Science.gov

Sample records for x-ray spectroscopy instrumentation

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

    NASA Astrophysics Data System (ADS)

    Robert, A.; Curtis, R.; Flath, D.; Gray, A.; Sikorski, M.; Song, S.; Srinivasan, V.; Stefanescu, D.

    2013-03-01

    The X-ray Correlation Spectroscopy instrument (XCS) at the Linac Coherent Light Source (LCLS) is a dedicated instrument using coherent x-ray scattering techniques to investigate dynamics in condensed matter systems. XCS can probe both slow and ultrafast dynamics on lengthscales of interest. It employs an extensive suite of X-ray instrumentation to tailor the LCLS X-ray beam properties to experimental requirements. Results demonstrating the full transverse coherence of the LCLS beam are presented.

  2. Timepix detector at the X-ray Correlation Spectroscopy instrument at LCLS

    NASA Astrophysics Data System (ADS)

    van Bakel, N. A.; Robert, A.; Sikorski, M.; Ford, C.; van Beveren, V.; van der Heijden, B.; van Beuzekom, M.

    2013-03-01

    The Timepix detector can be operated in Time-over-Threshold mode to allow for charge integration measurements as required by short (< 50 fs) x-ray pulses of the Linac Coherent Light Source (LCLS). Initial commissioning activities have started at the X-ray Correlation Spectroscopy (XCS) instrument at LCLS, where speckle patterns have been measured.

  3. The X-ray correlation spectroscopy instrument at the Linac Coherent Light Source

    SciTech Connect

    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

    2015-03-03

    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. In addition, a description of the instrument capabilities and recent achievements is presented.

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

    PubMed Central

    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

  5. The X-ray correlation spectroscopy instrument at the Linac Coherent Light Source

    DOE PAGESBeta

    Alonso-Mori, Roberto; Caronna, Chiara; Chollet, Matthieu; Curtis, Robin; Damiani, Daniel S.; Defever, Jim; Feng, Yiping; Flath, Daniel L.; Glownia, James M.; Lee, Sooheyong; et al

    2015-03-03

    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. In addition, a description of the instrument capabilities and recent achievements is presented.

  6. Solar X-Ray Spectroscopy And Polarimetry By Instrument Ping-M Onboard Interhelioprobe

    NASA Astrophysics Data System (ADS)

    Kotov, Yury; Dergachev, Valentin; Kochemasov, Alexey; Yurov, Vitaly; Tyshkevich, V.; Glyanenko, Alexander; Savchenko, Mikhail; Lazutkov, Vadim; Skorodumov, Dmitry; Trofimov, Yury; Zakharov, Mikhail; Rubtsov, Igor; Kruglov, Evgeniy

    The instrument PING-M for X-ray spectroscopy and polarimetry of solar full disk radiation is described. It will be the part of scientific instrument set for the InterHelioProbe space mission. Instrument consists of three detectors: the Soft X-ray detector (SXRD), the Hard X-ray detector (HXRD) and Hard X-ray polarimeter (PING-P). Spectrometer SXRD is based on a relatively novel type of semiconductor detector SDD (Silicon Drift Detector) that will operate in the energy range 1.5-25 keV, which is similar to GOES X-Ray Sensor (XRS) region. Unlike GOES the SXRD is capable to measure the energy of each photon with high resolution (better 200 eV at 5.9 keV) and operate with high count rate. The X-ray spectra of solar flares obtained by the SXRD should show evidence of Fe and Fe/Ni line emission and multi-thermal plasma. HXRD operates in energy range 15-150 keV. Fast nonorganic scintillator (is based on LaBr3(Ce)) with good energy resolution (≤12% at 60keV and ≤3.5% at 662keV) is used. Apart from measurement of spectra the value of the break energy point that separates the thermal and non-thermal processes in flare would be revealed. In the talk the results of testing of laboratory models are presented. PING-P Hard X-ray polarimeter consists of active scatterer made of three organic p-terphenyl scintillators and six peripheral scattered radiation detectors made of CsI(Tl) scintillators. Effective area of polarimeter is about 5 cm2 in its energy range. Minimal measurable degree of polarization is 0.9 % for 100 sec exposition and X1 solar flare.

  7. Photon excitation for satellite free x-ray spectroscopy: Instrumentation challenges

    SciTech Connect

    Perera, R.C.C.

    1991-10-01

    First systematic study of satellites in x-ray emission spectra was performed by Deslattes using quasi-monochromatic photon excitation from a group of L{alpha} x-ray sources lying close to the K edge of Cl. He observed significant alterations in the Cl K{beta} spectrum of KCl depending on the character of the excitation radiation and identified the initial state of these satellites as a double vacancy state. Recently, the valence electronic structure of the chlorofluoromethanes were analyzed by chlorine K x-ray emission under satellite-free conditions. These studies were based on the use of synchrotron radiation to eliminate the multivacancy effects that are inherent in conventional x-ray spectroscopy. In this report, satellite free x-ray emission spectra from chlorofluoromethanes will be presented to demonstrate that the simplified spectra can be obtained using selective photon excitation. Results from various research groups world wide, utilizing the tunable photon excitation form synchrotron sources to eliminate the obscuring features in x-ray emission spectra of rare-gas solids (RGS) and metals will be discussed. Also, the technical challenges in utilizing the small phase-space attributes of high brightness from third generation SR sources producing x-ray and vacuum ultra-violet wavelengths to study weak features like satellites in x-ray emission spectra will be presented.

  8. A versatile instrument for ambient pressure x-ray photoelectron spectroscopy: The Lund cell approach

    NASA Astrophysics Data System (ADS)

    Knudsen, Jan; Andersen, Jesper N.; Schnadt, Joachim

    2016-04-01

    During the past one and a half decades ambient pressure x-ray photoelectron spectroscopy (APXPS) has grown to become a mature technique for the real-time investigation of both solid and liquid surfaces in the presence of a gas or vapour phase. APXPS has been or is being implemented at most major synchrotron radiation facilities and in quite a large number of home laboratories. While most APXPS instruments operate using a standard vacuum chamber as the sample environment, more recently new instruments have been developed which focus on the possibility of custom-designed sample environments with exchangeable ambient pressure cells (AP cells). A particular kind of AP cell solution has been driven by the development of the APXPS instrument for the SPECIES beamline of the MAX IV Laboratory: the solution makes use of a moveable AP cell which for APXPS measurements is docked to the electron energy analyser inside the ultrahigh vacuum instrument. Only the inner volume of the AP cell is filled with gas, while the surrounding vacuum chamber remains under vacuum conditions. The design enables the direct connection of UHV experiments to APXPS experiments, and the swift exchange of AP cells allows different custom-designed sample environments. Moreover, the AP cell design allows the gas-filled inner volume to remain small, which is highly beneficial for experiments in which fast gas exchange is required. Here we report on the design of several AP cells and use a number of cases to exemplify the utility of our approach.

  9. The MIT high resolution X-ray spectroscopy instruments on AXAF

    NASA Astrophysics Data System (ADS)

    Canizares, C. R.; Dewey, D.; Galton, E. B.; Markert, T. H.; Smith, Henry I.; Schattenburg, M. L.; Woodgate, B. E.; Jordan, S.

    1992-03-01

    The general design and performance characteristics of MIT's two dispersive spectrometers, the Bragg Crystal Spectrometer (BCS) and the High Energy Transmission Grating Spectrometer (HETG), now being developed for the Advanced X-ray Astrophysics Facility (AXAF), are described. Particular attention is given to the development of the critical technologies incorporated into these instruments, including BCS diffractors, imaging gas flow proportional counters, and grating elements for the HETG. The principal stages and the current status of the developments are reviewed.

  10. A laser-based instrument for the study of ultrafast chemical dynamics by soft x-ray-probe photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Nugent-Glandorf, Lora; Scheer, Michael; Samuels, David A.; Bierbaum, Veronica; Leone, Stephen R.

    2002-04-01

    A laser-based instrument is described for the study of femtosecond dissociation dynamics of gas phase molecules via time-resolved vacuum ultraviolet and soft x-ray photoelectron spectroscopy. Visible or UV pump pulses are generated with nonlinear crystal techniques on a Ti:sapphire laser output, while soft x-ray probe pulses are created via high-order harmonic generation of the same laser in rare gases. Here we describe the optical layout of the pump-probe system, the means for separation of the high-order harmonics in the soft x-ray probe beam, including a description of the two grating setup used to compress the high-harmonic pulses and the magnetic bottle photoelectron spectrometer used for data collection. The feasibility of using the generated high-harmonic pulses for an array of gaseous phase photoelectron spectroscopy experiments is established. These include measurements of valence shell and core-level photoelectron transitions in atoms and molecules, the tunability of the soft x-ray harmonic through Rydberg resonances, and the energy bandwidths of the harmonics. Cross correlations between the visible/UV and soft x-ray pulses, by above threshold ionization, are used to establish the pulse timing, pulse duration, and spatial overlap for ultrafast studies. The observed real time photodissociation of Br2 serves as a demonstration of the pump-probe ultrafast technique and the applicability to ultrafast time-resolved chemical dynamics.

  11. X-ray Absorption Spectroscopy

    SciTech Connect

    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.

  12. Tokamak x ray diagnostic instrumentation

    SciTech Connect

    Hill, K.W.; Beiersdorfer, P.; Bitter, M.; Fredrickson, E.; Von Goeler, S.; Hsuan, H.; Johnson, L.C.; Liew, S.L.; McGuire, K.; Pare, V.

    1987-01-01

    Three classes of x-ray diagnostic instruments enable measurement of a variety of tokamak physics parameters from different features of the x-ray emission spectrum. (1) The soft x-ray (1 to 50 keV) pulse-height-analysis (PHA) diagnostic measures impurity concentrations from characteristic line intensities and the continuum enhancement, and measures the electron temperature from the continuum slope. (2) The Bragg x-ray crystal spectrometer (XCS) measures the ion temperature and neutral-beam-induced toroidal rotation velocity from the Doppler broadening and wavelength shift, respectively, of spectral lines of medium-Z impurity ions. Impurity charge state distributions, precise wavelengths, and inner-shell excitation and recombination rates can also be studied. X rays are diffracted and focused by a bent crystal onto a position-sensitive detector. The spectral resolving power E/..delta..E is greater than 10/sup 4/ and time resolution is 10 ms. (3) The x-ray imaging system (XIS) measures the spatial structure of rapid fluctuations (0.1 to 100 kHZ) providing information on MHD phenomena, impurity transport rates, toroidal rotation velocity, plasma position, and the electron temperature profile. It uses an array of silicon surface-barrier diodes which view different chords of the plasma through a common slot aperture and operate in current (as opposed to counting) mode. The effectiveness of shields to protect detectors from fusion-neutron radiation effects has been studied both theoretically and experimentally.

  13. X-ray Echo Spectroscopy.

    PubMed

    Shvyd'ko, Yuri

    2016-02-26

    X-ray echo spectroscopy, a counterpart of neutron spin echo, is being introduced here to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a pointlike x-ray source is defocused by a dispersing system comprised of asymmetrically cut specially arranged Bragg diffracting crystals. The defocused image is refocused into a point (echo) in a time-reversal dispersing system. If the defocused beam is inelastically scattered from a sample, the echo signal acquires a spatial distribution, which is a map of the inelastic scattering spectrum. The spectral resolution of the echo spectroscopy does not rely on the monochromaticity of the x rays, ensuring strong signals along with a very high spectral resolution. Particular schemes of x-ray echo spectrometers for 0.1-0.02 meV ultrahigh-resolution IXS applications (resolving power >10^{8}) with broadband ≃5-13  meV dispersing systems are introduced featuring more than 10^{3} signal enhancement. The technique is general, applicable in different photon frequency domains. PMID:26967404

  14. X-ray Echo Spectroscopy.

    PubMed

    Shvyd'ko, Yuri

    2016-02-26

    X-ray echo spectroscopy, a counterpart of neutron spin echo, is being introduced here to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a pointlike x-ray source is defocused by a dispersing system comprised of asymmetrically cut specially arranged Bragg diffracting crystals. The defocused image is refocused into a point (echo) in a time-reversal dispersing system. If the defocused beam is inelastically scattered from a sample, the echo signal acquires a spatial distribution, which is a map of the inelastic scattering spectrum. The spectral resolution of the echo spectroscopy does not rely on the monochromaticity of the x rays, ensuring strong signals along with a very high spectral resolution. Particular schemes of x-ray echo spectrometers for 0.1-0.02 meV ultrahigh-resolution IXS applications (resolving power >10^{8}) with broadband ≃5-13  meV dispersing systems are introduced featuring more than 10^{3} signal enhancement. The technique is general, applicable in different photon frequency domains.

  15. Technology development for soft X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    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.

  16. Large Area X-ray Spectroscopy Mission

    NASA Technical Reports Server (NTRS)

    Tananbaum, Harvey

    1996-01-01

    The Large Area X-ray Spectroscopy (LAXS) mission study concept has evolved strongly over the last year culminating in the merging of LAXS with the Goddard Space Flight Center (GSFC) proposal for a similar mission, the Next Generation X-ray Observatory (NGXO, PI: Nick White). The resulting merger, re-named the High Throughput X-rays Spectroscopy (HTXS) Mission has also expanded by the inclusion of another SAO proposed new mission concept proposal, the Hard X-Ray Telescope (PI: Paul Gorenstein). The resultant multi-instrument mission retains much of heritage from the LAXS proposal, including the use of multiple satellites for robustness. These mergers resulted from a series of contacts between various team members, via e-mail, telecons, and in-person meetings. The impetus for the mergers was the fundamental similarity between the missions, and the recognition that all three proposal teams had significant contributions to make in the effort to define the next stage in the X-ray exploration of the universe. We have enclosed four items that represent some of the work that has occurred during the first year of the study: first, a presentation at the Leicester meeting, second a presentation that was made to Dan Goldin following the merging of LAXS and NGXO, third a copy of the first announcement for the Workshop, and finally the interim report that was prepared by the HTXS study team towards the end of the first year. This last document provides the foundation for the HTXS Technology Roadmap that is being generated. The HTXS roadmap will define the near-term goals that the merged mission must achieve over the next few years. A web site has been developed and populated that contains much of the material that has been generated over the past year.

  17. X-ray Spectroscopy of Cooling Cluster

    SciTech Connect

    Peterson, J.R.; 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.

  18. MSL Chemistry and Mineralogy X-ray Diffraction X-ray Fluorescence (CheMin) Instrument

    NASA Astrophysics Data System (ADS)

    Zimmerman, W.; Blake, D.; Harris, W.; Morookian, J. M.; Randall, D.; Reder, L. J.; Sarrazin, P.

    This paper provides an overview of the Mars Science Laboratory (MSL) Chemistry and Mineralogy X-ray Diffraction (XRD), X-ray Fluorescence (XRF) (CheMin) Instrument, an element of the landed Curiosity rover payload, which landed on Mars in August of 2012. The scientific goal of the MSL mission is to explore and quantitatively assess regions in Gale Crater as a potential habitat for life - past or present. The CheMin instrument will receive Martian rock and soil samples from the MSL Sample Acquisition/Sample Processing and Handling (SA/SPaH) system, and process it utilizing X-Ray spectroscopy methods to determine mineral composition. The Chemin instrument will analyze Martian soil and rocks to enable scientists to investigate geophysical processes occurring on Mars. The CheMin science objectives and proposed surface operations are described along with the CheMin hardware with an emphasis on the system engineering challenges associated with developing such a complex instrument.

  19. Soft X-Ray Absorption Spectroscopy at an X-ray Free Electron Laser

    NASA Astrophysics Data System (ADS)

    Higley, Daniel; Schlotter, William; Turner, Joshua; Moeller, Stefan; Mitra, Ankush; Tsukamoto, Arata; Marvel, Robert; Haglund, Richard; Durr, Hermann; Stohr, Joachim; Dakovski, Georgi

    2015-03-01

    X-ray free electron lasers, providing coherent, ultrafast, high intensity x-ray pulses, have enabled groundbreaking scattering experiments to probe the atomic structure of materials on femtosecond timescales. Nonetheless, x-ray absorption spectroscopy (XAS), one of the most fundamental and common x-ray techniques practiced at synchrotron light sources, has proven challenging to conduct with satisfactory signal-to-noise levels at soft x-ray energies using free electron laser sources. The ability to routinely collect high quality XAS spectra, especially in a time-resolved manner, will open many new scientific possibilities in the areas of ultrafast demagnetization, phase transitions and chemical dynamics to highlight a few. Here, we report how XAS using total fluorescence yield detection yields high signal-to-noise x-ray absorption spectra at an x-ray free electron laser source. Data were collected over multiple absorption edges on technologically relevant materials. These measurements were recorded on the Soft X-Ray Materials Science instrument at the Linac Coherent Light Source. The results are easily extendable to time-resolved measurements.

  20. Large Area X-Ray Spectroscopy Mission

    NASA Technical Reports Server (NTRS)

    Tananbaum, H.

    1997-01-01

    The Large Area X-ray Spectroscopy (LAXS) mission concept study continues to evolve strongly following the merging of the LAXS mission with the Next Generation X-ray Observatory (NGXO, PI: Nick White) into the re-named High Throughput X-ray Spectroscopy (HTXS) Mission. HTXS retains key elements of the LAXS proposal, including the use of multiple satellites for risk-reduction and cost savings. A key achievement of the program has been the recommendation by the Structure and Evolution of the Universe (SEUS) (April 1997) for a new start for the HTXS mission in the 2000-2004 timeframe.

  1. European XFEL: Soft X-Ray instrumentation

    SciTech Connect

    Molodtsov, S. L.

    2011-12-15

    The currently constructed European X-Ray Free Electron Laser (XFEL) will generate new knowledge in almost all the technical and scientific disciplines that are shaping our daily life-including nanotechnology, medicine, pharmaceutics, chemistry, materials science, power engineering and electronics. On 8 January 2009, civil engineering work (tunnels, shafts, halls) has been started at all three construction sites. In this presentation status and parameters of the European XFEL facility and instrumentation as well as planned research applications particularly in the range of soft X-rays are reviewed.

  2. MSL Chemistry and Mineralogy X-Ray Diffraction X-Ray Fluorescence (CheMin) Instrument

    NASA Technical Reports Server (NTRS)

    Zimmerman, Wayne; Blake, Dave; Harris, William; Morookian, John Michael; Randall, Dave; Reder, Leonard J.; Sarrazin, Phillipe

    2013-01-01

    This paper provides an overview of the Mars Science Laboratory (MSL) Chemistry and Mineralogy Xray Diffraction (XRD), X-ray Fluorescence (XRF) (CheMin) Instrument, an element of the landed Curiosity rover payload, which landed on Mars in August of 2012. The scientific goal of the MSL mission is to explore and quantitatively assess regions in Gale Crater as a potential habitat for life - past or present. The CheMin instrument will receive Martian rock and soil samples from the MSL Sample Acquisition/Sample Processing and Handling (SA/SPaH) system, and process it utilizing X-Ray spectroscopy methods to determine mineral composition. The Chemin instrument will analyze Martian soil and rocks to enable scientists to investigate geophysical processes occurring on Mars. The CheMin science objectives and proposed surface operations are described along with the CheMin hardware with an emphasis on the system engineering challenges associated with developing such a complex instrument.

  3. X-ray absorption spectroscopy of metalloproteins.

    PubMed

    Ward, Jesse; Ollmann, Emily; Maxey, Evan; Finney, Lydia A

    2014-01-01

    Metalloproteins are enormously important in biology. While a variety of techniques exist for studying metals in biology, X-ray absorption spectroscopy is particularly useful in that it can determine the local electronic and physical structure around the metal center, and is one of the few avenues for studying "spectroscopically silent" metal ions like Zn(II) and Cu(I) that have completely filled valence bands. While X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) are useful for studying metalloprotein structure, they suffer the limitation that the detected signal is an average of all the various metal centers in the sample, which limits its usefulness for studying metal centers in situ or in cell lysates. It would be desirable to be able to separate the various proteins in a mixture prior to performing X-ray absorption studies, so that the derived signal is from one species only. Here we describe a method for performing X-ray absorption spectroscopy on protein bands following electrophoretic separation and western blotting.

  4. X-ray spectroscopy: Enlightened state

    NASA Astrophysics Data System (ADS)

    McCusker, James K.

    2014-07-01

    Determining the sequence of events following photon absorption by a molecule can be a surprisingly challenging task. An innovative use of time-resolved X-ray spectroscopy has revealed an important insight into the ultrafast excited-state dynamics of a well-known inorganic chromophore.

  5. A laboratory-based hard x-ray monochromator for high-resolution x-ray emission spectroscopy and x-ray absorption near edge structure measurements

    SciTech Connect

    Seidler, G. T. Mortensen, D. R.; Remesnik, A. J.; Pacold, J. I.; Ball, N. A.; Barry, N.; Styczinski, M.; Hoidn, O. R.

    2014-11-15

    We report the development of a laboratory-based Rowland-circle monochromator that incorporates a low power x-ray (bremsstrahlung) tube source, a spherically bent crystal analyzer, and an energy-resolving solid-state detector. This relatively inexpensive, introductory level instrument achieves 1-eV energy resolution for photon energies of ∼5 keV to ∼10 keV while also demonstrating a net efficiency previously seen only in laboratory monochromators having much coarser energy resolution. Despite the use of only a compact, air-cooled 10 W x-ray tube, we find count rates for nonresonant x-ray emission spectroscopy comparable to those achieved at monochromatized spectroscopy beamlines at synchrotron light sources. For x-ray absorption near edge structure, the monochromatized flux is small (due to the use of a low-powered x-ray generator) but still useful for routine transmission-mode studies of concentrated samples. These results indicate that upgrading to a standard commercial high-power line-focused x-ray tube or rotating anode x-ray generator would result in monochromatized fluxes of order 10{sup 6}–10{sup 7} photons/s with no loss in energy resolution. This work establishes core technical capabilities for a rejuvenation of laboratory-based hard x-ray spectroscopies that could have special relevance for contemporary research on catalytic or electrical energy storage systems using transition-metal, lanthanide, or noble-metal active species.

  6. A laboratory-based hard x-ray monochromator for high-resolution x-ray emission spectroscopy and x-ray absorption near edge structure measurements

    NASA Astrophysics Data System (ADS)

    Seidler, G. T.; Mortensen, D. R.; Remesnik, A. J.; Pacold, J. I.; Ball, N. A.; Barry, N.; Styczinski, M.; Hoidn, O. R.

    2014-11-01

    We report the development of a laboratory-based Rowland-circle monochromator that incorporates a low power x-ray (bremsstrahlung) tube source, a spherically bent crystal analyzer, and an energy-resolving solid-state detector. This relatively inexpensive, introductory level instrument achieves 1-eV energy resolution for photon energies of ˜5 keV to ˜10 keV while also demonstrating a net efficiency previously seen only in laboratory monochromators having much coarser energy resolution. Despite the use of only a compact, air-cooled 10 W x-ray tube, we find count rates for nonresonant x-ray emission spectroscopy comparable to those achieved at monochromatized spectroscopy beamlines at synchrotron light sources. For x-ray absorption near edge structure, the monochromatized flux is small (due to the use of a low-powered x-ray generator) but still useful for routine transmission-mode studies of concentrated samples. These results indicate that upgrading to a standard commercial high-power line-focused x-ray tube or rotating anode x-ray generator would result in monochromatized fluxes of order 106-107 photons/s with no loss in energy resolution. This work establishes core technical capabilities for a rejuvenation of laboratory-based hard x-ray spectroscopies that could have special relevance for contemporary research on catalytic or electrical energy storage systems using transition-metal, lanthanide, or noble-metal active species.

  7. X-ray resonant Raman spectroscopy

    SciTech Connect

    Cowan, P.L.; LeBrun, T.; Deslattes, R.D.

    1995-08-01

    X-ray resonant Raman scattering presents great promise as a high-resolution spectroscopic probe of the electronic structure of matter. Unlike other methods, the technique avoids the loss of energy resolution resulting from the lifetime broadening of short-lived core-excited states. In addition, measurements of polarization and angular anisotropies yield information on the symmetries of electronic states of atoms and molecules. We studied the L{sub 3} edge of xenon, where the lifetime broadening is a major feature of the spectra recorded previously. X-ray fluorescence spectra were taken of both the L{alpha}{sub l,2} and L{beta}{sub 2,15} peaks over a range of energies from 10 eV below the edge to 40 eV above. These spectra show the evolution of resonant Raman scattering into characteristic fluorescence as the photon energy is scanned across the edge, and confirm several features of these spectra such as asymmetries in resonant peak shapes due to the onset of the ionization continuum. These results constitute the most comprehensive study of X-ray resonant Raman scattering to date, and were submitted for publication. Studies of other cases are under way, and new instruments that would match the unique characteristics of the APS - and thus render a new range of experiments possible - are under consideration.

  8. X-ray diffraction: instrumentation and applications.

    PubMed

    Bunaciu, Andrei A; Udriştioiu, Elena Gabriela; Aboul-Enein, Hassan Y

    2015-01-01

    X-ray diffraction (XRD) is a powerful nondestructive technique for characterizing crystalline materials. It provides information on structures, phases, preferred crystal orientations (texture), and other structural parameters, such as average grain size, crystallinity, strain, and crystal defects. X-ray diffraction peaks are produced by constructive interference of a monochromatic beam of X-rays scattered at specific angles from each set of lattice planes in a sample. The peak intensities are determined by the distribution of atoms within the lattice. Consequently, the X-ray diffraction pattern is the fingerprint of periodic atomic arrangements in a given material. This review summarizes the scientific trends associated with the rapid development of the technique of X-ray diffraction over the past five years pertaining to the fields of pharmaceuticals, forensic science, geological applications, microelectronics, and glass manufacturing, as well as in corrosion analysis.

  9. Laser plasma x-ray source for ultrafast time-resolved x-ray absorption spectroscopy.

    PubMed

    Miaja-Avila, L; O'Neil, G C; Uhlig, J; Cromer, C L; Dowell, M L; Jimenez, R; Hoover, A S; Silverman, K L; Ullom, J N

    2015-03-01

    We describe a laser-driven x-ray plasma source designed for ultrafast x-ray absorption spectroscopy. The source is comprised of a 1 kHz, 20 W, femtosecond pulsed infrared laser and a water target. We present the x-ray spectra as a function of laser energy and pulse duration. Additionally, we investigate the plasma temperature and photon flux as we vary the laser energy. We obtain a 75 μm FWHM x-ray spot size, containing ∼10(6) photons/s, by focusing the produced x-rays with a polycapillary optic. Since the acquisition of x-ray absorption spectra requires the averaging of measurements from >10(7) laser pulses, we also present data on the source stability, including single pulse measurements of the x-ray yield and the x-ray spectral shape. In single pulse measurements, the x-ray flux has a measured standard deviation of 8%, where the laser pointing is the main cause of variability. Further, we show that the variability in x-ray spectral shape from single pulses is low, thus justifying the combining of x-rays obtained from different laser pulses into a single spectrum. Finally, we show a static x-ray absorption spectrum of a ferrioxalate solution as detected by a microcalorimeter array. Altogether, our results demonstrate that this water-jet based plasma source is a suitable candidate for laboratory-based time-resolved x-ray absorption spectroscopy experiments. PMID:26798792

  10. Laser plasma x-ray source for ultrafast time-resolved x-ray absorption spectroscopy

    DOE PAGESBeta

    Miaja-Avila, L.; O'Neil, G. C.; Uhlig, J.; Cromer, C. L.; Dowell, M. L.; Jimenez, R.; Hoover, A. S.; Silverman, K. L.; Ullom, J. N.

    2015-03-02

    We describe a laser-driven x-ray plasma source designed for ultrafast x-ray absorption spectroscopy. The source is comprised of a 1 kHz, 20 W, femtosecond pulsed infrared laser and a water target. We present the x-ray spectra as a function of laser energy and pulse duration. Additionally, we investigate the plasma temperature and photon flux as we vary the laser energy. We obtain a 75 μm FWHM x-ray spot size, containing ~106 photons/s, by focusing the produced x-rays with a polycapillary optic. Since the acquisition of x-ray absorption spectra requires the averaging of measurements from >107 laser pulses, we also presentmore » data on the source stability, including single pulse measurements of the x-ray yield and the x-ray spectral shape. In single pulse measurements, the x-ray flux has a measured standard deviation of 8%, where the laser pointing is the main cause of variability. Further, we show that the variability in x-ray spectral shape from single pulses is low, thus justifying the combining of x-rays obtained from different laser pulses into a single spectrum. Finally, we show a static x-ray absorption spectrum of a ferrioxalate solution as detected by a microcalorimeter array. Altogether, our results demonstrate that this water-jet based plasma source is a suitable candidate for laboratory-based time-resolved x-ray absorption spectroscopy experiments.« less

  11. Laser plasma x-ray source for ultrafast time-resolved x-ray absorption spectroscopy.

    PubMed

    Miaja-Avila, L; O'Neil, G C; Uhlig, J; Cromer, C L; Dowell, M L; Jimenez, R; Hoover, A S; Silverman, K L; Ullom, J N

    2015-03-01

    We describe a laser-driven x-ray plasma source designed for ultrafast x-ray absorption spectroscopy. The source is comprised of a 1 kHz, 20 W, femtosecond pulsed infrared laser and a water target. We present the x-ray spectra as a function of laser energy and pulse duration. Additionally, we investigate the plasma temperature and photon flux as we vary the laser energy. We obtain a 75 μm FWHM x-ray spot size, containing ∼10(6) photons/s, by focusing the produced x-rays with a polycapillary optic. Since the acquisition of x-ray absorption spectra requires the averaging of measurements from >10(7) laser pulses, we also present data on the source stability, including single pulse measurements of the x-ray yield and the x-ray spectral shape. In single pulse measurements, the x-ray flux has a measured standard deviation of 8%, where the laser pointing is the main cause of variability. Further, we show that the variability in x-ray spectral shape from single pulses is low, thus justifying the combining of x-rays obtained from different laser pulses into a single spectrum. Finally, we show a static x-ray absorption spectrum of a ferrioxalate solution as detected by a microcalorimeter array. Altogether, our results demonstrate that this water-jet based plasma source is a suitable candidate for laboratory-based time-resolved x-ray absorption spectroscopy experiments.

  12. Laser plasma x-ray source for ultrafast time-resolved x-ray absorption spectroscopy

    SciTech Connect

    Miaja-Avila, L.; O'Neil, G. C.; Uhlig, J.; Cromer, C. L.; Dowell, M. L.; Jimenez, R.; Hoover, A. S.; Silverman, K. L.; Ullom, J. N.

    2015-03-02

    We describe a laser-driven x-ray plasma source designed for ultrafast x-ray absorption spectroscopy. The source is comprised of a 1 kHz, 20 W, femtosecond pulsed infrared laser and a water target. We present the x-ray spectra as a function of laser energy and pulse duration. Additionally, we investigate the plasma temperature and photon flux as we vary the laser energy. We obtain a 75 μm FWHM x-ray spot size, containing ~106 photons/s, by focusing the produced x-rays with a polycapillary optic. Since the acquisition of x-ray absorption spectra requires the averaging of measurements from >107 laser pulses, we also present data on the source stability, including single pulse measurements of the x-ray yield and the x-ray spectral shape. In single pulse measurements, the x-ray flux has a measured standard deviation of 8%, where the laser pointing is the main cause of variability. Further, we show that the variability in x-ray spectral shape from single pulses is low, thus justifying the combining of x-rays obtained from different laser pulses into a single spectrum. Finally, we show a static x-ray absorption spectrum of a ferrioxalate solution as detected by a microcalorimeter array. Altogether, our results demonstrate that this water-jet based plasma source is a suitable candidate for laboratory-based time-resolved x-ray absorption spectroscopy experiments.

  13. Laser plasma x-ray source for ultrafast time-resolved x-ray absorption spectroscopy

    PubMed Central

    Miaja-Avila, L.; O'Neil, G. C.; Uhlig, J.; Cromer, C. L.; Dowell, M. L.; Jimenez, R.; Hoover, A. S.; Silverman, K. L.; Ullom, J. N.

    2015-01-01

    We describe a laser-driven x-ray plasma source designed for ultrafast x-ray absorption spectroscopy. The source is comprised of a 1 kHz, 20 W, femtosecond pulsed infrared laser and a water target. We present the x-ray spectra as a function of laser energy and pulse duration. Additionally, we investigate the plasma temperature and photon flux as we vary the laser energy. We obtain a 75 μm FWHM x-ray spot size, containing ∼106 photons/s, by focusing the produced x-rays with a polycapillary optic. Since the acquisition of x-ray absorption spectra requires the averaging of measurements from >107 laser pulses, we also present data on the source stability, including single pulse measurements of the x-ray yield and the x-ray spectral shape. In single pulse measurements, the x-ray flux has a measured standard deviation of 8%, where the laser pointing is the main cause of variability. Further, we show that the variability in x-ray spectral shape from single pulses is low, thus justifying the combining of x-rays obtained from different laser pulses into a single spectrum. Finally, we show a static x-ray absorption spectrum of a ferrioxalate solution as detected by a microcalorimeter array. Altogether, our results demonstrate that this water-jet based plasma source is a suitable candidate for laboratory-based time-resolved x-ray absorption spectroscopy experiments. PMID:26798792

  14. Miniaturization in x ray and gamma ray spectroscopy

    NASA Technical Reports Server (NTRS)

    Iwanczyk, Jan S.; Wang, Yuzhong J.; Bradley, James G.

    1993-01-01

    The paper presents advances in two new sensor technologies and a miniaturized associated electronics technology which, when combined, can allow for very significant miniaturization and for the reduction of weight and power consumption in x-ray and gamma-ray spectroscopy systems: (1) Mercuric iodide (HgI2) x-ray technology, which allows for the first time the construction of truly portable, high-energy resolution, non-cryogenic x-ray fluorescence (XRF) elemental analyzer systems, with parameters approaching those of laboratory quality cryogenic instruments; (2) the silicon avalanche photodiode (APD), which is a solid-state light sensitive device with internal amplification, capable of uniquely replacing the vacuum photomultiplier tube in scintillation gamma-ray spectrometer applications, and offering substantial improvements in size, ruggedness, low power operation and energy resolution; and (3) miniaturized (hybridized) low noise, low power amplification and processing electronics, which take full advantage of the favorable properties of these new sensors and allow for the design and fabrication of advanced, highly miniaturized x-ray and gamma-ray spectroscopy systems. The paper also presents experimental results and examples of spectrometric systems currently under construction. The directions for future developments are discussed.

  15. X-ray microprobe for micro x-ray fluorescence and absorption spectroscopies at GSECARS

    NASA Astrophysics Data System (ADS)

    Newville, M.; Sutton, S.; Rivers, M.

    2002-12-01

    The hard x-ray microprobe for x-ray fluorescence and absorption spectroscopy at GeoSoilEnviroCARS is presented. Using focused synchrotron radiation from an undulator beamline at the Advanced Photon Source at Argonne National Lab, the x-ray microprobe provides bright, monochromatic x-rays with typical spot sizes down to 1x1 μm for x-ray fluorescence and absorption spectroscopies. Quantitative x-ray fluorescence (XRF) analysis gives precise elemental composition and correlations, while x-ray absorption spectroscopy (XAS) gives the chemical state and local atomic coordination for a selected atomic species. These two techniques can be used in conjunction with one another on a wide range of samples, including minerals, glasses, fluid inclusions, soils, sediments, and plant tissue. This x-ray microprobe is part of the GeoSoilEnviroCARS user facility, available for use in all areas geological, soil, and environmental sciences, and selected examples from these fields will be given.

  16. Nonlinear X-Ray and Auger Spectroscopy at X-Ray Free-Electron Laser Sources

    NASA Astrophysics Data System (ADS)

    Rohringer, Nina

    2015-05-01

    X-ray free-electron lasers (XFELs) open the pathway to transfer non-linear spectroscopic techniques to the x-ray domain. A promising all x-ray pump probe technique is based on coherent stimulated electronic x-ray Raman scattering, which was recently demonstrated in atomic neon. By tuning the XFEL pulse to core-excited resonances, a few seed photons in the spectral tail of the XFEL pulse drive an avalanche of resonant inelastic x-ray scattering events, resulting in exponential amplification of the scattering signal by of 6-7 orders of magnitude. Analysis of the line profile of the emitted radiation permits to demonstrate the cross over from amplified spontaneous emission to coherent stimulated resonance scattering. In combination with statistical covariance mapping, a high-resolution spectrum of the resonant inelastic scattering process can be obtained, opening the path to coherent stimulated x-ray Raman spectroscopy. An extension of these ideas to molecules and a realistic feasibility study of stimulated electronic x-ray Raman scattering in CO will be presented. Challenges to realizing stimulated electronic x-ray Raman scattering at present-day XFEL sources will be discussed, corroborated by results of a recent experiment at the LCLS XFEL. Due to the small gain cross section in molecular targets, other nonlinear spectroscopic techniques such as nonlinear Auger spectroscopy could become a powerful alternative. Theory predictions of a novel pump probe technique based on resonant nonlinear Auger spectroscopic will be discussed and the method will be compared to stimulated x-ray Raman spectroscopy.

  17. X-ray photoelectron spectroscopy peak assignment for perfluoropolyether oils

    NASA Technical Reports Server (NTRS)

    Mori, Shigeyuki; Morales, Wilfredo

    1990-01-01

    Perfluoroalkylpolyether (PFPE) oils are increasingly being used as vacuum pump oils and as lubricants for magnetic recording media and instrumentation for satellites. In this paper, the relative binding energies of three PFPE oils are determined. When sample oils are continuously irradiated during X-ray spectroscopy (XPS) measurements, the relative peak intensity of the spectra is altered significantly, indicating that gaseous products form from the oils during XPS measurements. Thus, attention should be paid to chemical changes when XPE is used to characterize fluorinated carbons such as PFPE oils.

  18. Current Problems in X-Ray Emission Spectroscopy

    NASA Technical Reports Server (NTRS)

    Goldstein, Joseph I.; Williams, David B.; Lyman, Charles E.

    1989-01-01

    Various problems that limit X-ray analysis in the analytical electron microscope are reviewed. Major emphasis is given to the trade-off between minimum mass fraction and spatial resolution. New developments such as high-brightness electron guns, new X-ray spectrometers and clean high-vacuum analysis conditions will lead to major improvements in the accuracy and detectability limits of X-ray emission spectroscopy.

  19. X-ray astronomy instrumentation studies

    NASA Astrophysics Data System (ADS)

    Gregory, J. C.

    1981-11-01

    Preliminary designs were made for a multiplane, multiwire position sensitive proportional counter for X-ray use. Anode spacing was 2 mm and cathode spacing 1 mm. Assistance was provided in setting up and operating two multiwire proportional counters, one with 5 mm anode spacing, and the other with 2 mm spacing. Argon-based counter gases were used for preliminary work in assembling a working experimental system to measure xenon fluorescence yields. The design and specification of a high purity gas filling system capable of supplying mixtures of xenon and other gases to proportional counters was also performed. The system is mounted on a cart, is fully operational, and is flexible enough to be easily used as a pumping station for other clean applications. When needed, assistance was given to put into operation various computer-related pieces of equipment.

  20. Crystals for astronomical X-ray spectroscopy

    NASA Technical Reports Server (NTRS)

    Burek, A.

    1976-01-01

    Crystal spectrometric properties and the factors that affect their measurement are discussed. Theoretical and experimental results on KAP are summarized and theoretical results based on the dynamical theory of X-ray diffraction are given for the acid phthalates as well as for the commonly used planes of ADP, PET and EDDT. Anomalous dispersion is found to be important for understanding the details of crystal Bragg reflection properties at long X-ray wavelengths and some important effects are pointed out. The theory of anomalous dispersion is applied to explain the anomalous reflectivity exhibited by KAP at 23.3 A.

  1. XEUS: The x-ray evolving universe spectroscopy mission

    NASA Astrophysics Data System (ADS)

    Parmar, A. N.; Arnaud, M.; Barcons, X.; Bleeker, J.; Hasinger, G.; Kunieda, H.; Palumbo, G.; Takahashi, T.; Turner, M.; de Korte, P.; Willingale, R.; Rando, N.; Lyngvi, A.; Gondoin, P.; Lumb, D.; Bavdaz, M.; Verhoeve, P.

    2006-06-01

    XEUS is the potential successor to ESA's XMM-Newton X-ray observatory and is being proposed in response to the Cosmic Vision 2015-2025 long term plan for ESA's Science Programme. Novel light-weight optics with an effective area of 5 m2 at 1 keV and 2 m2 at 7 keV and 2-5" HEW spatial resolution together with advanced detectors will provide much improved imaging, spectroscopic and timing performances and open new vistas in X-ray astronomy in the post 2015 timeframe. XEUS will allow the study of the birth, growth and spin of the super-massive black holes in early AGN, allow the cosmic feedback between galaxies and their environment to be investigated through the study of inflows and outflows and relativistic acceleration and allow the growth of large scale structures and metal synthesis to be probed using the hot X-ray emitting gas in clusters of galaxies and the warm/hot filamentary structures observable with X-ray absorption spectroscopy. High time resolution studies will allow the Equation of State of supra-nuclear material in neutron stars to be constrained. These science goals set very demanding requirements on the mission design which is based on two formation flying spacecraft launched to the second Earth-Sun Lagrangian point by an Ariane V ECA. One spacecraft will contain the novel high performance optics while the other, separated by the 35 m focal length, will contain narrow and wide field imaging spectrometers and other specialized instruments.

  2. Hard X-ray Pump, X-ray Probe Spectroscopy of Single Crystals

    NASA Astrophysics Data System (ADS)

    Loether, Aaron; Decamp, Matt; Walko, Donald

    Recent advancements in intense x-ray pulses have made it possible to perform hard x-ray pump probe spectroscopy. Inspired by optical pump probe, we've built a retroreflector for use with synchrotron based x-rays, using Germanium crystals at Bragg condition in place of mirrors, to control relative timing of x-ray pulses and perform time resolved measurements. Testing of multiple versions of the retroreflector was done both experimentally and via simulation; the comparison allows us to show efficiencies achievable theoretically and realistically. A proof of concept time resolved diffraction experiment on a Germanium 111 crystal was performed utilizing high intensity broadband x-ray pulses and the resulting heating and propagated strains were measured by low intensity monochromatic x-ray pulses. This work was supported from the DOE-EPSCoR Grant No. DE-FG02-11ER46816. Use of the 178 Advanced Photon Source was supported by the U. S. Department of Energy, Office of Science, 179 Office of Basic Energy Sciences, under Contract No. DE-AC02-06CH11357.

  3. Beyond hard x-ray photoelectron spectroscopy: Simultaneous combination with x-ray diffraction

    SciTech Connect

    Rubio-Zuazo, Juan; Castro, German R.

    2013-05-15

    Hard x-ray photoelectron spectroscopy (HAXPES) is a powerful and novel emerging technique for the nondestructive determination of electronic properties and chemical composition of bulk, buried interfaces and surfaces. It benefits from the exceptionally large escape depth of high kinetic energy photoelectrons, increasing the information depth up to several tens of nanometers. Complementing HAXPES with an atomic structure sensitive technique (such as x-ray diffraction) opens a new research field with major applications for materials science. At SpLine, the Spanish CRG beamline at the European Synchrotron Radiation Facility, we have developed a novel experimental set-up that combines HAXPES and x-ray diffraction (x-ray reflectivity, surface x-ray diffraction, grazing incidence x-ray diffraction, and reciprocal space maps). Both techniques can be operated simultaneously on the same sample and using the same excitation source. The set-up includes a robust 2S + 3D diffractometer hosting a ultrahigh vacuum chamber equipped with a unique photoelectron spectrometer (few eV < electron kinetic energy < 15 keV), x-ray tube (Mg/Ti), 15 keV electron gun, and auxiliary standard surface facilities (molecular beam epitaxy evaporator, ion gun, low energy electron diffraction, sample heating/cooling system, leak valves, load-lock sample transfer, etc.). This end-station offers the unique possibility of performing simultaneous HAXPES + x-ray diffraction studies. In the present work, we describe the experimental set-up together with two experimental examples that emphasize its outstanding capabilities: (i) nondestructive characterization of the Si/Ge and HfO{sub 2}/SiO{sub 2} interfaces on Ge-based CMOS devices, and (ii) strain study on La{sub 0.7}Ca{sub 0.3}MnO{sub 3} ultrathin films grown on SrTiO{sub 3}(001) substrate.

  4. X-ray spectroscopy of manganese clusters

    SciTech Connect

    Grush, M.M. |

    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.

  5. X-Ray Spectroscopy of Gold Nanoparticles

    NASA Astrophysics Data System (ADS)

    Nahar, Sultana N.; Montenegro, M.; Pradhan, A. K.; Pitzer, R.

    2009-06-01

    Inner shell transitions, such as 1s-2p, in heavy elements can absorb or produce hard X-rays, and hence are widely used in nanoparticles. Bio-medical research for cancer treatment has been using heavy element nanoparticles, embeded in malignant tumor, for efficient absorption of irradiated X-rays and leading emission of hard X-rays and energetic electrons to kill the surrounding cells. Ejection of a 1s electron during ionization of the element by absorption of a X-ray photon initiates the Auger cascades of emission of photons and electrons. We have investigated gold nanoparticles for the optimal energy range, below the K-edge (1s) ionization threshold, that corresponds to resonant absorption of X-rays with large attenuation coefficients, orders of magnitude higher over the background as well as to that at K-edge threshold. We applied these attenuation coefficients in Monte Carlo simulation to study the intensities of emission of photons and electrons by Auger cascades. The numerical experiments were carried out in a phantom of water cube with a thin layer, 0.1mm/g, of gold nanoparticles 10 cm inside from the surface using the well-known code Geant4. We will present results on photon and electron emission spectra from passing monochromatic X-ray beams at 67 keV, which is the resonant energy for resonant K_{α} lines, at 82 keV, the K-shell ionization threshold, and at 2 MeV where the resonant effect is non-existent. Our findings show a high peak in the gold nanoparticle absorption curve indicating complete absorption of radiation within the gold layer. The photon and electron emission spectra show resonant features. Acknowledgement: Partially supported by a Large Interdisciplinary Grant award of the Ohio State University and NASA APRA program (SNN). The computational work was carried out on the Cray X1 and Itanium 4 cluster at the Ohio Supercomputer Center, Columbus Ohio. "Resonant X-ray Irradiation of High-Z Nanoparticles For Cancer Theranostics" (refereed

  6. Soft X-ray induced damage in PVA-based membranes in water environment monitored by X-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Tzvetkov, George; Späth, Andreas; Fink, Rainer H.

    2014-10-01

    The effect of synchrotron X-ray flux in a soft X-ray scanning-transmission microspectroscope (STXM) instrument on the chemical structure of air-filled poly(vinyl alcohol) (PVA) based microbubbles and their stabilizing shell has been examined. Prolonged soft X-ray illumination of the particles in aqueous suspension leads to the breaking of the microbubbles' protective polymer shell and substantial chemical changes. The latter were clarified via a micro-spot C K-edge near-edge X-ray absorption fine structure (NEXAFS) spectroscopy with further respect to the absorbed X-ray doses. Our results revealed a continuous degradation of the PVA network associated with formation of carbonyl- and carboxyl-containing species as well as an increased content of unsaturated bonds. The observed effects must be taken into account in studies of micro- and nanostructured polymer materials utilizing X-rays.

  7. The Advanced X-ray Spectroscopy and Imaging Observatory (AXSIO)

    NASA Technical Reports Server (NTRS)

    White, Nicholas E.; Bookbinder, Jay; Petre, Robert; Smith, Randall; Ptak, Andrew; Tananbaum, Harvey; Garcia, Michael

    2012-01-01

    Following recommendations from the 2010 "New Worlds, New Horizons" (NWNH) report, the Advanced X-ray Spectroscopy and Imaging Observatory (AXSIO) concept streamlines the International X-ray Observatory (IXO) mission to concentrate on the science objectives that are enabled by high-resolution spectroscopic capabilities. AXSIO will trace orbits close to the event horizon of black holes, measure black hole spin for tens of supermassive black holes (SMBH), use spectroscopy to characterize outflows and the environment of AGN during their peak activity, observe 5MBH out to redshift z=6, map bulk motions and turbulence in galaxy clusters, find the missing baryons in the cosmic web using background quasars, and observe the process of cosmic feedback where black holes and supernovae inject energy on galactic and intergalactic scales. These measurements are enabled by a 0.9 sq m collecting area at 1.25 keV, a micro calorimeter array providing high-resolution spectroscopic imaging and a deployable high efficiency grating spectrometer. AXSIO delivers a 30-fold increase in effective area for high resolution spectroscopy. The key simplifications are guided by recommendations in the NWNH panel report include a reduction in focal length from 20m to 10m, eliminating the extendable optical bench, and a reduction in the instrument complement from six to two, avoiding a movable instrument platform. A focus on spectroscopic science allows the spatial resolution requirement to be relaxed to 10 arc sec (with a 5 arc sec goal). These simplifications decrease the total mission cost to under the $2B cost to NASA recommended by NWNH. AXSIO will be available to the entire astronomical community with observing allocations based on peer-review.

  8. Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

    NASA Technical Reports Server (NTRS)

    Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

    2010-01-01

    An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

  9. Soft-x-ray spectroscopy study of nanoscale materials

    SciTech Connect

    Guo, J.-H.

    2005-07-30

    The ability to control the particle size and morphology of nanoparticles is of crucial importance nowadays both from a fundamental and industrial point of view considering the tremendous amount of high-tech applications. Controlling the crystallographic structure and the arrangement of atoms along the surface of nanostructured material will determine most of its physical properties. In general, electronic structure ultimately determines the properties of matter. Soft X-ray spectroscopy has some basic features that are important to consider. X-ray is originating from an electronic transition between a localized core state and a valence state. As a core state is involved, elemental selectivity is obtained because the core levels of different elements are well separated in energy, meaning that the involvement of the inner level makes this probe localized to one specific atomic site around which the electronic structure is reflected as a partial density-of-states contribution. The participation of valence electrons gives the method chemical state sensitivity and further, the dipole nature of the transitions gives particular symmetry information. The new generation synchrotron radiation sources producing intensive tunable monochromatized soft X-ray beams have opened up new possibilities for soft X-ray spectroscopy. The introduction of selectively excited soft X-ray emission has opened a new field of study by disclosing many new possibilities of soft X-ray resonant inelastic scattering. In this paper, some recent findings regarding soft X-ray absorption and emission studies of various nanostructured systems are presented.

