology of China, Hefei, Anhui 230027 (China); Chu, W.S.; Yang, F.F.; Yu, M.J.; Chen, D.L.; Guo, X.Y. [Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China); Zhou, D.W.; Shi, N. [Hefei National Laboratory for Physical Sciences at Microscale and School of Life Sciences, University of Science and Technology of China, Hefei, Anhui 230027 (China); Marcelli, A. [Istituto Nazionale di Fisica Nucleare, Laboratori Nazionali di Frascati, P.O. Box 13, Frascati 00044 (Italy); Niu, L.W.; Teng, M.K. [Hefei National Laboratory for Physical Sciences at Microscale and School of Life Sciences, University of Science and Technology of China, Hefei, Anhui 230027 (China); Gong, W.M. [Institute of Biophysics, Chinese Academy of Sciences, Beijing 100101 (China); Benfatto, M. [Istituto Nazionale di Fisica Nucleare, Laboratori Nazionali di Frascati, P.O. Box 13, Frascati 00044 (Italy); Wu, Z.Y. [Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China); Istituto Nazionale di Fisica Nucleare, Laboratori Nazionali di Frascati, P.O. Box 13, Frascati 00044 (Italy)], E-mail: wuzy@ihep.ac.cn

    2007-09-21

    The last several years have witnessed a tremendous increase in biological applications using X-ray absorption spectroscopy (BioXAS), thanks to continuous advancements in synchrotron radiation (SR) sources and detector technology. However, XAS applications in many biological systems have been limited by the intrinsic limitations of the Extended X-ray Absorption Fine Structure (EXAFS) technique e.g., the lack of sensitivity to bond angles. As a consequence, the application of the X-ray absorption near-edge structure (XANES) spectroscopy changed this scenario that is now continuously changing with the introduction of the first quantitative XANES packages such as Minut XANES (MXAN). Here we present and discuss the XANES code MXAN, a novel XANES-fitting package that allows a quantitative analysis of experimental data applied to Zn K-edge spectra of two metalloproteins: Leptospira interrogans Peptide deformylase (LiPDF) and acutolysin-C, a representative of snake venom metalloproteinases (SVMPs) from Agkistrodon acutus venom. The analysis on these two metallohydrolases reveals that proteolytic activities are correlated to subtle conformation changes around the zinc ion. In particular, this quantitative study clarifies the occurrence of the LiPDF catalytic mechanism via a two-water-molecules model, whereas in the acutolysin-C we have observed a different proteolytic activity correlated to structural changes around the zinc ion induced by pH variations.

  13. Time resolved X-ray absorption spectroscopy in condensed matter: A road map to the future

    Energy Technology Data Exchange (ETDEWEB)

    Dell’Angela, Martina [Elettra-Sincrotrone Trieste S.C.p.A., Trieste (Italy); Parmigiani, Fulvio [Elettra-Sincrotrone Trieste S.C.p.A., Trieste (Italy); Department of Physics, University of Trieste, Trieste (Italy); Institute of Physics II, University of Cologne, Cologne (Germany); Malvestuto, Marco, E-mail: marco.malvestuto@elettra.eu [Elettra-Sincrotrone Trieste S.C.p.A., Trieste (Italy)

    2015-04-15

    Highlights: • We provide perspectives in the field Time resolved XAS in condensed matter. • A look at the new technological innovations that are shaping the field of pulsed X-ray sources are introduced. • New experimental schemes for tr-XAS are illustrated. - Abstract: Nowadays cutting edge femtosecond EUV and soft X-rays radiation sources are the driving force of groundbreaking time resolved X-ray spectroscopies. These new light sources are allowing pioneering experiments in the field of ultrafast phenomena and disclosing new insights about the physics of the out-of-equilibrium matter. Here we report an introductory and concise outlook about some possible perspectives in this field.

  14. Soft X-ray spectroscopy of oxide-embedded and functionalized silicon nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Kelly, Joel A.; Henderson, Eric J. [Department of Chemistry, University of Alberta, Edmonton, Alberta, T6G 2G2 (Canada); Hessel, Colin M. [Department of Chemical Engineering, University of Texas at Austin, Austin, TX 78712 (United States); Cavell, Ronald G. [Department of Chemistry, University of Alberta, Edmonton, Alberta, T6G 2G2 (Canada); Veinot, Jonathan G.C., E-mail: jveinot@ualberta.c [Department of Chemistry, University of Alberta, Edmonton, Alberta, T6G 2G2 (Canada)

    2010-02-15

    An X-ray absorption spectroscopic investigation into the electronic and optical properties of silicon nanocrystals (Si-NCs) derived from the thermal processing of hydrogen silsesquioxane (HSQ) is presented. Hydrofluoric (HF) acid etching and subsequent photochemical hydrosilylation with styrene liberates the as-synthesized oxide-embedded Si-NCs from their matrix and renders them solution dispersible through the formation of surface Si-C bonds. The impact of this process on the photoluminescence behavior exhibited by these materials has been studied through near edge X-ray absorption fine structure (NEXAFS) and X-ray excited optical luminescence (XEOL) spectroscopies.

  15. First results from the high-brightness x-ray spectroscopy beamline at ALS

    Energy Technology Data Exchange (ETDEWEB)

    Perera, R.C.C.; Ng, W.; Jones, G. [Lawrence Berkeley National Lab., CA (United States)] [and others

    1997-04-01

    Beamline 9.3.1 at the Advanced Light Source (ALS) is a windowless beamline, covering the 1-6 keV photon-energy range, designed to achieve the goal of high brightness at the sample for use in the X-ray Atomic and Molecular Spectroscopy (XAMS) science, surface and interface science, biology and x-ray optical development programs at ALS. X-ray absorption and time of flight photo emission measurements in 2 - 5 keV photon energy in argon along with the flux, resolution, spot size and stability of the beamline will be discussed. Prospects for future XAMS measurements will also be presented.

  16. Advanced experimental applications for x-ray transmission gratings spectroscopy using a novel grating fabrication method

    Energy Technology Data Exchange (ETDEWEB)

    Hurvitz, G.; Ehrlich, Y.; Shpilman, Z.; Levy, I.; Fraenkel, M. [Plasma Physics Department, Applied Physics Division, Soreq NRC, Yavne (Israel); Strum, G. [Solid State Department, Applied Physics Division, Soreq NRC, Yavne (Israel)

    2012-08-15

    A novel fabrication method for soft x-ray transmission grating and other optical elements is presented. The method uses focused-ion-beam technology to fabricate high-quality free standing grating bars on transmission electron microscopy grids. High quality transmission gratings are obtained with superb accuracy and versatility. Using these gratings and back-illuminated CCD camera, absolutely calibrated x-ray spectra can be acquired for soft x-ray source diagnostics in the 100-3000 eV spectral range. Double grating combinations of identical or different parameters are easily fabricated, allowing advanced one-shot application of transmission grating spectroscopy. These applications include spectroscopy with different spectral resolutions, bandwidths, dynamic ranges, and may serve for identification of high-order contribution, and spectral calibrations of various x-ray optical elements.

  17. A time-correlation function approach to nuclear dynamical effects in X-ray spectroscopy

    CERN Document Server

    Karsten, Sven; Aziz, Saadullah G; Ivanov, Sergei D; Kühn, Oliver

    2016-01-01

    Modern X-ray spectroscopy has proven itself as a robust tool for probing the electronic structure of atoms in complex environments. Despite working on energy scales that are much larger than those corresponding to nuclear motions, taking nuclear dynamics and the associated nuclear correlations into account may be of importance for X-ray spectroscopy. Recently, we have developed an efficient protocol to account for nuclear dynamics in X-ray absorption and resonant inelastic X-ray scattering spectra [Karsten \\textit{et al.} arXiv:1608.03436], based on ground state molecular dynamics accompanied with state-of-the-art calculations of electronic excitation energies and transition dipoles. Here, we present an alternative derivation of the formalism and elaborate on the developed simulation protocol on the examples of gas phase and bulk water. The specific spectroscopic features stemming from the nuclear motions are analyzed and traced down to the dynamics of electronic energy gaps and transition dipole correlation ...

  18. X-ray spectroscopy of energy materials under in situ/operando conditions

    Energy Technology Data Exchange (ETDEWEB)

    Crumlin, Ethan J., E-mail: ejcrumlin@lbl.gov [Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Liu, Zhi [State Key Laboratory of Functional Materials for Informatics, Shanghai Institute of Microsystem and Information Technology, Chinese Academy of Sciences, Shanghai 200050 (China); School of Physical Science and Technology, ShanghaiTech University, Shanghai 200031 (China); Bluhm, Hendrik [Chemical Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Yang, Wanli; Guo, Jinghua [Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Hussain, Zahid, E-mail: zhussain@lbl.gov [Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States)

    2015-04-15

    A perspective and brief review of in situ/operando X-ray spectroscopic techniques with focus on energy materials is presented, including discussion on current status, choice of cells and suitable X-ray energy range. Initial discussion focuses on the scientific advancement achieved using ambient pressure X-ray photoelectron spectroscopy (APXPS) at the solid/gas interface, and then progresses through the techniques evolution to probe the liquid/vapor and the emerging solid/liquid interface. This is followed by an overview of soft X-ray adsorption spectroscopy (sXAS) for energy science using both window and windowless cell configurations. Concluding remarks provide a future outlook for where the authors believe these techniques and class of science will progress toward.

  19. X-ray spectroscopy of the pionic deuterium atom

    Energy Technology Data Exchange (ETDEWEB)

    Chatellard, D.; Egger, J.-P.; Jeannet, E. [Neuchatel Univ. (Switzerland). Inst. de Physique; Badertscher, A.; Bogdan, M.; Goudsmit, P.F.A.; Janousch, M.; Leisi, H.J.; Matsinos, E.; Schroeder, H.-C.; Sigg, D.; Zhao, Z.G. [Institut fuer Teilchenphysik der ETHZ, CH-5232 Villigen PSI (Switzerland); Aschenauer, E.C.; Gabathuler, K.; Hauser, P.; Simons, L.M. [Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); Rusi El Hassani, A.J. [Ecole Mohammadia des Ingenieurs, Rabat (Morocco)

    1997-11-10

    The low energy X-rays of the pionic deuterium 3P-1S transition were measured using a high resolution crystal spectrometer, together with a cyclotron trap (a magnetic device to increase the pion stopping density) and a CCD (charge-coupled device) detector system. The spectrometer resolution was 0.65 eV FWHM for a measured energy of approximately 3075 eV. This energy was measured with a precision of 0.1 eV. Compared to conventional methods, the cyclotron trap allowed for a gain in stopping density of about an order of magnitude. The CCDs had excellent spatial and energy resolutions. Non-X-ray background could therefore be almost completely eliminated. The 1S strong interaction shift {epsilon}{sub 1S} and total decay width {Gamma}{sub 1S} were determined from the position and line shape of the X-ray peak. They are {epsilon}{sub 1S}(shift)=2.43{+-}0.10 eV (repulsive), {Gamma}{sub 1S}(width)=1.02{+-}0.21 eV, where the statistical and systematic errors were added linearly. The total (complex) pionic deuterium S-wave scattering length a{sub {pi}{sup -}d} was deduced: a{sub {pi}{sup -}d}=-0.0259({+-}0.0011)+i0. 0054({+-}0.0011)m{sub {pi}}{sup -1}. From the real part of a{sub {pi}{sup -}d} a constraint in terms of the isoscalar and isovector {pi}N scattering lengths b{sub 0} and b{sub 1} was deduced. From Im a{sub {pi}{sup -}d} we determined the isoscalar coupling constant for {pi}{sup -} absorption: vertical stroke g{sub 0} vertical stroke =(2.6{+-}0.3)10{sup -2}m{sub {pi}}{sup -2}. The experiments of the pionic hydrogen and deuterium S-wave scattering lengths were analyzed within the framework of a search for isospin symmetry violation. The data are still compatible with isospin conservation. The scattering lengths deduced from the Karlsruhe-Helsinki phase shift analysis disagree with the present results. (orig.). 45 refs.

  20. Laboratory micro-X-ray fluorescence spectroscopy instrumentation and applications

    CERN Document Server

    Haschke, Michael

    2014-01-01

    Micro-X-ray fluorescence offers the possibility for a position- sensitive and non-destructive analysis that can be used for the analysis of non-homogeneous materials and layer systems. This analytical technique has shown a dynamic development in the last 15 years and is used for the analysis of small particles, inclusions, of elemental distributions for a wide range of different applications both in research and quality control. The first experiments were performed on synchrotrons but there is a requirement for laboratory instruments which offers a fast and immediate access for analytical results. The book discuss the main components of a µ-XRF instrument and the different measurement modes, it gives an overview about the various instruments types, considers the special requirements for quantification of non-homogeneous materials and presents a wide range of application for single point and multi-point analysis as well as for distribution analysis in one, two and three dimensions.

  1. Environment-Dependent Radiation Damage in Atmospheric Pressure X-ray Spectroscopy.

    Science.gov (United States)

    Weatherup, Robert S; Wu, Cheng Hao; Escudero, Carlos; Pérez-Dieste, Virginia; Salmeron, Miquel B

    2017-09-18

    Atmospheric pressure X-ray spectroscopy techniques based on soft X-ray excitation can provide powerful interface-sensitive chemical information about a solid surface immersed in a gas or liquid environment. However, X-ray illumination of such dense phases can lead to the generation of considerable quantities of radical species by radiolysis. Soft X-ray absorption measurements of Cu films in both air and aqueous alkali halide solutions reveal that this can cause significant evolution of the Cu oxidation state. In air and NaOH (0.1 M) solutions, the Cu is oxidized toward CuO, while the addition of small amounts of CH3OH to the solution leads to reduction toward Cu2O. For Ni films in NaHCO3 solutions, the oxidation state of the surface is found to remain stable under X-ray illumination and can be electrochemically cycled between a reduced and oxidized state. We provide a consistent explanation for this behavior based on the products of X-ray-induced radiolysis in these different environments and highlight a number of general approaches that can mitigate radiolysis effects when performing operando X-ray measurements.

  2. Scanning electron microscopy and X-ray spectroscopy applied to mycelial phase of sporothrix schenckii

    Directory of Open Access Journals (Sweden)

    M. Thibaut

    1975-04-01

    Full Text Available Scanning electron microscopy applied to the mycelial phase of Sporothrix schenckii shows a matted mycelium with conidia of a regular pattern. X-Ray microanalysis applied in energy dispersive spectroscopy and also in wavelength dispersive spectroscopy reveals the presence of several elements of Mendeleef's classification.

  3. Probing spin-vibronic dynamics using femtosecond X-ray spectroscopy

    DEFF Research Database (Denmark)

    Penfold, T. J.; Pápai, Mátyás Imre; Rozgonyi, T.

    2016-01-01

    we use wavepacket dynamics of the photoexcited decay of a new Fe(ii) complex, [Fe(bmip)2]2+ (bmip = 2,6-bis(3-methyl-imidazole-1-ylidine)pyridine), to simulate the experimental observables associated with femtosecond Fe K-edge X-ray Absorption Near-Edge Structure (XANES) and X-ray emission (XES......Ultrafast pump-probe spectroscopy within the X-ray regime is now possible owing to the development of X-ray Free Electrons Lasers (X-FELs) and is opening new opportunities for the direct probing of femtosecond evolution of the nuclei, the electronic and spin degrees of freedom. In this contribution...

  4. Ultrafast conversions between hydrogen bonded structures in liquid water observed by femtosecond x-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Wen, Haidan; Huse, Nils; Schoenlein, Robert W.; Lindenberg, Aaron M.

    2010-05-01

    We present the first femtosecond soft x-ray spectroscopy in liquids, enabling the observation of changes in hydrogen bond structures in water via core-hole excitation. The oxygen K-edge of vibrationally excited water is probed with femtosecond soft x-ray pulses, exploiting the relation between different water structures and distinct x-ray spectral features. After excitation of the intramolecular OH stretching vibration, characteristic x-ray absorption changes monitor the conversion of strongly hydrogen-bonded water structures to more disordered structures with weaker hydrogen-bonding described by a single subpicosecond time constant. The latter describes the thermalization time of vibrational excitations and defines the characteristic maximum rate with which nonequilibrium populations of more strongly hydrogen-bonded water structures convert to less-bonded ones. On short time scales, the relaxation of vibrational excitations leads to a transient high-pressure state and a transient absorption spectrum different from that of statically heated water.

  5. Structural changes in a-Si:H studied by x-ray photoemission spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Sheng, S.; Sacher, E.; Yelon, A.; Branz, H.M.; Masson, D.P.

    1999-07-01

    X-ray irradiation-induced structural changes in undoped a-Si:H have been investigated in detail by X-ray photoemission spectroscopy (XPS). The Si2s and the Si2p peaks were found to shift simultaneously to lower bonding energies, by the same amount, with X-ray irradiation. The shifts are near saturation, at about 0.1 eV, after one hour of irradiation at the intensity used; they can be reversed almost completely, seemingly with an activation energy lower than that for the metastable changes in electronic properties (Staebler-Wronski effect). The present results suggest that essentially the whole Si network structure is affected by the X-ray irradiation.

  6. X-ray excited optical luminescence, photoluminescence, photostimulated luminescence and x-ray photoemission spectroscopy studies on BaFBr:Eu

    CERN Document Server

    Subramanian, N; Govinda-Rajan, K; Mohammad-Yousuf; Santanu-Bera; Narasimhan, S V

    1997-01-01

    The results of x-ray excited optical luminescence (XEOL), photoluminescence (PL), photostimulated luminescence (PSL) and x-ray photoemission spectroscopy (XPS) studies on the x-ray storage phosphor BaFBr:Eu are presented in this paper. Analyses of XEOL, PL and PSL spectra reveal features corresponding to the transitions from 4f sup 6 td sup 1 to 4f sup 7 configurations in different site symmetries of Eu sup 2 sup +. Increasing x-ray dose is seen to lead to a red shift in the maximum of the PL excitation spectrum for the 391 nm emission. The XEOL and XPS spectra do not show any signature of Eu sup 3 sup + in the samples studied by us, directly raising doubts about the model of Takahashi et al in which Eu sup 2 sup + is expected to ionize to Eu sup 3 sup + upon x-ray irradiation and remain stable until photostimulation. XEOL and PSL experiments with simultaneous x-ray irradiation and He - Ne laser excitation as well as those with sequential x-ray irradiation and laser stimulation bring out the competition betwe...

  7. Optical and x-ray photoelectron spectroscopy studies of α-Al2O3

    Science.gov (United States)

    Prakash, Ram; Kumar, Sandeep; Kumar, Vinay; Choudhary, R. J.; Phase, D. M.

    2016-05-01

    α-Al2O3 powder sample was synthesized at 550 °C via solution combustion synthesis (SCS) method using urea as an organic fuel. The sample was characterized by X-ray diffraction (XRD), Optical spectroscopy and X-ray photoelectron spectroscopy (XPS) without any further thermal treatment. XRD study reveals that the powder crystallized directly in the hexagons α-Al2O3 phase. A band gap of 5.7 eV was estimated using diffuse reflectance spectra. For surface investigation X-ray photo electron spectroscopy (XPS) was carried out. The XPS survey scan study of α-Al2O3 powder reveals that the sample is free from impurity. The core levels of Al-2s and O-1s are also reported.

  8. The X-ray Correlation Spectroscopy instrument at the Linac Coherent Light Source

    Energy Technology Data Exchange (ETDEWEB)

    Alonso-Mori, Roberto; Caronna, Chiara; Chollet, Matthieu; Curtis, Robin; Damiani, Daniel S.; Defever, Jim; Feng, Yiping; Flath, Daniel L.; Glownia, James M. [Linac Coherent Light Source, SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, CA 94025 (United States); Lee, Sooheyong [Linac Coherent Light Source, SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, CA 94025 (United States); Hasylab at DESY, Notkestrasse 85, D-22607 Hamburg (Germany); Lemke, Henrik T.; Nelson, Silke; Bong, Eric; Sikorski, Marcin; Song, Sanghoon; Srinivasan, Venkat; Stefanescu, Daniel; Zhu, Diling; Robert, Aymeric, E-mail: aymeric@slac.stanford.edu [Linac Coherent Light Source, SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, CA 94025 (United States)

    2015-04-14

    A description of the X-ray Correlation Spectroscopy instrument at the Linac Coherent Light Source is presented. Recent highlights illustrate the coherence properties of the source as well as some recent dynamics measurements and future directions. The X-ray Correlation Spectroscopy instrument is dedicated to the study of dynamics in condensed matter systems using the unique coherence properties of free-electron lasers. It covers a photon energy range of 4–25 keV. The intrinsic temporal characteristics of the Linac Coherent Light Source, in particular the 120 Hz repetition rate, allow for the investigation of slow dynamics (milliseconds) by means of X-ray photon correlation spectroscopy. Double-pulse schemes could probe dynamics on the picosecond timescale. A description of the instrument capabilities and recent achievements is presented.

  9. Mode-Locked Multichromatic X-Rays in a Seeded Free-Electron Laser for Single-Shot X-Ray Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Xiang, Dao; Ding, Yuantao; Raubenheimer, Tor; Wu, Juhao; /SLAC

    2012-05-10

    We present the promise of generating gigawatt mode-locked multichromatic x rays in a seeded free-electron laser (FEL). We show that, by using a laser to imprint periodic modulation in electron beam phase space, a single-frequency coherent seed can be amplified and further translated to a mode-locked multichromatic output in an FEL. With this configuration the FEL output consists of a train of mode-locked ultrashort pulses which span a wide frequency gap with a series of equally spaced sharp lines. These gigawatt multichromatic x rays may potentially allow one to explore the structure and dynamics of a large number of atomic states simultaneously. The feasibility of generating mode-locked x rays ranging from carbon K edge ({approx}284 eV) to copper L{sub 3} edge ({approx}931 eV) is confirmed with numerical simulation using the realistic parameters of the linac coherent light source (LCLS) and LCLS-II. We anticipate that the mode-locked multichromatic x rays in FELs may open up new opportunities in x-ray spectroscopy (i.e. resonant inelastic x-ray scattering, time-resolved scattering and spectroscopy, etc.).

  10. The X-ray Correlation Spectroscopy instrument at the Linac Coherent Light Source.

    Science.gov (United States)

    Alonso-Mori, Roberto; Caronna, Chiara; Chollet, Matthieu; Curtis, Robin; Damiani, Daniel S; Defever, Jim; Feng, Yiping; Flath, Daniel L; Glownia, James M; Lee, Sooheyong; Lemke, Henrik T; Nelson, Silke; Bong, Eric; Sikorski, Marcin; Song, Sanghoon; Srinivasan, Venkat; Stefanescu, Daniel; Zhu, Diling; Robert, Aymeric

    2015-05-01

    The X-ray Correlation Spectroscopy instrument is dedicated to the study of dynamics in condensed matter systems using the unique coherence properties of free-electron lasers. It covers a photon energy range of 4-25 keV. The intrinsic temporal characteristics of the Linac Coherent Light Source, in particular the 120 Hz repetition rate, allow for the investigation of slow dynamics (milliseconds) by means of X-ray photon correlation spectroscopy. Double-pulse schemes could probe dynamics on the picosecond timescale. A description of the instrument capabilities and recent achievements is presented.

  11. The X-ray Correlation Spectroscopy instrument at the Linac Coherent Light Source

    Science.gov (United States)

    Alonso-Mori, Roberto; Caronna, Chiara; Chollet, Matthieu; Curtis, Robin; Damiani, Daniel S.; Defever, Jim; Feng, Yiping; Flath, Daniel L.; Glownia, James M.; Lee, Sooheyong; Lemke, Henrik T.; Nelson, Silke; Bong, Eric; Sikorski, Marcin; Song, Sanghoon; Srinivasan, Venkat; Stefanescu, Daniel; Zhu, Diling; Robert, Aymeric

    2015-01-01

    The X-ray Correlation Spectroscopy instrument is dedicated to the study of dynamics in condensed matter systems using the unique coherence properties of free-electron lasers. It covers a photon energy range of 4–25 keV. The intrinsic temporal characteristics of the Linac Coherent Light Source, in particular the 120 Hz repetition rate, allow for the investigation of slow dynamics (milli­seconds) by means of X-ray photon correlation spectroscopy. Double-pulse schemes could probe dynamics on the picosecond timescale. A description of the instrument capabilities and recent achievements is presented. PMID:25931061

  12. A broadband x-ray imaging spectroscopy with high-angular resolution: the FORCE mission

    Science.gov (United States)

    Mori, Koji; Tsuru, Takeshi Go; Nakazawa, Kazuhiro; Ueda, Yoshihiro; Okajima, Takashi; Murakami, Hiroshi; Awaki, Hisamitsu; Matsumoto, Hironori; Fukazawa, Yasushi; Tsunemi, Hiroshi; Takahashi, Tadayuki; Zhang, William W.

    2016-07-01

    We are proposing FORCE (Focusing On Relativistic universe and Cosmic Evolution) as a future Japan-lead Xray observatory to be launched in the mid 2020s. Hitomi (ASTRO-H) possesses a suite of sensitive instruments enabling the highest energy-resolution spectroscopy in soft X-ray band, a broadband X-ray imaging spectroscopy in soft and hard X-ray bands, and further high energy coverage up to soft gamma-ray band. FORCE is the direct successor to the broadband X-ray imaging spectroscopy aspect of Hitomi (ASTRO-H) with significantly higher angular resolution. The current design of FORCE defines energy band pass of 1-80 keV with angular resolution of black holes" in various mass-scales: "buried supermassive black holes (SMBHs)" (> 104 M⊙) residing in the center of galaxies in a cosmological distance, "intermediate-mass black holes" (102-104 M⊙) acting as the possible seeds from which SMBHs grow, and "orphan stellar-mass black holes" (< 102 M⊙) without companion in our Galaxy. In addition to these missing BHs, hunting for the nature of relativistic particles at various astrophysical shocks is also in our scope, utilizing the broadband X-ray coverage with high angular-resolution. FORCE are going to open a new era in these fields. The satellite is proposed to be launched with the Epsilon vehicle that is a Japanese current solid-fuel rocket. FORCE carries three identical pairs of Super-mirror and wide-band X-ray detector. The focal length is currently planned to be 10 m. The silicon mirror with multi-layer coating is our primary choice to achieve lightweight, good angular optics. The detector is a descendant of hard X-ray imager onboard Hitomi (ASTRO-H) replacing its silicon strip detector with SOI-CMOS silicon pixel detector, allowing an extension of the low energy threshold down to 1 keV or even less.

  13. Ultrafast Time-Resolved Hard X-Ray Emission Spectroscopy on a Tabletop

    Directory of Open Access Journals (Sweden)

    Luis Miaja-Avila

    2016-09-01

    Full Text Available Experimental tools capable of monitoring both atomic and electronic structure on ultrafast (femtosecond to picosecond time scales are needed for investigating photophysical processes fundamental to light harvesting, photocatalysis, energy and data storage, and optical display technologies. Time-resolved hard x-ray (>3  keV spectroscopies have proven valuable for these measurements due to their elemental specificity and sensitivity to geometric and electronic structures. Here, we present the first tabletop apparatus capable of performing time-resolved x-ray emission spectroscopy. The time resolution of the apparatus is better than 6 ps. By combining a compact laser-driven plasma source with a highly efficient array of microcalorimeter x-ray detectors, we are able to observe photoinduced spin changes in an archetypal polypyridyl iron complex [Fe(2,2^{′}-bipyridine_{3}]^{2+} and accurately measure the lifetime of the quintet spin state. Our results demonstrate that ultrafast hard x-ray emission spectroscopy is no longer confined to large facilities and now can be performed in conventional laboratories with 10 times better time resolution than at synchrotrons. Our results are enabled, in part, by a 100- to 1000-fold increase in x-ray collection efficiency compared to current techniques.

  14. CdZnTe detector in mammographic x-ray spectroscopy.

    Science.gov (United States)

    Miyajima, Satoshi; Imagawa, Kotaro

    2002-11-21

    A CdZnTe (CZT) detector was utilized in mammographic x-ray spectroscopy under clinical conditions. First, the detector response was investigated using y-rays from 241Am. The escape of secondary (Compton scattered and K fluorescent) x-rays and tailing due to carrier trapping were minor in the mammographic energy range. In addition, the transmission of primary x-rays was minimal from the results calculated using the mass attenuation coefficients of CZT. Therefore, spectral distortion in this energy range was expected to be negligible. Secondly, x-ray spectroscopy was carried out with the CZT detector. The measured spectra were in good agreement with the spectra obtained with the Compton-scatter method with a high-purity germanium detector. Moreover, the half-value layers (HVLs) calculated from the CZT spectra were consistent with the HVLs measured with an ionization chamber. The results indicate that a CZT detector can be utilized in mammographic x-ray spectroscopy without any corrections.

  15. AXSIS: Exploring the frontiers in attosecond X-ray science, imaging and spectroscopy

    Science.gov (United States)

    Kärtner, F. X.; Ahr, F.; Calendron, A.-L.; Çankaya, H.; Carbajo, S.; Chang, G.; Cirmi, G.; Dörner, K.; Dorda, U.; Fallahi, A.; Hartin, A.; Hemmer, M.; Hobbs, R.; Hua, Y.; Huang, W. R.; Letrun, R.; Matlis, N.; Mazalova, V.; Mücke, O. D.; Nanni, E.; Putnam, W.; Ravi, K.; Reichert, F.; Sarrou, I.; Wu, X.; Yahaghi, A.; Ye, H.; Zapata, L.; Zhang, D.; Zhou, C.; Miller, R. J. D.; Berggren, K. K.; Graafsma, H.; Meents, A.; Assmann, R. W.; Chapman, H. N.; Fromme, P.

    2016-09-01

    X-ray crystallography is one of the main methods to determine atomic-resolution 3D images of the whole spectrum of molecules ranging from small inorganic clusters to large protein complexes consisting of hundred-thousands of atoms that constitute the macromolecular machinery of life. Life is not static, and unravelling the structure and dynamics of the most important reactions in chemistry and biology is essential to uncover their mechanism. Many of these reactions, including photosynthesis which drives our biosphere, are light induced and occur on ultrafast timescales. These have been studied with high time resolution primarily by optical spectroscopy, enabled by ultrafast laser technology, but they reduce the vast complexity of the process to a few reaction coordinates. In the AXSIS project at CFEL in Hamburg, funded by the European Research Council, we develop the new method of attosecond serial X-ray crystallography and spectroscopy, to give a full description of ultrafast processes atomically resolved in real space and on the electronic energy landscape, from co-measurement of X-ray and optical spectra, and X-ray diffraction. This technique will revolutionize our understanding of structure and function at the atomic and molecular level and thereby unravel fundamental processes in chemistry and biology like energy conversion processes. For that purpose, we develop a compact, fully coherent, THz-driven attosecond X-ray source based on coherent inverse Compton scattering off a free-electron crystal, to outrun radiation damage effects due to the necessary high X-ray irradiance required to acquire diffraction signals. This highly synergistic project starts from a completely clean slate rather than conforming to the specifications of a large free-electron laser (FEL) user facility, to optimize the entire instrumentation towards fundamental measurements of the mechanism of light absorption and excitation energy transfer. A multidisciplinary team formed by laser

  16. High precision spectroscopy of pionic and antiprotonic atoms; Spectroscopie de precision des atomes pioniques et antiprotoniques

    Energy Technology Data Exchange (ETDEWEB)

    El-Khoury, P

    1998-04-15

    The study of exotic atoms, in which an orbiting electron of a normal atom is replaced by a negatively charged particle ({pi}{sup -}, {mu}{sup -}, p, {kappa}{sup -}, {sigma}{sup -},...) may provide information on the orbiting particle and the atomic nucleus, as well as on their interaction. In this work, we were interested in pionic atoms ({pi}{sup -14} N) on the one hand in order to determine the pion mass with high accuracy (4 ppm), and on the other hand in antiprotonic atoms (pp-bar) in order to study the strong nucleon-antinucleon interaction at threshold. In this respect, a high-resolution crystal spectrometer was coupled to a cyclotron trap which provides a high stop density for particles in gas targets at low pressure. Using curved crystals, an extended X-ray source could be imaged onto the detector. Charge-Coupled Devices were used as position sensitive detectors in order to measure the Bragg angle of the transition to a high precision. The use of gas targets resolved the ambiguity owing to the number of K electrons for the value of the pion mass, and, for the first time, strong interaction shift and broadening of the 2p level in antiprotonic hydrogen were measured directly. (author)

  17. Microscale X-ray Absorption Spectroscopy on the GSECARS Sector 13 at the APS

    CERN Document Server

    Stephen-Sutto

    2000-01-01

    GeoSoilEnviroCARS (GSECARS) is a national user facility for frontier research in the earth sciences using synchrotrons radiation at the Advanced Photon Source, Argonne National Laboratory. GSECARS provides earth scientists with access to the high-brilliance hard x-rays from this third-generation synchrotrons light source. The research conducted at this facility will advance our knowledge of the composition, structure and properties of earth materials, the processes they control and the processes that produce them. All principal synchrotron-based analytical techniques in demand by earth scientists are being brought to bear on earth science problems: (1) high-pressure/high-temperature crystallography and spectroscopy using the diamond anvil cell; (2) high-pressure/high-temperature crystallography using the large-volume press; (3) powder, single crystal and interface diffraction; (4) x-ray absorption fine structure (XAFS) spectroscopy; (5) x-ray fluorescence microprobe analysis and microspectroscopy; and (6) mic...

  18. X-ray spectroscopy of highly-charged heavy ions at FAIR

    Energy Technology Data Exchange (ETDEWEB)

    Gumberidze, A. [Laboratoire Kastler Brossel, Universite P. et M. Curie, Paris (France)], E-mail: a.gumberidze@gsi.de; Stoehlker, Th. [Gesellschaft fur Schwerionenforschung mbh, 64291 GSI-Darmstadt (Germany); Physikalisches Institut, Universitt Heidelberg, D-69120 Heidelberg (Germany); Beyer, H.F.; Bosch, F.; Braeuning-Demian, A.; Hagmann, S.; Kozhuharov, C.; Kuehl, Th.; Mann, R. [Gesellschaft fur Schwerionenforschung mbh, 64291 GSI-Darmstadt (Germany); Indelicato, P. [Laboratoire Kastler Brossel, Universite P. et M. Curie, Paris (France); Quint, W. [Gesellschaft fur Schwerionenforschung mbh, 64291 GSI-Darmstadt (Germany); Schuch, R. [Stockholm University, Stockholm (Sweden); Warczak, A. [Institute of Physics, Jagiellonian University, Cracow (Poland)

    2009-01-15

    In the current contribution, we give an overview of the envisioned X-ray spectroscopy program within the atomic physics research collaboration SPARC (Stored Particle Atomic Research Collaboration) at FAIR (Facility for Antiproton and Ion Research). These activities comprise, among others, the investigation of relativistic collision dynamics, electron correlation in the presence of strong fields, the test of Quantum Electrodynamics in extremely strong electromagnetic fields, and ideas to test the predictions of fundamental theories besides Quantum Electrodynamics. The state of the art X-ray spectroscopy will be of key importance for realization of these challenging goals. The world-wide unique experimental conditions and opportunities offered by the future FAIR facility will be combined with advanced X-ray detection devices, i.e. large-area, segmented solid-state detectors, high-resolution crystal spectrometers, calorimetric detectors etc.

  19. High-Resolution Structure of the Photosynthetic Mn4Ca Catalyst from X-ray Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Yachandra, Vittal; Yano, Junko; Kern, Jan; Pushkar, Yulia; Sauer, Kenneth; Glatzel, Pieter; Bergmann, Uwe; Messinger, Johannes; Zouni, Athina; Yachandra, Vittal K.

    2007-08-01

    The application of high-resolution X-ray spectroscopy methods to study the photosynthetic water oxidizing complex, which contains a unique hetero-nuclear catalytic Mn4Ca cluster, are described. Issues of X-ray damage especially at the metal sites in the Mn4Ca cluster are discussed. The structure of the Mn4Ca catalyst at high-resolution which has so far eluded attempts of determination by X-ray diffraction, EXAFS and other spectroscopic techniques has been addressed using polarized EXAFS techniques applied to oriented PS II membrane preparations and PS II single crystals. A review of how the resolution of traditional EXAFS techniques can be improved, using methods such as range-extended EXAFS is presented, and the changes that occur in the structure of the cluster as it advances through the catalytic cycle are described. X-ray absorption and emission techniques (XANES and K? emission) have been used earlier to determine the oxidation states of the Mn4Ca cluster, and in this report we review the use of X-ray resonant Raman spectroscopy to understand the electronic structure of the Mn4Ca cluster as it cycles through the intermediate S-states.

  20. XDS: a flexible beamline for X-ray diffraction and spectroscopy at the Brazilian synchrotron.

    Science.gov (United States)

    Lima, F A; Saleta, M E; Pagliuca, R J S; Eleotério, M A; Reis, R D; Fonseca Júnior, J; Meyer, B; Bittar, E M; Souza-Neto, N M; Granado, E

    2016-11-01

    The majority of the beamlines at the Brazilian Synchrotron Light Source Laboratory (LNLS) use radiation produced in the storage-ring bending magnets and are therefore currently limited in the flux that can be used in the harder part of the X-ray spectrum (above ∼10 keV). A 4 T superconducting multipolar wiggler (SCW) was recently installed at LNLS in order to improve the photon flux above 10 keV and fulfill the demands set by the materials science community. A new multi-purpose beamline was then installed at the LNLS using the SCW as a photon source. The XDS is a flexible beamline operating in the energy range between 5 and 30 keV, designed to perform experiments using absorption, diffraction and scattering techniques. Most of the work performed at the XDS beamline concentrates on X-ray absorption spectroscopy at energies above 18 keV and high-resolution diffraction experiments. More recently, new setups and photon-hungry experiments such as total X-ray scattering, X-ray diffraction under high pressures, resonant X-ray emission spectroscopy, among others, have started to become routine at XDS. Here, the XDS beamline characteristics, performance and a few new experimental possibilities are described.

  1. Hard X-ray photoelectron and X-ray absorption spectroscopy characterization of oxidized surfaces of iron sulfides

    Energy Technology Data Exchange (ETDEWEB)

    Mikhlin, Yuri, E-mail: yumikh@icct.ru [Institute of Chemistry and Chemical Technology of the Siberian Branch of the Russian Academy of sciences, Akademgorodok, 50/24, Krasnoyarsk, 660036 (Russian Federation); Tomashevich, Yevgeny [Institute of Chemistry and Chemical Technology of the Siberian Branch of the Russian Academy of sciences, Akademgorodok, 50/24, Krasnoyarsk, 660036 (Russian Federation); Vorobyev, Sergey [Institute of Chemistry and Chemical Technology of the Siberian Branch of the Russian Academy of sciences, Akademgorodok, 50/24, Krasnoyarsk, 660036 (Russian Federation); Siberian Federal University, Svobodny pr. 79, Krasnoyarsk, 660041 (Russian Federation); Saikova, Svetlana [Siberian Federal University, Svobodny pr. 79, Krasnoyarsk, 660041 (Russian Federation); Romanchenko, Alexander [Institute of Chemistry and Chemical Technology of the Siberian Branch of the Russian Academy of sciences, Akademgorodok, 50/24, Krasnoyarsk, 660036 (Russian Federation); Félix, Roberto [Renewable Energy, Helmholtz-Zentrum Berlin für Materialien und Energie GmbH, Lise-Meitner-Campus, Hahn-Meitner-Platz 1, 14109 Berlin (Germany)

    2016-11-30

    Highlights: • Pyrite and pyrrhotite in-air abraded and etched in aqueous Fe{sup 3+} solution were studied. • HAXPES (2 keV-6 keV) and Fe K-, S K-edge XANES (TEY and PFY mode) were measured. • Outer “polysulfide”, strongly S-excessive layers are no more than 1–4 nm thick. • “Metal-depleted” layers depend on the treatment and differ for pyrite and pyrrhotite. • Extended nearly-stoichiometric “defective” underlayers were detected using TEY XANES. - Abstract: Hard X-ray photoelectron spectroscopy (HAXPES) using an excitation energy range of 2 keV to 6 keV in combination with Fe K- and S K-edge XANES, measured simultaneously in total electron (TEY) and partial fluorescence yield (PFY) modes, have been applied to study near-surface regions of natural polycrystalline pyrite FeS{sub 2} and pyrrhotite Fe{sub 1−x}S before and after etching treatments in an acidic ferric chloride solution. It was found that the following near-surface regions are formed owing to the preferential release of iron from oxidized metal sulfide lattices: (i) a thin, no more than 1–4 nm in depth, outer layer containing polysulfide species, (ii) a layer exhibiting less pronounced stoichiometry deviations and low, if any, concentrations of polysulfide, the composition and dimensions of which vary for pyrite and pyrrhotite and depend on the chemical treatment, and (iii) an extended almost stoichiometric underlayer yielding modified TEY XANES spectra, probably, due to a higher content of defects. We suggest that the extended layered structure should heavily affect the near-surface electronic properties, and processes involving the surface and interfacial charge transfer.

  2. Low-energy gamma-ray spectroscopy using an X-ray-escape gated proportional counter

    DEFF Research Database (Denmark)

    Gregers Hansen, P.; Nielsen, H.L.; Williams, E.T.

    1965-01-01

    The utility of a gas-filled proportional counter in low-energy γ spectroscopy is greatly increased if it is operated in coincidence with an escaping fluorescent X-ray. An apparatus, having an efficiency greater than 10% of singles, is described and several examples are given. An efficiency curve...

  3. Quasiparticle lifetimes and tunneltimes in SIS junctions for X-ray spectroscopy

    NARCIS (Netherlands)

    Luiten, D.J.; Lieshout, H.L.; Michels, F.A.; Valko, P.; Bruijn, M.P.; Kiewiet, F.; Adelerhof, D.J.; Hamster, A.W.; Brons, G.C.S.; Flokstra, Jakob

    1996-01-01

    The quasiparticle lifetimes and tunneltimes in SIS tunnel junctions are essential parameters in the development of these devices for high resolution X-ray spectroscopy. We present a simple analytical model which allows us to calculate both the risetime and the total charge of the integrated tunnel

  4. 2p3d Resonant X-ray emission spectroscopy of cobalt compounds

    NARCIS (Netherlands)

    van Schooneveld, M.M.|info:eu-repo/dai/nl/315032863

    2013-01-01

    This manuscript demonstrates that 2p3d resonant X-ray emission spectroscopy (RXES) yields unique information on the chemically relevant valence electrons of transition metal atoms or ions. Experimental data on cobalt compounds and several theories were used hand-in-hand. In chapter 1 2p3d RXES was

  5. Optical and X-ray photoelectron spectroscopy of PbGeO 3 and Pb 5 ...

    Indian Academy of Sciences (India)

    Optical and X-ray photoelectron spectroscopy of PbGeO3 and Pb5Ge3O11 single crystals ... Optical Properties Volume 33 Issue 4 August 2010 pp 395-400 ... On gamma ray irradiation, the transmission of both the crystals is observed to deteriorate uniformly over the entire wavelength range, which has been attributed to the ...

  6. Enzymatic Synthesis of Amylose Brushes Revisited : Details from X-Ray Photoelectron Spectroscopy and Spectroscopic Ellipsometry

    NARCIS (Netherlands)

    Mazzocchetti, Laura; Tsoufis, Theodorus; Rudolf, Petra; Loos, Katja

    The successful synthesis of amylose brushes via enzymatic ‘‘grafting from’’ polymerization and the detailed characterization of all synthetic steps by X-ray photoelectron spectroscopy (XPS) and spectroscopic ellipsometry measurements are reported. Au and Si surfaces are amino-functionalized with

  7. Structural investigation of bistrifluron using x-ray crystallography, NMR spectroscopy, and molecular modeling

    CERN Document Server

    Moon, J K; Rhee, S K; Kim, G B; Yun, H S; Chung, B J; Lee, S S; Lim, Y H

    2002-01-01

    A new insecticide, bistrifluron acts as an inhibitor of insect development and interferes with the cuticle formation of insects. Since it shows low acute oral and dermal toxicities, it can be one of potent insecticides. Based on X-ray crystallography, NMR spectroscopy and molecular modeling, the structural studies of bistrifluron have been carried out.

  8. Use of x-ray fluorescence microprobe and x-ray photoelectron spectroscopy to study variations in bulk and surface chemistry of minerals

    Energy Technology Data Exchange (ETDEWEB)

    Perry, D.L.; Schlueter, E.M. [Lawrence Berkeley National Lab., CA (United States)

    1996-12-31

    Two experimental approaches, synchrotron x-ray fluorescence microprobe and x-ray photoelectron spectroscopy, can be used to study the chemistry of minerals. The former technique yields data at the micron level of depth, whereas the latter approach gives data at the Angstrom level and thus more indicative of the surface conditions of the sample. The present work makes use of the difference in depths being sampled by the two techniques and using them in conjunction with lateral microscopic profiling to study bulk and surface chemistry in oxide and sulfide minerals. A complementary method, angle resolved x-ray photoelectron spectroscopy, is also discussed with respect to both the bulk chemistry and multiple layer films that can occur as reactions products on the surfaces of minerals.

  9. Energy-dispersive X-ray emission spectroscopy using an X-ray free-electron laser in a shot-by-shot mode

    Science.gov (United States)

    Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; Sokaras, Dimosthenis; Weng, Tsu-Chien; Lassalle-Kaiser, Benedikt; Tran, Rosalie; Hattne, Johan; Laksmono, Hartawan; Hellmich, Julia; Glöckner, Carina; Echols, Nathaniel; Sierra, Raymond G.; Schafer, Donald W.; Sellberg, Jonas; Kenney, Christopher; Herbst, Ryan; Pines, Jack; Hart, Philip; Herrmann, Sven; Grosse-Kunstleve, Ralf W.; Latimer, Matthew J.; Fry, Alan R.; Messerschmidt, Marc M.; Miahnahri, Alan; Seibert, M. Marvin; Zwart, Petrus H.; White, William E.; Adams, Paul D.; Bogan, Michael J.; Boutet, Sébastien; Williams, Garth J.; Zouni, Athina; Messinger, Johannes; Glatzel, Pieter; Sauter, Nicholas K.; Yachandra, Vittal K.; Yano, Junko; Bergmann, Uwe

    2012-01-01

    The ultrabright femtosecond X-ray pulses provided by X-ray free-electron lasers open capabilities for studying the structure and dynamics of a wide variety of systems beyond what is possible with synchrotron sources. Recently, this “probe-before-destroy” approach has been demonstrated for atomic structure determination by serial X-ray diffraction of microcrystals. There has been the question whether a similar approach can be extended to probe the local electronic structure by X-ray spectroscopy. To address this, we have carried out femtosecond X-ray emission spectroscopy (XES) at the Linac Coherent Light Source using redox-active Mn complexes. XES probes the charge and spin states as well as the ligand environment, critical for understanding the functional role of redox-active metal sites. Kβ1,3 XES spectra of MnII and Mn2III,IV complexes at room temperature were collected using a wavelength dispersive spectrometer and femtosecond X-ray pulses with an individual dose of up to >100 MGy. The spectra were found in agreement with undamaged spectra collected at low dose using synchrotron radiation. Our results demonstrate that the intact electronic structure of redox active transition metal compounds in different oxidation states can be characterized with this shot-by-shot method. This opens the door for studying the chemical dynamics of metal catalytic sites by following reactions under functional conditions. The technique can be combined with X-ray diffraction to simultaneously obtain the geometric structure of the overall protein and the local chemistry of active metal sites and is expected to prove valuable for understanding the mechanism of important metalloproteins, such as photosystem II. PMID:23129631

  10. Coherent Multidimensional Core Spectroscopy of Molecules with Multiple X-ray pulses

    Science.gov (United States)

    Mukamel, Shaul

    2017-04-01

    Multidimensional spectroscopy uses sequences of optical pulses to study dynamical processes in complex molecules through correlation plots involving several time delay periods. Extensions of these techniques to the x-ray regime will be discussed. Ultrafast nonlinear x-ray spectroscopy is made possible by newly developed free electron laser and high harmonic generation sources. The attosecond duration of X-ray pulses and the atomic selectivity of core X-ray excitations offer a uniquely high spatial and temporal resolution. We demonstrate how stimulated Raman detection of an X-ray probe may be used to monitor the phase and dynamics of the nonequilibrium valence electronic state wavepacket created by e.g. photoexcitation, photoionization and Auger processes. Spectroscopy of multiplecore excitations provides a new window into electron correlations. Applications will be presented to long-range charge transfer in proteins and to excitation energy transfer in porphyrin arrays. Conical intersections (CoIn) dominate the pathways and outcomes of virtually all photophysical and photochemical molecular processes. Despite extensive experimental and theoretical effort CoIns have not been directly observed yet and the experimental evidence is being inferred from fast reaction rates and some vibrational signatures. Novel ultrafast X ray probes for these processes will be presented. Short X-ray pulses can directly detect the passage through a CoIn with the adequate temporal and spectral sensitivity. The technique is based on a coherent Raman process that employs a composite femtosecond/attosecond X-ray pulse to directly detect the electronic coherences (rather than populations) that are generated as the system passes through the CoIn. Streaking of time-resolved photoelectron spectroscopy (TRPES) signals offers another powerful window into the joint electronic/vibrational dynamics at concial intersections. Strong coupling of molecules to the vacuum field of micro cavities can modify

  11. STROBE-X: X-ray Timing & Spectroscopy on Dynamical Timescales from Microseconds to Years

    DEFF Research Database (Denmark)

    Wilson-Hodge, C.~A.; Ray, P. S.; Maccarone, T. J.

    We describe a probe-class mission concept that provides an unprecedentedview of the X-ray sky, performing timing and 0.2-30 keV spectroscopy overtimescales from microseconds to years. The Spectroscopic Time-Resolving Observatory for Broadband Energy X-rays (STROBE-X) comprises three primary......, with enhanced optics to take advantage of the longer focal length of STROBE-X. The second uses large-area collimated silicon drift detectors, developed for ESA's LOFT, to cover the 2-30 keV band. These two instruments each provide an order of magnitude improvement ineffective area compared with its predecessor...... (NICER and RXTE, respectively). Finally, a sensitive sky monitor triggers pointed observations, provides high duty cycle, high time resolution, high spectral resolution monitoring of the X-ray sky with ~20 times the sensitivity of the RXTE ASM,and enables multi-wavelength and multi-messenger studies...

  12. Pushing the Boundaries of X-ray Grating Spectroscopy in a Suborbital Rocket

    Science.gov (United States)

    McEntaffer, Randall L.; DeRoo, Casey; Schultz, Ted; Zhang, William W.; Murray, Neil J.; O'Dell, Stephen; Cash, Webster

    2013-01-01

    Developments in grating spectroscopy are paramount for meeting the soft X-ray science goals of future NASA X-ray Observatories. While developments in the laboratory setting have verified the technical feasibility of using off-plane reflection gratings to reach this goal, flight heritage is a key step in the development process toward large missions. To this end we have developed a design for a suborbital rocket payload employing an Off-Plane X-ray Grating Spectrometer. This spectrometer utilizes slumped glass Wolter-1 optics, an array of gratings, and a CCD camera. We discuss the unique capabilities of this design, the expected performance, the science return, and the perceived impact to future missions.

  13. High-pressure x-ray absorption spectroscopy study of tin tungstates

    Science.gov (United States)

    Kuzmin, A.; Anspoks, A.; Kalinko, A.; Timoshenko, J.; Kalendarev, R.; Nataf, L.; Baudelet, F.; Irifune, T.

    2015-09-01

    Room-temperature pressure-dependent (0-25 GPa) x-ray absorption spectroscopy at the W {L}{1,3}-edges of α-SnWO4 and β-SnWO4 was performed using a dispersive setup and a high-pressure nanodiamond anvil cell. The detailed analysis of experimental x-ray absorption near-edge structure and extended x-ray absorption fine structure data suggests that upon increasing pressure, a displacement of tungsten atoms by about 0.2 Å toward the center of the WO6 octahedra occurs in α-SnWO4, whereas the coordination of tungsten atoms changes from tetrahedral to distorted octahedral in β-SnWO4.

  14. X-RAY ABSORPTION SPECTROSCOPY OF YB3+-DOPED OPTICAL FIBERS

    Energy Technology Data Exchange (ETDEWEB)

    Citron, Robert; Kropf, A.J.

    2008-01-01

    Optical fibers doped with Ytterbium-3+ have become increasingly common in fiber lasers and amplifiers. Yb-doped fibers provide the capability to produce high power and short pulses at specific wavelengths, resulting in highly effective gain media. However, little is known about the local structure, distribution, and chemical coordination of Yb3+ in the fibers. This information is necessary to improve the manufacturing process and optical qualities of the fibers. Five fibers doped with Yb3+ were studied using Extended X-ray Absorption Fine Structure (EXAFS) spectroscopy and X-ray Absorption Near Edge Spectroscopy (XANES), in addition to Yb3+ mapping. The Yb3+ distribution in each fiber core was mapped with 2D and 1D intensity scans, which measured X-ray fluorescence over the scan areas. Two of the five fibers examined showed highly irregular Yb3+ distributions in the core center. In four of the five fibers Yb3+ was detected outside of the given fiber core dimensions, suggesting possible Yb3+ diffusion from the core, manufacturing error, or both. X-ray absorption spectroscopy (XAS) analysis has so far proven inconclusive, but did show that the fibers had differing EXAFS spectra. The Yb3+ distribution mapping proved highly useful, but additional modeling and examination of fiber preforms must be conducted to improve XAS analysis, which has been shown to have great potential for the study of similar optical fi bers.

  15. High-resolution X-ray absorption spectroscopy of iron carbonyl complexes

    OpenAIRE

    Atkins, A.J.; Bauer, M; Jacob, C.R.

    2015-01-01

    We apply high-energy-resolution fluorescence-detected (HERFD) X-ray absorption near-edge spectroscopy (XANES) to study iron carbonyl complexes. Mono-, bi-, and tri-nuclear carbonyl complexes and pure carbonyl complexes as well as carbonyl complexes containing hydrocarbon ligands are considered. The HERFD-XANES spectra reveal multiple pre-edge peaks with individual signatures for each complex, which could not be detected previously with conventional XANES spectroscopy. These peaks are assigned...

  16. Calorimetric Low-Temperature Detectors for X-Ray Spectroscopy on Trapped Highly-Charged Heavy Ions

    Science.gov (United States)

    Kilbourne, Caroline; Kraft-Bermuth, S.; Andrianov, V.; Bleile, A.; Echler, A.; Egelhof, P.; Ilieva, S.; Kilbourne, C.; McCammon, D.

    2012-01-01

    The application of Calorimetric Low-Temperature Detectors (CLTDs) has been proposed at the Heavy-Ion TRAP facility HITRAP which is currently being installed at the Helmholtz Research Center for Heavy Ion Research GSI. This cold ion trap setup will allow the investigation of X-rays from ions practically at rest, for which the excellent energy resolution of CLTDs can be used to its full advantage. However, the relatively low intensities at HITRAP demand larger solid angles and an optimized cryogenic setup. The influence of external magnetic fields has to be taken into account. CLTDs will also be a substantial part of the instrumental equipment at the future Facility for Antiproton and Heavy Ion Research (FAIR), for which a wide variety of high-precision X-ray spectroscopy experiments has been proposed. This contribution will give an overview on the chances and challenges for the application of CLTDs at HITRAP as well as perspectives for future experiments at the FAIR facility.

  17. The GALAXIES beamline at the SOLEIL synchrotron: inelastic X-ray scattering and photoelectron spectroscopy in the hard X-ray range.

    Science.gov (United States)

    Rueff, J P; Ablett, J M; Céolin, D; Prieur, D; Moreno, Th; Balédent, V; Lassalle-Kaiser, B; Rault, J E; Simon, M; Shukla, A

    2015-01-01

    The GALAXIES beamline at the SOLEIL synchrotron is dedicated to inelastic X-ray scattering (IXS) and photoelectron spectroscopy (HAXPES) in the 2.3-12 keV hard X-ray range. These two techniques offer powerful complementary methods of characterization of materials with bulk sensitivity, chemical and orbital selectivity, resonant enhancement and high resolving power. After a description of the beamline components and endstations, the beamline capabilities are demonstrated through a selection of recent works both in the solid and gas phases and using either IXS or HAXPES approaches. Prospects for studies on liquids are discussed.

  18. Characterization of metallic nanoparticles by high-resolution X-ray absorption and X-ray emission spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Kuehn, Timna-Josua

    2012-03-15

    In almost all areas of technology, metallic nanoparticles are of interest due to their special thermal, electronic, magnetic and optical properties. Their special properties are mainly due to their small size which implies the relevance of quantum effects as well as the significance of the surface: For 2 nm nanoparticles, the surface-to-volume ratio is already 1:1. However, the identification of surface-to-volume interactions - that are responsible for the new properties - is a difficult task due to the small size that inhibits a lot of 'standard' techniques to be applicable. Here X-ray absorption/emission spectroscopy (XAS/XES) is a favorable tool for the characterization of nanoparticles, independent on size, degree of crystallinity and shape/condition of the surface. Using XAS, a tempered nanosized Co{sub 3}Pt/C catalyst have been investigated. Its outstanding oxygen-reduction reaction (ORR) properties in a fuel cell could be related to a lowered Pt 5d-band center connected to a tightened Pt-Pt bonding distance, leading to a weakening of the oxygen adsorption strength so that the ORR may proceed faster. One drawback remains, however, as the properties found by (standard) XAS are summed up for different chemical environments of the chosen element. Thus, no distinction can be made between, e.g., the pure metal in a nanoparticles' interior and the ligated metal in the outer shells or surface. Here, high-resolution fluorescence-detected XAS (HRFD-XAS) provides additional opportunities as, due to its chemical sensitivity, it leads to site-selective XAS. For a system of 6 nm sized Co nanoparticles, build up of a metallic core surrounded by a protecting shell, that resulted from the 'smooth oxidation' process, this technique of site-selective XAS was proven to be applicable. For the first time, the interior and outer shell of a metallic nanoparticle could be characterized separately. In particular, the Co-hcp phase could be determined for the

  19. Near-edge x-ray absorption fine structure spectroscopy at atmospheric pressure with a table-top laser-induced soft x-ray source

    Energy Technology Data Exchange (ETDEWEB)

    Kühl, Frank-Christian, E-mail: Frank-christian.kuehl@mail.de; Müller, Matthias, E-mail: matthias.mueller@llg-ev.de; Schellhorn, Meike; Mann, Klaus [Laser-Laboratorium Göttingen e.V., Hans-Adolf-Krebs-Weg 1, D-37077 Göttingen (Germany); Wieneke, Stefan [Hochschule für angewandte Wissenschaft und Kunst, Von-Ossietzky-Str 99, D-37085 Göttingen (Germany); Eusterhues, Karin [Friedrich-Schiller-Universität Jena, Fürstengraben 1, D-07743 Jena (Germany)

    2016-07-15

    The authors present a table-top soft x-ray absorption spectrometer, accomplishing investigations of the near-edge x-ray absorption fine structure (NEXAFS) in a laboratory environment. The system is based on a low debris plasma ignited by a picosecond laser in a pulsed krypton gas jet, emitting soft x-ray radiation in the range from 1 to 5 nm. For absorption spectroscopy in and around the “water window” (2.3–4.4 nm), a compact helium purged sample compartment for experiments at atmospheric pressure has been constructed and tested. NEXAFS measurements on CaCl{sub 2} and KMnO{sub 4} samples were conducted at the calcium and manganese L-edges, as well as at the oxygen K-edge in air, atmospheric helium, and under vacuum, respectively. The results indicate the importance of atmospheric conditions for an investigation of sample hydration processes.

  20. Thin film subsurface environments; Advanced X-ray spectroscopies and a novel Bayesian inference modeling algorithm

    Science.gov (United States)

    Church, Jonathan R.

    New condensed matter metrologies are being used to probe ever smaller length scales. In support of the diverse field of materials research synchrotron based spectroscopies provide sub-micron spatial resolutions and a breadth of photon wavelengths for scientific studies. For electronic materials the thinnest layers in a complementary metal-oxide-semiconductor (CMOS) device have been reduced to just a few nanometers. This raises concerns for layer uniformity, complete surface coverage, and interfacial quality. Deposition processes like chemical vapor deposition (CVD) and atomic layer deposition (ALD) have been shown to deposit the needed high-quality films for the requisite thicknesses. However, new materials beget new chemistries and, unfortunately, unwanted side-reactions and by-products. CVD/ALD tools and chemical precursors provided by our collaborators at Air Liquide utilized these new chemistries and films were deposited for which novel spectroscopic characterization methods were used. The second portion of the thesis focuses on fading and decomposing paint pigments in iconic artworks. Efforts have been directed towards understanding the micro-environments causing degradation. Hard X-ray photoelectron spectroscopy (HAXPES) and variable kinetic energy X-ray photoelectron spectroscopy (VKE-XPS) are advanced XPS techniques capable of elucidating both chemical environments and electronic band structures in sub-surface regions of electronic materials. HAXPES has been used to study the electronic band structure in a typical CMOS structure; it will be shown that unexpected band alignments are associated with the presence of electronic charges near a buried interface. Additionally, a computational modeling algorithm, Bayes-Sim, was developed to reconstruct compositional depth profiles (CDP) using VKE-XPS data sets; a subset algorithm also reconstructs CDP from angle-resolved XPS data. Reconstructed CDP produced by Bayes-Sim were most strongly correlated to the real

  1. Ultrafast Structural Dynamics by X-Ray Diffraction and Structural Spectroscopy

    Science.gov (United States)

    Weber, Peter M.

    2015-05-01

    The ability to observe molecular reactions in real time is expected to aid the exploration of new reaction mechanisms, the development of catalysts, the understanding of biomolecular processes and the control of chemical reactions and material properties on a molecular level. To reach this goal, we have developed a gas-phase x-ray diffraction experiment that uses the ultrashort x-ray pulses from the Linac Coherent Light Source (LCLS) to capture atomic motions within molecules in a dilute gas (movie'' of the observed dynamics is constructed by comparing ab initio quantum molecular dynamics simulations with the experimental diffraction signal to derive weighted trajectories that provide a good representation of the structural dynamics, with the weighted ensemble of trajectories corresponding to the nuclear flux during the chemical reaction. The x-ray structural data thus provide reaction pathways for which ionization energies can be calculated at each step. We use ultrafast time-resolved multiphoton - ionization photoelectron spectroscopy to measure the travel time required for the molecule to reach certain resonance windows to Rydberg states. By so combining the results from the ultrafast x-ray diffraction with observations from ultrafast (structural) spectroscopy, it appears that we can make significant progress towards the ultimate goal: a comprehensive understanding of the spatially resolved photochemical reaction dynamics.

  2. High resolution x-ray fluorescence spectroscopy - a new technique for site- and spin-selectivity

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Xin [Univ. of California, Davis, CA (United States). Dept. of Applied Science

    1996-12-01

    X-ray spectroscopy has long been used to elucidate electronic and structural information of molecules. One of the weaknesses of x-ray absorption is its sensitivity to all of the atoms of a particular element in a sample. Through out this thesis, a new technique for enhancing the site- and spin-selectivity of the x-ray absorption has been developed. By high resolution fluorescence detection, the chemical sensitivity of K emission spectra can be used to identify oxidation and spin states; it can also be used to facilitate site-selective X-ray Absorption Near Edge Structure (XANES) and site-selective Extended X-ray Absorption Fine Structure (EXAFS). The spin polarization in K fluorescence could be used to generate spin selective XANES or spin-polarized EXAFS, which provides a new measure of the spin density, or the nature of magnetic neighboring atoms. Finally, dramatic line-sharpening effects by the combination of absorption and emission processes allow observation of structure that is normally unobservable. All these unique characters can enormously simplify a complex x-ray spectrum. Applications of this novel technique have generated information from various transition-metal model compounds to metalloproteins. The absorption and emission spectra by high resolution fluorescence detection are interdependent. The ligand field multiplet model has been used for the analysis of K{alpha} and K{beta} emission spectra. First demonstration on different chemical states of Fe compounds has shown the applicability of site selectivity and spin polarization. Different interatomic distances of the same element in different chemical forms have been detected using site-selective EXAFS.

  3. X-ray and photoelectron spectroscopy of the structure, reactivity, and electronic structure of semiconductor nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Hamad, Kimberly Sue [Univ. of California, Berkeley, CA (United States)

    2000-01-01

    Semiconductor nanocrystals are a system which has been the focus of interest due to their size dependent properties and their possible use in technological applications. Many chemical and physical properties vary systematically with the size of the nanocrystal and thus their study enables the investigation of scaling laws. Due to the increasing surface to volume ratio as size is decreased, the surfaces of nanocrystals are expected to have a large influence on their electronic, thermodynamic, and chemical behavior. In spite of their importance, nanocrystal surfaces are still relatively uncharacterized in terms of their structure, electronic properties, bonding, and reactivity. Investigation of nanocrystal surfaces is currently limited by what techniques to use, and which methods are suitable for nanocrystals is still being determined. This work presents experiments using x-ray and electronic spectroscopies to explore the structure, reactivity, and electronic properties of semiconductor (CdSe, InAs) nanocrystals and how they vary with size. Specifically, x-ray absorption near edge spectroscopy (XANES) in conjunction with multiple scattering simulations affords information about the structural disorder present at the surface of the nanocrystal. X-ray photoelectron spectroscopy (XPS) and ultra-violet photoelectron spectroscopy (UPS) probe the electronic structure in terms of hole screening, and also give information about band lineups when the nanocrystal is placed in electric contact with a substrate. XPS of the core levels of the nanocrystal as a function of photo-oxidation time yields kinetic data on the oxidation reaction occurring at the surface of the nanocrystal.

  4. Performing elemental microanalysis with high accuracy and high precision by scanning electron microscopy/silicon drift detector energy-dispersive X-ray spectrometry (SEM/SDD-EDS).

    Science.gov (United States)

    Newbury, Dale E; Ritchie, Nicholas W M

    Electron-excited X-ray microanalysis performed in the scanning electron microscope with energy-dispersive X-ray spectrometry (EDS) is a core technique for characterization of the microstructure of materials. The recent advances in EDS performance with the silicon drift detector (SDD) enable accuracy and precision equivalent to that of the high spectral resolution wavelength-dispersive spectrometer employed on the electron probe microanalyzer platform. SDD-EDS throughput, resolution, and stability provide practical operating conditions for measurement of high-count spectra that form the basis for peak fitting procedures that recover the characteristic peak intensities even for elemental combination where severe peak overlaps occur, such PbS, MoS2, BaTiO3, SrWO4, and WSi2. Accurate analyses are also demonstrated for interferences involving large concentration ratios: a major constituent on a minor constituent (Ba at 0.4299 mass fraction on Ti at 0.0180) and a major constituent on a trace constituent (Ba at 0.2194 on Ce at 0.00407; Si at 0.1145 on Ta at 0.0041). Accurate analyses of low atomic number elements, C, N, O, and F, are demonstrated. Measurement of trace constituents with limits of detection below 0.001 mass fraction (1000 ppm) is possible within a practical measurement time of 500 s.

  5. Toward Femtosecond X-ray Spectroscopy at the Advanced Light Source

    Energy Technology Data Exchange (ETDEWEB)

    Chong, Henry Herng Wei [Univ. of California, Berkeley, CA (United States)

    2004-01-01

    The realization of tunable, ultrashort pulse x-ray sources promises to open new venues of science and to shed new light on long-standing problems in condensed matter physics and chemistry. Fundamentally new information can now be accessed. Used in a pump-probe spectroscopy, ultrashort x-ray pulses provide a means to monitor atomic rearrangement and changes in electronic structure in condensed-matter and chemical systems on the physically-limiting time-scales of atomic motion. This opens the way for the study of fast structural dynamics and the role they play in phase transitions, chemical reactions and the emergence of exotic properties in materials with strongly interacting degrees of freedom. The ultrashort pulse x-ray source developed at the Advanced Light Source at the Lawrence Berkeley Laboratory is based on electron slicing in storage rings, and generates ~100 femtosecond pulses of synchrotron radiation spanning wavelengths from the far-infrared to the hard x-ray region of the electromagnetic spectrum. The tunability of the source allows for the adaptation of a broad range of static x-ray spectroscopies to useful pump-probe measurements. Initial experiments are attempted on transition metal complexes that exhibit relatively large structural changes upon photo-excitation and which have excited-state evolution determined by strongly interacting structural, electronic and magnetic degrees of freedom. Specifically, iron(II) complexes undergo a spin-crossover transition upon optical irradiation. The dynamics of the transition involve a metal-to-ligand charge transfer, a ΔS=2 change in magnetic moment and 10% bond dilation in the first coordination shell of the iron. Studies of the electronic dynamics are studied with time-resolved optical absorption measurements. The current progress of time-resolved structural studies to complete the picture of the spin-crossover transition is presented.

  6. Preliminary research on organics recognition by x-ray absorption spectroscopy detection and classification

    Science.gov (United States)

    Wang, Qian; Wu, Xiaomei; Zhang, Wei; He, Shuting; Feng, Haifeng; Fang, Zheng

    2016-01-01

    X-ray Absorption Spectroscopy (XAS) was been applied for the material recognition in this paper. Twelve kinds of plastics were selected as specimens. Each specimen was tested for 100 times by different operators for data processing. Seventy sets of spectral data of each specimen were randomly selected as training set and the other 30 sets were selected as testing set. Training set was calculated with Principal Component Analysis (PCA) to get the first four Principal Components, which totally explain 99% of the original spectrum. The first four Principal Components were built plastic classification model respectively through K-Nearest Neighbor (KNN) and Support Vector Machine (SVM) methods. The classification accuracy reached 89.22%-98.17%. Experimental results demonstrate that organics could be recognized by XAS. It shows that the X-ray absorption spectroscopy contains the potential of other organics recognition or even organisms.

  7. Retention Characteristics of CBTi144 Thin Films Explained by Means of X-Ray Photoemission Spectroscopy

    Directory of Open Access Journals (Sweden)

    G. Biasotto

    2010-01-01

    Full Text Available CaBi4Ti4O15 (CBTi144 thin films were grown on Pt/Ti/SiO2/Si substrates using a soft chemical solution and spin-coating method. Structure and morphology of the films were characterized by the X-ray Diffraction (XRD, Fourier-transform infrared spectroscopy (FT-IR, Raman analysis, X-ray photoemission spectroscopy (XPS, and transmission electron microscopy (TEM. The films present a single phase of layered-structured perovskite with polar axis orient. The a/b-axis orientation of the ferroelectric film is considered to be associated with the preferred orientation of the Pt bottom electrode. XPS measurements were employed to understand the nature of defects on the retention behavior of CBTi144 films. We have observed that the main source of retention-free characteristic of the capacitors is the oxygen environment in the CBTi144 lattice.

  8. X-ray spectroscopy of the photosynthetic oxygen-evolving complex

    Energy Technology Data Exchange (ETDEWEB)

    Sauer, Ken; Yano, Junko; Yachandra, Vittal K

    2007-04-05

    Water oxidation to dioxygen in photosynthesis is catalyzed by a Mn4Ca cluster with O bridging in Photosystem II (PS II) of plants, algae and cyanobacteria. A variety of spectroscopic methods have been applied to analyzing the participation of the complex. X-ray spectroscopy is particularly useful because it is element-specific, and because it can reveal important structural features of the complex with high accuracy and identify the participation of Mn in the redox chemistry. Following a brief history of the application of X-ray spectroscopy to PS II, an overview of newer results will be presented and a description of the present state of our knowledge based on this approach.

  9. Insights into the physics and chemistry of chalcogenides obtained from x-ray absorption spectroscopy

    Science.gov (United States)

    Kolobov, Alexander V.; Fons, Paul

    2017-12-01

    In this review, after a brief description of the underlying principles of x-ray absorption spectroscopy, we describe the results that enable one to obtain fundamental new insights into the rich physics and chemistry of chalcogenides. We start with chalcogenide glasses taking the readers from the structure of amorphous selenium and confined single Se chains and carry on to photo-induced structural changes. We subsequently describe application of EXAFS to monolayers of transition-metal dichalcogenides. The review is concluded by the results that were seminal to understand the phase-transition mechanism in so-called phase-change alloys that are widely used in optical and non-volatile memory devices. We place special accent on the conclusions that were only possible to draw based on the local nature of x-ray absorption spectroscopy.

  10. X-ray absorption spectroscopy on the basis of hybrid X-pinch radiation

    Energy Technology Data Exchange (ETDEWEB)

    Tilikin, I. N., E-mail: ivan.tilikin@gmail.com; Shelkovenko, T. A.; Pikuz, S. A., E-mail: pikuz@mail.ru [Russian Academy of Sciences, Lebedev Physical Institute (Russian Federation); Knapp, P. F.; Hammer, D. A. [Cornell University (United States)

    2015-07-15

    Results of experiments on X-ray absorption spectroscopy carried out at the BIN (270 kA, 100 ns) and XP (450 kA, 45 ns) facilities are presented. Continuum radiation of a Mo hybrid X-pinch was used as probing radiation, against which absorption lines of the plasma of exploded Al wires placed in the return current circuit of a hybrid X-pinch, as well as in a two- and four-wire array, were observed. The experiments have demonstrated that the radiation of a hybrid X-pinch hot spot can be used as probing radiation for X-ray absorption spectroscopy and that, in many parameters, such a source surpasses those on the basis of laser-produced plasma. The plasma parameters in arrays made of two and four Al wires were studied experimentally.

  11. Origin-independent calculation of quadrupole intensities in X-ray spectroscopy

    CERN Document Server

    Bernadotte, Stephan; Jacob, Christoph R

    2012-01-01

    For electronic excitations in the ultraviolet and visible range of the electromagnetic spectrum, the intensities are usually calculated within the dipole approximation, which assumes that the oscillating electric field is constant over the whole molecule. For the short wavelengths used in X-ray spectroscopy, this dipole approximation breaks down and it becomes necessary to include higher-order contributions. In quantum-chemical approaches to X-ray spectroscopy, these so-called quadrupole intensities have so far been calculated by including contributions depending on the square of the electric-quadrupole and magnetic-dipole transition moments. However, the resulting quadrupole intensities depend on the choice of the origin of the coordinate system. Here, we show that for obtaining an origin-independent theory, one has to include all contributions that are of the same order in the wave vector consistently. This leads to two additional contributions depending on products of the electric-dipole and electric-octup...

  12. An X-ray photoelectron spectroscopy study of uranyl-chitosan interaction

    Directory of Open Access Journals (Sweden)

    Veleshko Alexander N.

    2008-01-01

    Full Text Available An X-ray photoelectron spectroscopy study of uranium sorption by spherically-granulated chitosan in sulphate solutions, as well as the study of the nature of the U(VI - chitosan interaction was carried out in this work. The X-ray photoelectron spectroscopy analysis showed that the uranyl - chitosan interaction results in the formation of complexes with aminogroup nitrogen, and possibly chitin ring oxygens and free hydroxyl groups in the equatorial plane. Under the UHV in the spectrometer chamber, the uranyl-amin and uranyl-hyroxide bonds were shown to break and tetravalent uranium compounds were shown to form on the sample surface. Hydroxyl groups were shown to evaporate. The calculated DG0 = -1,3 kJ/mol can be an evidence of several concurrent processes, some of which require energy, as well as of the formation of a surface chemical compound.

  13. The first X-ray imaging spectroscopy of quiescent solar active regions with NuSTAR

    DEFF Research Database (Denmark)

    Hannah, Iain G.; Grefenstette, Brian W.; Smith, David M.

    2016-01-01

    We present the first observations of quiescent active regions (ARs) using the Nuclear Spectroscopic Telescope Array (NuSTAR), a focusing hard X-ray telescope capable of studying faint solar emission from high-temperature and non-thermal sources. We analyze the first directly imaged and spectrally...... resolved X-rays above 2 keV from non-flaring ARs, observed near the west limb on 2014 November 1. The NuSTAR X-ray images match bright features seen in extreme ultraviolet and soft X-rays. The NuSTAR imaging spectroscopy is consistent with isothermal emission of temperatures 3.1-4.4 MK and emission...... measures 1-8 × 1046 cm−3. We do not observe emission above 5 MK, but our short effective exposure times restrict the spectral dynamic range. With few counts above 6 keV, we can place constraints on the presence of an additional hotter component between 5 and 12 MK of∼1046 cm−3 and ∼1043cm−3, respectively...

  14. Recent progress of soft X-ray photoelectron spectroscopy studies of uranium compounds

    Energy Technology Data Exchange (ETDEWEB)

    Fujimori, Shin-ichi; Takeda, Yukiharu; Okane, Tetsuo; Saitoh, Yuji [Condensed Matter Science Divisions, Japan Atomic Energy Agency, Sayo, Hyogo (Japan); Fujimori, Atsushi [Condensed Matter Science Divisions, Japan Atomic Energy Agency, Sayo, Hyogo (Japan); Department of Physics, University of Tokyo, Hongo, Tokyo 113-0033 (Japan); Yamagami, Hiroshi [Condensed Matter Science Divisions, Japan Atomic Energy Agency, Sayo, Hyogo (Japan); Department of Physics, Faculty of Science, Kyoto Sangyo University, Kyoto 603-8555 (Japan); Yamamoto, Etsuji; Haga, Yoshinori [Advanced Science Research Center, Japan Atomic Energy Agency, Tokai, Ibaraki 319-1195 (Japan); Ōnuki, Yoshichika [Advanced Science Research Center, Japan Atomic Energy Agency, Tokai, Ibaraki 319-1195 (Japan); Faculty of Science, University of the Ryukyus, Nishihara, Okinawa 903-0213 (Japan)

    2016-04-15

    Recent progresses in the soft X-ray photoelectron spectroscopy (PES) studies (hν ≳ 100 eV) for uranium compounds are briefly reviewed. The soft X-ray PES has enhanced sensitivities for the bulk U 5f electronic structure, which is essential to understand the unique physical properties of uranium compounds. In particular, the recent remarkable improvement in energy resolutions from an order of 1 eV to 100 meV made it possible to observe fine structures in U 5f density of states. Furthermore, soft X-ray ARPES becomes available due to the increase of photon flux at beamlines in third generation synchrotron radiation facilities.The technique made it possible to observe bulk band structures and Fermi surfaces of uranium compounds and therefore, the results can be directly compared with theoretical models such as band-structure calculations. The core-level spectra of uranium compounds show a systematic behavior depending on their electronic structures, suggesting that they can be utilized to determine basic physical parameters such as the U 5f-ligand hybridizations or Comlomb interaction between U 5f electrons. It is shown that soft X-ray PES provides unique opportunities to understand the electronic structures of uranium compounds.

  15. Atomic structure of machined semiconducting chips: An x-ray absorption spectroscopy study

    Energy Technology Data Exchange (ETDEWEB)

    Paesler, M.; Sayers, D.

    1988-12-01

    X-ray absorption spectroscopy (XAS) has been used to examine the atomic structure of chips of germanium that were produced by single point diamond machining. It is demonstrated that although the local (nearest neighbor) atomic structure is experimentally quite similar to that of single crystal specimens information from more distant atoms indicates the presence of considerable stress. An outline of the technique is given and the strength of XAS in studying the machining process is demonstrated.

  16. Band-gap measurements of bulk and nanoscale hematite by soft x-ray spectroscopy

    DEFF Research Database (Denmark)

    Gilbert, B.; Frandsen, Cathrine; Maxey, E.R.

    2009-01-01

    -gap determination in bulk and nanoscale itinerant electron semiconductors such as CdS and ZnO, but this approach has not been established for materials such as iron oxides that possess band-edge electronic structure dominated by electron correlations. We performed soft x-ray spectroscopy at the oxygen K...... of phase-pure hematite nanoparticles, we find that there is no evidence for size-driven change in the band gap of hematite nanoparticles down to around 8 nm....

  17. Energy dispersive x-ray spectroscopy for nanostructured thin film density evaluation

    OpenAIRE

    Prencipe, Irene; Dellasega, David; Zani, Alessandro; Rizzo, Daniele; Passoni, Matteo

    2015-01-01

    In this paper, we report on two fast and non-destructive methods for nanostructured film density evaluation based on a combination of energy dispersive x-ray spectroscopy for areal density measurement and scanning electron microscopy (SEM) for thickness evaluation. These techniques have been applied to films with density ranging from the density of a solid down to a few , with different compositions and morphologies. The high resolution of an electron microprobe has been exploited to characte...

  18. Probing the stability of the spin of compact objects with X-ray reflection spectroscopy

    Science.gov (United States)

    Deich, Alex; Alex

    2018-01-01

    X-ray reflection spectroscopy has recently been shown to be a viable method of directly measuring the parameters of Kerr spacetimes (Bambi 2017). In this work, we use this method to focus on the stability of the Kerr spin parameter. We present simulations of spectra resulting from various spin-up and spin-down scenarios and use these results to look for any evidence of objects with a changing spin in archival Swift data.

  19. X-ray instrumentation for SR beamlines

    CERN Document Server

    Kovalchuk, M V; Zheludeva, S I; Aleshko-Ozhevsky, O P; Arutynyan, E H; Kheiker, D M; Kreines, A Y; Lider, V V; Pashaev, E M; Shilina, N Y; Shishkov, V A

    2000-01-01

    The main possibilities and parameters of experimental X-ray stations are presented: 'Protein crystallography', 'X-ray structure analysis', 'High-precision X-ray optics', 'X-ray crystallography and material science', 'X-ray topography', 'Photoelectron X-ray standing wave' that are being installed at Kurchatov SR source by A.V. Shubnikov Institute of Crystallography.

  20. Soft X-ray synchrotron radiation investigations of actinidematerials systems utilizing X-ray emission spectroscopy and resonantinelastic X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Shuh, D.K.; Butorin, S.M.; Guo, J.-H.; Nordgren, J.

    2004-01-03

    Synchrotron radiation (SR) methods have been utilized with increasing frequency over the past several years to study topics in actinide science, ranging from those of a fundamental nature to those that address a specifically-targeted technical need. In particular, the emergence of microspectroscopic and fluorescence-based techniques have permitted investigations of actinide materials at sources of soft x-ray SR. Spectroscopic techniques with fluorescence-based detection are useful for actinide investigations since they are sensitive to small amounts of material and the information sampling depth may be varied. These characteristics also serve to simplify both sample preparation and safety considerations. Examples of investigations using these fluorescence techniques will be described along with their results, as well as the prospects for future investigations utilizing these methodologies.

  1. Investigation Of Li{sub X}CoO{sub 2} Li- Intercalation Electrodes Using X-Ray Absorption Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Haas, O.; Holzapfel, M.; Yang, X.Q. [BNL Lab (United States); Yoon, W.-S. [BNL Lab (United States); Chung, K.-Y. [BNL Lab (United States)

    2005-03-01

    Li{sub X}CoO{sub 2} was investigated with X-ray absorption spectroscopy using hard and soft X-rays and compared with some results obtained in previous investigations of La{sub (1-x)}-Ca{sub x}CoO{sub 3}, which has a similar electron configuration. (author)

  2. Microelemental and mineral compositions of pathogenic biomineral concrements: SRXFA, X-ray powder diffraction and vibrational spectroscopy data

    Energy Technology Data Exchange (ETDEWEB)

    Moroz, T.N. [Institute of Geology and Mineralogy, SB RAS, Pr. Akad. Koptyuga, 3, 630090 Novosibirsk (Russian Federation)], E-mail: moroz@uiggm.nsc.ru; Palchik, N.A.; Dar' in, A.V. [Institute of Geology and Mineralogy, SB RAS, Pr. Akad. Koptyuga, 3, 630090 Novosibirsk (Russian Federation)

    2009-05-11

    X-ray fluorescence analysis using synchrotron radiation (SRXRF), X-ray powder diffraction, infrared and Raman spectroscopy had been applied for determination of microelemental and mineral composition of the kidney stones, gallstones and salivalities from natives of Novosibirsk and Novosibirsk region, Russia. The relationship between mineral, organic and microelemental composition of pathogenic calcilus was shown.

  3. Al{sub 0.2}Ga{sub 0.8}As X-ray photodiodes for X-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Whitaker, M.D.C., E-mail: M.Whitaker@sussex.ac.uk; Lioliou, G.; Butera, S.; Barnett, A.M.

    2016-12-21

    Three custom-made Al{sub 0.2}Ga{sub 0.8}As p-i-n mesa X-ray photodiodes (200 µm diameter, 3 µm i layer) were electrically characterised and investigated for their response to illumination with soft X-rays from an {sup 55}Fe radioisotope X-ray source (Mn Kα = 5.9 keV; Mn Kβ = 6.49 keV). The AlGaAs photodiodes were shown to be suitable for photon counting X-ray spectroscopy at room temperature. When coupled to a custom-made low-noise charge-sensitive preamplifier, a mean energy resolution (as quantified by the full width at half maximum of the 5.9 keV photopeak) of 1.24 keV was measured at room temperature. Parameters such as the depletion width (1.92 µm at 10 V), charge trapping noise (61.7 e{sup −} rms ENC at 5 V, negligible at 10 V) and the electronic noise components (known dielectric noise (63.4 e{sup −} rms), series white noise (27.7 e{sup −} rms), parallel white noise (9.5 e{sup −} rms) and 1/f series noise (2.2 e{sup −} rms) at 10 V reverse bias) affecting the achieved energy resolution were computed. The estimated charge trapping noise and mean energy resolution were compared to similar materials (e.g. Al{sub 0.8}Ga{sub 0.2}As) previously reported, and discussed. These results are the first demonstration of photon counting X-ray spectroscopy with Al{sub 0.2}Ga{sub 0.8}As reported to date.

  4. Combination of Raman, infrared, and X-ray energy-dispersion spectroscopies and X-ray d diffraction to study a fossilization process

    Energy Technology Data Exchange (ETDEWEB)

    Sousa Filho, Francisco Eduardo de [Departamento de Fisica, Universidade Regional do Cariri, Crato, CE (Brazil); Joao Herminio da Silva [Universidade Federal do Ceara, Cariri, Juazeiro do Norte, CE (Brazil); Saraiva, Antonio Alamo Feitosa; Brito, Deyvid Dennys S. [Departamento de Ciencias Biologicas, Universidade Regional do Cariri, Crato, CE (Brazil); Viana, Bartolomeu Cruz [Departamento de Fisica, Universidade Federal do Piaui, Teresina, PI, (Brazil); Abagaro, Bruno Tavares de Oliveira; Freire, Paulo de Tarso Cavalcante, E-mail: tarso@fisica.ufc.br [Departamento de Fisica, Universidade Federal do Ceara, Fortaleza, CE (Brazil)

    2011-12-15

    X-ray diffraction was combined with X-ray energy-dispersion, Fourier-transform infrared, and Raman spectroscopies to study the fossilization of a Cretaceous specimen of the plant Brachyphyllum castilhoi, a fossil from the Ipubi Formation, in the Araripe Sedimentary Basin, Northeastern Brazil. Among the possible fossilization processes, which could involve pyrite, silicon oxide, calcium oxide, or other minerals, we were able to single out pyritization as the central mechanism producing the fossil, more than 100 million years ago. In addition to expanding the knowledge of the Ipubi Formation, this study shows that, when combined with other experimental techniques, Raman spectroscopy is a valuable tool at the paleontologist's disposal. (author)

  5. High-brightness beamline for x-ray spectroscopy at the ALS

    Energy Technology Data Exchange (ETDEWEB)

    Perera, R.C.C.; Jones, G. [Ernest Orlando Lawrence Berkeley National Lab., CA (United States); Lindle, D.W. [Univ. of Nevada, Las Vegas, NV (United States)

    1997-04-01

    Beamline 9.3.1 at the Advanced Light Source (ALS) is a windowless beamline, covering the 1-6 keV photon-energy range, designed to achieve the goals of high energy resolution, high flux, and high brightness at the sample. When completed later this year, it will be the first ALS monochromatic hard x-ray beamline, and its brightness will be an order of magnitude higher than presently available in this energy range. In addition, it will provide flux and resolution comparable to any other beamline now in operation. To achieve these goals, two technical improvements, relative to existing x-ray beamlines, were incorporated. First, a somewhat novel optical design for x-rays, in which matched toroidal mirrors are positioned before and after the double-crystal monochromator, was adopted. This configuration allows for high resolution by passing a collimated beam through the monochromator, and for high brightness by focusing the ALS source on the sample with unit magnification. Second, a new {open_quotes}Cowan type{close_quotes} double-crystal monochromator based on the design used at NSLS beamline X-24A was developed. The measured mechanical precision of this new monochromator shows significant improvement over existing designs, without using positional feedback available with piezoelectric devices. Such precision is essential because of the high brightness of the radiation and the long distance (12 m) from the source (sample) to the collimating (focusing) mirror. This combination of features will provide a bright, high resolution, and stable x-ray beam for use in the x-ray spectroscopy program at the ALS.

  6. A structural study of bone changes in knee osteoarthritis by synchrotron-based X-ray fluorescence and X-ray absorption spectroscopy techniques

    Science.gov (United States)

    Sindhupakorn, Bura; Thienpratharn, Suwittaya; Kidkhunthod, Pinit

    2017-10-01

    Osteoarthritis (OA) is characterized by degeneration of articular cartilage and thickening of subchondral bone. The present study investigated the changing of biochemical components of cartilage and bone compared between normal and OA people. Using Synchrotron-based X-ray fluorescence (SR-XRF) and X-ray absorption spectroscopy (XAS) techniquesincluding X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) were employed for the bone changes in kneeosteoarthritisstudies. The bone samples were collected from various osteoarthritis patients with both male and female in the ages range between 20 and 74 years old. SR-XRF results excited at 4240 eV for Ca elements show a majority three main groups, based on their XRF intensities, 20-36 years, 40-60 years and over 70 years, respectively. By employing XAS techniques, XANES features can be used to clearly explain in term of electronic transitions occurring in bone samples which are affected from osteoarthritis symptoms. Moreover, a structural change around Ca ions in bone samples is obviously obtained by EXAFS results indicating an increase of Ca-amorphous phase when the ages increase.

  7. Unveiling the Structure of Active Galactic Nuclei with Hard X-ray Spectroscopy

    Science.gov (United States)

    Balokovic, Mislav

    Despite the long history of studies of active galactic nuclei (AGN), details of the structure of the accretion flow onto supermassive black holes are far from clear. Work presented in this thesis is directed at unveiling properties of AGN structure through broadband X-ray spectroscopy, with particular emphasis on the hard X-ray band (photon energies above 10 keV). With its unprecedented sensitivity in this energy band, the NuSTAR telescope provides the key observational diagnostics of the properties of the AGN X-ray source, the corona, and the surrounding gas in the accretion disk, the broad-line region, and the torus. The first study presented in this thesis focuses on measurements of the optical depth and the temperature of the plasma in the corona of an obscured AGN. Fitting theoretical spectral models for coronal emission to the NuSTAR data constrained these two basic physical parameters under the assumption of either spherical or disk-like geometry for the corona. The remainder of the thesis is dedicated to studies of the anisotropic obscuring structure broadly referred to as the torus. One of them is a case study of three heavily obscured AGN with spectra dominated by the X-ray light scattered and reprocessed in the torus, where it is possible to constrain one of the basic torus properties - its globally averaged column density. The following study presents the calculation of a new spectral model for reprocessing of the intrinsic X-ray continuum within the torus. Its added flexibility compared to previously available models allows for both the average column density of the torus and its covering factor to be constrained from broadband X-ray spectra of a wide variety of AGN. The final part of the thesis in based on a large survey of the local obscured AGN population performed with NuSTAR. Spectral modeling of more than a hundred individual AGN, including both old and new spectral models, is presented. From analyses of the X-ray data for a large and

  8. Scanning electron microscopy and X-ray spectroscopy applied to mycelial phase of sporothrix schenckii

    Directory of Open Access Journals (Sweden)

    M. Thibaut

    1975-04-01

    Full Text Available Scanning electron microscopy applied to the mycelial phase of Sporothrix schenckii shows a matted mycelium with conidia of a regular pattern. X-Ray microanalysis applied in energy dispersive spectroscopy and also in wavelength dispersive spectroscopy reveals the presence of several elements of Mendeleef's classification.Sporothrix schenckii foi estudado em microscopia eletrônica. Foram observados caracteres das hífas e dos esporos, vários elementos da classificação periódica foram postos em evidência graças à micro-análise a raios X.

  9. Surface Arsenic Speciation of a Drinking-Water Treatment Residual Using X-Ray Absorption Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Makris, K.C.; Sarkar, D.; Parsons, J.G.; Datta, R.; Gardea-Torresdey, J.L.

    2009-06-03

    Drinking-water treatment residuals (WTRs) present a low-cost geosorbent for As-contaminated waters and soils. Previous work has demonstrated the high affinity of WTRs for As, but data pertaining to the stability of sorbed As is missing. Sorption/desorption and X-ray absorption spectroscopy (XAS), both XANES (X-ray absorption near edge structure) and EXAFS (extended X-ray absorption fine structure) studies, were combined to determine the stability of As sorbed by an Fe-based WTR. Arsenic(V) and As(III) sorption kinetics were biphasic in nature, sorbing <90% of the initial added As (15,000 mg kg{sup -1}) after 48 h of reaction. Subsequent desorption experiments with a high P load (7500 mg kg{sup -1}) showed negligible As desorption for both As species, approximately <3.5% of sorbed As; the small amount of desorbed As was attributed to the abundance of sorption sites. XANES data showed that sorption kinetics for either As(III) or As(V) initially added to solution had no effect on the sorbed As oxidation state. EXAFS spectroscopy suggested that As added either as As(III) or as As(V) formed inner-sphere mononuclear, bidentate complexes, suggesting the stability of the sorbed As, which was further corroborated by the minimum As desorption from the Fe-WTR.

  10. Mineral identification in Colombian coals using Moessbauer spectroscopy and X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Fajardo, M. [Universidad del Valle, A.A, Departamento de Fisica (Colombia); Mojica, J. [Instituto Nacional de Investigaciones en Geociencia, Mineria y Quimica (INGEOMINAS) (Colombia); Barraza, J. [Universidad del Valle, A.A, Departamento de Procesos Quimicos, Facultad de Ingenieria (Colombia); Perez Alcazar, G.A.; Tabares, J.A. [Universidad del Valle, A.A, Departamento de Fisica (Colombia)

    1999-11-15

    Minerals were identified in three Colombian coal samples from the Southwest of the country using Moessbauer spectroscopy and X-ray diffraction. Original and sink separated coal fractions of specific gravity 1.40 and 1.60 with particle size less than 600 {mu}m were used in the study. Using Moessbauer spectroscopy, the minerals identified in the original coal samples were pyrite jarosite, ankerite, illite and ferrous sulfate, whereas by means of X-ray diffraction, minerals identified were kaolinite, quartz, pyrite, and jarosite. Differences in mineral composition were found in the original and sink separated fractions using both techniques. Moessbauer spectra show that the mineral phases in low concentrations such as illite, ankerite and ferrous sulfate do not always appear in the spectra of sink coals, despite of those minerals occurring in the original coal, due to the fact that they are associated with the organic matter and not liberated in the grinding process. X-ray results show that the peak intensity grows as the specific gravity is increased indicating that the density separation method could be an effective process to clean coal.

  11. A short-pulse X-ray beamline for spectroscopy and scattering.

    Science.gov (United States)

    Reininger, R; Dufresne, E M; Borland, M; Beno, M A; Young, L; Evans, P G

    2014-09-01

    Experimental facilities for picosecond X-ray spectroscopy and scattering based on RF deflection of stored electron beams face a series of optical design challenges. Beamlines designed around such a source enable time-resolved diffraction, spectroscopy and imaging studies in chemical, condensed matter and nanoscale materials science using few-picosecond-duration pulses possessing the stability, high repetition rate and spectral range of synchrotron light sources. The RF-deflected chirped electron beam produces a vertical fan of undulator radiation with a correlation between angle and time. The duration of the X-ray pulses delivered to experiments is selected by a vertical aperture. In addition to the radiation at the fundamental photon energy in the central cone, the undulator also emits the same photon energy in concentric rings around the central cone, which can potentially compromise the time resolution of experiments. A detailed analysis of this issue is presented for the proposed SPXSS beamline for the Advanced Photon Source. An optical design that minimizes the effects of off-axis radiation in lengthening the duration of pulses and provides variable X-ray pulse duration between 2.4 and 16 ps is presented.

  12. In situ/Operando studies of electrocatalysts using hard X-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Lassalle-Kaiser, Benedikt [Synchrotron SOLEIL, Gif-sur-Yvette (France); Gul, Sheraz [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Molecular Biophysics and Integrated Bioimaging Div.; Kern, Jan [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Molecular Biophysics and Integrated Bioimaging Div.; SLAC National Accelerator Lab., Menlo Park, CA (United States). Linac Coherent Light Source (LCLS); Yachandra, Vittal K. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Molecular Biophysics and Integrated Bioimaging Div.; Yano, Junko [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Molecular Biophysics and Integrated Bioimaging Div.

    2017-05-02

    This review focuses on the use of X-ray absorption and emission spectroscopy techniques using hard X-rays to study electrocatalysts under in situ/operando conditions. The importance and the versatility of methods in the study of electrodes in contact with the electrolytes are described, when they are being cycled through the catalytic potentials during the progress of the oxygen-evolution, oxygen reduction and hydrogen evolution reactions. The catalytic oxygen evolution reaction is illustrated with examples using three oxides, Co, Ni and Mn, and two sulfides, Mo and Co. These are used as examples for the hydrogen evolution reaction. A bimetallic, bifunctional oxygen evolving and oxygen reducing Ni/Mn oxide is also presented. The various advantages and constraints in the use of these techniques and the future outlook are discussed.

  13. Probing Transient Valence Orbital Changes with Picosecond Valence-to-Core X-ray Emission Spectroscopy

    DEFF Research Database (Denmark)

    March, Anne Marie; Assefa, Tadesse A.; Boemer, Christina

    2017-01-01

    valence orbitals to the nascent core-hole. Vtc-XES offers particular insight into the molecular orbitals directly involved in the light-driven dynamics; a change in the metal ligand orbital overlap results in an intensity reduction and a blue energy shift in agreement with our theoretical calculations......We probe the dynamics of valence electrons in photoexcited [Fe(terpy)2]2+ in solution to gain deeper insight into the Fe ligand bond changes. We use hard X-ray emission spectroscopy (XES), which combines element specificity and high penetration with sensitivity to orbital structure, making...... it a powerful technique for molecular studies in a wide variety of environments. A picosecond-time-resolved measurement of the complete Is X-ray emission spectrum captures the transient photoinduced changes and includes the weak valence-to-core (vtc) emission lines that correspond to transitions from occupied...

  14. Strontium Localization in Bone Tissue Studied by X-Ray Absorption Spectroscopy

    DEFF Research Database (Denmark)

    Frankær, Christian Grundahl; Raffalt, Anders Christer; Ståhl, Kenny

    2014-01-01

    Strontium has recently been introduced as a pharmacological agent for the treatment and prevention of osteoporosis. We determined the localization of strontium incorporated into bone matrix from dogs treated with Sr malonate by X-ray absorption spectroscopy. A new approach for analyzing the X......-ray absorption spectra resulted in a compositional model and allowed the relative distribution of strontium in the different bone components to be estimated. Approximately 35–45 % of the strontium present is incorporated into calcium hydroxyapatite (CaHA) by substitution of some of the calcium ions occupying...... highly ordered sites, and at least 30 % is located at less ordered sites where only the first solvation shell is resolved, suggesting that strontium is sur- rounded by only oxygen atoms similar to Sr2? in solution. Strontium was furthermore shown to be absorbed in collagen in which it obtains a higher...

  15. High average power, highly brilliant laser-produced plasma source for soft X-ray spectroscopy.

    Science.gov (United States)

    Mantouvalou, Ioanna; Witte, Katharina; Grötzsch, Daniel; Neitzel, Michael; Günther, Sabrina; Baumann, Jonas; Jung, Robert; Stiel, Holger; Kanngiesser, Birgit; Sandner, Wolfgang

    2015-03-01

    In this work, a novel laser-produced plasma source is presented which delivers pulsed broadband soft X-radiation in the range between 100 and 1200 eV. The source was designed in view of long operating hours, high stability, and cost effectiveness. It relies on a rotating and translating metal target and achieves high stability through an on-line monitoring device using a four quadrant extreme ultraviolet diode in a pinhole camera arrangement. The source can be operated with three different laser pulse durations and various target materials and is equipped with two beamlines for simultaneous experiments. Characterization measurements are presented with special emphasis on the source position and emission stability of the source. As a first application, a near edge X-ray absorption fine structure measurement on a thin polyimide foil shows the potential of the source for soft X-ray spectroscopy.

  16. Effects of partial coherence on correlation functions measured by x-ray photon correlation spectroscopy

    Science.gov (United States)

    Gutt, C.; Ghaderi, T.; Tolan, M.; Sinha, S. K.; Grübel, G.

    2008-03-01

    We present a rigorous description of the effects of partial coherence and detector resolution on intensity autocorrelation functions as they can be measured by x-ray photon correlation spectroscopy (XPCS). Based on the Huygens-Fresnel propagation law and on the first Born approximation, we derive a general expression for the normalized intensity autocorrelation function. We calculate how the mutual coherence function of the x-ray beam propagates from an aperture to the sample and how it propagates after the scattering process to the detector area and consequently influences the intensity autocorrelation function. We illustrate our calculation with examples of XPCS intensity autocorrelation functions of liquid surfaces calculated for grazing incidence geometry.

  17. Structure and dynamics of hemeproteins using X-ray Absorption Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Arcovito, Alessandro [Istituto di Biochimica e Biochimica Clinica, Universita Cattolica del Sacro Cuore, L.go F. Vito 1, 00168 Rome (Italy); D' Angelo, Paola [Dipartimento di Chimica, Sapienza-Universita di Roma, P.le A. Moro 5, 00185 Rome (Italy); Longa, Stefano Della, E-mail: alessandro.arcovito@rm.unicatt.i, E-mail: dlonga@caspur.i [Dipartimento di Medicina Sperimentale, Universita ' L' Aquila' , Via Vetoio, 67100 L' Aquila (Italy)

    2009-11-15

    Experimental investigations on protein dynamics are usually carried out in solution; however, in most cases, the determination of protein structure is done by crystallography that relies on the diffraction properties of the protein arranged in a three-dimensional lattice. X-ray Absorption Spectroscopy (XAS) is an ideal tool to investigate the deep relationships between structure and dynamics, on a wide class of metal containing proteins, including hemeproteins. In fact, this technique can be used either as a structural refinement of X-ray diffraction on the same crystal, or as an independent tool to study structural dynamic properties both in crystal and solution. Different examples will be presented and discussed, with particular emphasis onto the original contribution due to the application of the MXAN software package to the analysis of XANES spectra.

  18. Design of solar cell materials via soft X-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Himpsel, F.J., E-mail: fhimpsel@wisc.edu [Department of Physics, University of Wisconsin Madison, Madison, WI 53706 (United States); Cook, P.L. [Natural Sciences Department, University of Wisconsin Superior, Superior, WI 54880 (United States); Torre, G. de la [Departamento de Química Orgánica, Facultad de Ciencias, Universidad Autónoma de Madrid, Campus de Cantoblanco, 28049 Madrid (Spain); Garcia-Lastra, J.M. [Material Physics Center (MPC), Centro de Física de Materiales (CSIC-UPV/EHU), Donostia International Physics Center - DIPC, Departamento de Fisica Aplicada I, Universidad del Pais Vasco, 20018 San Sebastian (Spain); Department of Physics, Center for Atomic-scale Materials Design, Technical University of Denmark, DK-2800 Kgs. Lyngby (Denmark); Gonzalez-Moreno, R. [Material Physics Center (MPC), Centro de Física de Materiales (CSIC-UPV/EHU), Donostia International Physics Center - DIPC, Departamento de Fisica Aplicada I, Universidad del Pais Vasco, 20018 San Sebastian (Spain); Guo, J.-H. [Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Hamers, R.J. [Department of Chemistry, University of Wisconsin Madison, Madison, WI 53706 (United States); Kronawitter, C.X. [Environmental Energy Technologies Division, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Johnson, P.S. [Department of Physics, University of Wisconsin Madison, Madison, WI 53706 (United States); Ortega, J.E.; Pickup, D. [Material Physics Center (MPC), Centro de Física de Materiales (CSIC-UPV/EHU), Donostia International Physics Center - DIPC, Departamento de Fisica Aplicada I, Universidad del Pais Vasco, 20018 San Sebastian (Spain); and others

    2013-10-15

    Highlights: ► The use of soft X-ray spectroscopy for developing new materials for solar cells is illustrated. ► A generic layout of a solar cell is given, which facilitates the discussion of the energy levels involved in a solar cell and their optimization. ► Systematic measurements of organometallic dyes are presented in combination with density functional theory. ► The data reveal trends that are useful for tailoring materials for solar cells. ► A solar cell design based on thin film p-type diamond as donor is used as example. -- Abstract: This overview illustrates how spectroscopy with soft X-rays can assist the development of new materials and new designs for solar cells. The starting point is the general layout of a solar cell, which consists of a light absorber sandwiched between an electron donor and an electron acceptor. There are four relevant energy levels that can be measured with a combination of X-ray absorption spectroscopy and photoelectron spectroscopy, as illustrated for an organic dye as absorber attached to a p-doped diamond film as donor. Systematic measurements of organometallic dyes (phthalocyanines and porphyrins) as a function of the metal atom are presented for the metal 2p and N 1s absorption edges. In combination with density functional theory one can discern trends that are useful for tailoring absorber molecules. A customized porphyrin molecule is investigated that combines an absorber with a donor and a linker to an oxide acceptor. The bridge to device fabrication is crossed by correlating spectroscopic features with the photocurrent in hematite photoanodes for water splitting. For speeding up the development of new materials and designs of solar cells a feedback loop between spectroscopy, theory, synthesis and device fabrication is envisioned.

  19. Characterization of the Carancas-Puno meteorite by energy dispersive X-ray fluorescence, X-ray diffractometry and transmission Moessbauer spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Ceron Loayza, Maria L., E-mail: malucelo@hotmail.com; Bravo Cabrejos, Jorge A. [Universidad Nacional Mayor de San Marcos, Laboratorio de Analisis de Suelos, Facultad de Ciencias Fisicas (Peru)

    2011-11-15

    We report the results of the study of a meteorite that impacted an inhabited zone on 15 September 2007 in the neighborhood of the town of Carancas, Puno Region, about 1,300 km south of Lima. The analysis carried out by energy dispersive X-ray fluorescence, X-ray diffractometry and transmission Moessbauer spectroscopy (at room temperature and at 4.2 K), reveal the presence in the meteorite sample of magnetic sites assigned to taenite (Fe,Ni) and troilite (Fe,S) phases, and of two paramagnetic doublets assigned to Fe{sup 2 + }, one associated with olivine and the other to pyroxene. In accord with these results, this meteorite is classified as a type IV chondrite meteorite.

  20. X-ray spectroscopy for chemical and energy sciences: the case of heterogeneous catalysis.

    Science.gov (United States)

    Frenkel, Anatoly I; van Bokhoven, Jeroen A

    2014-09-01

    Heterogeneous catalysis is the enabling technology for much of the current and future processes relevant for energy conversion and chemicals synthesis. The development of new materials and processes is greatly helped by the understanding of the catalytic process at the molecular level on the macro/micro-kinetic time scale and on that of the actual bond breaking and bond making. The performance of heterogeneous catalysts is inherently the average over the ensemble of active sites. Much development aims at unravelling the structure of the active site; however, in general, these methods yield the ensemble-average structure. A benefit of X-ray-based methods is the large penetration depth of the X-rays, enabling in situ and operando measurements. The potential of X-ray absorption and emission spectroscopy methods (XANES, EXAFS, HERFD, RIXS and HEROS) to directly measure the structure of the catalytically active site at the single nanoparticle level using nanometer beams at diffraction-limited storage ring sources is highlighted. The use of pump-probe schemes coupled with single-shot experiments will extend the time range from the micro/macro-kinetic time domain to the time scale of bond breaking and making.

  1. X-ray spectroscopy with a multi-anode sawtooth silicon drift detector: the diffusion process

    Energy Technology Data Exchange (ETDEWEB)

    Sonsky, J. E-mail: sonsky@iri.tudelft.nl; Hollander, R.W.; Sarro, P.M.; Eijk, C.W.E. van

    2002-01-21

    The position sensitive detection of low-energy X-rays can be realized by means of a multi-anode linear silicon drift detector (SDD). However, a severe worsening of the spectroscopic quality of the detector is observed due to the lateral broadening of the X-ray generated electron cloud during drift. Recently, we have proved experimentally that electron confinement can be achieved by means of sawtooth-shaped p{sup +} strips; the sawtooth concept. This paper will present room temperature X-ray spectroscopy measurements clearly demonstrating the improvement of spectroscopic quality of the sawtooth SDD as compared with a traditional linear SDD. Using a sawtooth SDD we have measured an energy resolution of 1.4 keV FWHM at the 13.9 keV peak of {sup 241}Am at room temperature and a substantial reduction of the number of split events is also observed. The calculation of the influence of diffusion on the quality of the pulse height spectrum will also be given.

  2. X-ray spectroscopy with a multi-anode sawtooth silicon drift detector the diffusion process

    CERN Document Server

    Sonsky, J; Sarro, P M; Eijk, C W

    2002-01-01

    The position sensitive detection of low-energy X-rays can be realized by means of a multi-anode linear silicon drift detector (SDD). However, a severe worsening of the spectroscopic quality of the detector is observed due to the lateral broadening of the X-ray generated electron cloud during drift. Recently, we have proved experimentally that electron confinement can be achieved by means of sawtooth-shaped p sup + strips; the sawtooth concept. This paper will present room temperature X-ray spectroscopy measurements clearly demonstrating the improvement of spectroscopic quality of the sawtooth SDD as compared with a traditional linear SDD. Using a sawtooth SDD we have measured an energy resolution of 1.4 keV FWHM at the 13.9 keV peak of sup 2 sup 4 sup 1 Am at room temperature and a substantial reduction of the number of split events is also observed. The calculation of the influence of diffusion on the quality of the pulse height spectrum will also be given.

  3. Ultrafast Absorption Spectroscopy of Aluminum Plasmas Created by LCLS using Betatron X-Ray Radiation

    Energy Technology Data Exchange (ETDEWEB)

    Albert, Felicie [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2016-10-12

    This document summarizes the goals and accomplishments of a six month-long LDRD project, awarded through the LLNL director Early and Mid Career Recognition (EMCR) program. This project allowed us to support beamtime awarded at the Matter under Extreme Conditions (MEC) end station of the Linac Coherent Light Source (LCLS). The goal of the experiment was to heat metallic samples with the bright x-rays from the LCLS free electron laser. Then, we studied how they relaxed back to equilibrium by probing them with ultrafast x-ray absorption spectroscopy using laser-based betatron radiation. Our work enabled large collaborations between LLNL, SLAC, LBNL, and institutions in France and in the UK, while providing training to undergraduate and graduate students during the experiment. Following this LDRD project, the PI was awarded a 5-year DOE early career research grant to further develop applications of laser-driven x-ray sources for high energy density science experiments and warm dense matter states.

  4. Time-resolved X-ray Absorption Spectroscopy for Electron Transport Study in Warm Dense Gold

    Science.gov (United States)

    Lee, Jong-Won; Bae, Leejin; Engelhorn, Kyle; Heimann, Philip; Ping, Yuan; Barbrel, Ben; Fernandez, Amalia; Beckwith, Martha Anne; Cho, Byoung-Ick; GIST Team; IBS Team; LBNL Collaboration; SLAC Collaboration; LLNL Collaboration

    2015-11-01

    The warm dense Matter represents states of which the temperature is comparable to Fermi energy and ions are strongly coupled. One of the experimental techniques to create such state in the laboratory condition is the isochoric heating of thin metal foil with femtosecond laser pulses. This concept largely relies on the ballistic transport of electrons near the Fermi-level, which were mainly studied for the metals in ambient conditions. However, they were barely investigated in warm dense conditions. We present a time-resolved x-ray absorption spectroscopy measured for the Au/Cu dual layered sample. The front Au layer was isochorically heated with a femtosecond laser pulse, and the x-ray absorption changes around L-edge of Cu, which was attached on the backside of Au, was measured with a picosecond resolution. Time delays between the heating of the `front surface' of Au layer and the alternation of x-ray spectrum of Cu attached on the `rear surface' of Au indicate the energetic electron transport mechanism through Au in the warm dense conditions. IBS (IBS-R012-D1) and the NRF (No. 2013R1A1A1007084) of Korea.

  5. Electronic structure of Fe2P(10 1 bar 0) studied by soft X-ray photoelectron spectroscopy and X-ray absorption spectroscopy

    Science.gov (United States)

    Sugizaki, Y.; Motoyama, H.; Edamoto, K.; Ozawa, K.

    2017-10-01

    The electronic structure of Fe2P(10 1 bar 0) has been investigated by photoelectron spectroscopy (PES) and X-ray absorption spectroscopy (XAS). The surface prepared by cycles of Ar+ ion sputtering and annealing at 500-800 °C showed a c(2 × 2) low-energy electron diffraction (LEED) pattern. An Fe 3d-P 3p hybrid band (main band) and a satellite were observed at 0-4 eV and 5-8 eV, respectively, in PES spectra of c(2 × 2) Fe2P(10 1 bar 0). The main band showed a clear cut-off at the Fermi edge, indicating the metallic nature of Fe2P. The satellite intensity showed a resonant maximum around the Fe 3p threshold, suggesting that the satellite is caused through a shake-up process. Three types of surface-shifted components were found in P 2p PES spectra. All the P 2p peaks have symmetric line shapes, while the Fe 2p PES and Fe L-edge XAS spectra have asymmetric line shapes, suggesting that the electronic states around the Fermi level are mostly composed of Fe 3d components. These results suggest that the stabilization of the electronic structure at metal sites through the bonding with P atoms is ineffective on Fe2P(10 1 bar 0), as in the case of Fe2P(0001).

  6. Ultrafast Excited State Relaxation of a Metalloporphyrin Revealed by Femtosecond X-ray Absorption Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Shelby, Megan L. [Chemical; Department; Lestrange, Patrick J. [Department; Jackson, Nicholas E. [Department; Haldrup, Kristoffer [Physics; Mara, Michael W. [Chemical; Department; Stickrath, Andrew B. [Chemical; Zhu, Diling [LCLS, SLAC National Laboratory, Menlo Park, California 94025, United States; Lemke, Henrik T. [LCLS, SLAC National Laboratory, Menlo Park, California 94025, United States; Chollet, Matthieu [LCLS, SLAC National Laboratory, Menlo Park, California 94025, United States; Hoffman, Brian M. [Department; Li, Xiaosong [Department; Chen, Lin X. [Chemical; Department

    2016-07-06

    Photoexcited Nickel(II) tetramesitylporphyrin (NiTMP), like many open-shell metalloporphyrins, relaxes rapidly through multiple electronic states following an initial porphyrin-based excitation, some involving metal centered electronic configuration changes that could be harnessed catalytically before excited state relaxation. While a NiTMP excited state present at 100 ps was previously identified by X-ray transient absorption (XTA) spectroscopy at a synchrotron source as a relaxed (d,d) state, the lowest energy excited state (J. Am. Chem. Soc., 2007, 129, 9616 and Chem. Sci., 2010, 1, 642), structural dynamics before thermalization were not resolved due to the similar to 100 ps duration of the available X-ray probe pulse. Using the femtosecond (fs) X-ray pulses of the Linac Coherent Light Source (LCLS), the Ni center electronic configuration from the initial excited state to the relaxed (d,d) state has been obtained via ultrafast Ni K-edge XANES (X-ray absorption near edge structure) on a time scale from hundreds of femtoseconds to 100 ps. This enabled the identification of a short-lived Ni(I) species aided by time-dependent density functional theory (TDDFT) methods. Computed electronic and nuclear structure for critical excited electronic states in the relaxation pathway characterize the dependence of the complex's geometry on the electron occupation of the 3d orbitals. Calculated XANES transitions for these excited states assign a short-lived transient signal to the spectroscopic signature of the Ni(I) species, resulting from intramolecular charge transfer on a time scale that has eluded previous synchrotron studies. These combined results enable us to examine the excited state structural dynamics of NiTMP prior to thermal relaxation and to capture intermediates of potential photocatalytic significance.

  7. Characterising legacy spent nuclear fuel pond materials using microfocus X-ray absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Bower, W.R. [Research Centre for Radwaste Disposal, School of Earth and Environmental Sciences, The University of Manchester, Oxford Road, Manchester M13 9PL (United Kingdom); National Nuclear Laboratory, Chadwick House, Warrington Road, Birchwood Park, Warrington, WA3 6AE (United Kingdom); Centre for Radiochemistry Research, Chemistry Building, The University of Manchester, Brunswick Street, Manchester M13 9PL (United Kingdom); Morris, K. [Research Centre for Radwaste Disposal, School of Earth and Environmental Sciences, The University of Manchester, Oxford Road, Manchester M13 9PL (United Kingdom); Mosselmans, J.F.W. [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE (United Kingdom); Thompson, O.R. [National Nuclear Laboratory, Chadwick House, Warrington Road, Birchwood Park, Warrington, WA3 6AE (United Kingdom); Banford, A.W. [National Nuclear Laboratory, Chadwick House, Warrington Road, Birchwood Park, Warrington, WA3 6AE (United Kingdom); School of Chemical Engineering and Analytical Science, The University of Manchester, Oxford Road, Manchester, M13 9PL (United Kingdom); Law, K. [Centre for Radiochemistry Research, Chemistry Building, The University of Manchester, Brunswick Street, Manchester M13 9PL (United Kingdom); Pattrick, R.A.D., E-mail: richard.pattrick@manchester.ac.uk [Research Centre for Radwaste Disposal, School of Earth and Environmental Sciences, The University of Manchester, Oxford Road, Manchester M13 9PL (United Kingdom)

    2016-11-05

    Highlights: • A sample from a spent fuel pond wall has been analysed via X-ray spectroscopy. • Autoradiography shows a patchy distribution of radioactivity on the core face. • μXAS across a ‘hot spot’ showed Sr associates with the TiO{sub 2} pigment in the paint. • Original concrete coatings prove effective at limiting radionuclide migration. • Sorption studies show Sr immobilisation by the concrete and Cs by aggregate clasts. - Abstract: Analysis of a radioactive, coated concrete core from the decommissioned, spent nuclear fuel cooling pond at the Hunterston-A nuclear site (UK) has provided a unique opportunity to study radionuclides within a real-world system. The core, obtained from a dividing wall and sampled at the fill level of the pond, exhibited radioactivity (dominantly {sup 137}Cs and {sup 90}Sr) heterogeneously distributed across both painted faces. Chemical analysis of the core was undertaken using microfocus spectroscopy at Diamond Light Source, UK. Mapping of Sr across the surface coatings using microfocus X-ray fluorescence (μXRF) combined with X-ray absorption spectroscopy showed that Sr was bound to TiO{sub 2} particles in the paint layers, suggesting an association between TiO{sub 2} and radiostrontium. Stable Sr and Cs sorption experiments using concrete coupons were also undertaken to assess their interactions with the bulk concrete in case of a breach in the coating layers. μXRF and scanning electron microscopy showed that Sr was immobilized by the cement phases, whilst at the elevated experimental concentrations, Cs was associated with clay minerals in the aggregates. This study provides a crucial insight into poorly understood infrastructural contamination in complex systems and is directly applicable to the UK’s nuclear decommissioning efforts.

  8. Development of 32-channel silicon drift detectors and digital electronics for X-ray spectroscopy.

    Science.gov (United States)

    Gauthier, C; Goujon, G; Goulon, J; Moguiline, E; Dressler, P; Henck, R; Lampert, M O

    1998-05-01

    The performance of silicon-drift-detector (SDD) arrays and digital electronics designed for X-ray absorption spectroscopy in the fluorescence excitation mode is reported. Different detectors have been manufactured and tested: two single-channel SDDs with different active areas (10 mm(2) and 1 cm(2)) and a monolithic 2 cm(2) SDD with eight readout anodes. The energy resolution varies between 160 and 170 eV FWHM. A new digital multichannel shaping amplifier has been produced. Its performance is presented in comparison with that of a standard commercial shaper.

  9. A fast energy-dispersive multi-element detector for X-ray absorption spectroscopy.

    Science.gov (United States)

    Welter, Edmund; Hansen, Karsten; Reckleben, Christian; Diehl, Inge

    2009-03-01

    In this paper results are presented from fluorescence-yield X-ray absorption fine-structure spectroscopy measurements with a new seven-cell silicon drift detector (SDD) module. The complete module, including an integrated circuit for the detector readout, was developed and realised at DESY utilizing a monolithic seven-cell SDD. The new detector module is optimized for applications like XAFS which require an energy resolution of approximately 250-300 eV (FWHM Mn Kalpha) at high count rates. Measurements during the commissioning phase proved the excellent performance for this type of application.

  10. Analysis of the Peiting Woman Using Portable X-Ray Fluorescence Spectroscopy

    Directory of Open Access Journals (Sweden)

    Bauerochse, Andreas

    2013-04-01

    Full Text Available Portable X-ray Fluorescence Spectroscopy was applied to the skeletal remains of 13 bog bodies and their bog burial environments. The objective was to create a better understanding of Northern European bog environmental chemistry and its diagenetic effects on interred bog bodies, determine bog body geographic disparity and/or origin, and identify if post-discovery preservation procedures were applied to the bog body remains. This paper summarizes the findings for one of those 13 bog bodies: the Peiting Woman from Bavaria, Germany. The elements analyzed include Antimony, Cobalt, Copper, Iron, Manganese, Molybdenum, Lead, Strontium, Titanium, Zinc, and Zirconium.

  11. X-ray photoelectron spectroscopy study of synchrotron radiation irradiation of a polytetrafluoroethylene surface

    CERN Document Server

    Haruyama, Y; Matsui, S; Ideta, T; Ishigaki, H

    2003-01-01

    The effect of synchrotron radiation (SR) irradiation of a polytetrafluoroethylene (PTFE) surface was investigated using X-ray photoelectron spectroscopy (XPS). After the SR irradiation, the relative intensity of the F ls peak to the C ls peak decreased markedly. The chemical composition ratio to the F atoms to C atoms was estimated to be 0.29. From the curve fitting analysis of C ls and F ls XPS spectra, the chemical components and their intensity ratio were determined. The reason for the chemical composition change by the SR irradiation was discussed. (author)

  12. Observation of Filler Dynamics in Rubber with X-ray Photon Correlation Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Shinohara, Yuya; Maejima, Taketo; Nishikawa, Hisashi; Takata, Masakazu; Amemiya, Yoshiyuki [Department of Advanced Materials Science, Graduate School of Frontier Sciences, University of Tokyo, Kashiwa, Chiba 277-8561 (Japan); Kishimoto, Hiroyuki, E-mail: yuya@k.u-tokyo.ac.jp [Sumitomo Rubber Industries Co. Ltd., Kobe, Hyogo 651-0071 (Japan)

    2011-09-19

    Understanding of the microscopic dynamics of fillers in rubber is a key to understand the property of macroscopic response of filled rubber. In the present study, we observe microscopic dynamics of silica and carbon black nanoparticles in unvulcanized rubber by using X-ray Photon Correlation Spectroscopy (XPCS). Dependence of dynamics on the temperature of sample, the volume fraction of particles and the interface between filler particles and rubber chains is observed. The results clearly show the usefulness of XPCS to investigate the filler dynamics in rubber.

  13. Slow dynamics of nanocomposite polymer aerogels as revealed by X-ray photocorrelation spectroscopy (XPCS)

    Energy Technology Data Exchange (ETDEWEB)

    Hernández, Rebeca, E-mail: rhernandez@ictp.csic.es, E-mail: aurora.nogales@csic.es; Mijangos, Carmen [Instituto de Ciencia y Tecnología de Polímeros, ICTP-CSIC, Juan de la Cierva, 3, 28006 Madrid (Spain); Nogales, Aurora, E-mail: rhernandez@ictp.csic.es, E-mail: aurora.nogales@csic.es; Ezquerra, Tiberio A. [Instituto de Estructura de la Materia, IEM-CSIC, Serrano 121, 28006 Madrid (Spain); Sprung, Michael [Petra III at DESY, Notkestr. 85, 22607 Hamburg (Germany)

    2014-01-14

    We report on a novel slow dynamics of polymer xerogels, aerogels, and nanocomposite aerogels with iron oxide nanoparticles, as revealed by X-ray photon correlation spectroscopy. The polymer aerogel and its nanocomposite aerogels, which are porous in nature, exhibit hyper-diffusive dynamics at room temperature. In contrast, non-porous polymer xerogels exhibit an absence of this peculiar dynamics. This slow dynamical process has been assigned to a relaxation of the characteristic porous structure of these materials and not to the presence of nanoparticles.

  14. X-ray Photoelectron Spectroscopy Investigation on Electrochemical Degradation of Proton Exchange Membrane Fuel Cell Electrodes

    DEFF Research Database (Denmark)

    Andersen, Shuang Ma; Dhiman, Rajnish; Skou, Eivind Morten

    2015-01-01

    X-ray photoelectron spectroscopy studies were systematically carried out on the electrodes before and after the electrochemical stress tests in an aqueous electrolyte at 20 °C and 70 °C. The electrodes have different ionomer structures (no ionomer, only ionomer, physically mixed ionomer and hot...... pressed ionomer) but have identical, commercial catalyst and catalyst loading. A significant degree of carbon corrosion, platinum migration and ionomer degradation were observed in the electrodes after the treatment. The degradation of the ionomer in the electrode is more severe than that of membrane...

  15. Probing interfacial electron dynamics with time-resolved X-ray spectroscopy

    Science.gov (United States)

    Neppl, Stefan

    2015-05-01

    Time-resolved core-level spectroscopy techniques using laser pulses to initiate and short X-ray pulses to probe photo-induced processes have the potential to provide electronic state- and atomic site-specific insight into fundamental electron dynamics at complex interfaces. We describe the implementation of femto- and picosecond time-resolved photoelectron spectroscopy at the Linac Coherent Light Source (LCLS) and at the Advanced Light Source (ALS) in order to follow light-driven electron dynamics at dye-semiconductor interfaces on femto- to nanosecond timescales, and from the perspective of individual atomic sites. A distinct transient binding-energy shift of the Ru3d photoemission lines originating from the metal centers of N3 dye-molecules adsorbed on nanoporous ZnO is observed 500 fs after resonant HOMO-LUMO excitation with a visible laser pulse. This dynamical chemical shift is accompanied by a characteristic surface photo-voltage response of the semiconductor substrate. The two phenomena and their correlation will be discussed in the context of electronic bottlenecks for efficient interfacial charge-transfer and possible charge recombination and relaxation pathways leading to the neutralization of the transiently oxidized dye following ultrafast electron injection. First steps towards in operando time-resolved X-ray absorption spectroscopy techniques to monitor interfacial chemical dynamics will be presented.

  16. Application of ultra-small-angle X-ray scattering / X-ray photon correlation spectroscopy to relate equilibrium or non-equilibrium dynamics to microstructure

    Science.gov (United States)

    Allen, Andrew; Zhang, Fan; Levine, Lyle; Ilavsky, Jan

    2013-03-01

    Ultra-small-angle X-ray scattering (USAXS) can probe microstructures over the nanometer-to-micrometer scale range. Through use of a small instrument entrance slit, X-ray photon correlation spectroscopy (XPCS) exploits the partial coherence of an X-ray synchrotron undulator beam to provide unprecedented sensitivity to the dynamics of microstructural change. In USAXS/XPCS studies, the dynamics of local structures in a scale range of 100 nm to 1000 nm can be related to an overall hierarchical microstructure extending from 1 nm to more than 1000 nm. Using a point-detection scintillator mode, the equilibrium dynamics at ambient temperature of small particles (which move more slowly than nanoparticles) in aqueous suspension have been quantified directly for the first time. Using a USAXS-XPCS scanning mode for non-equilibrium dynamics incipient processes within dental composites have been elucidated, prior to effects becoming detectable using any other technique. Use of the Advanced Photon Source, an Office of Science User Facility operated for the United States Department of Energy (U.S. DOE) Office of Science by Argonne National Laboratory, was supported by the U.S. DOE under Contract No. DE-AC02-06CH11357.

  17. High-resolution X-ray absorption spectroscopy of iron carbonyl complexes.

    Science.gov (United States)

    Atkins, Andrew J; Bauer, Matthias; Jacob, Christoph R

    2015-06-07

    We apply high-energy-resolution fluorescence-detected (HERFD) X-ray absorption near-edge spectroscopy (XANES) to study iron carbonyl complexes. Mono-, bi-, and tri-nuclear carbonyl complexes and pure carbonyl complexes as well as carbonyl complexes containing hydrocarbon ligands are considered. The HERFD-XANES spectra reveal multiple pre-edge peaks with individual signatures for each complex, which could not be detected previously with conventional XANES spectroscopy. These peaks are assigned and analysed with the help of TD-DFT calculations. We demonstrate that the pre-edge peaks can be used to distinguish the different types of iron-iron interactions in carbonyl complexes. This opens up new possibilities for applying HERFD-XANES spectroscopy to probe the electronic structure of iron catalysts.

  18. Combining selective sequential extractions, X-Ray Absorption Spectroscopy, and X-Ray Powder Diffraction for Cu (II speciation in soil and mineral phases

    Directory of Open Access Journals (Sweden)

    Tatiana Minkina

    2017-04-01

    Full Text Available Interaction of Cu (II ions with the matrix of soil and mineral phases of layered silicates was assessed by the Miller method of selective sequential fractionation and a set of synchrotron X-ray methods, including X-ray powder diffraction (XRD and X-ray absorption spectroscopy (XANES. It was shown that the input of Cu into Calcic Chernozem in the form of monoxide (CuO and salt (Cu(NO32 affected the transformation of Cu compounds and their affinity for metal-bearing phases. It was found that the contamination of soil with a soluble Cu(II salt increased the bioavailability of the metal and the role of organic matter and Fe oxides in the fixation and retention of Cu. During the incubation of soil with Cu monoxide, the content of the metal in the residual fractions increased, which was related to the possible entry of Cu in the form of isomorphic impurities into silicates, as well as to the incomplete dissolution of exogenic compounds at the high level of their input into the soil. A mechanism for the structural transformation of minerals was revealed, which showed that ion exchange processes result in the sorption of Cu (II ions from the saturated solution by active sites on the internal surface of the lattice of dioctahedral aluminosilicates. Surface hydroxyls at the octahedral aluminum atom play the main role. X-ray diagnostics revealed that excess Cu(II ions are removed from the system due to the formation and precipitation of coarsely crystalline Cu(NO3(OH3.

  19. Site- and phase-selective x-ray absorption spectroscopy based on phase-retrieval calculation.

    Science.gov (United States)

    Kawaguchi, Tomoya; Fukuda, Katsutoshi; Matsubara, Eiichiro

    2017-03-22

    Understanding the chemical state of a particular element with multiple crystallographic sites and/or phases is essential to unlocking the origin of material properties. To this end, resonant x-ray diffraction spectroscopy (RXDS) achieved through a combination of x-ray diffraction (XRD) and x-ray absorption spectroscopy (XAS) techniques can allow for the measurement of diffraction anomalous fine structure (DAFS). This is expected to provide a peerless tool for electronic/local structural analyses of materials with complicated structures thanks to its capability to extract spectroscopic information about a given element at each crystallographic site and/or phase. At present, one of the major challenges for the practical application of RXDS is the rigorous determination of resonant terms from observed DAFS, as this requires somehow determining the phase change in the elastic scattering around the absorption edge from the scattering intensity. This is widely known in the field of XRD as the phase problem. The present review describes the basics of this problem, including the relevant background and theory for DAFS and a guide to a newly-developed phase-retrieval method based on the logarithmic dispersion relation that makes it possible to analyze DAFS without suffering from the intrinsic ambiguities of conventional iterative-fitting. Several matters relating to data collection and correction of RXDS are also covered, with a final emphasis on the great potential of powder-sample-based RXDS (P-RXDS) to be used in various applications relevant to practical materials, including antisite-defect-type electrode materials for lithium-ion batteries.

  20. Identification of cremains using X-ray diffraction spectroscopy and a comparison to trace element analysis.

    Science.gov (United States)

    Bergslien, Elisa T; Bush, Mary; Bush, Peter J

    2008-03-05

    The ability to distinguish human cremains from filler materials can be important in a variety of situations, the most notorious recent example being the Tri-State Crematorium incident. However, the majority of the papers in the recent literature present methods that rely on trace or minor element analysis, usually followed by a statistical or variable cluster analysis, to determine attribution. This approach is inherently risky, as there is significant natural variation in the trace and minor element body burdens within the human population and no real baseline for comparison. Bones and teeth are a form of calcium phosphate that is part of the mineral group apatite, often referred to as bioapatite. X-ray diffraction (XRD) spectroscopy is a technique that is used to identify minerals by their crystalline structures rather than their elemental composition. The members of the mineral group apatite have a highly flexible hexagonal (6/m) structure that is able to incorporate small amounts of a wide variety of elements. However, its structure, and therefore its X-ray diffraction pattern, is distinct from the crystalline structures of all of the commonly reported filler materials, most of which are composed of some combination of Portland cement, limestone aggregate and quartz sand. XRD has several advantages over other analytical techniques for the identification of cremains. It is non-destructive, requires relatively small amounts of material, is unaffected by the elemental variations found in bioapatite, and can be used to semi-quantify the components of a mixture, thus determining the relative level of contamination of a sample. This paper presents the results of X-ray diffraction spectroscopy analysis of human cremains and a variety of common filler materials.

  1. Multifrequency high precise subTHz-THz-IR spectroscopy for exhaled breath research

    Science.gov (United States)

    Vaks, Vladimir L.; Domracheva, Elena G.; Pripolzin, Sergey I.; Chernyaeva, Mariya B.

    2016-09-01

    Nowadays the development of analytical spectroscopy with high performance, sensitivity and spectral resolution for exhaled breath research is attended. The method of two-frequency high precise THz spectroscopy and the method of high precise subTHz-THz-IR spectroscopy are presented. Development of a subTHz-THz-IR gas analyzer increases the number of gases that can be identified and the reliability of the detection by confirming the signature in both THz and MIR ranges. The testing measurements have testified this new direction of analytical spectroscopy to open widespread trends of its using for various problems of medicine and biology. First of all, there are laboratory investigations of the processes in exhaled breath and studying of their dynamics. Besides, the methods presented can be applied for detecting intermediate and short time living products of reactions in exhaled breath. The spectrometers have been employed for investigations of acetone, methanol and ethanol in the breath samples of healthy volunteers and diabetes patients. The results have demonstrated an increased concentration of acetone in breath of diabetes patients. The dynamic of changing the acetone concentration before and after taking the medicines is discovered. The potential markers of pre-cancer states and oncological diseases of gastrointestinal tract organs have been detected. The changes in the NO concentration in exhaled breath of cancer patients during radiotherapy as well as increase of the NH3 concentration at gastrointestinal diseases have been revealed. The preliminary investigations of biomarkers in three frequency ranges have demonstrated the advantages of the multifrequency high precise spectroscopy for noninvasive medical diagnostics.

  2. Development of a spectro-electrochemical cell for soft X-ray photon-in photon-out spectroscopy

    Science.gov (United States)

    Ishihara, Tomoko; Tokushima, Takashi; Horikawa, Yuka; Kato, Masaru; Yagi, Ichizo

    2017-10-01

    We developed a spectro-electrochemical cell for X-ray absorption and X-ray emission spectroscopy, which are element-specific methods to study local electronic structures in the soft X-ray region. In the usual electrochemical measurement setup, the electrode is placed in solution, and the surface/interface region of the electrode is not normally accessible by soft X-rays that have low penetration depth in liquids. To realize soft X-ray observation of electrochemical reactions, a 15-nm-thick Pt layer was deposited on a 150-nm-thick film window with an adhesive 3-nm-thick Ti layer for use as both the working electrode and the separator window between vacuum and a sample liquid under atmospheric pressure. The designed three-electrode electrochemical cell consists of a Pt film on a SiC window, a platinized Pt wire, and a commercial Ag|AgCl electrode as the working, counter, and reference electrodes, respectively. The functionality of the cell was tested by cyclic voltammetry and X-ray absorption and emission spectroscopy. As a demonstration, the electroplating of Pb on the Pt/SiC membrane window was measured by X-ray absorption and real-time monitoring of fluorescence intensity at the O 1s excitation.

  3. Surface functional group characterization using chemical derivatization X-ray photoelectron spectroscopy (CD-XPS)

    Energy Technology Data Exchange (ETDEWEB)

    Jagst, Eda

    2011-03-18

    Chemical derivatization - X-ray photolectron spectroscopy (CD-XPS) was applied successfully in order to determine different functional groups on thin film surfaces. Different amino group carrying surfaces, prepared by spin coating, self-assembly and plasma polymerization, were successfully investigated by (XPS) and near edge X-ray absorption fine structure (NEXAFS) spectroscopy. Amino groups were derivatized with the widely used primary amino group tags, pentafluorobenzaldehyde (PFB) and 4-(trifluoromethyl)-benzaldehyde (TFBA), prior to analysis. Primary amino group quantification was then carried out according to the spectroscopical data. Self-assembled monolayers (SAMs) of different terminal groups were prepared and investigated with XPS and spectra were compared with reference surfaces. An angle resolved NEXAFS measurement was applied to determine the orientation of SAMs. Plasma polymerized allylamine samples with different duty cycle, power and pressure values were prepared in order to study the effects of external plasma parameters on the primary amino group retention. CD-XPS was used to quantify the amino groups and experiments show, that the milder plasma conditions promote the retention of amino groups originating from the allylamine monomer. An interlaboratory comparison of OH group determination on plasma surfaces of polypropylene treated with oxygen plasma, was studied. The surfaces were investigated with XPS and the [OH] amount on the surfaces was calculated. (orig.)

  4. In situ X-ray photoelectron spectroscopy study of complex oxides under gas and vacuum environments

    Science.gov (United States)

    Paloukis, F.; Papazisi, K. M.; Balomenou, S. P.; Tsiplakides, D.; Bournel, F.; Gallet, J.-J.; Zafeiratos, S.

    2017-11-01

    For several decades an open question in many X-ray photoelectron spectroscopy (XPS) studies was whether or not the results obtained in ultra-high vacuum conditions (UHV) were representative of the sample state in gas atmospheres. As a consequence, near ambient pressure X-ray photoelectron spectroscopy (NAP-XPS) was received by surface scientists as an important tool for in situ characterization of the gas-solid interactions. However, it is not yet clear how, if at all, the surface state formed in contact with the gas is modified when this gas is evacuated. In this work we compare synchrotron-based XPS results recorded at 300 °C on Ni/yttria- stabilized zirconia cermet and La0.75Sr0.25Cr0.9Fe0.1O3 perovskite, under 3.5 mbar O2 and UHV environments. We found that the surface state formed in O2 is maintained to a large extent under vacuum. In addition, we demonstrate that the correlation of XPS spectra recorded in the two conditions can provide information regarding the electrical conductivity of the specific surface sites of these complex oxides. Our findings suggest that comparison of XPS measurements in gas and in vacuum environments might be particularly useful in applications where the electronic conductivity at the surface plays a crucial role, as for example in solid oxide electrochemical devices.

  5. X-ray Fluorescence Spectroscopy of Pre-Federal American Currency

    Science.gov (United States)

    Raddell, Mark; Manukyan, Khachatur; Aprahamian, Ani; Wiescher, Michael; Jordan, Louis

    2017-09-01

    X-ray Fluorescence Spectroscopy (XRF) was used to study 17th and 18th century Mexican, Potosí, and Massachusetts silver colonial coins from the University of Notre Dame's Rare Books and Special Collections. Using different configurations and devices, we have learned more about the limitations and optimizations of the method. We have developed a moveable stand that may be used for XRF mapping of coin surfaces. We created standard silver alloy materials for quantification of the elemental composition of the coins. Inductively coupled plasma (ICP) spectroscopy was applied to determine the precise composition of the standards for accurate and non-destructive analyses of the colonial coins. XRF measurements were performed using two different XRF spectrometers, in both air and vacuum conditions, as well as an x-ray beam tube of varying diameters from 2 mm, 1 mm, and 0.03 mm. We quantified both the major elements and the bulk and surface impurities for 90 coins. We are using PCA to look at possible correlations between compositions of coinage from different geographical regions. Preliminary data analyses suggest that Massachusetts coins were minted using silver from Latin American sources. These results are of great interest to historians in tracing the origins of the currency. This work was made possible by the Notre Dame College of Science Summer Undergraduate Research Fellowships (COS-SURF).