  10. X-ray split and delay device for ultrafast x-ray science at the AMO instrument at LCLS

    NASA Astrophysics Data System (ADS)

    Bozek, J. D.; Castagna, J. C.; Fang, L.; Hui, Z.; Kukk, E.; Murphy, B. F.; Berrah, N.

    2015-09-01

    Ultrafast molecular dynamics can be studied using x-rays from both synchrotrons sources and x-ray free electron lasers. Synchrotron studies are limited by the 10-100 ps duration pulses to processes where the Auger lifetime can be used to probe dynamics initiated by excitation of an inner-shell electron to an antibonding orbital. The short pulses produced by x-ray free electron lasers offer the opportunity to study molecular dynamics directly with pump-probe techniques. A two-mirror x-ray split and delay device has been developed for x- ray pump - x-ray probe experiments at the soft x-ray AMO instrument at the LCLS. The device operates over a photon energy range of 250-1800 eV with a variable delay of up to 200 femtoseconds with 0.1 fs resolution.

  11. Development of Instruments onboard ASTRO-H for Future X-ray Studies of Tori

    NASA Astrophysics Data System (ADS)

    Noda, H.

    2015-09-01

    The next astronomical X-ray satellite ASTRO-H will be launched by Japan Aerospace eXploration Agency (JAXA) in this Japanese fiscal year. It allows us to combine a simultaneous coverage of the 0.4-600 keV band, and a high energy-resolution spectroscopy in the 0.3-12 keV band with an FWHM energy resolution of < 7 eV at 6 keV. The wide-band capability is provided by several instruments; X-ray CCD cameras cover the 0.4-12 keV band at a focal plane of soft X-ray telescopes, a hard X-ray imager covers the 5-80 keV range with multilayer coating hard X-ray mirrors, and a non-focusing soft gamma-ray detector covers the 40-600 keV band. The high energy-resolution spectroscopy is realized by the X-ray micro-calorimeter array operated at 50 mK on a focal plane of the soft X-ray telescope. With the unprecedented performances, the ASTRO-H observations of active galactic nuclei are expected to give us important X-ray information about tori including their dynamics, size, ionization state and so on. In the present talk, we introduce the current status of developments of the instruments onboard ASTRO-H, especially focusing on the performance of the X-ray micro-calorimeter derived in the ongoing ground testing and calibration.

  12. Advanced X-ray Astrophysics Facility (AXAF) science instrumentation

    NASA Technical Reports Server (NTRS)

    Dailey, C. C.; Cumings, N. P.; Winkler, C. E.

    1985-01-01

    AXAF is to be equipped with a high performance X-ray telescope for the conduction of detailed astrophysics research. The observatory is to be serviced by the Space Station or the Shuttle, depending on capabilities during the AXAF operational period. The AXAF is to utilize the wavelength band from 1.2 A to 120 A. Attention is given to the AXAF science team, the AXAF observatory characteristics, the AXAF science instrument definition program, the Advanced Charge Coupled Device (CCD) Imaging Spectrometer (ACIS), the High Resolution Camera (HRC), the Bragg Crystal Spectrometer (BCS), the X-ray Spectrometer (XRS), the transmission gratings, and the program schedule.

  13. Development and applications of grazing exit micro X-ray fluorescence instrument using a polycapillary X-ray lens*1

    NASA Astrophysics Data System (ADS)

    Emoto, T.; Sato, Y.; Konishi, Y.; Ding, X.; Tsuji, K.

    2004-08-01

    A polycapillary X-ray lens is an effective optics to obtain a μm-size X-ray beam for micro-X-ray fluorescence spectrometry (μ-XRF). We developed a μ-XRF instrument using a polycapillary X-ray lens, which also enabled us to perform Grazing Exit μ-XRF (GE-μ-XRF). The evaluated diameter of the primary X-ray beam was 48 μm at the focal distance of the X-ray lens. Use of this instrument enabled two-dimensional mapping of the elemental distributions during growth of the plant "Quinoa". The results of the mapping revealed elemental transition during growth. In addition, a small region of thin film was analyzed by GE-μ-XRF. We expect that GE-μ-XRF will become an effective method of estimating the film thickness of a small region.

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

    PubMed

    Haldrup, Kristoffer; Gawelda, Wojciech; Abela, Rafael; Alonso-Mori, Roberto; Bergmann, Uwe; Bordage, Amélie; Cammarata, Marco; Canton, Sophie E; Dohn, Asmus O; van Driel, Tim Brandt; Fritz, David M; Galler, Andreas; Glatzel, Pieter; Harlang, Tobias; Kjær, Kasper S; Lemke, Henrik T; Møller, Klaus B; Németh, Zoltán; Pápai, Mátyás; Sas, Norbert; Uhlig, Jens; Zhu, Diling; Vankó, György; Sundström, Villy; Nielsen, Martin M; Bressler, Christian

    2016-02-18

    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 and structural changes, and local solvent structural changes are desired. We have studied the intra- and intermolecular dynamics of a model chromophore, aqueous [Fe(bpy)3](2+), with complementary X-ray tools in a single experiment exploiting intense XFEL radiation as a probe. We monitored the ultrafast structural 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 patterns reveal slower subpicosecond dynamics triggered by the intramolecular structural dynamics of the photoexcited solute. By simultaneous combination of both methods only, we can extract new information about the solvation dynamic processes unfolding during the first picosecond (ps). The measured bulk solvent density increase of 0.2% indicates a dramatic change of the solvation shell around each photoexcited solute, confirming previous ab initio molecular dynamics simulations. Structural changes in the aqueous solvent associated with density and temperature changes occur with ∼1 ps time constants, characteristic for structural dynamics in water. This slower time scale of the solvent response allows us to directly observe the structure of the excited solute molecules well before the solvent contributions become dominant. PMID:26783685

  15. EUV spectroscopy of high-redshift x-ray objects

    NASA Astrophysics Data System (ADS)

    Kowalski, M. P.; Wolff, M. T.; Wood, K. S.; Barbee, T. W., Jr.; Barstow, M. A.

    2010-07-01

    As astronomical observations are pushed to cosmological distances (z>3) the spectral energy distributions of X-ray objects, AGN for example, will be redshifted into the EUV waveband. Consequently, a wealth of critical spectral diagnostics, provided by, for example, the Fe L-shell complex and the O VII/VIII lines, will be lost to future planned X-ray missions (e.g., IXO, Gen-X) if operated at traditional X-ray energies. This opens up a critical gap in performance located at short EUV wavelengths, where critical X-ray spectral transitions occur in high-z objects. However, normal-incidence multilayer-grating technology, which performs best precisely at such wavelengths, together with advanced nanolaminate replication techniques have been developed and are now mature to the point where advanced EUV instrument designs with performance complementary to IXO and Gen-X are practical. Such EUV instruments could be flown either independently or as secondary instruments on these X-ray missions. We present here a critical examination of the limits placed on extragalactic EUV measurements by ISM absorption, the range where high-z measurements are practical, and the requirements this imposes on next-generation instrument designs. We conclude with a discussion of a breakthrough technology, nanolaminate replication, which enables such instruments.

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

    SciTech Connect

    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.

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

    PubMed

    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. PMID:27036761

  18. Combining scanning probe microscopy and x-ray spectroscopy

    PubMed Central

    2011-01-01

    A new versatile tool, combining Shear Force Microscopy and X-Ray Spectroscopy was designed and constructed to obtain simultaneously surface topography and chemical mapping. Using a sharp optical fiber as microscope probe, it is possible to collect locally the visible luminescence of the sample. Results of tests on ZnO and on ZnWO4 thin layers are in perfect agreement with that obtained with other conventional techniques. Twin images obtained by simultaneous acquisition in near field of surface topography and of local visible light emitted by the sample under X-Ray irradiation in synchrotron environment are shown. Replacing the optical fibre by an X-ray capillary, it is possible to collect local X-ray fluorescence of the sample. Preliminary results on Co-Ti sample analysis are presented. PMID:21711848

  19. A Polarization Propagator for Nonlinear X-ray Spectroscopies.

    PubMed

    Fahleson, Tobias; Ågren, Hans; Norman, Patrick

    2016-06-01

    A complex polarization propagator approach has been developed to third order and implemented in density functional theory (DFT), allowing for the direct calculation of nonlinear molecular properties in the X-ray wavelength regime without explicitly addressing the excited-state manifold. We demonstrate the utility of this propagator method for the modeling of coherent near-edge X-ray two-photon absorption using, as an example, DFT as the underlying electronic structure model. Results are compared with the corresponding near-edge X-ray absorption fine structure spectra, illuminating the differences in the role of symmetry, localization, and correlation between the two spectroscopies. The ramifications of this new technique for nonlinear X-ray research are briefly discussed. PMID:27159130

  20. Femtosecond x-ray absorption spectroscopy with hard x-ray free electron laser

    SciTech Connect

    Katayama, Tetsuo; Togashi, Tadashi; Tono, Kensuke; Kameshima, Takashi; Inubushi, Yuichi; Sato, Takahiro; Hatsui, Takaki; Yabashi, Makina; Obara, Yuki; Misawa, Kazuhiko; Bhattacharya, Atanu; Kurahashi, Naoya; Ogi, Yoshihiro; Suzuki, Toshinori

    2013-09-23

    We have developed a method of dispersive x-ray absorption spectroscopy with a hard x-ray free electron laser (XFEL), generated by a self-amplified spontaneous emission (SASE) mechanism. A transmission grating was utilized for splitting SASE-XFEL light, which has a relatively large bandwidth (ΔE/E ∼ 5 × 10{sup −3}), into several branches. Two primary split beams were introduced into a dispersive spectrometer for measuring signal and reference spectra simultaneously. After normalization, we obtained a Zn K-edge absorption spectrum with a photon-energy range of 210 eV, which is in excellent agreement with that measured by a conventional wavelength-scanning method. From the analysis of the difference spectra, the noise ratio was evaluated to be ∼3 × 10{sup −3}, which is sufficiently small to trace minute changes in transient spectra induced by an ultrafast optical laser. This scheme enables us to perform single-shot, high-accuracy x-ray absorption spectroscopy with femtosecond time resolution.

  1. Effect of X-ray flux on polytetrafluoroethylene in X-ray photoelectron spectroscopy

    NASA Technical Reports Server (NTRS)

    Wheeler, D. R.; Pepper, S. V.

    1982-01-01

    The effect of the X-ray flux in X-ray photoelectron spectroscopy (STAT) on the constitution of the polytetrafluoroethylene (PTFE) surface has been examined. The radiation dose rate for our specimen was about 10 to the 7th rad/s. The structure, magnitude and binding energy of the C(1s) and F(1s) features of the XPS spectrum and the mass spectrum of gaseous species evolved during irradiation are observed. The strong time dependence of these signals over a period of several hours indicated that the surface constitution of PTFE is greatly affected by this level of radiation dose. The results are consistent with the development of a heavily cross-linked or branched structure in the PTFE surface region and the evolution of short chain fragments into the gas phase.

  2. Soft X-ray spectroscopy of astrophysical plasmas

    NASA Astrophysics Data System (ADS)

    Kahn, Steven M.

    These lectures are intended to provide a review of the basic physics necessary for the interpretation of high resolution soft X-ray spectra of astrophysical sources. While many of the topics I discuss can be found at the requisite level of sophistication in standard textbooks on atomic physics and spectroscopy, I have made an attempt to highlight those aspects which are especially important for X-ray transitions, and which are relevant at the characteristic temperatures and densities typically found in various types of X-ray emitting astrophysical plasmas. My emphasis is on discrete atomic transitions, which dominate the spectra of most cosmic sources in the soft X-ray band (100eV≤E≤10 keV). I do not discuss basic continuum processes like bremsstrahlung, synchrotron emission, and inverse Compton emission, as these are covered well in the usual texts used to introduce students to radiative processes in astrophysics. The organization is as follows: I provide a brief introduction to the role of X-ray spectroscopy in astrophysics, and the physical conditions in various types of cosmic X-ray sources. Chapters 1 through 3 cover the essentials of atomic physics: classical and quantum radiation theory, atomic structure, and electron-ion collisional processes, respectively. In Chap. 4, I discuss the various types of equilibria that apply in astrophysical plasmas, and in Chap. 5, I provide a relatively brief review of the most important discrete-line spectral diagnostics that fall in the soft X-ray band. Chapter 6 includes a set of concluding remarks and some thoughts on where this field might be headed in the future.

  3. X-ray Photoelectron Spectroscopy Database (Version 4.1)

    National Institute of Standards and Technology Data Gateway

    SRD 20 X-ray Photoelectron Spectroscopy Database (Version 4.1) (Web, free access)   The NIST XPS Database gives access to energies of many photoelectron and Auger-electron spectral lines. The database contains over 22,000 line positions, chemical shifts, doublet splittings, and energy separations of photoelectron and Auger-electron lines.

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

    SciTech Connect

    Lovejoy, T. C.; Dellby, N.; Krivanek, O. L.; Ramasse, Q. M.; Falke, M.; Kaeppel, A.; Terborg, R.; Zan, R.

    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.

  5. EUV Spectroscopy of High-redshift X-ray Objects

    NASA Astrophysics Data System (ADS)

    Kowalski, Michael Paul; Wolff, M. T.; Wood, K. S.; Barbee, T. W., Jr.

    2010-03-01

    As astronomical observations are pushed to cosmological distances (z>3) the spectral energy distributions of X-ray objects, AGNs for example, will have their maxima redshifted into the EUV waveband ( 90-912 Å/0.1-0.01 keV). Consequently, a wealth of spectral diagnostics, provided by, for example, the Fe L-shell complex ( 60-6 Å/0.2-2.0 keV) and the O VII/VIII lines ( 20 Å/0.5 keV), will be lost to X-ray instruments operating at traditional ( 0.5-10 keV) and higher X-ray energies. There are precedents in other wavebands. For example, HST evolutionary studies will become largely the province of JWST. Despite the successes of EUVE, the ROSAT WFC, and the Chandra LETG, the EUV continues to be unappreciated and under-utilized, partly because of a preconception that absorption by neutral galactic Hydrogen in the ISM prevents any useful extragalactic measurements at all EUV wavelengths and, until recently, by a lack of a suitable enabling technology. Thus, if future planned X-ray missions (e.g., IXO, Gen-X) are optimized again for traditional X-ray energies, their performance (effective area, resolving power) will be cut off at ultrasoft X-ray energies or at best be radically reduced in the EUV. This opens up a critical gap in performance located right at short EUV wavelengths, where the critical X-ray spectral transitions occur in high-z objects. However, normal-incidence multilayer-grating technology, which performs best precisely at such wavelengths, together with advanced nano-laminate fabrication techniques have been developed and are now mature to the point where advanced EUV instrument designs with performance complementary to IXO and Gen-X are practical. Such EUV instruments could be flown either independently or as secondary instruments on these X-ray missions. We present here a critical examination of the limits placed on extragalactic EUV measurements by ISM absorption, the range where high-z measurements are practical, and the requirements this imposes on

  6. [Development of Nanotechnology for X-Ray Astronomy Instrumentation

    NASA Technical Reports Server (NTRS)

    Schattenburg, Mark L.

    2004-01-01

    This Research Grant provides support for development of nanotechnology for x-ray astronomy instrumentation. MIT has made significant progress in several development areas. In the last year we have made considerable progress in demonstrating the high-fidelity patterning and replication of x-ray reflection gratings. We developed a process for fabricating blazed gratings in silicon with extremely smooth and sharp sawtooth profiles, and developed a nanoimprint process for replication. We also developed sophisticated new fixturing for holding thin optics during metrology without causing distortion. We developed a new image processing algorithm for our Shack-Hartmann tool that uses Zernike polynomials. This has resulted in much more accurate and repeatable measurements on thin optics.

  7. Raman spectroscopy and X-ray diffraction studies on celestite

    NASA Astrophysics Data System (ADS)

    Chen, Yen-Hua; Yu, Shu-Cheng; Huang, Eugene; Lee, Pei-Lun

    2010-10-01

    High-pressure Raman spectroscopy and X-ray diffraction studies of celestite (SrSO 4) were carried out in a diamond anvil cell at room temperature. Variation in the Raman vibrational frequency and change of lattice parameters with pressure indicate that a transformation occurs in celestite. This transformation caused an adjustment in the Sr-O polyhedra that affected the stretching-force constant of SO 4. Moreover, compressibilities along the crystallographic axes decreased in the order a to c to b. From the compression data, the bulk modulus of the celestite was 87 GPa. Both X-ray and Raman data show that the transition in celestite is reversible.

  8. Improved x-ray spectroscopy with room temperature CZT detectors.

    PubMed

    Fritz, Shannon G; Shikhaliev, Polad M; Matthews, Kenneth L

    2011-09-01

    Compact, room temperature x-ray spectroscopy detectors are of interest in many areas including diagnostic x-ray imaging, radiation protection and dosimetry. Room temperature cadmium zinc telluride (CZT) semiconductor detectors are promising candidates for these applications. One of the major problems for CZT detectors is low-energy tailing of the energy spectrum due to hole trapping. Spectral post-correction methods to correct the tailing effect do not work well for a number of reasons; thus it is advisable to eliminate the hole trapping effect in CZT using physical methods rather than correcting an already deteriorated energy spectrum. One method is using a CZT detector with an electrode configuration which modifies the electric field in the CZT volume to decrease low-energy tailing. Another method is to irradiate the CZT surface at a tilted angle, which modifies depth of interaction to decrease low-energy tailing. Neither method alone, however, eliminates the tailing effect. In this work, we have investigated the combination of modified electric field and tilted angle irradiation in a single detector to further decrease spectral tailing. A planar CZT detector with 10 × 10 × 3 mm³ size and CZT detector with 5 × 5 × 5 mm³ size and cap-shaped electrode were used in this study. The cap-shaped electrode (referred to as CAPture technology) modifies the electric field distribution in the CZT volume and decreases the spectral tailing effect. The detectors were investigated at 90° (normal) and 30° (tilted angle) irradiation modes. Two isotope sources with 59.6 and 122 keV photon energies were used for gamma-ray spectroscopy experiments. X-ray spectroscopy was performed using collimated beams at 60, 80 and 120 kVp tube voltages, in both normal and tilted angle irradiation. Measured x-ray spectra were corrected for K x-ray escape fractions that were calculated using Monte Carlo methods. The x-ray spectra measured with tilted angle CAPture detector at 60, 80 and 120

  9. Simultaneous surface plasmon resonance and x-ray absorption spectroscopy

    SciTech Connect

    Serrano, A.; Rodriguez de la Fuente, O.; Collado, V.; Rubio-Zuazo, J.; Castro, G. R.; Monton, C.; Garcia, M. A.

    2012-08-15

    We present an experimental setup for the simultaneous measurement of surface plasmon resonance (SPR) and x-ray absorption spectroscopy (XAS) on metallic thin films at a synchrotron beamline. The system allows measuring in situ and in real time the effect of x-ray irradiation on the SPR curves to explore the interaction of x-rays with matter. It is also possible to record XAS spectra while exciting SPR in order to study changes in the films induced by the excitation of surface plasmons. Combined experiments recording simultaneously SPR and XAS curves while scanning different parameters can be also carried out. The relative variations in the SPR and XAS spectra that can be detected with this setup range from 10{sup -3} to 10{sup -5}, depending on the particular experiment.

  10. Simultaneous surface plasmon resonance and x-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Serrano, A.; Rodríguez de la Fuente, O.; Collado, V.; Rubio-Zuazo, J.; Monton, C.; Castro, G. R.; García, M. A.

    2012-08-01

    We present an experimental setup for the simultaneous measurement of surface plasmon resonance (SPR) and x-ray absorption spectroscopy (XAS) on metallic thin films at a synchrotron beamline. The system allows measuring in situ and in real time the effect of x-ray irradiation on the SPR curves to explore the interaction of x-rays with matter. It is also possible to record XAS spectra while exciting SPR in order to study changes in the films induced by the excitation of surface plasmons. Combined experiments recording simultaneously SPR and XAS curves while scanning different parameters can be also carried out. The relative variations in the SPR and XAS spectra that can be detected with this setup range from 10-3 to 10-5, depending on the particular experiment.

  11. Biological X-ray absorption spectroscopy and metalloproteomics.

    PubMed

    Ascone, Isabella; Strange, Richard

    2009-05-01

    In the past seven years the size of the known protein sequence universe has been rapidly expanding. At present, more then five million entries are included in the UniProtKB/TrEMBL protein database. In this context, a retrospective evaluation of recent X-ray absorption studies is undertaken to assess its potential role in metalloproteomics. Metalloproteomics is the structural and functional characterization of metal-binding proteins. This is a new area of active research which has particular relevance to biology and for which X-ray absorption spectroscopy is ideally suited. In the last three years, biological X-ray absorption spectroscopy (BioXAS) has been included among the techniques used in post-genomics initiatives for metalloprotein characterization. The emphasis of this review is on the progress in BioXAS that has emerged from recent meetings in 2007-2008. Developments required to enable BioXAS studies to better contribute to metalloproteomics throughput are also discussed. Overall, this paper suggests that X-ray absorption spectroscopy could have a higher impact on metalloproteomics, contributing significantly to the understanding of metal site structures and of reaction mechanisms for metalloproteins. PMID:19395808

  12. Simultaneous X-ray and optical spectroscopy of the Oef supergiant λ Cephei

    NASA Astrophysics Data System (ADS)

    Rauw, G.; Hervé, A.; Nazé, Y.; González-Pérez, J. N.; Hempelmann, A.; Mittag, M.; Schmitt, J. H. M. M.; Schröder, K.-P.; Gosset, E.; Eenens, P.; Uuh-Sonda, J. M.

    2015-08-01

    Context. Probing the structures of stellar winds is of prime importance for the understanding of massive stars. Based on their optical spectral morphology and variability, it has been suggested that the stars in the Oef class feature large-scale structures in their wind. Aims: High-resolution X-ray spectroscopy and time-series of X-ray observations of presumably single O-type stars can help us understand the physics of their stellar winds. Methods: We have collected XMM-Newton observations and coordinated optical spectroscopy of the O6 Ief star λ Cep to study its X-ray and optical variability and to analyse its high-resolution X-ray spectrum. We investigate the line profile variability of the He ii λ 4686 and Hα emission lines in our time series of optical spectra, including a search for periodicities. We further discuss the variability of the broadband X-ray flux and analyse the high-resolution spectrum of λ Cep using line-by-line fits as well as a code designed to fit the full high-resolution X-ray spectrum consistently. Results: During our observing campaign, the He ii λ 4686 line varies on a timescale of ~18 h. On the contrary, the Hα line profile displays a modulation on a timescale of 4.1 days which is likely the rotation period of the star. The X-ray flux varies on timescales of days and could in fact be modulated by the same 4.1-day period as Hα, although both variations are shifted in phase. The high-resolution X-ray spectrum reveals broad and skewed emission lines as expected for the X-ray emission from a distribution of wind-embedded shocks. Most of the X-ray emission arises within less than 2 R∗ above the photosphere. Conclusions: The properties of the X-ray emission of λ Cep generally agree with the expectations of the wind-embedded shock model. There is mounting evidence for the existence of large-scale structures that modulate the Hα line and about 10% of the X-ray emission of λ Cep. Based on observations collected with XMM-Newton, an ESA

  13. X-ray Spectroscopy of Accreting White Dwarfs

    NASA Astrophysics Data System (ADS)

    Ishida, Manabu

    2010-12-01

    The advent of the grating spectrometers onboard Chandra and XMM-Newton opened up a new era in plasma diagnostics of compact binaries. High resolution spectroscopy using these spectrometers is of particular use in investigating accretion plasmas in cataclysmic variables (CVs) because they show a wealth of emission lines owing to their optically thin thermal nature. In this review, I present recent progress on density measurements of the plasma in magnetic CVs by means of He-like triplet and iron L lines, and the outcome of line velocity measurements in the dwarf nova SS Cygni in outburst, to demonstrate the potential power of high resolution spectroscopy to elucidate the geometry of the plasma. In the end, our expectations for the Soft X-ray Spectrometer onboard the forthcoming X-ray mission Astro-H are summarized.

  14. What can be Learned from X-ray Spectroscopy Concerning Hot Gas in Local Bubble and Charge Exchange Processes?

    NASA Technical Reports Server (NTRS)

    Snowden, Steve

    2007-01-01

    What can be learned from x-ray spectroscopy in observing hot gas in local bubble and charge exchange processes depends on spectral resolution, instrumental grasp, instrumental energy band, signal-to-nose, field of view, angular resolution and observatory location. Early attempts at x-ray spectroscopy include ROSAT; more recently, astronomers have used diffuse x-ray spectrometers, XMM Newton, sounding rocket calorimeters, and Suzaku. Future observations are expected with calorimeters on the Spectrum Roentgen Gamma mission, and the Solar Wind Charge Exchange (SWCX). The Geospheric SWCX may provide remote sensing of the solar wind and magnetosheath and remote observations of solar CMEs moving outward from the sun.

  15. Atomic Multiplets in X-ray Spectroscopies of Solids

    NASA Astrophysics Data System (ADS)

    Delley, Bernard; Uldry, Anne-Christine

    2013-03-01

    The electronic structures of compounds involving open d- and f- shell are studied frequently by X-ray and electron spectroscopies. For a better understanding of the multiplets arising in spectra involving one or more open shells, we have developed recently an easy to use program multiX,[2] which is available to download.[3] This first step allows the inclusion of the crystal environment as a crystal field entered simply as positions and charges of a cluster of atoms around the core hole site. This often gives valuable insights in the case of x-ray absorption spectroscopy (XAS) and resonant inelastic x-ray spectroscopy (RIXS) measurements. However, in many cases it is desirable to allow for hybridization of the open shell electrons with the orbitals of neighbor atoms. This requires dealing with a significantly larger active Hilbert space. This is addressed with our recent Lanczos-based procedure to calculate spectra. First results will be discussed. Swiss SNF grant 200021-129970 is gratefully acknowledged.

  16. Pushing the Boundaries of Suborbital Soft X-ray Spectroscopy

    NASA Astrophysics Data System (ADS)

    McEntaffer, Randall

    optics are planned for every future large X-ray mission and flight-proving the design is extremely important. The gratings will be radially grooved and blazed to reduce grating aberrations and to focus the spectrum to one side of zero-order. Gratings of this type have been well developed by the IXO Off- Plane X-ray Grating Spectrometer concept study, but have not been flight proven. The spectrum will be focused onto high spatial resolution CCD detectors. OGRE will draw heavily from the heritage gained from OGRESS. OGRE will observe Capella. Due to its high flux and spectral line density, Capella is an ideal target for showcasing the resolution capabilities of our instrument. As an important calibration target, our improved resolution measurements will be extremely helpful for many future X-ray observations. OGRESS has already provided three thesis projects for past graduate students. The upgrades and flights proposed here will produce at least two more PhD theses. This program in hands-on training of young scientists in the techniques of instrumental X-ray astronomy has proven very successful over nearly three decades, leading to high rates of launch, publication, graduation, and flight qualification of instrumental PI's. It will also provide full experiment cycle experience - design, fabrication, tolerancing, assembly, flight-qualification, calibration, integration, launch, and data analysis - with reflection gratings, GEM and CCD detectors, and other technologies suitable for adaptation to NASA's major missions. The University of Iowa and University of Colorado programs in suborbital X-ray astronomy represent an exciting mix of compelling science, cutting- edge technology development, and training of young scientists.

  17. Probing deeper by hard x-ray photoelectron spectroscopy

    SciTech Connect

    Risterucci, P.; Renault, O. Martinez, E.; Delaye, V.; Detlefs, B.; Zegenhagen, J.; Gaumer, C.; Grenet, G.; Tougaard, S.

    2014-02-03

    We report an hard x-ray photoelectron spectroscopy method combining high excitation energy (15 keV) and improved modelling of the core-level energy loss features. It provides depth distribution of deeply buried layers with very high sensitivity. We show that a conventional approach relying on intensities of the core-level peaks is unreliable due to intense plasmon losses. We reliably determine the depth distribution of 1 ML La in a high-κ/metal gate stack capped with 50 nm a-Si. The method extends the sensitivity of photoelectron spectroscopy to depths beyond 50 nm.

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

    NASA Astrophysics Data System (ADS)

    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 capability of generating two intense, femtosecond x-ray pulses with a controlled time delay opens the possibility of performing time-resolved experiments for x-ray-induced phenomena. We have applied this capability to study the photoinduced dynamics in diatomic molecules. In molecules composed of low-Z elements, K -shell ionization creates a core-hole state in which the main decay mode is an Auger process involving two electrons in the valence shell. After Auger decay, the nuclear wave packets of the transient two-valence-hole states continue evolving on the femtosecond time scale, leading either to separated atomic ions or long-lived quasibound 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 the time evolution of the nuclear wave packets. 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 quasibound states.

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

    NASA Astrophysics Data System (ADS)

    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

  20. Observatory Science with the NICER X-ray Timing Instrument

    NASA Astrophysics Data System (ADS)

    Remillard, Ronald A.

    2016-04-01

    This presentation is submitted on behalf of the NICER Observatory Science Working Group. NICER will be deployed on the International Space Station later in 2016. The X-ray sensitivity spans 0.2-12 keV, with CCD-like spectral resolution, low background rates, and unprecedented timing accuracy. A Guest Observer (GO) Program has been approved by NASA as one of the proposed Science Enhancement Options, contingent on NICER meeting its Prime Mission Science Objectives. The NICER Science team will observe limited Observatory Science targets (i.e., sources other than neutron stars) in year 1, and GO observations will constitute 50% of the exposures in year 2. Thereafter, NICER will compete for continuation via the NASA Senior Review process. NICER Instrument performance is compared with Missions such as XMM-Newton and RXTE. We briefly highlight the expected themes for Observatory Science relating to accreting black holes on all mass scales, magnetic CVs, active stars, and clusters of galaxies.

  1. X-ray absorption spectroscopy of liquid surface

    NASA Astrophysics Data System (ADS)

    Watanabe, Iwao; Tanida, Hajime; Kawauchi, Sigehiro; Harada, Makoto; Nomura, Masaharu

    1997-09-01

    An apparatus has been constructed for x-ray absorption spectroscopy of elements at air/aqueous solution interface. Its surface sensitivity is gained from glancing incidence of synchrotron radiation under total reflection condition. The absorption is detected by total conversion He ion-yield method. This apparatus was operated at the beam line 7C of Photon Factory, where the incident photon beam comes from a sagittal focus double-crystal monochromator via a 70-cm-long bent mirror. The mirror focuses the beam vertically and changes the beam direction downward by 1 mrad to irradiate solution surface. The essential requirement of this technique, ripple-free liquid surface at accurate position, was attained by introducing a trough on a floating boat, continuous surface level monitoring, and an automatic Z-stage control. The x-ray absorption edge jump demonstrated that surface concentration of bromide ion follows the Langmuir type adsorption for tetraalkylammonuim bromide solution. By comparing the jump values for surface-active and -inactive bromide salt solutions, the detecting depth of the present technique was determined to be 8.8 nm. An extended x-ray absorption fine structure analysis of bromide ion segregated to the surface by stearyltrimethylammonium cation indicated that its solvation structure is different from that of bulk.

  2. 28 CFR 552.13 - X-ray, major instrument, fluoroscope, or surgical intrusion.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 28 Judicial Administration 2 2011-07-01 2011-07-01 false X-ray, major instrument, fluoroscope, or... INSTITUTIONAL MANAGEMENT CUSTODY Searches of Housing Units, Inmates, and Inmate Work Areas § 552.13 X-ray, major... reasons only, with the inmate's consent. (b) The institution physician may authorize use of an X-ray...

  3. 28 CFR 552.13 - X-ray, major instrument, fluoroscope, or surgical intrusion.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 28 Judicial Administration 2 2010-07-01 2010-07-01 false X-ray, major instrument, fluoroscope, or... INSTITUTIONAL MANAGEMENT CUSTODY Searches of Housing Units, Inmates, and Inmate Work Areas § 552.13 X-ray, major... reasons only, with the inmate's consent. (b) The institution physician may authorize use of an X-ray...

  4. 28 CFR 552.13 - X-ray, major instrument, fluoroscope, or surgical intrusion.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 28 Judicial Administration 2 2012-07-01 2012-07-01 false X-ray, major instrument, fluoroscope, or... INSTITUTIONAL MANAGEMENT CUSTODY Searches of Housing Units, Inmates, and Inmate Work Areas § 552.13 X-ray, major... reasons only, with the inmate's consent. (b) The institution physician may authorize use of an X-ray...

  5. 28 CFR 552.13 - X-ray, major instrument, fluoroscope, or surgical intrusion.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 28 Judicial Administration 2 2014-07-01 2014-07-01 false X-ray, major instrument, fluoroscope, or... INSTITUTIONAL MANAGEMENT CUSTODY Searches of Housing Units, Inmates, and Inmate Work Areas § 552.13 X-ray, major... reasons only, with the inmate's consent. (b) The institution physician may authorize use of an X-ray...

  6. 28 CFR 552.13 - X-ray, major instrument, fluoroscope, or surgical intrusion.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 28 Judicial Administration 2 2013-07-01 2013-07-01 false X-ray, major instrument, fluoroscope, or... INSTITUTIONAL MANAGEMENT CUSTODY Searches of Housing Units, Inmates, and Inmate Work Areas § 552.13 X-ray, major... reasons only, with the inmate's consent. (b) The institution physician may authorize use of an X-ray...

  7. Stochastic stimulated electronic x-ray Raman spectroscopy.

    PubMed

    Kimberg, Victor; Rohringer, Nina

    2016-05-01

    Resonant inelastic x-ray scattering (RIXS) is a well-established tool for studying electronic, nuclear, and collective dynamics of excited atoms, molecules, and solids. An extension of this powerful method to a time-resolved probe technique at x-ray free electron lasers (XFELs) to ultimately unravel ultrafast chemical and structural changes on a femtosecond time scale is often challenging, due to the small signal rate in conventional implementations at XFELs that rely on the usage of a monochromator setup to select a small frequency band of the broadband, spectrally incoherent XFEL radiation. Here, we suggest an alternative approach, based on stochastic spectroscopy, which uses the full bandwidth of the incoming XFEL pulses. Our proposed method is relying on stimulated resonant inelastic x-ray scattering, where in addition to a pump pulse that resonantly excites the system a probe pulse on a specific electronic inelastic transition is provided, which serves as a seed in the stimulated scattering process. The limited spectral coherence of the XFEL radiation defines the energy resolution in this process and stimulated RIXS spectra of high resolution can be obtained by covariance analysis of the transmitted spectra. We present a detailed feasibility study and predict signal strengths for realistic XFEL parameters for the CO molecule resonantly pumped at the [Formula: see text] transition. Our theoretical model describes the evolution of the spectral and temporal characteristics of the transmitted x-ray radiation, by solving the equation of motion for the electronic and vibrational degrees of freedom of the system self consistently with the propagation by Maxwell equations. PMID:26958585

  8. Stochastic stimulated electronic x-ray Raman spectroscopy

    PubMed Central

    Kimberg, Victor; Rohringer, Nina

    2016-01-01

    Resonant inelastic x-ray scattering (RIXS) is a well-established tool for studying electronic, nuclear, and collective dynamics of excited atoms, molecules, and solids. An extension of this powerful method to a time-resolved probe technique at x-ray free electron lasers (XFELs) to ultimately unravel ultrafast chemical and structural changes on a femtosecond time scale is often challenging, due to the small signal rate in conventional implementations at XFELs that rely on the usage of a monochromator setup to select a small frequency band of the broadband, spectrally incoherent XFEL radiation. Here, we suggest an alternative approach, based on stochastic spectroscopy, which uses the full bandwidth of the incoming XFEL pulses. Our proposed method is relying on stimulated resonant inelastic x-ray scattering, where in addition to a pump pulse that resonantly excites the system a probe pulse on a specific electronic inelastic transition is provided, which serves as a seed in the stimulated scattering process. The limited spectral coherence of the XFEL radiation defines the energy resolution in this process and stimulated RIXS spectra of high resolution can be obtained by covariance analysis of the transmitted spectra. We present a detailed feasibility study and predict signal strengths for realistic XFEL parameters for the CO molecule resonantly pumped at the O1s→π* transition. Our theoretical model describes the evolution of the spectral and temporal characteristics of the transmitted x-ray radiation, by solving the equation of motion for the electronic and vibrational degrees of freedom of the system self consistently with the propagation by Maxwell equations. PMID:26958585

  9. Near Edge X-Ray Absorption Fine Structure Spectroscopy with X-Ray Free-Electron Lasers

    SciTech Connect

    Bernstein, D.P.; Acremann, Y.; Scherz, A.; Burkhardt, M.; Stohr, J.; Beye, M.; Schlotter, W.F.; Beeck, T.; Sorgenfrei, F.; Pietzsch, A.; Wurth, W.; Fohlisch, A.; /Hamburg U.

    2009-12-11

    We demonstrate the feasibility of Near Edge X-ray Absorption Fine Structure (NEXAFS) spectroscopy on solids by means of femtosecond soft x-ray pulses from a free-electron laser (FEL). Our experiments, carried out at the Free-Electron Laser at Hamburg (FLASH), used a special sample geometry, spectrographic energy dispersion, single shot position-sensitive detection and a data normalization procedure that eliminates the severe fluctuations of the incident intensity in space and photon energy. As an example we recorded the {sup 3}D{sub 1} N{sub 4,5}-edge absorption resonance of La{sup 3+}-ions in LaMnO{sub 3}. Our study opens the door for x-ray absorption measurements on future x-ray FEL facilities.

  10. Hetero-site-specific X-ray pump-probe spectroscopy for femtosecond intramolecular dynamics

    DOE PAGESBeta

    Picón, A.; Lehmann, C. S.; Bostedt, C.; Rudenko, A.; Marinelli, A.; Osipov, T.; Rolles, D.; Berrah, N.; Bomme, C.; Bucher, M.; et al

    2016-05-23

    New capabilities at X-ray free-electron laser facilities allow the generation of two-colour femtosecond X-ray pulses, opening the possibility of performing ultrafast studies of X-ray-induced phenomena. Specifically, the experimental realization of hetero-site-specific X-ray-pump/X-ray-probe spectroscopy is of special interest, in which an X-ray pump pulse is absorbed at one site within a molecule and an X-ray probe pulse follows the X-ray-induced dynamics at another site within the same molecule. In this paper, we show experimental evidence of a hetero-site pump-probe signal. By using two-colour 10-fs X-ray pulses, we are able to observe the femtosecond time dependence for the formation of F ionsmore » during the fragmentation of XeF2 molecules following X-ray absorption at the Xe site.« less

  11. Hetero-site-specific X-ray pump-probe spectroscopy for femtosecond intramolecular dynamics

    PubMed Central

    Picón, A.; Lehmann, C. S.; Bostedt, C.; Rudenko, A.; Marinelli, A.; 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.; Moonshiram, D.; Ray, D.; Young, L.; Pratt, S. T.; Southworth, S. H.

    2016-01-01

    New capabilities at X-ray free-electron laser facilities allow the generation of two-colour femtosecond X-ray pulses, opening the possibility of performing ultrafast studies of X-ray-induced phenomena. Particularly, the experimental realization of hetero-site-specific X-ray-pump/X-ray-probe spectroscopy is of special interest, in which an X-ray pump pulse is absorbed at one site within a molecule and an X-ray probe pulse follows the X-ray-induced dynamics at another site within the same molecule. Here we show experimental evidence of a hetero-site pump-probe signal. By using two-colour 10-fs X-ray pulses, we are able to observe the femtosecond time dependence for the formation of F ions during the fragmentation of XeF2 molecules following X-ray absorption at the Xe site. PMID:27212390

  12. Small pixel CZT detector for hard X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Wilson, Matthew David; Cernik, Robert; Chen, Henry; Hansson, Conny; Iniewski, Kris; Jones, Lawrence L.; Seller, Paul; Veale, Matthew C.

    2011-10-01

    A new small pixel cadmium zinc telluride (CZT) detector has been developed for hard X-ray spectroscopy. The X-ray performance of four detectors is presented and the detectors are analysed in terms of the energy resolution of each pixel. The detectors were made from CZT crystals grown by the travelling heater method (THM) bonded to a 20×20 application specific integrated circuit (ASIC) and data acquisition (DAQ) system. The detectors had an array of 20×20 pixels on a 250 μm pitch, with each pixel gold-stud bonded to an energy resolving circuit in the ASIC. The DAQ system digitised the ASIC output with 14 bit resolution, performing offset corrections and data storage to disc in real time at up to 40,000 frames per second. The detector geometry and ASIC design was optimised for X-ray spectroscopy up to 150 keV and made use of the small pixel effect to preferentially measure the electron signal. A 241Am source was used to measure the spectroscopic performance and uniformity of the detectors. The average energy resolution (FWHM at 59.54 keV) of each pixel ranged from 1.09±0.46 to 1.50±0.57 keV across the four detectors. The detectors showed good spectral performance and uniform response over almost all pixels in the 20×20 array. A large area 80×80 pixel detector will be built that will utilise the scalable design of the ASIC and the large areas of monolithic spectroscopic grade THM grown CZT that are now available. The large area detector will have the same performance as that demonstrated here.

  13. Hubbard Model Approach to X-ray Spectroscopy

    NASA Astrophysics Data System (ADS)

    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

  14. Individual heteroatom identification with X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Stroud, R. M.; Lovejoy, T. C.; Falke, M.; Bassim, N. D.; Corbin, G. J.; Dellby, N.; Hrncirik, P.; Kaeppel, A.; Noack, M.; Hahn, W.; Rohde, M.; Krivanek, O. L.

    2016-04-01

    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-1 pA-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.

  15. X-ray Spectroscopy and Magnetism in Mineralogy

    NASA Astrophysics Data System (ADS)

    Sainctavit, Philippe; Brice-Profeta, Sandrine; Gaudry, Emilie; Letard, Isabelle; Arrio, Marie-Anne

    The objective of this paper is to present the kind of information that can be gained in the field of mineralogy from the use of x-ray magnetic spectroscopies. We review some of the questions that are unsettled and that could benefit from an interdisciplinary approach where magnetism, spectroscopy and mineralogy could be mixed. Most of the attention is focused on iron and some other 3d transition elements. The mineralogy of planetary cores and its relation with known meteorites are exemplified. The various oxide phases in the mantle and the nature of iron in these phases is also underlined. The presence of transition elements in insulating minerals and its relation with macroscopic properties such as the color of gemstones are reviewed. Finally an introduction to paleomagnetism is given with a special attention to nanomaghemites.

  16. Astrophysics with Laboratory X-ray and EUV spectroscopy

    NASA Astrophysics Data System (ADS)

    Beiersdorfer, Peter

    2016-05-01

    Improvements in the spectral resolution of x-ray observatories have necessitated increasing accuracies in the spectral models used in the analysis of astrophysical data. In response, we have been carrying out laboratory measurements to assess the fidelity of the atomic data used in the models and to calibrate specific spectral diagnostics. The goal is to meet the current need for spectroscopic models to be able to predict line intensities on the order of a few percent for the strongest transitions and to represent line positions with spectroscopic accuracy. Our spectroscopy measurements are performed in the extreme ultraviolet and x-ray regimes and are mostly carried out at the electron beam ion trap facility at Livermore, which produces the relevant ions in a density and temperature environment similar to those of astrophysical plasmas. Examples discussed in this talk fall into four categories. (1) The identification of lines seen in astrophysical spectra but missing in the models; (2) the establishment of benchmark wavelengths for K-shell transitions in M-shell ions and for L-shell transitions in L-shell ions needed for the interpretation of absorption line features; (3) the calibration of the line emission of key spectroscopic diagnostics, such as the L-shell lines of Fe XVII; (4) the disentanglement of line excitation processes, especially those associated with charge exchange, that produce x-ray emission from comets, planets, and the interstellar medium. This work was performed under the auspices of the U.S. Department of Energy by LLNL under Contract DE-AC52-07NA27344 and supported by NASA's Astrophysics Research and Analysis Program under Contracts NNG14WF24I and NNG13WF99I.

  17. Femtosecond time-resolved X-ray absorption spectroscopy of liquid using a hard X-ray free electron laser in a dual-beam dispersive detection method.

    PubMed

    Obara, Yuki; Katayama, Tetsuo; Ogi, Yoshihiro; Suzuki, Takayuki; Kurahashi, Naoya; Karashima, Shutaro; Chiba, Yuhei; Isokawa, Yusuke; Togashi, Tadashi; Inubushi, Yuichi; Yabashi, Makina; Suzuki, Toshinori; Misawa, Kazuhiko

    2014-01-13

    We present femtosecond time-resolved X-ray absorption spectroscopy of aqueous solution using a hard x-ray free electron laser (SACLA) and a synchronized Ti:sapphire laser. The instrumental response time is 200 fs, and the repetition rate of measurement is 10 Hz. A cylindrical liquid beam 100 μm in diameter of aqueous ammonium iron(III) oxalate solution is photoexcited at 400 nm, and the transient X-ray absorption spectra are measured in the K-edge region of iron, 7.10 - 7.26 keV, using a dual X-ray beam dispersive detection method. Each of the dual beams has the pulse energy of 1.4 μJ, and pump-induced absorbance change on the order of 10(-3) is successfully detected. The photoexcited iron complex exhibits a red shifted iron K-edge with the appearance time constant of 260 fs. The X-ray absorption difference spectra, with and without the pump pulses, are independent of time delay after 1.5 ps up to 100 ps, indicating that the photoexcited species is long-lived.

  18. Phase-resolved X-ray spectroscopy and spectral energy distribution of the X-ray soft polar RS Caeli

    NASA Astrophysics Data System (ADS)

    Traulsen, I.; Reinsch, K.; Schwope, A. D.; Schwarz, R.; Walter, F. M.; Burwitz, V.

    2014-02-01

    Context. RS Cae is the third target in our series of XMM-Newton observations of soft X-ray-dominated polars. Aims: Our observational campaign aims to better understand and describe the multiwavelength data, the physical properties of the system components, and the short- and long-term behavior of the component fluxes in RS Cae. Methods: We employ stellar atmosphere, stratified accretion-column, and widely used X-ray spectral models. We fit the XMM-Newton spectra, model the multiband light curves, and opt for a mostly consistent description of the spectral energy distribution. Results: Our XMM-Newton data of RS Cae are clearly dominated by soft X-ray emission. The X-ray light curves are shaped by emission from the main accretion region, which is visible over the whole orbital cycle, interrupted only by a stream eclipse. The optical light curves are formed by cyclotron and stream emission. The XMM-Newton X-ray spectra comprise a black-body-like and a plasma component at mean temperatures of 36 eV and 7 keV. The spectral fits give evidence of a partially absorbing and a reflection component. Multitemperature models, covering a broader temperature range in the X-ray emitting accretion regions, reproduce the spectra appropriately well. Including archival data, we describe the spectral energy distribution with a combination of models based on a consistent set of parameters and derive a lower limit estimate of the distance d ≳ 750 pc. Conclusions: The high bolometric soft-to-hard flux ratios and short-term variability of the (X-ray) light curves are characteristic of inhomogeneous accretion. RS Cae clearly belongs in the group of polars that show a very strong soft X-ray flux compared to their hard X-ray flux. The different black-body fluxes and similar hard X-ray and optical fluxes during the XMM-Newton and ROSAT observations show that soft and hard X-ray emission are not directly correlated. Based on observations obtained with XMM-Newton, an ESA science mission with

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

    SciTech Connect

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

    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.

  20. Synchrotron Radiation X-Ray Spectroscopy for Investigations of Intracellular Metallointercalators: X-Ray Fluorescence Imaging and X-Ray Absorption Spectroscopy

    NASA Astrophysics Data System (ADS)

    Dillon, Carolyn T.

    In an effort to determine the therapeutic feasibility of DNA metallointercalators as potential anticancer drugs it is important to confirm that they are capable of targeting DNA in cancer cells or tumours - as is the intended purpose of their design. Microprobe synchrotron radiation X-ray fluorescence (micro-SRXRF) spectroscopy is an ideal technique for investigating the cellular uptake and distribution of metallointercalators. The technique is capable of submicron elemental imaging so that samples as small as individual cells (~10 μm diameter), and the features within them, can be resolved. Consequently, the technique can ascertain whether intracellular metallointercalators colocalise with DNA; namely, in the nucleus during interphase or at the chromosomes during middle prophase to late anaphase. Metals, such as those commonly incorporated into metallointercalators (e.g., Cr, Ni, Co, Pd, Pt, Ru, Rh), are often naturally present in negligible quantities in cancer cells. This fact, together with their higher atomic number, Z, makes them ideal for direct probing using hard X-ray microprobes (as discussed in Sect. 11.2). There is no need for the incorporation of fluorescent tracker dyes or radioactive labels into their chemical structure. This is advantageous since it is unknown whether such chemical modifications alter the uptake kinetics of the metallointercalator [1, 2].

  1. Polytetrafluoroethylene transfer film studied with X-ray photoelectron spectroscopy

    NASA Technical Reports Server (NTRS)

    Wheeler, D. R.

    1980-01-01

    Polytetrafluoroethylene (PTFE) was rubbed against nickel in ultrahigh vacuum at loads up to 3.9 N and speeds up to 94 mm/sec. The transfer film formed on the nickel was analyzed using X-ray phototectron spectroscopy. The film was indistinguishable from bulk PTFE except for the possible presence of a small amount of NiF2. The transfer film was found to be about 1 molecule (0.5 nm) thick under all conditions; but at speeds above 10 mm/sec, there was evidence of bulk transfer in the form of fragments as well. The thickness measurements required a choice among conflicting published values of the inelastic mean free path for electrons in polymers. The values chosen gave internally consistent results.

  2. VUV and soft x-ray spectroscopy of actinides

    SciTech Connect

    Olson, C. G.; Joyce, J. J.; Durakiewicz, T.; Guziewicz, E.

    2004-01-01

    Optical and photoelectron spectroscopies using VUV and Soft X-ray photons are powerful tools for studies of elemental and compound actinides. Large changes in the relative atomic cross sections of the 5f, 6d and sp electrons allow decomposition of the character of the valence bands using photoemission. Resonant enhancement of photoelectrons and Auger electrons at the 5d core threshold further aids the decomposition and gives a measure of elemental specificity. Angle-resolved photoemission can be used to map the momentum dependence of the electronic states. The large changes in relative cross section with photon energy yields further details when the mapping is done at equivalent points in multiple zones. Spectra for well understood rare earth materials will be presented to establish spectral characteristics for known atomic character initial states. These signatures will be applied to the case of USb to investigate f-d hybridization near the Fermi level.