  6. Post-mortem analysis of radiation grafted fuel cell membrane using X-ray photoelectron spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Nasef, M. M. [Technological University PETRONAS, Chemical Engineering Program, Perak (Malaysia); Saidi, H. [Technological University of Malaysia, Membrane Research Unit, Kuala Lumpur (Malaysia)

    2002-07-01

    Post-mortem analysis of poly(tetrafluoroethylene-co-perfluorovinyl ether)-graft-polystyrene sulfonic acid (PFAS-g-PSSA) membrane was carried out at the end of a polymer electrolyte membrane (PEM) fuel cell test using X-ray photoelectron spectroscopy. The data obtained when the membrane was initially analyzed in its virgin state was used as a reference. Substantial structural changes were shown by the X-ray photoelectron spectroscopy, especially in terms of chemical composition and the concentration of its basic elemental components. The used membrane was found to have no sulfur and less oxygen compared to the virgin one, providing strong evidence for the complete elimination of the sulfonic acid groups from the membrane. Overall, the results suggests that membrane oxidative degradation during PEM fuel cell test is due to the decomposition of sulfonated polystyrene located in the hydrocarbon fraction. The chemical attack mostly occurs on the vulnerable tertiary hydrogen of the alpha-carbon causing a termination of the whole sulfonated polystyrene grafts. 22 refs., 7 figs.

  7. X-ray absorption spectroscopy investigation of structurally modified lithium niobate crystals

    Energy Technology Data Exchange (ETDEWEB)

    Vitova, Tonya

    2008-02-15

    The type and concentration of impurity centers in different valence states are crucial for tuning the photorefractive properties of doped Lithium Niobate (LN) crystals. X-ray Absorption Spectroscopy (XAS) is an appropriate tool for studying the local structure of impurity centers. XAS combined with absorption in UV/VIS/IR and High Resolution X-ray Emission Spectroscopy (HRXES) provide information about the valence state of the dopant ions in as-grown, reduced or oxidized doped LN crystals. Cu (Cu{sup 1+} and Cu{sup 2+}) and Fe (Fe{sup 2+} and Fe{sup 3+}) atoms are found in two different valence states, whereas there are indications for a third Mn valency, in addition to Mn{sup 2+} and Mn{sup 3+} in manganese-doped LN crystals. One of the charge compensation mechanisms during reduction of copper- doped LN crystals is outgassing of oxygen atoms. Cu ions in the reduced crystals have at least two different site symmetries: twofold (Cu{sup 1+}) and sixfold (Cu{sup 2+}) coordinated by O atoms. Fe and Mn atoms are coordinated by six O atoms. Cu and Fe ions are found to occupy only Li sites, whereas Mn ions are also incorporated into Li and Nb sites. The refractive index change in LN crystals irradiated with {sup 3}He{sup 2+} ions is caused by structurally disordered centers, where Nb atoms are displaced from normal crystallographic sites and Li or/and O vacancies are present. (orig.)

  8. Characterization of the Roraima savanna across of X-ray diffraction, thermomagnetic analysis and Moessbauer spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Gilmar A.; Araujo, R.C.; Sergio, C.S. [Universidade Federal de Roraima (UFRR), Boa Vista, RR (Brazil)

    2012-07-01

    Full text: The technique of X-ray diffraction has great resolving power to determine the phases present in crystalline material, thereby enabling it to determine the elements present in the materials as well as changes in structure that they can suffer when subjected to various physical processes and/or chemical means. The research had as objective to characterize the mineralogy of iron oxides, silicon, aluminum and other minerals in the soil of five points of the Roraima savannah. The points where samples were collected are five municipalities in the state of Roraima. The area of sampling is part of the savanna in Roraima. The samples were collected. We analyzed samples from five points from the collection of natural soil in the locations listed. The samples were placed in a mill to a uniform grain size. After the milling process, the magnetic material was separated using a permanent magnet. Then the samples were analyzed by x-ray diffraction, thermomagnetic analysis and Moessbauer spectroscopy. Preliminary results of XRD showed the occurrence of phases of oxides of iron, silicon, aluminum and other phases less. Thermomagnetic analysis show that the magnetic phases are magnetite and hematite. The results of the Moessbauer spectroscopy indicates the reliability in the two prior art and confirmed the presence of the phases of oxides of iron present in the soil analyzed. (author)

  9. FTIR spectroscopy and X-ray powder diffraction characterization of microcrystalline cellulose obtained from alfa fibers

    Directory of Open Access Journals (Sweden)

    Trache D.

    2013-07-01

    Full Text Available Many cereal straws have been used as raw materials for the preparation of microcrystalline cellulose (MCC. These raw materials were gradually replaced with wood products; nevertheless about 10% of the world overall pulp production is obtained from non-wood raw material. The main interest in pulp made from straw is that it provides excellent fibres for different industries with special properties, and that it is the major available source of fibrous raw material in some geographical areas. The aim of the present work was to characterize microcrystalline cellulose prepared from alfa fibers using the hydrolysis process. The products obtained are characterized with FTIR spectroscopy and X-ray powder diffraction. As a result, FTIR spectroscopy is an appropriate technique for studying changes occurred by any chemical treatment. The spectrum of alfa grass stems shows the presence of lignin and hemicelluloses. However, the cellulose spectrum indicates that the extraction of lignin and hemicellulose was effective. The X-ray analysis indicates that the microcrystalline cellulose is more crystalline than the source material.

  10. A flexible gas flow reaction cell for in situ x-ray absorption spectroscopy studies

    Energy Technology Data Exchange (ETDEWEB)

    Kroner, Anna B., E-mail: anna.kroner@diamond.ac.uk; Gilbert, Martin; Duller, Graham; Cahill, Leo; Leicester, Peter; Woolliscroft, Richard; Shotton, Elizabeth J. [Diamond Light Source Ltd., Diamond House, Harwell Science and Innovation Campus, Chilton, Oxfordshire, OX110DE (United Kingdom); Mohammed, Khaled M. H. [UK Catalysis Hub, Research Complex at Harwell, Rutherford Appleton Laboratory, Chilton, Oxfordshire, OX110FA (United Kingdom); School of Chemistry, University of Southampton, Southampton, SO17 1BJ (United Kingdom)

    2016-07-27

    A capillary-based sample environment with hot air blower and integrated gas system was developed at Diamond to conduct X-ray absorption spectroscopy (XAS) studies of materials under time-resolved, in situ conditions. The use of a hot air blower, operating in the temperature range of 298-1173 K, allows introduction of other techniques e.g. X-ray diffraction (XRD), Raman spectroscopy for combined techniques studies. The flexibility to use either quartz or Kapton capillaries allows users to perform XAS measurement at energies as low as 5600 eV. To demonstrate performance, time-resolved, in situ XAS results of Rh catalysts during the process of activation (Rh K-edge, Ce L{sub 3}-edge and Cr K-edge) and the study of mixed oxide membrane (La{sub 0.6}Sr{sub 0.4}Co{sub 0.2}Fe{sub 0.8}O{sub 3−δ}) under various partial oxygen pressure conditions are described.

  11. Characterising legacy spent nuclear fuel pond materials using microfocus X-ray absorption spectroscopy.

    Science.gov (United States)

    Bower, W R; Morris, K; Mosselmans, J F W; Thompson, O R; Banford, A W; Law, K; Pattrick, R A D

    2016-11-05

    Analysis of a radioactive, coated concrete core from the decommissioned, spent nuclear fuel cooling pond at the Hunterston-A nuclear site (UK) has provided a unique opportunity to study radionuclides within a real-world system. The core, obtained from a dividing wall and sampled at the fill level of the pond, exhibited radioactivity (dominantly (137)Cs and (90)Sr) heterogeneously distributed across both painted faces. Chemical analysis of the core was undertaken using microfocus spectroscopy at Diamond Light Source, UK. Mapping of Sr across the surface coatings using microfocus X-ray fluorescence (μXRF) combined with X-ray absorption spectroscopy showed that Sr was bound to TiO2 particles in the paint layers, suggesting an association between TiO2 and radiostrontium. Stable Sr and Cs sorption experiments using concrete coupons were also undertaken to assess their interactions with the bulk concrete in case of a breach in the coating layers. μXRF and scanning electron microscopy showed that Sr was immobilized by the cement phases, whilst at the elevated experimental concentrations, Cs was associated with clay minerals in the aggregates. This study provides a crucial insight into poorly understood infrastructural contamination in complex systems and is directly applicable to the UK's nuclear decommissioning efforts. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

  12. STROBE-X: X-ray Timing & Spectroscopy on Dynamical Timescales from Microseconds to Years

    Science.gov (United States)

    Ray, Paul; Wilson-Hodge, Colleen; Gendreau, Keith; Chakrabarty, Deepto; Feroci, Marco; Maccarone, Thomas; Arzoumanian, Zaven; Remillard, Ron; Wood, Kent; Griffith, Chris; Strobe-X Collaboration

    2017-01-01

    We describe a proposed probe-class mission concept that will provide an unprecedented view of the X-ray sky, performing timing and spectroscopy over a broad band (0.2-30 keV) probing timescale from microseconds to years. The Spectroscopic Time-Resolving Observatory for Broadband Energy X-rays (STROBE-X) comprises two primary instruments, one based on technology developed for the NICER mission and the other based on the European LOFT mission. The broad coverage will enable thermal components, non-thermal components, iron lines, and reflection features to be studied simultaneously from a single platform for the first time in accreting black holes at all scales. The massive collecting area will enable studies of the dense matter equation of state using multiple techniques. A broad range of other revolutionary science, such as high quality spectroscopy of clusters of galaxies and unprecedented timing investigations of active galactic nuclei, would also be obtained. We describe the mission concept and the planned trade studies that will optimize the mission to maximize the science return. This mission is being developed in collaboration with members of the European LOFT team, and a hardware contribution from Europe is expected.

  13. X-ray Absorption Spectroscopy Unveils the Formation of Gold Nanoparticles in Corn X-ray Absorption Spectroscopy Unveils the Formation of Gold Nanoparticles in Corn

    Directory of Open Access Journals (Sweden)

    Gustavo Cruz-Jiménez

    2012-02-01

    Full Text Available En este estudio se determinó, mediante espectroscopía de absorción de rayos-X, la posible biotransformación de oro en maíz (variedad Golden que se germinó y creció en KAuCl4. Adicionalmente se investigó el efecto de la tiourea y el tiocianato de amonio en la absorción de oro por la planta de maíz. Los resultados indicaron que concentraciones menores a 160 mg Au/L, no afectaron la germinación o el crecimiento de las plántulas. Tanto la tiourea como el tiocianato de amonio incrementaron 6 veces el contenido de oro en las raíces, mientras que la tiourea provocó un incremento de 10 veces la concentración de oro en tallos con respecto a los tratamientos sin este compuesto. El 91% del oro en el maíz se encontró como Au(0 y el resto como Au(III. Los análisis de estructura fi na revelaron que el oro se encontraba con un número de coordinación de 9,5 aproximadamente a 2,86 Å, indicando una esfera de coordinación incompleta, lo cual implica la presencia de una nano-fase. Usando la ecuación de Borowski se determinó que las nanopartículas tenían un tamaño promedio de 10,36 nm.In this study, X-ray absorption spectroscopy was used to determine the possible gold biotransformation by Zea mays (corn var. Golden, germinated and grown in a medium spikedwith KAuCl4. In addition, the gold uptake capacity of corn assisted by thiourea and ammoniumthiocyanate was investigated. Results showed that up to 160 mg/L, gold did no treduce corn seed germination or plant growth. Both thiourea and ammonium thiocyanateresulted in a 6-fold increase of gold concentration in roots and thiourea promoted a 10-fold increase of gold concentration in shoots. X-ray absorption near edge structure studies demonstrated that approximately 91% of the gold present in plant samples was Au(0. Theremaining 9% was present as Au(III. In addition, extended X-ray absorption fi ne structureresults showed that in corn roots, the gold coordination number was around 9

  14. Correlated single-crystal electronic absorption spectroscopy and X-ray crystallography at NSLS beamline X26-C.

    Science.gov (United States)

    Orville, Allen M; Buono, Richard; Cowan, Matt; Héroux, Annie; Shea-McCarthy, Grace; Schneider, Dieter K; Skinner, John M; Skinner, Michael J; Stoner-Ma, Deborah; Sweet, Robert M

    2011-05-01

    The research philosophy and new capabilities installed at NSLS beamline X26-C to support electronic absorption and Raman spectroscopies coupled with X-ray diffraction are reviewed. This beamline is dedicated full time to multidisciplinary studies with goals that include revealing the relationship between the electronic and atomic structures in macromolecules. The beamline instrumentation has been fully integrated such that optical absorption spectra and X-ray diffraction images are interlaced. Therefore, optical changes induced by X-ray exposure can be correlated with X-ray diffraction data collection. The installation of Raman spectroscopy into the beamline is also briefly reviewed. Data are now routinely generated almost simultaneously from three complementary types of experiments from the same sample. The beamline is available now to the NSLS general user population.

  15. Applications and results of X-ray spectroscopy in implosion experiments on the National Ignition Facility

    Science.gov (United States)

    Epstein, R.; Regan, S. P.; Hammel, B. A.; Suter, L. J.; Scott, H. A.; Barrios, M. A.; Bradley, D. K.; Callahan, D. A.; Cerjan, C.; Collins, G. W.; Dixit, S. N.; Döppner, T.; Edwards, M. J.; Farley, D. R.; Fournier, K. B.; Glenn, S.; Glenzer, S. H.; Golovkin, I. E.; Hamza, A.; Hicks, D. G.; Izumi, N.; Jones, O. S.; Key, M. H.; Kilkenny, J. D.; Kline, J. L.; Kyrala, G. A.; Landen, O. L.; Ma, T.; MacFarlane, J. J.; Mackinnon, A. J.; Mancini, R. C.; McCrory, R. L.; Meyerhofer, D. D.; Meezan, N. B.; Nikroo, A.; Park, H.-S.; Patel, P. K.; Ralph, J. E.; Remington, B. A.; Sangster, T. C.; Smalyuk, V. A.; Springer, P. T.; Town, R. P. J.; Tucker, J. L.

    2017-03-01

    hot-spot continuum in the shell. These features provide diagnostics of the central hot spot and the compressed shell, plus a measure of the shell mass that has mixed into the hot spot [S. P. Regan et al., Phys. Plasmas 19, 056307 (2012)] and evidence locating the origin of the mixed shell mass in the imploding ablator [S. P. Regan et al., Phys. Rev. Lett. 111, 045001 (2013)]. Spectra are analyzed and interpreted using detailed atomic models (including radiation-transport effects) to determine the characteristic temperatures, densities, and sizes of the emitting regions. A mix diagnostic based on enhanced continuum x-ray production, relative to neutron yield, provides sensitivity to the undoped shell material mixed into the hot spot [T. Ma et al., Phys. Rev. Lett., 111, 085004 (2013)]. Together, these mix-mass measurements confirm that mix is a serious impediment to ignition. The spectroscopy and atomic physics of shell dopants have become essential in confronting this impediment and will be described.

  16. STROBE-X: X-Ray Timing Spectroscopy on Dynamical Timescales from Microseconds to Years

    Science.gov (United States)

    Wilson-Hodge, Colleen A.; Ray, P. S.; Gendreau, K.; Arzoumanian, Z.; Chakrabarty, D.; Remillard, R.; Feroci, M.; Maccarone, T.; Wood, K.; Jenke, P.

    2017-01-01

    We describe a probe-class mission concept that provides an unprecedented view of the X-ray sky, performing timing and 0.2-30 keV spectroscopy over timescales from microseconds to years. The Spectroscopic Time-Resolving Observatory for Broadband Energy X-rays (STROBE-X) comprises three primary instruments. The first uses an array of lightweight optics (3-m focal length) that concentrate incident photons onto solid state detectors with CCD-level (85-130 eV) energy resolution, 100 ns time resolution, and low background rates to cover the 0.2-12 keV band. This technology is scaled up from NICER, with enhanced optics to take advantage of the longer focal length of STROBE-X. The second uses large-area collimated silicon drift detectors, developed for ESA's LOFT, to cover the 2-30 keV band. These two instruments each provide an order of magnitude improvement in effective area compared with its predecessor (NICER and RXTE, respectively). Finally, a sensitive sky monitor triggers pointed observations, provides high duty cycle, high time resolution, high spectral resolution monitoring of the X-ray sky with approx. 20 times the sensitivity of the RXTE ASM, and enables multi-wavelength and multi-messenger studies on a continuous, rather than scanning basis.For the first time, the broad coverage provides simultaneous study of thermal components, non-thermal components, iron lines, and reflection features from a single platform for accreting black holes at all scales. The enormous collecting area allows detailed studies of the dense matter equation of state using both thermal emission from rotation-powered pulsars and harder emission from X-ray burst oscillations. The combination of the wide-field monitor and the sensitive pointed instruments enables observations of potential electromagnetic counterparts to LIGO and neutrino events. Additional extragalactic science, such as high quality spectroscopy of clusters of galaxies and unprecedented timing investigations of active

  17. Silicon drift detectors with on-chip electronics for x-ray spectroscopy.

    Science.gov (United States)

    Fiorini, C; Longoni, A; Hartmann, R; Lechner, P; Strüder, L

    1997-01-01

    The silicon drift detector (SDD) is a semiconductor device based on high resistivity silicon fully depleted through junctions implanted on both sides of the semiconductor wafer. The electrons generated by the ionizing radiation are driven by means of a suitable electric field from the point of interaction toward a collecting anode of small capacitance, independent of the active area of the detector. A suitably designed front-end JFET has been directly integrated on the detector chip close to the anode region, in order to obtain a nearly ideal capacitive matching between detector and transistor and to minimize the stray capacitances of the connections. This feature allows it to reach high energy resolution also at high count rates and near room temperature. The present work describes the structure and the performance of SDDs specially designed for high resolution spectroscopy with soft x rays at high detection rate. Experimental results of SDDs used in spectroscopy applications are also reported.

  18. X-Ray Fluorescence and Laser-Induced Breakdown Spectroscopy analysis of Roman silver denarii

    Science.gov (United States)

    Pardini, L.; El Hassan, A.; Ferretti, M.; Foresta, A.; Legnaioli, S.; Lorenzetti, G.; Nebbia, E.; Catalli, F.; Harith, M. A.; Diaz Pace, D.; Anabitarte Garcia, F.; Scuotto, M.; Palleschi, V.

    2012-08-01

    In this paper we present the results of a study performed on a large collection of silver Roman republican denarii, encompassing about two centuries of history. The joint use of Laser-Induced Breakdown Spectroscopy (LIBS) and X-Ray Fluorescence (XRF) spectroscopy allowed for an accurate determination of the coins' elemental composition; the measurements, performed mostly in situ at the 'Monetiere' in Florence, revealed a striking connection between the 'quality' of the silver alloy and some crucial contemporary events. This finding was used to classify a group of denarii whose dating was otherwise impossible. The comparison with other contemporary denarii disproves a recent theory on the origin of the so called 'serrated' denarii (denarii showing notched chisel marks on the edge of the coin).

  19. Design of solar cell materials via soft X-ray spectroscopy

    DEFF Research Database (Denmark)

    Himpsel, F.J.; Cook, P.L.; de la Torre, G.

    2013-01-01

    to an oxide acceptor. The bridge to device fabrication is crossed by correlating spectroscopic features with the photocurrent in hematite photoanodes for water splitting. For speeding up the development of new materials and designs of solar cells a feedback loop between spectroscopy, theory, synthesis......This overview illustrates how spectroscopy with soft X-rays can assist the development of new materials and new designs for solar cells. The starting point is the general layout of a solar cell, which consists of a light absorber sandwiched between an electron donor and an electron acceptor......) as a function of the metal atom are presented for the metal 2p and N 1s absorption edges. In combination with density functional theory one can discern trends that are useful for tailoring absorber molecules. A customized porphyrin molecule is investigated that combines an absorber with a donor and a linker...

  20. Determination of electronic and atomic properties of surface, bulk and buried interfaces: Simultaneous combination of hard X-ray photoelectron spectroscopy and X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Rubio-Zuazo, J., E-mail: rubio@esrf.fr [SpLine, Spanish CRG BM25 Beamline at the ESRF, ESRF, B.P. 220, F-38043 Grenoble (France); Instituto de Ciencia de Materiales de Madrid, ICMM, CSIC, Cantoblanco, E-28049 Madrid (Spain); Castro, G.R. [SpLine, Spanish CRG BM25 Beamline at the ESRF, ESRF, B.P. 220, F-38043 Grenoble (France); Instituto de Ciencia de Materiales de Madrid, ICMM, CSIC, Cantoblanco, E-28049 Madrid (Spain)

    2013-10-15

    Highlights: •We have developed a novel and exceptional tool for non-destructive characterization of bulk and buried interfaces that combine XRD and HAXPES. •We studied the correlation between the atomic, electronic and transport properties of oxygen deficient manganite thin films. •The diffraction data showed a cooperative tilt of the MnO{sub 6} block along the out-of-plane direction. •We shown the absence of the conventional basal plane rotation for the oxygen deficient samples. -- Abstract: Hard X-ray photoelectron spectroscopy (HAXPES) is a powerful novel emerging technique for bulk compositional, chemical and electronic properties determination in a non-destructive way. It benefits from the exceptionally large escape depth of high kinetic energy photoelectrons enabling the study of bulk and buried interfaces up to several tens of nanometres depth. Its advantage over conventional XPS is based on the long mean free path of high kinetic energetic photoelectrons. Using the advantage of tuneable X-ray radiation provided by synchrotron sources the photoelectron kinetic energy, i.e. the information depth can be changed and consequently electronic and compositional depth profiles can be obtained. The combination of HAXPES with an atomic structure sensitive technique, as X-ray diffraction, opens a new research field with great potential for many systems in which their electronic properties are intimately linked to their crystallographic structure. At SpLine, the Spanish CRG Beamline at the European Synchrotron Radiation Facility (ESRF) we have developed a novel and exceptional set-up that combine grazing incidence X-ray diffraction (GIXRD) and HAXPES. Both techniques can be operated simultaneously on the same sample and using the same excitation source. The set-up includes a heavy 2S+3D diffractometer and UHV chamber equipped with an electrostatic analyzer. The UHV chamber has also MBE evaporation sources, an ion gun, a LEED optic, a sample heating and cooling

  1. X-ray Absorption Spectroscopy Characterization of Electrochemical Processes in Renewable Energy Storage and Conversion Devices

    Energy Technology Data Exchange (ETDEWEB)

    Farmand, Maryam [George Washington Univ., Washington, DC (United States)

    2013-05-19

    The development of better energy conversion and storage devices, such as fuel cells and batteries, is crucial for reduction of our global carbon footprint and improving the quality of the air we breathe. However, both of these technologies face important challenges. The development of lower cost and better electrode materials, which are more durable and allow more control over the electrochemical reactions occurring at the electrode/electrolyte interface, is perhaps most important for meeting these challenges. Hence, full characterization of the electrochemical processes that occur at the electrodes is vital for intelligent design of more energy efficient electrodes. X-ray absorption spectroscopy (XAS) is a short-range order, element specific technique that can be utilized to probe the processes occurring at operating electrode surfaces, as well for studying the amorphous materials and nano-particles making up the electrodes. It has been increasingly used in recent years to study fuel cell catalysts through application of the and #916; and mgr; XANES technique, in combination with the more traditional X-ray Absorption Near Edge Structure (XANES) and Extended X-ray Absorption Fine Structure (EXAFS) techniques. The and #916; and mgr; XANES data analysis technique, previously developed and applied to heterogeneous catalysts and fuel cell electrocatalysts by the GWU group, was extended in this work to provide for the first time space resolved adsorbate coverages on both electrodes of a direct methanol fuel cell. Even more importantly, the and #916; and mgr; technique was applied for the first time to battery relevant materials, where bulk properties such as the oxidation state and local geometry of a cathode are followed.

  2. Development of an X-ray delay unit for correlation spectroscopy and pump-probe experiments

    Energy Technology Data Exchange (ETDEWEB)

    Roseker, Wojciech

    2008-07-15

    Probing condensed matter on time scales ranging from femtoseconds to nanoseconds will be one of the key topics for future X-ray Free Electron Laser (XFEL) sources. The accessible time windows are, however, compromised by the intrinsic time structure of the sources. One way to overcome this limitation is the usage of a time delay unit. A prototype device capable of splitting an X-ray pulse into two adjustable fractions, delaying one of them with the aim to perform X-ray Photon Correlation Spectroscopy and pump-probe type studies was designed and manufactured. The device utilizes eight perfect crystals in vertical 90 scattering geometry. Its performance has been verified with 8.39 keV and 12.4 keV Xrays at various synchrotron sources. The measured throughput of the device with a Si(333) monochromator at 8.39 keV under ambient conditions is 0.6%. The stability was verified at 12.4 keV and operation without realignment and feedback was possible for more than 30 minutes. Time delays up to 2.95 ns have been achieved. The highest resolution achieved in an experiment was 15.4 ps, a value entirely determined by the diagnostics system. The influence of the delay unit optics on the coherence properties of the beam was investigated by means of Fraunhofer diffraction and static speckle analysis. The obtained high fringe visibility and contrast values larger than 23% indicate the feasibility of performing coherence based experiments with the delay line. (orig.)

  3. Spatially Resolved X-ray Spectroscopy of the Large Magellanic Cloud Supernova Remnant N132D

    Science.gov (United States)

    Plucinsky, Paul; Sharda, Piyush; Gaetz, Terrance; Kashyap, Vinay

    2018-01-01

    We perform detailed X-ray spectroscopy of the brightest Supernova Remnant (SNR), N132D, in the Large Magellanic Cloud (LMC) using observations taken by the Advanced CCD Imaging Spectrometer (ACIS) on the Chandra X-ray Observatory (Chandra). By studying the spectra of regions on the well-defined rim running from NW to NE, we determine an average abundance set for O, Ne, Mg, Si, S and Fe for the local LMC environment. We note that the elements other than Fe and Ne show significant trends across this region, implying they cannot be approximated by a single, constant value. We characterize the blast wave properties and find a simple plane parallel shock model is sufficient to explain the X-ray spectrum of the forward shock moving into ambient LMC material, with a shock velocity near 800 km/s and a shock age of 600-1100 years. We find evidence of enhanced Si near the western blast wave which would imply an asymmetric explosion. We fit a region near the central, optical O-rich knots which exhibits enhanced abundances of O, Ne, Mg, Si, and Fe. Comparison to nucleosynthesis models of the ratios of these elements indicates a progenitor mass of 28-35 solar masses, consistent with most previous estimates. Lastly, we find an intriguing presence of a very hot plasma with a temperature of ~4.5 keV (assuming a non-equilibrium ionization model) to explain the Fe-K emission which is centrally concentrated in the lower half of the remnant.

  4. Band gap opening in strongly compressed diamond observed by x-ray energy loss spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Gamboa, E. J. [SLAC National Accelerator Lab., Menlo Park, CA (United States); Fletcher, L. B. [SLAC National Accelerator Lab., Menlo Park, CA (United States); Lee, H. J. [SLAC National Accelerator Lab., Menlo Park, CA (United States); MacDonald, M. J. [SLAC National Accelerator Lab., Menlo Park, CA (United States); Univ. of Michigan, Ann Arbor, MI (United States); Zastrau, U. [High-Energy Density Science Group, Hamburg (Germany); Gauthier, M. [SLAC National Accelerator Lab., Menlo Park, CA (United States); Gericke, D. O. [Univ. of Warwick (United Kingdom); Vorberger, J. [Helmholtz Association of German Research Centres, Dresden (Germany); Granados, E. [SLAC National Accelerator Lab., Menlo Park, CA (United States); Hastings, J. B. [SLAC National Accelerator Lab., Menlo Park, CA (United States); Glenzer, S. H. [SLAC National Accelerator Lab., Menlo Park, CA (United States)

    2016-01-25

    The extraordinary mechanical and optical properties of diamond are the basis of numerous technical applications and make diamond anvil cells a premier device to explore the high-pressure behavior of materials. However, at applied pressures above a few hundred GPa, optical probing through the anvils becomes difficult because of the pressure-induced changes of the transmission and the excitation of a strong optical emission. Such features have been interpreted as the onset of a closure of the optical gap in diamond, and can significantly impair spectroscopy of the material inside the cell. In contrast, a comparable widening has been predicted for purely hydrostatic compressions, forming a basis for the presumed pressure stiffening of diamond and resilience to the eventual phase change to BC8. We here present the first experimental evidence of this effect at geo-planetary pressures, exceeding the highest ever reported hydrostatic compression of diamond by more than 200 GPa and any other measurement of the band gap by more than 350 GPa. We here apply laser driven-ablation to create a dynamic, high pressure state in a thin, synthetic diamond foil together with frequency-resolved x-ray scattering as a probe. The frequency shift of the inelastically scattered x-rays encodes the optical properties and, thus, the behavior of the band gap in the sample. Using the ultra-bright x-ray beam from the Linac Coherent Light Source (LCLS), we observe an increasing direct band gap in diamond up to a pressure of 370 GPa. This finding points to the enormous strains in the anvils and the impurities in natural Type Ia diamonds as the source of the observed closure of the optical window. Our results demonstrate that diamond remains an insulating solid to pressures approaching its limit strength.

  5. Resonant inelastic scattering in dilute magnetic semiconductors by x-ray fluorescence spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Lawniczak-Jablonska, K. [Lawrence Berkeley National Lab., CA (United States)]|[Institute of Physics, Warsaw (Poland); Jia, J.J.; Underwood, J.H. [Lawrence Berkeley National Lab., CA (United States)] [and others

    1997-04-01

    As modern, technologically important materials have become more complex, element specific techniques have become invaluable in studying the electronic structure of individual components from the system. Soft x-ray fluorescence (SXF) and absorption (SXA) spectroscopies provide a unique means of measuring element and angular momentum density of electron states, respectively, for the valence and conducting bands in complex materials. X-ray absorption and the decay through x-ray emission are generally assumed to be two independent one-photon processes. Recent studies, however have demonstrated that SXF excited near the absorption threshold generate an array of spectral features that depend on nature of materials, particularly on the localization of excited states in s and d-band solids and that these two processes can no be longer treated as independent. Resonant SXF offers thus the new way to study the dynamics of the distribution of electronic valence states in the presence of a hole which is bound to the electron low lying in the conduction band. This process can simulate the interaction between hole-electron pair in wide gap semiconductors. Therefore such studies can help in understanding of transport and optics phenomena in the wide gap semiconductors. The authors report the result of Mn and S L-resonant emission in Zn{sub 1{minus}x}Mn{sub x}S (with x=0.2 and 0.3) and MnS as the energy of exciting radiation is tuned across the Mn and S L{sub 3,2} absorption edge, along with the resonant excited spectra from elemental Mn as a reference.

  6. STROBE-X: X-ray Timing & Spectroscopy on Dynamical Timescales from Microseconds to Years

    Science.gov (United States)

    Wilson-Hodge, Colleen A.; Ray, Paul S.; Maccarone, Thomas J.; Chakrabarty, Deepto; Gendreau, Keith C.; Arzoumanian, Zaven; Jenke, Peter; Ballantyne, David; Bozzo, Enrico; Brandt, Soren; Brenneman, Laura; Christophersen, Marc; DeRosa, Alessandra; Feroci, Marco; Goldstein, Adam; Hartmann, Dieter; Hernanz, Margarita; McDonald, Michael; Phlips, Bernard; Remillard, Ronald; Stevens, Abigail; Tomsick, John; Watts, Anna; Wood, Kent S.; Zane, Silvia; STROBE-X Collaboration

    2018-01-01

    We describe a probe-class mission concept that provides an unprecedented view of the X-ray sky, performing timing and 0.2-30 keV spectroscopy over timescales from microseconds to years. The Spectroscopic Time-Resolving Observatory for Broadband Energy X-rays (STROBE-X) comprises three primary instruments. The first uses an array of lightweight optics (3-m focal length) that concentrate incident photons onto solid state detectors with CCD-level (85-130 eV) energy resolution, 100 ns time resolution, and low background rates to cover the 0.2-12 keV band. This technology is scaled up from NICER, with enhanced optics to take advantage of the longer focal length of STROBE-X. The second uses large-area collimated silicon drift detectors, developed for ESA's LOFT, to cover the 2-30 keV band. These two instruments each provide an order of magnitude improvement in effective area compared with its predecessor (NICER and RXTE, respectively). Finally, a sensitive sky monitor triggers pointed observations, provides high duty cycle, high time resolution, high spectral resolution monitoring of the X-ray sky with ~20 times the sensitivity of the RXTE ASM, and enables multi-wavelength and multi-messenger studies on a continuous, rather than scanning basis. We include updated instrument designs resulting from the GSFC IDL run in November 2017.For the first time, the broad coverage provides simultaneous study of thermal components, non-thermal components, iron lines, and reflection features from a single platform for accreting black holes at all scales. The enormous collecting area allows detailed studies of the dense matter equation of state using both thermal emission from rotation-powered pulsars and harder emission from X-ray burst oscillations. The combination of the wide-field monitor and the sensitive pointed instruments enables observations of potential electromagnetic counterparts to LIGO/Virgo and neutrino events. Extragalactic science, such as constraining bulk metalicity

  7. A X-ray photoelectron spectroscopy study of HDTMAB distribution within organoclays

    Science.gov (United States)

    He, Hongping; Zhou, Qin; Frost, Ray L.; Wood, Barry J.; Duong, Loc V.; Kloprogge, J. Theo

    2007-04-01

    X-ray photoelectron spectroscopy (XPS) in combination with X-ray diffraction (XRD) and high-resolution thermogravimetric analysis (HRTG) has been used to investigate the surfactant distribution within the organoclays prepared at different surfactant concentrations. This study demonstrates that the surfactant distribution within the organoclays depends strongly on the surfactant loadings. In the organoclays prepared at relative low surfactant concentrations, the surfactant cations mainly locate in the clay interlayer, whereas the surfactants occupy both the clay interlayer space and the interparticle pores in the organoclays prepared at high surfactant concentrations. This is in accordance with the dramatic pore volume decrease of organoclays compared to those of starting clays. XPS survey scans show that, at low surfactant concentration (organoclays prepared at high concentrations (>1.0 CEC). High-resolution XPS spectra show that the modification of clay with surfactants has prominent influences on the binding energies of the atoms in both clays and surfactants, and nitrogen is the most sensitive to the surfactant distribution within the organoclays.

  8. SUT-NANOTEC-SLRI beamline for X-ray absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Klysubun, Wantana; Kidkhunthod, Pinit; Tarawarakarn, Pongjakr; Sombunchoo, Panidtha; Kongmark, Chanapa; Limpijumnong, Sukit; Rujirawat, Saroj; Yimnirun, Rattikorn; Tumcharern, Gamolwan; Faungnawakij, Kajornsak

    2017-04-04

    The SUT-NANOTEC-SLRI beamline was constructed in 2012 as the flagship of the SUT-NANOTEC-SLRI Joint Research Facility for Synchrotron Utilization, co-established by Suranaree University of Technology (SUT), National Nanotechnology Center (NANOTEC) and Synchrotron Light Research Institute (SLRI). It is an intermediate-energy X-ray absorption spectroscopy (XAS) beamline at SLRI. The beamline delivers an unfocused monochromatic X-ray beam of tunable photon energy (1.25–10 keV). The maximum normal incident beam size is 13 mm (width) × 1 mm (height) with a photon flux of 3 × 108to 2 × 1010 photons s-1(100 mA)-1varying across photon energies. Details of the beamline and XAS instrumentation are described. To demonstrate the beamline performance,K-edge XANES spectra of MgO, Al2O3, S8, FeS, FeSO4, Cu, Cu2O and CuO, and EXAFS spectra of Cu and CuO are presented.

  9. Time-resolved x-ray absorption spectroscopy: Watching atoms dance

    Energy Technology Data Exchange (ETDEWEB)

    Milne, Chris J; Pham, Van-Thai; Veen, Renske M van der; El Nahhas, Amal; Lima, Frederico; Vithanage, Dimali A; Chergui, Majed [Laboratoire de Spectroscopie Ultrarapide, Ecole Polytechnique Federale de Lausanne (Switzerland); Gawelda, Wojciech [Laser Processing Group, Instituto de Optica, CSIC (Spain); Johnson, Steven L; Beaud, Paul; Ingold, Gerhard; Grolimund, Daniel; Borca, Camelia; Kaiser, Maik; Abela, Rafael [Swiss Light Source, Paul Scherrer Institut (Switzerland); Benfatto, Maurizio [Laboratori Nazionali di Frascati, INFN (Italy); Hauser, Andreas [Departement de Chimie Physique, Universite de Geneve (Switzerland); Bressler, Christian, E-mail: majed.chergui@epfl.c, E-mail: chris.milne@psi.c [European XFEL Project Team, Deutsches Elektronen Synchrotron (Germany)

    2009-11-15

    The introduction of pump-probe techniques to the field of x-ray absorption spectroscopy (XAS) has allowed the monitoring of both structural and electronic dynamics of disordered systems in the condensed phase with unprecedented accuracy, both in time and in space. We present results on the electronically excited high-spin state structure of an Fe(II) molecular species, [Fe{sup II}(bpy){sub 3}]{sup 2+}, in aqueous solution, resolving the Fe-N bond distance elongation as 0.2 A. In addition an analysis technique using the reduced {chi}{sup 2} goodness of fit between FEFF EXAFS simulations and the experimental transient absorption signal in energy space has been successfully tested as a function of excited state population and chemical shift, demonstrating its applicability in situations where the fractional excited state population cannot be determined through other measurements. Finally by using a novel ultrafast hard x-ray 'slicing' source the question of how the molecule relaxes after optical excitation has been successfully resolved using femtosecond XANES.

  10. Design of Molecular Solar Cells via Feedback from Soft X-ray Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Himpsel, Franz J. [Univ. of Wisconsin, Madison, WI (United States)

    2015-06-12

    Spectroscopy with soft X-rays was used to develop new materials and novel designs for solar cells and artificial photosynthesis. In order to go beyond the widely-used trial-and-error approach of gradually improving a particular design, we started from the most general layout of a solar cell (or a photo-electrochemical device) and asked which classes of materials are promising for best performance. For example, the most general design of a solar cell consists of a light absorber, an electron donor, and an electron acceptor. These are characterized by four energy levels, which were measured by a combination of spectroscopic X-ray techniques. Tuning synchrotron radiation to the absorption edges of specific elements provided element- and bond-selectivity. The spectroscopic results were complemented by state-of-the-art calculations of the electronic states. These helped explaining the observed energy levels and the orbitals associated with them. The calculations were extended to a large class of materials (for example thousands of porphyrin dye complexes) in order to survey trends in the energy level structure. A few highlights serve as examples: 1) Organic molecules combining absorber, donor, and acceptor with atomic precision. 2) Exploration of highly p-doped diamond films as inert, transparent electron donors. 3) Surface-sensitive characterization of nanorod arrays used as photoanodes in water splitting. 4) Computational design of molecular complexes for efficient solar cells using two photons.

  11. X-ray absorption spectroscopy and EPR studies of oriented spinach thylakoid preparations

    Energy Technology Data Exchange (ETDEWEB)

    Andrews, J.C. [Univ. of California, Berkeley, CA (United States). Dept. of Chemistry]|[Lawrence Berkeley Lab., CA (United States). Structural Biology Div.

    1995-08-01

    In this study, oriented Photosystem II (PS II) particles from spinach chloroplasts are studied with electron paramagnetic resonance (EPR) and x-ray absorption spectroscopy (XAS) to determine more details of the structure of the oxygen evolving complex (OEC). The nature of halide binding to Mn is also studied with Cl K-edge and Mn EXAFS (extended x-ray absorption fine structure) of Mn-Cl model compounds, and with Mn EXAFS of oriented PS II in which Br has replaced Cl. Attention is focused on the following: photosynthesis and the oxygen evolving complex; determination of mosaic spread in oriented photosystem II particles from signal II EPR measurement; oriented EXAFS--studies of PS II in the S{sub 2} state; structural changes in PS II as a result of treatment with ammonia: EPR and XAS studies; studies of halide binding to Mn: Cl K-edge and Mn EXAFS of Mn-Cl model compounds and Mn EXAFS of oriented Br-treated photosystem II.

  12. Strontium localization in bone tissue studied by X-ray absorption spectroscopy.

    Science.gov (United States)

    Frankær, Christian Grundahl; Raffalt, Anders Christer; Stahl, Kenny

    2014-02-01

    Strontium has recently been introduced as a pharmacological agent for the treatment and prevention of osteoporosis. We determined the localization of strontium incorporated into bone matrix from dogs treated with Sr malonate by X-ray absorption spectroscopy. A new approach for analyzing the X-ray absorption spectra resulted in a compositional model and allowed the relative distribution of strontium in the different bone components to be estimated. Approximately 35-45% of the strontium present is incorporated into calcium hydroxyapatite (CaHA) by substitution of some of the calcium ions occupying highly ordered sites, and at least 30% is located at less ordered sites where only the first solvation shell is resolved, suggesting that strontium is surrounded by only oxygen atoms similar to Sr(2+) in solution. Strontium was furthermore shown to be absorbed in collagen in which it obtains a higher structural order than when present in serum but less order than when it is incorporated into CaHA. The total amount of strontium in the samples was determined by inductively coupled plasma mass spectrometry, and the amount of Sr was found to increase with increasing dose levels and treatment periods, whereas the relative distribution of strontium among the different components appears to be independent of treatment period and dose level.

  13. X-ray emission spectroscopy of bulk liquid water in "no-man's land".

    Science.gov (United States)

    Sellberg, Jonas A; McQueen, Trevor A; Laksmono, Hartawan; Schreck, Simon; Beye, Martin; DePonte, Daniel P; Kennedy, Brian; Nordlund, Dennis; Sierra, Raymond G; Schlesinger, Daniel; Tokushima, Takashi; Zhovtobriukh, Iurii; Eckert, Sebastian; Segtnan, Vegard H; Ogasawara, Hirohito; Kubicek, Katharina; Techert, Simone; Bergmann, Uwe; Dakovski, Georgi L; Schlotter, William F; Harada, Yoshihisa; Bogan, Michael J; Wernet, Philippe; Föhlisch, Alexander; Pettersson, Lars G M; Nilsson, Anders

    2015-01-28

    The structure of bulk liquid water was recently probed by x-ray scattering below the temperature limit of homogeneous nucleation (TH) of ∼232 K [J. A. Sellberg et al., Nature 510, 381-384 (2014)]. Here, we utilize a similar approach to study the structure of bulk liquid water below TH using oxygen K-edge x-ray emission spectroscopy (XES). Based on previous XES experiments [T. Tokushima et al., Chem. Phys. Lett. 460, 387-400 (2008)] at higher temperatures, we expected the ratio of the 1b1' and 1b1″ peaks associated with the lone-pair orbital in water to change strongly upon deep supercooling as the coordination of the hydrogen (H-) bonds becomes tetrahedral. In contrast, we observed only minor changes in the lone-pair spectral region, challenging an interpretation in terms of two interconverting species. A number of alternative hypotheses to explain the results are put forward and discussed. Although the spectra can be explained by various contributions from these hypotheses, we here emphasize the interpretation that the line shape of each component changes dramatically when approaching lower temperatures, where, in particular, the peak assigned to the proposed disordered component would become more symmetrical as vibrational interference becomes more important.

  14. Determination of uranyl incorporation into biogenic manganese oxides using X-ray absorption spectroscopy and scattering

    Science.gov (United States)

    Webb, S.M.; Fuller, C.C.; Tebo, B.M.; Bargar, J.R.

    2006-01-01

    Biogenic manganese oxides are common and an important source of reactive mineral surfaces in the environment that may be potentially enhanced in bioremediation cases to improve natural attenuation. Experiments were performed in which the uranyl ion, UO22+ (U(VI)), at various concentrations was present during manganese oxide biogenesis. At all concentrations, there was strong uptake of U onto the oxides. Synchrotron-based extended X-ray absorption fine structure (EXAFS) spectroscopy and X-ray diffraction (XRD) studies were carried out to determine the molecular-scale mechanism by which uranyl is incorporated into the oxide and how this incorporation affects the resulting manganese oxide structure and mineralogy. The EXAFS experiments show that at low concentrations (2 mol % U, >4 ??M U(VI) in solution), the presence of U(VI) affects the stability and structure of the Mn oxide to form poorly ordered Mn oxide tunnel structures, similar to todorokite. EXAFS modeling shows that uranyl is present in these oxides predominantly in the tunnels of the Mn oxide structure in a tridentate complex. Observations by XRD corroborate these results. Structural incorporation may lead to more stable U(VI) sequestration that may be suitable for remediation uses. These observations, combined with the very high uptake capacity of the Mn oxides, imply that Mn-oxidizing bacteria may significantly influence dissolved U(VI) concentrations in impacted waters via sorption and incorporation into Mn oxide biominerals. ?? 2006 American Chemical Society.

  15. X-ray photoelectron spectroscopy of graphitic carbon nanomaterials doped with heteroatoms.

    Science.gov (United States)

    Susi, Toma; Pichler, Thomas; Ayala, Paola

    2015-01-01

    X-ray photoelectron spectroscopy (XPS) is one of the best tools for studying the chemical modification of surfaces, and in particular the distribution and bonding of heteroatom dopants in carbon nanomaterials such as graphene and carbon nanotubes. Although these materials have superb intrinsic properties, these often need to be modified in a controlled way for specific applications. Towards this aim, the most studied dopants are neighbors to carbon in the periodic table, nitrogen and boron, with phosphorus starting to emerge as an interesting new alternative. Hundreds of studies have used XPS for analyzing the concentration and bonding of dopants in various materials. Although the majority of works has concentrated on nitrogen, important work is still ongoing to identify its precise atomic bonding configurations. In general, care should be taken in the preparation of a suitable sample, consideration of the intrinsic photoemission response of the material in question, and the appropriate spectral analysis. If this is not the case, incorrect conclusions can easily be drawn, especially in the assignment of measured binding energies into specific atomic configurations. Starting from the characteristics of pristine materials, this review provides a practical guide for interpreting X-ray photoelectron spectra of doped graphitic carbon nanomaterials, and a reference for their binding energies that are vital for compositional analysis via XPS.

  16. SUT-NANOTEC-SLRI beamline for X-ray absorption spectroscopy.

    Science.gov (United States)

    Klysubun, Wantana; Kidkhunthod, Pinit; Tarawarakarn, Pongjakr; Sombunchoo, Panidtha; Kongmark, Chanapa; Limpijumnong, Sukit; Rujirawat, Saroj; Yimnirun, Rattikorn; Tumcharern, Gamolwan; Faungnawakij, Kajornsak

    2017-05-01

    The SUT-NANOTEC-SLRI beamline was constructed in 2012 as the flagship of the SUT-NANOTEC-SLRI Joint Research Facility for Synchrotron Utilization, co-established by Suranaree University of Technology (SUT), National Nanotechnology Center (NANOTEC) and Synchrotron Light Research Institute (SLRI). It is an intermediate-energy X-ray absorption spectroscopy (XAS) beamline at SLRI. The beamline delivers an unfocused monochromatic X-ray beam of tunable photon energy (1.25-10 keV). The maximum normal incident beam size is 13 mm (width) × 1 mm (height) with a photon flux of 3 × 108 to 2 × 1010 photons s-1 (100 mA)-1 varying across photon energies. Details of the beamline and XAS instrumentation are described. To demonstrate the beamline performance, K-edge XANES spectra of MgO, Al2O3, S8, FeS, FeSO4, Cu, Cu2O and CuO, and EXAFS spectra of Cu and CuO are presented.

  17. X-ray photoelectron spectroscopy of graphitic carbon nanomaterials doped with heteroatoms

    Directory of Open Access Journals (Sweden)

    Toma Susi

    2015-01-01

    Full Text Available X-ray photoelectron spectroscopy (XPS is one of the best tools for studying the chemical modification of surfaces, and in particular the distribution and bonding of heteroatom dopants in carbon nanomaterials such as graphene and carbon nanotubes. Although these materials have superb intrinsic properties, these often need to be modified in a controlled way for specific applications. Towards this aim, the most studied dopants are neighbors to carbon in the periodic table, nitrogen and boron, with phosphorus starting to emerge as an interesting new alternative. Hundreds of studies have used XPS for analyzing the concentration and bonding of dopants in various materials. Although the majority of works has concentrated on nitrogen, important work is still ongoing to identify its precise atomic bonding configurations. In general, care should be taken in the preparation of a suitable sample, consideration of the intrinsic photoemission response of the material in question, and the appropriate spectral analysis. If this is not the case, incorrect conclusions can easily be drawn, especially in the assignment of measured binding energies into specific atomic configurations. Starting from the characteristics of pristine materials, this review provides a practical guide for interpreting X-ray photoelectron spectra of doped graphitic carbon nanomaterials, and a reference for their binding energies that are vital for compositional analysis via XPS.

  18. Prediction of Ba, Co and Ni for tropical soils using diffuse reflectance spectroscopy and X-ray fluorescence spectroscopy

    Science.gov (United States)

    Arantes Camargo, Livia; Marques Júnior, José; Reynaldo Ferracciú Alleoni, Luís; Tadeu Pereira, Gener; De Bortoli Teixeira, Daniel; Santos Rabelo de Souza Bahia, Angélica

    2017-04-01

    Environmental impact assessments may be assisted by spatial characterization of potentially toxic elements (PTEs). Diffuse reflectance spectroscopy (DRS) and X-ray fluorescence spectroscopy (XRF) are rapid, non-destructive, low-cost, prediction tools for a simultaneous characterization of different soil attributes. Although low concentrations of PTEs might preclude the observation of spectral features, their contents can be predicted using spectroscopy by exploring the existing relationship between the PTEs and soil attributes with spectral features. This study aimed to evaluate, in three geomorphic surfaces of Oxisols, the capacity for predicting PTEs (Ba, Co, and Ni) and their spatial variability by means of diffuse reflectance spectroscopy (DRS) and X-ray fluorescence spectroscopy (XRF). For that, soil samples were collected from three geomorphic surfaces and analyzed for chemical, physical, and mineralogical properties, and then analyzed in DRS (visible + near infrared - VIS+NIR and medium infrared - MIR) and XRF equipment. PTE prediction models were calibrated using partial least squares regression (PLSR). PTE spatial distribution maps were built using the values calculated by the calibrated models that reached the best accuracy using geostatistics. PTE prediction models were satisfactorily calibrated using MIR DRS for Ba, and Co (residual prediction deviation - RPD > 3.0), Vis DRS for Ni (RPD > 2.0) and FRX for all the studied PTEs (RPD > 1.8). DRS- and XRF-predicted values allowed the characterization and the understanding of spatial variability of the studied PTEs.

  19. In situ X-ray absorption spectroscopy of transition metal based water oxidation catalysts

    NARCIS (Netherlands)

    van Oversteeg, Christina H M; Doan, Hoang Q; de Groot, Frank M F; Cuk, Tanja

    2016-01-01

    X-ray absorption studies of the geometric and electronic structure of primarily heterogeneous Co, Ni, and Mn based water oxidation catalysts are reviewed. The X-ray absorption near edge and extended X-ray absorption fine structure studies of the metal K-edge, characterize the metal oxidation state,

  20. Broadband x-ray imaging and spectroscopy of the crab nebula and pulsar with NuSTAR

    DEFF Research Database (Denmark)

    Madsen, Kristin K.; Reynolds, Stephen; Harrison, Fiona

    2015-01-01

    We present broadband (3-78 keV) NuSTAR X-ray imaging and spectroscopy of the Crab nebula and pulsar. We show that while the phase-averaged and spatially integrated nebula + pulsar spectrum is a power law in this energy band, spatially resolved spectroscopy of the nebula finds a break at ~9 ke...

  1. Low-energy d-d excitations in MnO studied by resonant x-ray fluorescence spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Butorin, S.M.; Guo, J.; Magnuson, M. [Uppsala Univ. (Sweden)] [and others

    1997-04-01

    Resonant soft X-ray emission spectroscopy has been demonstrated to possess interesting abilities for studies of electronic structure in various systems, such as symmetry probing, alignment and polarization dependence, sensitivity to channel interference, etc. In the present abstract the authors focus on the feasibility of resonant soft X-ray emission to probe low energy excitations by means of resonant electronic X-ray Raman scattering. Resonant X-ray emission can be regarded as an inelastic scattering process where a system in the ground state is transferred to a low excited state via a virtual core excitation. The energy closeness to a core excitation of the exciting radiation enhances the (generally) low probability for inelastic scattering at these wavelengths. Therefore soft X-ray emission spectroscopy (in resonant electronic Raman mode) can be used to study low energy d-d excitations in transition metal systems. The involvement of the intermediate core state allows one to use the selection rules of X-ray emission, and the appearance of the elastically scattered line in the spectra provides the reference to the ground state.

  2. Design and performance of a soft-x-ray interferometer for ultra-high-resolution fourier transform spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Moler, E.J.; Hussain, Z.; Duarte, R.M.; Howells, M.R. [Lawrence Berkeley National Lab., CA (United States)

    1997-04-01

    A Fourier Transform Soft X-ray spectrometer (FT-SX) has been designed and is under construction for the Advanced Light Source (ALS) at Lawrence Berkeley National Laboratory as a branch of beamline 9.3.2. The spectrometer is a novel soft x-ray interferometer designed for ultra-high resolution (theoretical resolving power E/{delta}E{approximately}10{sup 6}) spectroscopy in the photon energy region of 60-120 eV. This instrument is expected to provide experimental results which sensitively test models of correlated electron processes in atomic and molecular physics. The design criteria and consequent technical challenges posed by the short wavelengths of x-rays and desired resolving power are discussed. The fundamental and practical aspects of soft x-ray interferometry are also explored.

  3. Optical and x-ray photoelectron spectroscopy studies of α-Al{sub 2}O{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Prakash, Ram, E-mail: rpgiuc@gmail.com, E-mail: ramprakash@smvdu.ac.in; Kumar, Sandeep; Kumar, Vinay [School of Physics, Shri Mata Vaishno Devi University, Katra 182320 J& K (India); Choudhary, R. J.; Phase, D. M. [UGC DAE Consortium for Scientific Research, Indore-452001 (India)

    2016-05-23

    α-Al{sub 2}O{sub 3} powder sample was synthesized at 550 °C via solution combustion synthesis (SCS) method using urea as an organic fuel. The sample was characterized by X-ray diffraction (XRD), Optical spectroscopy and X-ray photoelectron spectroscopy (XPS) without any further thermal treatment. XRD study reveals that the powder crystallized directly in the hexagons α-Al{sub 2}O{sub 3} phase. A band gap of 5.7 eV was estimated using diffuse reflectance spectra. For surface investigation X-ray photo electron spectroscopy (XPS) was carried out. The XPS survey scan study of α-Al{sub 2}O{sub 3} powder reveals that the sample is free from impurity. The core levels of Al-2s and O-1s are also reported.

  4. X-ray absorption spectroscopy for the structural investigation of self-assembled-monolayer-directed mineralization.

    Science.gov (United States)

    Lee, Jonathan R I; Bagge-Hansen, Michael; Willey, Trevor M; Meulenberg, Robert W; Nielsen, Michael H; Tran, Ich C; van Buuren, Tony

    2013-01-01

    Self-assembled monolayers (SAMs) of organothiol molecules prepared on noble metal substrates are known to exert considerable influence over biomineral nucleation and growth and, as such, offer model templates for investigation of the processes of directed biomineralization. Identifying the structural evolution of SAM/crystal systems is essential for a more comprehensive understanding of the mechanisms by which organic monolayers mediate mineral growth. X-ray absorption spectroscopy (XAS) provides the attractive ability to study SAM structure at critical stages throughout the processes of crystallization in SAM/mineral systems. Here, we discuss important theoretical and experimental considerations for designing and implementing XAS studies of SAM/mineral systems. © 2013 Elsevier Inc. All rights reserved.

  5. X-ray Absorption Spectroscopy Characterization of a Li/S Cell

    Directory of Open Access Journals (Sweden)

    Yifan Ye

    2016-01-01

    Full Text Available The X-ray absorption spectroscopy technique has been applied to study different stages of the lithium/sulfur (Li/S cell life cycle. We have investigated how speciation of S in Li/S cathodes changes upon the introduction of CTAB (cetyltrimethylammonium bromide, CH3(CH215N+(CH33Br− and with charge/discharge cycling. The introduction of CTAB changes the synthesis reaction pathway dramatically due to the interaction of CTAB with the terminal S atoms of the polysulfide ions in the Na2Sx solution. For the cycled Li/S cell, the loss of electrochemically active sulfur and the accumulation of a compact blocking insulating layer of unexpected sulfur reaction products on the cathode surface during the charge/discharge processes make the capacity decay. A modified coin cell and a vacuum-compatible three-electrode electro-chemical cell have been introduced for further in-situ/in-operando studies.

  6. X-ray absorption spectroscopy studies of electrochemically deposited thin oxide films.

    Energy Technology Data Exchange (ETDEWEB)

    Balasubramanian, M.

    1998-06-02

    We have utilized ''in situ'' X-ray Absorption Fine Structure Spectroscopy to investigate the structure and composition of thin oxide films of nickel and iron that have been prepared by electrodeposition on a graphite substrate from aqueous solutions. The films are generally disordered. Structural information has been obtained from the analysis of the data. We also present initial findings on the local structure of heavy metal ions, e.g. Sr and Ce, incorporated into the electrodeposited nickel oxide films. Our results are of importance in a number of technological applications, among them, batteries, fuel cells, electrochromic and ferroelectric materials, corrosion protection, as well as environmental speciation and remediation.

  7. Thermal oxidation of vanadium-free Ti alloys: An X-ray photoelectron spectroscopy study

    Energy Technology Data Exchange (ETDEWEB)

    Lopez, Maria Francisca, E-mail: mflopez@icmm.csic.es [Department of Surfaces and Coatings, ICMM-CSIC, Sor Juana Ines de la Cruz, 3, Cantoblanco, 28049 Madrid (Spain); Gutierrez, Alejandro [Departamento de Fisica Aplicada and Instituto Nicolas Cabrera, Universidad Autonoma de Madrid, Cantoblanco, E-28049 Madrid (Spain); Jimenez, Jose Antonio [Centro Nacional de Investigaciones Metalurgicas, CSIC, Avda. Gregorio del Amo 8, E-28040 Madrid (Spain); Martinesi, Maria; Stio, Maria; Treves, Cristina [Department of Biochemical Sciences of University of Florence, Viale Morgagni 50, 50134 Florence (Italy)

    2010-04-06

    In the present work, X-ray photoelectron spectroscopy (XPS) was used to study the surface chemical composition of three alloys for biomedical applications: Ti-7Nb-6Al, Ti-13Nb-13Zr and Ti-15Zr-4Nb. The surface of these alloys was modified by annealing in air at 750 deg. C for different times with the aim of developing an oxide thick layer on top. The evolution of surface composition with annealing time was studied by XPS, and compared with the composition of the native oxide layer present on the samples before annealing. Two different oxidation trends were observed depending on the alloying elements and their corresponding diffusion kinetics, which give rise to different chemical species at the topmost layers. These results were linked with an evaluation of the biological response of the alloys by bringing them in contact with human peripheral blood mononuclear cells (PBMC).

  8. Arsenic K-edge X-ray absorption spectroscopy of arsenic in seafood.

    Science.gov (United States)

    George, Graham N; Prince, Roger C; Singh, Satya P; Pickering, Ingrid J

    2009-05-01

    It is well known that seafood contains high levels of arsenic. For marine animals arsenic is predominantly present as arsenobetaine and related compounds which are not metabolized and are thought to present no toxic hazard to humans. With edible seaweeds, arsenic is present in different forms, of which arsenosugars are the best known. These species may be metabolized by mammals, and the high arsenic contents of these materials represent a significant environmental source for human exposure to arsenicals in some populations. In this work, we explore the utility of As K-edge X-ray absorption near-edge spectroscopy as an in situ probe of the chemical forms of arsenic in seaweeds. We find that three different chemical types of arsenic are present, consistent with arsenate, an arsenosugar or tetra-alkyl-arsonium species, and a trivalent arsenic species.

  9. Reconstruction of confocal micro-X-ray fluorescence spectroscopy depth scans obtained with a laboratory setup.

    Science.gov (United States)

    Mantouvalou, Ioanna; Wolff, Timo; Seim, Christian; Stoytschew, Valentin; Malzer, Wolfgang; Kanngiesser, Birgit

    2014-10-07

    Depth profiling with confocal micro-X-ray fluorescence spectroscopy (confocal micro-XRF) is a nondestructive analytical method for obtaining elemental depth profiles in the micrometer region. Up until now, the quantitative reconstruction of thicknesses and elemental concentration of stratified samples has been only possible with monochromatic, thus, synchrotron radiation. In this work, we present a new calibration and reconstruction procedure, which renders quantification in the laboratory feasible. The proposed model uses the approximation of an effective spot size of the optic in the excitation channel and relies on the calibration of the transmission of this lens beforehand. Calibration issues are discussed and validation measurements on thick multielement reference material and a stratified system are presented.

  10. Analysis of zirconia films by grazing incidence X-ray absorption fine structure spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Degueldre, C. [LWV, NES, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland)]. E-mail: claude.degueldre@psi.ch; Dardenne, K. [INE, Forschungszentrum Karlsruhe, D-76344 Karlsruhe (Germany)

    2005-08-15

    X-ray absorption fine structure spectroscopy (XAFS) is used in for its non-destructive capability to probe and investigate nano-pores, dislocations or vacancies in zirconia films. XAFS is a powerful analytical tool that allows the collection of information to describe the atomic environment of component elements. This technique was applied in a grazing incidence (GI) mode to investigate layers obtained by zirconia sputtering on stainless steel and by zirconium alloy corrosion utilising the Zr K edge. XAFS analysis identify a decrease of next neighbour numbers of Zr in the corroded samples versus the sputtered samples. This may be due to the density of distortions for given average atom distances suggesting dislocations and defects. The discussion underlines that the technique reveals nano-pores, dislocations, vacancies or defect features difficult to observe using destructive techniques such as analytical electron microscopy. A strong decrease of the Zr next neighbour number is observed for zirconium alloy corrosion layers.

  11. Study of a neutron irradiated reactor pressure vessel steel by X-ray absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Cammelli, S. [LWV, NES, Paul Scherrer Institute, 5232 Villigen PSI (Switzerland)], E-mail: sebastiano.cammelli@psi.ch; Degueldre, C.; Kuri, G.; Bertsch, J. [LWV, NES, Paul Scherrer Institute, 5232 Villigen PSI (Switzerland)

    2008-11-15

    Reactor pressure vessel (RPV) reference steel samples submitted to neutron irradiations followed by thermal annealing were investigated by X-ray absorption fine structure (XAFS) spectroscopy. Several studies revealed that Cu and Ni impurities can form nanoclusters. In the unirradiated sample and in the only-irradiated sample no significant clustering is detected. In all irradiated and subsequently annealed samples increases of Cu and Ni atom densities are recorded around the absorber. Furthermore, the density of Cu and Ni atoms determined in the first and second shells around the absorber is found to be affected by the irradiation and annealing treatment. The comparison of the XAFS data at Cu and Ni K-edges shows that these elements reside in arrangements similar to bcc Fe. However, the local irradiation damage yields vacancy fractions which were determined from the analysis of XAFS data with a precision of {approx}5%.

  12. X-ray Spectroscopy and Imaging as Multiscale Probes of Intercalation Phenomena in Cathode Materials

    Science.gov (United States)

    Horrocks, Gregory A.; De Jesus, Luis R.; Andrews, Justin L.; Banerjee, Sarbajit

    2017-09-01

    Intercalation phenomena are at the heart of modern electrochemical energy storage. Nevertheless, as out-of-equilibrium processes involving concomitant mass and charge transport, such phenomena can be difficult to engineer in a predictive manner. The rational design of electrode architectures requires mechanistic understanding of physical phenomena spanning multiple length scales, from atomistic distortions and electron localization at individual transition metal centers to phase inhomogeneities and intercalation gradients in individual particles and concentration variances across ensembles of particles. In this review article, we discuss the importance of the electronic structure in mediating electrochemical storage and mesoscale heterogeneity. In particular, we discuss x-ray spectroscopy and imaging probes of electronic and atomistic structure as well as statistical regression methods that allow for monitoring of the evolution of the electronic structure as a function of intercalation. The layered α-phase of V2O5 is used as a model system to develop fundamental ideas on the origins of mesoscale heterogeneity.

  13. Dynamics of Lithium Polymer Electrolytes using X-ray Photon Correlation Spectroscopy and Rheology

    Science.gov (United States)

    Oparaji, Onyekachi; Narayanan, Suresh; Sandy, Alec; Hallinan, Daniel, Jr.

    Polymer electrolytes are promising materials for high energy density rechargeable batteries. Battery fade can be caused by structural evolution in the battery electrode and loss of electrode/electrolyte adhesion during cycling. Both of these effects are dependent on polymer mechanical properties. In addition, cycling rate is dictated by the ion mobility of the polymer electrolyte. Lithium ion mobility is expected to be strongly coupled to polymer dynamics. Therefore, we investigate polymer dynamics as a function of salt concentration using X-ray Photon Correlation Spectroscopy (XPCS) and rheology. We report the influence of lithium salt concentration on the structural relaxation time (XPCS) and stress relaxation time (rheology) of high molecular weight poly(styrene - ethylene oxide) block copolymer membranes.

  14. Electrostatic immobilization of polyoxometallates on silicon: X-ray Photoelectron Spectroscopy and electrochemical studies

    Energy Technology Data Exchange (ETDEWEB)

    Fleury, Benoit [INAC/LCIB/RICC (UMR E3 CEA-UJF, FRE CNRS 3200), CEA-Grenoble 17 rue des martyrs, 38054 Grenoble cedex 9 (France); Billon, Martial [INAC/SPrAM/CREAB (UMR 5819 CEA-CNRS-UJF), CEA-Grenoble 17 rue des martyrs, 38054 Grenoble cedex 9 (France); Duclairoir, Florence, E-mail: florence.duclairoir@cea.f [INAC/LCIB/RICC (UMR E3 CEA-UJF, FRE CNRS 3200), CEA-Grenoble 17 rue des martyrs, 38054 Grenoble cedex 9 (France); Dubois, Lionel [INAC/LCIB/RICC (UMR E3 CEA-UJF, FRE CNRS 3200), CEA-Grenoble 17 rue des martyrs, 38054 Grenoble cedex 9 (France); Fanton, Aurelien [LETI/DPTS/SCPIO/LCPO, CEA-Grenoble 17 rue des martyrs, 38054 Grenoble cedex 9 (France); Bidan, Gerard [INAC/DIR, CEA-Grenoble 17 rue des martyrs, 38054 Grenoble cedex 9 (France)

    2011-03-31

    Keggin-type dodecatungstosilicates polyoxometallates (POMs) ([SiW{sub 12}O{sub 40}]{sup 4-}) were immobilized in a straightforward manner by electrostatic interactions on ammonium layers covalently grafted on silicon. This method does not require any POM modification synthetical steps. The presence of [SiW{sub 12}O{sub 40}]{sup 4-} on the surface is demonstrated by X-ray Photoelectron Spectroscopy from a specific modification of the tungsten 4f{sub 7/2} signal. Moreover the surface coverage of [SiW{sub 12}O{sub 40}]{sup 4-} has been improved by 35% upon changing the nature of the anchoring ammonium groups from protonated to methylated amino groups. The organic-inorganic composite films have also been characterized by cyclic voltammetry showing that POMs have a specific behavior on silicon surfaces. In addition the use of a polyallylamine capping layer proved to stabilize efficiently the POM electrochemical response.

  15. Simulating systematic errors in X-ray absorption spectroscopy experiments: Sample and beam effects

    Energy Technology Data Exchange (ETDEWEB)

    Curis, Emmanuel [Laboratoire de Biomathematiques, Faculte de Pharmacie, Universite Rene, Descartes (Paris V)-4, Avenue de l' Observatoire, 75006 Paris (France)]. E-mail: emmanuel.curis@univ-paris5.fr; Osan, Janos [KFKI Atomic Energy Research Institute (AEKI)-P.O. Box 49, H-1525 Budapest (Hungary); Falkenberg, Gerald [Hamburger Synchrotronstrahlungslabor (HASYLAB), Deutsches Elektronen-Synchrotron (DESY)-Notkestrasse 85, 22607 Hamburg (Germany); Benazeth, Simone [Laboratoire de Biomathematiques, Faculte de Pharmacie, Universite Rene, Descartes (Paris V)-4, Avenue de l' Observatoire, 75006 Paris (France); Laboratoire d' Utilisation du Rayonnement Electromagnetique (LURE)-Ba-hat timent 209D, Campus d' Orsay, 91406 Orsay (France); Toeroek, Szabina [KFKI Atomic Energy Research Institute (AEKI)-P.O. Box 49, H-1525 Budapest (Hungary)

    2005-07-15

    The article presents an analytical model to simulate experimental imperfections in the realization of an X-ray absorption spectroscopy experiment, performed in transmission or fluorescence mode. Distinction is made between sources of systematic errors on a time-scale basis, to select the more appropriate model for their handling. For short time-scale, statistical models are the most suited. For large time-scale, the model is developed for sample and beam imperfections: mainly sample inhomogeneity, sample self-absorption, beam achromaticity. The ability of this model to reproduce the effects of these imperfections is exemplified, and the model is validated on real samples. Various potential application fields of the model are then presented.

  16. Endohedral fullerenes: a concurrent characterization by means of synchrotron radiation X-ray and IR spectroscopy

    Science.gov (United States)

    Xu, Wei; Marcelli, Augusto; Liu, Lei; Wang, Chunru; Wu, Ziyu

    2013-04-01

    Endohedral Metal Fullerenes exhibit a great variety of physical and chemical properties depending on the metal inserted into the cage. These systems are molecular conductors, magnets, ferroelectrics and also superconductors representing extremely promising materials for advanced technologies such as nano-medicine. Here we present temperature-dependent XANES and FTIR investigations of two La@C82 EMF isomers. The combinatorial investigation shows that guest ions move inside the cage perturbing the vibrational states of the carbon cage due to the charge transfer dynamics. Moreover, the principal component analysis points out a discrepancy between temperature-dependent FTIR and XANES based on the occurrence of a non-equilibrium process between charge transfer and cage dynamics. We propose to perform simultaneous time-resolved X-ray and infrared spectroscopy studies to resolve the complex interplay among charge, structure and electric properties of these systems.

  17. Comparative study of bandwidths in copper delafossites from x-ray emission spectroscopy

    Science.gov (United States)

    Shin, D.; Foord, J. S.; Payne, D. J.; Arnold, T.; Aston, D. J.; Egdell, R. G.; Godinho, K. G.; Scanlon, D. O.; Morgan, B. J.; Watson, G. W.; Mugnier, E.; Yaicle, C.; Rougier, A.; Colakerol, L.; Glans, P. A.; Piper, L. F. J.; Smith, K. E.

    2009-12-01

    The widths of the valence bands in the copper (I) delafossites CuGaO2 , CuInO2 , and CuScO2 have been measured by OK -shell x-ray emission spectroscopy and are compared with previous experimental work on CuAlO2 and CuCrO2 . In agreement with recent density-functional theory calculations it is found that the bandwidth decreases in the series CuAlO2>CuGaO2>CuInO2>CuScO2 . It is shown that states at the top of the valence band are of dominant Cu3dz2 atomic character but with significant mixing with O2p states.

  18. Atomic physics studies of highly charged ions on tokamaks using x-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Beiersdorfer, P.; von Goeler, S.; Bitter, M.; Hill, K.W.

    1989-07-01

    An overview is given of atomic physics issues which have been studied on tokamaks with the help resolution x-ray spectroscopy. The issues include the testing of model calculations predicting the excitation of line radiation, the determination of rate coefficients, and accurate atomic structure measurements. Recent research has focussed primarily on highly charged heliumlike (22 less than or equal to Z less than or equal to 28) and neonlike (34 less than or equal to Z less than or equal to 63) ions, and results are presented from measurements on the PLT and TFTR tokamaks. Many of the measurements have been aided by improved instrumental design and new measuring techniques. Remarkable agreement has been found between measurements and theory in most cases. However, in this review those areas are stressed where agreement is worst and where further investigations are needed. 19 refs., 13 figs., 2 tabs.

  19. Room temperature oxidation kinetics of Si nanoparticles in air, determined by x-ray photoelectron spectroscopy

    Science.gov (United States)

    Yang, D.-Q.; Gillet, Jean-Numa; Meunier, M.; Sacher, E.

    2005-01-01

    The air oxidation kinetics of low coverages of ˜5nm Si nanoparticles, deposited by pulsed excimer laser ablation (KrF, 248 nm) in He, have been characterized by x-ray photoelectron spectroscopy. A simple model, based on the evolution of the Si 2p spectral components during oxidation, has been developed to determine the nanoparticle oxide thickness. It is found that the short-term oxide thickness is greater, and the long-term room-temperature air oxidization rate of these nanoparticles is less, than those reported for bulk a-Si and c-Si. The results are also consistent with an earlier transmission electron microscope observation of the oxidation of larger Si particles at higher temperatures. The greater short-term oxide thickness may be attributed to surface defects on the prepared Si nanoparticles, and lower long-term oxidation rate is due to the nonlinear decrease of oxygen diffusion in spherical systems.

  20. X-Ray diffraction, spectroscopy and thermochemical characterization of the pharmaceutical paroxetine nitrate salt

    Science.gov (United States)

    Carvalho, Paulo S.; de Melo, Cristiane C.; Ayala, Alejandro P.; Ellena, Javier

    2016-08-01

    A comprehensive solid state study of Paroxetine nitrate hydrate, (PRX+·NO3-)H2O, is reported. This salt was characterized by a combination of methods, including Single crystal X-ray diffraction, Thermal analysis, Fourier transform infrared spectroscopy (FTIR) and Solubility measurements. (PRX+·NO3-)H2O crystallizes in the monoclinic C2 space group (Z‧ = 1) and its packing was analyzed in details, showing that the main supramolecular motif consists in a C22(4) chain formed by charge-assisted N+-H⋯O- hydrogen bonds. The salt formation and conformation features were also accuracy established via FTIR spectra. In comparison with the pharmaceutical approved (PRX+ṡCl-)ṡ0.5H2O, (PRX+ṡNO3-)ṡH2O showed a decrease of 24 °C in the drug melting peak and a slight reduction in its water solubility value.

  1. ZnO/ZnAl2O4 Nanocomposite Films Studied by X-Ray Diffraction, FTIR, and X-Ray Photoelectron Spectroscopy

    Directory of Open Access Journals (Sweden)

    S. Iaiche

    2015-01-01

    Full Text Available ZnO/ZnAl2O4 nanocomposite films were synthesised by ultrasonic spray pyrolysis (USP by extracting Al2O(SO42 oxide with zinc chloride hydrate in deionised water. The sample was then subjected to heat treatment at 650°C and 700°C for 1 h, which led to the formation of the spinel oxide (ZnAl2O4 and wurtzite (ZnO phases. Al2(SO43·18H2O salt was transformed into aluminum oxide sulfate Al2O(SO42, which is an intermediary decomposition product, by calcination at 795°C for 3 h. The structures of the synthesised ZnO/ZnAl2O4 films were confirmed by XRD, FTIR, and X-ray photoelectron spectroscopy (XPS. XPS spectra of the major Zn, Al, and O photoelectron lines and the major X-ray induced Zn LMM Auger lines for ZnO/ZnAl2O4 are presented.

  2. In situ flow cell for combined X-ray absorption spectroscopy, X-ray diffraction, and mass spectrometry at high photon energies under solar thermochemical looping conditions

    Science.gov (United States)

    Rothensteiner, Matthäus; Jenni, Joel; Emerich, Hermann; Bonk, Alexander; Vogt, Ulrich F.; van Bokhoven, Jeroen A.

    2017-08-01

    An in situ/operando flow cell for transmission mode X-ray absorption spectroscopy (XAS), X-ray diffraction (XRD), and combined XAS/XRD measurements in a single experiment under the extreme conditions of two-step solar thermochemical looping for the dissociation of water and/or carbon dioxide was developed. The apparatus exposes materials to relevant conditions of both the auto-reduction and the oxidation sub-steps of the thermochemical cycle at ambient temperature up to 1773 K and enables determination of the composition of the effluent gases by online quadrupole mass spectrometry. The cell is based on a tube-in-tube design and is heated by means of a focusing infrared furnace. It was tested successfully for carbon dioxide splitting. In combined XAS/XRD experiments with an unfocused beam, XAS measurements were performed at the Ce K edge (40.4 keV) and XRD measurements at 64.8 keV and 55.9 keV. Furthermore, XRD measurements with a focused beam at 41.5 keV were carried out. Equimolar ceria-hafnia was auto-reduced in a flow of argon and chemically reduced in a flow of hydrogen/helium. Under reducing conditions, all cerium(iv) was converted to cerium(iii) and a cation-ordered pyrochlore-type structure was formed, which was not stable upon oxidation in a flow of carbon dioxide.

  3. Investigation by laser induced breakdown spectroscopy, X-ray fluorescence and X-ray powder diffraction of the chemical composition of white clay ceramic tiles from Veliki Preslav

    Energy Technology Data Exchange (ETDEWEB)

    Blagoev, K., E-mail: kblagoev@issp.bas.bg [Institute of Solid State Physics, Bulgarian Academy of Sciences, 72 Tzarigradsko Chaussee, 1784 Sofia (Bulgaria); Grozeva, M., E-mail: margo@issp.bas.bg [Institute of Solid State Physics, Bulgarian Academy of Sciences, 72 Tzarigradsko Chaussee, 1784 Sofia (Bulgaria); Malcheva, G., E-mail: bobcheva@issp.bas.bg [Institute of Solid State Physics, Bulgarian Academy of Sciences, 72 Tzarigradsko Chaussee, 1784 Sofia (Bulgaria); Neykova, S., E-mail: sevdalinaneikova@abv.bg [National Institute of Archaeology with Museum, Bulgarian Academy of Sciences, 2 Saborna, 1000 Sofia (Bulgaria)

    2013-01-01

    The paper presents the results of the application of laser induced breakdown spectroscopy, X-ray fluorescence spectrometry, and X-ray powder diffraction in assessing the chemical and phase composition of white clay decorative ceramic tiles from the medieval archaeological site of Veliki Preslav, a Bulgarian capital in the period 893–972 AC, well-known for its original ceramic production. Numerous white clay ceramic tiles with highly varied decoration, produced for wall decoration of city's churches and palaces, were found during the archaeological excavations in the old capital. The examination of fourteen ceramic tiles discovered in one of the city's monasteries is aimed at characterization of the chemical profile of the white-clay decorative ceramics produced in Veliki Preslav. Combining different methods and comparing the obtained results provides complementary information regarding the white-clay ceramic production in Veliki Preslav and complete chemical characterization of the examined artefacts. - Highlights: ► LIBS, XRF and XRD analyses of medieval white-clay ceramic tiles fragments are done. ► Different elements and phases, presented in the ceramics fragments were determined. ► Differences in the tiles' raw material mineral composition are found. ► Information of the tiles' production process and the raw clay deposits is obtained.

  4. Arsenite Oxidation by a Poorly-Crystalline Manganese Oxide 2. Results from X-ray Absorption Spectroscopy and X-ray Diffraction

    Science.gov (United States)

    Lafferty, Brandon J.; Ginder-Vogel, Matthew; Zhu, Mengqiang; Livi, Kenneth J. T.; Sparks, Donald L.

    2010-01-01

    Arsenite (AsIII) oxidation by manganese oxides (Mn-oxides) serves to detoxify and, under many conditions, immobilize arsenic (As) by forming arsenate (AsV). AsIII oxidation by MnIV-oxides can be quite complex, involving many simultaneous forward reactions and subsequent back reactions. During AsIII oxidation by Mn-oxides, a reduction in oxidation rate is often observed, which is attributed to Mn-oxide surface passivation. X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) data show that MnII sorption on a poorly-crystalline hexagonal birnessite (δ-MnO2) is important in passivation early during reaction with AsIII. Also, it appears that MnIII in the δ-MnO2 structure is formed by conproportionation of sorbed MnII and MnIV in the mineral structure. The content of MnIII within the δ-MnO2 structure appears to increase as the reaction proceeds. Binding of AsV to δ-MnO2 also changes as MnIII becomes more prominent in the δ-MnO2 structure. The data presented indicate that AsIII oxidation and AsV sorption by poorly-crystalline δ-MnO2 is greatly affected by Mn oxidation state in the δ-MnO2 structure. PMID:20977204

  5. The aquatic hyphomycete Heliscus lugdunensis protects its hyphae tip cells from cadmium: A micro X-ray fluorescence and X-ray absorption near edge structure spectroscopy study

    Science.gov (United States)

    Isaure, Marie-Pierre; Leyh, Benjamin; Salomé, Murielle; Krauss, Gerd-Joachim; Schaumlöffel, Dirk; Dobritzsch, Dirk

    2017-11-01

    Aquatic fungi can be used to evaluate the functioning of natural ecosystems. Heliscus lugdunensis is an early colonizer of allochthone leafs. Since this aquatic hyphomycete is able to develop in metal contaminated habitats and tolerates cadmium, it appears to be a good candidate to investigate adaptation to metal pollution. This study aimed at examining the sequestration of Cd in the hyphae of H. lugdunensis, and particularly the role of the tip cells. For that, H. lugdunensis growth was evaluated under various Cd concentrations, and a combination of synchrotron micro X-ray fluorescence and X-ray absorption near edge structure spectroscopy was carried out to determine the compartments of Cd accumulation and the Cd chemical species, respectively. Results showed that the hyphal tip cells were depleted in Cd, and that the metal was stored in older cells. Cd was mainly associated with sulfur ligands and to a lesser extent bound to phosphates and carboxyl/hydroxyl groups from cell wall and/or organic acids. Finally, the aquatic fungus was able to maintain the tip cell as a functional system, thus allowing the colonization of contaminated environments.

  6. Ultra-small-angle X-ray scattering-X-ray photon correlation spectroscopy studies of incipient structural changes in amorphous calcium phosphate-based dental composites.

    Science.gov (United States)

    Zhang, Fan; Allen, Andrew J; Levine, Lyle E; Espinal, Laura; Antonucci, Joseph M; Skrtic, Drago; O'Donnell, Justin N R; Ilavsky, Jan

    2012-05-01

    The local structural changes in amorphous calcium phosphate (ACP)-based dental composites were studied under isothermal conditions using both static, bulk measurement techniques and a recently developed methodology based on combined ultra-small angle X-ray scattering-X-ray photon correlation spectroscopy (USAXS-XPCS), which permits a dynamic approach. While results from conventional bulk measurements do not show clear signs of structural change, USAXS-XPCS results reveal unambiguous evidence for local structural variations on a similar time scale to that of water loss in the ACP fillers. A thermal-expansion-based simulation indicates that thermal behavior alone does not account for the observed dynamics. Together, these results suggest that changes in the water content of ACP affect the composite morphology due to changes in ACP structure that occur without an amorphous-to-crystalline conversion. It is also noted that biomedical materials research could benefit greatly from USAXS-XPCS, a dynamic approach. Copyright © 2012 Wiley Periodicals, Inc.

  7. Advanced signal separation and recovery algorithms for digital x-ray spectroscopy

    Science.gov (United States)

    Mahmoud, Imbaby I.; El Tokhy, Mohamed S.

    2015-02-01

    X-ray spectroscopy is widely used for in-situ applications for samples analysis. Therefore, spectrum drawing and assessment of x-ray spectroscopy with high accuracy is the main scope of this paper. A Silicon Lithium Si(Li) detector that cooled with a nitrogen is used for signal extraction. The resolution of the ADC is 12 bits. Also, the sampling rate of ADC is 5 MHz. Hence, different algorithms are implemented. These algorithms were run on a personal computer with Intel core TM i5-3470 CPU and 3.20 GHz. These algorithms are signal preprocessing, signal separation and recovery algorithms, and spectrum drawing algorithm. Moreover, statistical measurements are used for evaluation of these algorithms. Signal preprocessing based on DC-offset correction and signal de-noising is performed. DC-offset correction was done by using minimum value of radiation signal. However, signal de-noising was implemented using fourth order finite impulse response (FIR) filter, linear phase least-square FIR filter, complex wavelet transforms (CWT) and Kalman filter methods. We noticed that Kalman filter achieves large peak signal to noise ratio (PSNR) and lower error than other methods. However, CWT takes much longer execution time. Moreover, three different algorithms that allow correction of x-ray signal overlapping are presented. These algorithms are 1D non-derivative peak search algorithm, second derivative peak search algorithm and extrema algorithm. Additionally, the effect of signal separation and recovery algorithms on spectrum drawing is measured. Comparison between these algorithms is introduced. The obtained results confirm that second derivative peak search algorithm as well as extrema algorithm have very small error in comparison with 1D non-derivative peak search algorithm. However, the second derivative peak search algorithm takes much longer execution time. Therefore, extrema algorithm introduces better results over other algorithms. It has the advantage of recovering and

  8. Where Water is Oxidized to Dioxygen: Structure of the Photosynthetic Mn4Ca Cluster from X-ray Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Yano, Junko; Yano, Junko; Yachandra, Vittal K.

    2007-10-24

    Light-driven oxidation of water to dioxygen in plants, algae and cyanobacteria iscatalyzed within photosystem II (PS II) by a Mn4Ca cluster. Although the cluster has been studied by many different methods, the structure and the mechanism have remained elusive. X-ray absorption and emission spectroscopy and EXAFS studies have been particularly useful in probing the electronic and geometric structure, and the mechanism of the water oxidation reaction. Recent progress, reviewed here, includes polarized X-ray absorption spectroscopy measurements of PS II single crystals. Analysis of those results has constrained the Mn4Ca cluster geometry to a setof three similar high-resolution structures. The structure of the cluster from the present study is unlike either the 3.0 or 3.5 Angstrom-resolution X-ray structures or other previously proposed models. The differences between the models derived from X-rayspectroscopy and crystallography are predominantly because of damage to the Mn4Ca cluster by X-rays under the conditions used for structure determination by X-ray crystallography. X-ray spectroscopy studies are also used for studying the changes in the structure of the Mn4Ca catalytic center as it cycles through the five intermediate states known as the Si-states (i=0-4). The electronic structure of the Mn4Ca cluster has been studied more recently using resonant inelastic X-ray scattering spectroscopy (RIXS), in addition to the earlier X-ray absorption and emission spectroscopy methods. These studies are revealing that the assignment of formaloxidation states is overly simplistic. A more accurate description should consider the charge density on the Mn atoms that includes the covalency of the bonds and delocalization of the charge over the cluster. The geometric and electronic structure of the Mn4Ca cluster in the S-states derived from X-ray spectroscopy are leading to a detailed understanding of the mechanism of the O-O bond formation during the photosynthetic water

  9. Structure of the ethylammonium nitrate surface: an X-ray reflectivity and vibrational sum frequency spectroscopy study.

    Science.gov (United States)

    Niga, Petru; Wakeham, Deborah; Nelson, Andrew; Warr, Gregory G; Rutland, Mark; Atkin, Rob

    2010-06-01

    X-ray reflectivity and vibrational sum frequency spectroscopy are used to probe the structure of the ethylammonium nitrate (EAN)-air interface. X-ray reflectivity reveals that the EAN-air interface is structured and consists of alternating nonpolar and charged layers that extend 31 A into the bulk. Vibrational sum frequency spectroscopy reveals interfacial cations have their ethyl moieties oriented toward air, with the CH(3) C(3) axis positioned approximately 36.5 degrees from interface normal. This structure is invariant between 15 and 51 degrees C. On account of its molecular symmetry, the orientation of the nitrate anion cannot be determined with certainty.

  10. Functional group analysis of coal and coal products by X-ray photoelectron spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Perry, D.L.; Grint, A.

    1986-04-01

    In a number of technologies such as polymers and carbon fibres, where there is a similar interest in the nature of organic functional groups and their effect on material performance, the technique of x-ray photoelectron spectroscopy (XPS), also known as electron spectroscopy for chemical analysis (ESCA), has been applied successfully to a wide range of problems. However XPS is a technique which is little used in coal science. Since it has high surface sensitivity and the specific surfaces properties of coals play an important role in a number of coal technologies, e.g. flotation and agglomeration, it is perhaps surprising that XPS is not used more extensively. The reasons for this may lie in some of the discouraging references in the literature. For example early work by Frost et al found no relationship between oxygen concentrations determined by XPS and the bulk analysis of a series of float-sink fractions. More recently Huffmann et al observed that oxidation of bituminous coals for up to 383 days at 50/sup 0/C in air completely destroyed Geiseler fluidity but neither XPS nor DRIFT (Diffuse Reflectance FTIR) spectroscopy could detect any parallel changes in the functional group composition of the coal. This paper describes the application of XPS to coal, coal reactions and coal products. The aim is to present a critical evaluation in the context of other techniques which are applied to coal.

  11. Synchrotron-based X-ray absorption spectroscopy for art conservation: looking back and looking forward.

    Science.gov (United States)

    Cotte, Marine; Susini, Jean; Dik, Joris; Janssens, Koen

    2010-06-15

    A variety of analytical techniques augmented by the use of synchrotron radiation (SR), such as X-ray fluorescence (SR-XRF) and X-ray diffraction (SR-XRD), are now readily available, and they differ little, conceptually, from their common laboratory counterparts. Because of numerous advantages afforded by SR-based techniques over benchtop versions, however, SR methods have become popular with archaeologists, art historians, curators, and other researchers in the field of cultural heritage (CH). Although the CH community now commonly uses both SR-XRF and SR-XRD, the use of synchrotron-based X-ray absorption spectroscopy (SR-XAS) techniques remains marginal, mostly because CH specialists rarely interact with SR physicists. In this Account, we examine the basic principles and capabilities of XAS techniques in art preservation. XAS techniques offer a combination of features particularly well-suited for the chemical analysis of works of art. The methods are noninvasive, have low detection limits, afford high lateral resolution, and provide exceptional chemical sensitivity. These characteristics are highly desirable for the chemical characterization of precious, heterogeneous, and complex materials. In particular, the chemical mapping capability, with high spatial resolution that provides information about local composition and chemical states, even for trace elements, is a unique asset. The chemistry involved in both the object's history (that is, during fabrication) and future (that is, during preservation and restoration treatments) can be addressed by XAS. On the one hand, many studies seek to explain optical effects occurring in historical glasses or ceramics by probing the molecular environment of relevant chromophores. Hence, XAS can provide insight into craft skills that were mastered years, decades, or centuries ago but were lost over the course of time. On the other hand, XAS can also be used to characterize unwanted reactions, which are then considered

  12. Radiation effects and metalloproteins studied by x-ray photoelectron spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Wurzbach, J.A.

    1975-07-01

    X-ray photoelectron spectroscopy (XPS) is used to study the bonding structure at the iron site of cytochrome c and the bonding of rare earth ions to the phosphate oxygens of ATP. Radiation effects are studied on several amino acid and simple peptide model systems. The emission spectrum of the x-ray source is calculated from literature references. The distributions of photon energy as a function of photon frequency and as a function of take-off angle are obtained. From these distributions, the radiation dose absorbed by an organic sample is found to be 10/sup 6/ rads/sec. The C 1s and N 1s spectra of amino acids and peptides are studied to characterize an internal reference standard for protein XPS spectra. Samples of native cytochrome c prepared from solutions of pH 1.5, 3, 7, and 11 are studied. Control samples include porphyrin cytochrome c (PCC), the metal free analogue of the native protein, and microperoxidase (MP), a mixture of heme peptides derived from the peptic digestion of cytochrome c. These samples show two S 2p peaks. The first peak has a binding energy (BE) of 163 eV, which corresponds to the S containing amino acids; the second peak is shifted to 167 eV. This large shift may be the result of Fe-S binding, or oxidation, or both. Low spin ferricytochrome c and ferri-MP were found to have Fe 3p BE's that are unusually low (51 eV) compared to other ferric compounds (54 to 58 eV) and even Fe metal (53 eV). X-ray crystal structures of these compounds show that low spin heme Fe lies in the porphyrin plane; while, high spin heme Fe is displaced above the plane. The N 1s and P 2p spectra of ATP show no change except slight broadening when Nd/sup 3 +/ is substituted for Na/sup +/. Thus, there is no inconsistency with proposals that rare earth ions might be useful as substitutes for alkali metal ions and alkaline earth ions in proteins.

  13. Magnetic coupling in (GaMn)As ferromagnetic semiconductors - studied by soft X-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Kronast, F.

    2006-07-01

    Manganese doped into Gallium Arsenide provides a local spin magnetic moment and acting as an acceptor it creates itinerant holes, which can mediate long range ferromagnetic order. We studied the magnetic coupling of Mn atoms and their hybridization with the GaAs host in epitactically grown (GaMn)As layers, utilizing X-ray absorption spectroscopy and X-ray magnetic circular dichroism at the Mn L2,3 absorption edges. Combining surface and bulk sensitive detection methods with additional reflectivity measurements we resolved a chemical and magnetic depth profile of Mn in the (GaMn)As layer. The depth profile reveals an inhomogeneous distribution of Mn in two different ground state configurations. The bulk is dominated by Mn residing at the Ga sites, for this substitutional Mn the hybridization with the sp-states of the As ligands causes an admixture of a 3d{sup 6} weight to the 3d{sup 5} ground state configuration. At the surface we find an accumulation of non-ferromagnetic Mn in a pure 3d{sup 5} electronic configuration. The enhanced surface segregation of this second Mn species upon annealing provides strong evidence that the surface layer is caused by the diffusion of interstitial Mn during the growth and the annealing. With increasing Mn concentration we find an increasing amount of Mn atoms not participating in the ferromagnetic ordering. Their number scales approximately with the number of Mn nearest neighbor pairs expected for a statistical Mn distribution. For the Mn atoms not participating in the ferromagnetic ordering we also find a reduced number of 3d electrons of close to 3d{sup 4}. Both observations can be explained by the presence of antiferromagnetically coupled Mn-Mn nearest neighbor pairs at higher Mn concentrations. So far antiferromagnetic coupling has only been observed in doped II-VI semiconductors. The pd-hybridization, mediating the magnetic exchange coupling, is usually assumed to be spherically isotropic. We studied the pd-hybridization by X-ray

  14. Hard X-ray photoelectron spectroscopy of bulk and thin films of Heusler compounds

    Energy Technology Data Exchange (ETDEWEB)

    Kozina, Xeniya

    2012-03-26

    X-ray photoemission spectroscopy (XPS) is one of the most universal and powerful tools for investigation of chemical states and electronic structures of materials. The application of hard X-rays increases the inelastic mean free path of the emitted electrons within the solid and thus makes hard X-ray photoelectron spectroscopy (HAXPES) a bulk sensitive probe for solid state research and especially a very effective nondestructive technique to study buried layers. This thesis focuses on the investigation of multilayer structures, used in magnetic tunnel junctions (MTJs), by a number of techniques applying HAXPES. MTJs are the most important components of novel nanoscale devices employed in spintronics. The investigation and deep understanding of the mechanisms responsible for the high performance of such devices and properties of employed magnetic materials that are, in turn, defined by their electronic structure becomes feasible applying HAXPES. Thus the process of B diffusion in CoFeB-based MTJs was investigated with respect to the annealing temperature and its influence on the changes in the electronic structure of CoFeB electrodes that clarify the behaviour and huge TMR ratio values obtained in such devices. These results are presented in chapter 6. The results of investigation of the changes in the valence states of buried off-stoichiometric Co{sub 2}MnSi electrodes were investigated with respect to the Mn content {alpha} and its influence on the observed TMR ratio are described in chapter 7. Magnetoelectronic properties such as exchange splitting in ferromagnetic materials as well as the macroscopic magnetic ordering can be studied by magnetic circular dichroism in photoemission (MCDAD). It is characterized by the appearance of an asymmetry in the photoemission spectra taken either from the magnetized sample with the reversal of the photon helicity or by reversal of magnetization direction of the sample when the photon helicity direction is fixed. Though

  15. X-ray absorption spectroscopy in biological systems. Opportunities and limitations

    Energy Technology Data Exchange (ETDEWEB)

    Bovenkamp, Gudrun Lisa

    2013-05-15

    X-ray absorption spectroscopy has become more important for applications in the material sciences, geology, environmental science and biology, specifically in the field of molecular biology. The scope of this thesis is to add more experimental evidence in order to show how applicable X-ray absorption near edge structure (XANES) is to biology. Two biological systems were investigated, at the molecular level, lead uptake in plants and the effect of silver on bacteria. This investigation also included an analysis of the sensitivity of Pb L{sub 3}- and Ag L{sub 3}-XANES spectra with regard to their chemical environment. It was shown that Pb L{sub 3}- and Ag L{sub 3}-XANES spectra are sensitive to an environment with at least differences in the second coordination shell. The non-destructive and element specific properties of XANES are the key advantages that were very important for this investigation. However, in both projects the adequate selection of reference compounds, which required in some cases a chemical synthesis, was the critical factor to determine the chemical speciation and, finally, possible uptake and storage mechanisms for plants and antibacterial mechanisms of silver. The chemical environment of Pb in roots and leaves of plants from four different plant families and a lichen from a former lead mining site in the Eifel mountains in Germany was determined using both solid compounds and aqueous solutions of different ionic strength, which simulate the plant environment. The results can be interpreted in such a way that lead is sorbed on the surface of cell walls. Silver bonding as reaction with Staphylococcus aureus, Listeria monocytogenes, and Escherichia coli bacteria was determined using inorganic silver compounds and synthesized silver amino acids. Silver binds to sulfur, amine and carboxyl groups in amino acids.

  16. High-Resolution X-Ray Spectroscopy of Galactic Supernova Remnants

    Directory of Open Access Journals (Sweden)

    Satoru Katsuda

    2014-12-01

    Full Text Available High-resolution X-ray spectroscopy of Galactic supernova remnants (SNRs, based on grating spectrometers onboard XMM-Newton and Chandra, has been revealing a variety of new astrophysical phenomena. Broadened oxygen lines for a northwestern compact knot in SN 1006 clearly show a high oxygen temperature of ~300 keV. The high temperature together with a lower electron temperature (kTe ~ 1 keV can be reasonably interpreted as temperature non-equilibration between electrons and oxygen behind a collisionless shock. An ejecta knot in the Puppis A SNR shows blueshifted line emission by ~ 1500kms-1. The line widths are fairly narrow in contrast to the SN 1006's knot; an upper limit of 0.9 eV is obtained for O VIII Lyα, which translates to an oxygen temperature of kTO < 30 keV. The low temperature suggests that the knot was heated by a reverse shock whose velocity is 4 times slower than that of a forward shock. Anomalous intensity ratios in O VII Heα lines, i.e., a stronger forbidden line than a resonance line, is found in a cloud-shock interaction region in Puppis A. The line ratio can be best explained by the charge-exchange emission that should arise at interfaces between the cold/warm clouds and the hot plasma. There are several other targets for which we plan to analyze high-quality grating data prior to the operation of the soft X-ray spectrometer onboard Astro-H.

  17. Au36(SPh)24 nanomolecules: X-ray crystal structure, optical spectroscopy, electrochemistry, and theoretical analysis.

    Science.gov (United States)

    Nimmala, Praneeth Reddy; Knoppe, Stefan; Jupally, Vijay Reddy; Delcamp, Jared H; Aikens, Christine M; Dass, Amala

    2014-12-11

    The physicochemical properties of gold:thiolate nanomolecules depend on their crystal structure and the capping ligands. The effects of protecting ligands on the crystal structure of the nanomolecules are of high interest in this area of research. Here we report the crystal structure of an all aromatic thiophenolate-capped Au36(SPh)24 nanomolecule, which has a face-centered cubic (fcc) core similar to other nanomolecules such as Au36(SPh-tBu)24 and Au36(SC5H9)24 with the same number of gold atoms and ligands. The results support the idea that a stable core remains intact even when the capping ligand is varied. We also correct our earlier assignment of "Au36(SPh)23" which was determined based on MALDI mass spectrometry which is more prone to fragmentation than ESI mass spectrometry. We show that ESI mass spectrometry gives the correct assignment of Au36(SPh)24, supporting the X-ray crystal structure. The electronic structure of the title compound was computed at different levels of theory (PBE, LDA, and LB94) using the coordinates extracted from the single crystal X-ray diffraction data. The optical and electrochemical properties were determined from experimental data using UV-vis spectroscopy, cyclic voltammetry, and differential pulse voltammetry. Au36(SPh)24 shows a broad electrochemical gap near 2 V, a desirable optical gap of ∼1.75 eV for dye-sensitized solar cell applications, as well as appropriately positioned electrochemical potentials for many electrocatalytic reactions.

  18. ACADEMIC TRAINING: Probing nature with high precision; particle traps, laser spectroscopy and optical combs

    CERN Multimedia

    Françoise Benz

    2002-01-01

    17, 18, 19 June LECTURE SERIES from 11.00 to 12.00 hrs - Auditorium, bldg. 500 Probing nature with high precision; particle traps, laser spectroscopy and optical combs by G. GABRIELSE / Harvard University, USA Experiments with atomic energy scales probe nature and its symmetries with exquisite precision. Particle traps allow the manipulation of single charged particles for months at a time, allow the most accurate comparison of theory and experiment, and promise to allow better measurement of fundamental quantities like the fine structure constant. Ions and atoms can be probed with lasers that are phase locked to microwave frequency standards via optical combs, thus calibrating optical sources in terms of the official cesium second. A series of three lectures will illustrate what can be measured and discuss key techniques.  ACADEMIC TRAINING Françoise Benz Tel. 73127 francoise.benz@cern.ch

  19. High precision (14 bit), high density (octal) analog to digital converter for spectroscopy applications.

    Science.gov (United States)

    Subramaniam, E T; Jain, Mamta; Bhowmik, R K; Tripon, Michel

    2008-10-01

    Nuclear and particle physics experiments with large number of detectors require signal processing and data collection strategies that call for the ability to collect large amount of data while not sacrificing the precision and accuracy of the data being collected. This paper deals with the development of a high precision pulse peak detection, analog to digital converter (ADC) module with eight independent channels in plug-in daughter card motherboard model, best suited for spectroscopy experiments. This module provides multiple channels without cross-talk and of 14 bit resolution, while maintaining high density (each daughter card has an area of just 4.2(")x0.51(")) and exhibiting excellent integral nonlinearity (< or = +/-2 mV or +/-0.02% full scale reading) and differential nonlinearity (< or = +/-1%). It was designed, developed and tested, in house, and gives added advantages of cost effectiveness and ease of maintenance.

  20. X-ray absorption and Raman spectroscopy studies of molybdenum environments in borosilicate waste glasses

    Science.gov (United States)

    McKeown, David A.; Gan, Hao; Pegg, Ian L.

    2017-05-01

    Mo-containing high-level nuclear waste borosilicate glasses were investigated as part of an effort to improve Mo loading while avoiding yellow phase crystallization. Previous work showed that additions of vanadium decrease yellow phase formation and increases Mo solubility. X-ray absorption spectroscopy (XAS) and Raman spectroscopy were used to characterize Mo environments in HLW borosilicate glasses and to investigate possible structural relationships between Mo and V. Mo XAS spectra for the glasses indicate isolated tetrahedral Mo6+O4 with Mo-O distances near 1.75 Å. V XANES indicate tetrahedral V5+O4 as the dominant species. Raman spectra show composition dependent trends, where Mo-O symmetrical stretch mode frequencies (ν1) are sensitive to the mix of alkali and alkaline earth cations, decreasing by up to 10 cm-1 for glasses that change from Li+ to Na+ as the dominant network-modifying species. This indicates that MoO4 tetrahedra are isolated from the borosilicate network and are surrounded, at least partly, by Na+ and Li+. Secondary ν1 frequency effects, with changes up to 7 cm-1, were also observed with increasing V2O5 and MoO3 content. These secondary trends may indicate MoO4-MoO4 and MoO4-VO4 clustering, suggesting that V additions may stabilize Mo in the matrix with respect to yellow phase formation.

  1. Soft X-ray synchrotron radiation spectroscopy study of molecule-based nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Lee, E. S.; Kim, D. H.; Kang, J. S.; Kim, P. [The Catholic University of Korea, Bucheon (Korea, Republic of); Kim, K. H. [Korea University, Jochiwon (Korea, Republic of); Baik, J. Y.; Shin, H. J. [POSTECH, Pohang (Korea, Republic of)

    2014-11-15

    The electronic structures of molecule-based nanoparticles, such as biomineralized Helicobacter pylori ferritin (Hpf), Heme, and RbCo[Fe(CN){sub 6}]H{sub 2}O (RbCoFe) Prussian blue analogue, have been investigated by employing photoemission spectroscopy and soft X-ray absorption spectroscopy. Fe ions are found to be nearly trivalent in Hpf and Heme nanoparticles, which provides evidence that the amount of magnetite (Fe{sub 3}O{sub 4}) should be negligible in the Hpf core and that the biomineralization of Fe oxides in the high-Fe-bound-state Hpf core arises from a hematite-like formation. On the other hand, Fe ions are nearly divalent and Co ions are Co{sup 2+}-Co{sup 3+} mixed-valent in RbCoFe. Therefore this finding suggests that the mechanism of the photo-induced transition in RbCoFe Prussian blue analogue is not a simple spin-state transition of Fe{sup 2+}-Co{sup 3+} → Fe{sup 3+}-Co{sup 2+}. It is likely that Co{sup 2+} ions have the high-spin configuration while Fe{sup 2+} ions have the low-spin configuration.

  2. Soft X-ray photoemission spectroscopy of selected neurotransmitters in the gas phase

    Energy Technology Data Exchange (ETDEWEB)

    Maris, Assimo; Melandri, Sonia; Evangelisti, Luca; Caminati, Walther [Dipartimento di Chimica ' G. Ciamician' dell' Universita, Via Selmi 2, I-40126 Bologna (Italy); Giuliano, Barbara M. [Departamento de Quimica da Universidade de Coimbra, 3004-535 Coimbra (Portugal); Plekan, Oksana [Sincrotrone Trieste, in Area Science Park, I-34149 Basovizza, Trieste (Italy); Feyer, Vitaliy [Sincrotrone Trieste, in Area Science Park, I-34149 Basovizza, Trieste (Italy); Electronic Properties (PGI-6), Peter Gruenberg Institute, Forschungszentrum Juelich GmbH, Leo-Brandt-Strasse, 52428 Juelich (Germany); Richter, Robert [Sincrotrone Trieste, in Area Science Park, I-34149 Basovizza, Trieste (Italy); Coreno, Marcello [CNR-IMIP, Montelibretti, I-00016 Rome (Italy); Prince, Kevin C., E-mail: kevin.prince@elettra.trieste.it [Sincrotrone Trieste, in Area Science Park, I-34149 Basovizza, Trieste (Italy); CNR-IOM, Laboratorio TASC, I-34149 Basovizza, Trieste (Italy)

    2012-09-15

    Highlights: Black-Right-Pointing-Pointer Neurotransmitter molecules. Black-Right-Pointing-Pointer Photoelectron spectroscopy. Black-Right-Pointing-Pointer Electronic structure. Black-Right-Pointing-Pointer Weak hydrogen bonding. -- Abstract: The valence molecular orbitals and core levels of tyramine, tryptamine and tryptophol in the gas phase have been studied using X-ray photoelectron spectroscopy (XPS) and theoretical methods. The energies of the outer valence region spectrum are found to be in agreement with previously reported He I spectra, while new data on the inner valence molecular orbitals are reported. The structures in the carbon, nitrogen and oxygen core level spectra of these molecules have been identified and assigned. These compounds are characterised by conformers with hydrogen bonding in which the {pi} systems of the phenol and indole groups act as hydrogen acceptors, but a spectroscopic signature of this hydrogen bond was not observed. This is in contrast with our previous spectra of amino acids, where conformers with specific hydrogen bonding showed strong effects in core level spectra. We attribute the difference to the weaker strength of the {pi}-hydrogen bonding.

  3. X-Ray Fluorescence and Laser-Induced Breakdown Spectroscopy analysis of Roman silver denarii

    Energy Technology Data Exchange (ETDEWEB)

    Pardini, L. [Istituto di Chimica dei Composti Organometallici del CNR, Research Area of Pisa, Via G. Moruzzi 1, 56124 Pisa (Italy); El Hassan, A. [National Institute for Laser- Enhanced Sciences (NILES), Cairo University Giza (Egypt); Ferretti, M. [Istituto per le Tecnologie Applicate ai Beni Culturali, Area della Ricerca del CNR di Montelibretti Roma (Italy); Foresta, A.; Legnaioli, S.; Lorenzetti, G. [Istituto di Chimica dei Composti Organometallici del CNR, Research Area of Pisa, Via G. Moruzzi 1, 56124 Pisa (Italy); Nebbia, E. [Universita degli Studi di Torino (Italy); Catalli, F. [Monetiere di Firenze, Museo Archeologico Nazionale Firenze (Italy); Harith, M.A. [National Institute for Laser- Enhanced Sciences (NILES), Cairo University Giza (Egypt); Diaz Pace, D. [Institute of Physics ' Arroyo Seco' , Faculty of Science, Tandil (Argentina); Anabitarte Garcia, F. [Photonics Engineering Group, University of Cantabria, Santander (Spain); Scuotto, M. [Dipartimento di Scienze Archeologiche, Via Galvani 1, 56126 Pisa (Italy); Palleschi, V., E-mail: vincenzo.palleschi@cnr.it [Istituto di Chimica dei Composti Organometallici del CNR, Research Area of Pisa, Via G. Moruzzi 1, 56124 Pisa (Italy); Dipartimento di Scienze Archeologiche, Via Galvani 1, 56126 Pisa (Italy)

    2012-08-15

    In this paper we present the results of a study performed on a large collection of silver Roman republican denarii, encompassing about two centuries of history. The joint use of Laser-Induced Breakdown Spectroscopy (LIBS) and X-Ray Fluorescence (XRF) spectroscopy allowed for an accurate determination of the coins' elemental composition; the measurements, performed mostly in situ at the 'Monetiere' in Florence, revealed a striking connection between the 'quality' of the silver alloy and some crucial contemporary events. This finding was used to classify a group of denarii whose dating was otherwise impossible. The comparison with other contemporary denarii disproves a recent theory on the origin of the so called 'serrated' denarii (denarii showing notched chisel marks on the edge of the coin). - Highlights: Black-Right-Pointing-Pointer We studied a large collection of Roman republican silver denarii. Black-Right-Pointing-Pointer XRF and LIBS allowed to determine the precious metal content of the coins. Black-Right-Pointing-Pointer A correlation of the 'quality' of the alloy with some contemporary events was found. Black-Right-Pointing-Pointer The study allowed to controvert a recent theory on the so called 'serrated' denarii.

  4. Behavior of oxygen doped SiC thin films: An x-ray photoelectron spectroscopy study

    Science.gov (United States)

    Avila, A.; Montero, I.; Galán, L.; Ripalda, J. M.; Levy, R.

    2001-01-01

    Thin silicon carbide films have been deposited by chemical vapor deposition on p-type (100) silicon substrates. The composition and bonds formed in these films have been analyzed by x-ray photoelectron spectroscopy (XPS) and infrared spectroscopy. The native surface oxide on the silicon carbide surface induced by air exposure has also been studied. Several phases are detected in the near-surface region: elemental Si, Si oxides (mainly SiO2), Si carbide (SiC) and Si oxicarbides (SiOxCy). Quantitative XPS analysis results indicate that, for atomic oxygen fractions silicon oxicarbide is observed, but a multiphase material formed by elemental Si, Si oxides and Si carbides is observed. In spite of the film being a complex phase mixture, a simple relationship is found between the overall carbon and oxygen compositions. The carbon atomic fraction in the film decreases quasilinearly as the oxygen content increases, with a slope of about -1. An overall composition of SiOxC3-x in the 0.5silicon carbide obtained by CHn+ ion implantation into monocrystalline silicon is made.

  5. Relative stability of protein structures determined by X-ray crystallography or NMR spectroscopy : A molecular dynamics simulation study

    NARCIS (Netherlands)

    Fan, H; Mark, AE

    2003-01-01

    The relative stability of protein structures determined by either X-ray crystallography or nuclear magnetic resonance (NMR) spectroscopy has been investigated by using molecular dynamics simulation techniques. Published structures of 34 proteins containing between 50 and 100 residues have been

  6. High-resolution soft X-ray beamline ADRESS at the Swiss Light Source for resonant inelastic X-ray scattering and angle-resolved photoelectron spectroscopies

    Science.gov (United States)

    Strocov, V. N.; Schmitt, T.; Flechsig, U.; Schmidt, T.; Imhof, A.; Chen, Q.; Raabe, J.; Betemps, R.; Zimoch, D.; Krempasky, J.; Wang, X.; Grioni, M.; Piazzalunga, A.; Patthey, L.

    2010-01-01

    The concepts and technical realisation of the high-resolution soft X-ray beamline ADRESS operating in the energy range from 300 to 1600 eV and intended for resonant inelastic X-ray scattering (RIXS) and angle-resolved photoelectron spectroscopy (ARPES) are described. The photon source is an undulator of novel fixed-gap design where longitudinal movement of permanent magnetic arrays controls not only the light polarization (including circular and 0–180° rotatable linear polarizations) but also the energy without changing the gap. The beamline optics is based on the well established scheme of plane-grating monochromator operating in collimated light. The ultimate resolving power E/ΔE is above 33000 at 1 keV photon energy. The choice of blazed versus lamellar gratings and optimization of their profile parameters is described. Owing to glancing angles on the mirrors as well as optimized groove densities and profiles of the gratings, the beamline is capable of delivering high photon flux up to 1 × 1013 photons s−1 (0.01% BW)−1 at 1 keV. Ellipsoidal refocusing optics used for the RIXS endstation demagnifies the vertical spot size down to 4 µm, which allows slitless operation and thus maximal transmission of the high-resolution RIXS spectrometer delivering E/ΔE > 11000 at 1 keV photon energy. Apart from the beamline optics, an overview of the control system is given, the diagnostics and software tools are described, and strategies used for the optical alignment are discussed. An introduction to the concepts and instrumental realisation of the ARPES and RIXS endstations is given. PMID:20724785

  7. STROBE-X: X-ray timing and spectroscopy on dynamical timescales from microseconds to years

    Science.gov (United States)

    Wilson-Hodge, Colleen A.; Ray, Paul S.; Gendreau, Keith; Chakrabarty, Deepto; Feroci, Marco; Arzoumanian, Zaven; Brandt, Soren; Hernanz, Margarita; Hui, C. Michelle; Jenke, Peter A.; Maccarone, Thomas; Remillard, Ron; Wood, Kent; Zane, Silvia; Strobe-X Collaboration

    The Spectroscopic Time-Resolving Observatory for Broadband Energy X-rays (STROBE-X) probes strong gravity for stellar mass to supermassive black holes and ultradense matter with unprecedented effective area, high time-resolution, and good spectral resolution, while providing a powerful time-domain X-ray observatory.

  8. A TES X-ray microcalorimeter-array for imaging spectroscopy

    NARCIS (Netherlands)

    de Korte, P.A.J.; Hoevers, H.F.C.; den Herder, J.W.A.; Bleeker, J.A.M.; Bergmann Tiest, W.M.; Bruijn, M.P.; Ridder, M.L.; Wiegerink, Remco J.; Kaastra, J.S.; van der Kuur, J.; Mels, W.A.

    2002-01-01

    Development of single pixel X-ray microcalorimeters at our institutes, employing superconducting-to-normal phase transition thermometers operating at about 100 mK, generally called Transition-Edge-Sensors (TES), has now resulted in an energy resolution of 3.9 eV FWHM for 5.89 keV X-rays in

  9. Multi-anode linear SDDs for high-resolution X-ray spectroscopy

    NARCIS (Netherlands)

    Sonsky, J.

    2002-01-01

    Radiation detectors are used in a variety of fields to sense X-rays and y-rays, visible, UV and IR photons, neutrons or charged particles. With their help, advanced medical diagnostics can be performed (e.g. X-ray radiography, computed tomography, fluoroscopy), material research can undergo a rapid

  10. Infrared and X-Ray Spectroscopy of the KES 75 Supernova Remnant Shell: Characterizing the Dust and Gas Properties

    Science.gov (United States)

    Temim, Tea; Dwek, Eli; Slane, Patrick; Arendt, Richard G.

    2009-01-01

    We present deep Chandra observations and Spitzer Space Telescope infrared (IR) spectroscopy of the shell in the composite supernova remnant (SNR) Kes 75 (G29.7-0.3). The remnant is composed of a central pulsar wind nebula and a bright partial shell in the south that is visible at radio, IR, and X-ray wavelengths. The X-ray emission can be modeled by either a single thermal component with a temperature of 1.5 keV, or with two thermal components with temperatures of 1.5 and 0.2 keV. Previous studies suggest that the hot component may originate from reverse-shocked SN ejecta. However, our new analysis shows no definitive evidence for enhanced abundances of Si, S, Ar, Mg, and Fe, as expected from supernova (SN) ejecta, or for the IR spectral signatures characteristic of confirmed SN condensed dust, thus favoring a circumstellar or interstellar origin for the X-ray and IR emission. The X-ray and ill emission in the shell are spatially correlated, suggesting that the dust particles are collisionally heated by the X-ray emitting gas. The IR spectrum of the shell is dominated by continuum emission from dust with little, or no line emission. Modeling the IR spectrum shows that the dust is heated to a temperature of 140 K by a relatively dense, hot plasma, that also gives rise to the hot X-ray emission component. The density inferred from the IR emission is significantly higher than the density inferred from the X-ray models, suggesting a low filling factor for this X-ray emitting gas. The total mass of the warm dust component is at least 1.3 x 10(exp -2) solar mass, assuming no significant dust destruction has occurred in the shell. The IR data also reveal the presence of an additional plasma component with a cooler temperature, consistent with the 0.2 keV gas component. Our IR analysis therefore provides an independent verification of the cooler component of the X-ray emission. The complementary analyses of the X-ray and IR emission provide quantitative estimates of

  11. INFRARED AND X-RAY SPECTROSCOPY OF THE Kes 75 SUPERNOVA REMNANT SHELL: CHARACTERIZING THE DUST AND GAS PROPERTIES

    Energy Technology Data Exchange (ETDEWEB)

    Temim, Tea; Arendt, Richard G. [Observational Cosmology Lab, Code 665, NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Slane, Patrick [Harvard-Smithsonian Center for Astrophysics, 60 Garden Street, Cambridge, MA 02138 (United States); Dwek, Eli, E-mail: tea.temim@nasa.gov [Oak Ridge Associated Universities (ORAU), Oak Ridge, TN 37831 (United States)

    2012-01-20

    We present deep Chandra observations and Spitzer Space Telescope infrared (IR) spectroscopy of the shell in the composite supernova remnant (SNR) Kes 75 (G29.7-0.3). The remnant is composed of a central pulsar wind nebula and a bright partial shell in the south that is visible at radio, IR, and X-ray wavelengths. The X-ray emission can be modeled by either a single thermal component with a temperature of {approx}1.5 keV, or with two thermal components with temperatures of 1.5 and 0.2 keV. Previous studies suggest that the hot component may originate from reverse-shocked supernova (SN) ejecta. However, our new analysis shows no definitive evidence for enhanced abundances of Si, S, Ar, Mg, and Fe, as expected from SN ejecta, or for the IR spectral signatures characteristic of confirmed SN condensed dust, thus favoring a circumstellar or interstellar origin for the X-ray and IR emission. The X-ray and IR emission in the shell are spatially correlated, suggesting that the dust particles are collisionally heated by the X-ray emitting gas. The IR spectrum of the shell is dominated by continuum emission from dust with little, or no line emission. Modeling the IR spectrum shows that the dust is heated to a temperature of {approx}140 K by a relatively dense, hot plasma that also gives rise to the hot X-ray emission component. The density inferred from the IR emission is significantly higher than the density inferred from the X-ray models, suggesting a low filling factor for this X-ray emitting gas. The total mass of the warm dust component is at least 1.3 Multiplication-Sign 10{sup -2} M{sub Sun }, assuming no significant dust destruction has occurred in the shell. The IR data also reveal the presence of an additional plasma component with a cooler temperature, consistent with the 0.2 keV gas component. Our IR analysis therefore provides an independent verification of the cooler component of the X-ray emission. The complementary analyses of the X-ray and IR emission provide

  12. Infrared and X-Ray Spectroscopy of the Kes 75 Supernova Shell Characterizing the Dust and Gas Properties

    Science.gov (United States)

    Temim, Tea; Arendt, Richard G.; Dwek, Eli; Slane, Patrick

    2012-01-01

    We present deep Chandra observations and Spitzer Space Telescope infrared (IR) spectroscopy of the shell in the composite supernova remnant (SNR) Kes 75 (G29.7-0.3). The remnant is composed of a central pulsar wind nebula and a bright partial shell in the south that is visible at radio, IR, and X-ray wavelengths. The X-ray emission can be modeled by either a single thermal component with a temperature of approx 1.5 keV, or with two thermal components with temperatures of 1.5 and 0.2 keY. Previous studies suggest that the hot component may originate from reverse-shocked SN ejecta. However, our new analysis shows no definitive evidence for enhanced abundances of Si, S, Ar, Mg, and Fe, as expected from supernova (SN) ejecta, or for the IR spectral signatures characteristic of confirmed SN condensed dust, thus favoring a circumstellar or interstellar origin for the X-ray and IR emission. The X-ray and IR emission in the shell are spatially correlated, suggesting that the dust particles are collisionally heated by the X-ray emitting gas. The IR spectrum of the shell is dominated by continuum emission from dust with little, or no line emission. Modeling the IR spectrum shows that the dust is heated to a temperature of approx 140 K by a relatively dense, hot plasma, that also gives rise to the hot X-ray emission component. The density inferred from the IR emission is significantly higher than the density inferred from the X-ray models, suggesting a low filling factor for this X-ray emitting gas. The total mass of the warm dust component is at least 1.3 x 10(exp -2) Solar Mass, assuming no significant dust destruction has occurred in the shell. The IR data also reveal the presence of an additional plasma component with a cooler temperature, consistent with the 0.2 keV gas component. Our IR analysis therefore provides an independent verification of the cooler component of the X-ray emission. The complementary analyses of the X-ray and IR emission provide quantitative

  13. Using X-ray spectroscopy of relativistic laser plasma interaction to reveal parametric decay instabilities : A modeling tool for astrophysics

    OpenAIRE

    Oks, E; Dalimier, E.; Faenov, A. Ya; Angelo, P.; Pikuz, S. A.; Tubman, E.; Butler, N. M H; Dance, R. J.; Pikuz, T. A.; Skobelev, I. Yu.; Alkhimova, M. A.; Booth, N.; Green, J.; Gregory, C; Andreev, A.

    2017-01-01

    By analyzing profiles of experimental x-ray spectral lines of Si XIV and Al XIII, we found that both Langmuir and ion acoustic waves developed in plasmas produced via irradiation of thin Si foils by relativistic laser pulses (intensities ∼1021 W/cm2). We prove that these waves are due to the parametric decay instability (PDI). This is the first time that the PDI-induced ion acoustic turbulence was discovered by the x-ray spectroscopy in laser-produced plasmas. These conclusions are also suppo...

  14. Soft X-ray spectroscopy of single sized CdS nanocrystals: size confinement and electronic structure

    Science.gov (United States)

    Lüning, J.; Rockenberger, J.; Eisebitt, S.; Rubensson, J.-E.; Karl, A.; Kornowski, A.; Weller, H.; Eberhardt, W.

    1999-08-01

    Soft X-ray spectroscopy of CdS nanocrystals within their crystalline superlattice allows to relate unambiguously, changes of the electronic structure with the particle size and shape which is known from single crystal X-ray diffraction. We find that the valence and conduction band edge shift contribute to the same extent to the total band gap opening of about 2 eV with respect to CdS bulk as the particle size decreases to 10 Å. Taking a finite height of the potential walls into account, we can reproduce these results within an effective mass approximation model.

  15. X-Ray Spectroscopy: An Experimental Technique to Measure Charge State Distribution Right at the Ion-Solid Interaction

    CERN Document Server

    Sharma, Prashant

    2015-01-01

    Charge state distributions of $^{56}$Fe and $^{58}$Ni projectile ions passing through thin carbon foils have been studied in the energy range of 1.44 - 2.69 MeV/u using a novel method from the x-ray spectroscopy technique. Interestingly the charge state distribution in the bulk show Lorentzian behavior instead of usual Gaussian distribution. Further, different parameters of charge state distribution like mean charge state, distribution width and asymmetric parameter are determined and compared with the empirical calculations and ETACHA predictions. It is found that the x-ray measurement technique is appropriate to determine the mean charge state right at the interaction zone or in the bulk. Interestingly, empirical formalism predicts much lower projectile mean charge states compare to x-ray measurements which clearly indicate multi-electron capture from the target surface. The ETACHA predictions and experimental results are found to be comparable for energies $\\geq$ 2 MeV/u.

  16. Diagnosis of a two wire X-pinch by X-ray absorption spectroscopy utilizing a doubly curved ellipsoidal crystal

    Energy Technology Data Exchange (ETDEWEB)

    Cahill, A. D., E-mail: adc87@cornell.edu; Hoyt, C. L., E-mail: adc87@cornell.edu; Shelkovenko, T. A., E-mail: adc87@cornell.edu; Pikuz, S. A., E-mail: adc87@cornell.edu; Hammer, D. A., E-mail: adc87@cornell.edu [Cornell University, 439 Rhodes Hall, Ithaca, NY 14853 (United States)

    2014-12-15

    X-ray absorption spectroscopy is a powerful tool for the diagnosis of plasmas over a wide range of both temperature and density. However, such a measurement is often limited to probing plasmas with temperatures well below that of the x-ray source in order to avoid object plasma emission lines from obscuring important features of the absorption spectrum. This has excluded many plasmas from being investigated by this technique. We have developed an x-ray spectrometer that provides the ability to record absorption spectra from higher temperature plasmas than the usual approach allows without the risk of data contamination by line radiation emitted by the plasma under study. This is accomplished using a doubly curved mica crystal which is bent both elliptically and cylindrically. We present here initial absorption spectra obtained from an aluminum x-pinch plasma.

  17. X-ray absorption spectroscopy study of granular Fe / Si{sub 3}N{sub 4} systems

    Energy Technology Data Exchange (ETDEWEB)

    Jimenez-Villacorta, F; Castro, G R [SpLine-Spanish CRG beamline at the European Synchrotron Radiation Facility, BP-220 38043 Grenoble Cedex (France) (France); Prieto, C, E-mail: jimenezv@esrf.f [Instituto de Ciencia de Materiales de Madrid, Consejo Superior de Investigaciones Cientificas. Cantoblanco, 28049 - Madrid (Spain)

    2009-11-15

    [Fe (t{sup Fe}) / Si{sub 3}N{sub 4} (3 nm)] multilayers were prepared by sequential magnetron sputtering. The Fe layer thickness has been varied for every sample. Magnetic properties show a gradual evolution from a ferromagnetic state for samples with larger metal thickness to a granular behaviour for the samples with the smallest Fe layer thickness. Microstructural features such as average thickness and granularity, as well as the local order around Fe atoms, were studied by x-ray reflectometry and x-ray absorption spectroscopy, respectively. X-ray reflectometry suggests that the formation of discontinuous metal-insulator multilayers is produced at t{sup Fe} {<=} 1.3 nm. Extended x-ray absorption fine structure (EXAFS) analysis shows a reduction, of the Fe-Fe coordination shell as the metal layer thickness decreases. Moreover, a new phase emerges, and it is visible at the samples with t{sup Fe} {<=} 1.3 nm. This coordination shell is attributed to the formation of Fe-N bonds likely placed at the interface regions. X-ray absorption near edge spectroscopy (XANES) at the Fe K-edge shows as well the evolution from the metallic spectrum to a combined contribution of 2 phases as the metal layer thickness decreases. XANES calculations performed within the real-space multiple-scattering formalism of two nanometric phases for metal bcc Fe and tetrahedral FeN in zinc-blende structure provide a successful explanation of the XANES spectral evolution. The appearance of a new phase linked to the interface regions obtained by X-ray absorption analysis suggests the granular morphology of samples with t{sup Fe} {<=} 1.3 nm.

  18. Ultrafast x-ray photoelectron spectroscopy in the microsecond time domain

    Energy Technology Data Exchange (ETDEWEB)

    Höfert, O.; Gleichweit, C.; Steinrück, H.-P.; Papp, C. [Lehrstuhl für Physikalische Chemie II, Universität Erlangen-Nürnberg, Egerlandstr. 3, 91058 Erlangen (Germany)

    2013-09-15

    We introduce a new approach for ultrafast in situ high-resolution X-ray photoelectron spectroscopy (XPS) to study surface processes and reaction kinetics on the microsecond timescale. The main idea is to follow the intensity at a fixed binding energy using a commercial 7 channeltron electron analyzer with a modified signal processing setup. This concept allows for flexible switching between measuring conventional XP spectra and ultrafast XPS. The experimental modifications are described in detail. As an example, we present measurements for the adsorption and desorption of CO on Pt(111), performed at the synchrotron radiation facility BESSY II, with a time resolution of 500 μs. Due to the ultrafast measurements, we are able to follow adsorption and desorption in situ at pressures of 2 × 10{sup −6} mbar and temperatures up to 500 K. The data are consistently analyzed using a simple model in line with data obtained with conventional fast XPS at temperatures below 460 K. Technically, our new approach allows measurement on even shorter timescales, down to 20 μs.

  19. {sup 57}Fe Moessbauer spectroscopy and x-ray diffraction study of some complex metamict minerals

    Energy Technology Data Exchange (ETDEWEB)

    Malczewski, Dariusz, E-mail: malczews@us.edu.pl [University of Silesia, Faculty of Earth Sciences (Poland); Frackowiak, Janusz E., E-mail: jfrack@us.edu.pl [University of Silesia, Faculty of Computer and Materials Science (Poland); Galuskin, Evgeny V., E-mail: galuskin@us.edu.pl [University of Silesia, Faculty of Earth Sciences (Poland)

    2005-11-15

    Metamict minerals are a class of natural amorphous materials which were initially crystalline but self-radiation damage mainly from alpha decays of {sup 238}U and {sup 232}Th series inside the structure can produce partially or fully amorphization (metamictization) of these minerals. This paper reports the results of {sup 57}Fe Moessbauer spectroscopy, gamma-ray spectrometry and X-ray diffraction (XRD) study of some complex metamict minerals like: davidite-(La), gadolinite, steenstrupine-(Ce), vesuvianite and comparatively epidote. The absorbed {alpha}-dose for these minerals varies in wide range from 1.9 x 10{sup 14} {alpha}-decay/mg (epidote) to as high as 2.7 x 10{sup 16} {alpha}-decay/mg (steenstrupine). The Moessbauer spectra show decreasing IS values (except steenstrupine) for Fe{sup 2+} components with absorbed {alpha}-dose. Rather unexpected feature of these spectra is a noticeable decrease of the spectral line widths with increasing absorbed {alpha}-dose both Fe{sup 2+} and Fe{sup 3+} components in gadolinite, davidite and steenstrupine.

  20. Reactive ZnO/Ti/ZnO interfaces studied by hard x-ray photoelectron spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Knut, Ronny, E-mail: Ronny.Knut@physics.gu.se; Lindblad, Rebecka; Rensmo, Håkan; Karis, Olof [Department of Physics and Astronomy, Uppsala University, Box 516, 75120 Uppsala (Sweden); Grachev, Sergey; Faou, Jean-Yvon; Søndergård, Elin [Unité Mixte CNRS/Sain-Gobain Recherche, 39 Quai Lucien Lefranc, 93303 Aubervilliers (France); Gorgoi, Mihaela [Helmholtz-Zentrum Berlin für Materialien und Energie, Albert-Einstein-Str. 15, D-12489 Berlin (Germany)

    2014-01-28

    The chemistry and intermixing at buried interfaces in sputter deposited ZnO/Ti/ZnO thin layers were studied by hard x-ray photoelectron spectroscopy. The long mean free path of the photoelectrons allowed for detailed studies of the oxidation state, band bending effects, and intrinsic doping of the buried interfaces. Oxidation of the Ti layer was observed when ZnO was deposited on top. When Ti is deposited onto ZnO, Zn Auger peaks acquire a metallic character indicating a strong reduction of ZnO at the interface. Annealing of the stack at 200 °C results in further reduction of ZnO and oxidation of Ti. Above 300 °C, oxygen transport from the bulk of the ZnO layer takes place, leading to re-oxidation of ZnO at the interface and further oxidation of Ti layer. Heating above 500 °C leads to an intermixing of the layers and the formation of a Zn{sub x}TiO{sub y} compound.

  1. X-ray spectroscopy as a probe for lithium polysulfide radicals.

    Science.gov (United States)

    Pascal, Tod A; Pemmaraju, C D; Prendergast, David

    2015-03-28

    The discharge mechanism in lithium sulfur batteries is still unknown and has been purported to involve significant concentrations of polysulfide radicals. Methods capable of quantifying these species in solution are therefore of paramount importance to revealing electrochemical pathways. Here we utilize DFT based X-ray Absorption Spectroscopy (XAS) simulations at the sulfur K-edge to obtain the spectra of polysulfide molecules in neutral, radical (-1) and dianionic (-2) charge states. Our calculations indicate that, contrary to recent propositions, the observed low energy, pre-edge feature in S K-edge XAS near 2470 eV is not exclusively due to radical species, but rather arises predominantly from core-excitations of terminal atoms, at the ends of linear polysulfides, to σ* orbitals, consistent with our previous results for the dianionic species. We do however find a spectral feature unique to radicals, lying 0.5-1 eV below the established pre-edge, that arises from 1s → π* transitions of the terminal atoms. Existing measurements on polysulfides show no evidence for such transitions. We predict that detection of linear radicals in polysulfide mixtures using XAS is limited to high mole fractions (>20%), due to the relatively weak XAS intensity of this π* feature.

  2. X-ray photoelectron spectroscopy studies on single crystalline β-FeSi{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Mao, Wei, E-mail: mao@nuclear.jp [The Micro Analysis Laboratory, Tandem Accelerator, The University Museum, The University of Tokyo, 2-11-16 Yayoi, Bunkyo-ku, Tokyo 113-0032 (Japan); Department of Nuclear Engineering and Management, School of Engineering, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656 (Japan); Udono, Haruhiko [Department of Electrical and Electronic Engineering, Ibaraki University, Hitachi, Ibaraki 316-8511 (Japan); Yamaguchi, Kenji [Quantum Beam Science Directorate, Japan Atomic Energy Agency, 2-4 Shirakata-shirane, Tokai, Naka, Ibaraki 319-1195 (Japan); Terai, Takayuki [Department of Nuclear Engineering and Management, School of Engineering, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656 (Japan); Matsuzaki, Hiroyuki [The Micro Analysis Laboratory, Tandem Accelerator, The University Museum, The University of Tokyo, 2-11-16 Yayoi, Bunkyo-ku, Tokyo 113-0032 (Japan); Department of Nuclear Engineering and Management, School of Engineering, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656 (Japan)

    2016-05-01

    In order to realize the photoluminescence of semiconducting β-FeSi{sub 2} homoepitaxial films, surface preparation of single crystalline β-FeSi{sub 2} is of critical importance. An atomically flat and clean substrate surface of β-FeSi{sub 2} was prepared by sputtering with 2 keV Ar{sup +} ions or by heating at 850 °C. The structure of the native surface oxide and the removal of this layer were investigated though X-ray photoelectron spectroscopy measurements. No significant deviation of the stoichiometry was detected in the surface region. Our results suggest that a surface prepared in this way is an eligible substrate for homoepitaxy of β-FeSi{sub 2}. - Highlights: • A clean surface of single crystalline (beta)-FeSi{sub 2} was prepared by Ar{sup +} sputtering or by heating. • The removal of surface oxide during the surface treatment is elucidated. • The native surface oxides are identified as SiO{sub 2} on top and SiO{sub x} as the inner layer. • There is no significant deviation of surface stoichiometry on the clean surface.

  3. Charge and lattice stripes studies by X-ray absorption spectroscopy

    CERN Document Server

    Oyanagi, H; Bianconi, A

    2002-01-01

    Lattice effects on superconductivity in high Tc oxide superconductors were investigated by X-ray absorption spectroscopy (XAS) giving a snapshot of local lattice distortions with a time scale of 10 sup - sup 1 sup 5 sec. Local structures of Bi sub 2 Sr sub 2 CaCu sub 2 O sub 8 , La sub 1 sub . sub 8 sub 5 Sr sub 0 sub . sub 1 sub 5 CuO sub 4 , YBa sub 2 Cu sub 3 O sub y and La sub 1 sub . sub 4 sub 8 Sr sub 0 sub . sub 1 sub 2 Nd sub 0 sub . sub 4 CuO sub 4 were investigated by polarized XAS over a wide temperature range. We found that the local lattice fluctuation in these materials increases at low temperature, segregates into distorted and undistorted domains, and finally forms a charge and lattice stripe. Local lattice distortions involve the elongated in-plane Cu-O bonds which introduce charge fluctuation or instability leading to ordering into localized and itinerant domains. Also at characteristic temperatures such as Tc and T, pronounced phonon anomalies were observed in the in-plane Cu-O stretching v...

  4. Electronic structure of advanced materials studied by x-ray emission spectroscopy

    Science.gov (United States)

    Kurmaev, E. Z.; Galakhov, V. R.; Yarmoshenko, Yu. M.; Trofimova, V. A.; Shamin, S. N.; Cherkashenko, V. M.; Poteryaev, A. I.; Anisimov, V. I.

    1997-01-01

    High resolution soft x-ray emission spectroscopy with high spatial resolution is used to study of the electronic structure and characterize advanced materials: high-Tc superconductors, transition metal compounds, porous silicon, solid-solid buried interfaces and hard materials. In high-Tc, the main attention is focused on the analysis of oxygen-cation interactions and the determination of the location of impurity atoms. In transition metal compounds the participation of different electronic states of constitute atoms in the valence band is analyzed and correctness of LDA band structure calculations is estimated. For CuFeO2 an unusual mutual position of the Cu3d and Fe3d bands was found which is attributed to strong electron-electron correlations. In porous silicon the local structure of silicon atoms is found to depend on the type of doping of the initial Si wafer. Solid-solid buried interfaces in thin semiconducting films irradiated by eximer laser are investigated. For the hard materials boron-carbonitride a structure consisting of hexagonal lattice planes of carbon and boron nitride is proposed.

  5. Optical and X-ray absorption spectroscopy in lead doped lithium fluoride crystals

    Energy Technology Data Exchange (ETDEWEB)

    Somma, F; Aloe, P; D' Acapito, F; Montereali, R M; Polosan, S; Secu, M; Vincenti, M A, E-mail: somma@fis.uniroma3.it

    2010-11-15

    LiF:Pb doped crystals were successfully grown by Kyropoulos method, starting with drying powders. The presence of Pb{sup 2+} ions in the LiF crystals were evidenced by the absorption band at 278 nm and by 375 nm photoluminescence. The presence of some other Pb structures with oxygen compounds in the as made samples was evidenced, decreasing after some annealing procedures. The local environment and valence state of Pb in LiF were studied by X-ray Absorption Spectroscopy at the Pb L{sub III} and L{sub I} edges. XANES data reveal that Pb is present as Pb{sup 2+} whereas EXAFS data show that it is incorporated in the crystal and not forming PbF{sub 2} precipitates. Identical spectra are obtained for samples as prepared and after thermal annealing up to 650 deg. C demonstrating the stability of the incorporation site. Also the concentration of Pb in the crystal has no effect on the location site of the metal as the same spectrum is obtained for specimens with different dopant concentrations.