  3. X-Ray Imaging-Spectroscopy of Abell 1835

    NASA Technical Reports Server (NTRS)

    Peterson, J. R.; Paerels, F. B. S.; Kaastra, J. S.; Arnaud, M.; Reiprich T. H.; Fabian, A. C.; Mushotzky, R. F.; Jernigan, J. G.; Sakelliou, I.

    2000-01-01

    We present detailed spatially-resolved spectroscopy results of the observation of Abell 1835 using the European Photon Imaging Cameras (EPIC) and the Reflection Grating Spectrometers (RGS) on the XMM-Newton observatory. Abell 1835 is a luminous (10(exp 46)ergs/s), medium redshift (z = 0.2523), X-ray emitting cluster of galaxies. The observations support the interpretation that large amounts of cool gas are present in a multi-phase medium surrounded by a hot (kT(sub e) = 8.2 keV) outer envelope. We detect O VIII Ly(alpha) and two Fe XXIV complexes in the RGS spectrum. The emission measure of the cool gas below kT(sub e) = 2.7 keV is much lower than expected from standard cooling-flow models, suggesting either a more complicated cooling process than simple isobaric radiative cooling or differential cold absorption of the cooler gas.

  4. Metalloprotein active site structure determination: synergy between X-ray absorption spectroscopy and X-ray crystallography.

    PubMed

    Cotelesage, Julien J H; Pushie, M Jake; Grochulski, Pawel; Pickering, Ingrid J; George, Graham N

    2012-10-01

    Structures of metalloprotein active sites derived from X-ray crystallography frequently contain chemical anomalies such as unexpected atomic geometries or elongated bond-lengths. Such anomalies are expected from the known errors inherent in macromolecular crystallography (ca. 0.1-0.2Å) and from the lack of appropriate restraints for metal sites which are often without precedent in the small molecule structure literature. Here we review the potential of X-ray absorption spectroscopy to provide information and perspective which could aid in improving the accuracy of metalloprotein crystal structure solutions. We also review the potential problem areas in analysis of the extended X-ray absorption fine structure (EXAFS) and discuss the use of density functional theory as another possible source of geometrical restraints for crystal structure analysis of metalloprotein active sites.

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

    SciTech Connect

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

    2015-07-15

    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.

  6. Electronic Structure of In2O3 from Resonant X-ray Emission Spectroscopy

    SciTech Connect

    Piper, L.; DeMasi, A; Cho, S; Smith, K; Fuchs, F; Bechstedt, F; Korber, C; Klein, A; Payne, D; Egdell, R

    2009-01-01

    The valence and conduction band structures of In2O3 have been measured using a combination of valence band x-ray photoemission spectroscopy, O K-edge resonant x-ray emission spectroscopy, and O K-edge x-ray absorption spectroscopy. Excellent agreement is noted between the experimental spectra and O 2p partial density of states calculated within hybrid density functional theory. Our data are consistent with a direct band gap for In2O3.

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

    SciTech Connect

    Orville, A.M.; Buono, R.; Cowan, M.; Heroux, A.; Shea-McCarthy, G.; Schneider, D. K.; Skinner, J. M.; Skinner, M. J.; Stoner-Ma, D.; Sweet, R. 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.

  8. Correlated Single-Crystal Electronic Absorption Spectroscopy and X-ray Crystallography at NSLS Beamline X26-C

    SciTech Connect

    A Orville; R Buono; M Cowan; A Heroux; G Shea-McCarthy; D Schneider; J Skinner; M Skinner; D Stoner-Ma; R Sweet

    2011-12-31

    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.

  9. Shakeup in soft-x-ray emission. II. Plasmon satellites and x-ray photoemission spectroscopy

    NASA Astrophysics Data System (ADS)

    Livins, Peteris; Schnatterly, S. E.

    1988-04-01

    We report the first observation of a plasmon satellite in the K emission spectrum of diamond. The previously identified plasmon satellites of Al and graphite are also presented, and data is compared with an oscillator model applicable to soft-x-ray emission and photoemission. The graphite satellite is shown to exhibit an anomalous location with respect to the parent emission. We report for the Al LI-LII,III core-core transitions a spin-orbit splitting of 0.42+/-0.02 eV with a Lorentzian width of 0.67+/-0.02 eV. The oscillator model applied to x-ray photoemission predicts a shift of the plasmon satellite with respect to the zero loss line as the final-electron kinetic energy is varied.

  10. Possible planetary XRF instrument with X-ray generator

    NASA Astrophysics Data System (ADS)

    Yin, Lo I.; Trombka, Jacob I.

    1986-01-01

    We explore in this paper the possibility of a planetary in situ XRF system using a newly developed battery-operated miniature X-ray generator as the excitation source. Furthermore, recent advances in refrigeration technology and HgI2 detectors make it possible to consider realistically the inclusion of a high-resolution energy-dispersive spectrometer as part of the system. It will be shown that by the simple coupling of the miniature X-ray generator and a standard Si(Li) detector qualitative characterization of geochemical samples can be easily carried out without elaborate calibrations and spectrum stripping. Similar battery-operated miniature X-ray generators with a variety of anodes are now commercially available.

  11. X-Ray Absorption Spectroscopy of Strontium(II) Coordination.

    PubMed

    Sahai; Carroll; Roberts; O'Day

    2000-02-15

    Sorption of dissolved strontium on kaolinite, amorphous silica, and goethite was studied as a function of pH, aqueous strontium concentration, the presence or absence of atmospheric CO(2) or dissolved phosphate, and aging over a 57-day period. Selected sorption samples ([Sr(aq)](i) approximately 0.5-1x10(-3) m) were examined with synchrotron X-ray absorption spectroscopy (XAS) at low (13-23 K) and room temperatures to determine the local molecular coordination around strontium. Quantitative analyses of the extended X-ray absorption fine structure (EXAFS) of kaolinite, amorphous silica, and most goethite sorption samples showed a single first shell of 9-10 (+/-1) oxygen atoms around strontium at an average Sr-O bond-distance of 2.61 (+/-0.02) Å, indicating hydrated surface complexes. The EXAFS spectra were unchanged after reaction for up to 57 days. Likewise, in kaolinite sorption samples prepared in 100% nitrogen atmosphere, the presence of dissolved phosphate (0.5x10(-3) m) in addition to strontium did not change the local coordination around strontium. In two goethite sorption samples reacted in air at pH approximately 8.5, the EXAFS spectra (collected at low and room temperature) clearly showed that the local structure around strontium is that of strontianite (SrCO(3)(s)). We also noted an increase in strontium uptake on goethite in the presence of atmospheric CO(2) in batch experiments, relative to CO(2)-free experiments. These observations suggest that sorption of carbonate may nucleate the precipitation of SrCO(3) in the pH range in which carbonate sorption on goethite is near a maximum. At higher pH, carbonate surface sorption decreases as dissolved CO(2) decreases. For goethite sorption samples above pH 8.6, hydrated surface complexes, rather than a precipitate, were observed in the EXAFS spectra. Copyright 2000 Academic Press.

  12. X-ray and EUV diagnostics for the Nevada Terawatt Facility: Plasma imaging, spectroscopy and polarimetry

    SciTech Connect

    Kantsyrev, V.L.; Bauer, B.S.; Mancini, R.C.

    1999-07-01

    A wide variety of advanced extreme ultraviolet (EUV) and x-ray diagnostics ar being developed for the Nevada Terawatt Facility (NTF) at the University of Nevada, Reno. Time-resolved short-wavelength imaging, backlighting, imaging spectroscopy, and polarization spectroscopy will be employed to measure profiles of plasma temperature, density, flow, charge state, and magnetic field. These diagnostics will be used to examine the early-time evolution of a current-driven wire, the formation of a plasma sheet from the explosion and merging of wires, etc. Wire materials will include Al, Ti, W, and various coatings (e.g., Mg, Ni, Cu). Doping of local regions of wires is planned, for additional spatial resolution of the plasma profiles. The instruments are state-of-the-art applications of glass capillary converters (GCC), multilayer mirrors (MLM), and crystals. The devices include: a prototype of a new glass-capillary-based two-dimensional imaging spectrometer; a pinhole camera with 6 MCP imagers; a 5-channel crystal/MLM spectrometer (Polychromator) with fast x-ray diodes and an added transmission grating spectrometer; a convex-crystal x-ray survey spectrometer; a prototype of an x-ray polarimeter/spectrometer; and a multiframe x-pinch backlighter yielding point-protection microscopy with few-micron, sub-ns resolution. Spectroscopic data will be interpreted with state-of-the-art spectral calculations that take into account line intensity, plasma broadening, opacity, and polarization effects, for both resonance and satellite lines. Emission spectroscopy will be used to measure plasma density and temperature in the hot plasma around exploding wires, with polarization measurements helping to determine the electron distribution function and the magnetic field in this region. The density and temperature of the high-density, low-temperature plasma inside exploding Al wires will be measured with absorption spectroscopy.

  13. Combined measurement of X-ray photon correlation spectroscopy and diffracted X-ray tracking using pink beam X-rays.

    PubMed

    Shinohara, Yuya; Watanabe, Akira; Kishimoto, Hiroyuki; Amemiya, Yoshiyuki

    2013-09-01

    Combined X-ray photon correlation spectroscopy (XPCS) and diffracted X-ray tracking (DXT) measurements of carbon-black nanocrystals embedded in styrene-butadiene rubber were performed. From the intensity fluctuation of speckle patterns in a small-angle scattering region (XPCS), dynamical information relating to the translational motion can be obtained, and the rotational motion is observed through the changes in the positions of DXT diffraction spots. Graphitized carbon-black nanocrystals in unvulcanized styrene-butadiene rubber showed an apparent discrepancy between their translational and rotational motions; this result seems to support a stress-relaxation model for the origin of super-diffusive particle motion that is widely observed in nanocolloidal systems. Combined measurements using these two techniques will give new insights into nanoscopic dynamics, and will be useful as a microrheology technique.

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

    NASA Astrophysics Data System (ADS)

    Mascali, David; Castro, Giuseppe; Biri, Sándor; Rácz, Richárd; Pálinkás, József; Caliri, Claudia; Celona, Luigi; Neri, Lorenzo; Romano, Francesco Paolo; Torrisi, Giuseppe; Gammino, Santo

    2016-02-01

    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.

  15. Application of X-ray synchrotron microscopy instrumentation in biology

    SciTech Connect

    Gasperini, F. M.; Pereira, G. R.; Granjeiro, J. M.; Calasans-Maia, M. D.; Rossi, A. M.; Perez, C. A.; Lopes, R. T.; Lima, I.

    2011-07-01

    X-ray micro-fluorescence imaging technique has been used as a significant tool in order to investigate minerals contents in some kinds of materials. The aim of this study was to evaluate the elemental distribution of calcium and zinc in bone substitute materials (nano-hydroxyapatite spheres) and cortical bones through X-Ray Micro-fluorescence analysis with the increment of Synchrotron Radiation in order to evaluate the characteristics of the newly formed bone and its interface, the preexisting bone and biomaterials by the arrangement of collagen fibers and its birefringence. The elemental mapping was carried out at Brazilian Synchrotron Light Laboratory, Campinas - Sao Paulo, Brazil working at D09-XRF beam line. Based on this study, the results suggest that hydroxyapatite-based biomaterials are biocompatible, promote osteo-conduction and favored bone repair. (authors)

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

    SciTech Connect

    Moler, E.J.; Hussain, Z.; Duarte, R.M.; Howells, M.R.

    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.

  17. Near Edge X-ray Absorption Spectroscopy of Polymers

    NASA Astrophysics Data System (ADS)

    Dhez, Olivier; Ade, Harald; Urquhart, Stephen

    2001-03-01

    Synthetic and natural polymers exhibit a rich carbon, nitrogen and oxygen K-edge Near Edge X-ray Absorption Fine Structure (NEXAFS). The spectroscopic variations with chemical structure and composition are interesting in their own right. In addition, the large spectroscopic variability can be utilized for the compositional analysis of materials. This is particularly useful for high spatial resolution NEXAFS microanalysis at lateral spatial resolutions exceeding that achievable with more traditional compositional analysis tools such as Infrared and NMR spectroscopy. To increase our understanding of NEXAFS spectra and to start a database for microanalysis, we acquired carbon NEXAFS spectra of the following polymers: polycarbonate, poly(oxybenzoate-co-2,6oxynaphthoate), poly (p-phenylene terephtalamide), toluene diisocyanate polyurethane, toluene diisocyanate polyurea, 4,4'-methylene di-p-phenylene isocyanate polyurethane, 4,4'-methylene di-p-phenylene isocyanate polyurea, poly(ether ether ketone), poly(alpha-methylstyrene), poly-styrene, poly bromostyrene, poly(2-vinyl styrene), polyethylene, poly(ethylene oxide), polypropylene, poly(propylene oxide), polyisobutylene, ethylene propylene rubber, poly(methyl -metacrylate). These spectra were obtained in transmission with an energy resolution of 150 meV. The energy scale was carefully calibrated in-situ utilizing C02 gas as a reference. Spectral assignments are made based on model compounds and theoretical calculations.

  18. Testing black holes via X-ray reflection spectroscopy

    NASA Astrophysics Data System (ADS)

    Bambi, Cosimo; Nampalliwar, Sourabh; Cardenas-Avendano, Alejandro

    2016-07-01

    Astrophysical black hole candidates are thought to be the Kerr black holes of general relativity. However, a direct observational evidence is still lacking. The study of the properties of the radiation emitted by gas in the inner part of the accretion disk can provide useful information on the spacetime geometry around these compact objects and test the Kerr black hole hypothesis. The iron line method is the most promising techniques to test black hole candidates. In this talk, we present a new reflection model for testing the Kerr black hole hypothesis. We use the formalism of the transfer function and we split the calculations into two blocks. One is the calculation of the transfer function, which takes into account all the relativistic effects and only depends on the background metric. The second block is the calculation of the intrinsic spectrum in the rest frame of the gas. We have developed a code to compute transfer functions in arbitrary stationary and axisymmetric spacetimes. The transfer functions are tabulated in FITS files and combined with XILLVER, which is the best reflection code available today. The result is best model to test black hole candidates via X-ray reflection spectroscopy.

  19. X-ray Imaging and Spectroscopy in Space

    NASA Astrophysics Data System (ADS)

    Schnopper, Herbert

    2002-04-01

    Extra-solar X-ray astronomy became a reality in 1962 after a successful rocket flight discovered an X-ray source in the constellation Scorpius. The X-ray "telescope" consisted of a roughly collimated Geiger counter. New sources were discovered by many groups in a rapid series of rocket flights that were characterized by finer angular and spectral measurements made with better mechanical collimators and proportional detectors. These discoveries led to the association of the newly discovered X-ray sources with objects already know in other wavelength bands. It was quickly understood that high precision measurements of angular position, spectral features and timing fluctuations were needed to make physical sense of the X-ray data and to put it into the context of the wealth of data obtained from other wavelength bands. These needs were met by a succession of major missions that began with UHURU (1970) and followed with the X-ray telescopes on EINSTEIN (1977), EXOSAT (1983), ROSAT (1990), GINGA (1987), ASCA (1993), CHANDRA (1999) and XMM.(1999). Each brought greater precision to measurements that allowed highly refined interpretations of the properties of x-ray sources. Several of the technical milestones that made these advances possible will be discussed.

  20. Electron Spectroscopy: Ultraviolet and X-Ray Excitation.

    ERIC Educational Resources Information Center

    Baker, A. D.; And Others

    1980-01-01

    Reviews recent growth in electron spectroscopy (54 papers cited). Emphasizes advances in instrumentation and interpretation (52); photoionization, cross-sections and angular distributions (22); studies of atoms and small molecules (35); transition, lanthanide and actinide metal complexes (50); organometallic (12) and inorganic compounds (2);…

  1. Flares from small to large: X-ray spectroscopy of Proxima Centauri with XMM-Newton

    NASA Astrophysics Data System (ADS)

    Güdel, M.; Audard, M.; Reale, F.; Skinner, S. L.; Linsky, J. L.

    2004-03-01

    We report results from a comprehensive study of the nearby M dwarf Proxima Centauri with the XMM-Newton satellite, using simultaneously its X-ray detectors and the Optical Monitor with its U band filter. We find strongly variable coronal X-ray emission, with flares ranging over a factor of 100 in peak flux. The low-level emission is found to be continuously variable on at least three time scales (a slow decay of several hours, modulation on a time scale of 1 hr, and weak flares with time scales of a few minutes). Several weak flares are characteristically preceded by an optical burst, compatible with predictions from standard solar flare models. We propose that the U band bursts are proxies for the elusive stellar non-thermal hard X-ray bursts suggested from solar observations. In the course of the observation, a very large X-ray flare started and was observed essentially in its entirety. Its peak luminosity reached 3.9× 1028 erg s-1 [0.15-10 keV], and the total X-ray energy released in the same band is derived to be 1.5× 1032 ergs. This flare has for the first time allowed to measure significant density variations across several phases of the flare from X-ray spectroscopy of the O VII He-like triplet; we find peak densities reaching up to 4× 1011 cm-3 for plasma of about 1-5 MK. Abundance ratios show little variability in time, with a tendency of elements with a high first ionization potential to be overabundant relative to solar photospheric values. Using Fe XVII lines with different oscillator strengths, we do not find significant effects due to opacity during the flare, indicating that large opacity increases are not the rule even in extreme flares. We model the large flare in terms of an analytic 2-Ribbon flare model and find that the flaring loop system should have large characteristic sizes (≈ 1R*) within the framework of this simplistic model. These results are supported by full hydrodynamic simulations. Comparing the large flare to flares of similar

  2. A new endstation at the Swiss Light Source for ultraviolet photoelectron spectroscopy, X-ray photoelectron spectroscopy, and X-ray absorption spectroscopy measurements of liquid solutions.

    PubMed

    Brown, Matthew A; Redondo, Amaia Beloqui; Jordan, Inga; Duyckaerts, Nicolas; Lee, Ming-Tao; Ammann, Markus; Nolting, Frithjof; Kleibert, Armin; Huthwelker, Thomas; Müächler, Jean-Pierre; Birrer, Mario; Honegger, Juri; Wetter, Reto; Wörner, Hans Jakob; van Bokhoven, Jeroen A

    2013-07-01

    A new liquid microjet endstation designed for ultraviolet (UPS) and X-ray (XPS) photoelectron, and partial electron yield X-ray absorption (XAS) spectroscopies at the Swiss Light Source is presented. The new endstation, which is based on a Scienta HiPP-2 R4000 electron spectrometer, is the first liquid microjet endstation capable of operating in vacuum and in ambient pressures up to the equilibrium vapor pressure of liquid water at room temperature. In addition, the Scienta HiPP-2 R4000 energy analyzer of this new endstation allows for XPS measurements up to 7000 eV electron kinetic energy that will enable electronic structure measurements of bulk solutions and buried interfaces from liquid microjet samples. The endstation is designed to operate at the soft X-ray SIM beamline and at the tender X-ray Phoenix beamline. The endstation can also be operated using a Scienta 5 K ultraviolet helium lamp for dedicated UPS measurements at the vapor-liquid interface using either He I or He II α lines. The design concept, first results from UPS, soft X-ray XPS, and partial electron yield XAS measurements, and an outlook to the potential of this endstation are presented. PMID:23902081

  3. A new endstation at the Swiss Light Source for ultraviolet photoelectron spectroscopy, X-ray photoelectron spectroscopy, and X-ray absorption spectroscopy measurements of liquid solutions

    SciTech Connect

    Brown, Matthew A.; Redondo, Amaia Beloqui; Duyckaerts, Nicolas; Mächler, Jean-Pierre; Jordan, Inga; Wörner, Hans Jakob; Lee, Ming-Tao; Ammann, Markus; Nolting, Frithjof; Kleibert, Armin; Huthwelker, Thomas; Birrer, Mario; Honegger, Juri; Wetter, Reto; Bokhoven, Jeroen A. van

    2013-07-15

    A new liquid microjet endstation designed for ultraviolet (UPS) and X-ray (XPS) photoelectron, and partial electron yield X-ray absorption (XAS) spectroscopies at the Swiss Light Source is presented. The new endstation, which is based on a Scienta HiPP-2 R4000 electron spectrometer, is the first liquid microjet endstation capable of operating in vacuum and in ambient pressures up to the equilibrium vapor pressure of liquid water at room temperature. In addition, the Scienta HiPP-2 R4000 energy analyzer of this new endstation allows for XPS measurements up to 7000 eV electron kinetic energy that will enable electronic structure measurements of bulk solutions and buried interfaces from liquid microjet samples. The endstation is designed to operate at the soft X-ray SIM beamline and at the tender X-ray Phoenix beamline. The endstation can also be operated using a Scienta 5 K ultraviolet helium lamp for dedicated UPS measurements at the vapor-liquid interface using either He I or He II α lines. The design concept, first results from UPS, soft X-ray XPS, and partial electron yield XAS measurements, and an outlook to the potential of this endstation are presented.

  4. The Soft X-ray research instrument at the Linac Coherent Light Source

    DOE PAGESBeta

    Dakovski, Georgi L.; Heimann, Philip; Holmes, Michael; Krupin, Oleg; European XFEL, Hamburg; Minitti, Michael P.; Mitra, Ankush; Moeller, Stefan; Rowen, Michael; Schlotter, William F.; et al

    2015-04-02

    The Soft X-ray Research instrument provides intense ultrashort X-ray pulses in the energy range 280–2000 eV. A diverse set of experimental stations may be installed to investigate a broad range of scientific topics such as ultrafast chemistry, highly correlated materials, magnetism, surface science, and matter under extreme conditions. A brief description of the main instrument components will be given, followed by some selected scientific highlights.

  5. Johann Spectrometer for High Resolution X-ray Spectroscopy

    SciTech Connect

    Machek, Pavel; Froeba, Michael; Welter, Edmund; Caliebe, Wolfgang; Brueggmann, Ulf; Draeger, Guenter

    2007-01-19

    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 {mu}m 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 5x1010photons/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.

  6. Johann Spectrometer for High Resolution X-ray Spectroscopy

    NASA Astrophysics Data System (ADS)

    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.

  7. TES-based microcalorimeter for future X-ray astronomy missions. Software development for instrument calibration

    NASA Astrophysics Data System (ADS)

    Fraga-Encinas, R.; Cobo, B.; Ceballos, M.; Schuurmans, J.; van der Kuur, J.; Carrera, F.; Barcons, X.

    2013-05-01

    The XMS (X-ray Microcalorimeter Spectrometer) is an instrument prototype with imaging capability in X-rays and high-spectral resolution. This instrument is a microcalorimeter based on transition edge sensors. As part of the Spanish contribution to the advancement of the XMS, we present the work carried out by the X-ray astronomy group at the Instituto de Física de Cantabria in collaboration with The Netherlands Institute for Space Research. The main work hereby presented includes the development and testing of software for this prototype with the purpose of instrument calibration and characterization, X-ray pulse detection and energy resolution calculations (Bergmann 2004, Tekst. Proefschrift Universiteit Utrecht; Boyce et al. 1999, Proc SPIE 3765; Den Herder et al. 2011, SRON-XMS-RP-2011-033; ATHENA Assessment Study Report, ESA/SRE(2011)17)

  8. Detection limits for actinides in a monochromatic, wavelength-dispersive x-ray fluorescence instrument

    SciTech Connect

    Collins, Michael L; Havrilla, George J

    2009-01-01

    Recent developments in x-ray optics have made it possible to examine the L x-rays of actinides using doubly-curved crystals in a bench-top device. A doubly-curved crystal (DCC) acts as a focusing monochromatic filter for polychromatic x-rays. A Monochromatic, Wavelength-Dispersive X-Ray Fluorescence (MWDXRF) instrument that uses DCCs to measure Cm and Pu in reprocessing plant liquors was proposed in 2007 by the authors at Los Alamos National Laboratory. A prototype design of this MWDXRF instrument was developed in collaboration with X-ray Optical Systems Inc. (XOS), of East Greenbush, New York. In the MWDXRF instrument, x-rays from a Rhodium-anode x-ray tube are passed through a primary DCC to produce a monochromatic beam of 20.2-keV photons. This beam is focused on a specimen that may contain actinides. The 20.2-keV interrogating beam is just above the L3 edge of Californium; each actinide (with Z = 90 to 98) present in the specimen emits characteristic L x-rays as the result of L3-shell vacancies. In the LANL-XOS prototype MWDXRf, these x-rays enter a secondary DCC optic that preferentially passes 14.961-keV photons, corresponding to the L-alpha-1 x-ray peak of Curium. In the present stage of experimentation, Curium-bearing specimens have not been analyzed with the prototype MWDXRF instrument. Surrogate materials for Curium include Rubidium, which has a K-beta-l x-ray at 14.961 keV, and Yttrium, which has a K-alpha-1 x-ray at 14.958 keV. In this paper, the lower limit of detection for Curium in the LANL-XOS prototype MWDXRF instrument is estimated. The basis for this estimate is described, including a description of computational models and benchmarking techniques used. Detection limits for other actinides are considered, as well as future safeguards applications for MWDXRF instrumentation.

  9. Centaurus X-3. [early x-ray binary star spectroscopy

    NASA Technical Reports Server (NTRS)

    Hutchings, J. B.; Cowley, A. P.; Crampton, D.; Van Paradus, J.; White, N. E.

    1979-01-01

    Spectroscopic observations of Krzeminski's star at dispersions 25-60 A/mm are described. The primary is an evolved star of type O6-O8(f) with peculiarities, some of which are attributable to X-ray heating. Broad emission lines at 4640A (N III), 4686 A(He II) and H-alpha show self-absorption and do not originate entirely from the region near the X-ray star. The primary is not highly luminous (bolometric magnitude about -9) and does not show signs of an abnormally strong stellar wind. The X-ray source was 'on' at the time of optical observations. Orbital parameters are presented for the primary, which yield masses of 17 + or - 2 and 1.0 + or - 3 solar masses for the stars. The optical star is undermassive for its luminosity, as are other OB-star X-ray primaries. The rotation is probably synchronized with the orbital motion. The distance to Cen X-3 is estimated to be 10 + or - 1 kpc. Basic data for 12 early-type X-ray primaries are discussed briefly

  10. Double conical crystal x-ray spectrometer for high resolution ultrafast x-ray absorption near-edge spectroscopy of Al K edge

    SciTech Connect

    Levy, A.; Dorchies, F.; Fourment, C.; Harmand, M.; Hulin, S.; Santos, J. J.; Descamps, D.; Petit, S.; Bouillaud, R.

    2010-06-15

    An x-ray spectrometer devoted to dynamical studies of transient systems using the x-ray absorption fine spectroscopy technique is presented in this article. Using an ultrafast laser-induced x-ray source, this optical device based on a set of two potassium acid phthalate conical crystals allows the extraction of x-ray absorption near-edge spectroscopy structures following the Al absorption K edge. The proposed experimental protocol leads to a measurement of the absorption spectra free from any crystal reflectivity defaults and shot-to-shot x-ray spectral fluctuation. According to the detailed analysis of the experimental results, a spectral resolution of 0.7 eV rms and relative fluctuation lower than 1% rms are achieved, demonstrated to be limited by the statistics of photon counting on the x-ray detector.

  11. X27A - A New Hard X-ray Micro-Spectroscopy Facility at the National Synchrtron Light Source

    SciTech Connect

    Ablett,J.; Kao, C.; Reeder, R.; Tang, Y.; Lanzirotti, A.

    2006-01-01

    A new hard X-ray micro-spectroscopy beamline has recently been installed at bending-magnet beamline X27A at the National Synchrotron Light Source, where the focus of research is primarily directed towards the environmental, geological and materials science communities. This instrument delivers moderate, {approx}10 {micro}m spatial resolution using achromatic dynamically bent Kirkpatrick-Baez mirrors, in addition to providing high X-ray flux throughput and selectable energy resolution. The balance between moderate spatial resolution and high flux throughput, in combination with a liquid nitrogen-cooled 13-element energy-dispersive high-purity germanium detector, is particularly well suited to the investigation of dilute and thin-film systems using the fluorescence X-ray absorption fine-structure mode of detection. In this paper, we report on the design and performance of this instrument and highlight a recent experimental study undertaken at this facility.

  12. Examination of the local structure in composite and lowdimensional semiconductor by X-ray Absorption Spectroscopy

    SciTech Connect

    Lawniczak-Jablonska, K.; Demchenko, I.N.; Piskorska, E.; Wolska,A.; Talik, E.; Zakharov, D.N.; Liliental-Weber, Z.

    2006-09-25

    X-ray absorption methods have been successfully used to obtain quantitative information about local atomic composition of two different materials. X-ray Absorption Near Edge Structure analysis and X-Ray Photoelectron Spectroscopy allowed us to determine seven chemical compounds and their concentrations in c-BN composite. Use of Extended X-ray Absorption Fine Structure in combination with Transmission Electron Microscopy enabled us to determine the composition and size of buried Ge quantum dots. It was found that the quantum dots consisted out of pure Ge core covered by 1-2 monolayers of a layer rich in Si.

  13. X-ray and optical spectroscopy of the massive young open cluster IC 1805

    NASA Astrophysics Data System (ADS)

    Rauw, G.; Nazé, Y.

    2016-10-01

    Context. Very young open clusters are ideal places to study the X-ray properties of a homogeneous population of early-type stars. In this respect, the IC 1805 open cluster is very interesting as it hosts the O4 If+ star HD 15570 thought to be in an evolutionary stage intermediate between a normal O-star and a Wolf-Rayet star. Aims: Such a star could provide a test for theoretical models aiming at explaining the empirical scaling relation between the X-ray and bolometric luminosities of O-type stars. Methods: We have observed IC 1805 with XMM-Newton and further collected optical spectroscopy of some of the O-star members of the cluster. Results: The optical spectra allow us to revisit the orbital solutions of BD+60° 497 and HD 15558, and provide the first evidence of binarity for BD+60° 498. X-ray emission from colliding winds does not appear to play an important role among the O-stars of IC 1805. Notably, the X-ray fluxes do not vary significantly between archival X-ray observations and our XMM-Newton pointing. The very fast rotator BD+60° 513, and to a lesser extent the O4 If+ star HD 15570 appear somewhat underluminous. Whilst the underluminosity of HD 15570 is only marginally significant, its amplitude is found to be compatible with theoretical expectations based on its stellar and wind properties. A number of other X-ray sources are detected in the field, and the brightest objects, many of which are likely low-mass pre-main sequence stars, are analyzed in detail. Based on observations collected with XMM-Newton, an ESA science mission with instruments and contributions directly funded by ESA member states and the USA (NASA), and with the TIGRE telescope (La Luz, Mexico).Table A.1 is only available at the CDS via anonymous ftp to http://cdsarc.u-strasbg.fr (http://130.79.128.5) or via http://cdsarc.u-strasbg.fr/viz-bin/qcat?J/A+A/594/A82

  14. X-ray spectroscopy studies of nonradiative energy transfer processes in luminescent lanthanide materials

    NASA Astrophysics Data System (ADS)

    Pacold, Joseph I.

    having a strong charge-transfer character. A second primary result comes from an an x-ray excited optical luminescence (XEOL) study that demonstrates, for the first time, that the high flux of modern synchrotron light sources can induce high fractional populations of excited states in trivalent lanthanide phosphors. In this work we have identified the leading-order nonlinear-response mechanism by drawing on strong similarities between XEOL and cathodoluminescence. These results establish the groundwork for studies that would allow deeper inquiry into energy-transfer mechanisms through time-resolved x-ray pump/optical-probe spectroscopies, through time-resolved x-ray emission spectroscopy, or through quantifying of higher-order nonlinear effects at further-enhanced fractional excitation levels. The above scientific results are augmented by a supporting effort in instrumental methodology. This includes the development of high-efficiency x-ray emission spectrometers and their use in collaborations to study pressure-induced changes in f-electron physics and to characterize the intermediate states that occur after photoexcitation of the photosystem-II protein.

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

    NASA Astrophysics Data System (ADS)

    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.

  16. Application of confocal X-ray fluorescence micro-spectroscopy to the investigation of paint layers.

    PubMed

    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.

  17. The soft x-ray instrument for materials studies at the linac coherent light source x-ray free-electron laser

    SciTech Connect

    Schlotter, W. F.; Turner, J. J.; Rowen, M.; Holmes, M.; Messerschmidt, M.; Moeller, S.; Krzywinski, J.; Lee, S.; Coffee, R.; Hays, G.; Heimann, P.; Krupin, O.; Soufli, R.; Fernandez-Perea, M.; Hau-Riege, S.; Kelez, N.; Beye, M.; Gerken, N.; Sorgenfrei, F.; Wurth, W.; and others

    2012-04-15

    The soft x-ray materials science instrument is the second operational beamline at the linac coherent light source x-ray free electron laser. The instrument operates with a photon energy range of 480-2000 eV and features a grating monochromator as well as bendable refocusing mirrors. A broad range of experimental stations may be installed to study diverse scientific topics such as: ultrafast chemistry, surface science, highly correlated electron systems, matter under extreme conditions, and laboratory astrophysics. Preliminary commissioning results are presented including the first soft x-ray single-shot energy spectrum from a free electron laser.

  18. An instrument for combining x-ray multiple diffraction and x-ray topographic imaging for examining crystal microcrystallography and perfection

    SciTech Connect

    Lai, X.; Ma, C. Y.; Roberts, K. J.; Cardoso, L. P.; Santos, A. O. dos; Bogg, D.; Miller, M. C.

    2009-03-15

    Diffraction imaging using x-ray topography (XRT) and x-ray multiple diffraction (XRMD) provide valuable tools for examining the growth defects in crystals and the distributions from ideal lattice symmetry (microcrystallography). The topographic x-ray multiple diffraction microprobe (TMDM) combines the complementary aspects of both techniques enabling XRT and XRMD studies within the same instrument providing a useful resource for the structural characterization of materials that are not very stable in vacuum and electron beam environments. The design of the TMDM instrument is described together with data taken on GaAs (001) and potassium dihydrogen phosphate (001)

  19. Corrosion and degradation studies utilizing X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Hixson, Holly Gwyndolen

    1997-08-01

    This dissertation involves studies of corrosion behavior at the surface of various metal samples, as well as the degradation of wool fibers obtained from the Star-Spangled Banner. Molybdenum metal and iron-zinc alloys were examined under corrosive conditions, and the degradation of the wool fibers was studied. The behavior of a polished molybdenum metal surface upon exposure to both aerated and deaerated water and 1.0 M NaCl solution was studied by X-ray Photoelectron Spectroscopy (XPS). Exposure to deaerated water and NaCl failed to produce oxidation of the metal surfaces, but exposing the polished metal surface to aerated water produced significant oxidation. Metal surfaces cleaned by argon-ion etching were found to be inert to oxidation by aerated water. The etching process also appears to passivate the metal surface. The behavior of molybdenum metal in 0.5 M Hsb2SOsb4 treated at various potentials has been studied using core and valence band XPS. The study indicates that Mosp{IV} and Mosp{VI} (including possibly Mosp{V} in some cases) were formed as the potential of the system was increased within the active range of molybdenum. The corrosive behavior of iron-zinc alloys that have been electroplated on plain steel in both aerated and deaerated quadruply-distilled water has been studied using XPS. Several different iron-zinc alloys were electroplated for comparative purposes: an iron-rich alloy, a zinc-rich alloy, and an alloy of similar iron and zinc composition. Treatment in aerated water produces oxidation for the iron-rich and similar composition alloys, but the oxide is reduced for the zinc-rich alloy. Degradation of the fibers in the original Star-Spangled Banner has been monitored using XPS and Scanning Electron Microscopy (SEM). Comparison of white and red wool fibers and linen fibers from the flag with new, mechanically-abraded, and chemically-treated white, red, and linen fibers, respectively, was performed in an attempt to determine the fibers' levels

  20. Si(Li) X-ray astronomical spectroscopy

    NASA Technical Reports Server (NTRS)

    Holt, S. S.

    1975-01-01

    The general considerations involved in the choice of Si(Li) as a non-dispersive spectrometer for X-ray astronomy are discussed. In particular, its adaptation to HEAO-B is described as an example of the space-borne application of Si(Li) technology.

  1. The Coherent X-ray Imaging instrument at the Linac Coherent Light Source

    SciTech Connect

    Liang, Mengning; Williams, Garth J.; Messerschmidt, Marc; Seibert, M. Marvin; Montanez, Paul A.; Hayes, Matt; Milathianaki, Despina; Aquila, Andrew; Hunter, Mark S.; Koglin, Jason E.; Schafer, Donald W.; Guillet, Serge; Busse, Armin; Bergan, Robert; Olson, William; Fox, Kay; Stewart, Nathaniel; Curtis, Robin; Miahnahri, Alireza Alan; Boutet, Sébastien

    2015-04-15

    The Coherent X-ray Imaging (CXI) instrument specializes in hard X-ray, in-vacuum, high power density experiments in all areas of science. Two main sample chambers, one containing a 100 nm focus and one a 1 µm focus, are available, each with multiple diagnostics, sample injection, pump–probe and detector capabilities. The flexibility of CXI has enabled it to host a diverse range of experiments, from biological to extreme matter.

  2. New Homogeneous Standards by Atomic Layer Deposition for Synchrotron X-ray Fluorescence and Absorption Spectroscopies.

    SciTech Connect

    Butterworth, A.L.; Becker, N.; Gainsforth, Z.; Lanzirotti, A.; Newville, M.; Proslier, T.; Stodolna, J.; Sutton, S.; Tyliszczak, T.; Westphal, A.J.; Zasadzinski, J.

    2012-03-13

    Quantification of synchrotron XRF analyses is typically done through comparisons with measurements on the NIST SRM 1832/1833 thin film standards. Unfortunately, these standards are inhomogeneous on small scales at the tens of percent level. We are synthesizing new homogeneous multilayer standards using the Atomic Layer Deposition technique and characterizing them using multiple analytical methods, including ellipsometry, Rutherford Back Scattering at Evans Analytical, Synchrotron X-ray Fluorescence (SXRF) at Advanced Photon Source (APS) Beamline 13-ID, Synchrotron X-ray Absorption Spectroscopy (XAS) at Advanced Light Source (ALS) Beamlines 11.0.2 and 5.3.2.1 and by electron microscopy techniques. Our motivation for developing much-needed cross-calibration of synchrotron techniques is borne from coordinated analyses of particles captured in the aerogel of the NASA Stardust Interstellar Dust Collector (SIDC). The Stardust Interstellar Dust Preliminary Examination (ISPE) team have characterized three sub-nanogram, {approx}1{micro}m-sized fragments considered as candidates to be the first contemporary interstellar dust ever collected, based on their chemistries and trajectories. The candidates were analyzed in small wedges of aerogel in which they were extracted from the larger collector, using high sensitivity, high spatial resolution >3 keV synchrotron x-ray fluorescence spectroscopy (SXRF) and <2 keV synchrotron x-ray transmission microscopy (STXM) during Stardust ISPE. The ISPE synchrotron techniques have complementary capabilities. Hard X-ray SXRF is sensitive to sub-fg mass of elements Z {ge} 20 (calcium) and has a spatial resolution as low as 90nm. X-ray Diffraction data were collected simultaneously with SXRF data. Soft X-ray STXM at ALS beamline 11.0.2 can detect fg-mass of most elements, including cosmochemically important oxygen, magnesium, aluminum and silicon, which are invisible to SXRF in this application. ALS beamline 11.0.2 has spatial resolution

  3. The BioCAT undulator beamline 18ID: A facility for biological non-crystalline diffraction and x-ray absorption spectroscopy at the APS

    SciTech Connect

    Fischetti, R.; Stepanov, S.; Rosenbaum, G.; Barrea, R.; Black, E.; Gore, D.; Heurich, R.; Kondrashkina, E.; Kropf, A.J.; Wang, S.; Zhang, K.; Irving, T.C.; Bunker, G.B.

    2008-07-02

    The 18ID undulator beamline of the Biophysics Collaborative Access Team at the Advanced Photon Source, Argonne, IL, USA, is a high-performance instrument designed for, and dedicated to, the study of partially ordered and disordered biological materials using the techniques of small-angle X-ray scattering, fiber diffraction, and X-ray absorption spectroscopy. The beamline and associated instrumentation are described in detail and examples of the representative experimental results are presented.

  4. Development of Compton X-ray spectrometer for high energy resolution single-shot high-flux hard X-ray spectroscopy.

    PubMed

    Kojima, Sadaoki; Ikenouchi, Takahito; Arikawa, Yasunobu; Sakata, Shohei; Zhang, Zhe; Abe, Yuki; Nakai, Mitsuo; Nishimura, Hiroaki; Shiraga, Hiroyuki; Ozaki, Tetsuo; Miyamoto, Shuji; Yamaguchi, Masashi; Takemoto, Akinori; Fujioka, Shinsuke; Azechi, Hiroshi

    2016-04-01

    Hard X-ray spectroscopy is an essential diagnostics used to understand physical processes that take place in high energy density plasmas produced by intense laser-plasma interactions. A bundle of hard X-ray detectors, of which the responses have different energy thresholds, is used as a conventional single-shot spectrometer for high-flux (>10(13) photons/shot) hard X-rays. However, high energy resolution (Δhv/hv < 0.1) is not achievable with a differential energy threshold (DET) X-ray spectrometer because its energy resolution is limited by energy differences between the response thresholds. Experimental demonstration of a Compton X-ray spectrometer has already been performed for obtaining higher energy resolution than that of DET spectrometers. In this paper, we describe design details of the Compton X-ray spectrometer, especially dependence of energy resolution and absolute response on photon-electron converter design and its background reduction scheme, and also its application to the laser-plasma interaction experiment. The developed spectrometer was used for spectroscopy of bremsstrahlung X-rays generated by intense laser-plasma interactions using a 200 μm thickness SiO2 converter. The X-ray spectrum obtained with the Compton X-ray spectrometer is consistent with that obtained with a DET X-ray spectrometer, furthermore higher certainly of a spectral intensity is obtained with the Compton X-ray spectrometer than that with the DET X-ray spectrometer in the photon energy range above 5 MeV. PMID:27131669

  5. Development of Compton X-ray spectrometer for high energy resolution single-shot high-flux hard X-ray spectroscopy.

    PubMed

    Kojima, Sadaoki; Ikenouchi, Takahito; Arikawa, Yasunobu; Sakata, Shohei; Zhang, Zhe; Abe, Yuki; Nakai, Mitsuo; Nishimura, Hiroaki; Shiraga, Hiroyuki; Ozaki, Tetsuo; Miyamoto, Shuji; Yamaguchi, Masashi; Takemoto, Akinori; Fujioka, Shinsuke; Azechi, Hiroshi

    2016-04-01

    Hard X-ray spectroscopy is an essential diagnostics used to understand physical processes that take place in high energy density plasmas produced by intense laser-plasma interactions. A bundle of hard X-ray detectors, of which the responses have different energy thresholds, is used as a conventional single-shot spectrometer for high-flux (>10(13) photons/shot) hard X-rays. However, high energy resolution (Δhv/hv < 0.1) is not achievable with a differential energy threshold (DET) X-ray spectrometer because its energy resolution is limited by energy differences between the response thresholds. Experimental demonstration of a Compton X-ray spectrometer has already been performed for obtaining higher energy resolution than that of DET spectrometers. In this paper, we describe design details of the Compton X-ray spectrometer, especially dependence of energy resolution and absolute response on photon-electron converter design and its background reduction scheme, and also its application to the laser-plasma interaction experiment. The developed spectrometer was used for spectroscopy of bremsstrahlung X-rays generated by intense laser-plasma interactions using a 200 μm thickness SiO2 converter. The X-ray spectrum obtained with the Compton X-ray spectrometer is consistent with that obtained with a DET X-ray spectrometer, furthermore higher certainly of a spectral intensity is obtained with the Compton X-ray spectrometer than that with the DET X-ray spectrometer in the photon energy range above 5 MeV.

  6. Electrochemical in-situ reaction cell for X-ray scattering, diffraction and spectroscopy

    SciTech Connect

    Braun, Artur; Granlund, Eric; Cairns, Elton J.

    2003-01-27

    An electrochemical in-situ reaction cell for hard X-ray experiments with battery electrodes is described. Applications include the small angle scattering, diffraction, and near-edge spectroscopy of lithium manganese oxide electrodes.

  7. Instrument for x-ray magnetic circular dichroism measurements at high pressures

    SciTech Connect

    Haskel, D.; Tseng, Y. C.; Lang, J. C.; Sinogeikin, S.

    2007-08-15

    An instrument has been developed for x-ray magnetic circular dichroism (XMCD) measurements at high pressures and low temperatures. This instrument couples a nonmagnetic copper-beryllium diamond anvil cell featuring perforated diamonds with a helium flow cryostat and an electromagnet. The applied pressure can be controlled in situ using a gas membrane and calibrated using Cu K-edge x-ray absorption fine structure measurements. The performance of this instrument was tested by measuring the XMCD spectra of the Gd{sub 5}Si{sub 2}Ge{sub 2} giant magnetocaloric material.

  8. A New Instrument for the Measurement of the Waveform in X-Ray Units

    NASA Astrophysics Data System (ADS)

    Ramírez-Jiménez, Francisco J.; Martínez-Hernández, Marco A.

    2004-09-01

    The experience gained in the quality control in X-ray units used in Radiology has demonstrated that the measurement of the waveform of the X-ray beam, measured as the response of a radiation detector is very helpful to decide if the unit fulfills the quality control requirements and also has been useful to define some kind of faults in the unit. Several instruments are available on the market to make this measurement but they need in general a storage or digital oscilloscope to see the waveform. In this work a stand alone new instrument is proposed in which the waveform is seen in a Liquid Crystal Display (LCD). The instrument is based in the X-ray response of a photo diode. The analog response depending on time is converted to digital numbers that are stored sequentially in a memory. The stored information is recovered with a microcontroller and reconstructed in the screen of the LCD. The instrument is able to measure in the mammographic range from 22 kV to 35 kV and in the conventional range from 40 kV to 120 kV in the different settings of current encountered on practical applications, the time range for the measurement of the X-ray shot is from 100 ms to 3 s. The instrument can be useful in quality control practices and in the verification and maintenance of X-ray units.

  9. A novel instrument for quantitative nanoanalytics involving complementary X-ray methodologies

    SciTech Connect

    Lubeck, J.; Beckhoff, B.; Fliegauf, R.; Holfelder, I.; Hoenicke, P.; Mueller, M.; Pollakowski, B.; Reinhardt, F.; Weser, J.

    2013-04-15

    A novel ultra-high vacuum instrument for X-ray reflectometry and spectrometry-related techniques for nanoanalytics by means of synchrotron radiation has been constructed and commissioned. This versatile instrument was developed by the Physikalisch-Technische Bundesanstalt, Germany's national metrology institute, and includes a 9-axis manipulator that allows for an independent alignment of the samples with respect to all degrees of freedom. In addition, a rotational and translational movement of several photodiodes as well as a translational movement of an aperture system in and out of the beam is provided. Thus, the new instrument enables various analytical techniques based on energy dispersive X-ray detectors such as reference-free X-ray fluorescence analysis (XRF), total-reflection XRF, grazing-incidence XRF in addition to optional X-ray reflectometry measurements or polarization-dependent X-ray absorption fine structure analyses. With this instrument samples having a size of up to 100 mm Multiplication-Sign 100 mm can be analyzed with respect to their mass deposition, elemental or spatial composition, or the species in order to probe surface contamination, layer composition and thickness, the depth profile of matrix elements or implants, the species of nanolayers, nanoparticles or buried interfaces as well as the molecular orientation of bonds. Selected applications of this advanced ultra-high vacuum instrument demonstrate both its flexibility and capability.

  10. High Resolution X-ray Spectroscopy of SN 1006

    NASA Astrophysics Data System (ADS)

    Vink, Jacco

    2005-06-01

    I discuss the high resolution XMM-Newton Reflection Grating Spectrometer (RGS) spectrum of SN 1006. SN 1006 is one of the best examples of a supernova remnant that is far out of ionization equilibrium. Moreover, optical, UV and X-ray data indicate that it is also out of temperature equilibrium. I discuss the X-ray evidence for this. In addition I discuss the lower resolution RGS spectrum of the eastern rim of SN 1006. Despite the lower resolution, the spectrum contains significant evidence for an asymmetric expansion velocity. Two likely solutions fit the O VII triplet. One with no significant thermal broadening and a shell velocity of ~ 6500 km s-1, and one with significant broadening and a shell velocity of 9500 km s -1. The first solution seems the most plausible, as it is consistent with radio expansion measurements, which suggests a decelerated shell.

  11. X-ray absorption spectroscopy of chicken sulfite oxidase crystals

    SciTech Connect

    George, G.N.; Pickering, I.J.; Kisker, C.

    1999-05-17

    Sulfite oxidase catalyzes the physiologically vital oxidation of sulfite to sulfate. Recently, the crystal structure of chicken sulfite oxidase has been reported at 1.9 {angstrom} resolution. In contrast to the information available from previous X-ray absorption spectroscopic studies, the active site indicated by crystallography was a mono-oxo species. Because of this the possibility that the crystals did in fact contain a reduced molybdenum species was considered in the crystallographic work. The authors report herein an X-ray absorption spectroscopic study of polycrystalline sulfite oxidase prepared in the same manner as the previous single-crystal samples, and compare this with data for frozen solutions of oxidized and reduced enzyme.

  12. Beam synchronous detection techniques for X-Ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Goujon, Gérard; Rogalev, Andreï; Goulon, José; Feite, Serge; Wilhelm, Fabrice

    2013-03-01

    The Photo diode detectors combine a set of properties that make them most appropriate, in particular, for X-ray Magnetic Circular Dichroism (XMCD) experiments. Under standard operating conditions, the detection bandwidth is primarily limited by the transimpedance preamplifier that converts the very low ac photocurrent into a voltage. On the other hand, when the photodiode is reverse biased, its finite shunt resistance will cause an undesirable, temperature dependent DC dark current. The best strategy to get rid of it is to use synchronous detection techniques. A classical implementation is based on the use of a chopper modulating the X-ray beam intensity at rather low frequencies (typically below 1 kHz). Here we report on the recent development of a fast Xray detection which has the capability to fully exploit the frequency structure of the ESRF X-ray beam (355 KHz and its harmonics). The availability of new wide band preamplifiers allowed us to extend the working frequency range up to a few MHz. A beam synchronous data processing was implemented in large FPGAs. Performances of the new detection system implemented at the ESRF beamline ID12 are illustrated with detection of the Fe K-edge XMCD spectra in garnets, using 4 bunches operation mode with modulation frequency of 1.4 MHz.

  13. Cylindrical Crystal Imaging Spectrometer (CCIS) for cosmic X-ray spectroscopy

    NASA Technical Reports Server (NTRS)

    Schnopper, H. W.; Taylor, P. O.