  6. Closing the pressure gap in x-ray photoelectron spectroscopy by membrane hydrogenation

    Energy Technology Data Exchange (ETDEWEB)

    Delmelle, Renaud; Borgschulte, Andreas, E-mail: andreas.borgschulte@empa.ch [Laboratory for Advanced Analytical Technologies, Swiss Federal Laboratories for Materials Science and Technology (Empa), Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); Laboratory for Hydrogen and Energy, Swiss Federal Laboratories for Materials Science and Technology (Empa), Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); Probst, Benjamin; Alberto, Roger [Department of Chemistry, University of Zürich (UZH), CH-8057 Zürich (Switzerland); Züttel, Andreas [Laboratory for Hydrogen and Energy, Swiss Federal Laboratories for Materials Science and Technology (Empa), Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); Ecole Polytechnique Fédérale de Lausanne (EPFL), SB, ISIC, LMER, CH-1015 Lausanne (Switzerland); Bleiner, Davide [Laboratory for Advanced Analytical Technologies, Swiss Federal Laboratories for Materials Science and Technology (Empa), Überlandstrasse 129, CH-8600 Dübendorf (Switzerland)

    2015-05-15

    Comprehensive studies of gas-solid reactions require the in-situ interaction of the gas at a pressure beyond the operating pressure of ultrahigh vacuum (UHV) X-ray photoelectron spectroscopy (XPS). The recent progress of near ambient pressure XPS allows to dose gases to the sample up to a pressure of 20 mbar. The present work describes an alternative to this experimental challenge, with a focus on H{sub 2} as the interacting gas. Instead of exposing the sample under investigation to gaseous hydrogen, the sample is in contact with a hydrogen permeation membrane, through which hydrogen is transported from the outside to the sample as atomic hydrogen. Thereby, we can reach local hydrogen concentrations at the sample inside an UHV chamber, which is equipped with surface science tools, and this corresponds to a hydrogen pressure up to 1 bar without affecting the sensitivity or energy resolution of the spectrometer. This experimental approach is validated by two examples, that is, the reduction of a catalyst precursor for CO{sub 2} hydrogenation and the hydrogenation of a water reduction catalyst for photocatalytic H{sub 2} production, but it opens the possibility of the new in situ characterisation of energy materials and catalysts.

  7. Band alignments in Fe/graphene/Si(001) junctions studied by x-ray photoemission spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Le Breton, J.-C., E-mail: jean-christophe.lebreton@univ-rennes1.fr; Tricot, S.; Delhaye, G.; Lépine, B.; Turban, P.; Schieffer, P. [Département Matériaux et Nanosciences, Institut de Physique de Rennes, UMR 6251, CNRS-Université de Rennes 1, Campus de Beaulieu, Bât 11 E, 35042 Rennes Cedex (France)

    2016-08-01

    The control of tunnel contact resistance is of primary importance for semiconductor-based spintronic devices. This control is hardly achieved with conventional oxide-based tunnel barriers due to deposition-induced interface states. Manipulation of single 2D atomic crystals (such as graphene sheets) weakly interacting with their substrate might represent an alternative and efficient way to design new heterostructures for a variety of different purposes including spin injection into semiconductors. In the present paper, we study by x-ray photoemission spectroscopy the band alignments and interface chemistry of iron–graphene-hydrogenated passivated silicon (001) surfaces for a low and a high n-doping concentration. We find that the hydrogen passivation of the Si(001) surface remains efficient even with a graphene sheet on the Si(001) surface. For both doping concentrations, the semiconductor is close to flat-band conditions which indicates that the Fermi level is unpinned on the semiconductor side of the Graphene/Si(001):H interface. When iron is deposited on the graphene/Si(001):H structures, the Schottky barrier height remains mainly unaffected by the metallic overlayer with a very low barrier height for electrons, a sought-after property in semiconductor based spintronic devices. Finally, we demonstrate that the graphene layer intercalated between the metal and semiconductor also serves as a protection against iron-silicide formation even at elevated temperatures preventing from the formation of a Si-based magnetic dead layer.

  8. Recent Advances in the Study of Black Holes using X-ray Reflection Spectroscopy

    Science.gov (United States)

    Garcia, Javier; Dauser, Thomas; Wilms, Joern; Kallman, Timothy; Harrison, Fiona

    2018-01-01

    Reflection spectroscopy has proven to be a versatile tool for the study of accreting black holes. It enables assessment of key physical parameters related to the black hole (e.g., its spin); of the accretion disk (e.g., inner radius, inclination, ionization state and iron abundance); and, more recently, the of the corona that produces the X-ray emission (e.g., temperature, optical depth, and geometry). We present an overview of the state of the art of the models most commonly used, highlighting their limitations and recent developments, which include, but are not limited to, the implementation of a physical Comptonization model for the illumination of the disk, the calculation of reflection models for high densities, and the improvement of the ray tracing techniques used to simulate the relativistic effects affecting the observed spectra. We also discuss current outstanding issues in the interpretation of the observational data, such as the large iron abundances frequently required to fit the reflection spectra of both black hole binaries and AGN.

  9. Molybdenum and selenium speciation in uranium mine tailings using x-ray absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Essilfie-Dughan, J.; Hendry, M.J.; Pickering, I.; George, G., E-mail: joe377@mail.usask.ca [Univ. of Saskatchewan, Dept. of Geological Sciences, Saskatoon, SK (Canada); Kotzer, T. [Univ. of Saskatchewan, Dept. of Geological Sciences, Saskatoon, SK (Canada); Cameco Corp., Saskatoon, SK (Canada)

    2010-07-01

    Mined uranium (U) ore often contains relatively high concentrations of elements (other than uranium) that may be deleterious to the environment. These include molybdenum (Mo) and selenium (Se), which are liberated from uranium oxides and associated sulphide minerals during milling processing. A critical environmental concern in the U mining industry is the possibility of long-term mobilization of elements such as Mo and Se from tailings deposited in in-pit tailings facilities to regional groundwater systems. In this study, x-ray absorption spectroscopy (XAS) was used to study the molecular speciation of these elements of concern (EOC) in samples from the Deilmann Tailings Management Facility (DTMF) at Key Lake in northern Saskatchewan, Canada. An understanding of Mo and Se speciation will help to characterize their long-term stability and evolution in the mine tailings. Results indicate Mo exists mainly as molybdate (+6 oxidation state) and Se exists mainly as selenite (+4 oxidation state). Linear combination fitting (LCF) analysis of the Mo K-edge XANES spectra on tailings samples using standard reference compounds suggests various proportions of NiMoO{sub 4} and CaMoO{sub 4} complexes as well as molybdate adsorbed onto ferrihydrite. (author)

  10. Magneto-optical reflection spectroscopy on graphene/Co in the soft x-ray range

    Science.gov (United States)

    Mertins, H.-Ch.; Jansing, C.; Gilbert, M.; Krivenkov, M.; Sanchez-Barriga, J.; Varykhalov, A.; Rader, O.; Wahab, H.; Timmers, H.; Gaupp, A.; Tesch, M.; Sokolov, A.; Legut, D.; Oppeneer, P. M.

    2017-10-01

    The existence of ferromagnetic ordering in graphene on cobalt is demonstrated by means of resonant magnetic reflection spectroscopy exploiting the transversal magneto-optical Kerr-effect (T-MOKE). Using linearly polarized synchrotron radiation in the soft x-ray range with energies spanning the carbon 1s edge, the π- and σ- bonds of graphene were excited individually, showing that magnetism in graphene is carried by the π – orbitals. Magnetic signals were detected over a wide energy range from 257 – 340 eV with a T-MOKE peak value of 1.1 % at the π – resonance energy near 285 eV. By comparison with corresponding spectra measured at the 2p edges of the Co substrate, a large induced magnetic moment of 0.14 μB was derived for graphene. Individual hysteresis curves monitored at the Co 2p and C 1s edges show that the carbon magnetism is induced by the Co substrate.

  11. The surface of 1-euro coins studied by X-ray photoelectron spectroscopy

    Science.gov (United States)

    Gou, F.; Gleeson, M. A.; Villette, J.; Kleyn, S. E. F.; Kleyn, A. W.

    2004-03-01

    The two alloy surfaces (pill and ring) that are present on 1-euro coins have been studied by X-ray photoelectron spectroscopy (XPS). Comparison is made between coins from general circulation and coin surfaces that have been subjected to a variety of cleaning and oxidation treatments. The concentrations and possible oxidation states of the metals (nickel, copper and zinc) at the surface were derived from analysis of the 2p 3/2 core levels. The surface atomic ratios measured for the pill and the ring parts of the euro coins were compared to the official bulk ratios. This study shows a clear nickel enrichment of both pill and ring surfaces. Nickel at surface seems to be present mainly in hydroxide form although the chloride form cannot be excluded. A small concentration of zinc was present on the surface of the pill, even though it is not present in the bulk alloy. Evidence of both nickel and zinc surface enrichment is observed for the ring. No surface enrichment is observed for the atomically clean or oxidized alloy surfaces over a 60-h time scale.

  12. The surface of 1-euro coins studied by X-ray photoelectron spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Gou, F.; Gleeson, M.A.; Villette, J.; Kleyn, S.E.F.; Kleyn, A.W

    2004-03-30

    The two alloy surfaces (pill and ring) that are present on 1-euro coins have been studied by X-ray photoelectron spectroscopy (XPS). Comparison is made between coins from general circulation and coin surfaces that have been subjected to a variety of cleaning and oxidation treatments. The concentrations and possible oxidation states of the metals (nickel, copper and zinc) at the surface were derived from analysis of the 2p{sub 3/2} core levels. The surface atomic ratios measured for the pill and the ring parts of the euro coins were compared to the official bulk ratios. This study shows a clear nickel enrichment of both pill and ring surfaces. Nickel at surface seems to be present mainly in hydroxide form although the chloride form cannot be excluded. A small concentration of zinc was present on the surface of the pill, even though it is not present in the bulk alloy. Evidence of both nickel and zinc surface enrichment is observed for the ring. No surface enrichment is observed for the atomically clean or oxidized alloy surfaces over a 60-h time scale.

  13. Investigation of the surface composition of electrodeposited black chromium by X-ray photoelectron spectroscopy

    Science.gov (United States)

    Survilienė, S.; Češūnienė, A.; Jasulaitienė, V.; Jurevičiūtė, I.

    2015-01-01

    The paper reviews black chromium electrodeposited from a trivalent chromium bath containing ZnO as a second main component. The chemical compositions of the top layers of the black chromium coatings were studied by the X-ray photoelectron spectroscopy method. The surface of black chromium was found to be almost entirely covered with organic substances. To gain information on the state of each element in the deposit bulk, the layer-by-layer etching of the black chromium surface with argon gas was used. Analysis of XPS spectra has shown that the top layers of black chromium without zinc are composed of various Cr(III) components, organic substances and metallic Cr, whereas metallic Cr is almost absent in black chromium containing some amount of Zn(II) compounds. The ratios of metal/oxide phases were found to be 10/27 and 2/28 for black chromium without and with zinc, respectively. It has been determined that owing to the presence of ZnO in the Cr(III) bath, the percentage of metallic chromium is substantially reduced in black chromium which is quite important for good solar selective characteristics of the coating. The results confirm some of earlier observations and provide new information on the composition of the near-surface layers.

  14. Speciation of Selenium in Stream Insects Using X-Ray Absorption Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Andrahennadi, R.; Wayland, M.; Pickering, I.J.

    2009-05-28

    Selenium contamination in the environment is a widespread problem affecting insects and other wildlife. Insects occupy a critical middle link and aid in trophic transfer of selenium in many terrestrial and freshwater food chains, but the mechanisms of selenium uptake through the food chain are poorly understood. In particular, biotransformation of selenium by insects into different chemical forms will greatly influence how toxic or benign the selenium is to that organism or to its predators. We have used X-ray absorption spectroscopy (XAS) to identify the chemical form of selenium in insects inhabiting selenium contaminated streams near Hinton, Alberta (Canada). Selenium K near-edge spectra indicate a variability of selenium speciation among the insects that included mayflies (Ephemeroptera), stoneflies (Plecoptera), caddisflies (Trichoptera), and craneflies (Diptera). Higher percentages of inorganic selenium were observed in primary consumers, detritivores, and filter feeders than in predatory insects. Among the organic forms of selenium, organic selenides constituted a major fraction in most organisms. A species modeled as trimethylselenonium was observed during the pupal stage of caddisflies. These results provide insights into how the insects cope with their toxic cargo, including how the selenium is biotransformed into less toxic forms and how it can be eliminated from the insects. More broadly, this study demonstrates the strengths of XAS to probe the effects of heavy elements at trace levels in insects from the field.

  15. Detection of suspended nanoparticles with near-ambient pressure x-ray photoelectron spectroscopy

    Science.gov (United States)

    Kjærvik, Marit; Hermanns, Anja; Dietrich, Paul; Thissen, Andreas; Bahr, Stephan; Ritter, Benjamin; Kemnitz, Erhard; Unger, Wolfgang E. S.

    2017-11-01

    Two systems of suspended nanoparticles have been studied with near-ambient pressure x-ray photoelectron spectroscopy: silver nanoparticles in water and strontium fluoride—calcium fluoride core-shell nanoparticles in ethylene glycol. The corresponding dry samples were measured under ultra high vacuum for comparison. The results obtained under near-ambient pressure were overall comparable to those obtained under ultra high vacuum, although measuring silver nanoparticles in water requires a high pass energy and a long acquisition time. A shift towards higher binding energies was found for the silver nanoparticles in aqueous suspension compared to the corresponding dry sample, which can be assigned to a change of surface potential at the water-nanoparticle interface. The shell-thickness of the core-shell nanoparticles was estimated based on simulated spectra from the National Institute of Standards and Technology database for simulation of electron spectra for surface analysis. With the instrumental set-up presented in this paper, nanoparticle suspensions in a suitable container can be directly inserted into the analysis chamber and measured without prior sample preparation.

  16. Atomic Structure of Pt3Ni Nanoframe Electrocatalysts by in Situ X-ray Absorption Spectroscopy.

    Science.gov (United States)

    Becknell, Nigel; Kang, Yijin; Chen, Chen; Resasco, Joaquin; Kornienko, Nikolay; Guo, Jinghua; Markovic, Nenad M; Somorjai, Gabor A; Stamenkovic, Vojislav R; Yang, Peidong

    2015-12-23

    Understanding the atomic structure of a catalyst is crucial to exposing the source of its performance characteristics. It is highly unlikely that a catalyst remains the same under reaction conditions when compared to as-synthesized. Hence, the ideal experiment to study the catalyst structure should be performed in situ. Here, we use X-ray absorption spectroscopy (XAS) as an in situ technique to study Pt3Ni nanoframe particles which have been proven to be an excellent electrocatalyst for the oxygen reduction reaction (ORR). The surface characteristics of the nanoframes were probed through electrochemical hydrogen underpotential deposition and carbon monoxide electrooxidation, which showed that nanoframe surfaces with different structure exhibit varying levels of binding strength to adsorbate molecules. It is well-known that Pt-skin formation on Pt-Ni catalysts will enhance ORR activity by weakening the binding energy between the surface and adsorbates. Ex situ and in situ XAS results reveal that nanoframes which bind adsorbates more strongly have a rougher Pt surface caused by insufficient segregation of Pt to the surface and consequent Ni dissolution. In contrast, nanoframes which exhibit extremely high ORR activity simultaneously demonstrate more significant segregation of Pt over Ni-rich subsurface layers, allowing better formation of the critical Pt-skin. This work demonstrates that the high ORR activity of the Pt3Ni hollow nanoframes depends on successful formation of the Pt-skin surface structure.

  17. Magnetism at spinel thin film interfaces probed through soft x-ray spectroscopy techniques

    Energy Technology Data Exchange (ETDEWEB)

    Chopdekar, R.V.; Liberati, M.; Takamura, Y.; Kourkoutis, L. Fitting; Bettinger, J. S.; Nelson-Cheeseman, B. B.; Arenholz, E.; Doran, A.; Scholl, A.; Muller, D. A.; Suzuki, Y.

    2009-12-16

    Magnetic order and coupling at the interfaces of highly spin polarized Fe{sub 3}O{sub 4} heterostructures have been determined by surface sensitive and element specific soft x-ray spectroscopy and spectromicroscopy techniques. At ambient temperature, the interface between paramagnetic CoCr{sub 2}O{sub 4} or MnCr{sub 2}O{sub 4} and ferrimagnetic Fe{sub 3}O{sub 4} isostructural bilayers exhibits long range magnetic order of Co, Mn and Cr cations which cannot be explained in terms of the formation of interfacial MnFe{sub 2}O{sub 4} or CoFe{sub 2}O{sub 4}. Instead, the ferrimagnetism is induced by the adjacent Fe{sub 3}O{sub 4} layer and is the result of the stabilization of a spinel phase not achievable in bulk form. Magnetism at the interface region is observable up to 500 K, far beyond the chromite bulk Curie temperature of 50-95 K.

  18. CHARACTERIZING SURFACE LAYERS IN NITINOL USING X-RAY PHOTOELECTRON SPECTROSCOPY

    Energy Technology Data Exchange (ETDEWEB)

    Christopfel, R.; Mehta, A.

    2008-01-01

    Nitinol is a shape memory alloy whose properties allow for large reversible deformations and a return to its original geometry. This nickel-titanium (NiTi) alloy has become a material used widely in the biomedical fi eld as a stent to open up collapsed arteries. Both ambient and biological conditions cause surface oxidation in these devices which in turn change its biocompatibility. The thickness of oxidized layers can cause fractures in the material if too large and can allow for penetration if too thin. Depending on the type and abundance of the chemical species on or near the surface, highly toxic metal ions can leak into the body causing cell damage or even cell death. Thus, biocompatibility of such devices is crucial. By using highly surface sensitive x-ray photoelectron spectroscopy to probe the surface of these structures, it is possible to decipher both layer composition and layer thickness. Two samples, both of which were mechanically polished, were investigated. Of the two samples, one was then exposed to a phosphate buffered saline (PBS) solution to mimic the chemical properties of blood, while the other remained unexposed. Although both samples were found to have oxide layers of appropriate thickness (on the order of a few nm), it was found that the sample exposed to the saline solution had a slightly thicker oxide layer and more signifi cantly, a phosphate layer very near the surface suggesting toxic metal components are well contained within the sample. These are considerable indications of a biocompatible device.

  19. THE CHANDRA MULTI-WAVELENGTH PROJECT: OPTICAL SPECTROSCOPY AND THE BROADBAND SPECTRAL ENERGY DISTRIBUTIONS OF X-RAY-SELECTED AGNs

    Energy Technology Data Exchange (ETDEWEB)

    Trichas, Markos; Green, Paul J.; Aldcroft, Tom; Kim, Dong-Woo; Mossman, Amy [Harvard-Smithsonian Center for Astrophysics, Cambridge, MA 02138 (United States); Silverman, John D. [Institute for the Physics and Mathematics of the Universe (IPMU), University of Tokyo, Kashiwanoha 5-1-5, Kashiwa-shi, Chiba 277-8568 (Japan); Barkhouse, Wayne [Department of Physics and Astrophysics, University of North Dakota, Grand Forks, ND 58202 (United States); Cameron, Robert A. [W. W. Hansen Experimental Physics Laboratory, Kavli Institute for Particle Astrophysics and Cosmology, Department of Physics and SLAC National Accelerator Laboratory, Stanford University, Stanford, CA 94305 (United States); Constantin, Anca [Department of Physics and Astronomy, James Madison University, PHCH, Harrisonburg, VA 22807 (United States); Ellison, Sara L. [Department of Physics and Astronomy, University of Victoria, Victoria, BC V8P 1A1 (Canada); Foltz, Craig [Division of Astronomical Sciences, National Science Foundation, 4201 Wilson Blvd., Arlington, VA 22230 (United States); Haggard, Daryl [Center for Interdisciplinary Exploration and Research in Astrophysics, Northwestern University, 2145 Sheridan Road, Evanston, IL 60208 (United States); Jannuzi, Buell T. [NOAO, Kitt Peak National Observatory, Tucson, AZ 85726 (United States); Marshall, Herman L. [Kavli Institute for Astrophysics and Space Research, Massachusetts Institute of Technology, 77 Massachusetts Ave., Cambridge, MA 02139 (United States); Perez, Laura M. [Department of Astronomy, California Institute of Technology, 1200 East California Blvd, Pasadena, CA 91125 (United States); Romero-Colmenero, Encarni [South African Astronomical Observatory, P.O. Box 9, Observatory, 7935 (South Africa); Ruiz, Angel [Osservatorio Astronomico di Brera-INAF, Milan (Italy); Smith, Malcolm G., E-mail: mtrichas@cfa.harvard.edu [Cerro Tololo Interamerican Observatory, La Serena (Chile); and others

    2012-06-01

    From optical spectroscopy of X-ray sources observed as part of the Chandra Multi-wavelength Project (ChaMP), we present redshifts and classifications for a total of 1569 Chandra sources from our targeted spectroscopic follow-up using the FLWO/1.5 m, SAAO/1.9 m, WIYN 3.5 m, CTIO/4 m, KPNO/4 m, Magellan/6.5 m, MMT/6.5 m, and Gemini/8 m telescopes, and from archival Sloan Digital Sky Survey (SDSS) spectroscopy. We classify the optical counterparts as 50% broad-line active galactic nuclei (AGNs), 16% emission line galaxies, 14% absorption line galaxies, and 20% stars. We detect QSOs out to z {approx} 5.5 and galaxies out to z {approx} 3. We have compiled extensive photometry, including X-ray (ChaMP), ultraviolet (GALEX), optical (SDSS and ChaMP-NOAO/MOSAIC follow-up), near-infrared (UKIDSS, Two Micron All Sky Survey, and ChaMP-CTIO/ISPI follow-up), mid-infrared (WISE), and radio (FIRST and NVSS) bands. Together with our spectroscopic information, this enables us to derive detailed spectral energy distributions (SEDs) for our extragalactic sources. We fit a variety of template SEDs to determine bolometric luminosities, and to constrain AGNs and starburst components where both are present. While {approx}58% of X-ray Seyferts (10{sup 42} erg s{sup -1} < L{sub 2-10keV} <10{sup 44} erg s{sup -1}) require a starburst event (>5% starburst contribution to bolometric luminosity) to fit observed photometry only 26% of the X-ray QSO (L{sub 2-10keV} >10{sup 44} erg s{sup -1}) population appear to have some kind of star formation contribution. This is significantly lower than for the Seyferts, especially if we take into account torus contamination at z > 1 where the majority of our X-ray QSOs lie. In addition, we observe a rapid drop of the percentage of starburst contribution as X-ray luminosity increases. This is consistent with the quenching of star formation by powerful QSOs, as predicted by the merger model, or with a time lag between the peak of star formation and QSO

  20. Two-dimensional x-ray correlation spectroscopy of remote core states

    Directory of Open Access Journals (Sweden)

    Daniel Healion

    2014-01-01

    Full Text Available Nonlinear all-X-ray signals that involve large core-atom separation compared to the X-ray wavelengths may not be described by the dipole approximation since they contain additional phase factors. Expressions for the rotationally averaged 2D X-ray photon echo signals from randomly oriented systems that take this position-dependent phase into account for arbitrary ratio between the core separation and the resonant wavelength are presented. Application is made to the Se K-edge of a selenium dipeptide system.

  1. Atom-specific look at the surface chemical bond using x-ray emission spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Nilsson, A.; Wassdahl, N.; Weinelt, M. [Uppsala Univ. (Sweden)] [and others

    1997-04-01

    CO and N{sub 2} adsorbed on the late transition metals have become prototype systems regarding the general understanding of molecular adsorption. It is in general assumed that the bonding of molecules to transition metals can be explained in terms of the interaction of the frontier HOMO and LUMO molecular orbitals with the d-orbitals. In such a picture the other molecular orbitals should remain essentially the same as in the free molecule. For the adsorption of the isoelectronic molecules CO and N{sub 2} this has led to the so called Blyholder model i.e., a synergetic {sigma} (HOMO) donor and {pi} (LUMO) backdonation bond. The authors results at the ALS show that such a picture is oversimplified. The direct observation and identification of the states related to the surface chemical bond is an experimental challenge. For noble and transition metal surfaces, the adsorption induced states overlap with the metal d valence band. Their signature is therefore often obscured by bulk substrate states. This complication has made it difficult for techniques such as photoemission and inverse photoemission to provide reliable information on the energy of chemisorption induced states and has left questions unanswered regarding the validity of the frontier orbitals concept. Here the authors show how x-ray emission spectroscopy (XES), in spite of its inherent bulk sensitivity, can be used to investigate adsorbed molecules. Due to the localization of the core-excited intermediate state, XE spectroscopy allows an atomic specific separation of the valence electronic states. Thus the molecular contributions to the surface measurements make it possible to determine the symmetry of the molecular states, i.e., the separation of {pi} and {sigma} type states. In all the authors can obtain an atomic view of the electronic states involved in the formation of the chemical bond to the surface.

  2. Synchrotron X-ray microscopy and spectroscopy analysis of iron in hemochromatosis liver and intestines

    Energy Technology Data Exchange (ETDEWEB)

    Ko, J .Y. Peter; Sham, Tsun-Kong; Chakrabarti, Subrata; Adams, Paul C.; (UWO)

    2009-12-01

    Hemochromatosis is a genetic disorder that causes body to store excess iron in organs such as heart or liver. Distribution of iron, as well as copper, zinc and calcium, and chemical identity of iron in hemochromatosis liver and intestine were investigated by X-ray microprobe experiments, which consist of X-ray microscopy and micro-X-ray absorption fine structure. Our results show that iron concentration in hemochromatosis liver tissue is high, while much less Fe is found in intestinal tissue. Moreover, chemical identity of Fe in hemochromatosis liver can be identified. X-ray microprobe experiments allows for examining elemental distribution at an excellent spatial resolution. Moreover, chemical identity of element of interest can be obtained.

  3. XMM-Newton Spectroscopy of the X-ray Detected Broad Absorption Line QSO CSO 755

    Science.gov (United States)

    Brandt, Niel

    2005-01-01

    We present the results from XMM-Newton observations of the highly optically polarized broad absorption line quasar (BALQSO) CSO 755. By analyzing its X-ray spectrum with a total of approximately 3000 photons we find that this source has an X-ray continuum of "typical" radio-quiet quasars, with a photon index of Gamma=1.83, and a rather flat (X-ray bright) intrinsic optical-to-X-ray spectral slope of alpha_ox=- 1.51. The source shows evidence for intrinsic absorption, and fitting the spectrum with a neutral-absorption model gives a column density of N_H approximately 1.2x10^22 cm^{-2}; this is among the lowest X-ray columns measured for BALQSOs. We do not detect, with high significance, any other absorption features in the X-ray spectrum. Upper limits we place on the rest-frame equivalent width of a neutral (ionized) Fe K-alpha line, less than =180 eV (less than =120 eV), and on the Compton-reflection component parameter, R less than =0.2, suggest that most of the X-rays from the source are directly observed rather than being scattered or reflected; this is also supported by the relatively flat intrinsic alpha ox we measure. The possibility that most of the X-ray flux is scattered due to the high level of UV-optical polarization is ruled out. Considering data for 46 BALQSOs from the literature, including CSO 755, we have found that the UV-optical continuum polarization level of BALQSOs is not correlated with any of their X-ray properties. A lack of significant short-term and long-term X-ray flux variations in the source may be attributed to a large black-hole mass in CSO 755. We note that another luminous BALQSO, PG 2112+059, has both similar shallow C IV BALs and moderate X-ray absorption.

  4. Crystal chemistry, surface morphology and X-ray photoelectron spectroscopy of Fe-rich osumilite from Mt. Arci, Sardinia (Italy)

    Science.gov (United States)

    Elmi, Chiara; Brigatti, Maria Franca; Pasquali, Luca; Montecchi, Monica; Laurora, Angela; Malferrari, Daniele; Nannarone, Stefano

    2010-09-01

    Microprobe analysis, single crystal X-ray diffraction, X-ray photoelectron spectroscopy, atomic force microscopy, and X-ray absorption spectroscopy were applied on Fe-rich osumilite from the volcanic massif of Mt. Arci, Sardinia, Italy. Osumilite belongs to the space group P6/ mcc with unit cell parameters a = 10.1550(6), c = 14.306(1) Å and chemical formula (K0.729)C (Na0.029)B (Si10.498 Al1.502)T1 (Al2.706 Fe{0.294/2+})T2 (Mg0.735 Mn0.091 Fe{1.184/2+})AO30. Structure refinement converged at R = 0.0201. Unit cell parameter a is related to octahedral edge length as well as to Fe2+ content, unlike the c parameter which does not seem to be affected by chemical composition. The determination of the amount of each element on the mineral surface, obtained through X-ray photoelectron spectroscopy high-resolution spectra in the region of the Si2p, Al2p, Mg1s and Fe2p core levels, suggests that Fe presents Fe2+ oxidation state and octahedral coordination. Two peaks at 103.1 and 100.6 eV can be related to Si4+ and Si1+ components, respectively, both in tetrahedral coordination. The binding energy of Al2p, at 74.5 eV, indicates that Al is mostly present in the distorted T2 site, whereas the Mg peak at 1,305.2 eV suggests that this cation is located at the octahedral site. X-ray absorption at the Fe L2,3-edges confirms that iron is present in the mineral structure, prevalently in the divalent state and at the A octahedral site.

  5. Soft X-ray Spectroscopy Study of the Electronic Structure of Oxidized and Partially Oxidized Magnetite Nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Gilbert, Benjamin; Katz, Jordan E.; Denlinger, Jonathan D.; Yin, Yadong; Falcone, Roger; Waychunas, Glenn A.

    2010-10-24

    The crystal structure of magnetite nanoparticles may be transformed to maghemite by complete oxidation, but under many relevant conditions the oxidation is partial, creating a mixed-valence material with structural and electronic properties that are poorly characterized. We used X-ray diffraction, Fe K-edge extended X-ray absorption fine structure (EXAFS) spectroscopy, and soft X-ray absorption and emission spectroscopy to characterize the products of oxidizing uncoated and oleic acid-coated magnetite nanoparticles in air. The oxidization of uncoated magnetite nanoparticles creates a material that is structurally and electronically indistinguishable from maghemite. By contrast, while oxidized oleic acid-coated nanoparticles are also structurally indistinguishable from maghemite, Fe L-edge spectroscopy revealed the presence of interior reduced iron sites even after a 2-year period. We used X-ray emission spectroscopy at the O K-edge to study the valence bands (VB) of the iron oxide nanoparticles, using resonant excitation to remove the contributions from oxygen atoms in the ligands and from low-energy excitations that obscured the VB edge. The bonding in all nanoparticles was typical of maghemite, with no detectable VB states introduced by the long-lived, reduced-iron sites in the oleic acid-coated sample. However, O K-edge absorption spectroscopy observed a 0.2 eV shift in the position of the lowest unoccupied states in the coated sample, indicating an increase in the semiconductor band gap relative to bulk stoichiometric maghemite that was also observed by optical absorption spectroscopy. The results show that the ferrous iron sites within ferric iron oxide nanoparticles coated by an organic ligand can persist under ambient conditions with no evidence of a distinct interior phase and can exert an effect on the global electronic and optical properties of the material. This phenomenon resembles the band gap enlargement caused by electron accumulation in the

  6. A novel method for resonant inelastic soft X-ray scattering via photoelectron spectroscopy detection.

    Science.gov (United States)

    Dakovski, Georgi L; Lin, Ming Fu; Damiani, Daniel S; Schlotter, William F; Turner, Joshua J; Nordlund, Dennis; Ogasawara, Hirohito

    2017-11-01

    A method for measuring resonant inelastic X-ray scattering based on the conversion of X-ray photons into photoelectrons is presented. The setup is compact, relies on commercially available detectors, and offers significant flexibility. This method is demonstrated at the Linac Coherent Light Source with ∼0.5 eV resolution at the cobalt L3-edge, with signal rates comparable with traditional grating spectrometers.

  7. Application of confocal X-ray fluorescence micro-spectroscopy to the investigation of paint layers.

    Science.gov (United States)

    Sun, Tianxi; Liu, Zhiguo; Wang, Guangfu; Ma, Yongzhong; Peng, Song; Sun, Weiyuan; Li, Fangzuo; Sun, Xuepeng; Ding, Xunliang

    2014-12-01

    A confocal micro X-ray fluorescence (MXRF) spectrometer based on polycapillary X-ray optics was used for the identification of paint layers. The performance of the confocal MXRF was studied. Multilayered paint fragments of a car were analyzed nondestructively to demonstrate that this confocal MXRF instrument could be used in the discrimination of the various layers in multilayer paint systems. Copyright © 2014 Elsevier Ltd. All rights reserved.

  8. Instrumentations in x-ray plasma polarization spectroscopy. Crystal spectrometer, polarimeter and detectors for astronomical observations

    Energy Technology Data Exchange (ETDEWEB)

    Baronova, Elena O.; Stepanenko, Mikhail M. [RRC Kurchatov Institute, Nuclear Fusion Institute, Moscow (Russian Federation); Jakubowski, Lech [Soltan Institute for Nuclear Studies, Swierk-Otwock (Poland); Tsunemi, Hiroshi [Osaka Univ., Graduate School of Science, Osaka (Japan)

    2002-08-01

    This report discusses the various problems which are encountered when a crystal spectrometer is used for the purpose of observing polarized x-ray lines. A polarimeter is proposed based on the novel idea of using two series of equivalent atomic planes in a single crystal. The present status of the astronomical x-ray detection techniques are described with emphasis on two dimensional detectors which are polarization sensitive. (author)

  9. Probing the influence of X-rays on aqueous copper solutions using time-resolved in situ combined video/X-ray absorption near-edge/ultraviolet-visible spectroscopy

    NARCIS (Netherlands)

    Mesu, J. Gerbrand; Beale, Andrew M.|info:eu-repo/dai/nl/325802068; de Groot, Frank M. F.|info:eu-repo/dai/nl/08747610X; Weckhuysen, Bert M.|info:eu-repo/dai/nl/285484397

    2006-01-01

    Time-resolved in situ video monitoring and ultraviolet-visible spectroscopy in combination with X-ray absorption near-edge spectroscopy (XANES) have been used for the first time in a combined manner to study the effect of synchrotron radiation on a series of homogeneous aqueous copper solutions in a

  10. Application of imaging plates to x-ray imaging and spectroscopy in laser plasma experiments (invited)

    Science.gov (United States)

    Izumi, N.; Snavely, R.; Gregori, G.; Koch, J. A.; Park, H.-S.; Remington, B. A.

    2006-10-01

    We report recent progress in x-ray diagnosis of laser-plasma experiments using imaging plates. Imaging plates are photostimulable phosphor screens [BaF(Br0.85,I0.15):Eu2+] deposited on flexible metal or plastic substrates. We applied imaging plates to x-ray microscopy of inertial confinement fusion experiments. Self-emission x-ray images of imploded cores were obtained successfully with high-magnification, target-mounted pinholes using imaging plates as detectors. Imaging plates were also used in ultraintense laser experiments at the Rutherford Appleton Laboratory, where small samarium foils were irradiated by high intensity laser pulses from the Vulcan laser system. K-shell x rays from the foil (˜40keV) were used as a line x-ray source for one-dimensional microscopic radiography, and the performance of imaging plates on high-energy x-ray backlit radiography experiments was demonstrated by imaging sinusoidal grooves of 6μm amplitude on a Au foil. Detailed K-shell spectra from Cu targets were also obtained by coupling an imaging plate with a highly ordered pyrolytic graphite crystal spectrometer. The performance of the imaging plates as evaluated in actual laser plasma experiments is presented.

  11. Component analyses of urinary nanocrystallites of uric acid stone formers by combination of high-resolution transmission electron microscopy, fast Fourier transformation, energy dispersive X-ray spectroscopy, X-ray diffraction and Fourier transform infrared spectroscopy.

    Science.gov (United States)

    Sun, Xin-Yuan; Xue, Jun-Fa; Xia, Zhi-Yue; Ouyang, Jian-Ming

    2015-06-01

    This study aimed to analyse the components of nanocrystallites in urines of patients with uric acid (UA) stones. X-ray diffraction (XRD), Fourier transform infrared spectroscopy, high-resolution transmission electron microscopy (HRTEM), fast Fourier transformation (FFT) of HRTEM, and energy dispersive X-ray spectroscopy (EDS) were performed to analyse the components of these nanocrystallites. XRD and FFT showed that the main component of urinary nanocrystallites was UA, which contains a small amount of calcium oxalate monohydrate and phosphates. EDS showed the characteristic absorption peaks of C, O, Ca and P. The formation of UA stones was closely related to a large number of UA nanocrystallites in urine. A combination of HRTEM, FFT, EDS and XRD analyses could be performed accurately to analyse the components of urinary nanocrystallites.

  12. High-precision gamma-ray spectroscopy for enhancing production and application of medical isotopes

    Science.gov (United States)

    McCutchan, E. A.; Sonzogni, A. A.; Smith, S. V.; Muench, L.; Nino, M.; Greene, J. P.; Carpenter, M. P.; Zhu, S.; Chillery, T.; Chowdhury, P.; Harding, R.; Lister, C. J.

    2015-10-01

    Nuclear medicine is a field which requires precise decay data for use in planning radionuclide production and in imaging and therapeutic applications. To address deficiencies in decay data, sources of medical isotopes were produced and purified at the Brookhaven Linear Isotope Producer (BLIP) then shipped to Argonne National Laboratory where high-precision, gamma-ray measurements were performed using Gammasphere. New decay schemes for a number of PET isotopes and the impact on dose calculations will be presented. To investigate the production of next-generation theranostic or radiotherapeutic isotopes, cross section measurements with high energy protons have also been explored at BLIP. The 100-200 MeV proton energy regime is relatively unexplored for isotope production, thus offering high discovery potential but at the same time a challenging analysis due to the large number of open channels at these energies. Results of cross sections deduced from Compton-suppressed, coincidence gamma-ray spectroscopy performed at Lowell will be presented, focusing on the production of platinum isotopes by irradiating natural platinum foils with 100 to 200 MeV protons. DOE Isotope Program is acknowledged for funding ST5001030. Work supported by the US DOE under Grant DE-FG02-94ER40848 and Contracts DE-AC02-98CH10946 and DE-AC02-06CH11357.

  13. Fully stabilized mid-infrared frequency comb for high-precision molecular spectroscopy.

    Science.gov (United States)

    Vainio, Markku; Karhu, Juho

    2017-02-20

    A fully stabilized mid-infrared optical frequency comb spanning from 2.9 to 3.4 µm is described in this article. The comb is based on half-harmonic generation in a femtosecond optical parametric oscillator, which transfers the high phase coherence of a fully stabilized near-infrared Er-doped fiber laser comb to the mid-infrared region. The method is simple, as no phase-locked loops or reference lasers are needed. Precise locking of optical frequencies of the mid-infrared comb to the pump comb is experimentally verified at sub-20 mHz level, which corresponds to a fractional statistical uncertainty of 2 × 10-16 at the center frequency of the mid-infrared comb. The fully stabilized mid-infrared comb is an ideal tool for high-precision molecular spectroscopy, as well as for optical frequency metrology in the mid-infrared region, which is difficult to access with other stabilized frequency comb techniques.

  14. Frontiers of QC Laser spectroscopy for high precision isotope ratio analysis of greenhouse gases

    Science.gov (United States)

    Emmenegger, Lukas; Mohn, Joachim; Harris, Eliza; Eyer, Simon; Ibraim, Erkan; Tuzson, Béla

    2016-04-01

    An important milestone for laser spectroscopy was achieved when isotope ratios of greenhouse gases were reported at precision levels that allow addressing research questions in environmental sciences. Real-time data with high temporal resolution at moderate cost and instrument size make the optical approach highly attractive, complementary to the well-established isotope-ratio mass-spectrometry (IRMS) method. Especially appealing, in comparison to IRMS, is the inherent specificity to structural isomers having the same molecular mass. Direct absorption in the MIR in single or dual QCL configuration has proven highly reliable for the sta-ble isotopes of CO2, N2O and CH4. The longest time series of real-time measurements is currently available for δ13C and δ18O in CO2 at the high-alpine station Jung-fraujoch. At this well-equipped site, QCL based direct absorption spectroscopy (QCLAS) measurements are ongoing since 2008 1,2. Applications of QCLAS for N2O and CH4 stable isotopes are considerably more challenging because of the lower atmospheric mixing ratios, especially for the less abundant species, such as N218O and CH3D. For high precision (automated preconcentration unit yielding an up to 500 times concentration increase and the capability to separate the target gas from spectral interferants by se-quential desorption 3. Here, we review our recent developments on high precision isotope ratio analysis of greenhouse gases, with special focus on the isotopic species of N2O and CH4. Furthermore, we show environ-mental applications illustrating the highly valuable information that isotope ratios of atmospheric trace gases can carry. For example, the intramolecular distribution of 15N in N2O gives important information on the geochemical cycle of N2O4-6, while the analysis of δ13C and δ D in CH4 may be applied to disentangle microbial, fossil and landfill sources 7. 1 Sturm, P., Tuzson, B., Henne, S. & Emmenegger, L. Tracking isotopic signatures of CO2 at the high

  15. Inter-Diffusion of Copper and Hafnium as Studied by X-Ray Photoelectron Spectroscopy

    Science.gov (United States)

    Pearson, Justin Seth

    The purpose of this study is to investigate the interdiffusion of copper and hafnium. Thin films (thicknesses ranging from 100 nm to 150 nm) of hafnium were deposited on a silicon substrate. About 80 nm of copper was then deposited on such samples. High purity samples have been used in this investigation. The deposition of the elements was done by the e-beam technique. The interfaces thus formed were annealed for a fixed time (30 minutes) at temperatures of 100, 200, and 300°C. The samples were characterized in situ by the x-ray photoelectron spectroscopy technique. To carry out the depth profiling of these samples a controlled amount of the over layer was removed and the spectral data were acquired. The argon ion sputtering technique was used to sputter the layers away. Spectral data in the copper 2p and hafnium 4f regions were investigated. The atomic concentration of the constituents as a function of depth across the interface was determined by analyzing the areas under the curves. The depth profiling data thus obtained was analyzed by the Matano-Boltzmann's procedure. For this analysis the Matano plane was determined based on the criteria of equal area on each side of the interface. The Fick's Law second law was used to calculate the interdiffuison coefficient for each of these interfaces. The interdiffusion coefficient as a function of temperature was determined from these analyses. From these coefficients the activation energy and the pre-exponential factor was determined by using the Arrhenius plot. The activation energy was found to be 0.128 eV/atom and the pre-exponential factor was 3.33E-14 cm2/s. The results from this investigation will be useful in the application of Cu/Hf interface in design and fabrication of semiconductor devices.

  16. Study of archaeological iron objects by PGAA, Mössbauer spectroscopy and X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Wagner, F. E., E-mail: fwagner@tum.de [Technische Universität München, Physik- Department E15 (Germany); Gebhard, R. [Archäologische Staatssammlung München (Germany); Häusler, W.; Wagner, U. [Technische Universität München, Physik- Department E15 (Germany); Albert, P.; Hess, H. [Archäologische Staatssammlung München (Germany); Révay, Z.; Kudejová, P.; Kleszcz, K. [Technische Universität München, Forschungsneutronenquelle Heinz Maier-Leibnitz (FRM II) (Germany)

    2016-12-15

    Archaeological iron objects often corrode rapidly after their excavation, even though they have survived long times of burial in the ground. Chlorine that accumulates during burial is thought to play a major role in this destructive post-excavation corrosion. It is therefore important for the conservation of such objects to determine the chlorine content in a non-destructive manner and, if necessary, to remove the chlorine from the artefacts by appropriate methods. Such methods are leaching in alkaline solutions or heating in a reducing atmosphere at temperatures up to 800 {sup ∘}C. We have studied the efficiency of the heating method using prompt gamma activation analysis (PGAA) for monitoring the Cl content and Mössbauer spectroscopy at room temperature (RT) and 4.2 K as well as X-ray diffraction to study the mineralogical transformations of the rust layers. The heat treatments were performed a N{sub 2}/H{sub 2} (90/10) mixture at temperatures up to 750 {sup ∘}C. As test specimens sections of iron rods from the Celtic oppidum of Manching (Bavaria) were used. The initial Cl contents of the pieces varied in the range of several hundred ppm, referring to the iron mass. Annealing for 24 h at 350, 550 and 750 {sup ∘}C was found to reduce the Cl contents of the specimens, to about 70, 30 and 15 % of the original values, respectively. The rust consists mainly of goethite with admixtures of magnetite, lepidocrocite and akaganeite, which is thought to be a major carrier of chlorine, probably together with iron chlorides. Much of the goethite is so fine-grained that it does not split magnetically at RT. Annealing converts the rust mainly to maghemite at 350 {sup ∘}C, to magnetite at 550 {sup ∘}C and to wüstite plus magnetite and metallic iron at 750 {sup ∘}C. Pure akaganeite behaves in nearly the same manner.

  17. Multivariate analysis of quaternary carbamazepine-saccharin mixtures by X-ray diffraction and infrared spectroscopy.

    Science.gov (United States)

    Caliandro, Rocco; Di Profio, Gianluca; Nicolotti, Orazio

    2013-05-05

    Co-crystallization brings new opportunities for improving the solubility and dissolution rate of drugs with the chance of finely tuning some relevant chemical-physical properties of mixtures containing bioactive compounds. As co-crystallization process involves several molecular species, which are generally solid at room conditions, its control requires accurate knowledge and monitoring of the different phase that might appear during the formulation stage. In the present study the suitability of X-ray powder diffraction (XRPD) and Fourier-transformed infrared (FTIR) spectroscopy in quantifying mixtures of carbamazepine polymorphs (forms I and III), saccharin, and carbamazepine-saccharin cocrystals (form I) is assessed. Quaternary crystalline mixtures typically produced in the process of co-crystal production were analyzed by multivariate methods. Principal component analysis (PCA) was used for the identification of the crystal phases, while unsupervised simultaneous fitting of the spectra from pure phases, or supervised partial least squares (PLS) methods were used for their quantitative determination. The performance of data analysis was enhanced by applying peculiar pre-processing methods, such as SNIP filtering in case of FTIR and PCA filtering in case of XRPD. It was found that, for XRPD data, the automatic multi-fitting procedures and PLS models developed in this study are able to quantify single phases in mixtures to an accuracy level comparable to that obtained by the widely used Rietveld method, which, however, requires knowledge of the crystal structures. For FTIR data the results here obtained prove that this technique can be used as a fast method for polymorph characterization. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Infrared and X-Ray Spectroscopy of the Kes 75 Supernova Remnant Shell: Characterizing the Dust and Gas Properties

    Science.gov (United States)

    Temim, Tea; Slane, Patrick; Arendt, Richard G.; Dwek, Eli

    2011-01-01

    We present deep Chandra observations and Spitzer Space Telescope infrared (IR) spectroscopy of the shell in the composite supernova remnant (SNR) Kes 75 (G29.7-0.3). The remnant is composed of a central pulsar wind nebula and a bright partial shell in the south that is visible at radio, IR, and X-ray wavelengths. The X-ray emission can be modeled by either a single thermal component with a temperature of approximately 1.5 keY, or with two thermal components with temperatures of 1.5 and 0.2 keY. Previous studies suggest that the hot component may originate from reverse-shocked supernova (SN) ejecta. However, our new analysis shows no definitive evidence for enhanced abundances of Si, S, Ar, Mg, and Fe, as expected from SN ejecta, or for the IR spectral signatures characteristic of confirmed SN condensed dust, thus favoring a circumstellar or interstellar origin for the X-ray and IR emission. The X-ray and IR emission in the shell are spatially correlated, suggesting that the dust particles are collisionally heated by the X-ray emitting gas. The IR spectrum of the shell is dominated by continuum emission from dust with little, or no line emission. Modeling the IR spectrum shows that the dust is heated to a temperature of approximately 140 K by a relatively dense, hot plasma that also gives rise to the hot X-my emission component. The density inferred from the IR emission is significantly higher than the density inferred from the X-ray models, suggesting a low filling factor for this X-my emitting gas. The total mass of the warm dust component is at least 1.3 x 10(exp -2) x solar mass, assuming no significant dust destruction has occurred in the shell. The IR data also reveal the presence of an additional plasma component with a cooler temperature, consistent with the 0.2 keV gas component. Our IR analysis therefore provides an independent verification of the cooler component of the X-ray emission. The complementary analyses of the X-ray and IR emission provide

  19. UV-Raman spectroscopy, X-ray photoelectron spectroscopy, and temperature programmed desorption studies of model and bulk heterogeneous catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Tewell, Craig Richmond [Univ. of California, Berkeley, CA (United States)

    2002-01-01

    X-ray photoelectron spectroscopy (XPS) and Temperature Programmed Desorption (TPD) have been used to investigate the surface structure of model heterogeneous catalysts in ultra-high vacuum (UHV). UV-Raman spectroscopy has been used to probe the structure of bulk model catalysts in ambient and reaction conditions. The structural information obtained through UV-Raman spectroscopy has been correlated with both the UHV surface analysis and reaction results. The present day propylene and ethylene polymerization catalysts (Ziegler-Natta catalysts) are prepared by deposition of TiCl4 and a Al(Et)3 co-catalyst on a microporous Mg-ethoxide support that is prepared from MgCl2 and ethanol. A model thin film catalyst is prepared by depositing metallic Mg on a Au foil in a UHV chamber in a background of TiCl4 in the gas phase. XPS results indicate that the Mg is completely oxidized to MgCl2 by TiCl4 resulting in a thin film of MgCl2/TiClx, where x = 2, 3, and 4. To prepare an active catalyst, the thin film of MgCl2/TiClx on Au foil is enclosed in a high pressure cell contained within the UHV chamber and exposed to ~1 Torr of Al(Et)3.

  20. Bimetallic Catalysts and Platinum Surfaces Studied by X-ray Absorption Spectroscopy and Scanning Tunnelling Microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Roenning, Magnus

    2000-07-01

    Bimetallic catalyst systems used in Fischer-Tropsch synthesis (Co-Re/Al{sub 2}O{sub 3}) and in the naphtha reforming process (Pt-Re/Al{sub 2}O{sub 3}) have been studied in situ using X-ray absorption spectroscopy (EXAFS). Additionally, the adsorption of ethene on platinum single crystal surfaces has been investigated using scanning tunnelling microscopy. In situ EXAFS at the cobalt K absorption edge have been carried out at 450{sup o}C on the hydrogen reduction of a rhenium-promoted Co{sub 3}O{sub 4}/Al{sub 2}O{sub 3} catalyst. Reductions carried out using 100% hydrogen and 5% hydrogen in helium gave different results. Whereas the reduction using dilute hydrogen leads to bulk-like metallic cobalt particles (hcp or fcc), reaction with pure hydrogen yields a more dispersed system with smaller cobalt metal particles (< 40 A). The results are rationalised in terms of different degrees of reoxidation of cobalt by the higher and lower concentrations of water generated during the reduction of cobalt oxide by 100% and 5% hydrogen, respectively. Additionally, in both reduction protocols a small fraction (3 -4 wt%) of the cobalt content is randomly dispersed over the tetrahedral vacancies of the alumina support. This dispersion occurs during reduction and not calcination. The cobalt in these sites cannot be reduced at 450 {sup o}C. The local environments about the rhenium atoms in Co-Re/{gamma}-A1{sub 2}O{sub 3} catalyst after different reduction periods have been studied by X-ray absorption spectroscopy. A bimetallic catalyst containing 4.6 wt% cobalt and 2 wt% rhenium has been compared with a corresponding monometallic sample with 2 wt% rhenium on the same support. The rhenium L{sub III} EXAFS analysis shows that bimetallic particles are formed after reduction at 450{sup o}C with the average particle size being 10-15 A. Rhenium is shown to be reduced at a later stage than cobalt. The fraction of cobalt atoms entering the support obstructs the access to the support for the

  1. NuSTAR HARD X-RAY SURVEY OF THE GALACTIC CENTER REGION. I. HARD X-RAY MORPHOLOGY AND SPECTROSCOPY OF THE DIFFUSE EMISSION

    Energy Technology Data Exchange (ETDEWEB)

    Mori, Kaya; Hailey, Charles J.; Perez, Kerstin; Nynka, Melania; Zhang, Shuo; Canipe, Alicia M. [Columbia Astrophysics Laboratory, Columbia University, New York, NY 10027 (United States); Krivonos, Roman; Tomsick, John A.; Barrière, Nicolas; Boggs, Steven E.; Craig, William W. [Space Sciences Laboratory, University of California, Berkeley, CA 94720 (United States); Hong, Jaesub [Harvard-Smithsonian Center for Astrophysics, Cambridge, MA 02138 (United States); Ponti, Gabriele [Max-Planck-Institut f. extraterrestrische Physik, HEG, Garching (Germany); Bauer, Franz [Instituto de Astrofísica, Facultad de Física, Pontificia Universidad Católica de Chile, 306, Santiago 22 (Chile); Alexander, David M. [Department of Physics, Durham University, Durham DH1 3LE (United Kingdom); Baganoff, Frederick K. [Kavli Institute for Astrophysics and Space Research, Massachusets Institute of Technology, Cambridge, MA 02139 (United States); Barret, Didier [Université de Toulouse, UPS-OMP, IRAP, Toulouse (France); Christensen, Finn E. [DTU Space—National Space Institute, Technical University of Denmark, Elektrovej 327, DK-2800 Lyngby (Denmark); Forster, Karl [Cahill Center for Astronomy and Astrophysics, California Institute of Technology, Pasadena, CA 91125 (United States); Giommi, Paolo, E-mail: kaya@astro.columbia.edu [ASI Science Data Center, Via del Politecnico snc I-00133, Roma (Italy); and others

    2015-12-01

    We present the first sub-arcminute images of the Galactic Center above 10 keV, obtained with NuSTAR. NuSTAR resolves the hard X-ray source IGR J17456–2901 into non-thermal X-ray filaments, molecular clouds, point sources, and a previously unknown central component of hard X-ray emission (CHXE). NuSTAR detects four non-thermal X-ray filaments, extending the detection of their power-law spectra with Γ ∼ 1.3–2.3 up to ∼50 keV. A morphological and spectral study of the filaments suggests that their origin may be heterogeneous, where previous studies suggested a common origin in young pulsar wind nebulae (PWNe). NuSTAR detects non-thermal X-ray continuum emission spatially correlated with the 6.4 keV Fe Kα fluorescence line emission associated with two Sgr A molecular clouds: MC1 and the Bridge. Broadband X-ray spectral analysis with a Monte-Carlo based X-ray reflection model self-consistently determined their intrinsic column density (∼10{sup 23} cm{sup −2}), primary X-ray spectra (power-laws with Γ ∼ 2) and set a lower limit of the X-ray luminosity of Sgr A* flare illuminating the Sgr A clouds to L{sub X} ≳ 10{sup 38} erg s{sup −1}. Above ∼20 keV, hard X-ray emission in the central 10 pc region around Sgr A* consists of the candidate PWN G359.95–0.04 and the CHXE, possibly resulting from an unresolved population of massive CVs with white dwarf masses M{sub WD} ∼ 0.9 M{sub ⊙}. Spectral energy distribution analysis suggests that G359.95–0.04 is likely the hard X-ray counterpart of the ultra-high gamma-ray source HESS J1745–290, strongly favoring a leptonic origin of the GC TeV emission.

  2. In situ study of the Porticello Bronzes by portable X-ray fluorescence and laser-induced breakdown spectroscopy

    Science.gov (United States)

    Ferretti, M.; Cristoforetti, G.; Legnaioli, S.; Palleschi, V.; Salvetti, A.; Tognoni, E.; Console, E.; Palaia, P.

    2007-12-01

    This paper reports the results of a measurement campaign performed at the National Museum of Magna Grecia in Reggio Calabria (Italy). Portable X-Ray Fluorescence (XRF) and Laser-Induced Breakdown Spectroscopy (LIBS) instrumentation allowed in situ analysis of several bronze pieces belonging to the group of the so-called Porticello Bronzes. The find occurred at sea, off the village of Porticello (Reggio Calabria) in 1969 and consists of a number of fragments, including a bearded head, pertaining to at least two statues. The use of X-Ray Fluorescence and Laser-Induced Breakdown Spectroscopy techniques allowed for a classification of the fragments according to their elemental composition. The fragments appear to belong to at least two different statues; although, in general, the compositional classification agrees well with the stylistic analysis of the fragments, significant improvements with respect to previous achievements emerge from the joint results of the two techniques used.

  3. Band structure of TiO sub 2 -doped yttria-stabilized zirconia probed by soft-x-ray spectroscopy

    CERN Document Server

    Higuchi, T; Kobayashi, K; Yamaguchi, S; Fukushima, A; Shin, S

    2003-01-01

    The electronic structure of TiO sub 2 -doped yttria-stabilized zirconia (YSZ) has been studied by soft-X-ray emission spectroscopy (SXES) and X-ray absorption spectroscopy (XAS). The valence band is mainly composed of the O 2p state. The O 1s XAS spectrum exhibits the existence of the Ti 3d unoccupied state under the Zr 4d conduction band. The intensity of the Ti 3d unoccupied state increases with increasing TiO sub 2 concentration. The energy separation between the top of the valence band and the bottom of the Ti 3d unoccupied state is in accord with the energy gap, as expected from dc-polarization and total conductivity measurements. (author)

  4. In situ study of the Porticello Bronzes by portable X-ray fluorescence and laser-induced breakdown spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Ferretti, M. [Istituto per le Tecnologie Applicate ai Beni Culturali, Via Salaria, km 29.300, c.p.10, 00016 Monterotondo St. - Roma (Italy); Cristoforetti, G.; Legnaioli, S. [Applied Laser Spectroscopy Laboratory, Istituto per i Processi Chimico Fisici del CNR, Area di Ricerca di Pisa, Via G.Moruzzi, 1-56124 Pisa (Italy); Palleschi, V. [Applied Laser Spectroscopy Laboratory, Istituto per i Processi Chimico Fisici del CNR, Area di Ricerca di Pisa, Via G.Moruzzi, 1-56124 Pisa (Italy); Salvetti, A.; Tognoni, E. [Applied Laser Spectroscopy Laboratory, Istituto per i Processi Chimico Fisici del CNR, Area di Ricerca di Pisa, Via G.Moruzzi, 1-56124 Pisa (Italy); Console, E. [T.E.A. s.a.s., Via Luigi Pascali, 23/25-88100 Catanzaro (Italy)], E-mail: elena@teacz.191.it; Palaia, P. [T.E.A. s.a.s., Via Luigi Pascali, 23/25-88100 Catanzaro (Italy)

    2007-12-15

    This paper reports the results of a measurement campaign performed at the National Museum of Magna Grecia in Reggio Calabria (Italy). Portable X-Ray Fluorescence (XRF) and Laser-Induced Breakdown Spectroscopy (LIBS) instrumentation allowed in situ analysis of several bronze pieces belonging to the group of the so-called Porticello Bronzes. The find occurred at sea, off the village of Porticello (Reggio Calabria) in 1969 and consists of a number of fragments, including a bearded head, pertaining to at least two statues. The use of X-Ray Fluorescence and Laser-Induced Breakdown Spectroscopy techniques allowed for a classification of the fragments according to their elemental composition. The fragments appear to belong to at least two different statues; although, in general, the compositional classification agrees well with the stylistic analysis of the fragments, significant improvements with respect to previous achievements emerge from the joint results of the two techniques used.

  5. Pt and Ru X-ray absorption spectroscopy of PtRu anode catalysts in operating direct methanol fuel cells.

    Science.gov (United States)

    Stoupin, Stanislav; Chung, Eun-Hyuk; Chattopadhyay, Soma; Segre, Carlo U; Smotkin, Eugene S

    2006-05-25

    In situ X-ray absorption spectroscopy, ex situ X-ray fluorescence, and X-ray powder diffraction enabled detailed core analysis of phase segregated nanostructured PtRu anode catalysts in an operating direct methanol fuel cell (DMFC). No change in the core structures of the phase segregated catalyst was observed as the potential traversed the current onset potential of the DMFC. The methodology was exemplified using a Johnson Matthey unsupported PtRu (1:1) anode catalyst incorporated into a DMFC membrane electrode assembly. During DMFC operation the catalyst is essentially metallic with half of the Ru incorporated into a face-centered cubic (FCC) Pt alloy lattice and the remaining half in an amorphous phase. The extended X-ray absorption fine structure (EXAFS) analysis suggests that the FCC lattice is not fully disordered. The EXAFS indicates that the Ru-O bond lengths were significantly shorter than those reported for Ru-O of ruthenium oxides, suggesting that the phases in which the Ru resides in the catalysts are not similar to oxides.

  6. Femtosecond time-resolved X-ray absorption spectroscopy of anatase TiO2 nanoparticles using XFEL

    Directory of Open Access Journals (Sweden)

    Yuki Obara

    2017-07-01

    Full Text Available The charge-carrier dynamics of anatase TiO2 nanoparticles in an aqueous solution were studied by femtosecond time-resolved X-ray absorption spectroscopy using an X-ray free electron laser in combination with a synchronized ultraviolet femtosecond laser (268 nm. Using an arrival time monitor for the X-ray pulses, we obtained a temporal resolution of 170 fs. The transient X-ray absorption spectra revealed an ultrafast Ti K-edge shift and a subsequent growth of a pre-edge structure. The edge shift occurred in ca. 100 fs and is ascribed to reduction of Ti by localization of generated conduction band electrons into shallow traps of self-trapped polarons or deep traps at penta-coordinate Ti sites. Growth of the pre-edge feature and reduction of the above-edge peak intensity occur with similar time constants of 300–400 fs, which we assign to the structural distortion dynamics near the surface.

  7. Catalytic Properties of Surfaces Sites on Metal Oxides and Their Characterization by X-Ray Photoelectron Spectroscopy

    Science.gov (United States)

    1974-01-01

    chromium tha w-xs tcdbilized during reaction. The results of the iodometric titration of the surface oxide are shown in Figures 7 and 8. Th...catalysts to elicit further information; oxygen chemisorption (dispersion), x-ray fluorescence spectroscopy, iodometric determination of oxidation...between the surface oxidation state following reaction and the mean oxidation state determined iodometrically . A large change in the catalys

  8. X-ray and {Gamma}-ray spectroscopy of solids under pressure: Final technical progress report, November 1993--October 1996

    Energy Technology Data Exchange (ETDEWEB)

    Ingalls, R.L.

    1996-04-30

    This report briefly describes the studies of various materials at high pressures, in the last three years, by means of x-ray and {gamma}-ray absorption spectroscopy. High pressure provides a very effective means of studying materials. Virtually every property is altered, from the color and crystal structure, to the electrical and magnetic properties. The fundamental reason, of course, is that the quantum levels depend upon the atomic spacing, so that both the electronic and vibrational structure are affected.

  9. Combining mid infrared and total X-ray fluorescence spectroscopy for prediction of soil properties

    Science.gov (United States)

    Towett, Erick; Shepherd, Keith; Sila, Andrew; Aynekulu, Ermias; Cadisch, Georg

    2015-04-01

    Mid-infrared diffuse reflectance spectroscopy (MIR) can predict many soil properties but extractable nutrients are often predicted poorly. We evaluated the potential of MIR and total elemental analysis using total X-ray fluorescence spectroscopy (TXRF), both individually and combined, to predict results of conventional soil tests. Total multi-elemental analysis provides a fingerprint of soil mineralogy and could predict some soil properties and help improve MIR predictions. A set of 700 georeferenced soil samples associated with the Africa Soil Information Service (AfSIS) (www.africasoils.net) from 44 stratified randomly-located 100-km2 sentinel sites distributed across sub-Saharan Africa were analysed for physico-chemical composition using conventional reference methods, and compared to MIR and TXRF spectra using the Random Forests regression algorithm and an internal out-of-bag validation. MIR spectra resulted in good prediction models (R2 >0.80) for organic C and total N, Mehlich-3 Ca and Al, and pH. To test the combined spectroscopic approach, TXRF element concentration data was included as a property predictor along with the first derivative of MIR spectral data using the RF algorithm. Including TXRF did not improve prediction of these properties. TXRF was poorer (R2 0.86) as these elements are not directly determined with TXRF, however the variance explained is still quite high and may be attributable to TXRF signatures relating to mineralogy correlated with protection of soil organic matter. TXRF model for Mehlich-3 Al had excellent prediction capability explaining 81% of the observed variation in extractable Al content and was comparable to that of MIR (R2 = 0.86). However, models for pH and Mehlich-3 exchangeable Ca exhibited R2 values of 0.74 and 0.79 respectively and thus had moderate predictive accuracy, compared to MIR alone with R2 values of 0.82 and 0.84 respectively. Both MIR and TXRF methods predicted soil properties that relate to nutrient

  10. Investigation of photon counting pixel detectors for X-ray spectroscopy and imaging

    Energy Technology Data Exchange (ETDEWEB)

    Talla, Patrick Takoukam

    2011-04-07

    The Medipix2 and Medipix3 detectors are hybrid pixelated photon counting detectors with a pixel pitch of 55 {mu}m. The sensor material used in this thesis was silicon. Because of their small pixel size they suffer from charge sharing i.e. an incoming photon can be registered by more than one pixel. In order to correct for charge sharing due to lateral diffusion of charge carriers, the Medipix3 detector was developed: with its Charge Summing Mode, the charge collected in a cluster of 2 x 2 pixel is added up and attributed to only one pixel whose counter is incremented. The adjustable threshold of the detectors allows to count the photons and to gain information on their energy. The main purposes of the thesis are to investigate spectral and imaging properties of pixelated photon counting detectors from the Medipix family such as Medipix2 and Medipix3. The investigations are based on simulations and measurements. In order to investigate the spectral properties of the detectors measurements were performed using fluorescence lines of materials such as molybdenum, silver but also some radioactive sources such as Am-241 or Cd-109. From the measured data, parameters like the threshold dispersion and the gain variation from pixel-to-pixel were extracted and used as input in the Monte Carlo code ROSI to model the responses of the detector to monoenergetic photons. The measured data are well described by the simulations for Medipix2 and for Medipix3 operating in Charge Summing Mode. Due to charge sharing and due to the energy dependence of attenuation processes in silicon and to Compton scattering the incoming and the measured spectrum differ substantially from each other. Since the responses to monoenergetic photons are known, a deconvolution was performed to determine the true incoming spectrum. Several direct and iterative methods were successfully applied on measured and simulated data of an X-ray tube and radioactive sources. The knowledge of the X-ray spectrum is

  11. Exploring Galaxy Halos and the Cosmic Web through X-Ray Spectroscopy

    Science.gov (United States)

    Bregman, Joel; Anderson, Mike; Dai, Xinyu; Miller, Matt; Hodges-Kluck, Edmund

    2015-10-01

    About 90 of the metals produced in the universe and 50 of the baryons are unaccounted for through UV-IR and radio studies of stars and gas. This large amount of gas and metals likely lies in a hot phase 0.5-10E6 K and must be enriched to about 0.2-0.3 of the solar metallicity, so it should be a good absorber of X-rays in the resonance lines of common elements. X-ray absorption lines against background AGNs should show hot extended halos around galaxies out to the virial radius, if not beyond. The outer parts of galaxy groups and some cosmic filaments are other potential sources of absorption. For the Milky Way, high X-ray spectral resolution allows us to determine the dynamics of the hot halo, including the rotation as a function of radius as well as the accretion or outflow rate.

  12. Multireference X-Ray Emission and Absorption Spectroscopy calculations from Monte Carlo Configuration Interaction

    CERN Document Server

    Coe, J P

    2015-01-01

    We adapt the method of Monte Carlo configuration interaction to calculate core-hole states and use this for the computation of X-ray emission and absorption values. We consider CO, CH$_{4}$, NH$_{3}$, H$_{2}$O, HF, HCN, CH$_{3}$OH, CH$_{3}$F, HCl and NO using a 6-311G** basis. We also look at carbon monoxide with a stretched geometry and discuss the dependence of its results on the cutoff used. The Monte Carlo configuration interaction results are compared with EOM-CCSD values for X-ray emission and with experiment for X-ray absorption. Oscillator strengths are also computed and we quantify the multireference nature of the wavefunctions to suggest when approaches based on a single reference would be expected to be successful.

  13. Ultrafast Excited State Relaxation of a Metalloporphyrin Revealed by Femtosecond X-ray Absorption Spectroscopy

    DEFF Research Database (Denmark)

    Shelby, Megan L.; Lestrange, Patrick J.; Jackson, Nicholas E.

    2016-01-01

    Photoexcited Nickel(II) tetramesitylporphyrin (NiTMP), like many open-shell metalloporphyrins, relaxes rapidly through multiple electronic states following an initial porphyrin-based excitation, some involving metal centered electronic configuration changes that could be harnessed catalytically......), structural dynamics before thermalization were not resolved due to the similar to 100 ps duration of the available X-ray probe pulse. Using the femtosecond (fs) X-ray pulses of the Linac Coherent Light Source (LCLS), the Ni center electronic configuration from the initial excited state to the relaxed (d...

  14. Chemical Analysis of Impurity Boron Atoms in Diamond Using Soft X-ray Emission Spectroscopy

    OpenAIRE

    Muramatsu, Yasuji

    2009-01-01

    To analyze the local structure and/or chemical states of boron atoms in boron-doped diamond, which can be synthesized by the microwave plasma-assisted chemical vapor deposition method (CVD-B-diamond) and the temperature gradient method at high pressure and high temperature (HPT-B-diamond), we measured the soft X-ray emission spectra in the CK and BK regions of B-diamonds using synchrotron radiation at the Advanced Light Source (ALS). X-ray spectral analyses using the fingerprint method and mo...

  15. Combined Operando X-ray Diffraction/Raman Spectroscopy of Catalytic Solids in the Laboratory: The Co/TiO2 Fischer-Tropsch Synthesis Catalyst Showcase

    NARCIS (Netherlands)

    Cats, Korneel H.; Weckhuysen, Bert M.

    2016-01-01

    A novel laboratory setup for combined operando X-ray diffraction and Raman spectroscopy of catalytic solids with online product analysis by gas chromatography is presented. The setup can be used with a laboratory-based X-ray source, which results in important advantages in terms of time-on-stream

  16. The use of C-near edge X-ray absorption fine structure spectroscopy for the elaboration of chemistry in lignocellulosics

    Science.gov (United States)

    Lucian A. Lucia; Hiroki Nanko; Alan W. Rudie; Doug G. Mancosky; Sue Wirick

    2006-01-01

    The research presented elucidates the oxidation chemistry occurring in hydrogen peroxide bleached kraft pulp fibers by employing carbon near edge x-ray absorption fine structure spectroscopy (C-NEXAFS). C-NEXAFS is a soft x-ray technique that selectively interrogates atomic moieties using photoelectrons (Xrays) of variable energies. The X1A beam line at the National...

  17. Novel visualization studies of lignocellulosic oxidation chemistry by application of C-near edge X-ray absorption fine structure spectroscopy

    Science.gov (United States)

    Douglas G. Mancosky; Lucian A. Lucia; Hiroki Nanko; Sue Wirick; Alan W. Rudie; Robert Braun

    2005-01-01

    The research presented herein is the first attempt to probe the chemical nature of lignocellulosic samples by the application of carbon near edge X-ray absorption fine structure spectroscopy (C-NEXAFS). C-NEXAFS is a soft X-ray technique that principally provides selective interrogation of discrete atomic moieties using photoelectrons of variable energies. The X1A beam...

  18. Electrochemical impedance spectroscopy and X-ray photoelectron spectroscopy study of the corrosion behaviour of galvanized steel and electroplating steel

    Energy Technology Data Exchange (ETDEWEB)

    Lebrini, M., E-mail: mlebrini@yahoo.fr [Laboratoire des Procedes d' Elaboration des Revetements Fonctionnels, PERF-LSPES UMR CNRS 8008, ENSCL, BP 90108, F-59652 Villeneuve d' Ascq Cedex (France); Traisnel, M. [Laboratoire des Procedes d' Elaboration des Revetements Fonctionnels, PERF-LSPES UMR CNRS 8008, ENSCL, BP 90108, F-59652 Villeneuve d' Ascq Cedex (France); Gengembre, L. [Unite de Catalyse et Chimie du solide UMR 8181 Bat C3, USTL, F-59655, Villeneuve d' Ascq Cedex (France); Fontaine, G. [Laboratoire des Procedes d' Elaboration des Revetements Fonctionnels, PERF-LSPES UMR CNRS 8008, ENSCL, BP 90108, F-59652 Villeneuve d' Ascq Cedex (France); Lerasle, O.; Genet, N. [TOTAL France, Centre de Recherche de Solaize, Chemin du canal, BP 22, F-69360 Solaize (France)

    2011-02-01

    The efficiency of a formula containing 2-{l_brace}(2-hydroxyethyl)[(4-methyl-1H-1,2,3-benzotriazol-1-yl)methyl] amino{r_brace}ethanol (tolyltriazole) and decanoic acid as corrosion inhibitor for galvanized steel and electroplating steel in aqueous solution have been determined by electrochemical impedance spectroscopy (EIS) techniques. The experimental data obtained from this method show a frequency distribution and therefore a modelling element with frequency dispersion behaviour, a constant phase element (CPE) has been used. The corrosion behaviour in the presence of different concentration of decanoic acid (DA) in the formula was also investigated by EIS. Results obtained reveal that, the formula is a good inhibitor for galvanized steel and electroplating steel in aqueous solution, the better performance was obtained in the case of galvanized steel. The ability of the inhibitor to be adsorbed on the surface was dependent on the nature of metal. X-ray photoelectron spectroscopy surface analysis with inhibitor shows that it's chemisorbed at the galvanized and electroplating steel/aqueous solution interface.

  19. A Complete Overhaul of the Electron Energy-Loss Spectroscopy and X-Ray Absorption Spectroscopy Database: eelsdb.eu.

    Science.gov (United States)

    Ewels, Philip; Sikora, Thierry; Serin, Virginie; Ewels, Chris P; Lajaunie, Luc

    2016-06-01

    The electron energy-loss spectroscopy (EELS) and X-ray absorption spectroscopy (XAS) database has been completely rewritten, with an improved design, user interface, and a number of new tools. The database is accessible at https://eelsdb.eu/ and can now be used without registration. The submission process has been streamlined to encourage spectrum submissions and the new design gives greater emphasis on contributors' original work by highlighting their papers. With numerous new filters and a powerful search function, it is now simple to explore the database of several hundred EELS and XAS spectra. Interactive plots allow spectra to be overlaid, facilitating online comparison. An application-programming interface has been created, allowing external tools and software to easily access the information held within the database. In addition to the database itself, users can post and manage job adverts and read the latest news and events regarding the EELS and XAS communities. In accordance with the ongoing drive toward open access data increasingly demanded by funding bodies, the database will facilitate open access data sharing of EELS and XAS spectra.

  20. Obtaining two attosecond pulses pulses for x-ray stimulated Raman spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Zholents, Alexander; Penn, G.

    2009-06-23

    Attosecond x-ray pulses are an indispensable tool for the study of electronic and structural changes in molecules undergoing chemical reactions. They have a wide bandwidth comparable to the energy bands of valence electronic states and, therefore, are well suited for making and probing multiple valence electronic excitations using core electron transitions. Here we propose a method of creating a sequence of two attosecond soft x-ray pulses in a free electron laser by optical manipulation of electrons located in two different sections of the electron bunch. The energy of each x-ray pulse can be of the order of 100 nJ and the pulse width of the order of 250 attoseconds. The carrier frequency of each x-ray pulse can be independently tuned to a resonant core electron transition of a specific atom of the molecule. The time interval between the two attosecond pulses is tunable from a few femtoseconds to a hundred femtoseconds with better than 100 attoseconds precision.

  1. Hit detection in serial femtosecond crystallography using X-ray spectroscopy of plasma emission

    Directory of Open Access Journals (Sweden)

    H. Olof Jönsson

    2017-11-01

    Full Text Available Serial femtosecond crystallography is an emerging and promising method for determining protein structures, making use of the ultrafast and bright X-ray pulses from X-ray free-electron lasers. The upcoming X-ray laser sources will produce well above 1000 pulses per second and will pose a new challenge: how to quickly determine successful crystal hits and avoid a high-rate data deluge. Proposed here is a hit-finding scheme based on detecting photons from plasma emission after the sample has been intercepted by the X-ray laser. Plasma emission spectra are simulated for systems exposed to high-intensity femtosecond pulses, for both protein crystals and the liquid carrier systems that are used for sample delivery. The thermal radiation from the glowing plasma gives a strong background in the XUV region that depends on the intensity of the pulse, around the emission lines from light elements (carbon, nitrogen, oxygen. Sample hits can be reliably distinguished from the carrier liquid based on the characteristic emission lines from heavier elements present only in the sample, such as sulfur. For buffer systems with sulfur present, selenomethionine substitution is suggested, where the selenium emission lines could be used both as an indication of a hit and as an aid in phasing and structural reconstruction of the protein.

  2. X-ray absorption spectroscopy of PbMoO 4 single crystals

    Indian Academy of Sciences (India)

    X-ray absorption spectra of PbMoO4 (LMO) crystals have been investigated for the first time in literature. The measurements have been carried out at Mo absorption edge at the dispersive EXAFS beamline (BL-8) of INDUS-2 Synchrotron facility at Indore, India. The optics of the beamline was set to obtain a band of 2000 eV ...

  3. STROBE-X: X-Ray Timing and Spectroscopy on Dynamical Timescales from Microseconds to Years

    DEFF Research Database (Denmark)

    Wilson-Hodge, Colleen A; Ray, Paul S.; Gendreau, Keith C.

    2017-01-01

    The Spectroscopic Time-Resolving Observatory for Broadband Energy X-rays (STROBE-X) probes strong gravity for stellar mass to supermassive black holes and ultradense matter with unprecedented effective area, high time-resolution, and good spectral resolution, while providing a powerful time...

  4. X-Ray Absorption Spectroscopy of Fe-Substituted Allophane and Imogolite

    Science.gov (United States)

    Baker, L. L.; Strawn, D. G.; Nickerson, R. D.; McDaniel, P.

    2011-12-01

    Martian rocks and sediments contain weathering products including clay minerals formed as a result of interaction between rocks and water, and these materials can act as important indicators of past surface conditions on Mars. Weathering of terrestrial volcanic rocks similar to those on Mars produces nano-sized, variably hydrated aluminosilicate and iron oxide minerals, including allophane, imogolite, halloysite, hisingerite, and ferrihydrite. The nanoaluminosilicates can contain isomorphically substituted Fe, which may affect their spectral and physical properties as well as their eventual recrystallization products. Detection and quantification of such minerals in natural environments on Earth is difficult due to their variable chemical composition and lack of long-range crystalline order. Their accurate detection and quantification on Mars requires a better understanding of how composition affects their spectral properties and evolution to more crystalline phases. Aluminosilicate nanoparticles of varying composition were synthesized with isomorphically substituted Fe at Fe:Al ratios of 1:100. Allophanes were synthesized with Al:Si ratios of 2:1, 1:1, and 1:3. The substituted Fe was probed using Fe K-edge X-ray absorption fine structure spectroscopy (XAFS). The XAFS spectrum contains information about the molecular environment surrounding the target atom, and is an ideal technique for studying poorly crystalline materials that are difficult to characterize using bulk methods such as XRD. The near-edge (XANES) and extended (EXAFS) portions of the XAFS spectrum were examined, and allophane backscattering paths were fit using coordinates for a modified nanoball model (1). XANES spectra rule out ferrihydrite in the synthetic samples, suggesting all Fe was incorporated into the aluminosilicate structure. The XAFS results suggest that Fe substituted into the allophane structure is present as Fe(III) in octahedral coordination in a well-ordered sheet. Some Fe

  5. OPTICAL SPECTROSCOPY OF X-RAY-SELECTED YOUNG STARS IN THE CARINA NEBULA

    Energy Technology Data Exchange (ETDEWEB)

    Vaidya, Kaushar [Physics Department, Birla Institute of Technology and Science Pilani, Pilani 333031, Rajasthan (India); Chen, Wen-Ping; Lee, Hsu-Tai [Graduate Institute of Astronomy, National Central University, 300 Zhongda Road, Zhongli 32001, Taiwan (China)

    2015-12-15

    We present low-resolution optical spectra for 29 X-ray sources identified as either massive star candidates or low-mass pre-main-sequence (PMS) star candidates in the clusters Trumpler 16 and Trumpler 14 of the Carina Nebula. Spectra of two more objects (one with an X-ray counterpart, and one with no X-ray counterpart), not originally our targets, but found close (∼3″) to two of our targets, are presented as well. Twenty early-type stars, including an O8 star, seven B1–B2 stars, two B3 stars, a B5 star, and nine emission-line stars, are identified. Eleven T Tauri stars, including eight classical T Tauri stars (CTTSs) and three weak-lined T Tauri stars, are identified. The early-type stars in our sample are more reddened compared to the previously known OB stars of the region. The Chandra hardness ratios of our T Tauri stars are found to be consistent with the Chandra hardness ratios of T Tauri stars of the Orion Nebula Cluster. Most early-type stars are found to be nonvariable in X-ray emission, except the B2 star J104518.81–594217.9, the B3 star J104507.84–594134.0, and the Ae star J104424.76–594555.0, which are possible X-ray variables. J104452.20–594155.1, a CTTS, is among the brightest and the hardest X-ray sources in our sample, appears to be a variable, and shows a strong X-ray flare. The mean optical and near-infrared photometric variability in the V and K{sub s} bands, of all sources, is found to be ∼0.04 and 0.05 mag, respectively. The T Tauri stars show significantly larger mean variation, ∼0.1 mag, in the K{sub s} band. The addition of one O star and seven B1–B2 stars reported here contributes to an 11% increase of the known OB population in the observed field. The 11 T Tauri stars are the first ever confirmed low-mass PMS stars in the Carina Nebula region.

  6. Frontiers in x-ray components for high-resolution spectroscopy and imaging laminar type varied-line-spacing holographic gratings for soft x-ray

    CERN Document Server

    Sano, K

    2003-01-01

    Laminar-type varied-line-spacing gratings have been widely used for soft x-ray monochromator recently because of the features of low stray lights and higher order lights. We have developed and advanced holographic recording and an ion-beam etching methods for the laminar type varied-line spacing gratings. This report describes a short review of the soft x-ray spectrometers using varied-line-spacing gratings, the fabrication process of the laminar-type holographic gratings, and the performance of the flat field spectrographs equipped with the laminar type varied-line spacing gratings comparing with the mechanically ruled replica gratings. It is concluded that, for the sake of the advanced design and fabrication processes and excellent spectroscopic performance, laminar-type holographic gratings will be widely used for soft x-ray spectrometers for various purposes in the near future. (author)

  7. Double core-hole spectroscopy of transient plasmas produced in the interaction of ultraintense x-ray pulses with neon

    CERN Document Server

    Gao, Cheng; Yuan, Jianmin

    2015-01-01

    Double core-hole (DCH) spectroscopy is investigated systematically for neon atomic system in the interaction with ultraintense x-ray pulses with photon energy from 937 eV to 2000 eV. A time-dependent rate equation, implemented in the detailed level accounting approximation, is utilized to study the dynamical evolution of the level population and emission properties of the highly transient plasmas. For x-ray pulses with photon energy in the range of 937-1030 eV, where $1s\\rightarrow 2p$ resonance absorption from single core-hole (SCH) states of neon charge states exist, inner-shell resonant absorption (IRA) effects play important roles in the time evolution of population and DCH spectroscopy. Such IRA physical effects are illustrated in detail by investigating the interaction of x-ray pulses at a photon energy of 944 eV, which corresponds to the $1s\\rightarrow 2p$ resonant absorption from the SCH states ($1s2s^22p^4$, $1s2s2p^5$ and $1s2p^6$) of Ne$^{3+}$. After averaging over the space and time distribution o...

  8. Resonant x-ray emission spectroscopy of liquid water: novel instrumentation, high resolution, and the"map" approach

    Energy Technology Data Exchange (ETDEWEB)

    Weinhardt, L.; Fuchs, O.; Blum, M.; B& #228; r, M.; Weigand, M.; Denlinger, J.D.; Zubavichus, Y.; Zharnikov, M.; Grunze, M.; Heske, C.; Umbach, E.

    2008-06-17

    Techniques to study the electronic structure of liquids are rare. Most recently, resonant x-ray emission spectroscopy (XES) has been shown to be an extremely versatile spectroscopy to study both occupied and unoccupied electronic states for liquids in thermodynamic equilibrium. However, XES requires high-brilliance soft x-ray synchrotron radiation and poses significant technical challenges to maintain a liquid sample in an ultra-high vacuum environment. Our group has therefore developed and constructed a novel experimental setup for the study of liquids, with the long-term goal of investigating the electronic structure of biological systems in aqueous environments. We have developed a flow-through liquid cell in which the liquid is separated from vacuum by a thin Si3N4 or SiC window and which allows a precise control of temperature. This approach has significant advantages compared to static liquids cells used in the past. Furthermore, we have designed a dedicated high-transmission, high-resolution soft x-ray spectrometer. The high transmission makes it possible to measure complete resonant XES"maps" in less than an hour, giving unprecedented detailed insight into the electronic structure of the investigated sample. Using this new equipment we have investigated the electronic structure of liquid water. Furthermore, our XES spectra and maps give information about ultra-fast dissociation on the timescale of the O 1s core hole lifetime, which is strongly affected by the initial state hydrogen bonding configuration.

  9. X-ray photoelectron spectroscopy study of the functionalization of carbon metal-containing nanotubes with phosphorus atoms

    Energy Technology Data Exchange (ETDEWEB)

    Shabanova, I.N., E-mail: xps@fti.udm.ru; Terebova, N.S.

    2013-08-15

    Highlights: •Carbon metal-containing nanotubes (Me–Cu, Ni, Fe) were functionalized with chemical groups containing different concentrations of phosphorous. •The C1s and Me3s spectra were measured by the X-ray photoelectron spectroscopy method. •The values of the atomic magnetic moment of the carbon metal-containing nanotubes were determined. -- Abstract: In the present paper, carbon metal-containing (Me: Cu, Ni, Fe) nanotubes functionalized with phosphorus atoms (ammonium polyphosphate) were studied by X-ray photoelectron spectroscopy (XPS) on an X-ray electron magnetic spectrometer. It is found that the functionalization leads to the change of the metal atomic magnetic moment, i.e. the value of the atomic magnetic moment in the functionalized carbon metal-containing (Cu, Ni, Fe) nanotubes increases and is higher than that in pristine nanotubes. It is shown that the covalent bond of Me and P atoms is formed. This leads to an increase in the activity of the nanostructure surface which is necessary for the modification of materials.

  10. Irradiation-induced structural changes in hydrogenated amorphous silicon as measured by X-ray photoemission spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Yelon, A.; Rochefort, A.; Sheng, S.; Sacher, E. [Ecole Polytechnique de Montreal, Quebec (Canada). Departement de Genie Physique

    2003-07-01

    The pertinent experimental literature on light- and X-ray-induced changes in a-Si:H, as measured by X-ray photoelectron spectroscopy are reviewed. Illumination causes both the Si2p and Si2s spectra to shift to lower binding energies by equal amounts. At least to the depth probed by X-ray photoemission spectroscopy (XPS), the shift, and the structural changes that lead to them, occur uniformly. We consider the relatively new finding of photo-induced metastable expansion in a-Si:H, and the likelihood that this phenomenon is related to the XPS shifts. In order to provide an answer to this question, we undertake preliminary density functional calculations on a simple model of a-Si:H, these calculations include effects that may occur during the metastable expansion, such as elongations of the length of compressed Si-Si bonds and variations in the Si-Si-Si dihedral angle. Our results indicate that, were the metastable expansion to be associated with the XPS shifts, unidirectional bond angle changes would have to occur uniformly throughout the bulk, and their effect would have to dominate those of all other structural changes. (author)

  11. Optical spectroscopy of the Be/X-ray binary V850 Centauri/GX 304-1 during faint X-ray periodical activity

    Science.gov (United States)

    Malacaria, C.; Kollatschny, W.; Whelan, E.; Santangelo, A.; Klochkov, D.; McBride, V.; Ducci, L.

    2017-07-01

    Context. Be/X-ray binaries (BeXRBs) are the most populous class of high-mass X-ray binaries. Their X-ray duty cycle is tightly related to the optical companion wind activity, which in turn can be studied through dedicated optical spectroscopic observations. Aims: We study optical spectral features of the Be circumstellar disk to test their long-term variability and their relation with the X-ray activity. Special attention has been given to the Hα emission line, one of the best tracers of the disk conditions. Methods: We obtained optical broadband medium resolution spectra from a dedicated campaign with the Anglo-Australian Telescope and the Southern African Large Telescope in 2014-2015. Data span over one entire binary orbit, and cover both X-ray quiescent and moderately active periods. We used Balmer emission lines to follow the evolution of the circumstellar disk. Results: We observe prominent spectral features, like double-peaked Hα and Hβ emission lines. The HαV/R ratio significantly changes over a timescale of about one year. Our observations are consistent with a system observed at a large inclination angle (I ≳ 60°). The derived circumstellar disk size shows that the disk evolves from a configuration that prevents accretion onto the neutron star, to one that allows only moderate accretion. This is in agreement with the contemporary observed X-ray activity. Our results are interpreted within the context of inefficient tidal truncation of the circumstellar disk, as expected for this source's binary configuration. We derived the Hβ-emitting region size, which is equal to about half of the corresponding Hα-emitting disk, and constrain the luminosity class of V850 Cen as III-V, consistent with the previously proposed class.

  12. High stability X-ray spectroscopy system with on-chip front-end in charge amplifier configuration

    Energy Technology Data Exchange (ETDEWEB)

    Guazzoni, Chiara; Chiesa, Marco; Sampietro, Marco E-mail: marco.sampietro@polimi.it; Lechner, Peter

    2003-10-11

    This paper presents the performance of a two-chip detector system based on a silicon drift detector and on a charge amplifier, part of the latter being integrated in the detector chip. The two-chip system is intended for high-resolution X-ray spectroscopy experiments in which stability of operation is mandatory to avoid on-line calibration procedures. Experimental measurements have been carried out to test the stability of the whole system with a quantitative analysis of the gain stability obtained by comparing X-ray spectra taken at different operating conditions, varying the temperature and/or the detector bias. A gain variation of less than 0.4% has been obtained at extreme operating conditions. The problems and critical aspects of the two-chip charge amplifier solution are discussed.

  13. What Can Be Learned from X-Ray Spectroscopy Concerning Hot Gas in the Local Bubble and Charge Exchange Processes?

    Science.gov (United States)

    Snowden, S. L.

    2008-01-01

    Both solar wind charge exchange emission and diffuse thermal emission from the Local Bubble are strongly dominated in the soft X-ray band by lines from highly ionized elements. While both processes share many of the same lines, the spectra should differ significantly due to the different production mechanisms, abundances, and ionization states. Despite their distinct spectral signatures, current and past observatories have lacked the spectral resolution to adequately distinguish between the two sources. High-resolution X-ray spectroscopy instrumentation proposed for future missions has the potential to answer fundamental questions such as whether there is any hot plasma in the Local Hot Bubble, and if so, what are the abundances of the emitting plasma and whether the plasma is in equilibrium. Such instrumentation will provide dynamic information about the solar wind including data on ion species which are currently difficult to track. It will also make possible remote sensing of the solar wind.

  14. A sealable ultrathin window sample cell for the study of liquids by means of soft X-ray spectroscopy

    Science.gov (United States)

    Grötzsch, D.; Streeck, C.; Nietzold, C.; Malzer, W.; Mantouvalou, I.; Nutsch, A.; Dietrich, P.; Unger, W.; Beckhoff, B.; Kanngießer, B.

    2017-12-01

    A new sample cell concept for the analysis of liquids or solid-liquid interfaces using soft X-ray spectroscopy is presented, which enables the complete sealing of the cell as well as the transport into vacuum via, for example, a load-lock system. The cell uses pressure monitoring and active as well as passive pressure regulation systems, thereby facilitating the full control over the pressure during filling, sealing, evacuation, and measurement. The cell design and sample preparation as well as the crucial sealing procedure are explained in detail. As a first proof-of-principle experiment, successful nitrogen K-edge fluorescence yield near-edge X-ray absorption fine structure experiments of a biomolecular solution are presented. For this purpose, it is shown that the careful evaluation of all involved parameters, such as window type or photon flux, is desirable for optimizing the experimental result.

  15. Crystal and molecular structure of norspermine copper(II) sulphate trihydrate studied by X-ray and IR spectroscopy

    Science.gov (United States)

    Perkowska, A.; Małuszyńska, H.

    1999-09-01

    The title compound [Cu(C 9H 18N 4)]SO 4·3H 2O [A] was studied by X-ray and IR spectroscopy. It crystallises as monoclinic, in the space group P2 1/c with a=9.719(2), b=13.470(3), c=12.865(3) Å, β=95.36(3) and Z=4. The copper atom is five-coordinated with four nitrogen atoms and one oxygen atom from the sulphate group, forming a tricyclic chelated norspermine complex consisting of three six-membered rings, one of which is disordered. The amine groups from norspermine are hydrogen bonded to the sulphate anions. The water molecules of crystallisation form infinite (H 2O) n chains and through the sulphate anions link the norspermine complexes in the three-dimensional hydrogen bond network. The FT-IR spectra before and after dehydration of [A] confirm the X-ray results.

  16. Composition measurement in substitutionally disordered materials by atomic resolution energy dispersive X-ray spectroscopy in scanning transmission electron microscopy.

    Science.gov (United States)

    Chen, Z; Taplin, D J; Weyland, M; Allen, L J; Findlay, S D

    2017-05-01

    The increasing use of energy dispersive X-ray spectroscopy in atomic resolution scanning transmission electron microscopy invites the question of whether its success in precision composition determination at lower magnifications can be replicated in the atomic resolution regime. In this paper, we explore, through simulation, the prospects for composition measurement via the model system of AlxGa1-xAs, discussing the approximations used in the modelling, the variability in the signal due to changes in configuration at constant composition, and the ability to distinguish between different compositions. Results are presented in such a way that the number of X-ray counts, and thus the expected variation due to counting statistics, can be gauged for a range of operating conditions. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Time- and space-resolved X-ray absorption spectroscopy of aluminum irradiated by a subpicosecond high-power laser

    Science.gov (United States)

    Tzortzakis, S.; Audebert, P.; Renaudin, P.; Bastiani-Ceccotti, S.; Geindre, J. P.; Chenais-Popovics, C.; Nagels, V.; Gary, S.; Shepherd, R.; Girard, F.; Matsushima, I.; Peyrusse, O.; Gauthier, J.-C.

    2006-05-01

    The ionization and recombination dynamics of transient aluminum plasmas was measured using point projection K-shell absorption spectroscopy. An aluminum plasma was produced with a subpicosecond beam of the 100-TW laser at the LULI facility and probed at different times with a picosecond X-ray backlighter created with a synchronized subpicosecond laser beam. Fourier-Domain-Interferometry (FDI) was used to measure the electron temperature at the peak of the heating laser pulse. Absorption X-ray spectra at early times are characteristic of a dense and rather homogeneous plasma, with limited longitudinal gradients as shown by hydrodynamic simulations. The shift of the Al K-edge was measured in the cold dense plasma located at the edge of the heated plasma. From the 1s 2p absorption spectra, the average ionization was measured as a function of time and was also modeled with a collisional-radiative atomic physics code coupled with hydrodynamic simulations.

  18. Time- and space-resolved X-ray absorption spectroscopy of aluminum irradiated by a subpicosecond high-power laser

    Energy Technology Data Exchange (ETDEWEB)

    Tzortzakis, S. [Laboratoire pour l' Utilisation des Lasers Intenses (LULI), UMR 7605, CNRS-CEA-Universite Paris VI-Ecole Polytechnique, 91128 Palaiseau (France)]. E-mail: gauthier@celia.ubordeaux1.fr; Audebert, P. [Laboratoire pour l' Utilisation des Lasers Intenses (LULI), UMR 7605, CNRS-CEA-Universite Paris VI-Ecole Polytechnique, 91128 Palaiseau (France); Renaudin, P. [Commissariat a l' Energie Atomique, 91680 Bruyeres-le-Chatel Cedex (France); Bastiani-Ceccotti, S. [Laboratoire pour l' Utilisation des Lasers Intenses (LULI), UMR 7605, CNRS-CEA-Universite Paris VI-Ecole Polytechnique, 91128 Palaiseau (France); Geindre, J.P. [Laboratoire pour l' Utilisation des Lasers Intenses (LULI), UMR 7605, CNRS-CEA-Universite Paris VI-Ecole Polytechnique, 91128 Palaiseau (France); Chenais-Popovics, C. [Laboratoire pour l' Utilisation des Lasers Intenses (LULI), UMR 7605, CNRS-CEA-Universite Paris VI-Ecole Polytechnique, 91128 Palaiseau (France); Nagels, V. [Laboratoire pour l' Utilisation des Lasers Intenses (LULI), UMR 7605, CNRS-CEA-Universite Paris VI-Ecole Polytechnique, 91128 Palaiseau (France); Gary, S. [Commissariat a l' Energie Atomique, 91680 Bruyeres-le-Chatel Cedex (France); Shepherd, R. [Lawrence Livermore National Laboratory, University of California, Livermore, CA 94550 (United States); Girard, F. [Commissariat a l' Energie Atomique, 91680 Bruyeres-le-Chatel Cedex (France); Matsushima, I. [National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba 3058568 (Japan); Peyrusse, O. [CELIA, UMR 5107, CNRS-CEA-Universite Bordeaux 1, 33405 Talence (France); Gauthier, J.-C. [CELIA, UMR 5107, CNRS-CEA-Universite Bordeaux 1, 33405 Talence (France)

    2006-05-15

    The ionization and recombination dynamics of transient aluminum plasmas was measured using point projection K-shell absorption spectroscopy. An aluminum plasma was produced with a subpicosecond beam of the 100-TW laser at the LULI facility and probed at different times with a picosecond X-ray backlighter created with a synchronized subpicosecond laser beam. Fourier-Domain-Interferometry (FDI) was used to measure the electron temperature at the peak of the heating laser pulse. Absorption X-ray spectra at early times are characteristic of a dense and rather homogeneous plasma, with limited longitudinal gradients as shown by hydrodynamic simulations. The shift of the Al K-edge was measured in the cold dense plasma located at the edge of the heated plasma. From the 1s-2p absorption spectra, the average ionization was measured as a function of time and was also modeled with a collisional-radiative atomic physics code coupled with hydrodynamic simulations.

  19. Anisotropy of chemical bonds in collagen molecules studied by X-ray absorption near-edge structure (XANES) spectroscopy.

    Science.gov (United States)

    Lam, Raymond S K; Metzler, Rebecca A; Gilbert, Pupa U P A; Beniash, Elia

    2012-03-16

    Collagen type I fibrils are the major building blocks of connective tissues. Collagen fibrils are anisotropic supramolecular structures, and their orientation can be revealed by polarized light microscopy and vibrational microspectroscopy. We hypothesized that the anisotropy of chemical bonds in the collagen molecules, and hence their orientation, might also be detected by X-ray photoemission electron spectromicroscopy (X-PEEM) and X-ray absorption near-edge structure (XANES) spectroscopy, which use linearly polarized synchrotron light. To test this hypothesis, we analyzed sections of rat-tail tendon, composed of parallel arrays of collagen fibrils. The results clearly indicate that XANES-PEEM is sensitive to collagen fibril orientation and, more specifically, to the orientations of carbonyl and amide bonds in collagen molecules. These data suggest that XANES-PEEM is a promising technique for characterizing the chemical composition and structural organization at the nanoscale of collagen-based connective tissues, including tendons, cartilage, and bone.

  20. Pb distribution in bones from the Franklin expedition: synchrotron X-ray fluorescence and laser ablation/mass spectroscopy

    Science.gov (United States)

    Martin, Ronald Richard; Naftel, Steven; Macfie, Sheila; Jones, Keith; Nelson, Andrew

    2013-04-01

    Synchrotron micro-X-ray Fluorescence has been used to map the metal distribution in selected bone fragments representative of remains associated with the Franklin expedition. In addition, laser ablation mass spectroscopy using a 25 μm diameter circular spot was employed to compare the Pb isotope distributions in small regions within the bone fragments. The X-ray Fluorescence mapping shows Pb to be widely distributed in the bone while the Pb isotope ratios obtained by laser ablation within small areas representative of bone with different Pb exchange rates do not show statistically significant differences. These results are inconsistent with the hypothesis that faulty solder seals in tinned meat were the principle source of Pb in the remains of the expedition personnel.

  1. Uranium aerosols at a nuclear fuel fabrication plant: Characterization using scanning electron microscopy and energy dispersive X-ray spectroscopy

    Science.gov (United States)

    Hansson, E.; Pettersson, H. B. L.; Fortin, C.; Eriksson, M.

    2017-05-01

    Detailed aerosol knowledge is essential in numerous applications, including risk assessment in nuclear industry. Cascade impactor sampling of uranium aerosols in the breathing zone of nuclear operators was carried out at a nuclear fuel fabrication plant. Collected aerosols were evaluated using scanning electron microscopy and energy dispersive X-ray spectroscopy. Imaging revealed remarkable variations in aerosol morphology at the different workshops, and a presence of very large particles (up to ≅ 100 × 50 μm2) in the operator breathing zone. Characteristic X-ray analysis showed varying uranium weight percentages of aerosols and, frequently, traces of nitrogen, fluorine and iron. The analysis method, in combination with cascade impactor sampling, can be a powerful tool for characterization of aerosols. The uranium aerosol source term for risk assessment in nuclear fuel fabrication appears to be highly complex.

  2. X-ray emission spectroscopy study of the Verwey transition in Fe sub 3 O sub 4

    CERN Document Server

    Moewes, A; Finkelstein, L D; Galakhov, A V; Gota, S; Gautier-Soyer, M; Rueff, J P; Hague, C F

    2003-01-01

    The temperature-dependent Verwey transition in a 500 A (111) thin film of Fe sub 3 O sub 4 (magnetite) has been studied using soft-x-ray emission spectroscopy at room temperature and below the transition temperature T sub V. The Fe L sub 2 sub , sub 3 x-ray emission spectra show an increase in the intensity of the L sub 2 emission relative to the L sub 3 emission below T sub V. This is independent of the excitation energy and is attributed to a metal-insulator transition across T sub V. Comparison of the Fe L sub 3 emission and O K alpha spectra with LDA band structure calculations supports the suggestion of charge ordering in Fe sub 3 O sub 4 at low temperature.

  3. Bright Linearly and Circularly Polarized Extreme Ultraviolet and Soft X-ray High Harmonics for Absorption Spectroscopy

    Science.gov (United States)

    Fan, Tingting

    High harmonic generation (HHG) is an extreme nonlinear optical process. When implemented in a phase-matched geometry, HHG coherent upconverts femtosecond laser light into coherent "X-ray laser" beams, while retaining excellent spatial and temporal coherence, as well as the polarization state of the driving laser. HHG has a tabletop footprint, with femtosecond to attosecond time resolution, combined with nanometer spatial resolution. As a consequence of these unique capabilities, HHG is now being widely adopted for use in molecular spectroscopy and imaging, materials science, as well as nanoimaging in general. In the first half of this thesis, I demonstrate high flux linearly polarized soft X-ray HHG, driven by a single-stage 10-mJ Ti:sapphire regenerative amplifier at a repetition rate of 1 kHz. I first down-converted the laser to 1.3 mum using an optical parametric amplifier, before up-converting it into the soft X-ray region using HHG in a high-pressure, phase-matched, hollow waveguide geometry. The resulting optimally phase-matched broadband spectrum extends to 200 eV, with a soft X-ray photon flux of > 106 photons/pulse/1% bandwidth at 1 kHz, corresponding to > 109 photons/s/1% bandwidth, or approximately a three orders-of-magnitude increase compared with past work. Using this broad bandwidth X-ray source, I demonstrated X-ray absorption spectroscopy of multiple elements and transitions in molecules in a single spectrum, with a spectral resolution of 0.25 eV, and with the ability to resolve the near edge fine structure. In the second half of this thesis, I discuss how to generate the first bright circularly polarized (CP) soft X-ray HHG and also use them to implement the first tabletop X-ray magnetic circular dichroism (XMCD) measurements. Using counter-rotating CP lasers at 1.3 mum and 0.79 mum, I generated CPHHG with photon energies exceeding 160 eV. The harmonic spectra emerge as a sequence of closely spaced pairs of left and right CP peaks, with energies

  4. High orbital angular momentum quantum numbers in the electronic ground states of Fe$_2^+$ and Co$_2^+$ as determined by x-ray absorption and x-ray magnetic circular dichroism spectroscopy

    CERN Document Server

    Zamudio-Bayer, V; Langenberg, A; Lawicki, A; Terasaki, A; Issendorff, B v; Lau, J T

    2015-01-01

    The $^6\\Delta$ electronic ground state of the Co$_2^+$ diatomic molecular cation has been assigned experimentally by x-ray absorption and x-ray magnetic circular dichroism spectroscopy in a cryogenic ion trap. Three candidates, $^6\\Phi$, $^6\\Gamma$, and $^8\\Gamma$, for the electronic ground state of Fe$_2^+$ have been identified. These states carry sizable ground-state orbital angular momenta that disagree with theoretical predictions from multireference configuration interaction and density functional theory. Our results show that the ground states of neutral and cationic diatomic molecules of $3d$ elements cannot be assumed to be connected by a one-electron process.

  5. Calibration of thickness-dependent k-factors for germanium X-ray lines to improve energy-dispersive X-ray spectroscopy of SiGe layers in analytical transmission electron microscopy

    OpenAIRE

    Qiu, Yi; Nguyen, Huy; A. Dobbie; Myronov, Maksym; Walther, T.

    2013-01-01

    We show that the accuracy of energy-dispersive X-ray spectroscopy can be improved by analysing and comparing multiple lines from the same element. For each line, an effective k-factor can be defined that varies as a function of the intensity ratio of multiple lines (e.g. K/L) from the same element. This basically performs an internal self-consistency check in the quantification using differently absorbed X-ray lines, which is in principle equivalent to an absorption correction as a function o...

  6. In-Situ Coherent Grazing Incidence Small Angle X-ray Scattering (Co-GISAXS) Studies of Surface Fluctuations of Sputter Deposited WSi2 using X-ray Photon Correlation Spectroscopy (XPCS)

    Science.gov (United States)

    Dahal, Som; Ulbrandt, Jeffrey; Headrick, Randall; Demasi, Alexander; Ludwig, Karl

    2014-03-01

    We performed Coherent Grazing Incidence Small Angle X-ray Scattering (Co-GISAXS) studies of surface dynamics during magnetron sputtering deposited WSi2 amorphous thin films. The local dynamics of surface fluctuations was studied by X-ray Photon Correlation Spectroscopy (XPCS) in the late time regime where the static GIXAXS stops evolving. Our studies reveal that the correlation time of the sputtered species varies as a power law with the in-plane momentum transfer. The experimentally obtained results are compared with predictions from continuum models of surface growth.

  7. In situ analyses of Ag speciation in tissues of cucumber and wheat using synchrotron-based X-ray absorption spectroscopy

    Data.gov (United States)

    U.S. Environmental Protection Agency — In situ analyses of Ag speciation in tissues of cucumber and wheat using synchrotron-based X-ray absorption spectroscopy showing spectral fitting and linear...

  8. Monte Carlo simulation of X-ray imaging and spectroscopy experiments using quadric geometry and variance reduction techniques

    Science.gov (United States)

    Golosio, Bruno; Schoonjans, Tom; Brunetti, Antonio; Oliva, Piernicola; Masala, Giovanni Luca

    2014-03-01

    The simulation of X-ray imaging experiments is often performed using deterministic codes, which can be relatively fast and easy to use. However, such codes are generally not suitable for the simulation of even slightly more complex experimental conditions, involving, for instance, first-order or higher-order scattering, X-ray fluorescence emissions, or more complex geometries, particularly for experiments that combine spatial resolution with spectral information. In such cases, simulations are often performed using codes based on the Monte Carlo method. In a simple Monte Carlo approach, the interaction position of an X-ray photon and the state of the photon after an interaction are obtained simply according to the theoretical probability distributions. This approach may be quite inefficient because the final channels of interest may include only a limited region of space or photons produced by a rare interaction, e.g., fluorescent emission from elements with very low concentrations. In the field of X-ray fluorescence spectroscopy, this problem has been solved by combining the Monte Carlo method with variance reduction techniques, which can reduce the computation time by several orders of magnitude. In this work, we present a C++ code for the general simulation of X-ray imaging and spectroscopy experiments, based on the application of the Monte Carlo method in combination with variance reduction techniques, with a description of sample geometry based on quadric surfaces. We describe the benefits of the object-oriented approach in terms of code maintenance, the flexibility of the program for the simulation of different experimental conditions and the possibility of easily adding new modules. Sample applications in the fields of X-ray imaging and X-ray spectroscopy are discussed. Catalogue identifier: AERO_v1_0 Program summary URL:http://cpc.cs.qub.ac.uk/summaries/AERO_v1_0.html Program obtainable from: CPC Program Library, Queen’s University, Belfast, N. Ireland

  9. Photoinduced molecular chirality probed by ultrafast resonant X-ray spectroscopy

    Directory of Open Access Journals (Sweden)

    Jérémy R. Rouxel

    2017-07-01

    Full Text Available Recently developed circularly polarized X-ray light sources can probe the ultrafast chiral electronic and nuclear dynamics through spatially localized resonant core transitions. We present simulations of time-resolved circular dichroism signals given by the difference of left and right circularly polarized X-ray probe transmission following an excitation by a circularly polarized optical pump with the variable time delay. Application is made to formamide which is achiral in the ground state and assumes two chiral geometries upon optical excitation to the first valence excited state. Probes resonant with various K-edges (C, N, and O provide different local windows onto the parity breaking geometry change thus revealing the enantiomer asymmetry.

  10. Precision Spectroscopy of Kaonic Helium-3 Atoms X-rays at J-PARC

    Directory of Open Access Journals (Sweden)

    Tanida K.

    2010-04-01

    Full Text Available We will measure the Balmer-series x-rays of kaonic-3He atoms using large-area high-resolution silicon drift x-rays detectors in order to provide the crucial information of K−-nucleus strong interaction at the low energy limit. The strong interaction 2p level shift will be determined with a precision of a few eV. At the present status, the construction of all detectors is in progress. In February, 2009, the first tuning of K1.8BR beamline was performed by the secondary beam generated in J-PARC hadron facility. The data taking will be started soon.

  11. Bragg x-ray optics for imaging spectroscopy of plasma microsources.

    Science.gov (United States)

    Pikuz, T A; Ya Faenov, A; Pikuz, S A; Romanova, V M; Shelkovenko, T A

    1995-01-01

    Bragg x-ray optics based on crystals with transmission and reflection properties bent on cylindrical or spherical surfaces are discussed. Applications of such optics for obtaining one- and two-dimensional monochromatic images of different plasma sources in the wide spectral range 1-20 Å are described. Samples of spectra obtained with spectral resolution of up to λ/Δλ ~ 10,000 and spatial resolution of up to 18 μm are presented.

  12. Comprehensive Study of Hydrated IDPs: X-Ray Diffraction, IR Spectroscopy and Electron Microscopic Analysis

    Science.gov (United States)

    Nakamura, K.; Keller, L. P.; Nakamura, T.; Noguchi, T.; Nozaki, W.; Tomeoka, K.

    2003-01-01

    Chondritic hydrated interplanetary dust particles (IDPs) comprise up to 50% of all IDPs collected in the stratosphere(1). Although much is known about the mineralogy, chemistry and carbon abundance of hydrated IDPs (2-4) controversies still exist regarding their formation, history, and relationship to other primitive solar system materials. Hydrated IDPs are generally believed to be derived from asteroidal sources that have undergone some degree of aqueous alteration. However, the high C contents of hydrated IDPs (by 2 to 6X CI levels (3,4) indicate that they are probably not derived from the same parent bodies sampled by the known chondritic meteorites. We report the comprehensive study of individual hydrated IDPs. The strong depletion in Ca (I) has been used as a diagnostic feature of hydrated IDPs. The particles are embedded in elemental sulfur or low viscosity epoxy and ultramicrotomed thin sections are observed using a transmission electron microscope (TEM) equipped with an energy-dispersive X-ray detector (EDX) followed by other measurements including: 1) FTIR microspectroscopy to understand the significant constraints on the organic functionality and the nature of the C-bearing phases and 2) powder X-ray difiaction using a synchrotron X-ray source to understand the bulk mineralogy of the particles.

  13. Debris of potassium–magnesium silicate glass generated by femtosecond laser-induced ablation in air: An analysis by near edge X-ray absorption spectroscopy, micro Raman and energy dispersive X-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Grehn, M., E-mail: grehn@physik.tu-berlin.de [Technische Universität Berlin, Institut für Optik und Atomare Physik, Straße des 17. Juni 135, 10623 Berlin (Germany); Seuthe, T. [Fraunhofer-Institut für Keramische Technologien und Systeme (IKTS), Winterbergstraße 28, 01277 Dresden (Germany); Reinhardt, F. [Physikalisch-Technische Bundesanstalt (PTB), Albert-Einstein-Straße 15, 12489 Berlin (Germany); Höfner, M.; Griga, N. [Technische Universität Berlin, Institut für Optik und Atomare Physik, Straße des 17. Juni 135, 10623 Berlin (Germany); Eberstein, M. [Fraunhofer-Institut für Keramische Technologien und Systeme (IKTS), Winterbergstraße 28, 01277 Dresden (Germany); Bonse, J. [BAM Bundesanstalt für Materialforschung und –prüfung, Unter den Eichen 87, 12205 Berlin (Germany)

    2014-05-01

    The redeposited material (debris) resulting from ablation of a potassium–magnesium silicate glass upon scanning femtosecond laser pulse irradiation (130 fs, 800 nm) in air environment is investigated by means of three complementary surface analytical methods. Changes in the electronic band structure of the glass constituent Magnesium (Mg) were identified by X-ray Absorption Near Edge Structure spectroscopy (XANES) using synchrotron radiation. An up-shift of ≈0.8 eV of a specific Magnesium K-edge absorption peak in the spectrum of the redeposited material along with a significant change in its leading edge position was detected. In contrast, the surface left after laser ablation exhibits a downshift of the peak position by ≈0.9 eV. Both observations may be related to a change of the Mg coordinative state of the laser modified/redeposited glass material. The presence of carbon in the debris is revealed by micro Raman spectroscopy (μ-RS) and was confirmed by energy dispersive X-ray spectroscopy (EDX). These observations are attributed to structural changes and chemical reactions taking place during the ablation process.

  14. Design and Performance of a TES X-ray Microcalorimeter Array for Energy Dispersive Spectroscopy on Scanning Transmission Electron Microscope

    Science.gov (United States)

    Muramatsu, Haruka; Nagayoshi, K.; Hayashi, T.; Sakai, K.; Yamamoto, R.; Mitsuda, K.; Yamasaki, N. Y.; Maehata, K.; Hara, T.

    2016-07-01

    We discuss the design and performance of a transition edge sensor (TES) X-ray microcalorimeter array for scanning transmission electron microscope (STEM)-energy dispersive X-ray spectroscopy (EDS). The TES X-ray microcalorimeter has better energy resolution compared to conventional silicon drift detector and STEM-EDS utilizing a TES detector makes it possible to map the distribution of elements on a specimen in addition to analyze the composition. The requirement for a TES detector is a high counting rate (>20 kcps), wide energy band (0.5-15 keV) and good energy resolution (<10 eV) full width at half maximum. The major improvement of this development is to increase the maximum counting rate. In order to accommodate the high counting rate, we adopted an 8 × 8 format, 64-pixel array and common biasing scheme for the readout method. We did all design and fabrication of the device in house. With the device we have fabricated most recently, the pulse decay time is 40 \\upmu s which is expected to achieve 50 kcps. For a single pixel, the measured energy resolution was 7.8 eV at 5.9 keV. This device satisfies the requirements of counting rate and energy resolution, although several issues remain where the performance must be confirmed.

  15. Study on the coordination structure of pt sorbed on bacterial cells using x-ray absorption fine structure spectroscopy.

    Directory of Open Access Journals (Sweden)

    Kazuya Tanaka

    Full Text Available Biosorption has been intensively investigated as a promising technology for the recovery of precious metals from solution. However, the detailed mechanism responsible for the biosorption of Pt on a biomass is not fully understood because of a lack of spectroscopic studies. We applied X-ray absorption fine structure spectroscopy to elucidate the coordination structure of Pt sorbed on bacterial cells. We examined the sorption of Pt(II and Pt(IV species on bacterial cells of Bacillus subtilis and Shewanella putrefaciens in NaCl solutions. X-ray absorption near-edge structure and extended X-ray absorption fine structure (EXAFS of Pt-sorbed bacteria suggested that Pt(IV was reduced to Pt(II on the cell's surface, even in the absence of an organic material as an exogenous electron donor. EXAFS spectra demonstrated that Pt sorbed on bacterial cells has a fourfold coordination of chlorine ions, similar to PtCl42-, which indicated that sorption on the protonated amine groups of the bacterial cells. This work clearly demonstrated the coordination structure of Pt sorbed on bacterial cells. The findings of this study will contribute to the understanding of Pt biosorption on biomass, and facilitate the development of recovery methods for rare metals using biosorbent materials.

  16. Direct Detection of Oxygen Ligation to the Mn4Ca Cluster of Photosystem II by X-ray Emission Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Pushkar, Yulia; Long, Xi; Glatzel, Pieter; Brudvig, Gary W.; Dismukes, G. Charles; Collins, Terrence J.; Yachandra, Vittal K.; Yano, Junko; Bergmann, Uwe

    2009-06-16

    Ligands play critical roles during the catalytic reactions in metalloproteins through bond formation/breaking, protonation/deprotonation, and electron/spin delocalization. While there are well-defined element-specific spectroscopic handles, such as X-ray spectroscopy and EPR, to follow the chemistry of metal catalytic sites in a large protein matrix, directly probing particular ligand atoms like C, N, and O is challenging due to their abundance in the protein. FTIR/Raman and ligand-sensitive EPR techniques such as ENDOR and ESEEM have been applied to study metal-ligand interactions. X-ray absorption spectroscopy (XAS) can also indirectly probe the ligand environment; its element-specificity allows us to focus only on the catalytic metal site, and EXAFS and XANES provide metal-ligand distances, coordination numbers, and symmetry of ligand environments. However, the information is limited, since one cannot distinguish among ligand elements with similar atomic number (i.e. C, N. and O). As an alternative and a more direct method to probe the specific metal-ligand chemistry in the protein matrix, we investigated the application of X-ray emission spectroscopy (XES). Using this technique we have identified the oxo-bridging ligands of the Mn{sub 4}Ca complex of photosystem II (PS II), a multisubunit membrane protein, that catalyzes the water oxidizing reaction. The catalytic mechanism has been studied intensively by Mn XAS. The fundamental question of this reaction, however, is how the water molecules are ligated to the Mn{sub 4}Ca cluster and how the O-O bond formation occurs before the evolution of O{sub 2}. This implies that it is necessary to follow the chemistry of the oxygen ligands in order to understand the mechanism.

  17. Gadolinium Deposition in Nephrogenic Systemic Fibrosis: An Examination of Tissue using Synchrotron X-ray Fluorescence Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    High, W.; Ranville, J; Brown, M; Punshon, T; Lanzirotti, A; Jackson, B

    2010-01-01

    Nephrogenic systemic fibrosis is a fibrosing disorder associated with gadolinium (Gd)-based contrast agents dosed during renal insufficiency. In two patients, Gd deposition in tissue affected by nephrogenic systemic fibrosis was quantified using inductively coupled plasma mass spectrometry. The presence of Gd was confirmed and mapped using synchrotron x-ray fluorescence spectroscopy. Affected skin and soft tissue from the lower extremity demonstrated 89 and 209 ppm ({micro}g/g, dry weight, formalin fixed) in cases 1 and 2, respectively. In case 2, the same skin and soft tissue was retested after paraffin embedding, with the fat content removed by xylene washes, and this resulted in a measured value of 189 ppm ({micro}g/g, dry weight, paraffin embedded). Synchrotron x-ray fluorescence spectroscopy confirmed Gd in the affected tissue of both cases, and provided high-sensitivity and high-resolution spatial mapping of Gd deposition. A gradient of Gd deposition in tissue correlated with fibrosis and cellularity. Gd deposited in periadnexal locations within the skin, including hair and eccrine ducts, where it colocalized to areas of high calcium and zinc content. Because of the difficulty in obtaining synchrotron x-ray fluorescence spectroscopy scans, tissue from only two patients were mapped. A single control with kidney disease and gadolinium-based contrast agent exposure did not contain Gd. Gd content on a gravimetric basis was impacted by processing that removed fat and altered the dry weight of the specimens. Gradients of Gd deposition in tissue corresponded to fibrosis and cellularity. Adnexal deposition of Gd correlated with areas of high calcium and zinc content.

  18. X-ray absorption spectroscopy by full-field X-ray microscopy of a thin graphite flake: Imaging and electronic structure via the carbon K-edge

    Directory of Open Access Journals (Sweden)

    Carla Bittencourt

    2012-04-01

    Full Text Available We demonstrate that near-edge X-ray-absorption fine-structure spectra combined with full-field transmission X-ray microscopy can be used to study the electronic structure of graphite flakes consisting of a few graphene layers. The flake was produced by exfoliation using sodium cholate and then isolated by means of density-gradient ultracentrifugation. An image sequence around the carbon K-edge, analyzed by using reference spectra for the in-plane and out-of-plane regions of the sample, is used to map and spectrally characterize the flat and folded regions of the flake. Additional spectral features in both π and σ regions are observed, which may be related to the presence of topological defects. Doping by metal impurities that were present in the original exfoliated graphite is indicated by the presence of a pre-edge signal at 284.2 eV.

  19. Center for X-Ray Optics, 1992

    Energy Technology Data Exchange (ETDEWEB)

    1993-08-01

    This report discusses the following topics: Center for X-Ray Optics; Soft X-Ray Imaging wit Zone Plate Lenses; Biological X-Ray microscopy; Extreme Ultraviolet Lithography for Nanoelectronic Pattern Transfer; Multilayer Reflective Optics; EUV/Soft X-ray Reflectometer; Photoemission Microscopy with Reflective Optics; Spectroscopy with Soft X-Rays; Hard X-Ray Microprobe; Coronary Angiography; and Atomic Scattering Factors.

  20. Temperature dependence of Al0.2Ga0.8As X-ray photodiodes for X-ray spectroscopy

    Science.gov (United States)

    Whitaker, M. D. C.; Butera, S.; Lioliou, G.; Barnett, A. M.

    2017-07-01

    Two custom-made Al0.2Ga0.8As p+-i-n+ mesa X-ray photodiodes (200 μm diameter, 3 μm i layer) have been electrically characterised across the temperature range -20 °C to 60 °C. The devices were connected to a custom-made charge sensitive preamplifier to produce an AlGaAs photon-counting X-ray spectrometer. The devices' responses to illumination with soft X-rays from an 55Fe radioisotope X-ray source (Mn Kα = 5.9 keV; Mn Kβ = 6.49 keV) were investigated across the temperature range -20 °C to 20 °C. The best energy resolution (FWHM at 5.9 keV) achieved at 20 °C was 1.06 keV (with the detector at 10 V reverse bias). Improved FWHM was observed with the devices at temperatures of 0 °C (0.86 keV) and -20 °C (0.83 keV) with the photodiode reverse biased at 30 V. The average electron hole pair creation energy was experimentally measured and determined to be 4.43 eV ± 0.09 eV at 20 °C, 4.44 eV ± 0.10 eV at 0 °C, and 4.56 eV ± 0.10 eV at -20 °C.

  1. Observation of electric potential in organic thin-film transistor by bias-applied hard X-ray photoemission spectroscopy

    Science.gov (United States)

    Watanabe, Takeshi; Tada, Keisuke; Yasuno, Satoshi; Oji, Hiroshi; Yoshimoto, Noriyuki; Hirosawa, Ichiro

    2016-03-01

    The effect of gate voltage on electric potential in a pentacene (PEN) layer was studied by hard X-ray photoelectron spectroscopy under a bias voltage. It was observed that applying a negative gate voltage substantially increases the width of a C 1s peak. This suggested that injected and accumulated carriers in an organic thin film transistor channel modified the potential depth profile in PEN. It was also observed that the C 1s kinetic energy tends to increase monotonically with threshold voltage.

  2. NATURAL CYCLOPENTANOID CYANOHYDRIN GLYCOSIDES .13. STRUCTURE DETERMINATION OF NATURAL EPOXYCYCLOPENTANES BY X-RAY CRYSTALLOGRAPHY AND NMR-SPECTROSCOPY

    DEFF Research Database (Denmark)

    Olafsdottir, E. S.; Sorensen, A. M.; Cornett, Claus

    1991-01-01

    nonannellated cyclopentane derivatives. The new glucosides were shown, by NMR spectroscopy (including NOE measurements), X-ray crystallography, and enzymatic hydrolysis to the corresponding cyanohydrins, to be (1R,2R,3R,4R)- and (1S,2S,3S,4S)-1-(beta-D-glucopyranosyloxy)-2,3-epoxy-4-hydroxycyclopenta ne-1...... side as the three oxygen substituents. In addition to the glucosides, two amides, (1S,2S,3R,4R)-2,3-epoxy-1,4-dihydroxycyclopentane-1-carboxamide and (1S,4R)-1,4-dihydroxy-2-cyclopentene-1-carboxamide, were isolated from P. suberosa and characterized; the amides are probably artefacts...

  3. An Energy Dispersive X-ray Spectroscopy Analysis of Elemental Changes of a Persimmon Phytobezoar Dissolved in Coca-Cola.

    Science.gov (United States)

    Iwamuro, Masaya; Urata, Haruo; Higashi, Reiji; Nakagawa, Masahiro; Ishikawa, Shin; Shiraha, Hidenori; Okada, Hiroyuki

    To investigate the mechanism of phytobezoar dissolution by Coca-Cola(®), persimmon phytobezoar pieces removed from a 60-year-old Japanese woman were analyzed by energy dispersive X-ray spectroscopy. The amount of calcium significantly decreased after dissolution treatment using Coca-Cola(®), suggesting a potential contribution of calcium to dissolution mechanisms. Moreover, immersion in Coca-Cola(®) for 120 hours on the exterior surface revealed that Coca-Cola(®) did not permeate persimmon phytobezoars. This is the first study to investigate the mechanisms of persimmon phytobezoar permeability and dissolution induced by Coca-Cola(®).

  4. Optical Spectroscopy of the High-mass X-ray Binary A0535+26 after the periastron

    Science.gov (United States)

    Stoyanov, K. A.; Zamanov, R.

    2016-02-01

    We present optical spectroscopy of the & nbsp; High-mass X-ray Binary A0535+26 (HDE 245770, V725 Tau) after the periastron passage (Giovannelli, Bisnovatyi-Kogan & amp; Klepnev, 2013, A & amp;A, 560, 1). The observations are performed with the ESpeRo spectrograph on the 2m RCC telescope at Rozhen NAO (Bulgaria) on the nights of 2015 Dec 24 (JD2457381.4285) and 2016 Jan 30 (JD2457418.2045). & nbsp; The equivalent widths of H-alpha emission line are -(11.5 & plusmn;1.5) Angstrom and -(9.3 & plusmn;1.0) Angstrom respectively.

  5. Medieval glass from the Cathedral in Paderborn: a comparative study using X-ray absorption spectroscopy, X-ray fluorescence, and inductively coupled laser ablation mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hormes, J. [University of Saskatchewan, Canadian Light Source Inc., Saskatoon, SK (Canada); Louisiana State University, CAMD, Baton Rouge, LA (United States); Roy, A.; Bovenkamp, G.L. [Louisiana State University, CAMD, Baton Rouge, LA (United States); Simon, K. [University of Goettingen, Geochemistry, Centre for Geosciences, Goettingen (Germany); Kim, C.Y. [University of Saskatchewan, Canadian Light Source Inc., Saskatoon, SK (Canada); Boerste, N. [Faculty for Theology Paderborn, Paderborn (Germany); Gai, S. [LWL - Archaeologie fuer Westfalen, Muenster (Germany)

    2013-04-15

    We have investigated four stained glass samples recovered from an archaeological excavation at the Cathedral in Paderborn (Germany) between 1978 and 1980. On two of the samples there are parts of paintings. Concentrations of major elements were determined using two independent techniques: LA-ICP-MS (a UV laser ablation microsampler combined with an inductively coupled plasma mass spectrometer) and synchrotron radiation X-ray excited X-ray fluorescence (SR-XRF). The SR-XRF data were quantified by using the program package PyMCA developed by the software group of the ESRF in Grenoble. Significant differences were found between the concentrations determined by the two techniques that can be explained by concentration gradients near the surface of the glasses caused, for example, by corrosion/leaching processes and the different surface sensitivities of the applied techniques. For several of the elements that were detected in the glass and in the colour pigments used for the paintings X-ray absorption near edge structure (XANES) spectra were recorded in order to determine the chemical speciation of the elements of interest. As was expected, most elements in the glass were found as oxides in their most stable form. Two notable exceptions were observed: titanium was not found as rutile - the most stable form of TiO{sub 2} - but in the form of anatase, and lead was not found in one defined chemical state but as a complex mixture of oxide, sulphate, and other compounds. (orig.)

  6. Quarry identification of historical building materials by means of laser induced breakdown spectroscopy, X-ray fluorescence and chemometric analysis

    Science.gov (United States)

    Colao, F.; Fantoni, R.; Ortiz, P.; Vazquez, M. A.; Martin, J. M.; Ortiz, R.; Idris, N.

    2010-08-01

    To characterize historical building materials according to the geographic origin of the quarries from which they have been mined, the relative content of major and trace elements were determined by means of Laser Induced Breakdown Spectroscopy (LIBS) and X-ray Fluorescence (XRF) techniques. 48 different specimens were studied and the entire samples' set was divided in two different groups: the first, used as reference set, was composed by samples mined from eight different quarries located in Seville province; the second group was composed by specimens of unknown provenance collected in several historical buildings and churches in the city of Seville. Data reduction and analysis on laser induced breakdown spectroscopy and X-ray fluorescence measurements was performed using multivariate statistical approach, namely the Linear Discriminant Analysis (LDA), Principal Component Analysis (PCA) and Soft Independent Modeling of Class Analogy (SIMCA). A clear separation among reference sample materials mined from different quarries was observed in Principal Components (PC) score plots, then a supervised soft independent modeling of class analogy classification was trained and run, aiming to assess the provenance of unknown samples according to their elemental content. The obtained results were compared with the provenance assignments made on the basis of petrographical description. This work gives experimental evidence that laser induced breakdown spectroscopy measurements on a relatively small set of elements is a fast and effective method for the purpose of origin identification.

  7. Solvation structure of the halides from x-ray absorption spectroscopy

    Science.gov (United States)

    Antalek, Matthew; Pace, Elisabetta; Hedman, Britt; Hodgson, Keith O.; Chillemi, Giovanni; Benfatto, Maurizio; Sarangi, Ritimukta

    2016-01-01

    Three-dimensional models for the aqueous solvation structures of chloride, bromide, and iodide are reported. K-edge extended X-ray absorption fine structure (EXAFS) and Minuit X-ray absorption near edge (MXAN) analyses found well-defined single shell solvation spheres for bromide and iodide. However, dissolved chloride proved structurally distinct, with two solvation shells needed to explain its strikingly different X-ray absorption near edge structure (XANES) spectrum. Final solvation models were as follows: iodide, 8 water molecules at 3.60 ± 0.13 Å and bromide, 8 water molecules at 3.40 ± 0.14 Å, while chloride solvation included 7 water molecules at 3.15 ± 0.10 Å, and a second shell of 7 water molecules at 4.14 ± 0.30 Å. Each of the three derived solvation shells is approximately uniformly disposed about the halides, with no global asymmetry. Time-dependent density functional theory calculations simulating the chloride XANES spectra following from alternative solvation spheres revealed surprising sensitivity of the electronic state to 6-, 7-, or 8-coordination, implying a strongly bounded phase space for the correct structure during an MXAN fit. MXAN analysis further showed that the asymmetric solvation predicted from molecular dynamics simulations using halide polarization can play no significant part in bulk solvation. Classical molecular dynamics used to explore chloride solvation found a 7-water solvation shell at 3.12 (−0.04/+0.3) Å, supporting the experimental result. These experiments provide the first fully three-dimensional structures presenting to atomic resolution the aqueous solvation spheres of the larger halide ions. PMID:27475372

  8. Identifying isomers of C-78 by means of x-ray spectroscopy

    DEFF Research Database (Denmark)

    Bassan, Arianna; Nyberg, Mats; Luo, Yi

    2002-01-01

    X-ray photoelectron and absorption spectra of C-78 isomers have been generated using density functional theory with inclusion of the full core-hole potentials. Strong isomer dependence has been found in absorption, but not in the photoelectron spectra. C-78 isomers can be thought to be formed by ...... by inserting 18 carbon atoms into an opened C-60. We have shown how the different local arrangements of these 18 carbon atoms are responsible for the significant isomer dependence observed. Our calculated spectra are in excellent agreement with the experimental counterparts....

  9. X-Ray Spectroscopy of Optically Bright Planets using the Chandra Observatory

    Science.gov (United States)

    Ford, P. G.; Elsner, R. F.

    2005-01-01

    Since its launch in July 1999, Chandra's Advanced CCD Imaging Spectrometer (ACIS) has observed several planets (Venus, Mars, Jupiter and Saturn) and 6 comets. At 0.5 arc-second spatial resolution, ACIS detects individual x-ray photons with good quantum efficiency (25% at 0.6 KeV) and energy resolution (20% FWHM at 0.6 KeV). However, the ACIS CCDs are also sensitive to optical and near-infrared light, which is absorbed by optical blocking filters (OBFs) that eliminate optical contamination from all but the brightest extended sources, e.g., planets. .Jupiter at opposition subseconds approx.45 arc-seconds (90 CCD pixels.) Since Chandra is incapable of tracking a moving target, the planet takes 10 - 20 kiloseconds to move across the most sensitive ACIS CCD, after which the observatory must be re-pointed. Meanwhile, the OBF covering that CCD adds an opt,ical signal equivalent to approx.110 eV to each pixel that lies within thc outline of the Jovian disk. This has three consequences: (1) the observatory must be pointed away from Jupiter while CCD bias maps are constructed; (2) most x-rays from within the optical image will be misidentified as charged-particle background and ignored; and (3) those x-rays that are reported will bc assigned anomalously high energies. The same also applies to thc other planets, but is less serious since they are either dimmer at optical wavelengths, or they show less apparent motion across the sky, permitting reduced CCD exposure times: the optical contamination from Saturn acids approx.15 eV per pixel, and from Mars and Venus approx.31 eV. After analyzing a series of short .Jupiter observations in December 2000, ACIS parameters were optimized for the February 2003 opposition. CCD bias maps were constructed while Chandra pointed away from Jupiter, and the subsequent observations employed on-board software to ignore any pixel that contained less charge than that expected from optical leakage. In addition, ACIS was commanded to report 5 x 5

  10. Comparison Between X-rays Absorption and Emission Spectroscopy Measurements on a Ceramic Envelop Lamp

    Science.gov (United States)

    Lafitte, Bruno; Aubes, Michel; Zissis, Georges

    2007-12-01

    Burners of metal halide lamps used for illumination are generally made of polycrystalline alumina ceramic (PCA) which is translucent to visible light. We show that the difficulty of selecting a line of sight through the lamp prevents the use of optical emission diagnostic. X-rays photons are mainly absorbed and not scattered by PCA. Absorption by mercury atoms contributing to the discharge allowed us to determine the density of mercury in the lamp. By comparing diagnostic methods, we put in evidence the difficulty of taking into account the scattering of light mathematically.

  11. Spatially resolved x-ray spectroscopy investigation of femtosecond laser irradiated Ar clusters.

    Science.gov (United States)

    Junkel-Vives, G C; Abdallah, J; Auguste, T; D'Oliveira, P; Hulin, S; Monot, P; Dobosz, S; Faenov, A Ya; Magunov, A I; Pikuz, T A; Skobelev, I Yu; Boldarev, A S; Gasilov, V A

    2002-03-01

    High temperature plasmas have been created by irradiating Ar clusters with high intensity 60-fs laser pulses. Detailed spectroscopic analysis of spatially resolved, high resolution x-ray data near the He(alpha) line of Ar is consistent with a two-temperature collisional-radiative model incorporating the effects of highly energetic electrons. The results of the spectral analysis are compared with a theoretical hydrodynamic model of cluster production, as well as interferometric data. The plasma parameters are notably uniform over one Rayleigh length (600 microm).

  12. Local detection of X-ray spectroscopies with an in-situ AFM

    OpenAIRE

    Rodrigues, Mario; Dhez, Olivier; Le Denmat, Simon; Chevrier, Joël; Felici, Roberto; Comin, Fabio

    2008-01-01

    International audience; The in situ combination of Scanning Probe Microscopies (SPM) with X-ray microbeams adds a variety of new possibilities to the panoply of synchrotron radiation techniques. In this paper we describe an optics-free AFM/STM that can be directly installed on synchrotron radiation end stations for such combined experiments. The instrument can be used just for AFM imaging of the investigated sample or can be used for detection of photoemitted electrons with a sharp STM-like t...

  13. NuSTAR Spectroscopy of Multi-Component X-Ray Reflection from NGC 1068

    DEFF Research Database (Denmark)

    Bauer, Franz E.; Arevalo, Patricia; Walton, Dominic J.

    2015-01-01

    We report on high-energy X-ray observations of the Compton-thick Seyfert 2 galaxy NGC 1068 with NuSTAR, which provide the best constraints to date on its >10 keV spectral shape. The NuSTAR data are consistent with those from past and current instruments to within cross-calibration uncertainties......, and we find no strong continuum or line variability over the past two decades, which is in line with its X-ray classification as a reflection-dominated Compton-thick active galactic nucleus. The combined NuSTAR, Chandra, XMM-Newton, and Swift BAT spectral data set offers new insights into the complex......, inconsistent viewing angles, or poor fits to the spatially resolved spectra). A multi-component reflector with three distinct column densities (e.g., with best-fit values of N-H of 1.4 x 10(23), 5.0 x 10(24), and 10(25) cm(-2)) provides a more reasonable fit to the spectral lines and Compton hump, with near...

  14. X-ray Induced Luminescence Spectroscopy of Samarium Doped Barium Sulfate Prepared by Sintering Method

    Science.gov (United States)

    Kumeda, T.; Maeda, K.; Shirano, Y.; Fujiwara, K.; Sakai, K.; Ikari, T.

    2015-06-01

    X-ray induced luminescence (XL) properties of phosphor materials made of samarium doped barium sulfate have been investigated. The samples were prepared by sintering method heated at 900-1250 °C for 3 hours in air from the mixture of BaSO4 and Sm2O3. The concentration of Sm were prepared from 0.01-6 at.%. In as-prepared sample, the Sm3+ was detected by photoluminescence (PL). The PL intensity is maximum about 2 at.% with Sm, and then starts decreasing. The PL intensity showed concentration quenching. The XL observed Sm2+ and Sm3+ ions. The XL was shown from the sample sintered up to 1200 °C. The XL intensity increased with Sm concentration up to 1 at.%. The intensity was almost constant larger than 1 at.% Sm. These concentration dependences is different since the X-ray energy absorbed to the host material at once, and the energy transferred to both Sm3+ and Sm2+ ions. Sm doped BaSO4 is found a host for XL phosphor materials.

  15. High-Energy Resolution Fluorescence Detected X-Ray Absorption Spectroscopy: A Powerful New Structural Tool in Environmental Biogeochemistry Sciences.