    1981-01-01

    A "stigmatic" focusing, Bragg crystal spectrometer was developed and used for high spectral resolution X-ray emission line diagnostics on hot laboratory plasmas. The concept be applied at the focal plane of an orbiting X-ray telescope where it offers several advantages over conventional spectrometers, i.e., mechanical simplicity, high resolving power and sensitivity, simultaneous measurement of an extended segment of spectrum, and good imaging properties. The instrument features a simple, unambiguous, non-scanning spectrum readout that is not adversely affected by either spacecraft pointing error or source extent. The performance of the instrument is estimated in the context of the Advanced X-Ray Astrophysical Facility mission.

  14. X-ray spectroscopy of hot white dwarfs

    NASA Astrophysics Data System (ADS)

    Adamczak, Jens

    2010-10-01

    X-ray spectra of two hot white dwarfs observed by the Chandra satellite have been analyzed. The first is a white dwarf of spectral class DA with an almost pure hydrogen atmosphere. Contrary to that, the atmosphere of the second object, a PG 1159 star, is basically hydrogen free. The reason for the different composition can be found in the differing evolution of these objects. Some DA white dwarfs show much smaller metallicities than predicted by the mechanism of radiative levitation. Many spectral lines of the heavy elements that are the key to the explanation to the unusual metal poorness are located in the X-ray wavelength range. Some PG 1159 stars are non-radial g-mode pulsators. The pulsations depend amongst others on the abundances of the elements in the atmosphere, log g, and T eff. The soft X-ray range is particularly temperature sensitive and allows to constrain the temperature of a non-pulsating PG 1159 star with respect to its pulsating spectroscopic twin. Detailed analysis of X-ray spectra of single white dwarfs do not yet exist. The aim of this thesis was to analyze spectra of the DA white dwarfs LB 1919 and GD 246 in different wavelength ranges in order to find out if the metals in the atmospheres of these objects are homogeneously mixed or chemically stratified. This helps to identify or exclude possible unexpected mechanisms that might disturb the equilibrium between gravitational and radiative forces in the atmosphere. For LB 1919 an additional aim was to identify photospheric features of several elements and determine their abundances for the first time. It was further intended to determine the temperature of the non-pulsating PG 1159 star PG 1520+525 precisely. The spectra of LB 1919 and GD 246 ranging from X-ray to optical wavelengths were analyzed with advanced homogeneous and stratified Non-LTE model atmospheres. The Chandra spectrum of the PG 1159 star PG 1520+525 was analyzed with homogeneous Non-LTE model atmospheres only since no

  15. High Resolution X-Ray Spectroscopy with a Microcalorimeter

    SciTech Connect

    Norrell, J.; Anderson, I.

    2005-01-01

    Energy-dispersive spectrometry (EDS) is often the preferred choice for X-ray microanalysis, but there are still many disadvantages associated with EDS, the most significant of which is the relatively poor energy resolution, which limits detection sensitivity and the ability to distinguish among closely spaced spectral features, limiting even qualitative analysis. A new type of EDS detector that operates on the principle of microcalorimetry has the potential to eliminate this shortcoming, reaching resolutions an order of magnitude better. The detector consists of an absorber in thermal contact with a transition edge sensor (TES). An X-ray from the specimen hits the absorber and manifests itself as a change in temperature. Because the system is kept at 80 mK, the heat capacity is low and the temperature spike is observable. The TES responds to the increase in temperature by transitioning from its superconducting to its normal conducting state, thus sharply raising the overall resistance of the circuit. The circuit is kept at a constant voltage, so the increase in resistance is manifested as a decrease in current flow. This decrease in current is measured by a superconducting quantum interference device (SQUID), and by integrating the current over time, the energy of the incident X-ray is determined. The prototype microcalorimeter was developed by NIST, and this technology is now available commercially through a partnership between Vericold Technologies and EDAX International. ORNL has received the first of these commercial microcalorimeters in the United States. The absorber in this detector is gold, and the TES consists of a gold-iridium bilayer. It is designed to offer spectral resolution of 10-15 eV at a count rate of ~150 s-1. The goal of this project was to analyze and document the performance of the detector, with particular attention given to the effects of an X-ray optic used to improve collection efficiency, the multiple window system and any other sources

  16. An instrument for 3D x-ray nano-imaging

    SciTech Connect

    Holler, M.; Raabe, J.; Diaz, A.; Guizar-Sicairos, M.; Quitmann, C.; Menzel, A.; Bunk, O.

    2012-07-15

    We present an instrument dedicated to 3D scanning x-ray microscopy, allowing a sample to be precisely scanned through a beam while the angle of x-ray incidence can be changed. The position of the sample is controlled with respect to the beam-defining optics by laser interferometry. The instrument achieves a position stability better than 10 nm standard deviation. The instrument performance is assessed using scanning x-ray diffraction microscopy and we demonstrate a resolution of 18 nm in 2D imaging of a lithographic test pattern while the beam was defined by a pinhole of 3 {mu}m in diameter. In 3D on a test object of copper interconnects of a microprocessor, a resolution of 53 nm is achieved.

  17. Feasibility of Valence-to-Core X-ray Emission Spectroscopy for Tracking Transient Species

    PubMed Central

    2015-01-01

    X-ray spectroscopies, when combined in laser-pump, X-ray-probe measurement schemes, can be powerful tools for tracking the electronic and geometric structural changes that occur during the course of a photoinitiated chemical reaction. X-ray absorption spectroscopy (XAS) is considered an established technique for such measurements, and X-ray emission spectroscopy (XES) of the strongest core-to-core emission lines (Kα and Kβ) is now being utilized. Flux demanding valence-to-core XES promises to be an important addition to the time-resolved spectroscopic toolkit. In this paper we present measurements and density functional theory calculations on laser-excited, solution-phase ferrocyanide that demonstrate the feasibility of valence-to-core XES for time-resolved experiments. We discuss technical improvements that will make valence-to-core XES a practical pump–probe technique. PMID:26568779

  18. The role of X-ray spectroscopy in understanding the geometric and electronic structure of nitrogenase.

    PubMed

    Kowalska, Joanna; DeBeer, Serena

    2015-06-01

    X-ray absorption (XAS) and X-ray emission spectroscopy (XES) provide element specific probes of the geometric and electronic structures of metalloprotein active sites. As such, these methods have played an integral role in nitrogenase research beginning with the first EXAFS studies on nitrogenase in the late 1970s. Herein, we briefly explain the information that can be extracted from XAS and XES. We then highlight the recent applications of these methods in nitrogenase research. The influence of X-ray spectroscopy on our current understanding of the atomic structure and electronic structure of iron molybdenum cofactor (FeMoco) is emphasized. Contributions of X-ray spectroscopy to understanding substrate interactions and cluster biosynthesis are also discussed. This article is part of a Special Issue entitled: Fe/S proteins: Analysis, structure, function, biogenesis and diseases.

  19. AEGIS: An Astrophysics Experiment for Grating and Imaging Spectroscopy---a Soft X-ray, High-resolution Spectrometer

    NASA Astrophysics Data System (ADS)

    Huenemoerder, David; Bautz, M. W.; Davis, J. E.; Heilmann, R. K.; Houck, J. C.; Marshall, H. L.; Neilsen, J.; Nicastro, F.; Nowak, M. A.; Schattenburg, M. L.; Schulz, N. S.; Smith, R. K.; Wolk, S.; AEGIS Team

    2012-01-01

    AEGIS is a concept for a high-resolution soft X-ray spectroscopic observatory developed in response to NASA's request for definitions of the next X-ray astronomy mission. At a small fraction of the cost of the once-planned International X-ray Observatory (IXO), AEGIS has capabilities that surpass IXO grating spectrometer requirements, and which are far superior to those of existing soft X-ray spectrometers. AEGIS incorporates innovative technology in X-ray optics, diffraction gratings and detectors. The mirror uses high area-to-mass ratio segmented glass architecture developed for IXO, but with smaller aperture and larger graze angles optimized for high-throughput grating spectroscopy with low mass and cost. The unique Critical Angle Transmission gratings combine low mass and relaxed figure and alignment tolerances of Chandra transmission gratings but with high diffraction efficiency and resolving power of blazed reflection gratings. With more than an order of magnitude better performance over Chandra and XMM grating spectrometers, AEGIS can obtain high quality spectra of bright AGN in a few hours rather than 10 days. Such high resolving power allows detailed kinematic studies of galactic outflows, hot gas in galactic haloes, and stellar accretion flows. Absorption line spectroscopy will be used to study large scale structure, cosmic feedback, and growth of black holes in thousands of sources to great distances. AEGIS will enable powerful multi-wavelength investigations, for example with Hubble/COS in the UV to characterize the intergalactic medium. AEGIS will be the first observatory with sufficient resolution below 1 keV to resolve thermally-broadened lines in hot ( 10 MK) plasmas. Here we describe key science investigations enable by Aegis, its scientific payload and mission plan. Acknowledgements: Support was provided in part by: NASA SAO contract SV3-73016 to MIT for the Chandra X-ray Center and Science Instruments; NASA grant NNX08AI62G; and the MKI

  20. Analytical characterization of a new mobile X-ray fluorescence and X-ray diffraction instrument combined with a pigment identification case study

    NASA Astrophysics Data System (ADS)

    Van de Voorde, Lien; Vekemans, Bart; Verhaeven, Eddy; Tack, Pieter; De Wolf, Robin; Garrevoet, Jan; Vandenabeele, Peter; Vincze, Laszlo

    2015-08-01

    A new, commercially available, mobile system combining X-ray diffraction and X-ray fluorescence has been evaluated which enables both elemental analysis and phase identification simultaneously. The instrument makes use of a copper or molybdenum based miniature X-ray tube and a silicon-Pin diode energy-dispersive detector to count the photons originating from the samples. The X-ray tube and detector are both mounted on an X-ray diffraction protractor in a Bragg-Brentano θ:θ geometry. The mobile instrument is one of the lightest and most compact instruments of its kind (3.5 kg) and it is thus very useful for in situ purposes such as the direct (non-destructive) analysis of cultural heritage objects which need to be analyzed on site without any displacement. The supplied software allows both the operation of the instrument for data collection and in-depth data analysis using the International Centre for Diffraction Data database. This paper focuses on the characterization of the instrument, combined with a case study on pigment identification and an illustrative example for the analysis of lead alloyed printing letters. The results show that this commercially available light-weight instrument is able to identify the main crystalline phases non-destructively, present in a variety of samples, with a high degree of flexibility regarding sample size and position.

  1. The X-ray Pump–Probe instrument at the Linac Coherent Light Source

    PubMed Central

    Chollet, Matthieu; Alonso-Mori, Roberto; Cammarata, Marco; Damiani, Daniel; Defever, Jim; Delor, James T.; Feng, Yiping; Glownia, James M.; Langton, J. Brian; Nelson, Silke; Ramsey, Kelley; Robert, Aymeric; Sikorski, Marcin; Song, Sanghoon; Stefanescu, Daniel; Srinivasan, Venkat; Zhu, Diling; Lemke, Henrik T.; Fritz, David M.

    2015-01-01

    The X-ray Pump–Probe instrument achieves femtosecond time-resolution with hard X-ray methods using a free-electron laser source. It covers a photon energy range of 4–24 keV. A femtosecond optical laser system is available across a broad spectrum of wavelengths for generating transient states of matter. The instrument is designed to emphasize versatility and the scientific goals encompass ultrafast physical, chemical and biological processes involved in the transformation of matter and transfer of energy at the atomic scale. PMID:25931060

  2. The X-ray Pump–Probe instrument at the Linac Coherent Light Source

    DOE PAGESBeta

    Chollet, Matthieu; Alonso-Mori, Roberto; Cammarata, Marco; Damiani, Daniel; Defever, Jim; Delor, James T.; Feng, Yiping; Glownia, James M.; Langton, J. Brian; Nelson, Silke; et al

    2015-04-21

    The X-ray Pump–Probe instrument achieves femtosecond time-resolution with hard X-ray methods using a free-electron laser source. It covers a photon energy range of 4–24 keV. A femtosecond optical laser system is available across a broad spectrum of wavelengths for generating transient states of matter. The instrument is designed to emphasize versatility and the scientific goals encompass ultrafast physical, chemical and biological processes involved in the transformation of matter and transfer of energy at the atomic scale.

  3. High-resolution spectroscopy of X-rays emitted from electron bombarded surfaces

    NASA Astrophysics Data System (ADS)

    Jabłoński, Ł.; Banaś, D.; Jagodziński, P.; Kubala-Kukuś, A.; Sobota, D.; Pajek, M.

    2015-07-01

    The investigations of a compact 6-crystal Johann/Johansson diffraction X-ray spectrometer, covering a wide range (70 eV-15 keV) of photon energies, applied to observe the X-rays emitted from electron bombarded surfaces are discussed in terms of its focusing properties and achievable energy resolution. In the present study the X-ray spectra of Si-Kα1,2 and Al-Kα1,2 X-ray lines excited by 5 keV electron beam were measured using PET and TAP crystal, respectively, in the "out-of-focus" geometry which will be used to study the electron/ion surface interactions at the electron beam ion source (EBIS) facility. The measured X-ray spectra were interpreted in terms of the performed ray-tracing simulations which demonstrate the key features of the "out-of-focus" geometry. It was demonstrated that in this case the energy resolution in the range 1-3 eV for photon energy 1-2 keV can be achieved with an increased acceptance for the extension of X-ray source, of about 1 mm, which is important feature for practical applications. Additionally, a dependence of the X-ray intensity and energy resolution on slit opening was studied in details. The results are important for investigations of surfaces with electron and ion impact, in particular, for the future high-resolution X-ray spectroscopy experiments at the EBIS facility.

  4. Soft x-ray emission spectroscopy using monochromatized synchrotron radiation (invited)

    NASA Astrophysics Data System (ADS)

    Nordgren, J.; Bray, G.; Cramm, S.; Nyholm, R.; Rubensson, J.-E.; Wassdahl, N.

    1989-07-01

    Soft x-ray emission spectroscopy is a common tool for the study of the electronic structure of molecules and solids. However, the interpretation of spectra is sometimes made difficult by overlaying lines due to satellite transitions or close-lying core holes. Also, irrelevant inner core transitions may accidentally fall in the wavelength region under study. These problems, which often arise for spectra excited with electrons or broadband photon sources can be removed by using monochromatized synchrotron radiation. In addition, one achieves other advantages as well, such as the ability to study resonant behavior. Another important aspect is the softness of this excitation agent, which allows chemically fragile compounds to be investigated. In this work we demonstrate the feasibility of using monochromatized synchrotron radiation to excite soft x-ray spectra. We also show new results which have been accomplished as a result of the selectivity of the excitation. The work has been carried out using the Flipper I wiggler beamline at HASYLAB in Hamburg using a new grazing incidence instrument designed specifically for this experiment. The photon flux at the Flipper I station (typically 5×1012 photons per second on the sample with a 1% bandpass) is enough to allow soft x-ray fluorescence spectra to be recorded at relatively high resolution and within reasonable accumulation times (typically, the spectra presented in this work were recorded in 30 min). The spectrometer is based on a new concept which allows the instrument to be quite small, still covering a large wavelength range (10-250 Å). The basic idea involves the use of several fixed mounted gratings and a large two-dimensional detector. The grating arrangement provides simple mounting within a limited space and, in particular, large spectral range. The detector can be moved in a three-axis coordinate system in order to cover the different Rowland curves defined by the different gratings. The arrangement permits

  5. X-ray spectroscopy of the SSME plume

    NASA Technical Reports Server (NTRS)

    Olive, Dan F.

    1988-01-01

    In order to examine the potential of using SSME exhaust plume radiation in the soft X-ray spectrum as an early warning system of imminent engine failure, a low cost, low risk experiment was devised. An approach was established, equipment was leased, the system was installed and checked out, and data were successfully acquired demonstrating the proof-of-concept. One spectrum measurement of the SSME plume was acquired during a 300 second burn on the A-1 Test Stand. This spectrum showed a prominent, line emission feature at about 34.5 KeV, a result which was not expected, nor can it be explained at this time. If X-ray spectra are to be useful as a means of monitoring nominal engine operation, it will be necessary to explore this region of the EM spectrum in greater detail. The presence of structure in the spectrum indicates that this technology may prove to be useful as an engine health monitoring system.

  6. Fast Detection Allows Analysis of the Electronic Structure of Metalloprotein by X-ray Emission Spectroscopy at Room Temperature.

    PubMed

    Davis, Katherine M; Mattern, Brian A; Pacold, Joseph I; Zakharova, Taisiya; Brewe, Dale; Kosheleva, Irina; Henning, Robert W; Graber, Timothy J; Heald, Steve M; Seidler, Gerald T; Pushkar, Yulia

    2012-07-19

    The paradigm of "detection-before-destruction" was tested for a metalloprotein complex exposed at room temperature to the high x-ray flux typical of third generation synchrotron sources. Following the progression of the x-ray induced damage by Mn Kβ x-ray emission spectroscopy, we demonstrated the feasibility of collecting room temperature data on the electronic structure of native Photosystem II, a trans-membrane metalloprotein complex containing a Mn(4)Ca cluster. The determined non-damaging observation timeframe (about 100 milliseconds using continuous monochromatic beam, deposited dose 1*10(7) photons/µm(2) or 1.3*10(4) Gy, and 66 microseconds in pulsed mode using pink beam, deposited dose 4*10(7) photons/µm(2) or 4.2*10(4) Gy) is sufficient for the analysis of this protein's electron dynamics and catalytic mechanism at room temperature. Reported time frames are expected to be representative for other metalloproteins. The described instrumentation, based on the short working distance dispersive spectrometer, and experimental methodology is broadly applicable to time-resolved x-ray emission analysis at synchrotron and x-ray free-electron laser light sources.

  7. Time-resolved X-ray spectroscopies of chemical systems: New perspectives.

    PubMed

    Chergui, Majed

    2016-05-01

    The past 3-5 years have witnessed a dramatic increase in the number of time-resolved X-ray spectroscopic studies, mainly driven by novel technical and methodological developments. The latter include (i) the high repetition rate optical pump/X-ray probe studies, which have greatly boosted the signal-to-noise ratio for picosecond (ps) X-ray absorption spectroscopy studies, while enabling ps X-ray emission spectroscopy (XES) at synchrotrons; (ii) the X-ray free electron lasers (XFELs) are a game changer and have allowed the first femtosecond (fs) XES and resonant inelastic X-ray scattering experiments to be carried out; (iii) XFELs are also opening the road to the development of non-linear X-ray methods. In this perspective, I will mainly focus on the most recent technical developments and briefly address some examples of scientific questions that have been addressed thanks to them. I will look at the novel opportunities in the horizon.

  8. Time-resolved X-ray spectroscopies of chemical systems: New perspectives.

    PubMed

    Chergui, Majed

    2016-05-01

    The past 3-5 years have witnessed a dramatic increase in the number of time-resolved X-ray spectroscopic studies, mainly driven by novel technical and methodological developments. The latter include (i) the high repetition rate optical pump/X-ray probe studies, which have greatly boosted the signal-to-noise ratio for picosecond (ps) X-ray absorption spectroscopy studies, while enabling ps X-ray emission spectroscopy (XES) at synchrotrons; (ii) the X-ray free electron lasers (XFELs) are a game changer and have allowed the first femtosecond (fs) XES and resonant inelastic X-ray scattering experiments to be carried out; (iii) XFELs are also opening the road to the development of non-linear X-ray methods. In this perspective, I will mainly focus on the most recent technical developments and briefly address some examples of scientific questions that have been addressed thanks to them. I will look at the novel opportunities in the horizon. PMID:27376102

  9. Time-resolved X-ray spectroscopies of chemical systems: New perspectives

    PubMed Central

    Chergui, Majed

    2016-01-01

    The past 3–5 years have witnessed a dramatic increase in the number of time-resolved X-ray spectroscopic studies, mainly driven by novel technical and methodological developments. The latter include (i) the high repetition rate optical pump/X-ray probe studies, which have greatly boosted the signal-to-noise ratio for picosecond (ps) X-ray absorption spectroscopy studies, while enabling ps X-ray emission spectroscopy (XES) at synchrotrons; (ii) the X-ray free electron lasers (XFELs) are a game changer and have allowed the first femtosecond (fs) XES and resonant inelastic X-ray scattering experiments to be carried out; (iii) XFELs are also opening the road to the development of non-linear X-ray methods. In this perspective, I will mainly focus on the most recent technical developments and briefly address some examples of scientific questions that have been addressed thanks to them. I will look at the novel opportunities in the horizon. PMID:27376102

  10. A novel von Hamos spectrometer for efficient X-ray emission spectroscopy in the laboratory

    SciTech Connect

    Anklamm, Lars Schlesiger, Christopher; Malzer, Wolfgang; Grötzsch, Daniel; Neitzel, Michael; Kanngießer, Birgit

    2014-05-15

    We present a novel, highly efficient von Hamos spectrometer for X-ray emission spectroscopy (XES) in the laboratory using highly annealed pyrolitic graphite crystals as the dispersive element. The spectrometer covers an energy range from 2.5 keV to 15 keV giving access to chemical speciation and information about the electronic configuration of 3d transition metals by means of the Kβ multiplet. XES spectra of Ti compounds are presented to demonstrate the speciation capabilities of the instrument. A spectral resolving power of E/ΔE = 2000 at 8 keV was achieved. Typical acquisition times range from 10 min for bulk material to hours for thin samples below 1 μm.

  11. X-ray imaging crystal spectroscopy for use in plasma transport research

    SciTech Connect

    Reinke, M. L.; Podpaly, Y. A.; Hutchinson, I. H.; Rice, J. E.; Gao, C.; Greenwald, M.; Howard, N. T.; Hubbard, A.; Hughes, J. W.; White, A. E.; Wolfe, S. M.; Bitter, M.; Delgado-Aparicio, L.; Hill, K.; Pablant, N.

    2012-11-15

    This research describes advancements in the spectral analysis and error propagation techniques associated with x-ray imaging crystal spectroscopy (XICS) that have enabled this diagnostic to be used to accurately constrain particle, momentum, and heat transport studies in a tokamak for the first time. Doppler tomography techniques have been extended to include propagation of statistical uncertainty due to photon noise, the effect of non-uniform instrumental broadening as well as flux surface variations in impurity density. These methods have been deployed as a suite of modeling and analysis tools, written in interactive data language (IDL) and designed for general use on tokamaks. Its application to the Alcator C-Mod XICS is discussed, along with novel spectral and spatial calibration techniques. Example ion temperature and radial electric field profiles from recent I-mode plasmas are shown, and the impact of poloidally asymmetric impurity density and natural line broadening is discussed in the context of the planned ITER x-ray crystal spectrometer.

  12. X-ray imaging crystal spectroscopy for use in plasma transport research.

    PubMed

    Reinke, M L; Podpaly, Y A; Bitter, M; Hutchinson, I H; Rice, J E; Delgado-Aparicio, L; Gao, C; Greenwald, M; Hill, K; Howard, N T; Hubbard, A; Hughes, J W; Pablant, N; White, A E; Wolfe, S M

    2012-11-01

    This research describes advancements in the spectral analysis and error propagation techniques associated with x-ray imaging crystal spectroscopy (XICS) that have enabled this diagnostic to be used to accurately constrain particle, momentum, and heat transport studies in a tokamak for the first time. Doppler tomography techniques have been extended to include propagation of statistical uncertainty due to photon noise, the effect of non-uniform instrumental broadening as well as flux surface variations in impurity density. These methods have been deployed as a suite of modeling and analysis tools, written in interactive data language (IDL) and designed for general use on tokamaks. Its application to the Alcator C-Mod XICS is discussed, along with novel spectral and spatial calibration techniques. Example ion temperature and radial electric field profiles from recent I-mode plasmas are shown, and the impact of poloidally asymmetric impurity density and natural line broadening is discussed in the context of the planned ITER x-ray crystal spectrometer.

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

    SciTech Connect

    Perera, R.C.C.; Ng, W.; Jones, G.

    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.

  14. Diamond solid state ionization chambers for x-ray absorption spectroscopy applications

    SciTech Connect

    De Sio, A.; Bocci, A.; Pace, E.; Castellano, C.; Cinque, G.; Tartoni, N.; D'Acapito, F.

    2008-08-25

    The photoresponse of a diamond detector has been compared with a standard ionization chamber in x-ray absorption spectroscopy applications. A photoconductive device based on a nitrogen-doped single crystal diamond has been tested by synchrotron radiation. Time stability and linearity have been studied by x rays at 10 keV to assess its performances. Finally, extended x-ray absorption fine structure at the Fe K-edge was carried on a standard iron target using both the diamond device and the IC. Spectroscopical results have been compared including references to literature.

  15. Very high resolution UV and X-ray spectroscopy and imagery of solar active regions

    NASA Technical Reports Server (NTRS)

    Bruner, M.; Brown, W. A.; Haisch, B. M.

    1987-01-01

    A scientific investigation of the physics of the solar atmosphere, which uses the techniques of high resolution soft X-ray spectroscopy and high resolution UV imagery, is described. The experiments were conducted during a series of three sounding rocket flights. All three flights yielded excellent images in the UV range, showing unprecedented spatial resolution. The second flight recorded the X-ray spectrum of a solar flare, and the third that of an active region. A normal incidence multi-layer mirror was used during the third flight to make the first astronomical X-ray observations using this new technique.

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

    SciTech Connect

    Hurvitz, G.; Ehrlich, Y.; Shpilman, Z.; Levy, I.; Fraenkel, M.; Strum, G.

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

    PubMed

    Hurvitz, G; Ehrlich, Y; Strum, G; Shpilman, Z; Levy, I; Fraenkel, M

    2012-08-01

    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.

  18. X-Ray Spectroscopy of Bromine Compounds and Biomedical Applications

    NASA Astrophysics Data System (ADS)

    Nahar, Sultana N.; Luo, Yi; Le, Linh; Pradhan, A. K.; Chowdhury, E.; Pitzer, R.; Montenegro, M.

    2010-06-01

    In conventional biomedical applications intense and broadband high energy X-rays are used in therapy and diagnostics (theranostics) to ensure sufficient tissue penetration for imaging or treatment. To avoid damages incurred by these, our proposed method, Resonant Theranosticsb,c, aims to find narrow energy regions that corresponds to resonant absorption or emission. We show that such energy bands lie below the K-shell ionization energy, contrary to the research focus on the K-shell ionization energy itself. Targeting these energy bands, Auger processes can be initiated to produce a number of photons and electrons from each atomic/molecular species via photon fluorescence and electron ejections. We will report our study on the bromine compound bromodeoxyuridyne (BUdR), widely used as radiological contrast agent in radiation imaging. The active system is Br^o-Br^+ combination, which can emit or absorb X-rays in the relative narrow energy range of 12 to 13.6 keV, through 1s-np transitions. We will present the oscillator strengths and transition probabilities for various Auger or K-shell 1s-np transitions. We will show that the corresponding cross sections and attenuation coefficients per unit mass, are orders of magnitude higher than the background and that at K-shell ionization energy. Employing these attenuation coefficients in the Monte Carlo simulation program Geant4, we study the intensities of photon and electron emission spectra. Acknowledgment: Partially support: Large Interdisciplinary Grant award of the Ohio State University and NASA (SNN). The computational work was carried out at the Ohio Supercomputer Center, Columbus Ohio. "Resonant X-Ray Enhancement of the Auger Effect in High-Z atoms, molecules, and Nanoparticles: Biomedical Applications", A. K. Pradhan, S. N. Nahar, M. Montenegro, Yan Yu, H. L. Zhang, C. Sur, M. Mrozik, R. M. Pitzer, J. of Phys. Chem. A, 113 (2009), 12356. "Monte Carlo Simulations and Atomic Calculations for Auger Processes in

  19. Measuring redshifts using X-ray spectroscopy of galaxy clusters: results from Chandra data and future prospects

    NASA Astrophysics Data System (ADS)

    Yu, H.; Tozzi, P.; Borgani, S.; Rosati, P.; Zhu, Z.-H.

    2011-05-01

    Context. The ubiquitous presence of the Fe line complex in the X-ray spectra of galaxy clusters offers the possibility of measuring their redshift without resorting to spectroscopic follow-up observations. In practice, the blind search of the Fe line in X-ray spectra is a difficult task and is affected not only by limited S/N (particularly at high redshift), but also by several systematic errors, associated with varying Fe abundance values, ICM temperature gradients, and instrumental characteristics. Aims: We assess the accuracy with which the redshift of galaxy clusters can be recovered from an X-ray spectral analysis of Chandra archival data. We present a strategy to compile large surveys of clusters whose identification and redshift measurement are both based on X-ray data alone. Methods: We apply a blind search for K-shell and L-shell Fe line complexes in X-ray cluster spectra using Chandra archival observations of galaxy clusters. The Fe line can be detected in the ICM spectra by simply analyzing the C-statistics variation ΔCstat as a function of the redshift parameter, when all the other model parameters are frozen to the best-fit values. We repeat the measurement under different conditions, and compare the X-ray derived redshift zX with the one obtained by means of optical spectroscopy zo. We explore how a number of priors on metallicity and luminosity can be effectively used to reduce catastrophic errors. The ΔCstat provides the most effective means of discarding wrong redshift measurements and estimating the actual error in zX. Results: We identify a simple and efficient procedure for optimally measuring the redshifts from the X-ray spectral analysis of clusters of galaxies. When this procedure is applied to mock catalogs extracted from high sensitivity, wide-area cluster surveys, such as those proposed with Wide Field X-ray Telescope (WFXT) mission, it is possible to obtain complete samples of X-ray clusters with reliable redshift measurements, thus

  20. The Coherent X-ray Imaging (CXI) Instrument at the Linac Coherent Light Source (LCLS)

    SciTech Connect

    Boutet, Sebastien; Williams, Garth J.; /SLAC

    2011-08-16

    The Linac Coherent Light Source (LCLS) has become the first ever operational hard X-ray Free Electron Laser in 2009. It will operate as a user facility capable of delivering unique research opportunities in multiple fields of science. The LCLS and the LCLS Ultrafast Science Instruments (LUSI) construction projects are developing instruments designed to make full use of the capabilities afforded by the LCLS beam. One such instrument is being designed to utilize the LCLS coherent beam to image with high resolution any sub-micron object. This instrument is called the Coherent X-ray Imaging (CXI) instrument. This instrument will provide a flexible optical system capable of tailoring key beam parameters for the users. A suite of shot-to-shot diagnostics will also be provided to characterize the beam on every pulse. The provided instrumentation will include multi-purpose sample environments, sample delivery and a custom detector capable of collecting 2D data at 120 Hz. In this article, the LCLS will be briefly introduced along with the technique of Coherent X-ray Diffractive Imaging (CXDI). A few examples of scientific opportunities using the CXI instrument will be described. Finally, the conceptual layout of the instrument will be presented along with a description of the key requirements for the overall system and specific devices required.

  1. X-ray Spectroscopy of Hot Dense Plasmas: Experimental Limits, Line Shifts and Field Effects

    SciTech Connect

    Renner, Oldrich; Sauvan, Patrick; Dalimier, Elisabeth; Riconda, Caterina; Rosmej, Frank B.; Weber, Stefan; Nicolai, Philippe; Peyrusse, Olivier; Uschmann, Ingo; Hoefer, Sebastian; Kaempfer, Tino; Loetzsch, Robert; Zastrau, Ulf; Foerster, Eckhart; Oks, Eugene

    2008-10-22

    High-resolution x-ray spectroscopy is capable of providing complex information on environmental conditions in hot dense plasmas. Benefiting from application of modern spectroscopic methods, we report experiments aiming at identification of different phenomena occurring in laser-produced plasma. Fine features observed in broadened profiles of the emitted x-ray lines and their satellites are interpreted using theoretical models predicting spectra modification under diverse experimental situations.

  2. Properties of Liquid Silicon Observed by Time-Resolved X-Ray Absorption Spectroscopy

    NASA Astrophysics Data System (ADS)

    Johnson, S. L.; Heimann, P. A.; Lindenberg, A. M.; Jeschke, H. O.; Garcia, M. E.; Chang, Z.; Lee, R. W.; Rehr, J. J.; Falcone, R. W.

    2003-10-01

    Time-resolved x-ray spectroscopy at the Si L edges is used to probe the electronic structure of an amorphous Si foil as it melts following absorption of an ultrafast laser pulse. Picosecond temporal resolution allows observation of the transient liquid phase before vaporization and before the liquid breaks up into droplets. The melting causes changes in the spectrum that match predictions of molecular dynamics and ab initio x-ray absorption codes.

  3. X-ray Spectroscopy for Quality Control of Chemotherapy Drugs

    SciTech Connect

    Greaves, E. D.; Barros, H.; Bermudez, J.; Sajo-Bohus, L.; Angeli-Greaves, M.

    2007-10-26

    We develop a method, employing Compton peak standardization and the use of matrix-matched spiked samples with Total Reflection X-ray Fluorescence (TXRF), for the determination of platinum plasma concentrations of patients undergoing chemotherapy with Pt-bearing drugs. Direct blood plasma analysis attains Pt detection limits of 70 ng/ml. Measurement results of prescribed drug doses are compared to achieved blood Pt concentrations indicating a lack of expected correlations. Direct analysis of Pt-containing infused drugs from a variety of suppliers indicates cases of abnormal concentrations which raises quality control issues. We demonstrate the potential usefulness of the method for pharmacokinetic studies or for routine optimization and quality control of Pt chemotherapy treatments.

  4. Gold nephropathy: tissue analysis by X-ray fluorescent spectroscopy.

    PubMed

    Viol, G W; Minielly, J A; Bistricki, T

    1977-12-01

    Three patients developed proteinuria following gold therapy for rheumatoid arthritis. The clinical syndrome was a self-limiting proteinuria with normal renal function. By light and electron microscopic appearances the renal lesion was an epimembranous deposit form of membranous glomerulopathy. Immunofluorescent study showed granular deposits of IgG and C3 complement along glomerular basement membranes. By X-ray fluorescent spectroscopic examination, gold was seen to be present within the proximal convoluted tubular cells but was not identified in the glomerular subepithelial deposits. These findings are consistent with an immune-complex form of glomerulopathy in which gold is neither the antigen nor a hapten in the glomerular deposits, and they suggest the hypothesis that antibodies to tubular epithelial antigens induced by gold therapy may be a causative factor in the renal disease associated with gold therapy in rheumatoid arthritis. PMID:412488

  5. Note: Application of a pixel-array area detector to simultaneous single crystal x-ray diffraction and x-ray absorption spectroscopy measurements

    SciTech Connect

    Sun, Cheng-Jun Brewe, Dale L.; Heald, Steve M.; Zhang, Bangmin; Chen, Jing-Sheng; Chow, G. M.; Venkatesan, T.

    2014-04-15

    X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorption near edge structure for Pr{sub 0.67}Sr{sub 0.33}MnO{sub 3} film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam.

  6. First application of superconducting transition-edge sensor microcalorimeters to hadronic atom X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Okada, S.; Bennett, D. A.; Curceanu, C.; Doriese, W. B.; Fowler, J. W.; Gard, J. D.; Gustafsson, F. P.; Hashimoto, T.; Hayano, R. S.; Hirenzaki, S.; Hays-Wehle, J. P.; Hilton, G. C.; Ikeno, N.; Iliescu, M.; Ishimoto, S.; Itahashi, K.; Iwasaki, M.; Koike, T.; Kuwabara, K.; Ma, Y.; Marton, J.; Noda, H.; O'Neil, G. C.; Outa, H.; Reintsema, C. D.; Sato, M.; Schmidt, D. R.; Shi, H.; Suzuki, K.; Suzuki, T.; Swetz, D. S.; Tatsuno, H.; Uhlig, J.; Ullom, J. N.; Widmann, E.; Yamada, S.; Yamagata-Sekihara, J.; Zmeskal, J.

    2016-09-01

    High-resolution pionic atom X-ray spectroscopy was performed with an X-ray spectrometer based on a 240 pixel array of superconducting transition-edge sensor (TES) microcalorimeters at the πM1 beam line of the Paul Scherrer Institute. X-rays emitted by pionic carbon via the 4f→3d transition and the parallel 4d→3p transition were observed with a full width at half maximum energy resolution of 6.8 eV at 6.4 keV. The measured X-ray energies are consistent with calculated electromagnetic values which considered the strong interaction effect assessed via the Seki-Masutani potential for the 3p energy level, and favor the electronic population of two filled 1s electrons in the K-shell. Absolute energy calibration with an uncertainty of 0.1 eV was demonstrated under a high-rate hadron beam condition of 1.45 MHz. This is the first application of a TES spectrometer to hadronic atom X-ray spectroscopy and is an important milestone towards next-generation high-resolution kaonic atom X-ray spectroscopy.

  7. X-ray imaging and spectroscopy using low cost COTS CMOS sensors

    NASA Astrophysics Data System (ADS)

    Lane, David W.

    2012-08-01

    Whilst commercial X-ray sensor arrays are capable of both imaging and spectroscopy they are currently expensive and this can limit their widespread use. This study examines the use of very low cost CMOS sensors for X-ray imaging and spectroscopy based on the commercial off the shelf (COTS) technology used in cellular telephones, PC multimedia and children's toys. Some examples of imaging using a 'webcam' and a modified OmniVision OV7411 sensor are presented, as well as a simple energy dispersive X-ray detector based on an OmniVision OV7221 sensor. In each case X-ray sensitivity was enabled by replacing the sensor's front glass window with a 5 μm thick aluminium foil, with X-rays detected as an increase in a pixel's dark current due to the generation of additional electron-hole pairs within its active region. The exposure control and data processing requirements for imaging and spectroscopy are discussed. The modified OV7221 sensor was found to have a linear X-ray energy calibration and a resolution of approximately 510 eV.

  8. Mineralogy by X-ray Diffraction on Mars: The Chemin Instrument on Mars Science Laboratory

    NASA Technical Reports Server (NTRS)

    Vaniman, D. T.; Bristow, T. F.; Bish, D. L.; Ming, D. W.; Blake, D. F.; Morris, R. V.; Rampe, E. B.; Chipera, S. J.; Treiman, A. H.; Morrison, S. M.; Achilles, C. N.; Downs, R. T.; Farmer, J. D.; Crisp, J. A.; Morookian, J. M.; Des Marais, D. J.; Grotzinger, J. P.; Sarrazin, P.; Yen, A. S.

    2014-01-01

    To obtain detailed mineralogy information, the Mars Science Laboratory rover Curiosity carries CheMin, the first X-ray diffraction (XRD) instrument used on a planet other than Earth. CheMin has provided the first in situ XRD analyses of full phase assemblages on another planet.

  9. McXtrace: a modern ray-tracing package for x-ray instrumentation

    NASA Astrophysics Data System (ADS)

    Knudsen, Erik B.; Prodi, Andrea; Willendrup, Peter; Lefmann, Kim; Baltser, Jana; Gundlach, Carsten; Sanchez del Rio, Manuel; Ferrero, Claudio; Feidenhans'l, Robert

    2011-09-01

    we present the developments of the McXtrace project, a free, open source software package based on Monte Carlo ray tracing for simulations and optimisation of complete X-ray instruments. The methodology of building a simulation is presented through an example beamline, namely Beamline 811 at MAX-lab, Lund, Sweden - a beamline dedicated to materials science.

  10. A robot-based detector manipulator system for a hard x-ray nanoprobe instrument.

    SciTech Connect

    Shu, D., Maser, J., Holt, M. , Winarski, R., Preissner, C.,Lai, B., Vogt, S., Stephenson, G.B.

    2007-11-11

    This paper presents the design of a robot-based detector manipulator for microdiffraction applications with a hard X-ray nanoprobe instrument system being constructed at the Advanced Photon Source (APS) for the Center for Nanoscale Materials (CNM) being constructed at Argonne National Laboratory (ANL). Applications for detectors weighing from 1.5 to 100 kg were discussed in three configurations.

  11. Broad-band soft x-ray diagnostic instruments at the LLNL Novette laser facility

    SciTech Connect

    Tirsell, K.G.; Lee, P.H.Y.; Nilson, D.G.; Medecki, H.

    1983-09-15

    Complementary broad-band instruments have been developed to measure time dependent, absolute soft x-ray spectra at the Lawrence Livermore National Laboratory (LLNL) Nd glass laser irradiation facilities. Absolute flux measurements of x rays emitted from laser-produced plasmas are important for understanding laser absorption and energy transport. We will describe two new 10-channel XRD systems that have been installed at the LLNL Novette facility for use in the 0.15- to 1.5-keV range. Since XRD channel time response is limited by available oscilloscope performance to 120 ps, a soft x-ray streak camera has been developed for better time resolution (20 ps) and greater dynamic range (approx.10/sup 3/) in the same x-ray energy region. Using suitable filters, grazing incidence mirrors, and a gold or cesium-iodide transmission cathode, this streak camera instrument has been installed at Novette to provide one broad and four relatively narrow channels. It can also be used in a single channel, spatially discriminating mode by means of pinhole imaging. The complementary nature of these instruments has been enhanced by locating them in close proximity and matching their channel energy responses. As an example of the use of these instruments, we present results from Novette 2..omega..(0.53 ..mu..m) gold disk irradiations at 1 ns and 10/sup 14/ to 10/sup 15/ W/cm/sup 2/.

  12. New Instruments for Spectrally-Resolved Solar Soft X-ray Observations from CubeSats, and Larger Missions

    NASA Astrophysics Data System (ADS)

    Caspi, A.; Shih, A.; Warren, H. P.; DeForest, C. E.; Woods, T. N.

    2015-12-01

    Solar soft X-ray (SXR) observations provide important diagnostics of plasma heating, during solar flares and quiescent times. Spectrally- and temporally-resolved measurements are crucial for understanding the dynamics and evolution of these energetic processes; spatially-resolved measurements are critical for understanding energy transport. A better understanding of the thermal plasma informs our interpretation of hard X-ray (HXR) observations of nonthermal particles, improving our understanding of the relationships between particle acceleration, plasma heating, and the underlying release of magnetic energy during reconnection. We introduce a new proposed mission, the CubeSat Imaging X-ray Solar Spectrometer (CubIXSS), to measure spectrally- and spatially-resolved SXRs from the quiescent and flaring Sun from a 6U CubeSat platform in low-Earth orbit during a nominal 1-year mission. CubIXSS includes the Amptek X123-SDD silicon drift detector, a low-noise, commercial off-the-shelf (COTS) instrument enabling solar SXR spectroscopy from ~0.5 to ~30 keV with ~0.15 keV FWHM spectral resolution with low power, mass, and volume requirements. An X123-CdTe cadmium-telluride detector is also included for ~5-100 keV HXR spectroscopy with ~0.5-1 keV FWHM resolution. CubIXSS also includes a novel spectro-spatial imager -- the first ever solar imager on a CubeSat -- utilizing a pinhole aperture and X-ray transmission diffraction grating to provide full-Sun imaging from ~0.1 to ~10 keV, with ~25 arcsec and ~0.1 Å FWHM spatial and spectral resolutions, respectively. We discuss scaled versions of these instruments, with greater sensitivity and dynamic range, and significantly improved spectral and spatial resolutions for the imager, for deployment on larger platforms such as Small Explorer missions.

  13. X-ray absorption spectroscopy and X-ray photoelectron spectroscopy studies of CaSO 4:Dy thermoluminescent phosphors

    NASA Astrophysics Data System (ADS)

    Bakshi, A. K.; Jha, S. N.; Olivi, L.; Phase, D. M.; Kher, R. K.; Bhattacharyya, D.

    2007-11-01

    Extended X-ray absorption fine structure (EXAFS) measurements have been carried out on CaSO4:Dy phosphor samples at the Dy L3 edge with synchrotron radiation. Measurements were carried out on a set of samples which were subjected to post-preparation annealing at different temperatures and for different cycles. The EXAFS data have been analysed to find the Dy-S and Dy-O bond lengths in the neighbourhood of the Dy atoms in a CaSO4 matrix. The observations from EXAFS measurements were verified with XANES and XPS techniques. On the basis of these measurements, efforts were made to explain the loss of thermoluminescence sensitivity of CaSO4:Dy phosphors after repeated cycles of annealing at 400 °C in air for 1 h.

  14. FORTRAN program for x ray photoelectron spectroscopy data reformatting

    NASA Technical Reports Server (NTRS)

    Abel, Phillip B.

    1989-01-01

    A FORTRAN program has been written for use on an IBM PC/XT or AT or compatible microcomputer (personal computer, PC) that converts a column of ASCII-format numbers into a binary-format file suitable for interactive analysis on a Digital Equipment Corporation (DEC) computer running the VGS-5000 Enhanced Data Processing (EDP) software package. The incompatible floating-point number representations of the two computers were compared, and a subroutine was created to correctly store floating-point numbers on the IBM PC, which can be directly read by the DEC computer. Any file transfer protocol having provision for binary data can be used to transmit the resulting file from the PC to the DEC machine. The data file header required by the EDP programs for an x ray photoelectron spectrum is also written to the file. The user is prompted for the relevant experimental parameters, which are then properly coded into the format used internally by all of the VGS-5000 series EDP packages.

  15. Evaluation of the medical exposure doses regarding dental examinations with different X-ray instruments

    NASA Astrophysics Data System (ADS)

    Liu, Yi-Chi; Chuang, Keh-Shih; Yu, Cheng-Ching; Chao, Jiunn-Hsing; Hsu, Fang-Yuh

    2015-11-01

    Modern dental X-ray examination that consists of traditional form, panorama, and cone-beamed 3D technologies is one of the most frequent diagnostic applications nowadays. This study used the Rando Phantom and thermoluminescence dosimeters (TLD) to measure the absorbed doses of radiosensitive organs recommended by International Commission on Radiological Protection (ICRP), and whole body effective doses which were delivered due to dental X-ray examination performed with different types of X-ray instrument. Besides, enamel samples which performed reading with Electronic Paramagnetic Resonance (EPR) procedure were also used to estimate the tooth doses. EPR is a dose reconstruction method of measuring free radicals induced by radiation exposure to the calcified tissue (mainly in the tooth enamel or bone) to evaluate the accepted high dose. The tooth doses estimated by TLD and EPR methods were compared. Relationships between the tooth doses and effective doses by dental X-ray examinations with different types of X-ray equipment were investigated in this work.

  16. Prototyping a Global Soft X-Ray Imaging Instrument for Heliophysics, Planetary Science, and Astrophysics Science

    NASA Technical Reports Server (NTRS)

    Collier, M. R.; Porter, F. S.; Sibeck, D. G.; Carter, J. A.; Chiao, M. P.; Chornay, D. J.; Cravens, T.; Galeazzi, M.; Keller, J. W.; Koutroumpa, D.; Kuntz, K.; Read, A. M.; Robertson, I. P.; Sembay, S.; Snowden, S.; Thomas, N.

    2012-01-01

    We describe current progress in the development of a prototype wide field-of-view soft X-ray imager that employs Lobstereye optics and targets heliophysics, planetary, and astrophysics science. The prototype will provide proof-of-concept for a future flight instrument capable of imaging the entire dayside magnetosheath from outside the magnetosphere. Such an instrument was proposed for the ESA AXIOM mission.

  17. Prototyping a Global Soft X-ray Imaging Instrument for Heliophysics, Planetary Science, and Astrophysics Science

    NASA Technical Reports Server (NTRS)

    Collier, Michael R.; Porter, F. Scott; Sibeck, David G.; Carter, Jenny A.; Chiao, Meng P.; Chornay, Dennis J.; Cravens, Thomas; Galeazzi, Massimiliano; Keller, John W.; Koutroumpa, Dimitra; Kuntz, Kip; Read, Any M.; Robertson, Ina P.; Sembay, Steve; Snowden, Steven; Thomas, Nick

    2012-01-01

    We describe current progress in the development of a prototype wide field-of-view soft X-ray imager that employs Lobster-eye optics and targets heliophysics, planetary, and astrophysics science. The prototype will provide proof-of-concept for a future flight instrument capable of imaging the entire dayside magnetosheath from outside the magnetosphere. Such an instrument was proposed for the FSA AXIOM mission

  18. Prototyping a global soft X-ray imaging instrument for heliophysics, planetary science, and astrophysics science

    NASA Astrophysics Data System (ADS)

    Collier, M. R.; Porter, F. S.; Sibeck, D. G.; Carter, J. A.; Chiao, M. P.; Chornay, D. J.; Cravens, T.; Galeazzi, M.; Keller, J. W.; Koutroumpa, D.; Kuntz, K.; Read, A. M.; Robertson, I. P.; Sembay, S.; Snowden, S.; Thomas, N.

    2012-04-01

    We describe current progress in the development of a prototype wide field-of-view soft X-ray imager that employs Lobster-eye optics and targets heliophysics, planetary, and astrophysics science. The prototype will provide proof-of-concept for a future flight instrument capable of imaging the entire dayside magnetosheath from outside the magnetosphere. Such an instrument was proposed for the ESA AXIOM mission.

  19. What Can Be Learned from X-Ray Spectroscopy Concerning Hot Gas in the Local Bubble and Charge Exchange Processes?

    NASA Technical Reports Server (NTRS)

    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.

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

    SciTech Connect

    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.

  1. A stored-ion target for x-ray spectroscopy of multicharged ions

    SciTech Connect

    Kanter, E.P.

    1996-08-01

    With the evolution of the new third generation synchrotron radiation sources providing intense beams of hard x-rays, it is natural to consider exploiting these to investigate the 3-body Coulomb problem. The atomic physics community could advance this field considerably by developing general techniques to investigate the x-ray spectroscopy of heliumlike ions. To do so, however, requires the development of a target of such ions with sufficient density to permit photoexcitation studies in the hard x-ray regime. A possible scheme to achieve this is described. Such a target system would permit x-ray studies with exotic species such as highly charged atomic ions, size-selected cluster ions, and atomic and molecular negative ions which have hitherto been impractical to study with conventional techniques.

  2. Laboratory von Hámos X-ray spectroscopy for routine sample characterization

    NASA Astrophysics Data System (ADS)

    Németh, Zoltán; Szlachetko, Jakub; Bajnóczi, Éva G.; Vankó, György

    2016-10-01

    High energy resolution, hard X-ray spectroscopies are powerful element selective probes of the electronic and local structure of matter, with diverse applications in chemistry, physics, biology, and materials science. The routine application of these techniques is hindered by the complicated and slow access to synchrotron radiation facilities. Here we propose a new, economic, easily operated laboratory high resolution von Hámos type X-ray spectrometer, which offers rapid transmission experiments for X-ray absorption and is also capable of recording X-ray emission spectra. The use of a cylindrical analyzer crystal and a position sensitive detector enabled us to build a robust, flexible setup with low operational costs, while delivering synchrotron grade signal to noise measurements in reasonable acquisition times. We demonstrate the proof of principle and give examples for both measurement types. Finally, tracking of a several day long chemical transformation, a case better suited for laboratory than synchrotron investigation, is also presented.