    Science.gov (United States)

    Proux, Olivier; Lahera, Eric; Del Net, William; Kieffer, Isabelle; Rovezzi, Mauro; Testemale, Denis; Irar, Mohammed; Thomas, Sara; Aguilar-Tapia, Antonio; Bazarkina, Elena F; Prat, Alain; Tella, Marie; Auffan, Mélanie; Rose, Jérôme; Hazemann, Jean-Louis

    2017-11-01

    The study of the speciation of highly diluted elements by X-ray absorption spectroscopy (XAS) is extremely challenging, especially in environmental biogeochemistry sciences. Here we present an innovative synchrotron spectroscopy technique: high-energy resolution fluorescence detected XAS (HERFD-XAS). With this approach, measurement of the XAS signal in fluorescence mode using a crystal analyzer spectrometer with a ∼1-eV energy resolution helps to overcome restrictions on sample concentrations that can be typically measured with a solid-state detector. We briefly describe the method, from both an instrumental and spectroscopic point of view, and emphasize the effects of energy resolution on the XAS measurements. We then illustrate the positive impact of this technique in terms of detection limit with two examples dealing with Ce in ecologically relevant organisms and with Hg species in natural environments. The sharp and well-marked features of the HERFD-X-ray absorption near-edge structure spectra obtained enable us to determine unambiguously and with greater precision the speciation of the probed elements. This is a major technological advance, with strong benefits for the study of highly diluted elements using XAS. It also opens new possibilities to explore the speciation of a target chemical element at natural concentration levels, which is critical in the fields of environmental and biogeochemistry sciences. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

  16. Electron band bending and surface sensitivity: X-ray photoelectron spectroscopy of polar GaN surfaces

    Science.gov (United States)

    Bartoš, I.; Romanyuk, O.; Paskova, T.; Jiříček, P.

    2017-10-01

    The role of electron band bending and surface sensitivity in determining the core level binding energies by X-ray photoelectron spectroscopy is investigated. A dominating contribution of surface atomic layers to photoemission intensity is confirmed for normal photoemission. The energy of the photoelectron core level peak does not deviate from core level peak energies of electrons photoemitted from the surface atomic layers of the crystal. The higher surface sensitivity regime, achieved e.g. at off-normal photoelectron detection angle, can be used to study the surface potential barrier in just a few topmost atomic layers. In addition, it is demonstrated that core level binding energy measured by angle-resolved X-ray photoelectron spectroscopy reflect the electron attenuation anisotropy. In particular, core level binding energy changes with emission angle and correlates with the forward focusing directions in a crystal. This effect is demonstrated by measuring the polar angle dependence of Ga 3d core levels on clean GaN(0001) and GaN(000 1 bar) surfaces with a higher and a lower band bending, respectively. The effect is explained by variation of emission depth in a crystal for normal and off-normal photoelectron emission angles.

  17. Moessbauer spectroscopy and X-ray diffraction analyses of clayey samples used as ceramic sourcing materials, in Peru

    Energy Technology Data Exchange (ETDEWEB)

    Quille, Ruben, E-mail: quilleruben@gmail.com; Bustamante, Angel [San Marcos National University, Laboratory of Ceramics and Nanomaterials, Faculty of Physical Sciences (Peru); Palomino, Ybar [National University of San Cristobal de Huamanga, Experimental Center of Ceramics (Peru)

    2011-11-15

    The ceramic industry is an important area of economic activity in the Ayacucho Region, in particular in the District of Quinua. As a consequence, there is a huge demand for clay to produce ceramic pastes in that region. This paper reports on results concerning the mineralogical characterization of four clayey samples, which were collected MAA and SPQA from the area Pampa de La Quinua with geographic coordinates 13 Degree-Sign 02 Prime 49 Double-Prime S 74 Degree-Sign 08 Prime 03 Double-Prime W, CE1M and CE2M from the Quinua locality 13 Degree-Sign 03 Prime 07 Double-Prime S 74 Degree-Sign 08 Prime 31 Double-Prime W, both in the District of Quinua, Province of Huamanga, Ayacucho, Peru. The chemical and mineralogical characterization of these samples was carried out with powder X-ray diffraction detecting quartz, albite, montmorillonite, kaolinite and glauconite mineral phases, Moessbauer spectroscopy detected iron in kaolinite, glauconite and montmorillonite minerals. Chemical analysis was performed through scanning electron microscopy and energy dispersive X-ray spectroscopy. Data obtained from the combination of these techniques provided relevant information about the morphology, chemical composition, and the mineralogy of samples.

  18. Mössbauer spectroscopy and X-ray diffraction analyses of clayey samples used as ceramic sourcing materials, in Peru

    Science.gov (United States)

    Quille, Rubén; Bustamante, Ángel; Palomino, Ybar

    2011-11-01

    The ceramic industry is an important area of economic activity in the Ayacucho Region, in particular in the District of Quinua. As a consequence, there is a huge demand for clay to produce ceramic pastes in that region. This paper reports on results concerning the mineralogical characterization of four clayey samples, which were collected MAA and SPQA from the area Pampa de La Quinua with geographic coordinates 13° 02' 49″ S 74° 08' 03″ W, CE1M and CE2M from the Quinua locality 13° 03' 07″ S 74° 08' 31″ W, both in the District of Quinua, Province of Huamanga, Ayacucho, Peru. The chemical and mineralogical characterization of these samples was carried out with powder X-ray diffraction detecting quartz, albite, montmorillonite, kaolinite and glauconite mineral phases, Mössbauer spectroscopy detected iron in kaolinite, glauconite and montmorillonite minerals. Chemical analysis was performed through scanning electron microscopy and energy dispersive X-ray spectroscopy. Data obtained from the combination of these techniques provided relevant information about the morphology, chemical composition, and the mineralogy of samples.

  19. Probing the hydrogen-bond network of water via time-resolved soft x-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Huse, Nils; Wen, Haidan; Nordlund, Dennis; Szilagyi, Erzsi; Daranciang, Dan; Miller, Timothy A.; Nilsson, Anders; Schoenlein, Robert W.; Lindenberg, Aaron M.

    2009-04-24

    We report time-resolved studies of hydrogen bonding in liquid H2O, in response to direct excitation of the O-H stretch mode at 3 mu m, probed via soft x-ray absorption spectroscopy at the oxygen K-edge. This approach employs a newly developed nanofluidic cell for transient soft x-ray spectroscopy in liquid phase. Distinct changes in the near-edge spectral region (XANES) are observed, and are indicative of a transient temperature rise of 10K following transient laser excitation and rapid thermalization of vibrational energy. The rapid heating occurs at constant volume and the associated increase in internal pressure, estimated to be 8MPa, is manifest by distinct spectral changes that differ from those induced by temperature alone. We conclude that the near-edge spectral shape of the oxygen K-edge is a sensitive probe of internal pressure, opening new possibilities for testing the validity of water models and providing new insight into the nature of hydrogen bonding in water.

  20. On the nature of citrate-derived surface species on Ag nanoparticles: Insights from X-ray photoelectron spectroscopy

    Science.gov (United States)

    Mikhlin, Yuri L.; Vorobyev, Sergey A.; Saikova, Svetlana V.; Vishnyakova, Elena A.; Romanchenko, Alexander S.; Zharkov, Sergey M.; Larichev, Yurii V.

    2018-01-01

    Citrate is an important stabilizing, reducing, and complexing reagent in the wet chemical synthesis of nanoparticles of silver and other metals, however, the exact nature of adsorbates, and its mechanism of action are still uncertain. Here, we applied X-ray photoelectron spectroscopy, soft X-ray absorption near-edge spectroscopy, and other techniques in order to determine the surface composition and to specify the citrate-related species at Ag nanoparticles immobilized from the dense hydrosol prepared using room-temperature reduction of aqueous Ag+ ions with ferrous ions and citrate as stabilizer (Carey Lea method). It was found that, contrary to the common view, the species adsorbed on the Ag nanoparticles are, in large part, products of citrate decomposition comprising an alcohol group and one or two carboxylate bound to the surface Ag, and minor unbound carboxylate group; these may also be mixtures of citrate with lower molecular weight anions. No ketone groups were specified, and very minor surface Ag(I) and Fe (mainly, ferric oxyhydroxides) species were detected. Moreover, the adsorbates were different at AgNPs having various size and shape. The relation between the capping and the particle growth, colloidal stability of the high-concentration sol and properties of AgNPs is briefly considered.

  1. High resolution X-ray emission spectroscopy of water and aqueous ions using the micro-jet technique

    Energy Technology Data Exchange (ETDEWEB)

    Lange, Kathrin M.; Koennecke, Rene; Ghadimi, Samira; Golnak, Ronny [Helmholtz-Zentrum Berlin fuer Materialien und Energie, c/o BESSY GmbH, Albert-Einstein-Strasse 15, 12489 Berlin (Germany); Soldatov, Mikhail A. [Helmholtz-Zentrum Berlin fuer Materialien und Energie, c/o BESSY GmbH, Albert-Einstein-Strasse 15, 12489 Berlin (Germany); Research Center for Nanoscale Structure of Matter, Southern Federal University, Sorge 5, Rostov-na-Donu 344090 (Russian Federation); Hodeck, Kai F. [Helmholtz-Zentrum Berlin fuer Materialien und Energie, c/o BESSY GmbH, Albert-Einstein-Strasse 15, 12489 Berlin (Germany); Soldatov, Alexander [Research Center for Nanoscale Structure of Matter, Southern Federal University, Sorge 5, Rostov-na-Donu 344090 (Russian Federation); Aziz, Emad F., E-mail: Emad.Aziz@helmholtz-berlin.de [Helmholtz-Zentrum Berlin fuer Materialien und Energie, c/o BESSY GmbH, Albert-Einstein-Strasse 15, 12489 Berlin (Germany); Freie Universitaet Berlin, FB Physik, Arnimallee 14, D-14195 Berlin (Germany)

    2010-11-25

    Graphical abstract: Soft X-ray absorption (XA) and emission (XE) spectroscopy is a powerful method for probing the local electronic structure of light elements (e.g. C, O, N, S) and transition metals, which are all of importance for biochemical systems. Here, we report for the first time on the XE spectra of a liquid micro-jet sample in a vacuum environment. We developed a high resolution X-ray emission spectrometer and recorded the spectra of pure water in full agreement with those of the literature, as well as of an aqueous solution of NiCl{sub 2}. For the latter system, ground state Hartree-Fock calculations using a self-consistent reaction field (SCRF) approach were carried out to specify the nature of the d-occupied orbital. Our results confirm the dark-channel-fluorescence-yield mechanism that we recently proposed for the case of metal ions in aqueous solutions. The ability to record absorption and emission spectra of an aqueous liquid-jet opens the way for the study of biochemical systems in physiological media. - Abstract: Soft X-ray absorption (XA) and emission (XE) spectroscopy is a powerful method for probing the local electronic structure of light elements (e.g. C, O, N, S) and transition metals, which are all of importance for biochemical systems. Here, we report for the first time on the XE spectra of a liquid micro-jet sample in a vacuum environment. We developed a high resolution X-ray emission spectrometer and recorded the spectra of pure water in full agreement with those of the literature, as well as of an aqueous solution of NiCl{sub 2}. For the latter system, ground state Hartree-Fock calculations using a self-consistent reaction field (SCRF) approach were carried out to specify the nature of the d-occupied orbital. Our results confirm the dark-channel-fluorescence-yield mechanism that we recently proposed for the case of metal ions in aqueous solutions. The ability to record absorption and emission spectra of an aqueous liquid-jet opens the

  2. Phase analysis study of copper ferrite aluminates by X-ray diffraction and Moessbauer spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Almokhtar, M. E-mail: almoktar@aun.edu.egalmoktar@acc.aun.eun.eg; Abdalla, A.M.Atef M.; Gaffar, M.A

    2004-05-01

    CuFe{sub 2-x}Al{sub x}O{sub 4} (where x=0.0-0.6) have been synthesized at 950 deg. C, 1000 deg. C, 1050 deg. C and 1100 deg. C using the usual ceramic method. The Moessbauer measurements show reasonable values of magnetic as well as electric hyperfine interactions. At higher sintering temperatures, the spinel ferrite phase is partially dissociated forming delafossite phase in addition to the main matrix. The delafossite phase manifested itself as paramagnetic doublet overlapping the main Moessbauer spectra measured at room temperature. Furthermore, X-ray diffraction studies confirmed the presence of the CuFeO{sub 2} (delafossite) phase of Cu-Al ferrite.

  3. Auto-oligomerization and hydration of pyrrole revealed by x-ray absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Advanced Light Source; Schwartz, Craig P.; Uejio, Janel S.; Duffin, Andrew M.; England, Alice H.; Prendergast, David; Saykally, Richard J

    2009-05-29

    Near edge x-ray absorption fine structure (NEXAFS) spectra have been measured at the carbon and nitrogen K-edges of the prototypical aromatic molecule, pyrrole, both in the gas phase and when solvated in water, and compared with spectra simulated using a combination of classical molecular dynamics and first principles density functional theory in the excited state core hole approximation. The excellent agreement enabled detailed assignments. Pyrrole is highly reactive, particularly in water, and reaction products formed by the auto-oligomerization of pyrrole are identified. The solvated spectra have been measured at two different temperatures, indicating that the final states remain largely unaffected by both hydration and temperature. This is somewhat unexpected, since the nitrogen in pyrrole can donate a hydrogen bond to water.

  4. X-ray absorption fine structure spectroscopy of plutonium complexes with bacillus sphaericus

    Energy Technology Data Exchange (ETDEWEB)

    Panak, P.J.; Booth, C.H.; Caulder, D.L.; Bucher, J.J.; Shuh, D.K. [Lawrence Berkeley National Lab. (LBNL), Chemical Sciences Div., The Glenn T. Seaborg Center, Berkeley, CA (United States); Nitsche, H. [Lawrence Berkeley National Lab. (LBNL), Chemical Sciences Div., The Glenn T. Seaborg Center, Berkeley, CA (United States); Univ. of California at Berkeley, Dept. of Chemistry, Berkeley, CA (United States)

    2002-07-01

    Knowledge of the plutonium complexes formed with bacterial cells is critical for predicting the influence of microbial interactions on the migration behavior of actinides in the environment. This investigation describes the interaction of plutonium(VI) with cells of the aerobic soil bacteria, Bacillus sphaericus. The studies include the quantification of carboxylate and phosphate functional groups on the cell walls by potentiometric titration and the determination of the plutonium speciation by X-ray absorption fine structure (XAFS). Extended-XAFS (EXAFS) was used to determine the identity of the Pu(VI) interfacial complex with the bacteria, and the Pu(VI) was found primarily bound to phosphate groups on the cell surface. No carboxylate complexation was detected. (orig.)

  5. Development of a krypton-doped gas symmetry capsule platform for x-ray spectroscopy of implosion cores on the NIF.

    Science.gov (United States)

    Ma, T; Chen, H; Patel, P K; Schneider, M B; Barrios, M A; Casey, D T; Chung, H-K; Hammel, B A; Berzak Hopkins, L F; Jarrott, L C; Khan, S F; Lahmann, B; Nora, R; Rosenberg, M J; Pak, A; Regan, S P; Scott, H A; Sio, H; Spears, B K; Weber, C R

    2016-11-01

    The electron temperature at stagnation of an ICF implosion can be measured from the emission spectrum of high-energy x-rays that pass through the cold material surrounding the hot stagnating core. Here we describe a platform developed on the National Ignition Facility where trace levels of a mid-Z dopant (krypton) are added to the fuel gas of a symcap (symmetry surrogate) implosion to allow for the use of x-ray spectroscopy of the krypton line emission.

  6. Monitoring of the heavy-metal hyperaccumulation in vegetal tissues by X-ray radiography and by femto-second laser induced breakdown spectroscopy.

    Science.gov (United States)

    Kaiser, J; Samek, O; Reale, L; Liska, M; Malina, R; Ritucci, A; Poma, A; Tucci, A; Flora, F; Lai, A; Mancini, L; Tromba, G; Zanini, F; Faenov, A; Pikuz, T; Cinque, G

    2007-02-01

    This article reports on the utilization of X-ray microradiography and laser induced breakdown spectroscopy (LIBS) techniques for investigation of the metal accumulation in different part of leaf samples. The potential of the LIBS-analysis for finding the proper plant species for phytoremediation is compared with the results of microradiography measurements at the HERCULES source at ENEA, Rome (Italy) and X-ray microradiography experiments at the ELETTRA Synchrotron, Trieste (Italy).

  7. Development of a krypton-doped gas symmetry capsule platform for x-ray spectroscopy of implosion cores on the NIF

    Energy Technology Data Exchange (ETDEWEB)

    Ma, T., E-mail: ma8@llnl.gov; Chen, H.; Patel, P. K.; Schneider, M. B.; Barrios, M. A.; Casey, D. T.; Hammel, B. A.; Berzak Hopkins, L. F.; Jarrott, L. C.; Khan, S. F.; Nora, R.; Pak, A.; Scott, H. A.; Spears, B. K.; Weber, C. R. [Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Chung, H.-K. [International Atomic Energy Agency, Vienna (Austria); Lahmann, B.; Sio, H. [Plasma Fusion and Science Center, Massachusetts Institute of Technology, Cambridge, Massachusetts 02139 (United States); Rosenberg, M. J.; Regan, S. P. [Laboratory for Laser Energetics, University of Rochester, Rochester, New York 14623 (United States)

    2016-11-15

    The electron temperature at stagnation of an ICF implosion can be measured from the emission spectrum of high-energy x-rays that pass through the cold material surrounding the hot stagnating core. Here we describe a platform developed on the National Ignition Facility where trace levels of a mid-Z dopant (krypton) are added to the fuel gas of a symcap (symmetry surrogate) implosion to allow for the use of x-ray spectroscopy of the krypton line emission.

  8. Development of a krypton-doped gas symmetry capsule platform for x-ray spectroscopy of implosion cores on the NIF

    Science.gov (United States)

    Ma, T.; Chen, H.; Patel, P. K.; Schneider, M. B.; Barrios, M. A.; Casey, D. T.; Chung, H.-K.; Hammel, B. A.; Berzak Hopkins, L. F.; Jarrott, L. C.; Khan, S. F.; Lahmann, B.; Nora, R.; Rosenberg, M. J.; Pak, A.; Regan, S. P.; Scott, H. A.; Sio, H.; Spears, B. K.; Weber, C. R.

    2016-11-01

    The electron temperature at stagnation of an ICF implosion can be measured from the emission spectrum of high-energy x-rays that pass through the cold material surrounding the hot stagnating core. Here we describe a platform developed on the National Ignition Facility where trace levels of a mid-Z dopant (krypton) are added to the fuel gas of a symcap (symmetry surrogate) implosion to allow for the use of x-ray spectroscopy of the krypton line emission.

  9. X-ray Emission Spectroscopy to Study Ligand Valence Orbitals in Mn Coordination Complexes

    Energy Technology Data Exchange (ETDEWEB)

    Smolentsev, Grigory; Soldatov, Alexander V; Messinger, Johannes; Merz, Kathrin; Weyhermuller, Thomas; Bergmann, Uwe; Pushkar, Yulia; Yano, Junko; Yachandra, Vittal K.; Glatzel, Pieter

    2009-03-02

    We discuss a spectroscopic method to determine the character of chemical bonding and for the identification of metal ligands in coordination and bioinorganic chemistry. It is based on the analysis of satellite lines in X-ray emission spectra that arise from transitions between valence orbitals and the metal ion 1s level (valence-to-core XES). The spectra, in connection with calculations based on density functional theory (DFT), provide information that is complementary to other spectroscopic techniques, in particular X-ray absorption (XANES and EXAFS). The spectral shape is sensitive to protonation of ligands and allows ligands, which differ only slightly in atomic number (e.g., C, N, O...), to be distinguished. A theoretical discussion of the main spectral features is presented in terms of molecular orbitals for a series of Mn model systems: [Mn(H2O)6]2+, [Mn(H2O)5OH]+, [Mn(H2O)5NH2]+, and [Mn(H2O)5NH3]2+. An application of the method, with comparison between theory and experiment, is presented for the solvated Mn2+ ion in water and three Mn coordination complexes, namely [LMn(acac)N3]BPh4, [LMn(B2O3Ph2)(ClO4)], and [LMn(acac)N]BPh4, where L represents 1,4,7-trimethyl-1,4,7-triazacyclononane, acac stands for the 2,4-pentanedionate anion, and B2O3Ph2 represents the 1,3-diphenyl-1,3-dibora-2-oxapropane-1,3-diolato dianion.

  10. Gallium Arsenide detectors for X-ray and electron (beta particle) spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Lioliou, G.; Barnett, A.M.

    2016-11-11

    Results characterizing GaAs p{sup +}-i-n{sup +} mesa photodiodes with a 10 µm i layer for their spectral response under illumination of X-rays and beta particles are presented. A total of 22 devices, having diameters of 200 µm and 400 µm, were electrically characterized at room temperature. All devices showed comparable characteristics with a measured leakage current ranging from 4 nA/cm{sup 2} to 67 nA/cm{sup 2} at an internal electric field of 50 kV/cm. Their unintentionally doped i layers were found to be almost fully depleted at 0 V due to their low doping density. {sup 55}Fe X-ray spectra were obtained using one 200 µm diameter device and one 400 µm diameter device. The best energy resolution (FWHM at 5.9 keV) achieved was 625 eV using the 200 µm and 740 eV using the 400 µm diameter device, respectively. Noise analysis showed that the limiting factor for the energy resolution of the system was the dielectric noise; if this noise was eliminated by better design of the front end of the readout electronics, the achievable resolution would be 250 eV. {sup 63}Ni beta particle spectra obtained using the 200 µm diameter device showed the potential utility of these detectors for electron and beta particle detection. The development of semiconductor electron spectrometers is important particularly for space plasma physics; such devices may find use in future space missions to study the plasma environment of Jupiter and Europa and the predicted electron impact excitation of water vapor plumes from Europa hypothesized as a result of recent Hubble Space Telescope (HST) UV observations.

  11. Applications of X-ray absorption spectroscopy and low temperature XMCD to metalloproteins

    Energy Technology Data Exchange (ETDEWEB)

    Christiansen, J.H. [Univ. of California, Davis, CA (United States). Dept. of Applied Science]|[Lawrence Berkeley National Lab., CA (United States). Energy and Environment Div.

    1996-01-01

    The author has used the extended X-ray absorption fine structure (EXAFS) and ultra-low temperature X-ray magnetic circular dichroism (XMCD) to study the environments of the metal sites in metalloproteins. EXAFS has been used to study the Zn site in spinach carbonic anhydrase. The EXAFS, in parallel with site directed mutagenesis studies, indicate that the active site Zn is in a cys-cys-his-H{sub 2}O environment, very different from the mammalian carbonic anhydrase active site. Nitrogenase, the primary enzyme in biological nitrogen fixation, contains two complex metal clusters of unique structure. EXAFS studies at the Fe and Mo K-edges of nitrogenase solutions and crystals yielded information about the various metal-metal distances in these two clusters. The author assigned 4 Fe and 3 Mo interactions >4 {angstrom}. Single crystal Mo K-edge EXAFS then found a very long Fe-Fe distance of {approximately}5.1 {angstrom}. These distances were then used to further refine the proposed crystallographic models to their highest accuracy yet. Studies were carried further by examining nitrogenas in oxidized and reduced forms--states for which there is no crystallographic information. Small structural changes were observed and an EXAFS model was put forth that attempts to deconvolute the EXAFS distances of the two metal clusters. Nitrogenase Apo I, a genetic mutant of nitrogenase which is though to contain only one of the two different metal clusters, was also examined using EXAFS. These studies showed results consistent with current models, yet the metal clusters were very disordered. Finally, ultra-low temperature methods were used to further the development of XMCD as a technique for studying biological systems. Experiments were performed on the copper in plastocyanin. Data was collected that definitively proves that the sample surface was at 0.55 {+-} 0.05 K. This result opens the door to further study of more complex biological metal clusters.

  12. X-ray spectroscopy study of ThO2 and ThF4

    Directory of Open Access Journals (Sweden)

    Teterin Anton Yu.

    2010-01-01

    Full Text Available The structure of the X-ray photoelectron, X-ray O(FKa-emission spectra from ThO2 and ThF4 as well as the Auger OKLL spectra from ThO2 was studied. The spectral structure was analyzed by using fully relativistic cluster discrete variational calculations of the electronic structure of the ThO8 D4h and ThF8 (C2 clusters reflecting thorium close environment in solid ThO2 and ThF4. As a result it was theoretically found and experimentally confirmed that during the chemical bond formation the filled O(F2p electronic states are distributed mainly in the binding energy range of the outer valence molecular orbitals from 0-13 eV, while the filled O(F2s electronic states - in the binding energy range of the inner valence molecular orbitals from 13-35 eV. It was shown that the Auger OKLL spectral structure from ThO2 characterizes not only the O2p electronic state density distribution, but also the O2s electronic state density distribution. It agrees with the suggestion that O2s electrons participate in formation of the inner valence molecular orbitals, in the binding energy range of 13-35 eV. The relative Auger OKL2-3L2-3 peak intensity was shown to reflect quantitatively the O2p electronic state density of the oxygen ion in ThO2.

  13. CO adsorption on Pd(100) studied by multimodal ambient pressure X-ray photoelectron and infrared reflection absorption spectroscopies

    Science.gov (United States)

    Head, Ashley R.; Karslıoǧlu, Osman; Gerber, Timm; Yu, Yi; Trotochaud, Lena; Raso, Joseph; Kerger, Philipp; Bluhm, Hendrik

    2017-11-01

    The adsorption of CO on Pd(100) was investigated using simultaneous ambient pressure X-ray photoelectron spectroscopy (APXPS) and infrared reflection absorption infrared spectroscopy (IRRAS). The measurements were performed as a function of CO partial pressures from ultra-high vacuum to 0.5 Torr. Total CO coverages estimated from the complementary APXPS and IRRAS measurements are in good agreement. A signal for atop CO, which is uncommon for Pd(100), was observed in the IRRAS data and was used to identify the C 1 s binding energy of this species. Discerning this binding configuration of CO on the Pd(100) surface at elevated pressures has significance for catalytic reactions involving CO, where bridging CO is often the only configuration considered. We also detail the combined APXPS/IRRAS instrumentation and discuss ways to improve these multimodal measurements, which should have wide applicability across many areas of surface and interface science.

  14. Combining X-ray computed tomography and visible near-infrared spectroscopy for prediction of soil structural properties

    DEFF Research Database (Denmark)

    Katuwal, Sheela; Hermansen, Cecilie; Knadel, Maria

    2018-01-01

    squares regression (PLSR) using the vis-NIR data (vis-NIR-PLSR) and multiple linear regression (MLR) based on soil texture and OC. The statistical prediction of macroporosity was poor, with both vis-NIR-PLSR and MLR (R2 ... near-infrared (vis-NIR) spectroscopy is a rapid analytical technique used successfully to predict various soil properties. In this study, the potential of using vis-NIR spectroscopy to predict X-ray CT derived soil structural properties was investigated. In this study, 127 soil samples from six...... (19 by 20 cm). Both macroporosity and CTmatix are soil structural properties that affect the degree of preferential transport. Bulk soils from the 127 sampling locations were scanned with a vis-NIR spectrometer (400–2500 nm). Macroporosity and CTmatrix were statistically predicted with partial least...

  15. Electronic structure simulation of chromium aluminum oxynitride by discrete variational-X alpha method and X-ray photoelectron spectroscopy

    CERN Document Server

    Choi, Y; Lee, J D; Kim, E; No, K

    2002-01-01

    We use a first-principles discrete variational (DV)-X alpha method to investigate the electronic structure of chromium aluminum oxynitride. When nitrogen is substituted for oxygen in the Cr-Al-O system, the N2p level appears in the energy range between O2p and Cr3d levels. Consequently, the valence band of chromium aluminum oxynitride becomes broader and the band gap becomes smaller than that of chromium aluminum oxide, which is consistent with the photoelectron spectra for the valence band using X-ray photoelectron spectroscopy (XPS) and ultraviolet photoelectron spectroscopy (UPS). We expect that this valence band structure of chromium aluminum oxynitride will modify the transmittance slope which is a requirement for photomask application.

  16. Soft X-ray angle-resolved photoemission spectroscopy of heavily boron-doped superconducting diamond films

    Directory of Open Access Journals (Sweden)

    T. Yokoya, T. Nakamura, T. Matushita, T. Muro, H. Okazaki, M. Arita, K. Shimada, H. Namatame, M. Taniguchi, Y. Takano, M. Nagao, T. Takenouchi, H. Kawarada and T. Oguchi

    2006-01-01

    Full Text Available We have performed soft X-ray angle-resolved photoemission spectroscopy (SXARPES of microwave plasma-assisted chemical vapor deposition diamond films with different B concentrations in order to study the origin of the metallic behavior of superconducting diamond. SXARPES results clearly show valence band dispersions with a bandwidth of ~23 eV and with a top of the valence band at gamma point in the Brillouin zone, which are consistent with the calculated valence band dispersions of pure diamond. Boron concentration-dependent band dispersions near the Fermi level (EF exhibit a systematic shift of EF, indicating depopulation of electrons due to hole doping. These SXARPES results indicate that diamond bands retain for heavy boron doping and holes in the diamond band are responsible for the metallic states leading to superconductivity at low temperature. A high-resolution photoemission spectroscopy spectrum near EF of a heavily boron-doped diamond superconductor is also presented.

  17. Visualizing chemical states and defects induced magnetism of graphene oxide by spatially-resolved-X-ray microscopy and spectroscopy.

    Science.gov (United States)

    Wang, Y F; Singh, Shashi B; Limaye, Mukta V; Shao, Y C; Hsieh, S H; Chen, L Y; Hsueh, H C; Wang, H T; Chiou, J W; Yeh, Y C; Chen, C W; Chen, C H; Ray, Sekhar C; Wang, J; Pong, W F; Takagi, Y; Ohigashi, T; Yokoyama, T; Kosugi, N

    2015-10-20

    This investigation studies the various magnetic behaviors of graphene oxide (GO) and reduced graphene oxides (rGOs) and elucidates the relationship between the chemical states that involve defects therein and their magnetic behaviors in GO sheets. Magnetic hysteresis loop reveals that the GO is ferromagnetic whereas photo-thermal moderately reduced graphene oxide (M-rGO) and heavily reduced graphene oxide (H-rGO) gradually become paramagnetic behavior at room temperature. Scanning transmission X-ray microscopy and corresponding X-ray absorption near-edge structure spectroscopy were utilized to investigate thoroughly the variation of the C 2p(π*) states that are bound with oxygen-containing and hydroxyl groups, as well as the C 2p(σ*)-derived states in flat and wrinkle regions to clarify the relationship between the spatially-resolved chemical states and the magnetism of GO, M-rGO and H-rGO. The results of X-ray magnetic circular dichroism further support the finding that C 2p(σ*)-derived states are the main origin of the magnetism of GO. Based on experimental results and first-principles calculations, the variation in magnetic behavior from GO to M-rGO and to H-rGO is interpreted, and the origin of ferromagnetism is identified as the C 2p(σ*)-derived states that involve defects/vacancies rather than the C 2p(π*) states that are bound with oxygen-containing and hydroxyl groups on GO sheets.

  18. Insight into the structure of Pd/ZrO2 during the total oxidation of methane using combined in situ XRD, X.-ray absorption and Raman spectroscopy

    DEFF Research Database (Denmark)

    Grunwaldt, Jan-Dierk; van Vegten, Niels; Baiker, Alfons

    2009-01-01

    The structure of palladium during the total combustion of methane has been studied by a combination of the complementary in situ techniques X-ray absorption spectroscopy, Raman spectroscopy and X-ray diffraction. The study demonstrates that finely dispersed and oxidized palladium is most active...... for the oxidation of methane. Upon heating in the reaction mixture a sudden reduction accompanied by strong sintering of the palladium particles occurs leading to a less active catalyst. Raman spectroscopy combined with XAS shows that palladium is re-oxidized during cooling but is not as finely dispersed as in its...

  19. X-ray absorption spectroscopy on the calcium cofactor to the manganese cluster in photosynthetic oxygen evolution

    Energy Technology Data Exchange (ETDEWEB)

    Cinco, Roehl M. [Univ. of California, Berkeley, CA (United States)

    1999-12-01

    Along with Mn, calcium and chloride ions are necessary cofactors for oxygen evolution in Photosystem II (PS II). To further test and verify whether Ca is close to the Mn cluster, the authors substituted strontium for Ca and probed from the Sr point of view for any nearby Mn. The extended X-ray absorption fine structure (EXAFS) of Sr-reactivated PS II indicates major differences between the intact and NH2OH-treated samples. In intact samples, the Fourier transform of the Sr EXAFS shows a Fourier peak that is missing in inactive samples. This peak II is best simulated by two Mn neighbors at a distance of 3.5 Angstrom, confirming the proximity of Ca (Sr) cofactor to the Mn cluster. In addition, polarized Sr EXAFS on oriented Sr-reactivated samples shows this peak II is dichroic: large magnitude at 10 degrees (angle between the PS II membrane normal and the x-ray electric field vector) and small at 80 degrees. Analysis of the dichroism yields the relative angle between the Sr-Mn vector and membrane normal (23 degrees ± 4 degrees), and the isotropic coordination number for these layered samples. X-ray absorption spectroscopy has also been employed to assess the degree of similarity between the manganese cluster in PS II and a family of synthetic manganese complexes containing the distorted cubane [Mn4O3X] core (X = benzoate, acetate, methoxide, hydroxide, azide, fluoride, chloride or bromide). In addition, Mn4O3Cl complexes containing three or six terminal Cl ligands at three of the Mn were included in this study. The EXAFS method detects the small changes in the core structures as X is varied in this series, and serves to exclude these distorted cubanes of C3v symmetry as a topological model for the Mn catalytic cluster. The sulfur K-edge x-ray absorption near-edge structure (XANES) spectra for the amino acids cysteine, methionine, their corresponding oxidized forms cystine and methionine sulfoxide, and

  20. Testing the theory of colliding winds: the periastron passage of 9 Sagittarii. I. X-ray and optical spectroscopy

    Science.gov (United States)

    Rauw, G.; Blomme, R.; Nazé, Y.; Spano, M.; Mahy, L.; Gosset, E.; Volpi, D.; van Winckel, H.; Raskin, G.; Waelkens, C.

    2016-05-01

    Context. The long-period, highly eccentric O-star binary 9 Sgr, known for its non-thermal radio emission and its relatively bright X-ray emission, went through its periastron in 2013. Aims: Such an event can be used to observationally test the predictions of the theory of colliding stellar winds over a broad range of wavelengths. Methods: We conducted a multi-wavelength monitoring campaign of 9 Sgr around the 2013 periastron. In this paper, we focus on X-ray observations and optical spectroscopy. Results: The optical spectra allow us to revisit the orbital solution of 9 Sgr and to refine its orbital period to 9.1 years. The X-ray flux is maximum at periastron over all energy bands, but with clear differences as a function of energy. The largest variations are observed at energies above 2 keV, whilst the spectrum in the soft band (0.5-1.0 keV) remains mostly unchanged, indicating that it arises far from the collision region, in the inner winds of the individual components. The level of the hard emission at periastron clearly deviates from the 1 /r relation expected for an adiabatic wind-interaction zone, whilst this relation seems to hold at the other phases that are covered by our observations. The spectra taken at phase 0.946 reveal a clear Fe xxv line at 6.7 keV, but no such line is detected at periastron (φ = 0.000), although a simple model predicts a strong line that should be easily visible in the data. Conclusions: The peculiarities of the X-ray spectrum of 9 Sgr could reflect the effect of radiative inhibition as well as a phase-dependent efficiency of particle acceleration on the shock properties. Based on observations with XMM-Newton, an ESA Science Mission with instruments and contributions directly funded by ESA Member states and the USA (NASA). Also based on observations collected at the European Southern Observatory (La Silla, Chile) and with the Mercator Telescope operated on the island of La Palma by the Flemish Community, at the Spanish

  1. NuSTAR SPECTROSCOPY OF MULTI-COMPONENT X-RAY REFLECTION FROM NGC 1068

    Energy Technology Data Exchange (ETDEWEB)

    Bauer, Franz E. [Pontificia Universidad Católica de Chile, Instituto de Astrofísica, Casilla 306, Santiago 22 (Chile); Arévalo, Patricia [EMBIGGEN Anillo, Concepción (Chile); Walton, Dominic J.; Baloković, Mislav; Brightman, Murray; Harrison, Fiona A. [Cahill Center for Astronomy and Astrophysics, California Institute of Technology, Pasadena, CA 91125 (United States); Koss, Michael J. [Institute for Astronomy, Department of Physics, ETH Zurich, Wolfgang-Pauli-Strasse 27, CH-8093 Zurich (Switzerland); Puccetti, Simonetta [ASDC-ASI, Via del Politecnico, I-00133 Roma (Italy); Gandhi, Poshak [School of Physics and Astronomy, University of Southampton, Highfield, Southampton SO17 1BJ (United Kingdom); Stern, Daniel [Jet Propulsion Laboratory, California Institute of Technology, 4800 Oak Grove Drive, Pasadena, CA 91109 (United States); Alexander, David M.; Moro, Agnese Del [Department of Physics, Durham University, South Road, Durham, DH1 3LE (United Kingdom); Boggs, Steve E.; Craig, William W. [Space Sciences Laboratory, University of California, Berkeley, CA 94720 (United States); Brandt, William N.; Luo, Bin [Department of Astronomy and Astrophysics, The Pennsylvania State University, 525 Davey Lab, University Park, PA 16802 (United States); Christensen, Finn E. [DTU Space, National Space Institute, Technical University of Denmark, Elektrovej 327, DK-2800 Lyngby (Denmark); Comastri, Andrea [INAF-Osservatorio Astronomico di Bologna, via Ranzani 1, I-40127 Bologna (Italy); Hailey, Charles J. [Columbia Astrophysics Laboratory, Columbia University, New York, NY 10027 (United States); Hickox, Ryan [Department of Physics and Astronomy, Dartmouth College, 6127 Wilder Laboratory, Hanover, NH 03755 (United States); and others

    2015-10-20

    We report on high-energy X-ray observations of the Compton-thick Seyfert 2 galaxy NGC 1068 with NuSTAR, which provide the best constraints to date on its >10 keV spectral shape. The NuSTAR data are consistent with those from past and current instruments to within cross-calibration uncertainties, and we find no strong continuum or line variability over the past two decades, which is in line with its X-ray classification as a reflection-dominated Compton-thick active galactic nucleus. The combined NuSTAR, Chandra, XMM-Newton, and Swift BAT spectral data set offers new insights into the complex secondary emission seen instead of the completely obscured transmitted nuclear continuum. The critical combination of the high signal-to-noise NuSTAR data and the decomposition of the nuclear and extranuclear emission with Chandra allow us to break several model degeneracies and greatly aid physical interpretation. When modeled as a monolithic (i.e., a single N{sub H}) reflector, none of the common Compton reflection models are able to match the neutral fluorescence lines and broad spectral shape of the Compton reflection hump without requiring unrealistic physical parameters (e.g., large Fe overabundances, inconsistent viewing angles, or poor fits to the spatially resolved spectra). A multi-component reflector with three distinct column densities (e.g., with best-fit values of N{sub H} of 1.4 × 10{sup 23}, 5.0 × 10{sup 24}, and 10{sup 25} cm{sup −2}) provides a more reasonable fit to the spectral lines and Compton hump, with near-solar Fe abundances. In this model, the higher N{sub H} component provides the bulk of the flux to the Compton hump, while the lower N{sub H} component produces much of the line emission, effectively decoupling two key features of Compton reflection. We find that ≈30% of the neutral Fe Kα line flux arises from >2″ (≈140 pc) and is clearly extended, implying that a significant fraction (and perhaps most) of the <10 keV reflected component

  2. Fabrication of blazed gratings for X-ray spectroscopy using substrate conformal imprint lithography

    Science.gov (United States)

    McCoy, Jake; Verschuuren, Marc; Lopez, Gerald; Zhang, Ningxiao; McEntaffer, Randall

    2017-08-01

    The majority of spectral lines relevant in high energy astrophysics exist at soft X-ray energies, where gratings dominate over microcalorimeters. Next-generation reflection gratings have been identified as a key technology to improve the spectroscopic capabilities of future X-ray observatories. Currently, the grating fabrication process centers on the production of a large-area (72 cm2) master template through techniques in electron-beam lithography, plasma etching and anisotropic wet etching in single-crystal Si. Then, many replicas are produced to populate a grating array, which intercepts and disperses the radiation coming to a focus in a Wolter-I telescope. Of importance is implenting a replication procedure that preserves the fidelity of the master grating template at a low cost. Traditionally, the Si master template has been used to stamp directly into a UV-curable resist coated on a fused silica substrate through the process of nanoimprint lithography (UV-NIL). Though the high stiffness of Si allows the desired inverse of the original pattern to be imprinted with high resolution, difficulties arise especially when imprinting over a large area. Substrate conformal imprint lithography (SCIL) is a relatively new commercial process intended to evade these problems. In contrast to UV-NIL, the SCIL process uses a flexible stamp formed from the master template for imprinting. The flexible stamp carries the inverse of the original pattern in a modified silicone rubber, which has increased stiffness compared to standard silicone used in soft lithography processes. This enables the positive of original pattern to be imprinted sequentially with high resolution while confroming to the bow of the substrate and reducing damage due to particulate contaminants. The desired inverse of the original pattern can be imprinted with SCIL by forming a second flexible stamp from the initial flexible stamp. Further, SCIL is compatible with an inorganic imprint resist that has been

  3. Molecular and supramolecular properties of nitroaromatic thiosemicarbazones: Synthesis, spectroscopy, X-ray structure elucidation and DFT calculations

    Science.gov (United States)

    Dias, L. C.; de Lima, G. M.; Pinheiro, C. B.; Nascimento, M. A. C.; Bitzer, R. S.

    2017-03-01

    The reactions of 6-nitropiperonal with H2Nsbnd NHsbnd C(S)sbnd NHR, R = Me, Et, Ph or H, afforded four nitroaromatic thiosemicarbazones 1-4, respectively. 1-4 were characterized by elemental analysis (CHN), FTIR, and 1H and 13C{1H} NMR spectroscopy. In addition, the crystal structures of 2 and 3 were determined by single-crystal X-ray diffraction. Our X-ray structural results have shown that the nitropiperonal and thiosemicarbazone moieties exhibit an almost coplanar arrangement for both 2 and 3. Moreover, they establish 2-D networks along the [111] base vector by means of classical and nonclassical hydrogen bonds. Electronic and spectroscopic properties of 1-4 were investigated at the DFT B3LYP/6-311G** level of calculation. The Cdbnd S group of 1-4 constitutes a nucleophilic region, whereas the NO2 group defines an electrophilic centre, as expected. Furthermore, a DFT vibrational analysis of 4 allowed a reliable assignment of the thiosemicarbazone-based vibrations. Also, a good agreement between theoretical and experimental 13C chemical shift values was obtained for 1-4.

  4. X-ray magnetic circular dichroism and reflection anisotropy spectroscopy Kerr effect studies of capped magnetic nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Cunniffe, J. P.; McNally, D.E.; Liberati, M.; Arenholz, E.; McGuinness, C.; McGilp, J. F.

    2010-03-02

    Aligned Co wires grown on Pt(997) under ultra-high vacuum conditions have been capped successfully by the epitaxial growth of Au monolayers (ML) at room temperature. The samples were kept under vacuum except when transferring between apparatus or when making some of the measurements. No degradation of the Co wires was detected during the measurements. The magneto-optic response of the system was measured using X-ray magnetic circular dichroism (XMCD) at the Co L{sub 2,3} edge and reflection anisotropy spectroscopy (RAS) at near normal incidence, which is sensitive to the normal component of the out-of-plane magnetization via the Kerr effect (MOKE). Capping the wires significantly impacts their magnetic properties. Comparison of the magneto-optic response of the system at X-ray and optical energies reveals small differences that are attributed to the induced moment in the Pt substrate and Au capping layer not picked up by the element specific XMCD measurements. The sensitivity of RAS-MOKE is sufficient to allow the determination of the easy axis direction of the capped wires to within a few degrees. The results for a 6-atom-wide Co wire sample, capped with 6 ML of Au, are consistent with the capped wires possessing perpendicular magnetization.

  5. Observation and modeling of interspecies ion separation in inertial confinement fusion implosions via imaging x-ray spectroscopy

    Science.gov (United States)

    Joshi, T. R.; Hakel, P.; Hsu, S. C.; Vold, E. L.; Schmitt, M. J.; Hoffman, N. M.; Rauenzahn, R. M.; Kagan, G.; Tang, X.-Z.; Mancini, R. C.; Kim, Y.; Herrmann, H. W.

    2017-05-01

    We report the first direct experimental evidence of interspecies ion separation in direct-drive inertial confinement fusion experiments performed at the OMEGA laser facility via spectrally, temporally, and spatially resolved imaging x-ray-spectroscopy data [S. C. Hsu et al., Europhys. Lett. 115, 65001 (2016)]. These experiments were designed based on the expectation that interspecies ion thermo-diffusion would be the strongest for species with a large mass and charge difference. The targets were spherical plastic shells filled with D2 and a trace amount of Ar (0.1% or 1% by atom). Ar K-shell spectral features were observed primarily between the time of first-shock convergence and slightly before the neutron bang time, using a time- and space-integrated spectrometer, a streaked crystal spectrometer, and two gated multi-monochromatic x-ray imagers fielded along quasi-orthogonal lines of sight. Detailed spectroscopic analyses of spatially resolved Ar K-shell lines reveal the deviation from the initial 1% Ar gas fill and show both Ar-concentration enhancement and depletion at different times and radial positions of the implosion. The experimental results are interpreted using radiation-hydrodynamic simulations that include recently implemented, first-principles models of interspecies ion diffusion. The experimentally inferred Ar-atom fraction profiles agree reasonably with calculated profiles associated with the incoming and rebounding first shock.

  6. X-Ray Spectroscopy, The Ellen Richards Prize, and Nuclear Proliferation: The Inspiring Life of Katherine Chamberlain

    Science.gov (United States)

    Geramita, Matthew

    2008-04-01

    In 1924, Katherine Chamberlain became the first woman to receive a doctorate in physics from the University of Michigan. As one of the first women in the world to earn a doctorate in physics, Katherine reached a level prominence in the scientific community that few women had achieved. As a scientist, Katherine studied the outer energy levels of various elements using x-ray spectroscopy at the University of Michigan. In her thesis, she showed the potential for x-rays to reduce highly oxidized compounds and in 1925 won the Ellen Richards Prize for the world's best scientific paper by a woman. As an educator, she taught an introduction to photography course for thirty-five years in the hopes of creating new ways to inspire a love for physics in her students. As a community leader, she worked with The United World Federalists and The Michigan Memorial Phoenix Project to find peaceful uses for nuclear energy. Looking at these aspects of Chamberlain's life offers a unique perspective on the physics community of the 1920's, physics education, and the nuclear panic that followed WWII.

  7. Optical design of the Short Pulse Soft X-ray Spectroscopy beamline at the Advanced Photon Source.

    Science.gov (United States)

    Reininger, R; Keavney, D J; Borland, M; Young, L

    2013-07-01

    The Short Pulse X-ray facility planned for the Advanced Photon Source (APS) upgrade will provide two sectors with photon beams having picosecond pulse duration. The Short Pulse Soft X-ray Spectroscopy (SPSXS) beamline will cover the 150-2000 eV energy range using an APS bending magnet. SPSXS is designed to take full advantage of this new timing capability in addition to providing circular polarized radiation. Since the correlation between time and electron momentum is in the vertical plane, the monochromator disperses in the horizontal plane. The beamline is designed to maximize flux and preserve the time resolution by minimizing the number of optical components. The optical design allows the pulse duration to be varied from 1.5 to 100 ps full width at half-maximum (FWHM) without affecting the energy resolution, and the resolution to be changed with minimal effect on the pulse duration. More than 10(9) photons s(-1) will reach the sample with a resolving power of 2000 and a pulse duration of ∼2 ps for photon energies between 150 and 1750 eV. The spot size expected at the sample position will vary with pulse duration and exit slit opening. At 900 eV and at a resolving power of 2000 the spot will be ∼10 µm × 10 µm with a pulse duration of 2.3 ps FWHM.

  8. Energy gaps, electronic structures, and x-ray spectroscopies of finite semiconductor single-walled carbon nanotubes.

    Science.gov (United States)

    Gao, Bin; Jiang, Jun; Wu, ZiYu; Luo, Yi

    2008-02-28

    We report hybrid density functional theory calculations for electronic structures of hydrogen-terminated finite single-walled carbon nanotubes (6,5) and (8,3) up to 100 nm in length. Gap states that are mainly arisen from the hydrogen-terminated edges have been found in (8,3) tubes, but their contributions to the density of states become invisible when the tube is longer than 10 nm. The electronic structures of (6,5) and (8,3) tubes are found to be converged around 20 nm. The calculated band-gap energies of 100 nm long nanotubes are in good agreement with experimental results. The valence band structures of (6,5), (8,3), as well as (5,5) tubes are also investigated by means of ultraviolet photoelectron spectra (UPS), x-ray emission spectroscopy (XES), and the resonant inelastic x-ray scattering (RIXS) spectra theoretically. The UPS, XES and RIXS spectra become converged already at 10 nm. The length-dependent oscillation behavior is found in the RIXS spectra of (5,5) tubes, indicating that the RIXS spectra may be used to determine the size and length of metallic nanotubes. Furthermore, the chiral dependence observed in the simulated RIXS spectra suggests that RIXS spectra could be a useful technique for the determination of chirality of carbon nanotubes.

  9. Super-Eddington accretion on to the neutron star NGC 7793 P13: Broad-band X-ray spectroscopy and ultraluminous X-ray sources

    Science.gov (United States)

    Walton, D. J.; Fürst, F.; Harrison, F. A.; Stern, D.; Bachetti, M.; Barret, D.; Brightman, M.; Fabian, A. C.; Middleton, M. J.; Ptak, A.; Tao, L.

    2018-02-01

    We present a detailed, broad-band X-ray spectral analysis of the ultraluminous X-ray source (ULX) pulsar NGC 7793 P13, a known super-Eddington source, utilizing data from the XMM-Newton, NuSTAR and Chandra observatories. The broad-band XMM-Newton+NuSTAR spectrum of P13 is qualitatively similar to the rest of the ULX sample with broad-band coverage, suggesting that additional ULXs in the known population may host neutron star accretors. Through time-averaged, phase-resolved and multi-epoch studies, we find that two non-pulsed thermal blackbody components with temperatures ∼0.5 and 1.5 keV are required to fit the data below 10 keV, in addition to a third continuum component which extends to higher energies and is associated with the pulsed emission from the accretion column. The characteristic radii of the thermal components appear to be comparable, and are too large to be associated with the neutron star itself, so the need for two components likely indicates the accretion flow outside the magnetosphere is complex. We suggest a scenario in which the thick inner disc expected for super-Eddington accretion begins to form, but is terminated by the neutron star's magnetic field soon after its onset, implying a limit of B ≲ 6 × 1012 G for the dipolar component of the central neutron star's magnetic field. Evidence of similar termination of the disc in other sources may offer a further means of identifying additional neutron star ULXs. Finally, we examine the spectrum exhibited by P13 during one of its unusual 'off' states. These data require both a hard power-law component, suggesting residual accretion on to the neutron star, and emission from a thermal plasma, which we argue is likely associated with the P13 system.

  10. X-ray and vibrational spectroscopy of manganese complexes relevant to the oxygen-evolving complex of photosynthesis

    Energy Technology Data Exchange (ETDEWEB)

    Visser, Hendrik [Univ. of California, Berkeley, CA (United States)

    2001-01-01

    Manganese model complexes, relevant to the oxygen-evolving complex (OEC) in photosynthesis, were studied with Mn K-edge X-ray absorption near-edge spectroscopy (XANES), Mn Kb X-ray emission spectroscopy (XES), and vibrational spectroscopy. A more detailed understanding was obtained of the influence of nuclearity, overall structure, oxidation state, and ligand environment of the Mn atoms on the spectra from these methods. This refined understanding is necessary for improving the interpretation of spectra of the OEC. Mn XANES and Kb XES were used to study a di-(mu)-oxo and a mono-(mu)-oxo di-nuclear Mn compound in the (III,III), (III,IV), and (IV,IV) oxidation states. XANES spectra show energy shifts of 0.8 - 2.2 eV for 1-electron oxidation-state changes and 0.4 - 1.8 eV for ligand-environment changes. The shifts observed for Mn XES spectra were approximately 0.21 eV for oxidation state-changes and only approximately 0.04 eV for ligand-environment changes. This indicates that Mn Kb XES i s more sensitive to the oxidation state and less sensitive to the ligand environment of the Mn atoms than XANES. These complimentary methods provide information about the oxidation state and the ligand environment of Mn atoms in model compounds and biological systems. A versatile spectroelectrochemical apparatus was designed to aid the interpretation of IR spectra of Mn compounds in different oxidation states. The design, based on an attenuated total reflection device, permits the study of a wide spectral range: 16,700 (600 nm) - 225

  11. X-ray and extreme ultraviolet spectroscopy on DIII-D

    Science.gov (United States)

    Victor, B. S.; Allen, S. L.; Beiersdorfer, P.; Magee, E. W.

    2017-06-01

    Two spectrometers were installed to measure tungsten emission in the core of DIII-D plasmas during a metal rings experimental campaign. The spectral range of the high-resolution (1340 spectral channels), variable-ruled grating X-ray and Extreme Ultraviolet Spectrometer (XEUS) extends from 10-71 dot A. The spectral range of the second spectrometer, the Long-Wavelength Extreme Ultraviolet Spectrometer (LoWEUS), measures between 31-174 dot A. Three groups of tungsten lines were identified with XEUS: W38+-W45+ from 47-63 dot A, W27+-W35+ from 45-55 dot A, and W28+-W33+ from 16-30 dot A. Emission lines from tungsten charge states W28+, W43+, W44+, and W45+ are identified and the line amplitude is presented versus time. Peak emission of W43+-W45+ occurs between core Te=2.5-3 keV, and peak emission of W28+ occurs at core Tetrack the sawtooth cycle. Sensitivity to the sawtooth cycle and the correlation of the peak emission with core electron temperature show that these spectrometers track the on-axis tungsten emission of DIII-D plasmas.

  12. Orientation of One-Dimensional Silicon Polymer Films Studied by X-Ray Absorption Spectroscopy

    Directory of Open Access Journals (Sweden)

    Md. Abdul Mannan

    2012-01-01

    Full Text Available Molecular orientations for thin films of one-dimensional silicon polymers grown by vacuum evaporation have been assigned by near-edge X-ray absorption fine structure (NEXAFS using linearly polarized synchrotron radiation. The polymer investigated was polydimethylsilane (PDMS which is the simplest stable silicon polymer, and one of the candidate materials for one-dimensional molecular wire. For PDMS films deposited on highly oriented pyrolytic graphite (HOPG, four resonance peaks have been identified in the Si K-edge NEXAFS spectra. Among these peaks, the intensities of the two peaks lower-energy at 1842.0 eV and 1843.2 eV were found to be strongly polarization dependent. The peaks are assigned to the resonance excitations from the Si 1s to σ∗ pyz and σ∗ px orbitals localized at the Si–C and Si–Si bonds, respectively. Quantitative evaluation of the polarization dependence of the NEXAFS spectra revealed that the molecules are self-assembled on HOPG surface, and the backbones of the PDMS are oriented nearly parallel to the surface. The observed orientation is opposite to the previously observed results for PDMS on the other surfaces such as oxide (indium tin oxide and metal (polycrystalline copper. The flat-lying feature of PDMS observed only on HOPG surface is attributed to the interaction between CH bonds in PDMS and π orbitals in HOPG surface.

  13. Iron near absorption edge X-ray spectroscopy at aqueous-membrane interfaces

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Wenjie; Kuzmenko, Ivan; Vaknin, David

    2014-01-01

    Employing synchrotron X-ray scattering, we systematically determine the absorption near-edge spectra (XANES) of iron in its ferrous (Fe2+) and ferric (Fe3+) states both as ions in aqueous solutions and as they bind to form a single layer to anionic templates that consist of carboxyl or phosphate groups at aqueous/vapor interfaces. While the XANES of bulk iron ions show that the electronic state and coordination of iron complexes in the bulk are isotropic, the interfacial bound ions show a signature of a broken inversion-symmetry environment. The XANES of Fe2+ and Fe3+ in the bulk possess distinct profiles however, upon binding they practically exhibit similar patterns. This indicates that both bound ions settle into a stable electronic and coordination configuration with an effective fractional valence (for example, Fe[2+nu]+, 0 < nu < 1) at charged organic templates. Such two dimensional properties may render interfacial iron, abundant in living organisms, a more efficient and versatile catalytic behavior.

  14. Iron near absorption edge X-ray spectroscopy at aqueous-membrane interfaces.

    Science.gov (United States)

    Wang, Wenjie; Kuzmenko, Ivan; Vaknin, David

    2014-07-14

    Employing synchrotron X-ray scattering, we systematically determine the absorption near-edge spectra (XANES) of iron in its ferrous (Fe(2+)) and ferric (Fe(3+)) states both as ions in aqueous solutions and as they bind to form a single layer to anionic templates that consist of carboxyl or phosphate groups at aqueous/vapor interfaces. While the XANES of bulk iron ions show that the electronic state and coordination of iron complexes in the bulk are isotropic, the interfacial bound ions show a signature of a broken inversion-symmetry environment. The XANES of Fe(2+) and Fe(3+) in the bulk possess distinct profiles however, upon binding they practically exhibit similar patterns. This indicates that both bound ions settle into a stable electronic and coordination configuration with an effective fractional valence (for example, Fe([2+ν]+), 0 < ν < 1) at charged organic templates. Such two dimensional properties may render interfacial iron, abundant in living organisms, a more efficient and versatile catalytic behavior.

  15. X-ray spectroscopy of nitrile hydratase at pH 7 and 9

    Energy Technology Data Exchange (ETDEWEB)

    Scarrow, R.C.; Duong, D.J.; Kindt, J.T. [Haverford College, PA (United States)] [and others

    1996-08-06

    The iron K-edge X-ray absorption spectrum of Rhodococcus sp. R312 (formerly Brevibacterium sp. R312) nitrile hydratase in frozen solutions at pH 7 and 9 has been analyzed to determine details of the iron coordination. EXAFS analysis implies two or three sulfur ligands per iron and overall six coordination; together with previous EPR and ENDOR results, this implies an N{sub 3}S{sub 2}O ligation sphere. The bond lengths from EXAFS analysis [r{sub av}(Fe-S) = 2.21 {angstrom} at pH 7.3; r{sub av}(Fe-N/O) = 1.99 {angstrom}] support cis coordination of two cysteine ligands and conclusively rule out nitric oxide coordination to the iron, a possibility proposed on the basis of an FTIR difference experiment. The higher-frequency EXAFS can be simulated well by inclusion of multiple scattering from two or three imidazole ligands; the fit to the data is improved if first-sphere multiple scattering pathways are also included. A slight shortening (by 0.02 {plus_minus} 0.01 {angstrom}) of one or both Fe-S bonds when the pH is raised from 7.3 to 9.0 is consistent with shifts observed in the Raman spectrum. 67 refs., 4 figs., 4 tabs.

  16. Oxidation mechanism of chalcopyrite revealed by X-ray photoelectron spectroscopy and first principles studies

    Science.gov (United States)

    Xiong, Xiaolu; Hua, Xiaoming; Zheng, Yongfei; Lu, Xionggang; Li, Shenggang; Cheng, Hongwei; Xu, Qian

    2018-01-01

    X-ray photoelectron spectroscopic (XPS) studies revealed that the iron site on the chalcopyrite (CuFeS2) surface was preferably oxidized to the Cu site when exposed to an oxidizing environment. Extensive density functional theory calculations were performed to investigate the surface structure of chalcopyrite and its reaction with both molecular oxygen (O2) and water. The adsorption and dissociation of a single O2 molecule, a single H2O molecule, as well as both molecules at the Fe and Cu sites on the CuFeS2 (001) surface were studied. Consistent with our experimental observation, the Fe site was found to be preferred for the adsorption and dissociation of O2 due to its lower energy barrier and greater exothermicity. The dissociation of H2O on the CuFeS2 (001) surface by itself was found to be unfavorable both thermodynamically and kinetically. However, the surface formed upon O2 dissociation was predicted to be much more reactive with H2O, which was attributed to favorable hydrogen transfer to the O site formed upon O2 dissociation to hydrogen transfer to the S site due to the much weaker Ssbnd H bond than the Osbnd H bond.

  17. Double resonance capacitance spectroscopy (DORCAS): A new experimental technique for assignment of X-ray absorption peaks to surface sites of semiconductor

    CERN Document Server

    Ishii, M

    2003-01-01

    As a new microspectroscopy for semiconductor surface analysis using an X-ray beam, double resonance capacitance spectroscopy (DORCAS) is proposed. For a microscopic X-ray absorption measurement, a local capacitance change owing to X-ray induced emission of localized electrons is detected by a microprobe. The applied bias voltage V sub b dependence of the capacitance also provides information on the surface density of state. The resonance of the Fermi energy with a surface level by V sub b control makes possible the selection of the observable surface site in the X-ray absorption measurements, i.e. site-specific spectroscopy. The double resonance of the surface site selection (V sub b resonance) and the resonant X-ray absorption of the selected site (photon energy h nu resonance) enhances the capacitance signal. The DORCAS measurement of the GaAs surface shows correlation peaks at h nu=10.402 keV and V sub b =-0.4 V and h nu=10.429 keV and V sub b =+0.1 V, indicating that these resonant X-ray absorption peaks ...

  18. Structural studies of advanced functional materials by synchrotron-based x-ray absorption spectroscopy: BL5.2 at SLRI, Thailand

    Science.gov (United States)

    Kidkhunthod, Pinit

    2017-09-01

    This paper highlights the use of the x-ray absorption spectroscopy (XAS) as a local structural tool unlike x-ray diffraction for selected atoms in advanced functional materials including energy storage materials, dielectric materials and thermoelectric materials. The information concerning the oxidation states and local atomic structure around probing atoms will be revealed using x-ray absorption near edge structure (XANES) and extended x-ray absorption fine structure (EXAFS). The XAS beamline: BL5.2 at the Synchrotron Light Research Institute (SLRI) (public organization), Thailand, and its characteristic including available of measured energy ranges, examples of measured spectra of Mg, S and Ti K-edge XAS are also presented. In addition, in situ XAS set up and experiment carried out at this beamline are also outlined. Invited talk at 5th Thailand International Nanotechnology Conference (Nano Thailand-2016), 27-29 November 2016, Nakhon Ratchasima, Thailand.

  19. A study of the Nb sub 3 Ge system by Ge K-edge extended x-ray absorption fine structure and x-ray absorption near-edge structure spectroscopy

    CERN Document Server

    Saini, N L; Wu Zi Yu; Oyanagi, H; Ihara, H; Iyo, A; Agrestini, S; Bianconi, A

    2002-01-01

    The local structure of Nb sub 3 Ge intermetallic superconductor has been studied by Ge K-edge absorption spectroscopy. Extended x-ray absorption fine structure (EXAFS) experiments show two Ge-Nb distances. In addition to the crystallographic distance of approx 2.87 A, there exists a second Ge-Nb distance, shorter than the first by approx 0.2 A, assigned to a phase with short-range symmetry related to local displacements in the Nb-Nb chains. The x-ray absorption near-edge structure (XANES) spectrum has been simulated by full multiple-scattering calculations considering the local displacements determined by the EXAFS analysis. The XANES spectrum has been well reproduced by considering a cluster of 99 atoms within a radius of about 7 A from the central Ge atom and introducing determined local displacements.

  20. Soft x-ray reflectometry, hard x-ray photoelectron spectroscopy and transmission electron microscopy investigations of the internal structure of TiO2(Ti/SiO2/Si stacks

    Directory of Open Access Journals (Sweden)

    Elena O Filatova, Igor V Kozhevnikov, Andrey A Sokolov, Evgeniy V Ubyivovk, Sergey Yulin, Mihaela Gorgoi and Franz Schäfers

    2012-01-01

    Full Text Available We developed a mathematical analysis method of reflectometry data and used it to characterize the internal structure of TiO2/SiO2/Si and Ti/SiO2/Si stacks. Atomic concentration profiles of all the chemical elements composing the samples were reconstructed from the analysis of the reflectivity curves measured versus the incidence angle at different soft x-ray reflection (SXR photon energies. The results were confirmed by the conventional techniques of hard x-ray photoelectron spectroscopy (HXPES and high-resolution transmission electron microscopy (HRTEM. The depth variation of the chemical composition, thicknesses and densities of individual layers extracted from SXR and HXPES measurements are in close agreement and correlate well with the HRTEM images.

  1. Following a Chemical Reaction on the Millisecond Time Scale by Simultaneous X-ray and UV/Vis Spectroscopy.

    Science.gov (United States)

    Olivo, Giorgio; Barbieri, Alessia; Dantignana, Valeria; Sessa, Francesco; Migliorati, Valentina; Monte, Manuel; Pascarelli, Sakura; Narayanan, Theyencheri; Lanzalunga, Osvaldo; Di Stefano, Stefano; D'Angelo, Paola

    2017-07-06

    An innovative approach aimed at disclosing the mechanism of chemical reactions occurring in solution on the millisecond time scale is presented. Time-resolved energy dispersive X-ray absorption and UV/vis spectroscopies with millisecond resolution are used simultaneously to directly follow the evolution of both the oxidation state and the local structure of the metal center in an iron complex. Two redox reactions are studied, the former involving the transformation of FeII into two subsequent FeIII species and the latter involving the more complex FeII-FeIII-FeIV-FeIII sequence. The structural modifications occurring around the iron center are correlated to the reaction mechanisms. This combined approach has the potential to provide unique insights into reaction mechanisms in the liquid phase and represents a new powerful tool to characterize short-lived intermediates that are silent to common spectroscopic techniques.

  2. X-ray photoelectron spectroscopy of trihalide ionic liquids: Comparison to halide-based analogues, anion basicity and beam damage

    Science.gov (United States)

    Men, Shuang; Lovelock, Kevin R. J.; Licence, Peter

    2017-07-01

    X-ray photoelectron spectroscopy is used to investigate two 1-octyl-3-methylimidazolium trihalide ionic liquids, with anions including triiodide and iododibromide. The electronic environment of each element present in ionic liquids studied herein is analysed and compared to their halide-based analogous. The anion basicity is compared based upon the measured N 1s binding energy. The iododibromide ionic liquid is studied as a representative sample to illustrate the beam damage effect. Due to the beam damage, there is a new formed bromine component observed. This effect is calculated and demonstrated for all elements present within the ionic liquid. It suggests that the beam induced decomposition caused a stoichiometric loss of bromine atom and iodine atom.

  3. Observation of Interspecies Ion Separation in Inertial-Confinement-Fusion Implosions via Imaging X-Ray Spectroscopy

    CERN Document Server

    Hsu, S C; Hakel, P; Vold, E L; Schmitt, M J; Hoffman, N M; Rauenzahn, R M; Kagan, G; Tang, X -Z; Mancini, R C; Kim, Y; Herrmann, H W

    2016-01-01

    We report direct experimental evidence of interspecies ion separation in direct-drive, inertial-confinement-fusion experiments on the OMEGA laser facility. These experiments, which used plastic capsules with D$_2$/Ar gas fill (1% Ar by atom), were designed specifically to reveal interspecies ion separation by exploiting the predicted, strong ion thermo-diffusion between ion species of large mass and charge difference. Via detailed analyses of imaging x-ray-spectroscopy data, we extract Ar-atom-fraction radial profiles at different times, and observe both enhancement and depletion compared to the initial 1%-Ar gas fill. The experimental results are interpreted with radiation-hydrodynamic simulations that include recently implemented, first-principles models of interspecies ion diffusion. The experimentally inferred Ar-atom-fraction profiles agree reasonably, but not exactly, with calculated profiles associated with the incoming and rebounding first shock.

  4. Modeling the Structure and Composition of Nanoparticles by Extended X-Ray Absorption Fine-Structure Spectroscopy

    Science.gov (United States)

    Frenkel, Anatoly I.; Yevick, Aaron; Cooper, Chana; Vasic, Relja

    2011-07-01

    Many metal clusters in the 1-nm size range are catalytically active, and their enhanced reactivity is often attributed to their size, structure, morphology, and details of alloying. Synchrotron sources provide a wide range of opportunities for studying catalysis. Among them, extended X-ray absorption fine-structure (EXAFS) spectroscopy is the premier method for investigating structure and composition of nanocatalysts. In this review, we summarize common methods of EXAFS analysis for geometric and compositional characterization of nanoparticles. We discuss several aspects of the experiments and analyses that are critical for reliably modeling EXAFS data. The most important are sample homogeneity, the width of the size and compositional distribution functions, and accounting for multiple-scattering contributions to EXAFS. We focus on the contribution of structural disorder and structural/compositional heterogeneity to the accuracy of three-dimensional modeling.

  5. Combined use of atomic force microscopy, X-ray photoelectron spectroscopy, and secondary ion mass spectrometry for cell surface analysis.

    Science.gov (United States)

    Dague, Etienne; Delcorte, Arnaud; Latgé, Jean-Paul; Dufrêne, Yves F

    2008-04-01

    Understanding the surface properties of microbial cells is a major challenge of current microbiological research and a key to efficiently exploit them in biotechnology. Here, we used three advanced surface analysis techniques with different sensitivity, probing depth, and lateral resolution, that is, in situ atomic force microscopy, X-ray photoelectron spectroscopy, and secondary ion mass spectrometry, to gain insight into the surface properties of the conidia of the human fungal pathogen Aspergillus fumigatus. We show that the native ultrastructure, surface protein and polysaccharide concentrations, and amino acid composition of three mutants affected in hydrophobin production are markedly different from those of the wild-type, thereby providing novel insight into the cell wall architecture of A. fumigatus. The results demonstrate the power of using multiple complementary techniques for probing microbial cell surfaces.

  6. Nanostructure Size Determination in N+-Type Porous Silicon by X-Ray diffractometry and Raman Spectroscopy

    CERN Document Server

    Ramirez-Porras, A

    1997-01-01

    A series of porous silicon surfaces were obtained after different exposition times of electrochemical etching on cristalline n+- type silicon in presence of hydrofluoric acid. These kind of surfaces show photoluminescence when illuminated by UV light. One possible explanation for this is that the treated surface is made up of small crystallites the nanometer scale that split away the semiconductor band edges up to optical photon energies for the band- to -band recombination processes. In this study, a nanometer size determination of such proposed structures was performed by the use of X-Ray Diffractometry and Raman Spectroscopy. The result suggest the consistency between the so called Quantum Confined Model and the experimental results. (Author)

  7. Structure determination of a multilayer with an island-like overlayer using hard x-ray photoelectron spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Isomura, N., E-mail: isomura@mosk.tytlabs.co.jp; Kataoka, K.; Horibuchi, K.; Dohmae, K.; Kitazumi, K.; Takahashi, N.; Kimoto, Y. [Toyota Central R& D Laboratories, Inc., 41-1 Yokomichi, Nagakute, Aichi 480-1192 (Japan); Oji, H.; Cui, Y.-T.; Son, J.-Y. [Japan Synchrotron Radiation Research Institute (JASRI), 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan)

    2016-07-27

    We use hard X-ray photoelectron spectroscopy (HAXPES) to obtain the surface structure of a multilayer Au/SiO{sub 2}/Si substrate sample with an island-like overlayer. Photoelectron intensities are measured as a function of incident photon energy (PE) and take-off angle (TOA, measured from the sample surface). The Au layer coverage and Au and SiO{sub 2} layer thicknesses are obtained by the PE dependence, and are used for the following TOA analysis. The Au island lateral width in the cross section is obtained by the TOA dependence, including information about surface roughness, in consideration of the island shadowing at small TOAs. In both cases, curve-fitting analysis is conducted. The surface structure, which consists of layer thicknesses, overlayer coverage and island width, is determined nondestructively by a combination of PE and TOA dependent HAXPES measurements.

  8. Electronic states of solids probed by bulk-sensitive high-resolution soft X-ray photoemission spectroscopy

    CERN Document Server

    Sekiyama, A

    2003-01-01

    High-energy and high-resolution soft x-ray photoemission studies have been performed on strongly correlated Ce compounds and vanadium oxides at BL25SU of SPring-8. The bulk spectra of CeRu sub 2 are explained by a band-structure calculation (itinerant model) whereas the other Ce 4f spectra are well reproduced by calculations based on the single impurity Anderson model (model from a localized limit). In a strong contrast to so far reported results, the bulk spectral functions are revealed to be insensitive to x for Sr sub 1 sub - sub x Ca sub x VO sub 3. Our study has demonstrated the importance of high-energy and high-resolution photoemission spectroscopy for revealing detailed bulk electronic states of strongly correlated systems. (author)

  9. X-ray photoelectron spectroscopy study of the chemical structure of thermally nitrided SiO2

    Science.gov (United States)

    Vasquez, R. P.; Hecht, M. H.; Grunthaner, F. J.; Naiman, M. L.

    1984-01-01

    X-ray photoelectron spectroscopy has been used to study the composition of 100-A thermally grown SiO2 films that have been thermally nitrided in ammonia. The SiO(x)N(y)/Si interface was studied both by chemical depth profiling of the oxynitride and by removal of the Si substrate with XeF2. It is found that N is distributed throughout the film, but with the concentration higher at the surface and in a region centered 25 A from the film/substrate interface. The interface region itself is found to be oxygen-rich relative to the rest of the film. Possible models which can explain these results are discussed.

  10. XPS studies of structure-induced radiation effects at the Si/SiO2 interface. [X ray Photoelectron Spectroscopy

    Science.gov (United States)

    Grunthaner, F. J.; Lewis, B. F.; Zamini, N.; Maserjian, J.; Madhukar, A.

    1980-01-01

    The interfacial structures of radiation hard and soft oxides grown by dry and wet processes on silicon substrates have been examined by high-resolution X-ray photoelectron spectroscopy. It is found that the primary difference in the local atomic structure at the Si/SiO2 interface is the significantly higher concentration of strained 120 deg SiO2 bonds and SiO interfacial species in soft samples. Results of in situ radiation damage experiments using low energy electrons (0-20 eV) are reported which correlate with the presence of a strained layer of SiO2 (20 A) at the interface. The results are interpreted in terms of a structural model for hole and electron trap generation by ionizing radiation.

  11. Chemical order in the glassy AsxS1-x system: An x-ray-absorption spectroscopy study

    Science.gov (United States)

    Yang, C. Y.; Paesler, M. A.; Sayers, D. E.

    1989-05-01

    We have examined chemical ordering in the glassy AsxS1-x system by determining the effect of composition on the local structure of these chalcogenide glasses using x-ray-absorption spectroscopy. Structural changes associated with composition indicate that with increasing S content, the S-rich glasses on the As site have a similar local structure to crystalline As2S3 (orpiment), but the As-S-As linkages are replaced by As-S-S linkages at higher S concentration. In As-rich glasses a breakdown of the local AsS3 configuration is evident and the formation of As-As bonds is observed. Further comparison between As-rich alloys and crystalline As4S4 (realgar) suggests that a significant fraction of disordered As4S4 molecular fragments is contained in the As-rich region.

  12. Probing the electron beam induced reduction of graphite oxide by in situ X-ray photoelectron spectroscopy/mass spectrometer

    Science.gov (United States)

    Zhu, Chunhua; Hao, Xiaofei; Liu, Yu; Wu, Yeping; Wang, Jianhua

    2018-01-01

    The graphite oxide (GO) was reduced successfully by electron-beam irradiation without solution chemistry and high temperature, where the chemical structural changes and gaseous species released during the exposure was monitored directly by X-ray photoelectron spectroscopy/mass spectrometer. The degree of reduction of GO can be tuned effectively by way of electron beam intensity and irradiation time, resulting a high C/O ratio of 5.27. The evolution of C 1s spectra with irradiation time was also investigated. The CO, CO2, H2 molecules and several organic species were detected during the irradiation, confirmed that the electron beam induced the photoreduction of GO. The combined chemical structure evolution and gas species analysis make the XPS-MS highly desirable as a powerful in situ analytical instrument for tracking the reaction process. The electron-beam-induced reduction described in detail here provides potential way to fabricate graphene device from GO in one step.

  13. Trace elemental analysis of school chalk using energy dispersive X-ray florescence spectroscopy (ED-XRF)

    Science.gov (United States)

    Maruthi, Y. A.; Das, N. Lakshmana; Ramprasad, S.; Ram, S. S.; Sudarshan, M.

    2015-08-01

    The present studies focus the quantitative analysis of elements in school chalk to ensure the safety of its use. The elements like Calcium (Ca), Aluminum (Al), Iron (Fe), Silicon (Si) and Chromium (Cr) were analyzed from settled chalk dust samples collected from five classrooms (CD-1) and also from another set of unused chalk samples collected from local market (CD-2) using Energy Dispersive X-Ray florescence(ED-XRF) spectroscopy. Presence of these elements in significant concentrations in school chalk confirmed that, it is an irritant and occupational hazard. It is suggested to use protective equipments like filtered mask for mouth, nose and chalk holders. This study also suggested using the advanced mode of techniques like Digital boards, marker boards and power point presentations to mitigate the occupational hazard for classroom chalk

  14. Native target chemistry during reactive dc magnetron sputtering studied by ex-situ x-ray photoelectron spectroscopy

    Science.gov (United States)

    Greczynski, G.; Mráz, S.; Schneider, J. M.; Hultman, L.

    2017-07-01

    We report x-ray photoelectron spectroscopy (XPS) analysis of native Ti target surface chemistry during magnetron sputtering in an Ar/N2 atmosphere. To avoid air exposure, the target is capped immediately after sputtering with a few-nm-thick Al overlayers; hence, information about the chemical state of target elements as a function of N2 partial pressure pN2 is preserved. Contrary to previous reports, which assume stoichiometric TiN formation, we present direct evidence, based on core-level XPS spectra and TRIDYN simulations, that the target surface is covered by TiNx with x varying in a wide range, from 0.27 to 1.18, depending on pN2. This has far-reaching consequences both for modelling of the reactive sputtering process and for everyday thin film growth where detailed knowledge of the target state is crucial.

  15. Assessment of the Quality of Newly Formed Bone around Titanium Alloy Implants by Using X-Ray Photoelectron Spectroscopy

    Directory of Open Access Journals (Sweden)

    Hiroshi Nakada

    2012-01-01

    Full Text Available The aim of this study was to evaluate differences in bones quality between newly formed bone and cortical bone formed around titanium alloy implants by using X-ray photoelectron spectroscopy. As a result of narrow scan measurement at 4 weeks, the newly formed bone of C1s, P2p, O1s, and Ca2p were observed at a different peak range and strength compared with a cortical bone. At 8 weeks, the peak range and strength of newly formed bone were similar to those of cortical bone at C1s, P2p, and Ca2p, but not O1s. The results from this analysis indicate that the peaks and quantities of each element of newly formed bone were similar to those of cortical bone at 8 weeks, suggestive of a strong physicochemical resemblance.

  16. Probing the electronic environment of binary and ternary ionic liquid mixtures by X-ray photoelectron spectroscopy

    Science.gov (United States)

    Men, Shuang; Licence, Peter

    2017-10-01

    X-ray photoelectron spectroscopy is used to probe the electronic environment of cations and anions for three binary and one ternary chlorostannate ionic liquid mixtures. The impact of the weighting of Cl- on the electronic environment of the cation-based nitrogen atom is revealed in detail. With the increasing of the concentration of Cl-, the N 1s binding energy is decreased. The electronic environment of the anion-based component is also compared based upon Sn 3d5/2 and Cl 2p3/2 binding energies. It is found that with the increasing of the weighting of Cl-, binding energies of Sn 3d5/2 and Cl 2p3/2 both decrease.

  17. Room temperature air oxidation of nanostructured Si thin films with varying porosities as studied by x-ray photoelectron spectroscopy

    Science.gov (United States)

    Yang, D.-Q.; Meunier, M.; Sacher, E.

    2006-04-01

    The room temperature air oxidation of nanostructured Si thin films, with varying porosities, has been followed by x-ray photoelectron spectroscopy (XPS), using films deposited by KrF excimer (248 nm) laser ablation in He gas ambients. The overall oxidation, determined from the Si2p XPS spectrum, was shown to be amenable to time-porosity superposition, with the extracted shift factors indicating that oxidation is controlled by the permeability of air in the pores. A model has been developed to describe the room temperature air oxidation process as a function of time and porosity, in accord with the experimental findings. Efforts to determine O:Si atomic ratios from O1s:Si2p spectral ratios have revealed the effect of porosity on both the photoelectron attenuation lengths and the size-dependent photoemission intensities of the nanoparticles that compose the samples.

  18. Study of decorated archeological ceramics by micro X-ray fluorescence spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Papadopoulou, D. [Archaeometry Laboratory, Cultural and Educational Technology Institute/R.C. ' Athena' , Tsimiski 58, 67100 Xanthi (Greece); Technological Educational Institute of Kavala, Department of Science, Agios Loukas, 654 04 Kavala (Greece); Sakalis, A. [Archaeometry Laboratory, Cultural and Educational Technology Institute/R.C. ' Athena' , Tsimiski 58, 67100 Xanthi (Greece)], E-mail: asakalis@ceti.gr; Merousis, N. [Hellenic Open University, Kyzikou 25-27, 55133 Kalamaria, Thessaloniki (Greece); Tsirliganis, N.C. [Archaeometry Laboratory, Cultural and Educational Technology Institute/R.C. ' Athena' , Tsimiski 58, 67100 Xanthi (Greece)

    2007-09-21

    Micro-X-ray fluorescence ({mu}-XRF) spectrometry is an analytical technique that is especially suitable for the study of archeological findings since it is non-destructive, rapid, universal, versatile and multi-elemental. In the present work a compact portable {mu}-XRF spectrometer was used to characterize decorated sherds of Neolithic pottery from Polyplatanos, North Greece. The sherds were divided into four decorative groups (crusted, classic Dimini, cream on red, and black on red) and the characterization was focused on the determination of certain major, minor and trace elements (Si, K, Ca, Ti, Cr, Mn, Fe, Ni) on the decorated surface and in the clay body. The aim of this characterization was to supplement and confirm archeological information regarding the origin of the artifacts and the manufacturing techniques used for their production. The most predominant chemical elements were determined, and representative ratios (Ca/K, Fe/Mn) were calculated and compared for each individual sample group. The crusted samples and the cream on red samples showed higher concentrations of Ca in the white-crusted surface in comparison with the clay body while Fe was the predominant element in the red decorated surface. The analysis of the samples of classic Dimini, revealed higher concentrations of Mn in the black painted surfaces and higher Ca content in the light-coloured clay bodies. Finally, most samples of the black on red group present high concentrations of Mn in their decoration surface. Zn and Ni were also detected in this group in contrast with the remaining groups.

  19. Phase identification of microfeatures using EPMA methods, especially high-resolution X-ray spectroscopy

    Science.gov (United States)

    Love; Scott

    2001-02-01

    Methods of electron-probe microanalysis (EPMA), with some input from scanning and transmission electron microscopy (SEM/TEM), are applied for the identification of micro-scale constituents in a solid matrix. The subject of the study is a magnesium alloy composite, which contains silicon carbide-based fibres made by a liquid metal infiltration process. Backscattered electron imaging of the composite in the SEM showed that during composite manufacture, fibres were chemically attacked by the metal, many of the fibres exhibiting three distinct grey levels, indicative of different reaction zones, and others appearing uniformly black. EPMA measurements showed that each region contained approximately 12wt.% oxygen and that penetration of the fibre by magnesium was accompanied by a reduction in the concentration of silicon and carbon. From studying the position and shape of specific X-ray lines it was shown that magnesium penetration involved a chemical reaction with silicon oxycarbide, established in earlier EPMA studies as one of the fibre constituents. Also, in the outermost region, aluminium in the alloy reacted with free carbon in the fibre to form aluminium carbide and with magnesium to produce a Mg-Al intermetallic. The composition of black fibres was quite different from the grey ones, with negligible silicon and only a small amount of aluminium. Oxygen levels in black fibres were consistent with complete oxidation, indicating these fibres were subjected, locally, to severe oxidising conditions during composite manufacture. In the metal matrix itself, particles of a mixed magnesium/aluminium oxide, silicon carbide and magnesium silicide were observed, the latter two phases forming as silicon and carbon were ejected from fibres.

  20. X-ray and Gamma-ray Spectroscopy of Solids under Pressure

    Energy Technology Data Exchange (ETDEWEB)

    None

    2000-03-01

    This report describes our recent synchrotrons x-ray absorption fine structure (XAFS) measurements on a number of systems that undergo pressure induced changes in local structure at high pressure. The reader should also refer to the accompanying renewal proposal for a more in-depth discussion of the general scope of this program, and its relevance to condensed matter science. We merely state that the methods here are aimed at using XAFS to probe the various phenomena that are caused by high pressure, especially including various structural, and/or electronic, changes or transitions. Our general technique is based upon a pressure cell which utilizes scintered boron carbide anvils, since diamond anvils generally produce Bragg glitches which spoil the high quality XAFS necessary for precision structural measurements. Sample pressure is determined at the beam-line by measuring and analyzing, via XAFS, the compression of some cubic material contained within the sample chamber. Recently we have extended this work to 77 K using helium gas for the applied force, rather than hydraulic oil. This report period has been productive. The increased flux available at the Stanford Synchrotrons Radiation Laboratory (SSRL) has permitted our going to smaller beams, on the order of 300 pm in diameter, for precision probing of the sample region. At the same time we have received ample amounts of beam time at SSRL, in part because of the high rating of our latest user proposal. We also were invited to share some of the beam time at the National Synchrotron Light Source (NSLS) assigned to the group of our collaborator, E. A. Stern. Below we describe in some detail our recent work. Some of the pending papers are reports on systems that have been under study for some time and have been described in past progress reports and, as such, need not be described again here.

  1. K-shell X-ray spectroscopy of laser produced aluminum plasma

    Science.gov (United States)

    Kaur, Channprit; Chaurasia, S.; Poswal, A. K.; Munda, D. S.; Rossall, A. K.; Deo, M. N.; Sharma, Surinder M.

    2017-01-01

    Optimization of a laser produced plasma (LPP) X-ray source has been performed by analyzing K-shell emission spectra of Al plasma at a laser intensity of 1013-1014 W/cm2. The effect of varying the laser intensity on the emissivity of the K-shell resonance lines is studied and found to follow a power law, Ix =(IL) α with α=2.2, 2.3, 2.4 for Heβ, Heγ, Heδ respectively. The emission of these resonance lines has been found to be heavily anisotropic. A Python language based code has been developed to generate an intensity profile of K-shell spectral lines from the raw data. In theoretical calculations, the temperature is estimated by taking the ratio of the Li-like satellite (1s22p-1s2p3p) and the Heβ (1s2-1s3p) resonance line and the ratio of the He-like satellite (1s2p-2p2) and the Lyα (1s-2p) resonance line. To determine the plasma density, stark broadening of the Lyβ spectral line is used. Simulation was carried out using the FLYCHK code to generate a synthetic emission spectrum. The results obtained by FLYCHK are Te=160 eV, Th=1 keV, f=0.008, ne=5×1020 cm-3 and the analytical model resulted Te=260-419 eV and ne=3x1020 cm-3.

  2. X-ray High-resolution Spectroscopy for Laser-produced Plasma

    Science.gov (United States)

    Barbato, F.; Scarpellini, D.; Malizia, A.; Gaudio, P.; Richetta, M.; Antonelli, L.

    The study of the emission spectrum gives information about the material generating the spectrum itself and the condition in which this is generated. The wavelength spectra lines are linked to the specific element and plasma conditions (electron temperature, density), while their shape is influenced by several physical effects like Stark and Doppler ones. In this work we study the X-ray emission spectra of a copper laser-produced plasma by using a spherical bent crystal spectrometer to measure the electron temperature. The facility used is the laser TVLPS, at the Tor Vergata University in Rome. It consists of a Nd:Glass source (in first harmonic - 1064 nm) whose pulse parameters are: 8 J in energy, time duration of 15 ns and a focal spot diameter of 200 μm. The adopted spectrometer is based on a spherical bent crystal of muscovite. The device combines the focusing property of a spherical mirror with the Bragg's law. This allows to obtain a great power resolution but a limited range of analysis. In our case the resolution is on average 80 eV. As it is well-known, the position of the detector on the Rowland's circle is linked to the specific spectral range which has been studied. To select the area to be investigated, we acquired spectra by means of a flat spectrometer. The selected area is centered on 8.88 Å. To calibrate the spectrum we wrote a ray-tracing MATLAB code, which calculates the detector alignment parameters and calibration curve. We used the method of line ratio to measure the electron temperature. This is possible because we assumed the plasma to be in LTE condition. The temperature value was obtained comparing the experimental one, given by the line ratio, with the theoretical one, preceded by FLYCHK simulations.

  3. Analysis of limestones and dolomites by x-ray fluorescence spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Wheeler, B.D.

    1999-07-01

    Sources of calcium are generally widespread and quite extensive. These sources are limestone, dolomite, marl, chalk, and oyster shell. Cement plants account for nearly half of the demand, while two hundred lime plants in the US and Puerto Rico consume about twenty five percent. Since the chemical composition of the limestone and other sources of calcium is critical in the cement and lime industry, particularly for the deleterious compounds such as sodium oxide, Na{sub 2}O, magnesium oxide, MgO, phosphorus pentoxide, P{sub 2}O{sub 5}, and potassium oxide, K{sub 2}O, accurate determinations are critical. Due to the tonnage per hour, these determinations must be made rapidly and accurately. X-ray fluorescence can thereby satisfy this need for accuracy and also precision. Production of lime is performed by calcining limestone or dolomite in which the industry is generally located and concentrated in the States of Michigan and Pennsylvania. The resulting product is quicklime, CaO, and hydrated lime, Ca(OH){sub 2}. Substantial amounts of quicklime is further processed into calcium carbide in order to produce acetylene gas. In this case, the determination of P{sub 2}O{sub 5} is critical since minor quantities of phosphorus in acetylene gas can cause premature explosions. Other uses for lime are well known in the treatment of water, the paper and pulp industry, and in the steel industry for the production of slag to remove impurities. Dolomitic lime is heavily utilized in the manufacture of magnesite refractories by reacting dolomitic lime with brines from the Michigan Basin to produce magnesium oxide, MgO, and calcium chloride, CaCl{sub 2}. Sample preparation for these materials usually is performed by grinding and pelletizing or fusion with lithium-tetra-borate, Li{sub 2}B{sub 4}O{sub 7}.

  4. Understanding Oxygen Reduction on Tantalum Oxyphosphate and Tantalum Oxide Supported Platinum by X-ray Absorption Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Korovina, Anna [George Washington University; Garsany, Yannick [Naval Research Laboratory, Washington, D.C.; Epshteyn, Albert [Naval Research Laboratory, Washington, D.C.; Purdy, Andrew [Naval Research Laboratory, Washington, D.C.; More, Karren Leslie [ORNL; Swyder-Lyons, Karen [Naval Research Laboratory, Washington, D.C.; Ramaker, David [George Washington University

    2012-01-01

    The Pt activity for the oxygen reduction reaction (ORR) is improved when Pt nanoparticles are supported on nanoscale layers of tantalum oxyphosphate (nominally, TaOPO{sub 4}) on Vulcan carbon (VC) and heated at high temperature (660 C) in reducing conditions. We attempt to explain the increased activity of the Pt-TaOPO{sub 4}/VC 'HT' by comparison to other less-active electrocatalysts comprising Pt on tantalum oxide (Pt-Ta{sub 2}O{sub 5}/VC) and Pt-TaOPO{sub 4}/VC heated to 200 C in air. Our toolbox for this analysis contains the rotating disk electrode methodology for characterization of the ORR and high-angle annular dark-field scanning transmission electron microscopy with high-resolution energy-dispersive X-ray spectroscopy (EDS) capabilities. The adsorption of molecular species on the Pt and Ta is determined from the {Delta}{mu} XANES (X-ray absorption near-edge structure) adsorbate isolation technique of X-ray absorption spectroscopy (XAS) data for electrocatalsyts in situ, whereby H and OH adsorption products from water activation can be used to infer how an electrocatalyst would react for oxygen reduction. The {Delta}{mu} XANES analysis at the Pt L{sub 2} edge suggests that interfacial hydrogen exists between the Pt and the support for Pt-Ta{sub 2}O{sub 5}/VC and Pt-TaOPO{sub 4}/VC 'HT' at potentials > 0.3 V vs RHE even after surface H is removed. More importantly, in the most active sample, Pt-TaOPO{sub 4}/VC 'HT', the onset potential for O(H) adsorption is highest in the {Delta}{mu} XANES. The XAS and microscopy/EDS results show that the Pt-TaOPO{sub 4}/VC 'HT' is Pt-Ta{sub 2}O{sub 5}/VC with polyphosphate groups directly associated with the Pt. From the body of results, we surmise that the nanoscale layer of polyphosphate on the Pt-TaOPO{sub 4}/VC 'HT' facilitates proton conduction to the Pt particles and hence moves the equilibrium for OH adsorption on the Pt to higher potentials.

  5. The Electronic Structure of Carbon and its Allotropes as Determined by Soft X-Ray Emission Spectroscopy

    Science.gov (United States)

    Velasquez, Steven

    1993-01-01

    A study of the electronic structure of the stage I and stage II alkali graphite intercalation compounds using soft x-ray emission spectroscopy has been done. The pi band of the alkali graphite intercalation compounds is strongly affected by the intercalation process as witnessed by the apparent change in shape of the density of states in comparison to highly oriented pyrolytic graphite. From the change in shape, it is possible to determine the amount of charge transferred from the intercalant to the graphite. Our result of complete charge transfer is in disagreement with the results of Wiech and his co-workers. A thorough discussion of both methods of analysis is presented. A comparison of the observed density of states of synthetically grown diamond with natural diamond indicates that synthetic diamond is not the same as natural diamond. A brief discussion of various techniques for growing diamond is presented, as well as the construction of a chemical vapor deposition apparatus to grow diamond-like thin films along with soft x-ray emission and Raman spectroscopy measurements. We find that diamond can only be grown at low pressures if it is highly defective. This is in agreement with theoretical models of chemical vapor deposition. We also discuss the electronic structure of a very rare form of diamond, Lonsdaleite (hexagonal diamond). Lonsdaleite is sp^3 bonded carbon but in a hexagonal matrix. It is only found in highly shocked systems and appears to be the metastable phase between graphite and diamond on the carbon phase diagram. We also briefly discuss the most recently discovered member of the carbon family, Buckminsterfullerene. We present electronic structure data on C_ {60} samples produced in a carbon-arc generator designed and built at the University. Comparison of our data to other published data shows very good agreement.

  6. Kissing G domains of MnmE monitored by X-ray crystallography and pulse electron paramagnetic resonance spectroscopy.

    Directory of Open Access Journals (Sweden)

    Simon Meyer

    2009-10-01

    Full Text Available MnmE, which is involved in the modification of the wobble position of certain tRNAs, belongs to the expanding class of G proteins activated by nucleotide-dependent dimerization (GADs. Previous models suggested the protein to be a multidomain protein whose G domains contact each other in a nucleotide dependent manner. Here we employ a combined approach of X-ray crystallography and pulse electron paramagnetic resonance (EPR spectroscopy to show that large domain movements are coupled to the G protein cycle of MnmE. The X-ray structures show MnmE to be a constitutive homodimer where the highly mobile G domains face each other in various orientations but are not in close contact as suggested by the GDP-AlF(x structure of the isolated domains. Distance measurements by pulse double electron-electron resonance (DEER spectroscopy show that the G domains adopt an open conformation in the nucleotide free/GDP-bound and an open/closed two-state equilibrium in the GTP-bound state, with maximal distance variations of 18 A. With GDP and AlF(x, which mimic the transition state of the phosphoryl transfer reaction, only the closed conformation is observed. Dimerization of the active sites with GDP-AlF(x requires the presence of specific monovalent cations, thus reflecting the requirements for the GTPase reaction of MnmE. Our results directly demonstrate the nature of the conformational changes MnmE was previously suggested to undergo during its GTPase cycle. They show the nucleotide-dependent dynamic movements of the G domains around two swivel positions relative to the rest of the protein, and they are of crucial importance for understanding the mechanistic principles of this GAD.

  7. Mg{sup +}-He{sup +} mixed crystals for high precision spectroscopy in the XUV

    Energy Technology Data Exchange (ETDEWEB)

    Knuenz, Sebastian; Hermann, Maximilian; Batteiger, Valentin; Ozawa, Akira; Udem, Thomas; Haensch, Theodor W. [Max-Planck-Institut fuer Quantenoptik, Garching (Germany); Zhu, Feng; Schuessler, Hans [Department of Physics, Texas A and M University, College Station, Texas (United States)

    2008-07-01

    The 1s-2s two photon transition of singly ionized hydrogen-like helium at 60 nm is an interesting candidate for precision tests of bound state QED. Rapid progress in the development of high-power XUV frequency combs lets high resolution spectroscopy of this transition come in sight for the first time. We report on important steps towards this goal. In our novel 6-rod RF trap, we generated and analyzed cold mixed crystals.

  8. Ultraviolet photochemical reaction of [Fe(III(C2O43]3− in aqueous solutions studied by femtosecond time-resolved X-ray absorption spectroscopy using an X-ray free electron laser

    Directory of Open Access Journals (Sweden)

    Y. Ogi

    2015-05-01

    Full Text Available Time-resolved X-ray absorption spectroscopy was performed for aqueous ammonium iron(III oxalate trihydrate solutions using an X-ray free electron laser and a synchronized ultraviolet laser. The spectral and time resolutions of the experiment were 1.3 eV and 200 fs, respectively. A femtosecond 268 nm pulse was employed to excite [Fe(III(C2O43]3− in solution from the high-spin ground electronic state to ligand-to-metal charge transfer state(s, and the subsequent dynamics were studied by observing the time-evolution of the X-ray absorption spectrum near the Fe K-edge. Upon 268 nm photoexcitation, the Fe K-edge underwent a red-shift by more than 4 eV within 140 fs; however, the magnitude of the redshift subsequently diminished within 3 ps. The Fe K-edge of the photoproduct remained lower in energy than that of [Fe(III(C2O43]3−. The observed red-shift of the Fe K-edge and the spectral feature of the product indicate that Fe(III is upon excitation immediately photoreduced to Fe(II, followed by ligand dissociation from Fe(II. Based on a comparison of the X-ray absorption spectra with density functional theory calculations, we propose that the dissociation proceeds in two steps, forming first [(CO2•Fe(II(C2O42]3− and subsequently [Fe(II(C2O42]2−.

  9. Proceedings of the eighth international colloquium on ultraviolet and x-ray spectroscopy of astrophysical and laboratory plasmas (IAU colloquium 86)

    Energy Technology Data Exchange (ETDEWEB)

    1984-01-01

    This volume represents the Proceedings of the Eighth International Colloquium on Ultraviolet and X-Ray Spectroscopy of Astrophysical and Laboratory Plasmas. The aim of this series of colloquia has been to bring together workers in the fields of astrophysical spectroscopy, laboratory spectroscopy and atomic physics in order to exchange ideas and results on problems which are common to these different disciplines. In addition to the presented papers there was a poster paper session. (WRF)

  10. Origin of Pressure-induced Superconducting Phase in KxFe2−ySe2 studied by Synchrotron X-ray Diffraction and Spectroscopy

    Science.gov (United States)

    Yamamoto, Yoshiya; Yamaoka, Hitoshi; Tanaka, Masashi; Okazaki, Hiroyuki; Ozaki, Toshinori; Takano, Yoshihiko; Lin, Jung-Fu; Fujita, Hidenori; Kagayama, Tomoko; Shimizu, Katsuya; Hiraoka, Nozomu; Ishii, Hirofumi; Liao, Yen-Fa; Tsuei, Ku-Ding; Mizuki, Jun’ichiro

    2016-01-01

    Pressure dependence of the electronic and crystal structures of KxFe2−ySe2, which has pressure-induced two superconducting domes of SC I and SC II, was investigated by x-ray emission spectroscopy and diffraction. X-ray diffraction data show that compressibility along the c-axis changes around 12 GPa, where a new superconducting phase of SC II appears. This suggests a possible tetragonal to collapsed tetragonal phase transition. X-ray emission spectroscopy data also shows the change in the electronic structure around 12 GPa. These results can be explained by the scenario that the two SC domes under pressure originate from the change of Fermi surface topology. Our results here show the pronounced increase of the density of states near the Fermi surface under pressure with a structural phase transition, which can help address our fundamental understanding for the appearance of the SC II phase. PMID:27499373

  11. Investigation of Co nanoparticle formation using time-dependent and spatially-resolved X-ray absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Zinoveva, S.

    2008-04-15

    A crucial step towards controlled synthesis of nanoparticles is the detailed understanding of the various chemical processes that take place during the synthesis. X-ray Absorption Spectroscopy (XAS) is especially suitable for elucidating the type and structure of the intermediate metal species. It is applicable to materials that have no long range order and provides information on both electronic and geometric structures. Here a comparative study is reported of the formation of cobalt nanoparticles via thermolysis of two organometallic precursors dicobalt octacarbonyl (DCO) and alkyne-bridged dicobalt hexacarbonyl (ADH) in the presence of aluminum organics. Using time-dependent XAS a reaction pathway different from both the atom based La Mer model and the Watzky and Finsky autocatalytic surface growth model is observed. Where prior to the nucleation several intermediates are formed and the initial nucleus is composed of Co atoms coordinated with ligands Co{sub n}(CO){sub m} with n=2-3, m=3-5. The formation of Co nanoparticles was also investigated using a reaction different from thermolysis of cobalt carbonyls, namely reduction of Co (II) acetate by sodium borohydrate. Here the combination of microreactor system and spatially resolved XAS allowed ''in situ'' monitoring of the wet chemical synthesis. Several steps of the reaction were spatially resolved in the microreactor. The vertical size of the X-ray beam (50 {mu}m) focused with Kirkpatrick-Baez mirror system, determines the time resolution (better than 2 ms). The results provide direct insight into rapid process of nanoparticles formation and demonstrate the potential of this new technique for the fundamental studies of such type of processes where miniaturization and timeresolution are important. Like in the carbonyls thermolysis no evidence for the reduction of the starting complex to isolated Co{sup 0} atoms followed by nucleation of Co{sup 0} atoms was observed. (orig.)

  12. Band offset in zinc oxy-sulfide/cubic-tin sulfide interface from X-ray photoelectron spectroscopy

    Science.gov (United States)

    K. C., Sanal; Nair, P. K.; Nair, M. T. S.

    2017-02-01

    Zinc oxy-sulfide, ZnOxS1-x, has been found to provide better band alignment in thin film solar cells of tin sulfide of orthorhombic crystalline structure. Here we examine ZnOxS1-x/SnS-CUB interface, in which the ZnOxS1-x thin film was deposited by radio frequency (rf) magnetron sputtering on SnS thin film of cubic (CUB) crystalline structure with a band gap (Eg) of 1.72 eV, obtained via chemical deposition. X-ray photoelectron spectroscopy provides the valence band maxima of the materials and hence places the conduction band offset of 0.41 eV for SnS-CUB/ZnO0.27S0.73 and -0.28 eV for SnS-CUB/ZnO0.88S0.12 interfaces. Thin films of ZnOxS1-x with 175-240 nm in thickness were deposited from targets prepared with different ZnO to ZnS molar ratios. With the target of molar ratio of 1:13.4, the thin films are of composition ZnO0.27S0.73 with hexagonal crystalline structure and with that of 1:1.7 ratio, it is ZnO0.88S0.12. The optical band gap of the ZnOxS1-x thin films varies from 2.90 eV to 3.21 eV as the sulfur to zinc ratio in the film increases from 0.12:1 to 0.73:1 as determined from X-ray diffraction patterns. Thus, band offsets sought for absorber materials and zinc oxy-sulfide in solar cells may be achieved through a choice of ZnO:ZnS ratio in the sputtering target.

  13. Study of Pd/Y based multilayers using high energy photoemission spectroscopy combined with x-ray standing waves

    Science.gov (United States)

    Wu, M.-Y.; Ilakovac, V.; André, J.-M.; Le Guen, K.; Giglia, A.; Rueff, J.-P.; Huang, Q.-S.; Wang, Z.-S.; Jonnard, P.

    2017-05-01

    We use hard x-ray photoemission spectroscopy combined with x-ray standing waves to characterize a series of Pd/Y multilayers designed to work in the 7.5-11 nm wavelength range. The samples, prepared by magnetron sputtering, are deposited either with or without nitrogen introduced in the sputtering gas. The aimed period of the samples is 4 nm. The experiments consist in obtaining the core level spectra of the various elements for a series of grazing angles. The angular scan is made in the range given by the Bragg law, the multilayer period and the incident photon energy. Given the period of the multilayer and the presence of a 2.5 nm-thick B4C capping layer, the photon energy is chosen to be 10 keV in order to probe the first 5-6 periods of the stack. Thus the Bragg angle is a little less than 1°. Rotating the sample enables putting the nodes of the electric field at some particular location of the stack, thus to make the excitation depth-selective, probing one interface or another or the center of one given layer. The changes of the chemical shift in the Pd 2p and 3d, Y 2p and 3d, O 1s, N 1s, C 1s and B 1s as a function of the angle, that is to say as a function of the location in the stack will give information about the possible interfacial process taking place in the Pd/Y multilayers.

  14. Broadband THz waveguiding and high-precision broadband time-resolved spectroscopy

    DEFF Research Database (Denmark)

    Cooke, David; Iwaszczuk, Krzysztof; Nielsen, Kristian

    2009-01-01

    , have tailored dispersion and may be bent into sharp bends. Due to the confinement of the THz field in the core of the fibers they are ideal for stable guiding of THz light in confined environments, and may serve as a useful basis for a wealth of fiber-based photonic components in the THz range......We demonstrate optical fibers designed for the THz frequency range, fabricated in a low-loss polymer. The polymer fibers display a broadband loss of 0.4 dB/cm over the 0.1-1 THz range, with a minimum loss of 0.1 dB/cm in the region near 500 GHz. The fibers, based on endlessly single-mode design......, particularly in spectroscopic applications where tight confinement of the THz field is required. We further demonstrate a new spectroscopic technique for ultrafast time-resolved THz time-domain spectroscopy which simultaneously acquires both reference and sample data. By using this scheme we show...

  15. High Precision Continuous and Real-Time Measurement of Atmospheric Oxygen Using Cavity Ring-Down Spectroscopy

    Science.gov (United States)

    Kim-Hak, David; Leuenberger, Markus; Berhanu, Tesfaye; Nyfeler, Peter; Hoffnagle, John; Sun, Minghua

    2017-04-01

    Oxygen (O2) is a major and vital component of the Earth atmosphere representing about 21% of its composition. It is consumed or produced through biochemical processes such as combustion, respiration, and photosynthesis and can be used as a top-down constraint on the carbon cycle. The observed variations of oxygen in the atmosphere are relatively small, in the order of a few ppm's. This presents the main technical challenge for the measurement since a very high level of precision on a large background is required. Only few analytical methods including mass spectrometry, fuel, ultraviolet[1] and paramagnetic cells are capable of achieving it. Here we present new developments of a high-precision gas analyzer that utilizes the technique of Cavity Ring-Down Spectroscopy to measure oxygen concentration and its oxygen isotope ratio 18O/16O. Its compact and ruggedness design combined with high precision and long-term stability allows the user to deploy the instrument in the field for continuous monitoring of atmospheric oxygen level. Measurements have a 1-σ 5-minute averaging precision of 1-2 ppm for O2 over a dynamic range of 0-50%. We will present comparative test results of this instrument against the incumbent technologies such as the mass spectrometer and the paramagnetic cell. In addition, we will demonstrate its long-term stability from a field deployment in Switzerland.

  16. BROADBAND X-RAY IMAGING AND SPECTROSCOPY OF THE CRAB NEBULA AND PULSAR WITH NuSTAR

    Energy Technology Data Exchange (ETDEWEB)

    Madsen, Kristin K.; Harrison, Fiona; Grefenstette, Brian W. [Cahill Center for Astronomy and Astrophysics, California Institute of Technology, Pasadena, CA 91125 (United States); Reynolds, Stephen [Physics Department, NC State University, Raleigh, NC 27695 (United States); An, Hongjun [Department of Physics, McGill University, Montreal, Quebec, H3A 2T8 (Canada); Boggs, Steven; Craig, William W.; Zoglauer, Andreas [Space Sciences Laboratory, University of California, Berkeley, CA 94720 (United States); Christensen, Finn E. [DTU Space, National Space Institute, Technical University of Denmark, Elektronvej 327, DK-2800 Lyngby (Denmark); Fryer, Chris L. [CCS-2, Los Alamos National Laboratory, Livermore, CA 94550 (United States); Hailey, Charles J.; Nynka, Melania [Columbia Astrophysics Laboratory, Columbia University, New York, NY 10027 (United States); Markwardt, Craig; Zhang, William [Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Stern, Daniel [Jet Propulsion Laboratory, California Institute of Technology, Pasadena, CA 91109 (United States)

    2015-03-01

    We present broadband (3-78 keV) NuSTAR X-ray imaging and spectroscopy of the Crab nebula and pulsar. We show that while the phase-averaged and spatially integrated nebula + pulsar spectrum is a power law in this energy band, spatially resolved spectroscopy of the nebula finds a break at ∼9 keV in the spectral photon index of the torus structure with a steepening characterized by ΔΓ ∼ 0.25. We also confirm a previously reported steepening in the pulsed spectrum, and quantify it with a broken power law with break energy at ∼12 keV and ΔΓ ∼ 0.27. We present spectral maps of the inner 100'' of the remnant and measure the size of the nebula as a function of energy in seven bands. These results find that the rate of shrinkage with energy of the torus size can be fitted by a power law with an index of γ = 0.094 ± 0.018, consistent with the predictions of Kennel and Coroniti. The change in size is more rapid in the NW direction, coinciding with the counter-jet where we find the index to be a factor of two larger. NuSTAR observed the Crab during the latter part of a γ-ray flare, but found no increase in flux in the 3-78 keV energy band.

  17. Determining Orientational Structure of Diamondoid Thiols Attached to Silver Using Near Edge X-ray Absorption Fine Structure Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Willey, T M; Lee, J I; Fabbri, J D; Wang, D; Nielsen, M; Randel, J C; Schreiner, P R; Fokin, A A; Tkachenko, B A; Fokina, N A; Dahl, J P; Carlson, R K; Terminello, L J; Melosh, N A; van Buuren, T

    2008-10-07

    Near-edge x-ray absorption fine structure spectroscopy (NEXAFS) is a powerful tool for determination of molecular orientation in self-assembled monolayers and other surface-attached molecules. A general framework for using NEXAFS to simultaneously determine molecular tilt and twist of rigid molecules attached to surfaces is presented. This framework is applied to self-assembled monolayers of higher diamondoid, hydrocarbon molecules with cubic-diamond-cage structures. Diamondoid monolayers chemisorbed on metal substrates are known to exhibit interesting electronic and surface properties. This work compares molecular orientation in monolayers prepared on silver substrates using two different thiol positional isomers of [121]tetramantane, and thiols derived from two different pentamantane structural isomers, [1212]pentamantane and [1(2,3)4]pentamantane. The observed differences in monolayer structure demonstrate the utility and limitations of NEXAFS spectroscopy and the framework. The results also demonstrate the ability to control diamondoid assembly, in particular the molecular orientational structure, providing a flexible platform for the modification of surface properties with this exciting new class of nanodiamond materials.

  18. Sulfur amino acids and alanine on pyrite (100) by X-ray photoemission spectroscopy: Surface or molecular role?

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez-Arenillas, M.; Galvez-Martinez, S.; Mateo-Marti, E., E-mail: mateome@cab.inta-csic.es

    2017-08-31

    Highlights: • Surface annealing pretreatment on pyrite surfaces can select molecular adsorption. • Enriched monosulfide species on pyrite (100) surface favors NH{sub 2} adsorption form. • Enriching disulfide species on pyrite (100) surface promotes NH{sub 3}{sup +} adsorption form. • Unique structure of each aminoacid provides a particular fingerprint in the process. • Spectroscopy evidence, pretreatment surface processes drives molecular adsorption. - Abstract: This paper describes the first successful adsorption of the cysteine, cystine, methionine and alanine amino acids on the pyrite (100) surface under ultra-high vacuum conditions with crucial chemical adsorption parameters driving the process. We have demonstrated by X-ray photoemission spectroscopy (XPS) that the surface pretreatment annealing process on pyrite surfaces is a critical parameter driving surface reactivity. The presence of enriched monosulfide species on the pyrite (100) surface favours the amino acid NH{sub 2} chemical form, whereas a longer annealing surface pretreatment of over 3 h repairs the sulfur vacancies in the pyrite, enriching disulfide species on the pyrite surface, which promotes NH{sub 3}{sup +} adsorption due to the sulfur vacancies in the pyrite being replaced by sulfur atom dimers (S{sub 2}{sup 2−}) on the surface. Furthermore, even if the surface chemistry (monosulfide or disulfide species enrichment) is the main factor promoting a partial conversion from NH{sub 2} to NH{sub 3}{sup +} species, the unique chemical structure of each amino acid provides a particular fingerprint in the process.

  19. The rapid formation of tin oxide pillared laponite by microwave heating: Characterisation by tin-119 Mössbauer spectroscopy, X-ray photoelectron spectroscopy and nuclear magnetic resonance

    Science.gov (United States)

    Berry, Frank J.; Ashcroft, R. Claire; Beevers, Martin S.; Bond, Stephen P.; Gelders, Andrew; Lawrence, Monique A. M.; McWhinnie, William R.

    1992-04-01

    The intercalation of organotin-compounds into laponite and the formation of tin(IV) oxide pillars is rapidly achieved when performed in a microwave oven.119Sn Mössbauer- and x-ray- photoelectron-spectroscopy suggest that Ph3SnCl and Ph2SnCl2 undergo hydrolysis on the surface once sorbed. The treatment of Ph3SnCl/laponite with microwave radiation also induces the formation of a metallic phase which contains both tin and magnesium.

  20. Internal dynamics in helical molecules studied by X-ray diffraction, NMR spectroscopy and DFT calculations

    Czech Academy of Sciences Publication Activity Database

    Dračínský, Martin; Storch, Jan; Církva, Vladimír; Císařová, I.; Sýkora, Jan

    2017-01-01

    Roč. 19, č. 4 (2017), s. 2900-2907 ISSN 1463-9076 R&D Projects: GA ČR GA15-11223S; GA ČR GA15-12719S Institutional support: RVO:61388963 ; RVO:67985858 Keywords : helicene * NMR spectroscopy * DFT calculations Subject RIV: CF - Physical ; Theoretical Chemistry OBOR OECD: Physical chemistry (UCHP-M) Impact factor: 4.123, year: 2016 http://pubs.rsc.org/en/content/articlehtml/2013/cp/c6cp07552e

  1. L-Edge X-ray Absorption Spectroscopy of Dilute Systems Relevant to Metalloproteins Using an X-ray Free-Electron Laser

    NARCIS (Netherlands)

    Mitzner, Rolf; Rehanek, Jens; Kern, Jan; Gul, Sheraz; Hattne, Johan; Taguchi, Taketo; Alonso-Mori, Roberto; Tran, Rosalie; Weniger, Christian; Schroeder, Henning; Quevedo, Wilson; Laksmono, Hartawan; Sierra, Raymond G.; Han, Guangye; Lassalle-Kaiser, Benedikt; Koroidov, Sergey; Kubicek, Katharina; Schreck, Simon; Kunnus, Kristjan; Brzhezinskaya, Maria; Firsov, Alexander; Minitti, Michael P.; Turner, Joshua J.; Moeller, Stefan; Sauter, Nicholas K.; Bogan, Michael J.; Nordlund, Dennis; Schlotter, William F.; Messinger, Johannes; Borovik, Andrew; Techert, Simone; de Groot, Frank M. F.|info:eu-repo/dai/nl/08747610X; Foehlisch, Alexander; Erko, Alexei; Bergmann, Uwe; Yachandra, Vittal K.; Wernet, Philippe; Yano, Junko

    2013-01-01

    L-edge spectroscopy of 3d transition metals provides important electronic structure information and has been used in many fields. However, the use of this method for studying dilute aqueous systems, such as metalloenzymes, has not been prevalent because of severe radiation damage and the lack of

  2. An investigation of the chromium oxidation state of a monoanionic chromium tris(catecholate) complex by X-ray absorption and EPR spectroscopies

    DEFF Research Database (Denmark)

    Pattison, D I; Levina, A; Davies, Michael Jonathan

    2001-01-01

    The well-known monoanionic Cr tris(3,5-di-tert-butylcatecholato) complex, [Cr(DTBC)3]-, has been studied by X-ray absorption spectroscopy. The multiple-scattering fit to the XAFS gave good correlation (R = 19.8%) and good values for all of the bond lengths, angles, and Debye-Waller factors. The p...

  3. Hydrogen as a Modifier of the Structure and Electronic Properties of Platinum in Acidic Zeolite. LTL: A Combined Infrared and X-ray Absorption Spectroscopy Study.

    NARCIS (Netherlands)

    Koningsberger, D.C.; Vaarkamp, M.; Mojet, B.L.; Kappers, M.J.; Miller, J.T.

    1995-01-01

    The structure and electronic properties of platinum in WH-LTL after reduction at 300 'C and heating in helium to 500 or 690 'C were determined using X-ray absorption and infrared spectroscopy. After reduction at 300 'C, the platinum particles were metallic, consisted of 4 or 5 atoms, and were

  4. Applicability of X-ray fluorescence spectroscopy as method to determine thickness and composition of stacks of metal thin films: A comparison with imaging and profilometry

    NARCIS (Netherlands)

    Vrielink, J.A.M.; Tiggelaar, Roald M.; Gardeniers, Johannes G.E.; Lefferts, Leonardus

    2012-01-01

    In this work the applicability of X-ray fluorescence spectroscopy (XRF) for fast, accurate and non-destructive determination of the thickness of a variety of single-layer and multi-layer metal thin films deposited on glass and silicon is investigated. Data obtained with XRF is compared with

  5. Characterization of thin heteroepitaxial diamond films on Ir/SrTiO3 by X-ray diffraction and micro-Raman spectroscopy

    OpenAIRE

    Stritzker, Bernd

    1999-01-01

    Characterization of thin heteroepitaxial diamond films on Ir/SrTiO3 by X-ray diffraction and micro-Raman spectroscopy / H. Roll, M. Schreck, B. Stritzker. – In: Applied Diamond Conference/ Frontier Carbon Technology Joint Conference 1999 / ed. by: M. Yoshikawa ... - Tsukuba : Tsukuba Research Center, 1999. S. 73-781

  6. CAT-ACT-A new highly versatile x-ray spectroscopy beamline for catalysis and radionuclide science at the KIT synchrotron light facility ANKA.

    Science.gov (United States)

    Zimina, A; Dardenne, K; Denecke, M A; Doronkin, D E; Huttel, E; Lichtenberg, H; Mangold, S; Pruessmann, T; Rothe, J; Spangenberg, Th; Steininger, R; Vitova, T; Geckeis, H; Grunwaldt, J-D

    2017-11-01

    CAT-ACT-the hard X-ray beamline for CATalysis and ACTinide/radionuclide research at the KIT synchrotron radiation facility ANKA-is dedicated to X-ray spectroscopy, including "flux hungry" photon-in/photon-out and correlative techniques and combines state-of-the-art optics with a unique infrastructure for radionuclide and catalysis research. Measurements can be performed at photon energies varying between 3.4 keV and 55 keV, thus encompassing the actinide M- and L-edge or potassium K-edge up to the K-edges of the lanthanide series such as cerium. Well-established X-ray absorption fine structure spectroscopy in transmission and fluorescence detection modes is available in combination with high energy-resolution X-ray emission spectroscopy or X-ray diffraction techniques. The modular beamline design with two alternately operated in-line experimental stations enables sufficient flexibility to adapt sample environments and detection systems to many scientific challenges. The ACT experimental station focuses on various aspects of nuclear waste disposal within the mission of the Helmholtz association to contribute to the solution of one of the greatest scientific and social challenges of our time-the safe disposal of heat producing, highly radioactive waste forms from nuclear energy production. It augments present capabilities at the INE-Beamline by increasing the flux and extending the energy range into the hard X-ray regime. The CAT experimental station focuses on catalytic materials, e.g., for energy-related and exhaust gas catalysis. Characterization of catalytically active materials under realistic reaction conditions and the development of in situ and operando cells for sample environments close to industrial reactors are essential aspects at CAT.

  7. CAT-ACT—A new highly versatile x-ray spectroscopy beamline for catalysis and radionuclide science at the KIT synchrotron light facility ANKA

    Science.gov (United States)

    Zimina, A.; Dardenne, K.; Denecke, M. A.; Doronkin, D. E.; Huttel, E.; Lichtenberg, H.; Mangold, S.; Pruessmann, T.; Rothe, J.; Spangenberg, Th.; Steininger, R.; Vitova, T.; Geckeis, H.; Grunwaldt, J.-D.

    2017-11-01

    CAT-ACT—the hard X-ray beamline for CATalysis and ACTinide/radionuclide research at the KIT synchrotron radiation facility ANKA—is dedicated to X-ray spectroscopy, including "flux hungry" photon-in/photon-out and correlative techniques and combines state-of-the-art optics with a unique infrastructure for radionuclide and catalysis research. Measurements can be performed at photon energies varying between 3.4 keV and 55 keV, thus encompassing the actinide M- and L-edge or potassium K-edge up to the K-edges of the lanthanide series such as cerium. Well-established X-ray absorption fine structure spectroscopy in transmission and fluorescence detection modes is available in combination with high energy-resolution X-ray emission spectroscopy or X-ray diffraction techniques. The modular beamline design with two alternately operated in-line experimental stations enables sufficient flexibility to adapt sample environments and detection systems to many scientific challenges. The ACT experimental station focuses on various aspects of nuclear waste disposal within the mission of the Helmholtz association to contribute to the solution of one of the greatest scientific and social challenges of our time—the safe disposal of heat producing, highly radioactive waste forms from nuclear energy production. It augments present capabilities at the INE-Beamline by increasing the flux and extending the energy range into the hard X-ray regime. The CAT experimental station focuses on catalytic materials, e.g., for energy-related and exhaust gas catalysis. Characterization of catalytically active materials under realistic reaction conditions and the development of in situ and operando cells for sample environments close to industrial reactors are essential aspects at CAT.

  8. Bismuth speciation in hydrothermal fluids: An X-ray absorption spectroscopy and solubility study

    Science.gov (United States)

    Tooth, Blake; Etschmann, Barbara; Pokrovski, Gleb S.; Testemale, Denis; Hazemann, Jean-Louis; Grundler, Pascal V.; Brugger, Joël

    2013-01-01

    The solubility of bismuth oxide (α-Bi2O3(s); bismite) in near-neutral sodium perchlorate solutions at 65 and 80 °C, and pure water from 150 to 600 °C, PSat to 800 bar was studied using various batch-reactor techniques and in situ XAS spectroscopy. The solubility of Bi2O3(s) follows a similar trend to Sb2O3(s) (senarmontite), which has been interpreted in terms of a neutral Sb(OH)3(aq) complex. Thus a similar neutral complex, Bi(OH)3(aq), is inferred for Bi. XANES spectroscopy confirms that the Bi(OH)3(aq) complex carries a stereochemically active lone electron pair, and EXAFS data suggest that the geometry of the complex changes little over the temperature range 380-610 °C at 800 bar, with three oxygen neighbors at ˜2.08 Å. The solubility data obtained in this study are used in conjunction with thermodynamic properties for α-Bi2O3(s) to obtain thermodynamic parameters for Bi(OH)3(aq) within the framework of the revised Helgeson-Kirkham-Flowers (HKF) equation of state. Speciation calculations using these new properties indicate that, similarly to arsenic and antimony, bismuth is transported predominantly as a neutral hydroxide complex in a wide range of temperature, pressure, and fluid compositions. In contrast to arsenic and antimony, bismuth is much less soluble in typical hydrothermal fluids in the form of hydroxide complexes, and high temperatures (⩾400 °C) are required for significant Bi transport by aqueous fluids. These results are consistent with the common association between Bi mineralization and magmatism.

  9. Room temperature redox reaction by oxide ion migration at carbon/Gd-doped CeO2 heterointerface probed by an in situ hard x-ray photoemission and soft x-ray absorption spectroscopies

    Directory of Open Access Journals (Sweden)

    Takashi Tsuchiya, Shogo Miyoshi, Yoshiyuki Yamashita, Hideki Yoshikawa, Kazuya Terabe, Keisuke Kobayashi and Shu Yamaguchi

    2013-01-01

    Full Text Available In situ hard x-ray photoemission spectroscopy (HX-PES and soft x-ray absorption spectroscopy (SX-XAS have been employed to investigate a local redox reaction at the carbon/Gd-doped CeO2 (GDC thin film heterointerface under applied dc bias. In HX-PES, Ce3d and O1s core levels show a parallel chemical shift as large as 3.2 eV, corresponding to the redox window where ionic conductivity is predominant. The window width is equal to the energy gap between donor and acceptor levels of the GDC electrolyte. The Ce M-edge SX-XAS spectra also show a considerable increase of Ce3+ satellite peak intensity, corresponding to electrochemical reduction by oxide ion migration. In addition to the reversible redox reaction, two distinct phenomena by the electrochemical transport of oxide ions are observed as an irreversible reduction of the entire oxide film by O2 evolution from the GDC film to the gas phase, as well as a vigorous precipitation of oxygen gas at the bottom electrode to lift off the GDC film. These in situ spectroscopic observations describe well the electrochemical polarization behavior of a metal/GDC/metal capacitor-like two-electrode cell at room temperature.

  10. X-ray photoelectron spectroscopy (XPS) and FTIR studies of vanadium barium phosphate glasses

    Energy Technology Data Exchange (ETDEWEB)

    Majjane, Abdelilah [Laboratoire de Physico-Chimie des Matériaux Vitreux et Cristallisés, Université Ibn Tofail, Faculté des Sciences, Kénitra 14090 (Morocco); Chahine, Abdelkrim, E-mail: abdelkrimchahine@gmail.com [Laboratoire de Physico-Chimie des Matériaux Vitreux et Cristallisés, Université Ibn Tofail, Faculté des Sciences, Kénitra 14090 (Morocco); Et-tabirou, Mohamed [Laboratoire de Physico-Chimie des Matériaux Vitreux et Cristallisés, Université Ibn Tofail, Faculté des Sciences, Kénitra 14090 (Morocco); Echchahed, Bousselham [Laboratoire d' Electrochimie, Corrosion et Environnement, Université Ibn Tofail, Faculté des Sciences, Kénitra (Morocco); Do, Trong-On [Département de génie chimique, Université Laval, G1K 7P4 (Canada); Breen, Peter Mc [Département de chimie, Université Laval, G1K 7P4 (Canada)

    2014-01-15

    Barium vanadophosphate glasses, having composition 50BaO–xV{sub 2}O{sub 5}–(50 − x)P{sub 2}O{sub 5}, (x = 0–50 mol%), were prepared by conventional melt quench method. Density, molar volume and glass transition temperature (T{sub g}) were measured as a function of V{sub 2}O{sub 5} content. Structural investigation was done using XPS and FTIR spectroscopy. First, substitution of the P{sub 2}O{sub 5} by the V{sub 2}O{sub 5} in the metaphosphate 50BaO–50P{sub 2}O{sub 5} glass increases the density and T{sub g} and decreases the molar volume. When the amount of V{sub 2}O{sub 5} increases, all these properties show a reverse trend. XPS measurement found in the O1s, P2p, and V2p core level spectra indicate the presence of primarily P–O–P, P–O–V and V–O–V structural bonds, the asymmetry in the P 2p spectra indeed arises from the spin-orbit splitting of P 2p core level, and more than one valence state of V ions being present. IR spectroscopy reveals the depolymerization of the phosphate glass network by systematic conversion of metaphosphate chains into pyrophosphate groups and then orthophosphate groups. Even though metaphosphate to pyrophosphate conversion is taking place due to breaking of P–O–P linkages, formation of P–O–V and P–O–Ba linkages provide cross linking between short P-structural units, which make the glass network more rigid. Above 10–20 mol% V{sub 2}O{sub 5} content, network is highly depolymerized due to the formation of orthophosphate units and V–O–V bridge bonds, resulting in poor cross-linking, making the glass network less rigid. - Highlights: • Barium–vanadium–phosphate glasses. • Structure has been investigated by XPS and IR spectra. • Variation in structure and properties with substitution of V{sub 2}O{sub 5} for P{sub 2}O{sub 5}. • Conversion of metaphosphate to pyrophosphate and finally to orthophosphate. • Substitution of P–O–P linkages by P–O–V, P–O–Ba and V–O–V linkages.

  11. Spatially resolved x-ray fluorescence spectroscopy of beryllium capsule implosions at the NIF

    Science.gov (United States)

    MacDonald, M. J.; Bishel, D. T.; Saunders, A. M.; Scott, H. A.; Kyrala, G.; Kline, J.; MacLaren, S.; Thorn, D. B.; Yi, S. A.; Zylstra, A. B.; Falcone, R. W.; Doeppner, T.

    2017-10-01

    Beryllium ablators used in indirectly driven inertial confinement fusion implosions are doped with copper to prevent preheat of the cryogenic hydrogen fuel. Here, we present analysis of spatially resolved copper K- α fluorescence spectra from the beryllium ablator layer. It has been shown that K- α fluorescence spectroscopy can be used to measure plasma conditions of partially ionized dopants in high energy density systems. In these experiments, K-shell vacancies in the copper dopant are created by the hotspot emission at stagnation, resulting in K-shell fluorescence at bang time. Spatially resolved copper K- α emission spectra are compared to atomic kinetics and radiation code simulations to infer density and temperature profiles. This work was supported by the US DOE under Grant No. DE-NA0001859, under the auspices of the US DOE by Lawrence Livermore National Laboratory under Contract No. DE-AC52-07NA27344, and by Los Alamos National Laboratory under contract DE-AC52-06NA52396.

  12. Quantitative Surface Analysis by Xps (X-Ray Photoelectron Spectroscopy: Application to Hydrotreating Catalysts

    Directory of Open Access Journals (Sweden)

    Beccat P.

    1999-07-01

    Full Text Available XPS is an ideal technique to provide the chemical composition of the extreme surface of solid materials, vastly applied to the study of catalysts. In this article, we will show that a quantitative approach, based upon fundamental expression of the XPS signal, has enabled us to obtain a consistent set of response factors for the elements of the periodic table. In-depth spadework has been necessary to know precisely the transmission function of the spectrometer used at IFP. The set of response factors obtained enables to perform, on a routine basis, a quantitative analysis with approximately 20% relative accuracy, which is quite acceptable for an analysis of such a nature. While using this quantitative approach, we have developed an analytical method specific to hydrotreating catalysts that allows obtaining the sulphiding degree of molybdenum quite reliably and reproducibly. The usage of this method is illustrated by two examples for which XPS spectroscopy has provided with information sufficiently accurate and quantitative to help understand the reactivity differences between certain MoS2/Al2O3 or NiMoS/Al2O3-type hydrotreating catalysts.

  13. Soft X-ray photoelectron spectroscopy of the ultrathin Ba/InGaN interface

    Science.gov (United States)

    Benemanskaya, G. V.; Pronin, V. P.; Timoshnev, S. N.; Nelyubov, A. V.

    2017-11-01

    Electronic structure of the clean In0.22Ga0.78N surface and the ultrathin Ba/In0.22Ga0.78N interface has been studied in situ by the synchrotron-based photoelectron spectroscopy during excitation in the photon energy range of 100-650 eV. Changes in the valence band and surface states spectra and in the In 3d, In 4d, N 1s, Ga 3d, Ba 4d, Ba 5p core levels spectra have been investigated under the step-by-step Ba submonolayer deposition. Changes in the surface electronic structure of the InGaN caused by Ba adsorption are found to originate predominantly from the local interaction of the Ga and In dangling bonds and Ba adatoms that results in effect of the suppression of the two intrinsic surface states and appearance of a new induced state. The Ba atomic layer deposition is revealed to induce the charge transfer between the Ba adatoms and the N surface atoms with increasing N-ionicity.

  14. Interference-free determination of ischemia-modified albumin using quantum dot coupled X-ray fluorescence spectroscopy.

    Science.gov (United States)

    Luo, Yang; Wang, Chaoming; Jiang, Tianlun; Zhang, Bo; Huang, Junfu; Liao, Pu; Fu, Weiling

    2014-01-15

    Ischemia-modified protein (IMA) is the most sensitive diagnostic biomarker of ischemic heart disease, but differentiation of IMA from human serum albumin (HSA), a ubiquitous serum protein, is still challenging owing to the shared antigenicity. In this investigation, we developed a rapid and interference-free approach for IMA determination using quantum dots-coupled X-ray Fluorescence Spectroscopy (Q-XRF). In a typical Q-XRF assay, serum total HSA is quantified using quantum dot-coupled sandwich immunoassay, and intact HSA (iHSA) is determined using a XRF spectroscopy, by measuring XRF intensity of Co (II) bonded to iHSA. IMA concentration is automatically determined within 30 min by calculating the difference between total HSA and iHSA. This strategy can effectively eliminate the interference from native HSA level. Results show that no significant influences have been observed from hemolysis or high levels of cholesterol (7 mg/L), triglyceride (5.2 mg/L), IgG (10 g/L), and fibrinogen (4 g/L). A linearity of 1-100mg/mL is obtained in iHSA determination using XRF (r(2)=0.979). The proposed Q-XRF assay demonstrates a lowest detection limit of 0.05 U/mL. Receiver-operating characteristic (ROC) curves reveal that Q-XRF assay provide an improved sensitivity than ACB assay (95.9% vs. 82.9%) in differentiating ischemic patients from health individuals, at an optimal cutoff point of 79.2U/mL. The proposed approach provides a new strategy for interference-free, simple and rapid evaluation of IMA concentration by combining sandwich immunoassay and XRF spectroscopy. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. X-ray emission spectroscopy applied to glycine adsorbed on Cu(110): An atom and symmetry projected view

    Energy Technology Data Exchange (ETDEWEB)

    Hasselstroem, J.; Karis, O.; Weinelt, M. [Uppsala Univ. (Sweden)] [and others

    1997-04-01

    When a molecule is adsorbed on a metal surface by chemical bonding new electronic states are formed. For noble and transition metals these adsorption-induced states overlap with the much more intense metal d-valence band, making them difficult to probe by for instance direct photoemission. However, it has recently been shown that X-ray emission spectroscopy (XES) can be applied to adsorbate systems. Since the intermediate state involves a core hole, this technique has the power to project out the partial density of states around each atomic site. Both the excitation and deexcitation processes are in general governed by the dipole selection rules. For oriented system, it is hence possible to obtain a complete separation into 2p{sub x}, 2p{sub y} and 2p{sub z} contributions using angular resolved measurements. The authors have applied XES together with other core level spectroscopies to glycine adsorption on Cu(110). Glycine (NH{sub 2}CH{sub 2}COOH) is the smallest amino acid and very suitable to study by core level spectroscopy since it has several functional groups, all well separated in energy by chemical shifts. Its properties are futhermore of biological interest. In summary, the authors have shown that it is possible to apply XES to more complicated molecular adsorbates. The assignment of different electronic states is however not as straight forward as for simple diatomic molecules. For a complete understanding of the redistribution and formation of new electronic states associated with the surface chemical bond, experimental data must be compared to theoretical calculations.

  16. High precision detector robot arm system

    Energy Technology Data Exchange (ETDEWEB)

    Shu, Deming; Chu, Yong

    2017-01-31

    A method and high precision robot arm system are provided, for example, for X-ray nanodiffraction with an X-ray nanoprobe. The robot arm system includes duo-vertical-stages and a kinematic linkage system. A two-dimensional (2D) vertical plane ultra-precision robot arm supporting an X-ray detector provides positioning and manipulating of the X-ray detector. A vertical support for the 2D vertical plane robot arm includes spaced apart rails respectively engaging a first bearing structure and a second bearing structure carried by the 2D vertical plane robot arm.

  17. Element Specific Versus Integral Structural and Magnetic Properties of Co:ZnO and Gd:GaN Probed with Hard X-ray Absorption Spectroscopy

    Directory of Open Access Journals (Sweden)

    Andreas Ney

    2010-06-01

    Full Text Available Dilute magnetic semiconductors (DMS are envisioned as sources of spin-polarized carriers for future semiconductor devices which simultaneously utilize spin and charge of the carriers. The hope of discovering a DMS with ferromagnetic order up to room temperature still motivates research on suitable DMS materials. Two candidate wide-band gap DMS are Gd:GaN and Co:ZnO. We have used hard X-ray absorption spectroscopy (XAS and in particular X-ray linear dichroism (XLD and X-ray magnetic circular dichroism (XMCD to study both DMS materials with element specificity and compare these findings with results from integral SQUID magnetometry as well as electron paramagnetic resonance (EPR.

  18. Unraveling the solid-liquid-vapor phase transition dynamics at the atomic level with ultrafast x-ray absorption near-edge spectroscopy.

    Science.gov (United States)

    Dorchies, F; Lévy, A; Goyon, C; Combis, P; Descamps, D; Fourment, C; Harmand, M; Hulin, S; Leguay, P M; Petit, S; Peyrusse, O; Santos, J J

    2011-12-09

    X-ray absorption near-edge spectroscopy (XANES) is a powerful probe of electronic and atomic structures in various media, ranging from molecules to condensed matter. We show how ultrafast time resolution opens new possibilities to investigate highly nonequilibrium states of matter including phase transitions. Based on a tabletop laser-plasma ultrafast x-ray source, we have performed a time-resolved (∼3  ps) XANES experiment that reveals the evolution of an aluminum foil at the atomic level, when undergoing ultrafast laser heating and ablation. X-ray absorption spectra highlight an ultrafast transition from the crystalline solid to the disordered liquid followed by a progressive transition of the delocalized valence electronic structure (metal) down to localized atomic orbitals (nonmetal-vapor), as the average distance between atoms increases.

  19. Soft x-ray absorption spectroscopy of metalloproteins and high-valent metal-complexes at room temperature using free-electron lasers.

    Science.gov (United States)

    Kubin, Markus; Kern, Jan; Gul, Sheraz; Kroll, Thomas; Chatterjee, Ruchira; Löchel, Heike; Fuller, Franklin D; Sierra, Raymond G; Quevedo, Wilson; Weniger, Christian; Rehanek, Jens; Firsov, Anatoly; Laksmono, Hartawan; Weninger, Clemens; Alonso-Mori, Roberto; Nordlund, Dennis L; Lassalle-Kaiser, Benedikt; Glownia, James M; Krzywinski, Jacek; Moeller, Stefan; Turner, Joshua J; Minitti, Michael P; Dakovski, Georgi L; Koroidov, Sergey; Kawde, Anurag; Kanady, Jacob S; Tsui, Emily Y; Suseno, Sandy; Han, Zhiji; Hill, Ethan; Taguchi, Taketo; Borovik, Andrew S; Agapie, Theodor; Messinger, Johannes; Erko, Alexei; Föhlisch, Alexander; Bergmann, Uwe; Mitzner, Rolf; Yachandra, Vittal K; Yano, Junko; Wernet, Philippe

    2017-09-01

    X-ray absorption spectroscopy at the L-edge of 3d transition metals provides unique information on the local metal charge and spin states by directly probing 3d-derived molecular orbitals through 2p-3d transitions. However, this soft x-ray technique has been rarely used at synchrotron facilities for mechanistic studies of metalloenzymes due to the difficulties of x-ray-induced sample damage and strong background signals from light elements that can dominate the low metal signal. Here, we combine femtosecond soft x-ray pulses from a free-electron laser with a novel x-ray fluorescence-yield spectrometer to overcome these difficulties. We present L-edge absorption spectra of inorganic high-valent Mn complexes (Mn ∼ 6-15 mmol/l) with no visible effects of radiation damage. We also present the