  3. X-ray photoemission and energy dispersive spectroscopy of hydroxyapatite-coated titanium

    SciTech Connect

    Drummond, J.L.; Steinberg, A.D.; Krauss, A.R.

    1997-07-01

    The purpose of this study was to determine the chemical composition changes of hydroxyapatite (HA) coated titanium using surface analysis (X-ray photoemission) and bulk analysis (energy dispersive spectroscopy). The specimens examined were controls and specimens aged 30 min and 3 h at room temperature in distilled water and 0.2M sodium phosphate buffer (pH 7.2). Each X-ray photoemission cycle consisted of three scans followed by argon sputtering for 10 min for usually 20 cycles, corresponding to a sampling depth of {approximately}1,500 {angstrom}. The energy dispersive spectroscopy analysis was on a 110 by 90 {micro}m area for 500 s. The X-ray photoemission results indicated the oxidation effect of water on the titanium (as TiO{sub 2}) and the effect of the buffer to increase the surface concentration of phosphorus. No differences in the chemical composition were observed by energy dispersive spectroscopy analysis.

  4. Ultra-soft x-ray absorption spectroscopy: A bulk and surface probe of materials

    SciTech Connect

    Fischer, D.A. ); Mitchell, G.E.; Dekoven, B.M. ); Yeh, A.T.; Gland, J.L. ); Moodenbaugh, A.R. )

    1993-01-01

    Direct comparisons between surface and bulk of diverse materials can be made by simultaneous electron yield (5 nm depth sensitivity) and fluorescence yield (200 nm) ultra soft x-ray absorption spectroscopy measurements utilizing a rapid sample interchange apparatus. For example the orientations of functional groups have been characterized at and near the surface of a series of model polymeric materials highlighting the chemical and molecular sensitivity of ultra soft x-ray absorption spectroscopy. In addition we discuss a bulk sensitive use of fluorescence yield to non destructively study a buried metal polymer interface. A second bulk sensitive example is the use of fluorescence yield oxygen K near edge x-ray spectroscopy as a method to determine the hole state density of high Tc materials.

  5. Ultra-soft x-ray absorption spectroscopy: A bulk and surface probe of materials

    SciTech Connect

    Fischer, D.A.; Mitchell, G.E.; Dekoven, B.M.; Yeh, A.T.; Gland, J.L.; Moodenbaugh, A.R.

    1993-06-01

    Direct comparisons between surface and bulk of diverse materials can be made by simultaneous electron yield (5 nm depth sensitivity) and fluorescence yield (200 nm) ultra soft x-ray absorption spectroscopy measurements utilizing a rapid sample interchange apparatus. For example the orientations of functional groups have been characterized at and near the surface of a series of model polymeric materials highlighting the chemical and molecular sensitivity of ultra soft x-ray absorption spectroscopy. In addition we discuss a bulk sensitive use of fluorescence yield to non destructively study a buried metal polymer interface. A second bulk sensitive example is the use of fluorescence yield oxygen K near edge x-ray spectroscopy as a method to determine the hole state density of high Tc materials.

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

    NASA Astrophysics Data System (ADS)

    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.

  7. In situ anodization of aluminum surfaces studied by x-ray reflectivity and electrochemical impedance spectroscopy

    NASA Astrophysics Data System (ADS)

    Bertram, F.; Zhang, F.; Evertsson, J.; Carlà, F.; Pan, J.; Messing, M. E.; Mikkelsen, A.; Nilsson, J.-O.; Lundgren, E.

    2014-07-01

    We present results from the anodization of an aluminum single crystal [Al(111)] and an aluminum alloy [Al 6060] studied by in situ x-ray reflectivity, in situ electrochemical impedance spectroscopy and ex situ scanning electron microscopy. For both samples, a linear increase of oxide film thickness with increasing anodization voltage was found. However, the slope is much higher in the single crystal case, and the break-up of the oxide film grown on the alloy occurs at a lower anodization potential than on the single crystal. The reasons for these observations are discussed as are the measured differences observed for x-ray reflectivity and electrochemical impedance spectroscopy.

  8. In situ anodization of aluminum surfaces studied by x-ray reflectivity and electrochemical impedance spectroscopy

    SciTech Connect

    Bertram, F. Evertsson, J.; Messing, M. E.; Mikkelsen, A.; Lundgren, E.; Zhang, F.; Pan, J.; Carlà, F.; Nilsson, J.-O.

    2014-07-21

    We present results from the anodization of an aluminum single crystal [Al(111)] and an aluminum alloy [Al 6060] studied by in situ x-ray reflectivity, in situ electrochemical impedance spectroscopy and ex situ scanning electron microscopy. For both samples, a linear increase of oxide film thickness with increasing anodization voltage was found. However, the slope is much higher in the single crystal case, and the break-up of the oxide film grown on the alloy occurs at a lower anodization potential than on the single crystal. The reasons for these observations are discussed as are the measured differences observed for x-ray reflectivity and electrochemical impedance spectroscopy.

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

    NASA Astrophysics Data System (ADS)

    Mikhlin, Yuri; Tomashevich, Yevgeny; Vorobyev, Sergey; Saikova, Svetlana; Romanchenko, Alexander; Félix, Roberto

    2016-11-01

    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 FeS2 and pyrrhotite Fe1-xS 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.

  10. CdZnTe detector in mammographic x-ray spectroscopy.

    PubMed

    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.

  11. CdZnTe detector in mammographic x-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Miyajima, Satoshi; Imagawa, Kotaro

    2002-11-01

    A CdZnTe (CZT) detector was utilized in mammographic x-ray spectroscopy under clinical conditions. First, the detector response was investigated using γ-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.

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

    NASA Astrophysics Data System (ADS)

    Miaja-Avila, Luis; O'Neil, Galen C.; Joe, Young I.; Alpert, Bradley K.; Damrauer, Niels H.; Doriese, William B.; Fatur, Steven M.; Fowler, Joseph W.; Hilton, Gene C.; Jimenez, Ralph; Reintsema, Carl D.; Schmidt, Daniel R.; Silverman, Kevin L.; Swetz, Daniel S.; Tatsuno, Hideyuki; Ullom, Joel N.

    2016-07-01

    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.

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

    SciTech Connect

    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.).

  14. Improved detection limits in PIXE analysis employing wavelength dispersive X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Kavčič, M.

    2010-11-01

    A wavelength dispersive X-ray spectroscopy was employed to measure the proton induced Lα X-ray emission spectra of Ag, Pd and Cd targets in order to lower detection limits for trace amounts of Pd and Cd in silver matrix. The measurements were performed with a Johansson-type crystal spectrometer having an energy resolution below the natural linewidths of the measured L X-ray lines. As a direct consequence of such ultrahigh experimental energy resolution, detection limits of only few tens of ppm were reached. The method presented in this work can be used in general to improve substantially PIXE detection limits compared to standard energy dispersive spectroscopy for the measurement of trace elements with atomic number in the close vicinity of the atomic number of the target matrix element.

  15. A model for testing strong gravity via X-ray reflection spectroscopy

    NASA Astrophysics Data System (ADS)

    Bambi, Cosimo; Nampalliwar, Sourabh; Cardenas-Avendano, Alejandro

    2016-07-01

    Astrophysical black hole candidates are thought to be the Kerr black holes of general relativity. However, a direct observational evidence is still lacking. The X-ray radiation produced in the inner part of the accretion disk can be a powerful tool to test the Kerr nature of these objects. In this talk, we present a new model for testing the Kerr black hole hypothesis via X-ray reflection spectroscopy. We employ the formalism of the transfer function proposed by Cunningham 40 years ago. The transfer function acts as an integration kernel and takes into account all the relativistic effects. We have developed a code to compute transfer functions in arbitrary stationary and axisymmetric spacetimes. These transfer functions are tabulated in FITS files and combined with XILLVER. The result is best model that we can have today for testing black hole candidates via X-ray reflection spectroscopy.

  16. Surface Dynamics of Block Copolymer Films by X-ray Photon Correlation Spectroscopy

    SciTech Connect

    Song, Sanghoon; Cha, Wonsuk; Lee, Heeju; Li, Xiaolong; Kim, Hyunjung; Jiang, Zhang; Narayanan, Suresh; Ruehm, Adrian; Sinha, S. K.

    2009-04-19

    We investigated the structure and dynamics of supported block copolymer films of poly(styrene)-b-poly(dimethylsiloxane)(PS-b-PDMS) in the spherical phase by x-ray photon correlation spectroscopy (XPCS) in grazing angle geometry. The temperature range studied was between 160 deg. and 210 deg. C, much higher than glass transition temperature (Tg), with thickness from 40 nm to 600 nm. Using x-ray reflectivity and x-ray photoelectron spectroscopy (XPS), we found that the PDMS-rich layer near the surface appeared at a temperature higher than Tg. Universal scaling of the dynamics, even with the bilayer model, was observed. From the fitting with the bilayer model, viscosities from both layers were obtained. The results from the surface dynamics are compared with the theory of overdamped thermal capillary waves on thin films.

  17. Deciphering the Complex Chemistry of Deep-Ocean Particles Using Complementary Synchrotron X-ray Microscope and Microprobe Instruments.

    PubMed

    Toner, Brandy M; German, Christopher R; Dick, Gregory J; Breier, John A

    2016-01-19

    The reactivity and mobility of natural particles in aquatic systems have wide ranging implications for the functioning of Earth surface systems. Particles in the ocean are biologically and chemically reactive, mobile, and complex in composition. The chemical composition of marine particles is thought to be central to understanding processes that convert globally relevant elements, such as C and Fe, among forms with varying bioavailability and mobility in the ocean. The analytical tools needed to measure the complex chemistry of natural particles are the subject of this Account. We describe how a suite of complementary synchrotron radiation instruments with nano- and micrometer focusing, and X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) capabilities are changing our understanding of deep-ocean chemistry and life. Submarine venting along mid-ocean ridges creates hydrothermal plumes where dynamic particle-forming reactions occur as vent fluids mix with deep-ocean waters. Whether plumes are net sources or sinks of elements in ocean budgets depends in large part on particle formation, reactivity, and transport properties. Hydrothermal plume particles have been shown to host microbial communities and exhibit complex size distributions, aggregation behavior, and composition. X-ray microscope and microprobe instruments can address particle size and aggregation, but their true strength is in measuring chemical composition. Plume particles comprise a stunning array of inorganic and organic phases, from single-crystal sulfides to poorly ordered nanophases and polymeric organic matrices to microbial cells. X-ray microscopes and X-ray microprobes with elemental imaging, XAS, and XRD capabilities are ideal for investigating these complex materials because they can (1) measure the chemistry of organic and inorganic constituents in complex matrices, usually within the same particle or aggregate, (2) provide strong signal-to-noise data with exceedingly small

  18. Deciphering the Complex Chemistry of Deep-Ocean Particles Using Complementary Synchrotron X-ray Microscope and Microprobe Instruments.

    PubMed

    Toner, Brandy M; German, Christopher R; Dick, Gregory J; Breier, John A

    2016-01-19

    The reactivity and mobility of natural particles in aquatic systems have wide ranging implications for the functioning of Earth surface systems. Particles in the ocean are biologically and chemically reactive, mobile, and complex in composition. The chemical composition of marine particles is thought to be central to understanding processes that convert globally relevant elements, such as C and Fe, among forms with varying bioavailability and mobility in the ocean. The analytical tools needed to measure the complex chemistry of natural particles are the subject of this Account. We describe how a suite of complementary synchrotron radiation instruments with nano- and micrometer focusing, and X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) capabilities are changing our understanding of deep-ocean chemistry and life. Submarine venting along mid-ocean ridges creates hydrothermal plumes where dynamic particle-forming reactions occur as vent fluids mix with deep-ocean waters. Whether plumes are net sources or sinks of elements in ocean budgets depends in large part on particle formation, reactivity, and transport properties. Hydrothermal plume particles have been shown to host microbial communities and exhibit complex size distributions, aggregation behavior, and composition. X-ray microscope and microprobe instruments can address particle size and aggregation, but their true strength is in measuring chemical composition. Plume particles comprise a stunning array of inorganic and organic phases, from single-crystal sulfides to poorly ordered nanophases and polymeric organic matrices to microbial cells. X-ray microscopes and X-ray microprobes with elemental imaging, XAS, and XRD capabilities are ideal for investigating these complex materials because they can (1) measure the chemistry of organic and inorganic constituents in complex matrices, usually within the same particle or aggregate, (2) provide strong signal-to-noise data with exceedingly small

  19. Picosecond-resolved X-ray absorption spectroscopy at low signal contrast using a hard X-ray streak camera

    SciTech Connect

    Adams, Bernhard W.; Rose-Petruck, Christoph; Jiao, Yishuo

    2015-06-24

    A picosecond-resolving hard-X-ray streak camera has been in operation for several years at Sector 7 of the Advanced Photon Source (APS). Several upgrades have been implemented over the past few years to optimize integration into the beamline, reduce the timing jitter, and improve the signal-to-noise ratio. These include the development of X-ray optics for focusing the X-rays into the sample and the entrance slit of the streak camera, and measures to minimize the amount of laser light needed to generate the deflection-voltage ramp. For the latter, the photoconductive switch generating the deflection ramp was replaced with microwave power electronics. With these, the streak camera operates routinely at 88 MHz repetition rate, thus making it compatible with all of the APS fill patterns including use of all the X-rays in the 324-bunch mode. Sample data are shown to demonstrate the performance.

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

    SciTech Connect

    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.

  1. Cosmic X-ray Physics: A Suborbital Investigation of the Diffuse X-ray Background Including Instrumentation Development

    NASA Astrophysics Data System (ADS)

    McCammon, Dan

    We propose an investigation to improve our understanding of the Galactic diffuse X-ray background. The ultimate purpose of this is to determine the role of hot phases of the interstellar medium in mediating stellar feedback in star formation, in transport of metals, and in determining the structure and evolution of the Galaxy. This work will involve a flight of an existing payload with small modifications in Woomera, South Australia, to observe the Galactic soft X-ray bulge and attempt to determine its nature and emission mechanisms. It will also involve the development of detectors capable of 1-2 eV FWHM energy resolution in the 100-400 eV range with the intent of obtaining a scientifically useful spectrum on a sounding rocket flight of the emission from one million degree gas in this energy range. This will require a total area of 1-2 cm^2 for the detector array. With the collaboration and advice of microwave experts at the Goddard Space Flight Center, we will fabricate and test waveguide-below-cutoff filters to provide the necessary attenuation of infrared radiation for these detectors while still allowing relatively good x- ray transmission below 300 eV. The detectors, filters, and flight experience with the detector readouts are all relevant to future NASA major missions. The filters would be particularly valuable in allowing thermal detectors (microcalorimeters) similar to those used here in the X-ray range to be applied to the EUV and vacuum ultraviolet, where they offer large potential gains over existing detectors. These investigations will provide the primary training for our graduate students, and will involve a substantial number of undergraduates.

  2. X-Ray Diffraction Techniques for a Field Instrument: Patterns of Lithologic Provences

    NASA Astrophysics Data System (ADS)

    Marshall, J.; Keaten, R.

    1999-09-01

    Future exploration of Mars will attempt to shed light on the mineralogy of surface materials. Instruments deployed from remote platforms should have the capability to conduct both intensive analyses as well as rapid, reconnaissance surveys while they function in the martian environment as surrogate geologists. In order to accommodate the reconnaissance mode of analysis and to compensate for analytical limitations imposed by the space-flight conditions, data analysis methods are being developed that will permit interpretation of data by recognition of signatures or "fingerprints". Specifically, we are developing a technique which will allow interpretation of diffraction patterns by recognition of characteristic signatures of different lithologic provences. This technique allows a remote vehicle to function in a rapid-scan mode using the lithologic signature to determine where a more thorough analysis is needed. An x-ray diffraction pattern is characterized by the angular positions of diffracted x-rays, x-ray intensity levels and background radiation levels. These elements may be used to identify a generalized x-ray signature. Lithologic signatures are being developed in two ways. A signature is composed using the ideal powder diffraction indices from the mineral assembledge common to a specific lithologic provence. This is then confirmed using a laboratory diffraction pattern of a whole rock powder. Preliminary results comparing the diffraction signatures of the major mineral assembledges common to basalt, carbonate, and evaporite basin deposits indicate that lithologies are differentiable as a "fingerprint". Statistical analyses are being performed to establish the confidence levels of this technique.

  3. X-Ray Diffraction Techniques for a Field Instrument: Patterns of Lithologic Provences

    NASA Technical Reports Server (NTRS)

    Marshall, J.; Keaten, R.

    1999-01-01

    Future exploration of Mars will attempt to shed light on the mineralogy of surface materials. Instruments deployed from remote platforms should have the capability to conduct both intensive analyses as well as rapid, reconnaissance surveys while they function in the martian environment as surrogate geologists. In order to accommodate the reconnaissance mode of analysis and to compensate for analytical limitations imposed by the space-flight conditions, data analysis methods are being developed that will permit interpretation of data by recognition of signatures or "fingerprints". Specifically, we are developing a technique which will allow interpretation of diffraction patterns by recognition of characteristic signatures of different lithologic provences. This technique allows a remote vehicle to function in a rapid-scan mode using the lithologic signature to determine where a more thorough analysis is needed. An x-ray diffraction pattern is characterized by the angular positions of diffracted x-rays, x-ray intensity levels and background radiation levels. These elements may be used to identify a generalized x-ray signature. Lithologic signatures are being developed in two ways. A signature is composed using the ideal powder diffraction indices from the mineral assembledge common to a specific lithologic provence. This is then confirmed using a laboratory diffraction pattern of a whole rock powder. Preliminary results comparing the diffraction signatures of the major mineral assembledges common to basalt, carbonate, and evaporite basin deposits indicate that lithologies are differentiable as a "fingerprint". Statistical analyses are being performed to establish the confidence levels of this technique.

  4. Laboratory studies into the effect of regolith on planetary X-ray fluorescence spectroscopy

    NASA Astrophysics Data System (ADS)

    Näränen, Jyri; Parviainen, Hannu; Muinonen, Karri; Carpenter, James; Nygård, Kim; Peura, Marko

    2008-12-01

    In the analysis of X-ray fluorescence spectra from planetary surfaces, it is traditionally assumed that the observed surface is a plane-parallel, smooth, and homogeneous medium. The spectral and spatial resolutions of the instruments that have been used to measure X-ray emission from planetary surfaces to date have been such that this has been a reasonable assumption, but a new generation of X-ray spectrometers will provide enhanced spectral and spatial resolutions when compared with previous instrumentation. In light of these improvements in performance, it is important to assess how the requirements on the methodology of analysis of spectra may change when the surface is considered as a regolith. At other wavelengths, varying physical properties of planetary regoliths, such as the packing density, are known to have an effect on the observed signal as a function of viewing geometry. In this paper, the results from laboratory X-ray fluorescence measurements of regolith analogue materials at different viewing geometries are presented. Characteristic properties of the regolith such as particle sizes and packing density are found to affect the measured elemental line ratios. A semiempirical function is introduced as a tool for fitting fluorescent line intensity dependences as a function of viewing geometry. The importance of the results is discussed and recommendations are made for the future analysis of planetary X-ray fluorescence data.

  5. Secondary ion mass spectrometry and X-ray photoelectron spectroscopy of derivitized coal surfaces

    SciTech Connect

    Martin, R.R.; Mc Intyre, N.S.; Mac Phee, J.A.; Aye, K.T.

    1987-04-01

    Secondary Ion Mass Spectrometry (SIMS) and X-ray Photoelectron Spectroscopy (XPS) have been used to study the low temperature oxidation of coal. /sup 18/O has been used to trace the oxygen distribution on the coal surface. Several chemical derivations have been observed on the oxidized coal surface and the reactivity of specific regions have been monitored.

  6. Properties of a transmission grating behind a grazing incidence telescope for cosmic x-ray spectroscopy.

    PubMed

    Beuermann, K P; Lenzen, R; Bräuninger, H

    1977-05-01

    Third-order aberrations are discussed of a transmission grating positioned behind a Wolter type I telescope, using Fermat's principle. We describe the conditions required to obtain a coma-free grating. The performance of a grating spectrometer for cosmic x-ray spectroscopy is discussed in some detail. PMID:20168712

  7. X-ray spectroscopy of highly-ionized atoms in an electron beam ion trap (EBIT)

    SciTech Connect

    Marrs, R.E.; Bennett, C.; Chen, M.H.; Cowan, T.; Dietrich, D.; Henderson, J.R.; Knapp, D.A.; Levine, M.A.; Schneider, M.B.; Scofield, J.H.

    1988-01-01

    An Electron Beam Ion Trap at Lawrence Livermore National Laboratory is being used to produce and trap very-highly-charged-ions (q /le/ 70+) for x-ray spectroscopy measurements. Recent measurements of dielectronic recombination, electron impact excitation and transition energies are presented. 15 refs., 12 figs., 1 tab.

  8. Application of x-ray absorption spectroscopy to the study of corrosion and inhibition

    SciTech Connect

    Davenport, A.J.; Isaacs, H.S.

    1991-01-01

    X-ray absorption spectroscopy is a powerful technique for determination of valency and coordination. Measurements can be made in air or in situ under electrochemical control. The technique will be described and its application to the analysis of passive oxide films, corrosion products, and inhibitors will be reviewed.

  9. X-ray and Dielectric Spectroscopy Studies Of Chiral Ferroelectric Liquid Crystals With Keto Group

    SciTech Connect

    Stojanovic, Maja; Obadovic, Dusanka Z.; Bubnov, Alexej; Hamplova, Vera; Kaspar, Miroslav

    2007-04-23

    Series of ferroelectric liquid crystals with the keto group attached to the molecule core and one lactate group as the chiral centre have been studied by X-ray and dielectric spectroscopy. The thickness of smectic layers and the average distance between the long axes of neighboring molecules increases with increase of both chains.

  10. Passive Spectroscopy Bolometers, Grating- And X-Ray Imaging Crystal Spectrometers

    SciTech Connect

    Bitter, M; Hill, K W; Scott, S; Paul, S; Ince-Cushmann, A; Reinke, M; Rice, J; Beiersdorfer, P; Gu, M F; Lee, S G; Broennimann, C; Eikenberry, E F

    2007-11-07

    This tutorial gives a brief introduction into passive spectroscopy and describes the working principles of bolometers, a high-resolution grating spectrometer, and a novel X-ray imaging crystal spectrometer, which is of particular interest for profile measurements of the ion temperature and plasma rotation velocity on ITER and future burning plasma experiments.

  11. Ab initio simulation of diffractometer instrumental function for high-resolution X-ray diffraction1

    PubMed Central

    Mikhalychev, Alexander; Benediktovitch, Andrei; Ulyanenkova, Tatjana; Ulyanenkov, Alex

    2015-01-01

    Modeling of the X-ray diffractometer instrumental function for a given optics configuration is important both for planning experiments and for the analysis of measured data. A fast and universal method for instrumental function simulation, suitable for fully automated computer realization and describing both coplanar and noncoplanar measurement geometries for any combination of X-ray optical elements, is proposed. The method can be identified as semi-analytical backward ray tracing and is based on the calculation of a detected signal as an integral of X-ray intensities for all the rays reaching the detector. The high speed of calculation is provided by the expressions for analytical integration over the spatial coordinates that describe the detection point. Consideration of the three-dimensional propagation of rays without restriction to the diffraction plane provides the applicability of the method for noncoplanar geometry and the accuracy for characterization of the signal from a two-dimensional detector. The correctness of the simulation algorithm is checked in the following two ways: by verifying the consistency of the calculated data with the patterns expected for certain simple limiting cases and by comparing measured reciprocal-space maps with the corresponding maps simulated by the proposed method for the same diffractometer configurations. Both kinds of tests demonstrate the agreement of the simulated instrumental function shape with the measured data. PMID:26089760

  12. Feasibility of an integrated X-ray instrument for Mars exobiology and geology. [Abstract only

    NASA Technical Reports Server (NTRS)

    Fonda, M. L.; Schwartz, D. E.; Koppel, L. N.; Franco, E. D.; Kerner, J. A.

    1994-01-01

    By employing an integrated X-ray instrument on a future Mars mission, data obtained will greatly augment those returned by Viking; details relevant to the possibility of the origin and evolution of life on Mars will be acquired. An integrated combined X Ray Fluorescence/X Ray Detection (XRF/XRD) instrument has been breadboarded and demonstrated to accommodate important exobiology and geology experiment objectives outlined for Mars Environmental Survey (MESUR) and future Mars missions. Among others, primary objectives for the exploration of Mars include: the intense study of local areas on Mars to 'establish the chemical, mineralogical, and petrological character of different components of the surface material; to determine the distribution, abundance and sources and sinks of volatile materials, including an assessment of the biologic potential, now and during past epochs; and to establish the global chemical and physical characteristics of the Martian surface'. The XRF/XRD breadboard instrument identifies and quantifies soil surface elemental, mineralogical, and petrological characteristics and acquires data necessary to address questions on volatile abundance and distribution. Additionally, the breadboard is able to characterize the biogenic element constituents of soil samples providing information on the biologic potential of the Mars environment.

  13. The Mn₄Ca photosynthetic water-oxidation catalyst studied by simultaneous X-ray spectroscopy and crystallography using an X-ray free-electron laser.

    PubMed

    Tran, Rosalie; Kern, Jan; Hattne, Johan; Koroidov, Sergey; Hellmich, Julia; Alonso-Mori, Roberto; Sauter, Nicholas K; Bergmann, Uwe; Messinger, Johannes; Zouni, Athina; Yano, Junko; Yachandra, Vittal K

    2014-07-17

    The structure of photosystem II and the catalytic intermediate states of the Mn₄CaO₅ cluster involved in water oxidation have been studied intensively over the past several years. An understanding of the sequential chemistry of light absorption and the mechanism of water oxidation, however, requires a new approach beyond the conventional steady-state crystallography and X-ray spectroscopy at cryogenic temperatures. In this report, we present the preliminary progress using an X-ray free-electron laser to determine simultaneously the light-induced protein dynamics via crystallography and the local chemistry that occurs at the catalytic centre using X-ray spectroscopy under functional conditions at room temperature.

  14. The Mn₄Ca photosynthetic water-oxidation catalyst studied by simultaneous X-ray spectroscopy and crystallography using an X-ray free-electron laser.

    PubMed

    Tran, Rosalie; Kern, Jan; Hattne, Johan; Koroidov, Sergey; Hellmich, Julia; Alonso-Mori, Roberto; Sauter, Nicholas K; Bergmann, Uwe; Messinger, Johannes; Zouni, Athina; Yano, Junko; Yachandra, Vittal K

    2014-07-17

    The structure of photosystem II and the catalytic intermediate states of the Mn₄CaO₅ cluster involved in water oxidation have been studied intensively over the past several years. An understanding of the sequential chemistry of light absorption and the mechanism of water oxidation, however, requires a new approach beyond the conventional steady-state crystallography and X-ray spectroscopy at cryogenic temperatures. In this report, we present the preliminary progress using an X-ray free-electron laser to determine simultaneously the light-induced protein dynamics via crystallography and the local chemistry that occurs at the catalytic centre using X-ray spectroscopy under functional conditions at room temperature. PMID:24914152

  15. New developments in micro-X-ray diffraction and X-ray absorption spectroscopy for high-pressure research at 16-BM-D at the Advanced Photon Source.

    PubMed

    Park, Changyong; Popov, Dmitry; Ikuta, Daijo; Lin, Chuanlong; Kenney-Benson, Curtis; Rod, Eric; Bommannavar, Arunkumar; Shen, Guoyin

    2015-07-01

    The monochromator and focusing mirrors of the 16-BM-D beamline, which is dedicated to high-pressure research with micro-X-ray diffraction (micro-XRD) and X-ray absorption near edge structure (XANES) (6-45 keV) spectroscopy, have been recently upgraded. Monochromatic X-rays are selected by a Si (111) double-crystal monochromator operated in an artificial channel-cut mode and focused to 5 μm × 5 μm (FWHM) by table-top Kirkpatrick-Baez type mirrors located near the sample stage. The typical X-ray flux is ∼5 × 10(8) photons/s at 30 keV. The instrumental resolution, Δq/qmax, reaches to 2 × 10(-3) and is tunable through adjustments of the detector distance and X-ray energy. The setup is stable and reproducible, which allows versatile application to various types of experiments including resistive heating and cryogenic cooling as well as ambient temperature compression. Transmission XANES is readily combined with micro-XRD utilizing the fixed-exit feature of the monochromator, which allows combined XRD-XANES measurements at a given sample condition.

  16. New developments in micro-X-ray diffraction and X-ray absorption spectroscopy for high-pressure research at 16-BM-D at the Advanced Photon Source

    NASA Astrophysics Data System (ADS)

    Park, Changyong; Popov, Dmitry; Ikuta, Daijo; Lin, Chuanlong; Kenney-Benson, Curtis; Rod, Eric; Bommannavar, Arunkumar; Shen, Guoyin

    2015-07-01

    The monochromator and focusing mirrors of the 16-BM-D beamline, which is dedicated to high-pressure research with micro-X-ray diffraction (micro-XRD) and X-ray absorption near edge structure (XANES) (6-45 keV) spectroscopy, have been recently upgraded. Monochromatic X-rays are selected by a Si (111) double-crystal monochromator operated in an artificial channel-cut mode and focused to 5 μm × 5 μm (FWHM) by table-top Kirkpatrick-Baez type mirrors located near the sample stage. The typical X-ray flux is ˜5 × 108 photons/s at 30 keV. The instrumental resolution, Δq/qmax, reaches to 2 × 10-3 and is tunable through adjustments of the detector distance and X-ray energy. The setup is stable and reproducible, which allows versatile application to various types of experiments including resistive heating and cryogenic cooling as well as ambient temperature compression. Transmission XANES is readily combined with micro-XRD utilizing the fixed-exit feature of the monochromator, which allows combined XRD-XANES measurements at a given sample condition.

  17. New developments in micro-X-ray diffraction and X-ray absorption spectroscopy for high-pressure research at 16-BM-D at the Advanced Photon Source

    SciTech Connect

    Park, Changyong Popov, Dmitry; Ikuta, Daijo; Lin, Chuanlong; Kenney-Benson, Curtis; Rod, Eric; Bommannavar, Arunkumar; Shen, Guoyin

    2015-07-15

    The monochromator and focusing mirrors of the 16-BM-D beamline, which is dedicated to high-pressure research with micro-X-ray diffraction (micro-XRD) and X-ray absorption near edge structure (XANES) (6-45 keV) spectroscopy, have been recently upgraded. Monochromatic X-rays are selected by a Si (111) double-crystal monochromator operated in an artificial channel-cut mode and focused to 5 μm × 5 μm (FWHM) by table-top Kirkpatrick-Baez type mirrors located near the sample stage. The typical X-ray flux is ∼5 × 10{sup 8} photons/s at 30 keV. The instrumental resolution, Δq/q{sub max}, reaches to 2 × 10{sup −3} and is tunable through adjustments of the detector distance and X-ray energy. The setup is stable and reproducible, which allows versatile application to various types of experiments including resistive heating and cryogenic cooling as well as ambient temperature compression. Transmission XANES is readily combined with micro-XRD utilizing the fixed-exit feature of the monochromator, which allows combined XRD-XANES measurements at a given sample condition.

  18. Testing LaMgAl11O19 crystal for X-ray spectroscopy

    SciTech Connect

    Chen, H; Beiersdorfer, P; Baronova, E; Kalashnikova, I; Stepanenko, M

    2004-03-31

    We investigated the properties of the rare earth crystal LaMgAl{sub 11}O{sub 19} and its application to soft X-ray spectroscopy. Its relative reflectivity and half width rocking curve were measured to up to the reflection order of 28. In addition, a comparative measurement of the iron L-shell soft X-ray line emission was made on the EBIT-I Livermore electron beam ion trap by fielding the LaMgAl{sub 11}O{sub 19} crystal side by side with a rubidium hydrogen phthalate crystal in a flat crystal spectrometer. From these measurements, reflectivity and spectral resolving power were determined.

  19. Two-dimensional stimulated resonance Raman spectroscopy of molecules with broadband x-ray pulses

    PubMed Central

    Biggs, Jason D.; Zhang, Yu; Healion, Daniel; Mukamel, Shaul

    2012-01-01

    Expressions for the two-dimensional stimulated x-ray Raman spectroscopy (2D-SXRS) signal obtained using attosecond x-ray pulses are derived. The 1D- and 2D-SXRS signals are calculated for trans-N-methyl acetamide (NMA) with broad bandwidth (181 as, 14.2 eV FWHM) pulses tuned to the oxygen and nitrogen K-edges. Crosspeaks in 2D signals reveal electronic Franck-Condon overlaps between valence orbitals and relaxed orbitals in the presence of the core-hole. PMID:22583220

  20. Soft-x-ray emission spectroscopy study of the electronic structure of nonstoichiometric silicon nitride

    NASA Astrophysics Data System (ADS)

    Nithianandam, V. Jeyasingh; Schnatterly, S. E.

    1987-07-01

    Soft-x-ray emission spectroscopy was used to investigate the electronic structure of nonstoichiometric silicon nitride samples of different compositions. The Si L23 x-ray emission spectra from these samples are presented and interpreted using a two-phase linear superposition model for the valence-band region. We assumed a model for the valence-band edge and for the emission in the gap region due to trap states and the Si 2p core exciton. The results obtained from these fits are compared with relevant models and other experiments.

  1. X-Ray Absorption Spectroscopy Study of Copper Doped ZnO Thin Films

    SciTech Connect

    Ma Qing

    2007-02-02

    X-ray absorption spectroscopy technique is used to study copper-doped ZnO thin films, prepared by pulsed-laser deposition. The samples with various doping levels are examined. It is found that the samples contain metallic clusters with the sizes {<=} 2 nm as well as Cu1+ and Cu2+ states. The Cu1+ states exist as stable oxide clusters, while the Cu2+ ones participate in the ZnO lattice some of which may be pertaining to the surfaces of the Cu clusters as well. The copper clusters of {approx}1 nm are unstable and fragment under monochromatic x-ray beam illumination.

  2. Thermal Expansion Behaviour of Silver Examined by Extended X-Ray Absorption Fine Structure Spectroscopy

    SciTech Connect

    Dubiel, M.; Chasse, A.; Haug, J.; Schneider, R.; Kruth, H.

    2007-02-02

    EXAFS (extended X-ray absorption fine structure) investigations are reported concerning the thermal expansion behaviour of silver in an extended range of temperature from 10 K to about 950 K measured in transmission mode. Both the ratio method and an EXAFS fitting procedure were applied to reveal the temperature dependence of EXAFS parameters. Models based on quantum and classical thermodynamic perturbation theory have been used to interpret experimental data and compared to XRD (X-ray diffraction) results of bulk silver material. The description of thermodynamic data of thermal expansion of silver in the complete range of temperature by EXAFS Spectroscopy was successful by first calculations using third order quantum perturbation theory.

  3. Near-infrared spectroscopy of faint discrete X-ray point sources constituting the Galactic ridge X-ray emission

    NASA Astrophysics Data System (ADS)

    Morihana, Kumiko; Tsujimoto, Masahiro; Dubath, Pierre; Yoshida, Tessei; Suzuki, Kensuke; Ebisawa, Ken

    2016-08-01

    The Galactic Ridge X-ray Emission (GRXE) is an apparently extended X-ray emission along the Galactic plane. The X-ray spectrum is characterized by a hard continuum with a strong Fe K emission feature in the 6-7 keV band. A substantial fraction (˜80%) of the GRXE in the Fe band was resolved into point sources by deep Chandra imaging observations; thus GRXE is mostly composed of dim Galactic X-ray point sources, at least in this energy band. To investigate the populations of these dim X-ray point sources, we carried out near-infrared (NIR) follow-up spectroscopic observations in two deep Chandra fields located in the Galactic plane at (l, b) = (0.1°, -1.4°) and (28.5°, 0.0°) using NTT/SofI and Subaru/MOIRCS. We obtained well-exposed NIR spectra from 65 objects and found that there are three main classes of Galactic sources based on the X-ray color and NIR spectral features: those having (A) hard X-ray spectra and NIR emission features such as H I (Brγ), He I, and He II (2 objects), (B) soft X-ray spectra and NIR absorption features such as H I, Na I, Ca I, and CO (46 objects), and (C) hard X-ray spectra and NIR absorption features such as H I, Na I, Ca I, and CO (17 objects). From these features, we argue that class A sources are cataclysmic variables (CVs), and class B sources are late-type stars with enhanced coronal activity, which is in agreement with current knowledge. Class C sources possibly belong to a new group of objects, which has been poorly studied so far. We argue that the candidate sources for class C are the binary systems hosting white dwarfs and late-type companions with very low accretion rates. It is likely that this newly recognized class of sources contribute to a non-negligible fraction of the GRXE, especially in the Fe K band.

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

    DOE PAGESBeta

    Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; Sokaras, Dimosthenis; Weng, Tsu -Chien; Lassalle-Kaiser, Benedikt; Tran, Rosalie; Hattne, Johan; Laksmono, Hartawan; Hellmich, Julia; et al

    2012-11-05

    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 wellmore » 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. Furthermore, 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.« less

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

    SciTech Connect

    Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; Sokaras, Dimosthenis; Weng, Tsu -Chien; Lassalle-Kaiser, Benedikt; Tran, Rosalie; Hattne, Johan; Laksmono, Hartawan; Hellmich, Julia; Glockner, 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, Sebastien; Williams, Garth J.; Zouni, Athina; Messinger, Johannes; Glatzel, Pieter; Sauter, Nicholas K.; Yachandra, Vittal K.; Yano, Junko; Bergmann, Uwe

    2012-11-05

    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. Furthermore, 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.

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

    PubMed Central

    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. Solar X-ray polarimetry and spectrometry instrument PING-M for the Interhelioprobe mission

    NASA Astrophysics Data System (ADS)

    Kotov, Yu. D.; Yurov, V. N.; Glyanenko, A. S.; Lupar, E. E.; Kochemasov, A. V.; Trofimov, Yu. A.; Zakharov, M. S.; Faradzhaev, R. M.; Tyshkevich, V. G.; Rubtsov, I. V.; Dergachev, V. A.; Kruglov, E. M.; Lazutkov, V. P.; Savchenko, M. I.; Skorodumov, D. V.

    2016-08-01

    The PING-M experiment is designed to investigate solar X-ray activity. The instrument includes a hard X-ray polarimeter (PING-P), a hard X-ray spectrometer (HXRS) and a soft X-ray spectrometer (SXRS). PING-P has the energy range of 20-150 keV and an effective area of about 2.5 cm2. It uses three organic scintillation detectors as active scatterers, which work in coincidence with six absorber detectors, based on CsI(Tl) scintillator. This technique allows us to considerably improve the polarimeter sensitivity. HXRS has the energy range of 20-600 keV and an effective area of about 15 cm2. It is based on a fast inorganic scintillator (LaBr3(Ce) or CeBr3) with a relatively high energy resolution of 3.5-4.5% at 662 keV. The SXRS energy range is 1.5-25 keV, and its aperture is ø0.1 mm, which provides the registration of solar flares in the range from C1 to X20 class of GOES scale. It is based on a SDD semiconductor detector with an energy resolution better than 200 eV at 5.9 keV line. The experiment will be performed onboard the Russian interplanetary mission Interhelioprobe which is planned for launch after 2025. The instrument will allow us to investigate angular and energy distributions of accelerated electrons, plasma heating processes, etc. Stereoscopic polarimetry and spectrometric observations will be possible if a similar instrument is installed onboard a near Earth satellite, or the second probe of the Interhelioprobe mission.

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

    NASA Technical Reports Server (NTRS)

    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.

  9. Characterization of surface carbon films on weathered Japaneseroof tiles by soft x-ray spectroscopy

    SciTech Connect

    Muramatsu, Y.; Yamashita, M.; Motoyama, M.; Hirose, M.; Denlinger, J.D.; Gullikson, E.M.; Perera, R.C.

    2004-07-15

    The effects of weathering on carbon films deposited onJapanese smoked roof tileswere investigated by soft x-ray absorption andemission spectroscopy using synchrotron radiation. X-ray absorptionmeasurements revealed that weathering oxidizes the carbon films and thatpartial carboxy chemical bonding occurs. Incident angle-dependent x-rayabsorption spectra in the C K region confirmed that the degree of theorientation at the surface of the oxidized carbon films decreases withweathering. However, the take-off angle-dependent C K x-ray emissionspectra showed that the orientation of the layered carbon structure ismaintained in the bulk portion when weathered. Therefore, it is confirmedthat oxidation proceeds from the surface of the carbon films. Weatheringdegrades and oxidizes the surface carbon films, which causes the metallicsilver color to change to darker gray.

  10. Sequential single shot X-ray photon correlation spectroscopy at the SACLA free electron laser

    SciTech Connect

    Lehmkühler, Felix; Kwaśniewski, Paweł; Roseker, Wojciech; Fischer, Birgit; Schroer, Martin A.; Tono, Kensuke; Katayama, Tetsuo; Sprung, Michael; Sikorski, Marcin; Song, Sanghoon; Glownia, James; Chollet, Matthieu; Nelson, Silke; Robert, Aymeric; Gutt, Christian; Yabashi, Makina; Ishikawa, Tetsuya; Grübel, Gerhard

    2015-11-27

    In this study, hard X-ray free electron lasers allow for the first time to access dynamics of condensed matter samples ranging from femtoseconds to several hundred seconds. In particular, the exceptional large transverse coherence of the X-ray pulses and the high time-averaged flux promises to reach time and length scales that have not been accessible up to now with storage ring based sources. However, due to the fluctuations originating from the stochastic nature of the self-amplified spontaneous emission (SASE) process the application of well established techniques such as X-ray photon correlation spectroscopy (XPCS) is challenging. Here we demonstrate a single-shot based sequential XPCS study on a colloidal suspension with a relaxation time comparable to the SACLA free-electron laser pulse repetition rate. High quality correlation functions could be extracted without any indications for sample damage. This opens the way for systematic sequential XPCS experiments at FEL sources.

  11. Sequential Single Shot X-ray Photon Correlation Spectroscopy at the SACLA Free Electron Laser.

    PubMed

    Lehmkühler, Felix; Kwaśniewski, Paweł; Roseker, Wojciech; Fischer, Birgit; Schroer, Martin A; Tono, Kensuke; Katayama, Tetsuo; Sprung, Michael; Sikorski, Marcin; Song, Sanghoon; Glownia, James; Chollet, Matthieu; Nelson, Silke; Robert, Aymeric; Gutt, Christian; Yabashi, Makina; Ishikawa, Tetsuya; Grübel, Gerhard

    2015-01-01

    Hard X-ray free electron lasers allow for the first time to access dynamics of condensed matter samples ranging from femtoseconds to several hundred seconds. In particular, the exceptional large transverse coherence of the X-ray pulses and the high time-averaged flux promises to reach time and length scales that have not been accessible up to now with storage ring based sources. However, due to the fluctuations originating from the stochastic nature of the self-amplified spontaneous emission (SASE) process the application of well established techniques such as X-ray photon correlation spectroscopy (XPCS) is challenging. Here we demonstrate a single-shot based sequential XPCS study on a colloidal suspension with a relaxation time comparable to the SACLA free-electron laser pulse repetition rate. High quality correlation functions could be extracted without any indications for sample damage. This opens the way for systematic sequential XPCS experiments at FEL sources. PMID:26610328

  12. Sequential Single Shot X-ray Photon Correlation Spectroscopy at the SACLA Free Electron Laser

    NASA Astrophysics Data System (ADS)

    Lehmkühler, Felix; Kwaśniewski, Paweł; Roseker, Wojciech; Fischer, Birgit; Schroer, Martin A.; Tono, Kensuke; Katayama, Tetsuo; Sprung, Michael; Sikorski, Marcin; Song, Sanghoon; Glownia, James; Chollet, Matthieu; Nelson, Silke; Robert, Aymeric; Gutt, Christian; Yabashi, Makina; Ishikawa, Tetsuya; Grübel, Gerhard

    2015-11-01

    Hard X-ray free electron lasers allow for the first time to access dynamics of condensed matter samples ranging from femtoseconds to several hundred seconds. In particular, the exceptional large transverse coherence of the X-ray pulses and the high time-averaged flux promises to reach time and length scales that have not been accessible up to now with storage ring based sources. However, due to the fluctuations originating from the stochastic nature of the self-amplified spontaneous emission (SASE) process the application of well established techniques such as X-ray photon correlation spectroscopy (XPCS) is challenging. Here we demonstrate a single-shot based sequential XPCS study on a colloidal suspension with a relaxation time comparable to the SACLA free-electron laser pulse repetition rate. High quality correlation functions could be extracted without any indications for sample damage. This opens the way for systematic sequential XPCS experiments at FEL sources.

  13. Superconducting Detector System for High-Resolution Energy-Dispersive Soft X-Ray Spectroscopy

    SciTech Connect

    Friedrich, S; Niedermayr, T; Drury, O; Funk, T; Frank, M; Labov, S E; Cramer, S

    2001-02-21

    Synchrotron-based soft x-ray spectroscopy is often limited by detector performance. Grating spectrometers have the resolution, but lack the efficiency for the analysis of dilute samples. Semiconducting Si(Li) or Ge detectors are efficient, but often lack the resolution to separate weak signals from strong nearby lines in multi-element samples. Superconducting tunnel junctions (STJs) operated at temperatures below 1 K can be used as high-resolution high-efficiency x-ray detectors. They combine high energy resolution around 10 eV FWHM with the broad band efficiency of energy-dispersive detectors. We have designed a two-stage adiabatic demagnetization refrigerator (ADR) to operate STJ detectors in x-ray fluorescence measurements at beam line 4 of the ALS. We demonstrate the capabilities of such a detector system for fluorescence analysis of dilute metal sites in proteins and inorganic model compounds.

  14. Sequential Single Shot X-ray Photon Correlation Spectroscopy at the SACLA Free Electron Laser

    PubMed Central

    Lehmkühler, Felix; Kwaśniewski, Paweł; Roseker, Wojciech; Fischer, Birgit; Schroer, Martin A.; Tono, Kensuke; Katayama, Tetsuo; Sprung, Michael; Sikorski, Marcin; Song, Sanghoon; Glownia, James; Chollet, Matthieu; Nelson, Silke; Robert, Aymeric; Gutt, Christian; Yabashi, Makina; Ishikawa, Tetsuya; Grübel, Gerhard

    2015-01-01

    Hard X-ray free electron lasers allow for the first time to access dynamics of condensed matter samples ranging from femtoseconds to several hundred seconds. In particular, the exceptional large transverse coherence of the X-ray pulses and the high time-averaged flux promises to reach time and length scales that have not been accessible up to now with storage ring based sources. However, due to the fluctuations originating from the stochastic nature of the self-amplified spontaneous emission (SASE) process the application of well established techniques such as X-ray photon correlation spectroscopy (XPCS) is challenging. Here we demonstrate a single-shot based sequential XPCS study on a colloidal suspension with a relaxation time comparable to the SACLA free-electron laser pulse repetition rate. High quality correlation functions could be extracted without any indications for sample damage. This opens the way for systematic sequential XPCS experiments at FEL sources. PMID:26610328

  15. Gas cell for in situ soft X-ray transmission-absorption spectroscopy of materials

    SciTech Connect

    Drisdell, W. S.; Kortright, J. B.

    2014-07-15

    A simple gas cell design, constructed primarily from commercially available components, enables in situ soft X-ray transmission-absorption spectroscopy of materials in contact with gas at ambient temperature. The cell has a minimum X-ray path length of 1 mm and can hold gas pressures up to ∼300 Torr, and could support higher pressures with simple modifications. The design enables cycling between vacuum and gas environments without interrupting the X-ray beam, and can be fully sealed to allow for measurements of air-sensitive samples. The cell can attach to the downstream port of any appropriate synchrotron beamline, and offers a robust and versatile method for in situ measurements of certain materials. The construction and operation of the cell are discussed, as well as sample preparation and proper spectral analysis, illustrated by examples of spectral measurements. Potential areas for improvement and modification for specialized applications are also mentioned.

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

    SciTech Connect

    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.

  17. A streaked X-ray spectroscopy platform for rapidly heated, near-solid density plasmas

    NASA Astrophysics Data System (ADS)

    Stillman, C. R.; Nilson, P. M.; Ivancic, S. T.; Mileham, C.; Begishev, I. A.; Junquist, R. K.; Nelson, D. J.; Froula, D. H.

    2016-11-01

    A picosecond, time-resolved, x-ray spectroscopy platform was developed to study the thermal line emission from rapidly heated solid targets containing buried aluminum or iron layers. The targets were driven by high-contrast 1ω or 2ω laser pulses at focused intensities up to 1 × 1019 W/cm2. The experimental platform combines time-integrating and time-resolved x-ray spectrometers. Picosecond time resolution was achieved with a pair of ultrafast x-ray streak cameras coupled to high-throughput Hall spectrometers. Time-integrated spectra were collected on each shot to correct the streaked data for variations in x-ray photocathode spectral sensitivity. The time-integrated spectrometer uses three elliptical crystals to disperse x rays with energies between 800 and 2100 eV with moderate (E/ΔE ˜ 450) resolving power. The streaked spectrometers accept four interchangeable conical crystals with higher resolving power (E/ΔE ˜ 650) to measure the brightest thermal lines in the 1300 to 1700 eV spectral range.

  18. An x-ray absorption spectroscopy study of Mo oxidation in Pb at elevated temperatures

    SciTech Connect

    Liu, Shanshan; Olive, Daniel; Terry, Jeff; Segre, Carlo U.

    2009-06-30

    The corrosion of fuel cladding and structural materials by lead and lead-bismuth eutectic in the liquid state at elevated temperatures is an issue that must be considered when designing advanced nuclear systems and high-power spallation neutron targets. In this work, lead corrosion studies of molybdenum were performed to investigate the interaction layer as a function of temperature by X-ray absorption spectroscopy. In situ X-ray absorption measurements on a Mo substrate with a 3-6 {micro}m layer of Pb deposited by thermal evaporation were performed at temperatures up to 900 C and at a 15{sup o} angle to the incident X-rays. The changes in the local atomic structure of the corrosion layer are visible in the difference extended X-ray absorption fine structure and the linear combination fitting of the X-ray absorption near-edge structure to as-deposited molybdenum sample and molybdenum oxide (MoO{sub 2} and MoO{sub 3}) standards. The data are consistent with the appearance of MoO{sub 3} in an intermediate temperature range (650-800 C) and the more stable MoO{sub 2} phase dominating at high and low temperatures.

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

    NASA Astrophysics Data System (ADS)

    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 (< 5 Torr). The delay time dependence of the gas x-ray diffraction pattern is measured in a pump-probe scheme with 267 nm excitation laser and 8.3 keV X-ray probe pulses. Optical excitation prepares 1,3-cyclohexadiene on the excited 1B surface, from where it accelerates past a conical intersection down the 2A potential energy surfaces before opening the ring structure on a 140 fs time scale. A ``molecular 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.

  20. Low temperature single crystal X-ray diffraction: advantages, instrumentation and applications.

    PubMed

    Goeta, A E; Howard, J A K

    2004-10-20

    The benefits of carrying out single crystal X-ray diffraction (SXRD) experiments at low temperatures have long been recognised by the scientific community, as clearly demonstrated by the massive increase in publications reporting the use of low temperature SXRD in the past 15 years. This tutorial review will summarise the advantages, many of them now often forgotten by its practitioners or never known by the newcomers to the field, of performing single crystal X-ray diffraction experiments at low temperatures. The instrumentation currently available to university laboratories, which has been greatly improved over the past 5 years, will also be briefly described and a few different examples covering a range of applications will be presented.

  1. Quantification of total element concentrations in soils using total X-ray fluorescence spectroscopy (TXRF).

    PubMed

    Towett, Erick K; Shepherd, Keith D; Cadisch, Georg

    2013-10-01

    Total X-ray fluorescence spectroscopy (TXRF) determines concentrations of major and trace elements in multiple media. We developed and tested a method for the use of TXRF for direct quantification of total element concentrations in soils using an S2 PICOFOX™ spectrometer (Bruker AXS Microanalysis GmbH, Germany). We selected 15 contrasting soil samples from across sub-Saharan Africa for element analysis to calibrate the instrument against concentrations determined using the inductively coupled plasma-mass spectroscopy (ICP-MS) standard method. A consistent underestimation of element concentrations using TXRF compared to ICP-MS reference analysis occurred, indicating that spectrometer recalibration was required. Single-element recalibration improved the TXRF spectrometer's sensitivity curve. Subsequent analysis revealed that TXRF determined total element concentrations of Al, K, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, and Ga accurately (model efficacy/slope close to 1:1 line, and R(2)>0.80) over a wide range of soil samples. Other elements that could be estimated with an acceptable precision (R(2)>0.60) compared with ICP-MS although generally somewhat under- or overestimated were P, Ca, As, Rb, Sr, Y, Pr, Ta and Pb. Even after recalibration, compared to ICP-MS the TXRF spectrometer produced underestimations for elements Na, Mg, Ba, Ce, Hf, La, Nd, W and Sm and overestimations for elements Bi, Tl and Zr. We validated the degree of accuracy of the TXRF analytical method after recalibration using an independent set of 20 soil samples. We also tested the accuracy of the analysis using 2 multi-element standards as well as the method repeatability on replicate samples. The resulting total element concentration repeatability for all elements analyzed were within 10% coefficient of variability after the instrument recalibration except for Cd and Tl. Our findings demonstrate that TXRF could be used as a rapid screening tool for total element concentrations in soils assuming that

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

    PubMed

    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.

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

    PubMed

    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. PMID:25537606

  4. Surface relaxation in liquid water and methanol studied by x-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Wilson, Kevin R.; Schaller, R. D.; Co, D. T.; Saykally, R. J.; Rude, Bruce S.; Catalano, T.; Bozek, J. D.

    2002-10-01

    X-ray absorption spectroscopy is a powerful probe of local electronic structure in disordered media. By employing extended x-ray absorption fine structure spectroscopy of liquid microjets, the intermolecular O-O distance has been observed to undergo a 5.9% expansion at the liquid water interface, in contrast to liquid methanol for which there is a 4.6% surface contraction. Despite the similar properties of liquid water and methanol (e.g., abnormal heats of vaporization, boiling points, dipole moments, etc.), this result implies dramatic differences in the surface hydrogen bond structure, which is evidenced by the difference in surface tension of these liquids. This result is consistent with surface vibrational spectroscopy, which indicates both stronger hydrogen bonding and polar ordering at the methanol surface as a consequence of "hydrophobic packing" of the methyl group.

  5. Soft x-ray spectroscopy studies of novel electronic materials using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Newby, David, Jr.

    Soft x-ray spectroscopy can provide a wealth of information on the electronic structure of solids. In this work, a suite of soft x-ray spectroscopies is applied to organic and inorganic materials with potential applications in electronic and energy generation devices. Using the techniques of x-ray absorption (XAS), x-ray emission spectroscopy (XES), and x-ray photoemission spectroscopy (XPS), the fundamental properties of these different materials are explored. Cycloparaphenylenes (CPPs) are a recently synthesized family of cyclic hydrocarbons with very interesting properties and many potential applications. Unusual UV/Visible fluorescence trends have spurred a number of theoretical investigations into the electronic properties of the CPP family, but thus far no comprehensive electronic structure measurements have been conducted. XPS, XAS, and XES data for two varieties, [8]- and [10]-CPP, are presented here, and compared with the results of relevant DFT calculations. Turning towards more application-centered investigations, similar measurements are applied to two materials commonly used in solid oxide fuel cell (SOFC) cathodes: La1-xSrxMnO 3 (LSMO) and La1-xSr1- xCo1-yFe yO3 (LSCF). Both materials are structurally perovskites, but they exhibit strikingly different electronic properties. SOFC systems very efficiently produce electricity by catalyzing reactions between oxygen and petroleum-based hydrocarbons at high temperatures (> 800 C). Such systems are already utilized to great effect in many industries, but more widespread adoption could be had if the cells could operate at lower temperatures. Understanding the electronic structure and operational evolution of the cathode materials is essential for the development of better low-temperature fuel cells. LSCF is a mixed ion-electron conductor which holds promise for low-temperature SOFC applications. XPS spectra of LSCF thin films are collected as the films are heated and gas-dosed in a controlled environment. The

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

    NASA Astrophysics Data System (ADS)

    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

  7. X-Ray Diffraction and Fluorescence Measurements for In Situ Planetary Instruments

    NASA Astrophysics Data System (ADS)

    Hansford, G.; Hill, K. S.; Talboys, D.; Vernon, D.; Ambrosi, R.; Bridges, J.; Hutchinson, I.; Marinangeli, L.

    2011-12-01

    The ESA/NASA ExoMars mission, due for launch in 2018, has a combined X-ray fluorescence/diffraction instrument, Mars-XRD, as part of the onboard analytical laboratory. The results of some XRF (X-ray fluorescence) and XRD (X-ray diffraction) tests using a laboratory chamber with representative performance are reported. A range of standard geological reference materials and analogues were used in these tests. The XRD instruments are core components of the forthcoming NASA Mars Science Laboratory (MSL) and ESA/NASA ExoMars missions and will provide the first demonstrations of the capabilities of combined XRD/XRF instrumentation in situ on an extraterrestrial planetary surface. The University of Leicester team is part of the Italy-UK collaboration that is responsible for building the ExoMars X-ray diffraction instrument, Mars-XRD [1,2]. Mars-XRD incorporates an Fe-55 radioisotope source and three fixed-position charge-coupled devices (CCDs) to simultaneously acquire an X-ray fluorescence spectrum and a diffraction pattern providing a measurement of both elemental and mineralogical composition. The CCDs cover an angular range of 2θ = 6° to 73° enabling the analysis of a wide range of geologically important minerals including phyllosilicates, feldspars, oxides, carbonates and evaporites. The identification of hydrous minerals may help identify past Martian hydrothermal systems capable of preserving traces of life. Here we present some initial findings from XRF and XRD tests carried out at the University of Leicester using an Fe-55 source and X-ray sensitive CCD. The XRF/XRD test system consists of a single CCD on a motorised arm, an Fe-55 X-ray source, a collimator and a sample table which approximately replicate the reflection geometry of the Mars-XRD instrument. It was used to test geological reference standard materials and Martian analogues. This work was funded by the Science and Technology Facilities Council, UK. References [1] Marinangeli, L., Hutchinson, I

  8. Diagnostics of the accretion plasma in magnetic CVs from high-resolution X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Burwitz, V.; Reinsch, K.; Haberl, F.; Gänsicke, B. T.; Predehl, P.

    2002-01-01

    High-resolution X-ray spectroscopy with the Chandra low energy transmission grating spectrometer (LETGS) provides an unprecedented diagnostic tool for the hot accretion plasma and the settling flow in the accretion column of magnetic cataclysmic variables (mCVs). We show first results from our analysis of spin-phase resolved X-ray spectroscopy of the two prototype magnetic CVs, AM Her and PQ Gem. The LETGS spectra cover the wavelength range 2--170Å with a spectral resolution λ/Δ λ = 200--3000. For the first time, absorption structures in the soft X-ray component of the heated white-dwarf atmosphere are revealed and individual emission lines of H- and He-like O and N ions including the density sensitive components of the He-like triplets are resolved in the hard X-ray component originating from the settling flow. In addition, phase dependent Doppler-shifts of the emission lines are detected providing detailed information on the geometry of the accretion funnel.

  9. Excited state X-ray absorption spectroscopy: Probing both electronic and structural dynamics

    NASA Astrophysics Data System (ADS)

    Neville, Simon P.; Averbukh, Vitali; Ruberti, Marco; Yun, Renjie; Patchkovskii, Serguei; Chergui, Majed; Stolow, Albert; Schuurman, Michael S.

    2016-10-01

    We investigate the sensitivity of X-ray absorption spectra, simulated using a general method, to properties of molecular excited states. Recently, Averbukh and co-workers [M. Ruberti et al., J. Chem. Phys. 140, 184107 (2014)] introduced an efficient and accurate L 2 method for the calculation of excited state valence photoionization cross-sections based on the application of Stieltjes imaging to the Lanczos pseudo-spectrum of the algebraic diagrammatic construction (ADC) representation of the electronic Hamiltonian. In this paper, we report an extension of this method to the calculation of excited state core photoionization cross-sections. We demonstrate that, at the ADC(2)x level of theory, ground state X-ray absorption spectra may be accurately reproduced, validating the method. Significantly, the calculated X-ray absorption spectra of the excited states are found to be sensitive to both geometric distortions (structural dynamics) and the electronic character (electronic dynamics) of the initial state, suggesting that core excitation spectroscopies will be useful probes of excited state non-adiabatic dynamics. We anticipate that the method presented here can be combined with ab initio molecular dynamics calculations to simulate the time-resolved X-ray spectroscopy of excited state molecular wavepacket dynamics.

  10. X-ray structure analysis of a metalloprotein with enhanced active-site resolution using in situ x-ray absorption near edge structure spectroscopy.

    PubMed

    Arcovito, Alessandro; Benfatto, Maurizio; Cianci, Michele; Hasnain, S Samar; Nienhaus, Karin; Nienhaus, G Ulrich; Savino, Carmelinda; Strange, Richard W; Vallone, Beatrice; Della Longa, Stefano

    2007-04-10

    X-ray absorption spectroscopy is exquisitely sensitive to the coordination geometry of an absorbing atom and therefore allows bond distances and angles of the surrounding atomic cluster to be measured with atomic resolution. By contrast, the accuracy and resolution of metalloprotein active sites obtainable from x-ray crystallography are often insufficient to analyze the electronic properties of the metals that are essential for their biological functions. Here, we demonstrate that the combination of both methods on the same metalloprotein single crystal yields a structural model of the protein with exceptional active-site resolution. To this end, we have collected an x-ray diffraction data set to 1.4-A resolution and Fe K-edge polarized x-ray absorption near edge structure (XANES) spectra on the same cyanomet sperm whale myoglobin crystal. The XANES spectra were quantitatively analyzed by using a method based on the multiple scattering approach, which yielded Fe-heme structural parameters with +/-(0.02-0.07)-A accuracy on the atomic distances and +/-7 degrees on the Fe-CN angle. These XANES-derived parameters were subsequently used as restraints in the crystal structure refinement. By combining XANES and x-ray diffraction, we have obtained an cyanomet sperm whale myoglobin structural model with a higher precision of the bond lengths and angles at the active site than would have been possible with crystallographic analysis alone.

  11. Cosmic X-ray Physics: Sounding rocket investigations of the diffuse X-ray background, including instrument development

    NASA Astrophysics Data System (ADS)

    McCammon, Dan

    We propose an investigation to improve our understanding of the Galactic diffuse X-ray background. The ultimate purpose of this is to determine the role of hot phases of the interstellar medium in mediating stellar feedback in star formation, in transport of metals, and in determining the structure and evolution of the Galaxy. It directly addresses SMD's astrophysics goal No. 2, to explore the origin and evolution of the galaxies, stars and planets that make up our universe. This work will involve a flight of an existing payload with small modifications in Woomera, South Australia, to observe the Galactic soft X-ray bulge and attempt to determine its nature and emission mechanisms. This flight should also either confirm or put strict upper limits on the "sterile neutrino" model for the 3.5 keV signal observed near the Galactic Center by XMM-Newton. Our investigation includes the development of thermal detectors with superconducting transition edge thermometers capable of 1-2 eV FWHM energy resolution in the 100-400 eV range with the intent of obtaining a scientifically useful spectrum on a sounding rocket flight of the emission from one million degree gas in this energy range. This will require a total area of 1-2 square centimeters for the detector array. To enable routine testing of such detectors in the lab and for necessary in-flight gain and resolution monitoring, we are trying to develop a pulsed-UV laser calibration source. In collaboration with Goddard Space Flight Center, we are investigating the practicality of waveguide-below-cutoff filters to provide the necessary attenuation of infrared radiation for these detectors while still allowing good x-ray transmission below 150 eV. The detectors, calibration source, filters, optimal high-rate pulse analysis and flight experience with the detector readouts are all relevant to future NASA major missions. The detectors we're working on for a low-energy sounding rocket flight would be an excellent match to what is

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

    SciTech Connect

    Wang, Xin

    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.

  13. On Relativistic Disk Spectroscopy in Compact Objects with X-ray CCD Cameras

    NASA Astrophysics Data System (ADS)

    Miller, J. M.; D'Aì, A.; Bautz, M. W.; Bhattacharyya, S.; Burrows, D. N.; Cackett, E. M.; Fabian, A. C.; Freyberg, M. J.; Haberl, F.; Kennea, J.; Nowak, M. A.; Reis, R. C.; Strohmayer, T. E.; Tsujimoto, M.

    2010-12-01

    X-ray charge-coupled devices (CCDs) are the workhorse detectors of modern X-ray astronomy. Typically covering the 0.3-10.0 keV energy range, CCDs are able to detect photoelectric absorption edges and K shell lines from most abundant metals. New CCDs also offer resolutions of 30-50 (E/ΔE), which is sufficient to detect lines in hot plasmas and to resolve many lines shaped by dynamical processes in accretion flows. The spectral capabilities of X-ray CCDs have been particularly important in detecting relativistic emission lines from the inner disks around accreting neutron stars and black holes. One drawback of X-ray CCDs is that spectra can be distorted by photon "pile-up," wherein two or more photons may be registered as a single event during one frame time. We have conducted a large number of simulations using a statistical model of photon pile-up to assess its impacts on relativistic disk line and continuum spectra from stellar-mass black holes and neutron stars. The simulations cover the range of current X-ray CCD spectrometers and operational modes typically used to observe neutron stars and black holes in X-ray binaries. Our results suggest that severe photon pile-up acts to falsely narrow emission lines, leading to falsely large disk radii and falsely low spin values. In contrast, our simulations suggest that disk continua affected by severe pile-up are measured to have falsely low flux values, leading to falsely small radii and falsely high spin values. The results of these simulations and existing data appear to suggest that relativistic disk spectroscopy is generally robust against pile-up when this effect is modest.

  14. Set of instruments for solar EUV and soft X-ray monitoring onboard satellite Coronas-Photon

    NASA Astrophysics Data System (ADS)

    Kotov, Yury; Kochemasov, Alexey; Kuzin, Sergey; Kuznetsov, Vladimir; Sylwester, Janusz; Yurov, Vitaly

    Coronas-Photon mission is the third satellite of the Russian Coronas program on solar activity observation. The main goal of the "Coronas-Photon" is the study of solar hard electromagnetic radiation in the wide energy range from UV up to high energy gamma-radiation (2000MeV). Scientific payload for solar radiation observation consists of three types of instruments: Monitors (Natalya-2M, Konus-RF, RT-2, Penguin-M, BRM, PHOKA, Sphin-X, SOKOL spectral and timing measurements of full solar disk radiation have timing in flare/burst mode up to one msec. Instruments Natalya-2M, Konus-RF, RT-2 will cover the wide energy range of hard X-rays and soft gamma-rays (15keV to 2000MeV) and will together constitute the largest area detectors ever used for solar observations. Detectors of gamma-ray monitors are based on structured inorganic scintillators. For X-ray and EUV monitors the scintillation phoswich detectors, gas proportional counter, CdZnTe assembly and filter-covered Si-diodes are used. Telescope-spectrometer TESIS for imaging solar spectroscopy in X-rays has angular resolution up to 1arcsec in three spectral lines. Satellite platform and scientific payload is under construction to be launched in autumn 2008. Satellite orbit is circular with initial height 550km and inclination 82.5degrees. Accuracy of the spacecraft orientation to the Sun is better 3arcmin. In the report the capability of PHOKA, SphinX, SOKOL and TESIS as well as the observation program are described and discussed.

  15. Instrumentation for a next-generation x-ray all-sky monitor

    SciTech Connect

    Peele, A. G.

    1999-12-15

    We have proposed an x-ray all-sky monitor for a small satellite mission that will be ten times more sensitive than past monitors and that opens up a new band of the soft x-ray spectrum (0.1-3.0 keV) for study. We discuss three approaches to the construction of the optics. The first method, well within the reach of existing technology, is to approximate the lobster-eye geometry by building crossed arrays of planar reflectors, this gives great control over the reflecting surface but is limited in terms of resolution at the baseline 4 arc minute level. The second method is to use microchannel plates; this technology has the potential to greatly exceed the baseline resolution and sensitivity but is yet to be fully demonstrated. The third method, while still in its infancy, may yet prove to be the most powerful; this approach relies on photolithography to expose a substrate that can then be developed and replicated. The scientific case for this mission is almost too broad to state here. The instrument we describe will allow investigation of the long term light curves of thousands of AGN, it will detect thousands of transients, including GRBs and type II supernova, and the stellar coronae of hundreds of the brightest x-ray stars can be monitored. In addition the classical objectives of all-sky monitors--long-term all-sky archive and watchdog alert to new events--will be fulfilled at an unprecedented level. We also note that by opening up a little-explored band of the x-ray sky the opportunity for new discovery is presented. A satisfying example of entering new territory while still retaining the guarantee of expanding the domain of existing research.

  16. X-ray photo-emission and energy dispersive spectroscopy of HA coated titanium

    SciTech Connect

    Drummond, J.L.; Steinberg, A.D.; Krauss, A.R.

    1997-08-01

    The purpose of this study was to determine the chemical composition changes of hydroxyapatite (HA) coated titanium using surface analysis (x-ray photo-emission) and bulk analysis (energy dispersive spectroscopy). The specimens examined were controls, 30 minutes and 3 hours aged specimens in distilled water or 0.2M sodium phosphate buffer (pH 7.2) at room temperature. Each x-ray photo-emission cycle consisted of 3 scans followed by argon sputtering for 10 minutes for a total of usually 20 cycles, corresponding to a sampling depth of {approximately} 1500 {angstrom}. The energy dispersive spectroscopy analysis was on a 110 by 90 {mu}m area for 500 sec. Scanning electron microscopy examination showed crystal formation (3P{sub 2}O{sub 5}*2CAO*?H{sub 2}O by energy dispersive spectroscopy analysis) on the HA coating for the specimens aged in sodium phosphate buffer. The x-ray photo-emission results indicated the oxidation effect of water on the titanium (as TiO{sub 2}) and the effect of the buffer to increase the surface concentration of phosphorous. No differences in the chemical composition were observed by energy dispersive spectroscopy analysis. The crystal growth was only observed for the sodium phosphate buffer specimens and only on the HA surface.

  17. Redox Chemisty of Tantalum Clusters on Silica Characterized by X-ray Absorption Spectroscopy

    SciTech Connect

    Nemana,S.; Gates, B.

    2006-01-01

    SiO{sub 2}-supported clusters of tantalum were synthesized from adsorbed Ta(CH{sub 2}Ph){sub 5} by treatment in H{sub 2} at 523 K. The surface species were characterized by X-ray absorption spectroscopy (extended X-ray absorption fine structure (EXAFS) spectroscopy and X-ray absorption near edge spectroscopy (XANES)) and ultraviolet-visible spectroscopy. The EXAFS data show that SiOO{sub 2}-supported tantalum clusters were characterized by a Ta-Ta coordination number of approximately 2, consistent with the presence of tritantalum clusters, on average. When these were reduced in H{sub 2} and reoxidized in O{sub 2}, the cluster nuclearity remained essentially unchanged, although reduction and oxidation occurred, respectively, as shown by XANES and UV-vis spectra; in the reoxidation, the tantalum oxidation state change was approximately two electronic charges per tritantalum cluster. The data demonstrate an analogy between the chemistry of group 5 metals on the SiO{sub 2} support and their chemistry in solution, as determined by the group of Cotton.

  18. Structure of the Mn complex in photosystem II: Insights from x-ray spectroscopy

    SciTech Connect

    Yachandra, Vittal K.

    2002-04-02

    We have used Mn K-edge absorption and Kb emission spectroscopies to determine the oxidation states of the Mn complex in the various S-states. We have started exploring the new technique of resonant inelastic X-ray scattering spectroscopy (RIXS); this technique can be characterized as a Raman process that uses K-edge energies (1s to 4p, {approx}6550 eV) to obtain L-edge-like spectra (2p to 3d, {approx}650 eV). The relevance of these data to the oxidation states and structure of the Mn complex is presented. We have obtained EXAFS data from the S0 and S3 states and observed heterogeneity in the Mn-Mn distances, leading us to conclude that there may be three rather than two di-(mu)-oxo bridged units present per tetranuclear Mn cluster. In addition, we have obtained data using Ca/Sr X-ray spectroscopy that provide evidence for a heteronuclear Mn/Ca cluster. The possibility of three di-(mu)-oxo-bridged Mn Mn moieties and the proximity of Ca is incorporated into developing structural models for the Mn cluster. The involvement of bridging and terminal O ligands of Mn in the mechanism of oxygen evolution is discussed in the context of our X-ray spectroscopy results.

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

    SciTech Connect

    Hamad, K.S.

    2000-05-01

    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.

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

    SciTech Connect

    Chong, Henry Herng Wei

    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.

  1. Use of X-ray absorption spectroscopy in the search for the best LIGO mirror coatings

    NASA Astrophysics Data System (ADS)

    McGuire, Stephen C.

    2008-03-01

    The Laser Interferometer Gravitational-wave Observatory (LIGO) seeks to improve its sensitivity for gravity-wave detection by a factor of ten during its next phase of operation, Advanced LIGO. In order to achieve this goal it is necessary to design and fabricate test mass mirrors that help minimize the noise in the interferometers and in doing so maximize gravity-wave detection capability. In this talk we will present recent results from our program of X-ray absorption spectroscopy measurements to obtain detailed chemical composition and structure of titania (TiO2)-doped tantala (Ta2O5) multilayers fabricated via ion beam sputtering on SiO2 substrates. Our investigations focus on how the microscopic features of the coatings influence their macroscopic mechanical loss properties. Our goal is to obtain correlations between chemical impurities and/or dopants and the optical absorption and mechanical loss characteristics of these multilayer coatings. To examine our samples we use synchrotron-based X-ray absorption Spectroscopy (XAS) techniques including Extended X-ray Absorption Fine Structure (EXAFS), X-ray Absorption Near Edge Structure (XANES) and X-ray Fluorescence (XRF). We present chemical and structural data obtained at the titanium K-edge and tantalum LIII-edge as well as relative elemental distribution information (Ti/Ta, Fe/Ta, and Cr/Ta) obtained via XRF. Following a brief description of the LIGO experiment, our program of research in optical materials for use in advanced versions of the interferometer will be described.

  2. X-Ray Spectroscopy of the Photosynthetic Oxygen-Evolving Complex

    SciTech Connect

    Sauer, K.; Yano, J.; Yachandra, V.K.

    2009-05-27

    Water oxidation to dioxygen in photosynthesis is catalyzed by a Mn{sub 4}Ca 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.

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

    SciTech Connect

    Tilikin, I. N. Shelkovenko, T. A.; Pikuz, S. A.; Knapp, P. F.; Hammer, D. A.

    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.

  4. Electrochemical flowcell for in-situ investigations by soft x-ray absorption and emission spectroscopy

    SciTech Connect

    Schwanke, C.; Lange, K. M.; Golnak, R.; Xiao, J.

    2014-10-15

    A new liquid flow-cell designed for electronic structure investigations at the liquid-solid interface by soft X-ray absorption and emission spectroscopy is presented. A thin membrane serves simultaneously as a substrate for the working electrode and solid state samples as well as for separating the liquid from the surrounding vacuum conditions. In combination with counter and reference electrodes this approach allows in-situ studies of electrochemical deposition processes and catalytic reactions at the liquid-solid interface in combination with potentiostatic measurements. As model system in-situ monitoring of the deposition process of Co metal from a 10 mM CoCl{sub 2} aqueous solution by X-ray absorption and emission spectroscopy is presented.

  5. Surface state analysis of wet ground silicon nitride powders by x-ray photoelectron spectroscopy

    SciTech Connect

    Kameshima, Yoshikazu; Yasumori, Atsuo; Okada, Kiyoshi

    1995-09-01

    Three kinds of silicon nitride powders, i.e. as-prepared direct-nitridation powder, HF-treated direct-nitridation powder, and as-prepared imide decomposition powder, were wet ground by ball milling in water and the surface state change due to the grinding was examined by X-ray photoelectron spectroscopy (XPS) and X-ray Auger electron spectroscopy (XAES). The thickness of the oxidized surface layer of the powder was calculated from the peak area ratio and the chemical composition was evaluated from the Auger parameter (AP). Surface oxidized phase amount gradually increased with longer milling time and the thickness increased almost three times after 7 days milling, compared to as those of the unground samples. Chemical composition of the oxidized phase formed by the grinding was pure silica irrespective to the samples, although those of the oxidized phase in the unground samples differed among the samples.

  6. Technology Development for the Constellation-X Spectroscopy X-Ray Telescope

    NASA Technical Reports Server (NTRS)

    Petre, Robert; Lehan, John; O'Dell, Stephen; Owens, Scott; Reid, Paul B.; Saha, Timo; Stewart, Jeff; Jones, William D.; Zhang, William

    2005-01-01

    The Constellation-X Spectroscopy X-ray Telescope (SXT) is a large diameter, high throughput, grazing incidence imaging mirror system, designed to perform high sensitivity spectroscopy of cosmic X-ray sources in the 0.2-10.0 keV band. The baseline effective area requirement is -3 m# at 1 keV. The system-level angular-resolution requirement is a 15-arcseconds half-power diameter, with a 5-arcsecond goal. The effective area is attained through a modular design, involving the nesting of many confocal, thin-walled Wolter I mirror segments. Considerable progress has been made in developing thin, thermally formed, glass mirror substrates that meet or better the angular-resolution requirement. Several approaches to mounting and aligning reflector segments into a mirror system are under investigation. We report here on the progress of the SXT technology development program toward reaching the performance goals.

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

    SciTech Connect

    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.

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

    PubMed Central

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

    2008-01-01

    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. PMID:19190720

  9. A von Hamos x-ray spectrometer based on a segmented-type diffraction crystal for single-shot x-ray emission spectroscopy and time-resolved resonant inelastic x-ray scattering studies

    SciTech Connect

    Szlachetko, J.; Nachtegaal, M.; Boni, E. de; Willimann, M.; Safonova, O.; Sa, J.; Smolentsev, G.; Szlachetko, M.; Bergamaschi, A.; Schmitt, B.; David, C.; Luecke, A.; Bokhoven, J. A. van; Dousse, J.-Cl.; Hoszowska, J.; Kayser, Y.; Jagodzinski, P.

    2012-10-15

    We report on the design and performance of a wavelength-dispersive type spectrometer based on the von Hamos geometry. The spectrometer is equipped with a segmented-type crystal for x-ray diffraction and provides an energy resolution in the order of 0.25 eV and 1 eV over an energy range of 8000 eV-9600 eV. The use of a segmented crystal results in a simple and straightforward crystal preparation that allows to preserve the spectrometer resolution and spectrometer efficiency. Application of the spectrometer for time-resolved resonant inelastic x-ray scattering and single-shot x-ray emission spectroscopy is demonstrated.

  10. A von Hamos x-ray spectrometer based on a segmented-type diffraction crystal for single-shot x-ray emission spectroscopy and time-resolved resonant inelastic x-ray scattering studies.

    PubMed

    Szlachetko, J; Nachtegaal, M; de Boni, E; Willimann, M; Safonova, O; Sa, J; Smolentsev, G; Szlachetko, M; van Bokhoven, J A; Dousse, J-Cl; Hoszowska, J; Kayser, Y; Jagodzinski, P; Bergamaschi, A; Schmitt, B; David, C; Lücke, A

    2012-10-01

    We report on the design and performance of a wavelength-dispersive type spectrometer based on the von Hamos geometry. The spectrometer is equipped with a segmented-type crystal for x-ray diffraction and provides an energy resolution in the order of 0.25 eV and 1 eV over an energy range of 8000 eV-9600 eV. The use of a segmented crystal results in a simple and straightforward crystal preparation that allows to preserve the spectrometer resolution and spectrometer efficiency. Application of the spectrometer for time-resolved resonant inelastic x-ray scattering and single-shot x-ray emission spectroscopy is demonstrated.

  11. In Situ identification of mineral resources with an X-ray-optical "Hand-Lens" instrument

    NASA Technical Reports Server (NTRS)

    Marshall, J.; Koppel, L.; Bratton, C.; Metzger, E.; Hecht, M.

    1997-01-01

    The recognition of material resources on a planetary surface requires exploration strategies not dissimilar to those employed by early field geologists who searched for ore deposits primarily from surface clues. In order to determine the location of mineral ores or other materials, it will be necessary to characterize host terranes at regional or subregional scales. This requires geographically broad surveys in which statistically significant numbers of samples are rapidly scanned from a roving platform. To enable broad-scale, yet power-conservative planetary-surface exploration, we are developing an instrument that combines x-ray diffractometry (XRD), x-ray fluorescence spectrometry (XRF), and optical capabilities; the instrument can be deployed at the end of a rover's robotic arm, without the need for sample capture or preparation. The instrument provides XRD data for identification of mineral species and lithological types; diffractometry of minerals is conducted by ascertaining the characteristic lattice parameters or "d-spacings" of mineral compounds. D-spacings of 1.4 to 25 angstroms can be determined to include the large molecular structures of hydrated minerals such as clays. The XRF data will identify elements ranging from carbon (Atomic Number = 6) to elements as heavy as barium (Atomic Number = 56).

  12. Benchtop Nonresonant X-ray Emission Spectroscopy: Coming Soon to Laboratories and XAS Beamlines Near You?

    NASA Astrophysics Data System (ADS)

    Mortensen, Devon R.; Seidler, Gerald T.; Ditter, Alexander S.; Glatzel, Pieter

    2016-05-01

    Recently developed instrumentation at the University of Washington has allowed for nonresonant x-ray emission spectra (XES) to be measured in a laboratory-setting with an inexpensive, easily operated system. We present a critical evaluation of this equipment by means of Kβ and valence-level XES measurements for several Co compounds. We find peak count rates of ∼5000/s for concentrated samples and a robust relative energy scale with reproducibility of 25 meV or better. We furthermore find excellent agreement with synchrotron measurements with only modest loss in energy resolution. Instruments such as ours, based on only conventional sources that are widely sold for elemental analysis by x-ray fluorescence, can fill an important role to diversify the research applications of XES both by their presence in non-synchrotron laboratories and by their use in conjunction with XAFS beamlines where the complementarity of XAFS and XES holds high scientific potential.

  13. Coherent X-ray and laser spectroscopy measurements of diffusion in concentrated alpha-crystallin solutions

    NASA Astrophysics Data System (ADS)

    Karunaratne, V. N. C.

    The mammalian eye lens is composed of a concentrated solution of water soluble proteins called crystallins. Alpha-crystallin, the most abundant protein found in the lens, plays a crucial role in maintaining lens transparency and lens accommodation. However, alpha-crystallins along with other ocular proteins suffer from irreversible processes such as oxidation. One cause of oxidation is radiation-induced radical formation which alters the inter-molecular interactions, thereby degrading the normal function of ocular proteins. The main goal of this thesis is to quantify molecular scale dynamics of concentrated solutions of alpha-crystallins using coherent X-rays and visible laser light. I believe a detailed analysis of the dynamics pertaining to alpha-crystallin will provide the foundation to understand molecular scale mechanisms that lead to conditions like cataract and presbyopia. I explore the dynamics of concentrated alpha-crystallin solutions by measuring diffusive motion over a range of length scales using Dynamic light scattering (DLS) and X-ray photon correlation spectroscopy (XPCS). To a certain extent, the dynamical properties of crystallins obtained in this manner are consistent with established theories in colloidal physics. However, there are some deviations, which I will address in this thesis. In terms of X-ray data, I employed a new, efficient photon correlation technique to obtain the best possible signal, furthermore this technique is embedded in a stand-alone software program that has the ability to provide real time results, quickly and efficiently with the help of high performance computing resources available at Northern Illinois University (NIU). The technique has potential to be used by the coherent X-ray spectroscopy community in the future. In addition, by using X-ray scattering data, I probe potential modifications and or damage effects on alpha-crystallins due to radiation exposure. The damage analysis methodology described in this thesis

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

    SciTech Connect

    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.

  15. X-ray photoelectron spectroscopy of γ-ray-irradiated single-stranded DNA

    NASA Astrophysics Data System (ADS)

    Lee, Eunmo; Hong, W.; Han, J. H.; Choi, D. M.; Lee, Cheol Eui; Kim, H. D.; Kim, J.

    2015-07-01

    The effects of γ-ray irradiation on herring sperm single-stranded DNA have been studied by using X-ray photoelectron spectroscopy (XPS) in the view of the bonding configurations and the structural modifications. The significant changes in the hydrogen, carbon, nitrogen, and phosphorous bonding energies, as revealed by the XPS analysis, indicate that electron transfers result in the creation of radicals and in DNA strand breaks.

  16. X-ray absorption spectroscopy beyond the core-hole lifetime

    SciTech Connect

    Haemaelaeinen, K.; Hastings, J.B.; Siddons, D.P.; Berman, L.

    1992-10-01

    A new technique to overcome the core-hole lifetime broadening in x-ray absorption spectroscopy is presented. It utilizes a high resolution fluorescence spectrometer which can be used to analyze the fluorescence photon energy with better resolution than the natural lifetime width. Furthermore, the high resolution spectrometer can also be used to select the final state in the fluorescence process which can offer spin selectivity even without long range magnetic order in the sample.

  17. X-ray absorption spectroscopy beyond the core-hole lifetime

    SciTech Connect

    Haemaelaeinen, K.; Hastings, J.B.; Siddons, D.P.; Berman, L.

    1992-01-01

    A new technique to overcome the core-hole lifetime broadening in x-ray absorption spectroscopy is presented. It utilizes a high resolution fluorescence spectrometer which can be used to analyze the fluorescence photon energy with better resolution than the natural lifetime width. Furthermore, the high resolution spectrometer can also be used to select the final state in the fluorescence process which can offer spin selectivity even without long range magnetic order in the sample.

  18. Slow dynamics and aging in colloidal gels studied by x-ray photon correlation spectroscopy

    SciTech Connect

    Fluerasu, Andrei; Moussaied, Abdellatif; Madsen, Anders; Schofield, Andrew

    2007-07-15

    Slow, nonequilibrium dynamics during delayed sedimentation in a colloidal depletion gel was studied by x-ray photon correlation spectroscopy. The intermediate scattering functions change during the process from stretched to compressed exponential decays, indicating a jamming transition toward full aging. A complex aging behavior follows this process; it is proposed that large-scale network deformations trigger an unjamming, leading to the final collapse of the gel.

  19. Development of Thin-Window Silicon Drift Detector for X-ray Spectroscopy

    SciTech Connect

    Chen, W.; Carini, G.A.; De Geronimo, G.; Fried, J.; Gaskin, J.A.; Keister, J.W.; Li, Z.; Ramsey, B.D.; Rehak, P.; Siddons, D.P.

    2009-10-01

    A new set of thin-window silicon drift detectors composed of an array of hexagonal shaped detectors has been designed, constructed and tested for X-ray spectroscopy. Each individual ThinWinSDD has a thin entrance window on one side and a spiral shaped hexagonal cathode around a center anode on the other side. To produce the thin entrance window a 10 keV implantation of boron through a 500 A silicon dioxide was used. The implantation was followed by an annealing at 700 C for 30 min and a reactive ion etching step to ensure the removal of silicon dioxide from the smallest feature (5 mum). An aluminum layer is coated in the same vacuum system after back-sputtering. This step involves removing the native oxide that has formed on the top of the silicon substrate and then sputtering a 1100 A thick layer of aluminum onto the X-ray entrance window. The aluminum layer must be thick enough to block visible light, but thin enough to be transparent to soft X-rays down to 280 eV. We discuss first test results that include detector leakage current measurements and the response for multiple detectors exposed to the National Synchrotron Light Source's UV beam line U3C located at Brookhaven National Laboratory for X-ray energies as low as 280 eV.

  20. High-Resolution X-ray Spectroscopy of Colliding Wind Binaries

    NASA Astrophysics Data System (ADS)

    Henely, David B.

    2005-02-01

    Massive stars have powerful winds which have profound effects on their surroundings and the stars' own evolution. Most such stars reside in binaries, in which the two stars' winds collide highly supersonically. The winds are shock-heated and produce copious X-rays, the study of which can be used to address poorly understood aspects of massive star winds. In this thesis, high-resolution X-ray spectroscopy is used to study in detail the structure of wind-wind collisions. We develop a model for synthesizing X-ray emission line profiles from colliding wind binaries. We then present analyses of X-ray spectra of two colliding wind systems: gamma(2) Velorum and eta Carinae, part of which includes applying the line synthesis model to these systems. The application of the model to a third system (WR 140) is also discussed. In general, the high-resolution spectra reveal that the physics in these systems is more complicated than is usually assumed. Given this, we go on to discuss how the future development of this work can be used to further the study of the physics of massive star winds and strong collisionless shocks.

  1. The First X-Ray Imaging Spectroscopy of Quiescent Solar Active Regions with NuSTAR

    NASA Astrophysics Data System (ADS)

    Hannah, Iain G.; Grefenstette, Brian W.; Smith, David M.; Glesener, Lindsay; Krucker, Säm; Hudson, Hugh S.; Madsen, Kristin K.; Marsh, Andrew; White, Stephen M.; Caspi, Amir; Shih, Albert Y.; Harrison, Fiona A.; Stern, Daniel; Boggs, Steven E.; Christensen, Finn E.; Craig, William W.; Hailey, Charles J.; Zhang, William W.

    2016-03-01

    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 ˜ {10}46 cm-3 and ˜ {10}43 cm-3, respectively, at least an order of magnitude stricter than previous limits. With longer duration observations and a weakening solar cycle (resulting in an increased livetime), future NuSTAR observations will have sensitivity to a wider range of temperatures as well as possible non-thermal emission.

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

    SciTech Connect

    Bernadotte, Stephan; Atkins, Andrew J.; Jacob, Christoph R.

    2012-11-28

    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 length scale of the transition. For the short wavelengths used in hard X-ray spectroscopy, the dipole approximation may not be adequate. In particular, for metal K-edge X-ray absorption spectroscopy (XAS), 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-octupole and of the electric-dipole and magnetic-quadrupole transition moments, respectively. We have implemented such an origin-independent calculation of quadrupole intensities in XAS within time-dependent density-functional theory, and demonstrate its usefulness for the calculation of metal and ligand K-edge XAS spectra of transition metal complexes.

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

    PubMed

    Bernadotte, Stephan; Atkins, Andrew J; Jacob, Christoph R

    2012-11-28

    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 length scale of the transition. For the short wavelengths used in hard X-ray spectroscopy, the dipole approximation may not be adequate. In particular, for metal K-edge X-ray absorption spectroscopy (XAS), 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-octupole and of the electric-dipole and magnetic-quadrupole transition moments, respectively. We have implemented such an origin-independent calculation of quadrupole intensities in XAS within time-dependent density-functional theory, and demonstrate its usefulness for the calculation of metal and ligand K-edge XAS spectra of transition metal complexes.

  4. Comparing Compositions of Modern Cast Bronze Sculptures: Optical Emission Spectroscopy Versus x-Ray Fluorescence Spectroscopy

    NASA Astrophysics Data System (ADS)

    Young, M. L.; Dunand, D. C.

    2015-07-01

    Bulk elemental compositions of 74 modern cast bronze sculptures from the collection at the Art Institute of Chicago, the Philadelphia Museum of Art, and the Rodin Museum (Philadelphia, PA) were determined using inductively coupled plasma-optical emission spectroscopy (ICP-OES) and a handheld x-ray fluorescence (XRF) spectrometer. The elemental compositions of the cast sculptures as measured previously by ICP-OES and presently by XRF are compared: A good match is found between the two methods for the base metal (Cu) and the two majority alloying elements (Zn and Sn). For both ICP-OES and XRF data, when the Zn composition is plotted versus the Sn composition, three discernable clusters are found that are related to the artist, foundry, casting date, and casting method; they consist of (A) high-zinc brass, (B) low-zinc, low-tin brass, and (C) low-zinc, tin bronze. Thus, our study confirms that the relatively fast, nondestructive XRF spectrometry can be used effectively over slower and invasive, but more accurate, ICP-OES to help determine a sculpture's artist, foundry, date of creation, date of casting, and casting method.

  5. Thermal design and performance of the REgolith x-ray imaging spectrometer (REXIS) instrument

    NASA Astrophysics Data System (ADS)

    Stout, Kevin D.; Masterson, Rebecca A.

    2014-08-01

    The REgolith X-ray Imaging Spectrometer (REXIS) instrument is a student collaboration instrument on the OSIRIS-REx asteroid sample return mission scheduled for launch in September 2016. The REXIS science mission is to characterize the elemental abundances of the asteroid Bennu on a global scale and to search for regions of enhanced elemental abundance. The thermal design of the REXIS instrument is challenging due to both the science requirements and the thermal environment in which it will operate. The REXIS instrument consists of two assemblies: the spectrometer and the solar X-ray monitor (SXM). The spectrometer houses a 2x2 array of back illuminated CCDs that are protected from the radiation environment by a one-time deployable cover and a collimator assembly with coded aperture mask. Cooling the CCDs during operation is the driving thermal design challenge on the spectrometer. The CCDs operate in the vicinity of the electronics box, but a 130 °C thermal gradient is required between the two components to cool the CCDs to -60 °C in order to reduce noise and obtain science data. This large thermal gradient is achieved passively through the use of a copper thermal strap, a large radiator facing deep space, and a two-stage thermal isolation layer between the electronics box and the DAM. The SXM is mechanically mounted to the sun-facing side of the spacecraft separately from the spectrometer and characterizes the highly variable solar X-ray spectrum to properly interpret the data from the asteroid. The driving thermal design challenge on the SXM is cooling the silicon drift detector (SDD) to below -30 °C when operating. A two-stage thermoelectric cooler (TEC) is located directly beneath the detector to provide active cooling, and spacecraft MLI blankets cover all of the SXM except the detector aperture to radiatively decouple the SXM from the flight thermal environment. This paper describes the REXIS thermal system requirements, thermal design, and analyses, with

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

    SciTech Connect

    Perera, R.C.C.; Jones, G.; Lindle, D.W.

    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.

  7. A X-Ray Absorption Spectroscopy Study of Manganese Containing Compounds and Photosynthetic Spinach Chloroplasts.

    NASA Astrophysics Data System (ADS)

    Kirby, Jon Allan

    The manganese sites in chloroplasts, long thought to be involved in photosynthetic oxygen evolution have been examined and partially characterized by X-ray Absorption Spectroscopy (XAS) using synchrotron radiation. The local environment about the manganese atoms is estimated from an analysis of the extended X-ray Absorption Fine Structure (EXAFS). Comparisons with and simulations of the manganese EXAFS for several reference compounds leads to a model in which the chloroplast manganese atoms are contained in a binuclear complex similar to di-u-oxo -tetrakis-(2,2'-bipyridine) dimanganese. It is suggested that the partner metal is another manganese. The bridging ligands are most probably oxygen. The remaining manganese ligands are carbon, oxygen, or nitrogen. A roughly linear correlation between the X-ray K edge onset energy and the "coordination charge" of a large number of manganese coordination complexes and compounds has been developed. Entry of the chloroplast manganese edge energy onto this correlation diagram establishes that the active pool of manganese is in an oxidation state greater than +2. If the manganese is in a dimeric form the oxidation states are most probably (II,III). Underlying these results is an extensive data analysis methodology. The method developed involves the use of many different background removal techniques, Fourier transforms and ultimately curve fitting to the modulations in the x-ray absorption cross sections. A large number of model compounds were used to evaluate the analysis method. These analyses are used to show that the two major curve fitting models available are essentially equivalent. Due to its greater versatility, the theoretical model of Teo and Lee is preferred (J. Am. Chem. Soc. (1979), 101, 2815). The results are also used to determine the informational limitations of XAS within the limits of the present understanding of X-ray absorption phenomena by inner shell electrons for atoms with atomic number greater than that

  8. Characterization and Evolution of the Swift X-ray Telescope Instrumental Background

    NASA Technical Reports Server (NTRS)

    Hill, Joanne; Pagani, C.; Morris, D. C.; Racusin, J.; Grupe, D.; Vetere, L.; Stroh, M.; Falcone, A.; Kennea, J.; Burrows, D. N.; Nousek, J. A.; Abbey, A. F.; Angelini, L.; Beardmore, A. P.; Campana, S.; Capalbi, M.; Chincarini, G.; Citterio O.; Cusumano, G.; Giommi, P.; Godet, O.; Hill, J. E.; LaParola, V.; Mangano, V.; Mineo, T.

    2007-01-01

    The X-ray telescope (XRT) on board the Swift Gamma Ray Burst Explorer has successfully operated since the spacecraft launch on 20 November 2004, automatically locating GRB afterglows, measuring their spectra and lightcurves and performing observations of high-energy sources. In this work we investigate the properties of the instrumental background, focusing on its dynamic behavior on both long and short timescales. The operational temperature of the CCD is the main factor that influences the XRT background level. After the failure of the Swift active on-board temperature control system, the XRT detector now operates at a temperature range between -75C and -45C thanks to a passive cooling Heat Rejection System. We report on the long-term effects on the background caused by radiation, consisting mainly of proton irradiation in Swift's low Earth orbit and on the short-term effects of transits through the South Atlantic Anomaly (SAA), which expose the detector to periods of intense proton flux. We have determined the fraction of the detector background that is due to the internal, instrumental background and the part that is due to unresolved astrophysical sources (the cosmic X-ray background) by investigating the degree of vignetting of the measured background and comparing it to the expected value from calibration data.

  9. Laboratory Scale X-ray Fluorescence Tomography: Instrument Characterization and Application in Earth and Environmental Science.

    PubMed

    Laforce, Brecht; Vermeulen, Bram; Garrevoet, Jan; Vekemans, Bart; Van Hoorebeke, Luc; Janssen, Colin; Vincze, Laszlo

    2016-03-15

    A new laboratory scale X-ray fluorescence (XRF) imaging instrument, based on an X-ray microfocus tube equipped with a monocapillary optic, has been developed to perform XRF computed tomography experiments with both higher spatial resolution (20 μm) and a better energy resolution (130 eV @Mn-K(α)) than has been achieved up-to-now. This instrument opens a new range of possible applications for XRF-CT. Next to the analytical characterization of the setup by using well-defined model/reference samples, demonstrating its capabilities for tomographic imaging, the XRF-CT microprobe has been used to image the interior of an ecotoxicological model organism, Americamysis bahia. This had been exposed to elevated metal (Cu and Ni) concentrations. The technique allowed the visualization of the accumulation sites of copper, clearly indicating the affected organs, i.e. either the gastric system or the hepatopancreas. As another illustrative application, the scanner has been employed to investigate goethite spherules from the Cretaceous-Paleogene boundary, revealing the internal elemental distribution of these valuable distal ejecta layer particles. PMID:26891032

  10. Laboratory Scale X-ray Fluorescence Tomography: Instrument Characterization and Application in Earth and Environmental Science.

    PubMed

    Laforce, Brecht; Vermeulen, Bram; Garrevoet, Jan; Vekemans, Bart; Van Hoorebeke, Luc; Janssen, Colin; Vincze, Laszlo

    2016-03-15

    A new laboratory scale X-ray fluorescence (XRF) imaging instrument, based on an X-ray microfocus tube equipped with a monocapillary optic, has been developed to perform XRF computed tomography experiments with both higher spatial resolution (20 μm) and a better energy resolution (130 eV @Mn-K(α)) than has been achieved up-to-now. This instrument opens a new range of possible applications for XRF-CT. Next to the analytical characterization of the setup by using well-defined model/reference samples, demonstrating its capabilities for tomographic imaging, the XRF-CT microprobe has been used to image the interior of an ecotoxicological model organism, Americamysis bahia. This had been exposed to elevated metal (Cu and Ni) concentrations. The technique allowed the visualization of the accumulation sites of copper, clearly indicating the affected organs, i.e. either the gastric system or the hepatopancreas. As another illustrative application, the scanner has been employed to investigate goethite spherules from the Cretaceous-Paleogene boundary, revealing the internal elemental distribution of these valuable distal ejecta layer particles.

  11. In Situ Identification of Mineral Resources with an X-Ray-Optical "Hands-Lens" Instrument

    NASA Technical Reports Server (NTRS)

    Marshall, J.; Koppel, L.; Bratton, C.; Metzger, E.; Hecht, M.

    1999-01-01

    The recognition of material resources on a planetary surface requires exploration strategies not dissimilar to those employed by early field geologists who searched for ore deposits primarily from surface clues. In order to determine the location of mineral ores or other materials, it will be necessary to characterize host terranes at regional or subregional scales. This requires geographically broad surveys in which statistically significant numbers of samples are rapidly scanned from a roving platform. To enable broad-scale, yet power-conservative planetary-surface exploration, we are developing an instrument that combines x-ray diffractometry (XRD), x-ray fluorescence spectrometry (XRF), and optical capabilities; the instrument can be deployed at the end of a rover's robotic arm, without the need for sample capture or preparation. The instrument provides XRD data for identification of mineral species and lithological types; diffractometry of minerals is conducted by ascertaining the characteristic lattice parameters or "d-spacings" of mineral compounds. D-spacings of 1.4 to 25 angstroms can be determined to include the large molecular structures of hydrated minerals such as clays. The XRF data will identify elements ranging from carbon (Atomic Number = 6) to elements as heavy as barium (Atomic Number = 56). While a sample is being x-rayed, the instrument simultaneously acquires an optical image of the sample surface at magnifications from lx to at least 50x (200x being feasible, depending on the sample surface). We believe that imaging the sample is extremely important as corroborative sample-identification data (the need for this capability having been illustrated by the experience of the Pathfinder rover). Very few geologists would rely on instrument data for sample identification without having seen the sample. Visual inspection provides critical recognition data such as texture, crystallinity, granularity, porosity, vesicularity, color, lustre, opacity, and

  12. In Situ Identification of Mineral Resources with an X-Ray-Optical "Hands-Lens" Instrument

    NASA Astrophysics Data System (ADS)

    Marshall, J.; Koppel, L.; Bratton, C.; Metzger, E.; Hecht, M.

    1999-09-01

    The recognition of material resources on a planetary surface requires exploration strategies not dissimilar to those employed by early field geologists who searched for ore deposits primarily from surface clues. In order to determine the location of mineral ores or other materials, it will be necessary to characterize host terranes at regional or subregional scales. This requires geographically broad surveys in which statistically significant numbers of samples are rapidly scanned from a roving platform. To enable broad-scale, yet power-conservative planetary-surface exploration, we are developing an instrument that combines x-ray diffractometry (XRD), x-ray fluorescence spectrometry (XRF), and optical capabilities; the instrument can be deployed at the end of a rover's robotic arm, without the need for sample capture or preparation. The instrument provides XRD data for identification of mineral species and lithological types; diffractometry of minerals is conducted by ascertaining the characteristic lattice parameters or "d-spacings" of mineral compounds. D-spacings of 1.4 to 25 angstroms can be determined to include the large molecular structures of hydrated minerals such as clays. The XRF data will identify elements ranging from carbon (Atomic Number = 6) to elements as heavy as barium (Atomic Number = 56). While a sample is being x-rayed, the instrument simultaneously acquires an optical image of the sample surface at magnifications from lx to at least 50x (200x being feasible, depending on the sample surface). We believe that imaging the sample is extremely important as corroborative sample-identification data (the need for this capability having been illustrated by the experience of the Pathfinder rover). Very few geologists would rely on instrument data for sample identification without having seen the sample. Visual inspection provides critical recognition data such as texture, crystallinity, granularity, porosity, vesicularity, color, lustre, opacity, and

  13. In Situ Identification of Mineral Resources with an X-Ray-Optical "Hands-Lens" Instrument

    NASA Technical Reports Server (NTRS)

    Marshall, J.; Koppel, L.; Bratton, C.; Metzger, E.; Hecht, M.

    1999-01-01

    The recognition of material resources on a planetary surface requires exploration strategies not dissimilar to those employed by early field geologists who searched for ore deposits primarily from surface clues. In order to determine the location of mineral ores or other materials, it will be necessary to characterize host terranes at regional or subregional scales. This requires geographically broad surveys in which statistically significant numbers of samples are rapidly scanned from a roving platform. To enable broad-scale, yet power-conservative planetary-surface exploration, we are developing an instrument that combines x-ray diffractometry (XRD), x-ray fluorescence spectrometry (XRF), and optical capabilities; the instrument can be deployed at the end of a rover's robotic arm, without the need for sample capture or preparation. The instrument provides XRD data for identification of mineral species and lithological types; diffractometry of minerals is conducted by ascertaining the characteristic lattice parameters or "d-spacings" of mineral compounds. D-spacings of 1.4 to 25 angstroms can be determined to include the large molecular structures of hydrated minerals such as clays. The XRF data will identify elements ranging from carbon (Atomic Number = 6) to elements as heavy as barium (Atomic Number = 56). While a sample is being x-rayed, the instrument simultaneously acquires an optical image of the sample surface at magnifications from lx to at least 50x (200x being feasible, depending on the sample surface). We believe that imaging the sample is extremely important as corroborative sample-identification data (the need for this capability having been illustrated by the experience of the Pathfinder rover). Very few geologists would rely on instrument data for sample identification without having seen the sample. Visual inspection provides critical recognition data such as texture, crystallinity, granularity, porosity, vesicularity, color, lustre, opacity, and

  14. In Situ Identification of Mineral Resources with an X-Ray-Optical "Hands-Lens" Instrument

    NASA Astrophysics Data System (ADS)

    Marshall, J.; Koppel, L.; Bratton, C.; Metzger, E.; Hecht, M.

    1999-09-01

    The recognition of material resources on a planetary surface requires exploration strategies not dissimilar to those employed by early field geologists who searched for ore deposits primarily from surface clues. In order to determine the location of mineral ores or other materials, it will be necessary to characterize host terranes at regional or subregional scales. This requires geographically broad surveys in which statistically significant numbers of samples are rapidly scanned from a roving platform. To enable broad-scale, yet power-conservative planetary-surface exploration, we are developing an instrument that combines x-ray diffractometry (XRD), x-ray fluorescence spectrometry (XRF), and optical capabilities; the instrument can be deployed at the end of a rover's robotic arm, without the need for sample capture or preparation. The instrument provides XRD data for identification of mineral species and lithological types; diffractometry of minerals is conducted by ascertaining the characteristic lattice parameters or "d-spacings" of mineral compounds. D-spacings of 1.4 to 25 angstroms can be determined to include the large molecular structures of hydrated minerals such as clays. The XRF data will identify elements ranging from carbon (Atomic Number = 6) to elements as heavy as barium (Atomic Number = 56). While a sample is being x-rayed, the instrument simultaneously acquires an optical image of the sample surface at magnifications from lx to at least 50x (200x being feasible, depending on the sample surface). We believe that imaging the sample is extremely important as corroborative sample-identification data (the need for this capability having been illustrated by the experience of the Pathfinder rover). Very few geologists would rely on instrument data for sample identification without having seen the sample. Visual inspection provides critical recognition data such as texture, crystallinity, granularity, porosity, vesicularity, color, lustre, opacity, and

  15. Effect of iron oxide reductive dissolution on the transformation and immobilization of arsenic in soils: New insights from X-ray photoelectron and X-ray absorption spectroscopy.

    PubMed

    Fan, Jian-Xin; Wang, Yu-Jun; Liu, Cun; Wang, Li-Hua; Yang, Ke; Zhou, Dong-Mei; Li, Wei; Sparks, Donald L

    2014-08-30

    The geochemical behavior and speciation of arsenic (As) in paddy soils is strongly controlled by soil redox conditions and the sequestration by soil iron oxyhydroxides. Hence, the effects of iron oxide reductive dissolution on the adsorption, transformation and precipitation of As(III) and As(V) in soils were investigated using batch experiments and synchrotron based techniques to gain a deeper understanding at both macroscopic and microscopic scales. The results of batch sorption experiments revealed that the sorption capacity of As(V) on anoxic soil was much higher than that on control soil. Synchrotron based X-ray fluorescence (μ-XRF) mapping studies indicated that As was heterogeneously distributed and was mainly associated with iron in the soil. X-ray absorption near edge structure (XANES), micro-X-ray absorption near edge structure (μ-XANES) and X-ray photoelectron spectroscopy (XPS) analyses revealed that the primary speciation of As in the soil is As(V). These results further suggested that, when As(V) was introduced into the anoxic soil, the rapid coprecipitation of As(V) with ferric/ferrous ion prevented its reduction to As(III), and was the main mechanism controlling the immobilization of As. This research could improve the current understanding of soil As chemistry in paddy and wetland soils. PMID:25064258

  16. Quick extended x-ray absorption fine structure instrument with millisecond time scale, optimized for in situ applications.

    PubMed

    Khalid, S; Caliebe, W; Siddons, P; So, I; Clay, B; Lenhard, T; Hanson, J; Wang, Q; Frenkel, A I; Marinkovic, N; Hould, N; Ginder-Vogel, M; Landrot, G L; Sparks, D L; Ganjoo, A

    2010-01-01

    In order to learn about in situ structural changes in materials at subseconds time scale, we have further refined the techniques of quick extended x-ray absorption fine structure (QEXAFS) and quick x-ray absorption near edge structure (XANES) spectroscopies at beamline X18B at the National Synchrotron Light Source. The channel cut Si (111) monochromator oscillation is driven through a tangential arm at 5 Hz, using a cam, dc motor, pulley, and belt system. The rubber belt between the motor and the cam damps the mechanical noise. EXAFS scan taken in 100 ms is comparable to standard data. The angle and the angular range of the monochromator can be changed to collect a full EXAFS or XANES spectrum in the energy range 4.7-40.0 KeV. The data are recorded in ascending and descending order of energy, on the fly, without any loss of beam time. The QEXAFS mechanical system is outside the vacuum system, and therefore changing the mode of operation from conventional to QEXAFS takes only a few minutes. This instrument allows the acquisition of time resolved data in a variety of systems relevant to electrochemical, photochemical, catalytic, materials, and environmental sciences.

  17. Highly multiplexible thermal kinetic inductance detectors for x-ray imaging spectroscopy

    SciTech Connect

    Ulbricht, Gerhard Mazin, Benjamin A.; Szypryt, Paul; Walter, Alex B.; Bockstiegel, Clint; Bumble, Bruce

    2015-06-22

    For X-ray imaging spectroscopy, high spatial resolution over a large field of view is often as important as high energy resolution, but current X-ray detectors do not provide both in the same device. Thermal Kinetic Inductance Detectors (TKIDs) are being developed as they offer a feasible way to combine the energy resolution of transition edge sensors with pixel counts approaching CCDs and thus promise significant improvements for many X-ray spectroscopy applications. TKIDs are a variation of Microwave Kinetic Inductance Detectors (MKIDs) and share their multiplexibility: working MKID arrays with 2024 pixels have recently been demonstrated and much bigger arrays are under development. In this work, we present a TKID prototype, which is able to achieve an energy resolution of 75 eV at 5.9 keV, even though its general design still has to be optimized. We further describe TKID fabrication, characterization, multiplexing, and working principle and demonstrate the necessity of a data fitting algorithm in order to extract photon energies. With further design optimizations, we expect to be able to improve our TKID energy resolution to less than 10 eV at 5.9 keV.

  18. Surface arsenic speciation of a drinking-water treatment residual using X-ray absorption spectroscopy.

    PubMed

    Makris, Konstantinos C; Sarkar, Dibyendu; Parsons, Jason G; Datta, Rupali; Gardea-Torresdey, Jorge L

    2007-07-15

    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(-1)) after 48 h of reaction. Subsequent desorption experiments with a high P load (7500 mg kg(-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.

  19. Multidimensional x-ray spectroscopy of valence and core excitations in cysteine

    PubMed Central

    Biggs, Jason D.; Zhang, Yu; Healion, Daniel; Mukamel, Shaul

    2013-01-01

    Several nonlinear spectroscopy experiments which employ broadband x-ray pulses to probe the coupling between localized core and delocalized valence excitation are simulated for the amino acid cysteine at the K-edges of oxygen and nitrogen and the K- and L-edges of sulfur. We focus on two-dimensional (2D) and 3D signals generated by two- and three-pulse stimulated x-ray Raman spectroscopy (SXRS) with frequency-dispersed probe. We show how the four-pulse x-ray signals \\documentclass[12pt]{minimal}\\begin{document}${\\bm k}_\\mathrm{I} =-{\\bm k} _1+{\\bm k} _2+{\\bm k} _3$\\end{document}kI=−k1+k2+k3 and \\documentclass[12pt]{minimal}\\begin{document}${\\bm k}_\\mathrm{II} ={\\bm k} _1-{\\bm k} _2+{\\bm k} _3$\\end{document}k II =k1−k2+k3 can give new 3D insight into the SXRS signals. The coupling between valence- and core-excited states can be visualized in three-dimensional plots, revealing the origin of the polarizability that controls the simpler pump-probe SXRS signals. PMID:24981531

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

    SciTech Connect

    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.

  1. Pixellated Cd(Zn)Te high-energy X-ray instrument

    NASA Astrophysics Data System (ADS)

    Seller, P.; Bell, S.; Cernik, R. J.; Christodoulou, C.; Egan, C. K.; Gaskin, J. A.; Jacques, S.; Pani, S.; Ramsey, B. D.; Reid, C.; Sellin, P. J.; Scuffham, J. W.; Speller, R. D.; Wilson, M. D.; Veale, M. C.

    2011-12-01

    We have developed a pixellated high energy X-ray detector instrument to be used in a variety of imaging applications. The instrument consists of either a Cadmium Zinc Telluride or Cadmium Telluride (Cd(Zn)Te) detector bump-bonded to a large area ASIC and packaged with a high performance data acquisition system. The 80 by 80 pixels each of 250 μm by 250 μm give better than 1 keV FWHM energy resolution at 59.5 keV and 1.5 keV FWHM at 141 keV, at the same time providing a high speed imaging performance. This system uses a relatively simple wire-bonded interconnection scheme but this is being upgraded to allow multiple modules to be used with very small dead space. The readout system and the novel interconnect technology is described and how the system is performing in several target applications.

  2. Pixellated Cd(Zn)Te high-energy X-ray instrument

    PubMed Central

    Seller, P.; Bell, S.; Cernik, R.J.; Christodoulou, C.; Egan, C.K.; Gaskin, J.A.; Jacques, S.; Pani, S.; Ramsey, B.D.; Reid, C.; Sellin, P.J.; Scuffham, J.W.; Speller, R.D.; Wilson, M.D.; Veale, M.C.

    2012-01-01

    We have developed a pixellated high energy X-ray detector instrument to be used in a variety of imaging applications. The instrument consists of either a Cadmium Zinc Telluride or Cadmium Telluride (Cd(Zn)Te) detector bump-bonded to a large area ASIC and packaged with a high performance data acquisition system. The 80 by 80 pixels each of 250 μm by 250 μm give better than 1 keV FWHM energy resolution at 59.5 keV and 1.5 keV FWHM at 141 keV, at the same time providing a high speed imaging performance. This system uses a relatively simple wire-bonded interconnection scheme but this is being upgraded to allow multiple modules to be used with very small dead space. The readout system and the novel interconnect technology is described and how the system is performing in several target applications. PMID:22737179

  3. Inside and Outside: X-ray Absorption Spectroscopy Mapping of Chemical Domains in Graphene Oxide.

    PubMed

    De Jesus, Luis R; Dennis, Robert V; Depner, Sean W; Jaye, Cherno; Fischer, Daniel A; Banerjee, Sarbajit

    2013-09-19

    The oxidative chemistry of graphite has been investigated for over 150 years and has attracted renewed interest given the importance of exfoliated graphene oxide as a precursor to chemically derived graphene. However, the bond connectivities, steric orientations, and spatial distribution of functional groups remain to be unequivocally determined for this highly inhomogeneous nonstoichiometric material. Here, we demonstrate the application of principal component analysis to scanning transmission X-ray microscopy data for the construction of detailed real space chemical maps of graphene oxide. These chemical maps indicate very distinct functionalization motifs at the edges and interiors and, in conjunction with angle-resolved near-edge X-ray absorption fine structure spectroscopy, enable determination of the spatial location and orientations of functional groups. Chemical imaging of graphene oxide provides experimental validation of the modified Lerf-Klinowski structural model. Specifically, we note increased contributions from carboxylic acid moieties at edge sites with epoxide and hydroxyl species dominant within the interior domains.

  4. In situ x-ray photoelectron spectroscopy for electrochemical reactions in ordinary solvents

    SciTech Connect

    Masuda, Takuya; Yoshikawa, Hideki; Kobata, Masaaki; Kobayashi, Keisuke; Noguchi, Hidenori; Kawasaki, Tadahiro; Uosaki, Kohei

    2013-09-09

    In situ electrochemical X-ray photoelectron spectroscopy (XPS) apparatus, which allows XPS at solid/liquid interfaces under potential control, was constructed utilizing a microcell with an ultra-thin Si membrane, which separates vacuum and a solution. Hard X-rays from a synchrotron source penetrate into the Si membrane surface exposed to the solution. Electrons emitted at the Si/solution interface can pass through the membrane and be analyzed by an analyzer placed in vacuum. Its operation was demonstrated for potential-induced Si oxide growth in water. Effect of potential and time on the thickness of Si and Si oxide layers was quantitatively determined at sub-nanometer resolution.

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

    PubMed

    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. PMID:25832284

  6. Elemental characterisation of melanin in feathers via synchrotron X-ray imaging and absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Edwards, Nicholas P.; van Veelen, Arjen; Anné, Jennifer; Manning, Phillip L.; Bergmann, Uwe; Sellers, William I.; Egerton, Victoria M.; Sokaras, Dimosthenis; Alonso-Mori, Roberto; Wakamatsu, Kazumasa; Ito, Shosuke; Wogelius, Roy A.

    2016-09-01

    Melanin is a critical component of biological systems, but the exact chemistry of melanin is still imprecisely known. This is partly due to melanin’s complex heterogeneous nature and partly because many studies use synthetic analogues and/or pigments extracted from their natural biological setting, which may display important differences from endogenous pigments. Here we demonstrate how synchrotron X-ray analyses can non-destructively characterise the elements associated with melanin pigment in situ within extant feathers. Elemental imaging shows that the distributions of Ca, Cu and Zn are almost exclusively controlled by melanin pigment distribution. X-ray absorption spectroscopy demonstrates that the atomic coordination of zinc and sulfur is different within eumelanised regions compared to pheomelanised regions. This not only impacts our fundamental understanding of pigmentation in extant organisms but also provides a significant contribution to the evidence-based colour palette available for reconstructing the appearance of fossil organisms.

  7. Elemental characterisation of melanin in feathers via synchrotron X-ray imaging and absorption spectroscopy

    PubMed Central

    Edwards, Nicholas P.; van Veelen, Arjen; Anné, Jennifer; Manning, Phillip L.; Bergmann, Uwe; Sellers, William I.; Egerton, Victoria M.; Sokaras, Dimosthenis; Alonso-Mori, Roberto; Wakamatsu, Kazumasa; Ito, Shosuke; Wogelius, Roy A.

    2016-01-01

    Melanin is a critical component of biological systems, but the exact chemistry of melanin is still imprecisely known. This is partly due to melanin’s complex heterogeneous nature and partly because many studies use synthetic analogues and/or pigments extracted from their natural biological setting, which may display important differences from endogenous pigments. Here we demonstrate how synchrotron X-ray analyses can non-destructively characterise the elements associated with melanin pigment in situ within extant feathers. Elemental imaging shows that the distributions of Ca, Cu and Zn are almost exclusively controlled by melanin pigment distribution. X-ray absorption spectroscopy demonstrates that the atomic coordination of zinc and sulfur is different within eumelanised regions compared to pheomelanised regions. This not only impacts our fundamental understanding of pigmentation in extant organisms but also provides a significant contribution to the evidence-based colour palette available for reconstructing the appearance of fossil organisms. PMID:27658854

  8. Wiggler-base Hard X-ray Spectroscopy Beamline at CLS

    SciTech Connect

    Jiang, D. T.; Chen, N.; Sheng, W.

    2007-01-19

    The CLS 06ID-1 Hard X-ray Micro-Analysis Beamline (HXMA) is a general purpose hard X-ray spectroscopy beamline (5 to 40 keV) designed to serve users in XAFS, diffraction and microprobe communities. The beamline uses the synchrotron radiation from a superconducting wiggler. The primary beamline optics include a 1.2 m water-cooled silicon collimating mirror (separate Rh and Pt coating stripes), a liquid nitrogen cooled double crystal monochromator (Kohzu CMJ-1) housing two crystal pairs (Si 111 and 220), and a 1.15 m long water-cooled silicon toroidal focusing mirror (separate Rh and Pt coating stripes). All mirrors are equipped with dynamical meridian benders. The experimental hutch hosts three experimental setups for XAFS, diffraction and microprobe, respectively. Primary design considerations and some commissioning results are discussed.

  9. Electronic structure of cobalt doped CdSe quantum dots using soft X-ray spectroscopy

    SciTech Connect

    Joshua T. Wright; Su, Dong; van Buuren, Tony; Meulenberg, Robert W.

    2014-08-21

    The electronic structure and magnetic properties of cobalt doped CdSe quantum dots (QDs) are studied using electron microscopy, soft X-ray spectroscopy, and magnetometry. Magnetometry measurements suggest these QDs are superparamagnetic, contrary to a spin-glass state observed in the bulk analogue. Moreover, the electron microscopy shows well formed QDs, but with cobalt existing as doped into the QD and as unreacted species not contained in the QD. X-ray absorption measurements at the Co L3-edge suggest that changes in spectra features as a function of particle size can be described considering combination of a cobalt ion in a tetrahedral crystal field and an octahedrally coordinated (impurity) phase. With decreasing particle sizes, the impurity phase increases, suggesting that small QDs can be difficult to dope.

  10. Xe nanocrystals in Si studied by x-ray absorption fine structure spectroscopy

    SciTech Connect

    Faraci, Giuseppe; Pennisi, Agata R.; Zontone, Federico

    2007-07-15

    The structural configuration of Xe clusters, obtained by ion implantation in a Si matrix, has been investigated as a function of the temperature by x-ray absorption fine structure spectroscopy. In contrast with previous results, we demonstrate that an accurate analysis of the data, using high order cumulants, gives evidence of Xe fcc nanocrystals at low temperature, even in the as-implanted Si; expansion of the Xe lattice is always found as a function of the temperature, with no appreciable overpressure. We point out that a dramatic modification of these conclusions can be induced by an incorrect analysis using standard symmetrical pair distribution function G(r); for this reason, all the results were checked by x-ray diffraction measurements.

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

    SciTech Connect

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

    2015-03-15

    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.

  12. Hard x-ray photoelectron spectroscopy using an environmental cell with silicon nitride membrane windows

    SciTech Connect

    Tsunemi, Eika; Watanabe, Yoshio; Oji, Hiroshi; Cui, Yi-Tao; Son, Jin-Young

    2015-06-21

    We applied hard x-ray photoelectron spectroscopy (HAXPES) to a sample under ambient pressure conditions using an environmental cell with an approximately 24 nm-thick SiN{sub x} membrane window. As a model chemical substance, europium (II) iodide (EuI{sub 2}) sealed in the cell with argon gas was investigated with HAXPES to identify the chemical species present inside the cell. The optical and morphological properties of the sample within the cell were measured with optical and fluorescent microscopy, scanning electron microscopy, cathodoluminescence, and energy dispersive x-ray spectrometry. We confirmed the effectiveness of the gas barrier properties of the cell with the SiN{sub x} window and demonstrated its applicability to various other optical and electron measurements as well as HAXPES.

  13. Application of X-ray Fluorescence Spectroscopy in Analysis of Oil Paint Pigments

    NASA Astrophysics Data System (ADS)

    Major, Cassandra; Formica, Sarah

    2011-10-01

    X-ray Fluorescence (XRF) spectroscopy is a rapid, noninvasive technique for both detecting and identifying chemical elements within a given sample. At North Georgia College and State University, a sealed tube x-ray source and slightly focusing polycapillary optic are used in nondestructive XRF analysis of oil paint pigments. Oil paints contain both organic and inorganic matter, and the inorganic ingredients such as titanium, vanadium, iron, zinc, and other elements are easily detected by XRF, which can be used to uniquely differentiate between various paint pigments. To calibrate the XRF system for paint color identification, six different colors of oil paint were fluoresced and identified based off of their characteristic spectra. By scanning the paint sample in two dimensions, the characteristic XRF spectra obtained were compiled to produce an XRF replica of the painting.

  14. [Measurement and analysis of lead in soil using X-ray fluorescence spectroscopy].

    PubMed

    Zhang, Rong; Zhang, Yu-Jun; Zhang, Wei; Chen, Dong; Yu, Xiao-Ya; Gao, Yan-Wei

    2013-02-01

    The present paper analyzed the characteristics of X-ray fluorescence spectroscopy (XRF) of metal element lead in soil using the NITON XLt793 portable X-ray fluorescence spectra of heavy metal analyzer under laboratory conditions. The characteristic spectral lines of L(alpha) (energy: 10. 55 keV) and L(beta) (energy: 12. 61 keV) with different matrix elements were selected respectively for lead in the experiment. By measuring the intensities of the characteristic spectral line with different Pb concentration, the results demonstrate that the relation between concentration [mass fraction 10 x 10(-6) - 1 800 x 10(-6)] of Pb element and the intensity of the characteristic spectrum is well linear. The calibration curve of Pb was plotted based on the different concentration measurement results, and the limit of detection of 7.89 x 10(-6) was obtained for Pb in soil.

  15. Note: Sample chamber for in situ x-ray absorption spectroscopy studies of battery materials

    SciTech Connect

    Pelliccione, CJ; Timofeeva, EV; Katsoudas, JP; Segre, CU

    2014-12-01

    In situ x-ray absorption spectroscopy (XAS) provides element-specific characterization of both crystalline and amorphous phases and enables direct correlations between electrochemical performance and structural characteristics of cathode and anode materials. In situ XAS measurements are very demanding to the design of the experimental setup. We have developed a sample chamber that provides electrical connectivity and inert atmosphere for operating electrochemical cells and also accounts for x-ray interactions with the chamber and cell materials. The design of the sample chamber for in situ measurements is presented along with example XAS spectra from anode materials in operating pouch cells at the Zn and Sn K-edges measured in fluorescence and transmission modes, respectively. (C) 2014 AIP Publishing LLC.

  16. Soft x-ray spectroscopy undulator beamline at the Advanced Photon Source

    SciTech Connect

    Randall, K.J.; Xu, Z.; Moore, J.F.; Gluskin, E.

    1997-09-01

    Construction of the high-resolution soft x ray spectroscopy undulator beamline, 2ID-C, at the Advanced Photon Source (APS) has been completed. The beamline, one of two soft x ray beamlines at the APS, will cover the photon energy range from 500 to 3,000 eV, with a maximum resolving power between 7,000 and 14,000. The optical design is based on a spherical grating monochromator (SGM) giving both high resolution and high flux throughput. Photon flux is calculated to be approximately 10{sup 12}--10{sup 13} photons per second with a beam size of approximately 1 x 1 mm{sup 2} at the sample.

  17. Picosecond time-resolved X-ray absorption spectroscopy of ultrafast aluminum plasmas.

    PubMed

    Audebert, P; Renaudin, P; Bastiani-Ceccotti, S; Geindre, J-P; Chenais-Popovics, C; Tzortzakis, S; Nagels-Silvert, V; Shepherd, R; Matsushima, I; Gary, S; Girard, F; Peyrusse, O; Gauthier, J-C

    2005-01-21

    We have used point-projection K-shell absorption spectroscopy to infer the ionization and recombination dynamics of transient aluminum plasmas. Two femtosecond beams of the 100 TW laser at the LULI facility were used to produce an aluminum plasma on a thin aluminum foil (83 or 50 nm), and a picosecond x-ray backlighter source. The short-pulse backlighter probed the aluminum plasma at different times by adjusting the delay between the two femtosecond driving beams. Absorption x-ray spectra at early times are characteristic of a dense and rather homogeneous plasma. Collisional-radiative atomic physics coupled with hydrodynamic simulations reproduce fairly well the measured average ionization as a function of time. PMID:15698184

  18. X-ray fluorescence/Auger-electron coincidence spectroscopy of vacancy cascades in atomic argon

    SciTech Connect

    Arp, U.; LeBrun, T.; Southworth, S.H.; Jung, M.; MacDonald, M.A.

    1996-12-01

    Argon L{sub 2.3}-M{sub 2.3}M{sub 2.3} Auger-electron spectra were measured in coincidence with K{alpha} fluorescent x-rays in studies of Ar K-shell vacancy decays at several photon energies above the K-threshold and on the 1s-4p resonance in atomic argon. The complex spectra recorded by conventional electron spectroscopy are greatly simplified when recorded in coincidence with fluorescent x-rays, allowing a more detailed analysis of the vacancy cascade process. The resulting coincidence spectra are compared with Hartree-Fock calculations which include shake-up transitions in the resonant case. Small energy shifts of the coincidence electron spectra are attributed to post-collision interaction with 1s photoelectrons.

  19. Detection, identification and mapping of iron anomalies in brain tissue using X-ray absorption spectroscopy

    SciTech Connect

    Mikhaylova, A.; Davidson, M.; Toastmann, H.; Channell, J.E.T.; Guyodo, Y.; Batich, C.; Dobson, J.

    2008-06-16

    This work describes a novel method for the detection, identification and mapping of anomalous iron compounds in mammalian brain tissue using X-ray absorption spectroscopy. We have located and identified individual iron anomalies in an avian tissue model associated with ferritin, biogenic magnetite and haemoglobin with a pixel resolution of less than 5 {micro}m. This technique represents a breakthrough in the study of both intra- and extra-cellular iron compounds in brain tissue. The potential for high-resolution iron mapping using microfocused X-ray beams has direct application to investigations of the location and structural form of iron compounds associated with human neurodegenerative disorders - a problem which has vexed researchers for 50 years.

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

    NASA Astrophysics Data System (ADS)

    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.

  1. Microcalorimeters for High Resolution X-Ray Spectroscopy of Laboratory and Astrophysical Plasmas

    NASA Technical Reports Server (NTRS)

    Silver, E.; Flowers, Bobby J. (Technical Monitor)

    2003-01-01

    The proposal has three major objectives. The first focuses on advanced neutron-transmutation-doped (NTD)-based microcalorimeter development. Our goal is to develop an array of microcalorimeters with sub- 5 eV energy resolution that can operate with pile-up-free throughput of at least 100 Hz per pixel. The second objective is to establish our microcalorimeter as an essential x-ray diagnostic for laboratory astrophysics studies. We propose to develop a dedicated microcalorimeter spectrometer for the EBIT (electron beam ion trap). This instrument will incorporate the latest detector and cryogenic technology that we have available. The third objective is to investigate innovative ideas related to possible flight opportunities. These include compact, long lived cryo-systems, ultra-low temperature cold stages, low mass and low power electronics, and novel assemblies of thin windows with high x-ray transmission.

  2. Injection Methods and Instrumentation for Serial X-ray Free Electron Laser Experiments

    NASA Astrophysics Data System (ADS)

    James, Daniel

    Scientists have used X-rays to study biological molecules for nearly a century. Now with the X-ray free electron laser (XFEL), new methods have been developed to advance structural biology. These new methods include serial femtosecond crystallography, single particle imaging, solution scattering, and time resolved techniques. The XFEL is characterized by high intensity pulses, which are only about 50 femtoseconds in duration. The intensity allows for scattering from microscopic particles, while the short pulses offer a way to outrun radiation damage. XFELs are powerful enough to obliterate most samples in a single pulse. While this allows for a "diffract and destroy" methodology, it also requires instrumentation that can position microscopic particles into the X-ray beam (which may also be microscopic), continuously renew the sample after each pulse, and maintain sample viability during data collection. Typically these experiments have used liquid microjets to continuously renew sample. The high flow rate associated with liquid microjets requires large amounts of sample, most of which runs to waste between pulses. An injector designed to stream a viscous gel-like material called lipidic cubic phase (LCP) was developed to address this problem. LCP, commonly used as a growth medium for membrane protein crystals, lends itself to low flow rate jetting and so reduces the amount of sample wasted significantly. This work discusses sample delivery and injection for XFEL experiments. It reviews the liquid microjet method extensively, and presents the LCP injector as a novel device for serial crystallography, including detailed protocols for the LCP injector and anti-settler operation.

  3. Algorithms for a hand-held miniature x-ray fluorescence analytical instrument

    SciTech Connect

    Elam, W.T.; Newman, D.; Ziemba, F.

    1998-12-31

    The purpose of this joint program was to provide technical assistance with the development of a Miniature X-ray Fluorescence (XRF) Analytical Instrument. This new XRF instrument is designed to overcome the weaknesses of spectrometers commercially available at the present time. Currently available XRF spectrometers (for a complete list see reference 1) convert spectral information to sample composition using the influence coefficients technique or the fundamental parameters method. They require either a standard sample with composition relatively close to the unknown or a detailed knowledge of the sample matrix. They also require a highly-trained operator and the results often depend on the capabilities of the operator. In addition, almost all existing field-portable, hand-held instruments use radioactive sources for excitation. Regulatory limits on such sources restrict them such that they can only provide relatively weak excitation. This limits all current hand-held XRF instruments to poor detection limits and/or long data collection times, in addition to the licensing requirements and disposal problems for radioactive sources. The new XRF instrument was developed jointly by Quantrad Sensor, Inc., the Naval Research Laboratory (NRL), and the Department of Energy (DOE). This report describes the analysis algorithms developed by NRL for the new instrument and the software which embodies them.

  4. X-ray photoelectron spectroscopy of copper(II), copper(I), and mixed valence systems.

    PubMed

    Rupp, H; Weser, U

    1976-01-01

    X-ray photoelectron spectroscopy using copper(II), copper(I) and the mixed valence Cu(II)/Cu(I) compounds was employed as a means of studying electron transfer reactions in copper proteins. The X-ray photoelectron spectra of copper(II) compounds display characteristic satellites of both variable size and resolution. Some of these satellites could be assigned to specific ligand interactions. Unlike electron paramagnetic resonance spectroscopy, the X-ray photoelectron spectroscopic measurements of copper(I) compounds allowed the unequivocal assignment of this oxidation state. No satellites at all could be detected in the Cu(I) spectra. Furthermore, established mixed valence Cu(II)/Cu(I) complexes including Cu2SO3-CuSO3-2H2O and Cu4Cl5 (ethylenediamine)2 proved essentially a mixture of distinct portions of Cu(I) and Cu(II). This indicates that both oxidation states of copper survive in such complexes. In contrast, all Cu X-ray photoelectron signals of the more tentatively described mixed valence complexes Na2Cu3S3 and the mineral covellite, CuI4CuII2(S2)2S2, could be attributed exclusively to Cu(I). In view of the known binding of copper with sulfur in many copper proteins, it was of utmost importance to study the copper-sulfur interactions. We have demonstrated the absence of Cu(II) in CuS. This indicates strong metal-induced polarization of sulfur resulting in electron transfer to copper to yield Cu(I). PMID:953045

  5. Effect of regolith on planetary X-ray fluorescence spectroscopy: laboratory and numerical studies

    NASA Astrophysics Data System (ADS)

    Naranen, Jyri; Carpenter, James; Parviainen, Hannu; Muinonen, Karri

    Fluorescent X-rays from the surfaces of airless planetary bodies in the inner solar system have been measured by instruments on several spacecraft. X-ray emission follows photoionisation by incident solar X-rays and charged particles and reveals the elemental composition of the surface. Analyses of X-ray spectra obtained by orbiting spacecraft, use the relative intensities of elemental emission lines (e.g., Ca/Si, Fe/Si) to determine the geochemistry of the target body. Historically, the analysis of X-ray spectra has assumed that surfaces can be considered as homogeneous plane-parallel media. It has been shown, however, that relative line intensities are affected by the physical properties of the target surface (e.g. particle size distribution and packing density of the regolith) and the viewing and illumination geometry of observations. We describe experimental investigations into the effects of regolith properties on the line ratios measured by a nadir pointing (emergence angle 0° ) orbiting instrument, with with solar illumination angles in the range 25-75° from zenith. The planetary regolith analogue used in these experiments was a terrestrial, olivine rich basalt, which has been used by previous authors as an analogue to the lunar maria. The basalt samples were ground to powder and sieved to discriminate particles in the ranges, <75µm, 75-250µm, and 250-500µm. These separate powders were then pressed into solid pellets. The separation of particles with different sizes allows some determination of the effects due to changes in particle size. All measurements were made at pressures of less than 0.5 mbar to prevent absorption of fluorescent X-rays in air. The relative fluorescent line ratios of several major rock forming elements (K, Ca, Ti, Si) were measured. We find that for measurements made in a "nadir" pointing geometry, the measured spectrum becomes increasingly hard as illumination angle increases (i.e. X-ray lines at higher energies are enhanced

  6. The X-ray Microcalorimeter Spectrometer (XMS): A Reference Cryogenic Instrument Design for Constellation-X

    NASA Technical Reports Server (NTRS)

    Whitehouse, Paul L.

    2003-01-01

    Constellation-X, a mission now belonging to the Beyond Einstein initiative, is being planned to inherit the x-ray sky from Chandra, XMM-Newton and Astro-E. The first two of four observatories in the constellation will be launched together in 2013 and followed a year later by the launch of the remaining two. The four will independently orbit the Sun-Earth Lagrange point L2. An instrument compliment resides in the Focal Plane Module (FPM) of each observatory 10 m from the Optics Module and consists of three Hard X-ray Telescope (HXT) detectors, a Reflection Grating Spectrometer (RGS) focal plane CCD camera and an X-ray Microcalorimeter Spectrometer (XMS). Instrument awards are scheduled for early 2006. The reference detector for XMS is a 32 x 32 array of microcalorimetric superconducting Transition Edge Sensors (TES). Each pixel casts a variable resistance in a SQUID based multiplexed readout circuit which is coupled to series SQUID arrays for amplification and finally read out by external electronics. A multi-stage continuous ADR will provide the stable 50 mK desired for the TES array and a stable 1 K for the series SQUID arrays while also lifting thermal parasitic and inefficiency loads to a 6 K cryocooler interface. The 6 K cryocooler is expected to emerge from the joint-project Advanced Cryocooler Technology Development Program (ACTDP) in which Constellation-X is an active participant. Project Pre-Formulation activities are marked by extensive technology development necessitating early, but realistic, thermal and cooling load requirements for ADR and ACTDP-cryocooler design points. Such requirements are driven by the encompassing XMS cryostat and ultimately by the thermal environment imposed by the FPM. It is further desired that the XMS instrument be able to operate on its side in the laboratory, with a warm vacuum shell, during an extensive calibration regime. It is that reference system design of the XMS instrument (microcalorimeter, ADR, cryocooler and

  7. New instruments for measuring x-rays from rocket-triggered lightning

    NASA Astrophysics Data System (ADS)

    Al Dayeh, M.; Dwyer, J. R.; Uman, M. A.; Rassoul, H. K.; Rakov, V. A.; Caraway, L.; Wright, B.; Chrest, A.; Rambo, K. J.; Jordan, D. M.; Jerauld, J.; Smyth, C.

    2003-12-01

    We have previously reported the observations of energetic radiation from rocket-triggered lightning made in the summer of 2002. These observations used one 12.7 cm diameter NaI(Tl)/PMT detector and one identical control detector (with no scintillator), housed in a container designed to operate in the electromagnetically noisy environment near lightning. Since then, we have constructed four new instruments, using seven 7.6 cm diameter NaI(Tl)/PMT detectors plus one control detector. The instruments were each housed in a heavy aluminum box. The sides of the boxes were 1.27 cm thick, except for a 0.32 cm thick Al window on the top that allowed x-rays with energies down to 30 keV to enter. The boxes were welded and RF gaskets and O-rings were used on all access doors to prevent RF noise, moisture and light from entering. The instruments were battery powered, and controlled on and off through fiber optic signals. In addition, the data were transmitted through fiber optic cables to a receiver in a shielded metal trailer and saved on the hard drives of three PCs. Data acquisition was initiated by an external trigger derived from the lightning current, signaling the time of the leading edge of the return strokes or other large current pulses. The entire waveforms from seven of the PMT detectors were then digitized with 0.2 microsecond resolution for 220 msec with 20 msec of pre-trigger sampling. For three detectors the waveforms were digitized with 10 nanosecond resolution for 10 msec with 1 msec of pre-trigger sampling. Measurements were made using these instruments at the International Center for Lightning Research and Testing (ICLRT) at Camp Blanding, FL during the summer of 2003, and 10 flashes were observed with a total of 28 dart leader/return strokes sequences and two initial continuous current intervals. For the first five lightning flashes, 1.7 cm thick bronze collimators were placed around and in front of the detectors in order to study the intensity and arrival

  8. Electronic Properties of Hydrogen Storage Materials with Photon-in/Photon-out Soft-X-Ray Spectroscopy

    SciTech Connect

    Guo, Jinghua

    2008-09-22

    The applications of resonant soft X-ray emission spectroscopy on a variety of carbon systems have yielded characteristic fingerprints. With high-resolution monochromatized synchrotron radiation excitation, resonant inelastic X-ray scattering has emerged as a new source of information about electronic structure and excitation dynamics. Photon-in/photon-out soft-X-ray spectroscopy is used to study the electronic properties of fundamental materials, nanostructure, and complex hydrides and will offer potential in-depth understanding of chemisorption and/or physisorption mechanisms of hydrogen adsorption/desorption capacity and kinetics.

  9. Characterizing Hohlraum Plasma Conditions at the National Ignition Facility (NIF) Using X-ray Spectroscopy

    NASA Astrophysics Data System (ADS)

    Barrios, Maria Alejandra

    2015-11-01

    Improved hohlraums will have a significant impact on increasing the likelihood of indirect drive ignition at the NIF. In indirect-drive Inertial Confinement Fusion (ICF), a high-Z hohlraum converts laser power into a tailored x-ray flux that drives the implosion of a spherical capsule filled with D-T fuel. The x-radiation drive to capsule coupling sets the velocity, adiabat, and symmetry of the implosion. Previous experiments in gas-filled hohlraums determined that the laser-hohlraum energy coupling is 20-25% less than modeled, therefore identifying energy loss mechanisms that reduce the efficacy of the hohlraum drive is central to improving implosion performance. Characterizing the plasma conditions, particularly the plasma electron temperature (Te) , is critical to understanding mechanism that affect the energy coupling such as the laser plasma interactions (LPI), hohlraum x-ray conversion efficiency, and dynamic drive symmetry. The first Te measurements inside a NIF hohlraum, presented here, were achieved using K-shell X-ray spectroscopy of an Mn-Co tracer dot. The dot is deposited on a thin-walled CH capsule, centered on the hohlraum symmetry axis below the laser entrance hole (LEH) of a bottom-truncated hohlraum. The hohlraum x-ray drive ablates the dot and causes it to flow upward, towards the LEH, entering the hot laser deposition region. An absolutely calibrated streaked spectrometer with a line of sight into the LEH records the temporal history of the Mn and Co X-ray emission. The measured (interstage) Lyα/ Heα line ratios for Co and Mn and the Mn-Heα/Co-Heα isoelectronic line ratio are used to infer the local plasma Te from the atomic physics code SCRAM. Time resovled x-ray images perpendicular to the hohlraum axis record the dot expansion and trajectory into the LEH region. The temporal evolution of the measured Te and dot trajectory are compared with simulations from radiation-hydrodynamic codes. This work was performed under the auspices of the U

  10. Study of hard disk and slider surfaces using X-ray photoemission electron microscopy and near-edge X-ray absorption fine structure spectroscopy

    SciTech Connect

    Anders, S.; Stammler, T.; Bhatia, C.S.; Fong, W.; Chen, C.Y.; Bogy, D.B.

    1998-04-01

    X-ray Photo Emission Electron Microscopy (X-PEEM) and Near Edge X-ray Absorption Fine Structure (NEXAFS) spectroscopy were applied to study the properties of amorphous hard carbon overcoats on disks and sliders, and the properties of the lubricant. The modification of lubricants after performing thermal desorption studies was measured by NEXAFS, and the results are compared to the thermal desorption data. The study of lubricant degradation in wear tracks is described. Sliders were investigated before and after wear test, and the modification of the slider coating as well as the transfer of lubricant to the slider was studied. The studies show that the lubricant is altered chemically during the wear. Fluorine is removed and carboxyl groups are formed.

  11. Thermal and magnetic anomalies of α-iron: an exploration by extended x-ray absorption fine structure spectroscopy and synchrotron x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Boccato, Silvia; Sanson, Andrea; Kantor, Innokenty; Mathon, Olivier; Dyadkin, Vadim; Chernyshov, Dmitry; Carnera, Alberto; Pascarelli, Sakura

    2016-09-01

    The local structure and dynamics of α-iron have been investigated by extended x-ray absorption fine structure (EXAFS) spectroscopy and x-ray diffraction (XRD) in order to shed light on some thermal and magnetic anomalies observed in the last decades. The quantitative EXAFS analysis of the first two coordination shells reveals a peculiar local vibrational dynamics of α-iron: the second neighbor distance exhibits anharmonicity and vibrational anisotropy larger than the first neighbor distance. We search for possible distortions of the bcc structure to justify the unexplained magnetostriction anomalies of α-iron and provide a value for the maximum dislocation of the central Fe atom. No thermal anomalies have been detected from the current XRD data. On the contrary, an intriguing thermal anomaly at about 150 K, ascribed to a stiffening of the Fe–Fe bonds, was found by EXAFS.

  12. Thermal and magnetic anomalies of α-iron: an exploration by extended x-ray absorption fine structure spectroscopy and synchrotron x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Boccato, Silvia; Sanson, Andrea; Kantor, Innokenty; Mathon, Olivier; Dyadkin, Vadim; Chernyshov, Dmitry; Carnera, Alberto; Pascarelli, Sakura

    2016-09-01

    The local structure and dynamics of α-iron have been investigated by extended x-ray absorption fine structure (EXAFS) spectroscopy and x-ray diffraction (XRD) in order to shed light on some thermal and magnetic anomalies observed in the last decades. The quantitative EXAFS analysis of the first two coordination shells reveals a peculiar local vibrational dynamics of α-iron: the second neighbor distance exhibits anharmonicity and vibrational anisotropy larger than the first neighbor distance. We search for possible distortions of the bcc structure to justify the unexplained magnetostriction anomalies of α-iron and provide a value for the maximum dislocation of the central Fe atom. No thermal anomalies have been detected from the current XRD data. On the contrary, an intriguing thermal anomaly at about 150 K, ascribed to a stiffening of the Fe-Fe bonds, was found by EXAFS.

  13. Thermal and magnetic anomalies of α-iron: an exploration by extended x-ray absorption fine structure spectroscopy and synchrotron x-ray diffraction.

    PubMed

    Boccato, Silvia; Sanson, Andrea; Kantor, Innokenty; Mathon, Olivier; Dyadkin, Vadim; Chernyshov, Dmitry; Carnera, Alberto; Pascarelli, Sakura

    2016-09-01

    The local structure and dynamics of α-iron have been investigated by extended x-ray absorption fine structure (EXAFS) spectroscopy and x-ray diffraction (XRD) in order to shed light on some thermal and magnetic anomalies observed in the last decades. The quantitative EXAFS analysis of the first two coordination shells reveals a peculiar local vibrational dynamics of α-iron: the second neighbor distance exhibits anharmonicity and vibrational anisotropy larger than the first neighbor distance. We search for possible distortions of the bcc structure to justify the unexplained magnetostriction anomalies of α-iron and provide a value for the maximum dislocation of the central Fe atom. No thermal anomalies have been detected from the current XRD data. On the contrary, an intriguing thermal anomaly at about 150 K, ascribed to a stiffening of the Fe-Fe bonds, was found by EXAFS.

  14. ATOMIC AND MOLECULAR PHYSICS: X-ray absorption near the edge structure and X-ray photoelectron spectroscopy studies on pyrite prepared by thermally sulfurizing iron films

    NASA Astrophysics Data System (ADS)

    Zhang, Hui; Liu, Ying-Shu; Wang, Bao-Yi; Wei, Long; Kui, Re-Xi; Qian, Hai-Jie

    2009-07-01

    This paper reports how pyrite films were prepared by thermal sulfurization of magnetron sputtered iron films and characterized by x-ray absorption near edge structure spectra and x-ray photoelectron spectroscopy on a 4B9B beam line at the Beijing Synchrotron Radiation Facility. The band gap of the pyrite agrees well with the optical band gap obtained by a spectrophotometer. The octahedral symmetry of pyrite leads to the splitting of the d orbit into t2g and eg levels. The high spin and low spin states were analysed through the difference of electron exchange interaction and the orbital crystal field. Only when the crystal field splitting is higher than 1.5 eV, the two weak peaks above the white lines can appear, and this was approved by experiments in the present work.

  15. 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

    NASA Astrophysics Data System (ADS)

    Blagoev, K.; Grozeva, M.; Malcheva, G.; Neykova, S.

    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.

  16. In Situ X-Ray Absorption Spectroscopy Study of the LiNiO2 Electrode

    NASA Astrophysics Data System (ADS)

    Mansour, A. N.; McBreen, J.; Melendres, C. A.

    1997-03-01

    LiNiO2 is one of the most promising active material for the development of novel 4V rechargeable lithium batteries. Recent x-ray diffraction studies showed that the electrochemical reactivity of this electrode is sensitive to the structure of the starting material as well as the charged products. To further examine this material, we have conducted an x-ray absorption spectroscopy (XAS) study to determine the structure of this electrode as a function of its charge state. Specifically, the x-ray absorption Ni K-edge energy, the pre-edge structure, and local structure parameters such as bond lengths, coordination numbers and disorders were investigated at various states of charge corresponding to Li_(1-x)NiO2 for x values of 0.0, 0.11, 0.23, 0.34, 0.45, 0.82, and 0.99. The charging which proceeds via lithium de-intercalation was conducted using constant current anodization at 0.5 mA in a non aqueous electrolyte consisting of 1M LiPF6 in 1:1:3 propylene ! carbonate, ethylene carbonate and dimethyl carbonate. The XAS results for this electrode will be compared with those of γ-NiOOH and KNiIO_6, the latter being used as a reference for quadrivalent nickel.

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

    PubMed

    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. PMID:25177997

  18. Nanoscale spectroscopy with polarized X-rays by NEXAFS-TXM

    NASA Astrophysics Data System (ADS)

    Guttmann, Peter; Bittencourt, Carla; Rehbein, Stefan; Umek, Polona; Ke, Xiaoxing; van Tendeloo, Gustaaf; Ewels, Chris P.; Schneider, Gerd

    2012-01-01

    Near-edge X-ray absorption spectroscopy (NEXAFS) is an essential analytical tool in material science. Combining NEXAFS with scanning transmission X-ray microscopy (STXM) adds spatial resolution and the possibility to study individual nanostructures. Here, we describe a full-field transmission X-ray microscope (TXM) that generates high-resolution, large-area NEXAFS data with a collection rate two orders of magnitude faster than is possible with STXM. The TXM optical design combines a spectral resolution of E/ΔE = 1 × 104 with a spatial resolution of 25 nm in a field of view of 15-20 µm and a data acquisition time of ~1 s. As an example, we present image stacks and polarization-dependent NEXAFS spectra from individual anisotropic sodium and protonated titanate nanoribbons. Our NEXAFS-TXM technique has the advantage that one image stack visualizes a large number of nanostructures and therefore already contains statistical information. This new high-resolution NEXAFS-TXM technique opens the way to advanced nanoscale science studies.

  19. X-ray Spectroscopy for Chemical and Energy Sciences. the Case of Heterogeneous Catalysis

    SciTech Connect

    Frenkel, A. I.; van Bokhoven, J. 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. Furthermore, 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. 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.

  20. Observation of iron spin-states using tabletop x-ray emission spectroscopy and microcalorimeter sensors

    NASA Astrophysics Data System (ADS)

    Joe, Y. I.; O'Neil, G. C.; Miaja-Avila, L.; Fowler, J. W.; Jimenez, R.; Silverman, K. L.; Swetz, D. S.; Ullom, J. N.

    2016-01-01

    X-ray emission spectroscopy (XES) is a powerful probe of the electronic and chemical state of elemental species embedded within complex compounds. X-ray sensors that combine high resolving power and high collecting efficiency are desirable for photon-starved XES experiments such as measurements of dilute, gaseous, and radiation-sensitive samples, time-resolved measurements, and in-laboratory XES. To assess whether arrays of cryogenic microcalorimeters will be useful in photon-starved XES scenarios, we demonstrate that these emerging energy-dispersive sensors can detect the spin-state of 3d electrons of iron in two different compounds, Fe2O3 and FeS2. The measurements were conducted with a picosecond pulsed laser-driven plasma as the exciting x-ray source. The use of this tabletop source suggests that time-resolved in-laboratory XES will be possible in the future. We also present simulations of {{K}}α and {{K}}β spectra that reveal the spin-state sensitivity of different combinations of sensor resolution and accumulated counts. These simulations predict that our current experimental apparatus can perform time-resolved XES measurements on some samples with a measurement time of a few 10 s of hours per time delay.

  1. Sequential single shot X-ray photon correlation spectroscopy at the SACLA free electron laser

    DOE PAGESBeta

    Lehmkühler, Felix; Kwaśniewski, Paweł; Roseker, Wojciech; Fischer, Birgit; Schroer, Martin A.; Tono, Kensuke; Katayama, Tetsuo; Sprung, Michael; Sikorski, Marcin; Song, Sanghoon; et al

    2015-11-27

    In this study, hard X-ray free electron lasers allow for the first time to access dynamics of condensed matter samples ranging from femtoseconds to several hundred seconds. In particular, the exceptional large transverse coherence of the X-ray pulses and the high time-averaged flux promises to reach time and length scales that have not been accessible up to now with storage ring based sources. However, due to the fluctuations originating from the stochastic nature of the self-amplified spontaneous emission (SASE) process the application of well established techniques such as X-ray photon correlation spectroscopy (XPCS) is challenging. Here we demonstrate a single-shotmore » based sequential XPCS study on a colloidal suspension with a relaxation time comparable to the SACLA free-electron laser pulse repetition rate. High quality correlation functions could be extracted without any indications for sample damage. This opens the way for systematic sequential XPCS experiments at FEL sources.« less

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

    NASA Astrophysics Data System (ADS)

    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.

  3. Investigation of the Ionic Hydration in Aqueous Salt Solutions by Soft X-ray Emission Spectroscopy.

    PubMed

    Jeyachandran, Y L; Meyer, F; Benkert, A; Bär, M; Blum, M; Yang, W; Reinert, F; Heske, C; Weinhardt, L; Zharnikov, M

    2016-08-11

    Understanding the molecular structure of the hydration shells and their impact on the hydrogen bond (HB) network of water in aqueous salt solutions is a fundamentally important and technically relevant question. In the present work, such hydration effects were studied for a series of representative salt solutions (NaCl, KCl, CaCl2, MgCl2, and KBr) by soft X-ray emission spectroscopy (XES) and resonant inelastic soft X-ray scattering (RIXS). The oxygen K-edge XES spectra could be described with three components, attributed to initial state HB configurations in pure water, water molecules that have undergone an ultrafast dissociation initiated by the X-ray excitation, and water molecules in contact with salt ions. The behavior of the individual components, as well as the spectral shape of the latter component, has been analyzed in detail. In view of the role of ions in such effects as protein denaturation (i.e., the Hofmeister series), we discuss the ion-specific nature of the hydration shells and find that the results point to a predominant role of anions as compared to cations. Furthermore, we observe a concentration-dependent suppression of ultrafast dissociation in all salt solutions, associated with a significant distortion of intact HB configurations of water molecules facilitating such a dissociation. PMID:27442708

  4. X-ray-absorption-spectroscopy study of manganese-containing compounds and photosynthetic spinach chloroplasts

    SciTech Connect

    Kirby, J.A.

    1981-05-01

    The manganese sites in chloroplasts, long thought to be involved in photosynthetic oxygen evolution have been examined and partially characterized by x-ray Absorption Spectroscopy (XAS) using synchrotron radiation. The local environment about the manganese atoms is estimated from an analysis of the extended X-ray Absorption Fine Structure (EXAFS). Comparisons with and simulations of the manganese EXAFS for several reference compounds leads to a model in which the chloroplast manganese atoms are contained in a binuclear complex similar to di-u-oxo-tetrakis-(2,2'-bipyridine) dimanganese. It is suggested that the partner metal is another manganese. The bridging ligands are most probably oxygen. The remaining manganese ligands are carbon, oxygen, or nitrogen. A roughly linear correlation between the X-ray K edge onset energy and the coordination charge of a large number of manganese coordination complexes and compounds has been developed. Entry of the chloroplast manganese edge energy onto this correlation diagram establishes that the active pool of manganese is in an oxidation state greater than +2.

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

    PubMed

    Shelby, Megan L; Lestrange, Patrick J; Jackson, Nicholas E; Haldrup, Kristoffer; Mara, Michael W; Stickrath, Andrew B; Zhu, Diling; Lemke, Henrik T; Chollet, Matthieu; Hoffman, Brian M; Li, Xiaosong; Chen, Lin X

    2016-07-20

    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 ∼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.

  6. Demonstration of a time-resolved x-ray scattering instrument utilizing the full-repetition rate of x-ray pulses at the Pohang Light Source

    NASA Astrophysics Data System (ADS)

    Jo, Wonhyuk; Eom, Intae; Landahl, Eric C.; Lee, Sooheyong; Yu, Chung-Jong

    2016-03-01

    We report on the development of a new experimental instrument for time-resolved x-ray scattering (TRXS) at the Pohang Light Source (PLS-II). It operates with a photon energy ranging from 5 to 18 keV. It is equipped with an amplified Ti:sappahire femtosecond laser, optical diagnostics, and laser beam delivery for pump-probe experiments. A high-speed single-element detector and high trigger-rate oscilloscope are used for rapid data acquisition. While this instrument is capable of measuring sub-nanosecond dynamics using standard laser pump/x-ray probe techniques, it also takes advantage of the dense 500 MHz standard fill pattern in the PLS-II storage ring to efficiently record nano-to-micro-second dynamics simultaneously. We demonstrate this capability by measuring both the (fast) impulsive strain and (slower) thermal recovery dynamics of a crystalline InSb sample following intense ultrafast laser excitation. Exploiting the full repetition rate of the storage ring results in a significant improvement in data collection rates compared to conventional bunch-tagging methods.

  7. Demonstration of a time-resolved x-ray scattering instrument utilizing the full-repetition rate of x-ray pulses at the Pohang Light Source.

    PubMed

    Jo, Wonhyuk; Eom, Intae; Landahl, Eric C; Lee, Sooheyong; Yu, Chung-Jong

    2016-03-01

    We report on the development of a new experimental instrument for time-resolved x-ray scattering (TRXS) at the Pohang Light Source (PLS-II). It operates with a photon energy ranging from 5 to 18 keV. It is equipped with an amplified Ti:sappahire femtosecond laser, optical diagnostics, and laser beam delivery for pump-probe experiments. A high-speed single-element detector and high trigger-rate oscilloscope are used for rapid data acquisition. While this instrument is capable of measuring sub-nanosecond dynamics using standard laser pump/x-ray probe techniques, it also takes advantage of the dense 500 MHz standard fill pattern in the PLS-II storage ring to efficiently record nano-to-micro-second dynamics simultaneously. We demonstrate this capability by measuring both the (fast) impulsive strain and (slower) thermal recovery dynamics of a crystalline InSb sample following intense ultrafast laser excitation. Exploiting the full repetition rate of the storage ring results in a significant improvement in data collection rates compared to conventional bunch-tagging methods. PMID:27036819

  8. Demonstration of a time-resolved x-ray scattering instrument utilizing the full-repetition rate of x-ray pulses at the Pohang Light Source.

    PubMed

    Jo, Wonhyuk; Eom, Intae; Landahl, Eric C; Lee, Sooheyong; Yu, Chung-Jong

    2016-03-01

    We report on the development of a new experimental instrument for time-resolved x-ray scattering (TRXS) at the Pohang Light Source (PLS-II). It operates with a photon energy ranging from 5 to 18 keV. It is equipped with an amplified Ti:sappahire femtosecond laser, optical diagnostics, and laser beam delivery for pump-probe experiments. A high-speed single-element detector and high trigger-rate oscilloscope are used for rapid data acquisition. While this instrument is capable of measuring sub-nanosecond dynamics using standard laser pump/x-ray probe techniques, it also takes advantage of the dense 500 MHz standard fill pattern in the PLS-II storage ring to efficiently record nano-to-micro-second dynamics simultaneously. We demonstrate this capability by measuring both the (fast) impulsive strain and (slower) thermal recovery dynamics of a crystalline InSb sample following intense ultrafast laser excitation. Exploiting the full repetition rate of the storage ring results in a significant improvement in data collection rates compared to conventional bunch-tagging methods.

  9. Synchrotron soft X-ray absorption spectroscopy study of carbon and silicon nanostructures for energy applications.

    PubMed

    Zhong, Jun; Zhang, Hui; Sun, Xuhui; Lee, Shuit-Tong

    2014-12-10

    Carbon and silicon materials are two of the most important materials involved in the history of the science and technology development. In the last two decades, C and Si nanoscale materials, e.g., carbon nanotubes, graphene, and silicon nanowires, and quantum dots, have also emerged as the most interesting nanomaterials in nanoscience and nanotechnology for their myriad promising applications such as for electronics, sensors, biotechnology, etc. In particular, carbon and silicon nanostructures are being utilized in energy-related applications such as catalysis, batteries, solar cells, etc., with significant advances. Understanding of the nature of surface and electronic structures of nanostructures plays a key role in the development and improvement of energy conversion and storage nanosystems. Synchrotron soft X-ray absorption spectroscopy (XAS) and related techniques, such as X-ray emission spectroscopy (XES) and scanning transmission X-ray microscopy (STXM), show unique capability in revealing the surface and electronic structures of C and Si nanomaterials. In this review, XAS is demonstrated as a powerful technique for probing chemical bonding, the electronic structure, and the surface chemistry of carbon and silicon nanomaterials, which can greatly enhance the fundamental understanding and also applicability of these nanomaterials in energy applications. The focus is on the unique advantages of XAS as a complementary tool to conventional microscopy and spectroscopy for effectively providing chemical and structural information about carbon and silicon nanostructures. The employment of XAS for in situ, real-time study of property evolution of C and Si nanostructures to elucidate the mechanisms in energy conversion or storage processes is also discussed.

  10. Capturing interfacial photoelectrochemical dynamics with picosecond time-resolved X-ray photoelectron spectroscopy.

    PubMed

    Neppl, Stefan; Shavorskiy, Andrey; Zegkinoglou, Ioannis; Fraund, Matthew; Slaughter, Daniel S; Troy, Tyler; Ziemkiewicz, Michael P; Ahmed, Musahid; Gul, Sheraz; Rude, Bruce; Zhang, Jin Z; Tremsin, Anton S; Glans, Per-Anders; Liu, Yi-Sheng; Wu, Cheng Hao; Guo, Jinghua; Salmeron, Miquel; Bluhm, Hendrik; Gessner, Oliver

    2014-01-01

    Time-resolved core-level spectroscopy using laser pulses to initiate and short X-ray pulses to trace photoinduced processes has the unique potential to provide electronic state- and atomic site-specific insight into fundamental electron dynamics in complex systems. Time-domain studies using transient X-ray absorption and emission techniques have proven extremely valuable to investigate electronic and structural dynamics in isolated and solvated molecules. Here, we describe the implementation of a picosecond time-resolved X-ray photoelectron spectroscopy (TRXPS) technique at the Advanced Light Source (ALS) and its application to monitor photoinduced electron dynamics at the technologically pertinent interface formed by N3 dye molecules anchored to nanoporous ZnO. Indications for a dynamical chemical shift of the Ru3d photoemission line originating from the N3 metal centre are observed ∼30 ps after resonant HOMO-LUMO excitation with a visible laser pump pulse. The transient changes in the TRXPS spectra are accompanied by a characteristic surface photovoltage (SPV) response of the ZnO substrate on a pico- to nanosecond time scale. The interplay between the two phenomena is discussed in the context of possible electronic relaxation and recombination pathways that lead to the neutralisation of the transiently oxidised dye after ultrafast electron injection. A detailed account of the experimental technique is given including an analysis of the chemical modification of the nano-structured ZnO substrate during extended periods of solution-based dye sensitisation and its relevance for studies using surface-sensitive spectroscopy techniques.

  11. Mineralogical and spectroscopic investigation of enstatite chondrites by X-ray diffraction and infrared reflectance spectroscopy

    NASA Astrophysics Data System (ADS)

    Izawa, M. R.; King, P. L.; Flemming, R. L.; Peterson, R. C.; McCausland, P. J.

    2009-05-01

    Reflectance spectroscopy of well-characterized meteorites provides an important means of linking meteorites to potential parent objects; an important objective in meteoritics research. There is a lack of such sample- correlated spectroscopic and mineralogical data sets in the literature to date. In an effort to improve this situation, the bulk mineralogy and infrared reflectance spectra of 13 enstatite chondrite meteorite finds, spanning the full range of textural alteration grades in both EL and EH classes have been investigated, including eleven recovered from the Antarctic and one from Northwest Africa. Rietveld refinement of high- resolution powder X-ray diffraction (XRD) data was used to identify the major mineral phases and quantify their modal abundances. The mineralogy and modes agree well with those of well-documented enstatite chondrites. Terrestrial weathering products such as Fe-oxyhydroxides, gypsum, and carbonates also occur in most of the meteorites from Antarctica. The mineral abundances determined via Rietveld refinement have been used to calculate model grain densities for each meteorite (i.e. density of the solid phases). Bulk magnetic susceptibility measurements combined with modal mineralogy reveal that as terrestrial weathering increases, both grain density and bulk susceptibility decrease. Sample-correlated thermal infrared (400-4500 cm-1, 2-25 μm) biconical (Diffuse) Reflectance Infrared Fourier Transform Spectroscopy data were collected for each meteorite to facilitate comparison with remote sensing data. The meteorite spectra are dominated by features corresponding to enstatite. Terrestrial weathering manifests itself as a broad, asymmetric H2O band centered near ~3400 cm-1, analogous to the "3 μm water of hydration feature" recognized in asteroid spectra, particularly from the enigmatic W-type asteroids. Additional sharp features superimposed on this band, as well as the sharpness of an asymmetric feature related to bound molecular

  12. Excited-state molecular structures captured by X-ray transient absorption spectroscopy: a decade and beyond.

    PubMed

    Chen, Lin X; Zhang, Xiaoyi; Lockard, Jenny V; Stickrath, Andrew B; Attenkofer, Klaus; Jennings, Guy; Liu, Di-Jia

    2010-03-01

    Transient molecular structures along chemical reaction pathways are important for predicting molecular reactivity, understanding reaction mechanisms, as well as controlling reaction pathways. During the past decade, X-ray transient absorption spectroscopy (XTA, or LITR-XAS, laser-initiated X-ray absorption spectroscopy), analogous to the commonly used optical transient absorption spectroscopy, has been developed. XTA uses a laser pulse to trigger a fundamental chemical process, and an X-ray pulse(s) to probe transient structures as a function of the time delay between the pump and probe pulses. Using X-ray pulses with high photon flux from synchrotron sources, transient electronic and molecular structures of metal complexes have been studied in disordered media from homogeneous solutions to heterogeneous solution-solid interfaces. Several examples from the studies at the Advanced Photon Source in Argonne National Laboratory are summarized, including excited-state metalloporphyrins, metal-to-ligand charge transfer (MLCT) states of transition metal complexes, and charge transfer states of metal complexes at the interface with semiconductor nanoparticles. Recent developments of the method are briefly described followed by a future prospective of XTA. It is envisioned that concurrent developments in X-ray free-electron lasers and synchrotron X-ray facilities as well as other table-top laser-driven femtosecond X-ray sources will make many breakthroughs and realise dreams of visualizing molecular movies and snapshots, which ultimately enable chemical reaction pathways to be controlled. PMID:20164647

  13. Excited-state molecular structures captured by x-ray transient absorption spectroscopy : a decade and beyond.

    SciTech Connect

    Chen, L. X.; Zhang, X.; Lockard, J. V.; Stickrath, A. B.; Attenkofer, K.; Jennings, G.; Liu, D.-J.; Northwestern Univ.

    2010-03-02

    Transient molecular structures along chemical reaction pathways are important for predicting molecular reactivity, understanding reaction mechanisms, as well as controlling reaction pathways. During the past decade, X-ray transient absorption spectroscopy (XTA, or LITR-XAS, laser-initiated X-ray absorption spectroscopy), analogous to the commonly used optical transient absorption spectroscopy, has been developed. XTA uses a laser pulse to trigger a fundamental chemical process, and an X-ray pulse(s) to probe transient structures as a function of the time delay between the pump and probe pulses. Using X-ray pulses with high photon flux from synchrotron sources, transient electronic and molecular structures of metal complexes have been studied in disordered media from homogeneous solutions to heterogeneous solution-solid interfaces. Several examples from the studies at the Advanced Photon Source in Argonne National Laboratory are summarized, including excited-state metalloporphyrins, metal-to-ligand charge transfer (MLCT) states of transition metal complexes, and charge transfer states of metal complexes at the interface with semiconductor nanoparticles. Recent developments of the method are briefly described followed by a future prospective of XTA. It is envisioned that concurrent developments in X-ray free-electron lasers and synchrotron X-ray facilities as well as other table-top laser-driven femtosecond X-ray sources will make many breakthroughs and realise dreams of visualizing molecular movies and snapshots, which ultimately enable chemical reaction pathways to be controlled.

  14. Contact-free pyroelectric measurements using x-ray photoelectron spectroscopy

    SciTech Connect

    Ehre, D.; Cohen, H.

    2013-07-29

    Non-contact pyroelectricity measurements based on x-ray photoelectron spectroscopy (XPS) are presented. Applied to Lithium Tantalate crystals, we demonstrate how the XPS-derived surface potential provides a simple probe of the desired property, free of all top-contact related difficulties. In particular, the increase in Lithium Tantalate spontaneous polarization under cooling, an experimentally challenging feature, is evaluated. We further inspect the roll of surface contaminants and the control over trapped surface charge in the XPS vacuum environment. Our approach can be extended to other non-contact probes, as well as to measuring additional electrical properties, such as piezoelectricity and ferroelectricity.

  15. Biological X-ray spectroscopy on 3rd generation synchrotron radiation sources

    NASA Astrophysics Data System (ADS)

    Ralston, Corie Y.; Chen, Jie; Peng, Gang; George, Simon J.; van Elp, Jan; Cramer, Stephen P.

    1995-02-01

    Third generation synchrotron radiation sources such as the Advanced Light Source (ALS) at Lawrence Berkeley Laboratory deliver 1-2 orders of magnitude more monochromatic flux (and many orders of magnitude higher brightness) than previously available. This paper describes the ring and existing beamlines of the advanced light source, and plans for crystallography and elliptical wiggler stations are discussed. Using nickel metalloprotein spectra recorded at NSLS and SSRL as examples, this paper describes how the higher monochromatic flux available from the ALS will be used for biological soft X-ray spectroscopy.

  16. Oxidation of stepped Pt(111) studied by x-ray photoelectron spectroscopy and density functional theory

    SciTech Connect

    Bandlow, Jochen; Kaghazchi, Payam; Jacob, Timo; Papp, C.; Traenkenschuh, B.; Streber, R.; Lorenz, M. P. A.; Fuhrmann, T.; Steinrueck, H.-P.; Denecke, R.

    2011-05-01

    In this comparative density functional theory and x-ray photoelectron spectroscopy study on the interaction of oxygen with stepped Pt(111) surfaces, we show that both the initial adsorption and oxidation occur at the steps rather than terraces. An equivalent behavior was observed for the oxide formation at higher chemical potentials, where, after the formation of a one-dimensional PtO{sub 2}-type oxide at the steps, similar oxide chains form on the (111) terraces, indicating the initial stages of bulk oxide formation.

  17. FPGA-based compression of streaming x-ray photon correlation spectroscopy data

    SciTech Connect

    Madden, Timothy; Jemian, Peter; Narayanan, Surcsh; Sandy, Alec; Sikorski, Marcin; Sprung, Michael; Weizeorick, John

    2011-08-09

    A data acquisition system to perform real-time background subtraction and lower-level-discrimination-based compression of streaming x-ray photon correlation spectroscopy (XPCS) data from a fast charge-coupled device (CCD) area detector has been built and put into service at the Advanced Photon source (APS) at Argonne National Laboratory. A commercial frame grabber with on-board field-programmable gate array (FPGA) was used in the design, and continuously processes 60 frames per second each consisting of 1,024 x 1,024 pixels with up to 64512 photon hits per frame.

  18. Composition of RF-sputtered refractory compounds determined by X-ray photoelectron spectroscopy

    NASA Technical Reports Server (NTRS)

    Wheeler, D. R.; Brainard, W. A.

    1978-01-01

    RF-sputtered coatings of CrB2, MoSi2, Mo2C, TiC, and MoS2 were examined by X-ray photoelectron spectroscopy (XPS). Data on stoichiometry, impurity content, and chemical bonding were obtained. The influences of sputtering target history, deposition time, RF power level, and substrate bias were studied. Significant deviations from stoichiometry and high oxide levels were related to target outgassing. The effect of substrate bias depended on the particular coating material studied.

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

    SciTech Connect

    Hernández, Rebeca E-mail: aurora.nogales@csic.es; Mijangos, Carmen; Nogales, Aurora E-mail: aurora.nogales@csic.es; Ezquerra, Tiberio A.; Sprung, Michael

    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.

  20. Iron location in O-carboxymethyl chitosans determined by X-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Klepka, Marcin T.; Lawniczak-Jablonska, Krystyna; Wolska, Anna; Slawska-Waniewska, Anna; Rodrigues, Clóvis A.; Lorini, Josiane; Cruz, Karianne Araujo da

    2011-01-01

    Chitosans represent a class of functional natural polymers. Their unique attribute is the capability to bind metal ions into their structure. This property can be exploited in many biomedical applications, but before that, some questions about metal binding mechanism must be answered. O-carboxymethyl chitosans with accumulated Fe atoms were studied by X-ray absorption spectroscopy. It was shown that iron bonding depends on the technological processes used in chitosan production. The applied technology allows for the selective introduction of either oxygen alone or of nitrogen and oxygen into the nearest neighbourhood of Fe. Therefore, it is possible to control the surroundings of a metal atom depending on requirements.

  1. An x-ray absorption spectroscopy study of Cd binding onto a halophilic archaeon

    NASA Astrophysics Data System (ADS)

    Showalter, Allison R.; Szymanowski, Jennifer E. S.; Fein, Jeremy B.; Bunker, Bruce A.

    2016-05-01

    X-ray absorption spectroscopy (XAS) and cadmium (Cd) isotherm experiments determine how Cd adsorbs to the surface of halophilic archaeon Halobacterium noricense. This archaeon, isolated from the Waste Isolation Pilot Plant (WIPP) near Carlsbad, New Mexico could be involved with the transport of toxic metals stored in the transuranic waste in the salt mine. The isotherm experiments show that adsorption is relatively constant across the tolerable pH range for H. noricense. The XAS results indicate that Cd adsorption occurs predominately via a sulfur site, most likely sulfhydryl, with the same site dominating all measured pH values.

  2. X-ray spectroscopy of laser-heated CF2-foils

    NASA Astrophysics Data System (ADS)

    Geissel, Matthias; Bock, R.; Faenov, Anatoly Y.; Hoffmann, D. H. H.; Pikuz, Tatiana A.; Pirzadeh, P.; Rosmej, Frank B.; Rosmej, O.; Roth, M.; Seelig, Wolfgang; Suess, W.; Tauschwitz, A.

    2001-04-01

    At the Z6 experimental area of the Gsesellshaft fur Schwerionenforschung in Darmstadt experiments with the nhelix laser facility were carried out to determine the plasma parameter sch as temperature, degree of ionization and expansion dynamics for laser heated targets, which are used for the ion beam-plasma-interaction experimental series. Spatially resolved x-ray spectroscopy with spherically bent mica crystals showed well collimated jets of He- and H-like ions emerging out of the front and rear surface of the target with energies in the MeV range.

  3. Real-time compression of streaming X-ray photon correlation spectroscopy area-detector data

    NASA Astrophysics Data System (ADS)

    Madden, T.; Jemian, P.; Narayanan, S.; Sandy, A. R.; Sikorski, M.; Sprung, M.; Weizeorick, J.

    2011-09-01

    We present a data acquisition system to perform on-the-fly background subtraction and lower-level discrimination compression of streaming X-ray photon correlation spectroscopy (XPCS) data from a fast charge-coupled device area detector. The system is built using a commercial frame grabber with an on-board field-programmable gate array (FPGA). The system is capable of continuously processing 60 CCD frames per second each consisting of 1024×1024 pixels with up to 64 512 photon hits per frame.

  4. High-Resolution Spectroscopy with the Chandra X-ray Observatory

    ScienceCinema

    Canizares, Claude R. [MIT, Cambridge, Massachusetts, United States

    2016-07-12

    The capabilities of the Chandra X-ray Observatory and XMM-Newton for high-resolution spectroscopy have brought tradition plasma diagnostic techniques to the study of cosmic plasma. Observations have probed nearly every class of astronomical object, from young proto-starts through massive O starts and black hole binaries, supernova remnants, active galactic nuclei, and the intergalactic medium. Many of these sources show remarkable rich spectra that reveal new physical information, such as emission measure distributions, elemental abundances, accretion disk and wind signatures, and time variability. This talk will present an overview of the Chandra instrumentaton and selected examples of spectral observations of astrophysical and cosmological importance.

  5. Quantitative analysis of annealed scanning probe tips using energy dispersive x-ray spectroscopy

    SciTech Connect

    Cobley, R. J.; Brown, R. A.; Barnett, C. J.; Maffeis, T. G. G.; Penny, M. W.

    2013-01-14

    A quantitative method to measure the reduction in oxide species on the surface of electrochemically etched tungsten tips during direct current annealing is developed using energy dispersive x-ray spectroscopy. Oxide species are found to decrease with annealing current, with the trend repeatable over many tips and along the length of the tip apex. A linear resistivity approximation finds significant oxide sublimation occurs at 1714 K, but surface melting and tip broadening at 2215 K. This method can be applied to calibrate any similar annealing stage, and to identify the tradeoff regime between required morphological and chemical properties.

  6. X-Ray Absorption Spectroscopy of Cuprous-Thiolate Clusters in Saccharomyces Cerevisiae Metallothionein

    SciTech Connect

    Zhang, L.; Pickering, I.J.; Winge, D.R.; George, G.N.

    2009-05-28

    Copper (Cu) metallothioneins are cuprous-thiolate proteins that contain multimetallic clusters, and are thought to have dual functions of Cu storage and Cu detoxification. We have used a combination of X-ray absorption spectroscopy (XAS) and density-functional theory (DFT) to investigate the nature of Cu binding to Saccharomyces cerevisiae metallothionein. We found that the XAS of metallothionein prepared, containing a full complement of Cu, was quantitatively consistent with the crystal structure, and that reconstitution of the apo-metallothionein with stoichiometric Cu results in the formation of a tetracopper cluster, indicating cooperative binding of the Cu ions by the metallothionein.

  7. Automated system for x-ray absorption spectroscopy of nanoparticle nucleation and growth

    SciTech Connect

    Calvin, S.; Carpenter, E.E.; Cestone, V.; Kurihara, L.K.; Harris, V.G.; Brown, E.C.

    2005-01-01

    X-ray absorption spectroscopy (XAS) is a useful tool for studying nanoparticle synthesis and growth. Described here is a system for automating synthesis and data collection, allowing time-resolved XAS measurements at a synchrotron to be accurately combined with measurements made under identical conditions elsewhere, and promising the ability to use XAS with experiments in combinatorial chemistry. The primary components of this system are a commercial parallel processor and a custom flow cell. The system has been used to collect data on the synthesis of iron oxides from iron(II) acetylacetonate.

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

    NASA Astrophysics Data System (ADS)

    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.

  9. Electronic structure of individual hybrid colloid particles studied by near-edge X-ray absorption fine structure (NEXAFS) spectroscopy in the X-ray microscope.

    PubMed

    Henzler, Katja; Guttmann, Peter; Lu, Yan; Polzer, Frank; Schneider, Gerd; Ballauff, Matthias

    2013-02-13

    The electronic structure of individual hybrid particles was studied by nanoscale near-edge X-ray absorption spectromicroscopy. The colloidal particles consist of a solid polystyrene core and a cross-linked poly-N-(isopropylacrylamide) shell with embedded crystalline titanium dioxide (TiO(2)) nanoparticles (d = 6 ± 3 nm). The TiO(2) particles are generated in the carrier network by a sol-gel process at room temperature. The hybrid particles were imaged with photon energy steps of 0.1 eV in their hydrated environment with a cryo transmission X-ray microscope (TXM) at the Ti L(2,3)-edge. By analyzing the image stacks, the obtained near-edge X-ray absorption fine structure (NEXAFS) spectra of our individual hybrid particles show clearly that our synthesis generates TiO(2) in the anastase phase. Additionally, our spectromicroscopy method permits the determination of the density distribution of TiO(2) in single carrier particles. Therefore, NEXAFS spectroscopy combined with TXM presents a unique method to get in-depth insight into the electronic structure of hybrid materials. PMID:23360082

  10. Hard X-ray and gamma-ray imaging spectroscopy for the next solar maximum

    NASA Technical Reports Server (NTRS)

    Hudson, H. S.; Crannell, C. J.; Dennis, B. R.; Spicer, D. S.; Davis, J. M.; Hurford, G. J.; Lin, R. P.

    1990-01-01

    The objectives and principles are described of a single spectroscopic imaging package that can provide effective imaging in the hard X- and gamma-ray ranges. Called the High-Energy Solar Physics (HESP) mission instrument for solar investigation, the device is based on rotating modulation collimators with germanium semiconductor spectrometers. The instrument is planned to incorporate thick modulation plates, and the range of coverage is discussed. The optics permit the coverage of high-contrast hard X-ray images from small- and medium-sized flares with large signal-to-noise ratios. The detectors allow angular resolution of less than 1 arcsec, time resolution of less than 1 arcsec, and spectral resolution of about 1 keV. The HESP package is considered an effective and important instrument for investigating the high-energy solar events of the near-term future efficiently.

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

    PubMed Central

    Yano, Junko; Yachandra, Vittal K.

    2014-01-01

    Light-driven oxidation of water to dioxygen in plants, algae, and cyanobacteria is catalyzed within photosystem II (PS II) by a Mn4Ca cluster. Although the cluster has been studied by many different methods, its structure and mechanism have remained elusive. X-ray absorption and emission spectroscopy and extended X-ray absorption fine structure studies have been particularly useful in probing the electronic and geometric structures 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 set of three similar high-resolution structures. The structure of the cluster from the present study is unlike either the 3.0- or 3.5-Å-resolution X-ray structures or other previously proposed models. The differences between the models derived from X-ray spectroscopy and crystallography are predominantly because of damage to the Mn4Ca cluster by X-rays under conditions used for the 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 formal oxidation states is overly simplistic. A more accurate description should consider the charge density on the Mn atoms, which includes the covalency of the bonds and delocalization of the charge over the cluster. The geometric and electronic structures of the Mn4Ca cluster in the S states derived from X-ray spectroscopy are leading to a detailed understanding of the mechanism of O–O bond formation

  12. X-ray magnetic circular dichroism and x-ray absorption spectroscopy of novel magnetic thin films

    SciTech Connect

    Brewer, M.A.; Ju, H.L.; Krishnan, K.M.

    1997-04-01

    The optimization of the magnetic properties of materials for a wide range of applications requires a dynamic iteration between synthesis, property measurements and characterization at appropriate length scales. The authors interest arises both from the increased appreciation of the degree to which magnetic properties can be influenced by tailored microstructures and the ability to characterize them by x-ray scattering/dichroism techniques. Preliminary results of this work at the ALS on `giant` moment in {alpha}{double_prime}-Fe{sub 16}N{sub 2} and `colossal` magnetoresistance in manganite perovskites is presented here. It has recently been claimed that {alpha}{double_prime}-Fe{sub 16}N{sub 2} possesses a giant magnetization of 2.9 T ({approximately}2300 emu/cc) when grown on lattice-matched In{sub 0.2}Ga{sub 0.8}As(001) and Fe/GaAs(001). However, attempts at growth on simpler substrates have resulted in only a modest enhancement in moment and often in multiphase mixtures. Theoretical calculations based on the band structure of Fe{sub 16}N{sub 2} predict values for the magnetization around 2.3 T ({approximately}1780 emu/cc), well below Sugita`s claims, but consistent with the magnetization reported by several other workers. Using appropriate sum rules applied to the integrated MCD spectrum, they hope to determine the magnetic moment of the iron species in the {alpha}{double_prime}-Fe{sub 16}N{sub 2} films and other phases and resolve the orbital and spin contributions to the moment. There is also rapidly growing interest in the `colossal magnetoresistance` effect observed in manganese oxides for both fundamental and commercial applications. To address some of these issues the authors have measured the electron energy loss spectra (EELS) of manganese perovskites at room temperature.

  13. Imaging x-ray sources at a finite distance in coded-mask instruments.

    PubMed

    Donnarumma, Immacolata; Pacciani, Luigi; Lapshov, Igor; Evangelista, Yuri

    2008-07-01

    We present a method for the correction of beam divergence in finite distance sources imaging through coded-mask instruments. We discuss the defocusing artifacts induced by the finite distance showing two different approaches to remove such spurious effects. We applied our method to one-dimensional (1D) coded-mask systems, although it is also applicable in two-dimensional systems. We provide a detailed mathematical description of the adopted method and of the systematics introduced in the reconstructed image (e.g., the fraction of source flux collected in the reconstructed peak counts). The accuracy of this method was tested by simulating pointlike and extended sources at a finite distance with the instrumental setup of the SuperAGILE experiment, the 1D coded-mask x-ray imager onboard the AGILE (Astro-rivelatore Gamma a Immagini Leggero) mission. We obtained reconstructed images of good quality and high source location accuracy. Finally we show the results obtained by applying this method to real data collected during the calibration campaign of SuperAGILE. Our method was demonstrated to be a powerful tool to investigate the imaging response of the experiment, particularly the absorption due to the materials intercepting the line of sight of the instrument and the conversion between detector pixel and sky direction. PMID:18594598

  14. Imaging x-ray sources at a finite distance in coded-mask instruments

    SciTech Connect

    Donnarumma, Immacolata; Pacciani, Luigi; Lapshov, Igor; Evangelista, Yuri

    2008-07-01

    We present a method for the correction of beam divergence in finite distance sources imaging through coded-mask instruments. We discuss the defocusing artifacts induced by the finite distance showing two different approaches to remove such spurious effects. We applied our method to one-dimensional (1D) coded-mask systems, although it is also applicable in two-dimensional systems. We provide a detailed mathematical description of the adopted method and of the systematics introduced in the reconstructed image (e.g., the fraction of source flux collected in the reconstructed peak counts). The accuracy of this method was tested by simulating pointlike and extended sources at a finite distance with the instrumental setup of the SuperAGILE experiment, the 1D coded-mask x-ray imager onboard the AGILE (Astro-rivelatore Gamma a Immagini Leggero) mission. We obtained reconstructed images of good quality and high source location accuracy. Finally we show the results obtained by applying this method to real data collected during the calibration campaign of SuperAGILE. Our method was demonstrated to be a powerful tool to investigate the imaging response of the experiment, particularly the absorption due to the materials intercepting the line of sight of the instrument and the conversion between detector pixel and sky direction.

  15. Imaging x-ray sources at a finite distance in coded-mask instruments.

    PubMed

    Donnarumma, Immacolata; Pacciani, Luigi; Lapshov, Igor; Evangelista, Yuri

    2008-07-01

    We present a method for the correction of beam divergence in finite distance sources imaging through coded-mask instruments. We discuss the defocusing artifacts induced by the finite distance showing two different approaches to remove such spurious effects. We applied our method to one-dimensional (1D) coded-mask systems, although it is also applicable in two-dimensional systems. We provide a detailed mathematical description of the adopted method and of the systematics introduced in the reconstructed image (e.g., the fraction of source flux collected in the reconstructed peak counts). The accuracy of this method was tested by simulating pointlike and extended sources at a finite distance with the instrumental setup of the SuperAGILE experiment, the 1D coded-mask x-ray imager onboard the AGILE (Astro-rivelatore Gamma a Immagini Leggero) mission. We obtained reconstructed images of good quality and high source location accuracy. Finally we show the results obtained by applying this method to real data collected during the calibration campaign of SuperAGILE. Our method was demonstrated to be a powerful tool to investigate the imaging response of the experiment, particularly the absorption due to the materials intercepting the line of sight of the instrument and the conversion between detector pixel and sky direction.

  16. High-resolution X-ray spectroscopy of T Tauri stars in the Taurus-Auriga complex

    NASA Astrophysics Data System (ADS)

    Telleschi, A.; Güdel, M.; Briggs, K. R.; Audard, M.; Scelsi, L.

    2007-06-01

    Context: Differences have been reported between the X-ray emission of accreting and non-accreting stars. Some observations have suggested that accretion shocks could be responsible for part of the X-ray emission in classical T Tauri stars (CTTS). Aims: We present high-resolution X-ray spectroscopy for nine pre-main sequence stars in order to test the proposed spectroscopic differences between accreting and non-accreting pre-main sequence stars. Methods: We used X-ray spectroscopy from the XMM-Newton Reflection Grating Spectrometers and the EPIC instruments. We interpret the spectra using optically thin thermal models with variable abundances, together with an absorption column density. For BP Tau and AB Aur we derive electron densities from the O vii triplets. Results: Using the O vii/O viii count ratios as a diagnostic for cool plasma, we find that CTTS display a soft excess (with equivalent electron temperatures of ≈2.5{-}3 MK) when compared with WTTS or zero-age main-sequence stars. Although the O vii triplet in BP Tau is consistent with a high electron density (3.4 × 1011 cm-3), we find low density for the accreting Herbig star AB Aur (ne < 1010 cm-3). The element abundances of accreting and non-accreting stars are similar. The Ne abundance is found to be high (4-6 times the Fe abundance) in all K and M-type stars. In contrast, for the three G-type stars (SU Aur, HD 283572, and HP Tau/G2), we find an enhanced Fe abundance (0.4-0.8 times solar photospheric values) compared to later-type stars. Conclusions: Adding the results from our sample to former high-resolution studies of T Tauri stars, we find a soft excess in all accreting stars, but in none of the non-accretors. On the other hand, high electron density and high Ne/Fe abundance ratios do not seem to be present in all accreting pre-main sequence stars.

  17. On the sensitivity of hard X-ray spectroscopies to the chemical state of Br.

    PubMed

    Bordage, Amélie; Pápai, Mátyás; Sas, Norbert S; Szlachetko, Jakub; Nachtegaal, Maarten; Vankó, György

    2013-07-14

    The sensitivity of the 1s X-ray emission and high-energy-resolution fluorescence-detected X-ray absorption spectroscopies (XES and HERFD-XAS) to resolve the variations in the chemical state (electronic structure and local coordination) of Br has been investigated for a selected set of compounds including NaBrO3, NH4Br and C2H4Br2 (1,2-dibromoethane). For the Br K-edge XAS, employing the HERFD mode significantly increases the energy resolution, which demonstrates that with a crystal spectrometer used as a detector the absorption technique becomes a more powerful analytical tool. In the case of XES, the experimental results as well as the density functional theory (DFT) modeling both show that the chemical sensitivity of the main 1s diagram emission lines (Kα1,2 and Kβ1,3) is rather limited. However, the valence-to-core (Kβ2) region of XES displays significant shape and intensity variations, as expected for transitions having the same final states as those of photoemission spectroscopy. The spectra are in good agreement with the molecular orbital description delivered by DFT calculations. Calculations for an extended series of Br compounds confirm that valence-to-core XES can serve as a probe for chemical analysis, and, being a hard X-ray photon-in/photon-out technique, it is particularly well-suited for in situ investigations of molecular transformations, even on the ultrafast time scales down to femtosecond time resolution.

  18. A liquid flatjet system for solution phase soft-x-ray spectroscopy

    PubMed Central

    Ekimova, Maria; Quevedo, Wilson; Faubel, Manfred; Wernet, Philippe; Nibbering, Erik T. J.

    2015-01-01

    We present a liquid flatjet system for solution phase soft-x-ray spectroscopy. The flatjet set-up utilises the phenomenon of formation of stable liquid sheets upon collision of two identical laminar jets. Colliding the two single water jets, coming out of the nozzles with 50 μm orifices, under an impact angle of 48° leads to double sheet formation, of which the first sheet is 4.6 mm long and 1.0 mm wide. The liquid flatjet operates fully functional under vacuum conditions (<10−3 mbar), allowing soft-x-ray spectroscopy of aqueous solutions in transmission mode. We analyse the liquid water flatjet thickness under atmospheric pressure using interferomeric or mid-infrared transmission measurements and under vacuum conditions by measuring the absorbance of the O K-edge of water in transmission, and comparing our results with previously published data obtained with standing cells with Si3N4 membrane windows. The thickness of the first liquid sheet is found to vary between 1.4–3 μm, depending on the transverse and longitudinal position in the liquid sheet. We observe that the derived thickness is of similar magnitude under 1 bar and under vacuum conditions. A catcher unit facilitates the recycling of the solutions, allowing measurements on small sample volumes (∼10 ml). We demonstrate the applicability of this approach by presenting measurements on the N K-edge of aqueous NH4+. Our results suggest the high potential of using liquid flatjets in steady-state and time-resolved studies in the soft-x-ray regime. PMID:26798824

  19. Some results from the exploration of the solar atmosphere with high-resolution x-ray-EUV spectroscopy at the Naval Research Laboratory.

    PubMed

    Doschek, G A

    2015-11-01

    The Naval Research Laboratory has been one of the world leaders in high-resolution UV-x-ray solar spectroscopy. Much has been learned about the morphology and physical conditions in the atmosphere from spectroscopic instrumentation flown on orbiting spacecraft. In this short summary I discuss the solar atmosphere and our current knowledge of it, and show some of the results obtained by spectroscopic investigations at the Naval Research Laboratory. PMID:26560622

  20. Three-Dimensional Electron Realm in VSe2 by Soft-X-Ray Photoelectron Spectroscopy: Origin of Charge-Density Waves

    NASA Astrophysics Data System (ADS)

    Strocov, Vladimir N.; Shi, Ming; Kobayashi, Masaki; Monney, Claude; Wang, Xiaoqiang; Krempasky, Juraj; Schmitt, Thorsten; Patthey, Luc; Berger, Helmuth; Blaha, Peter

    2012-08-01

    The resolution of angle-resolved photoelectron spectroscopy (ARPES) in three-dimensional (3D) momentum k is fundamentally limited by ill defined surface-perpendicular wave vector k⊥ associated with the finite photoelectron mean free path. Pushing ARPES into the soft-x-ray energy region sharpens the k⊥ definition, allowing accurate electronic structure investigations in 3D materials. We apply soft-x-ray ARPES to explore the 3D electron realm in a paradigm transition metal dichalcogenide VSe2. Essential to break through the dramatic loss of the valence band photoexcitation cross section at soft-x-ray energies is the advanced photon flux performance of our synchrotron instrumentation. By virtue of the sharp 3D momentum definition, the soft-x-ray ARPES experimental band structure and Fermi surface of VSe2 show a textbook clarity. We identify pronounced 3D warping of the Fermi surface and show that its concomitant nesting acts as the precursor for the exotic 3D charge-density waves in VSe2. Our results demonstrate the immense potential of soft-x-ray ARPES to explore details of 3D electronic structure.

  1. Study of air-induced paper discolorations by infrared spectroscopy, X-ray fluorescence, and scanning electron microscopy.

    PubMed

    Ferreira, Adriana; Figueira, Francisca; Pessanha, Sofia; Nielsen, Ingelise; Carvalho, Maria Luisa

    2010-02-01

    Air-induced paper discoloration is described as being different from other discoloration morphologies. It seems to be the result of prolonged exposure to air in a humid and polluted environment without appropriate protecting coverage. In this work, three folios from the same eighteenth century book, presenting three degrees of discoloration and opacity and subjected to different environmental conditions, were examined and compared. Samples were analyzed and compared by three different instrumental techniques, mid-infrared spectroscopy, X-ray fluorescence (XRF), and scanning electron microscopy (SEM). Chemical and physical changes were confirmed from the data collected by these techniques. The absence of the secondary amide band characteristic of proteins in the infrared spectra of the two discolored folios, accompanied by the appearance and increase of white mineral-like deposits visible in the SEM micrographs, support the idea that oxidation reactions occurred and that these two folios were subjected to more severe degradation hazard. PMID:20149275

  2. Measurement of c-axis angular orientation in calcite (CaCO3) nanocrystals using X-ray absorption spectroscopy

    PubMed Central

    Gilbert, P. U. P. A.; Young, Anthony; Coppersmith, Susan N.

    2011-01-01

    We demonstrate that the ability to manipulate the polarization of synchrotron radiation can be exploited to enhance the capabilities of X-ray absorption near-edge structure (XANES) spectroscopy, to include linear dichroism effects. By acquiring spectra at the same photon energies but different polarizations, and using a photoelectron emission spectromicroscope (PEEM), one can quantitatively determine the angular orientation of micro- and nanocrystals with a spatial resolution down to 10 nm. XANES-PEEM instruments are already present at most synchrotrons, hence these methods are readily available. The methods are demonstrated here on geologic calcite (CaCO3) and used to investigate the prismatic layer of a mollusk shell, Pinctada fucata. These XANES-PEEM data reveal multiply oriented nanocrystals within calcite prisms, previously thought to be monocrystalline. The subdivision into multiply oriented nanocrystals, spread by more than 50°, may explain the excellent mechanical properties of the prismatic layer, known for decades but never explained. PMID:21693647

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

    NASA Technical Reports Server (NTRS)

    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.

  4. Science with XEUS: the X-Ray Evolving Universe Spectroscopy mission

    NASA Astrophysics Data System (ADS)

    Parmar, Arvind N.; Arnaud, Monique; Barcons, Xavier; Bleeker, Johan M.; Hasinger, Guenther; Inoue, Hajime; Palumbo, Giorgio; Turner, Martin J. L.

    2004-10-01

    XEUS is the potential successor to ESA's XMM-Newton X-ray observatory. Novel light-weight optics with an effective area of 10 m2 at 1 keV and 2-5 HEW spatial resolution together with advanced imaging detectors will provide a sensitivity around 200 times better than XMM-Newton as well as much improved high-energy coverage, and spectroscopic performance. This enormous improvement in scientific capability will open up new vistas in X-ray astronomy. It will allow the detection of massive black holes in the earliest AGN and estimates of their mass, spin and red-shift through their Fe-K line properties. XEUS will study the first gravitationally bound, Dark Matter dominated, systems small groups of galaxies and trace their evolution into today's massive clusters. High-resolution spectroscopy of the hot intra-cluster gas will be used to investigate the evolution of metal synthesis to the present epoch. The hot filamentary structure will be studied using absorption line spectroscopy allowing the mass, temperature and density of the intergalactic medium to be characterized. As well as these studies of the deep universe, the enormous low-energy collecting area will provide a unique capability to investigate bright nearby objects with dedicated high-throughput, polarimetric and time resolution detectors.

  5. Impact of Oriented Clay Particles on X-Ray Spectroscopy Analysis

    NASA Astrophysics Data System (ADS)

    Lim, A. J. M. S.; Syazwani, R. N.; Wijeyesekera, D. C.

    2016-07-01

    Understanding the engineering properties of the mineralogy and microfabic of clayey soils is very complex and thus very difficult for soil characterization. Micromechanics of soils recognize that the micro structure and mineralogy of clay have a significant influence on its engineering behaviour. To achieve a more reliable quantitative evaluation of clay mineralogy, a proper sample preparation technique for quantitative clay mineral analysis is necessary. This paper presents the quantitative evaluation of elemental analysis and chemical characterization of oriented and random oriented clay particles using X-ray spectroscopy. Three different types of clays namely marine clay, bentonite and kaolin clay were studied. The oriented samples were prepared by placing the dispersed clay in water and left to settle on porous ceramic tiles by applying a relatively weak suction through a vacuum pump. Images form a Scanning Electron Microscope (SEM) was also used to show the comparison between the orientation patterns of both the sample preparation techniques. From the quantitative analysis of the X-ray spectroscopy, oriented sampling method showed more accuracy in identifying mineral deposits, because it produced better peak intensity on the spectrum and more mineral content can be identified compared to randomly oriented samples.

  6. X-ray photoelectron spectroscopy characterization of the {omega} phase in water quenched Ti-5553 alloy

    SciTech Connect

    Qin, Dongyang; Lu, Yafeng; Zhang, Kong; Liu, Qian; Zhou, Lian

    2012-11-15

    X-ray photoelectron spectroscopy was used to investigate the {omega} phase in water quenched Ti-5553 alloy with a nominal composition of Ti-5Al-5V-5Mo-3Cr (wt.%), and the {omega} and the {beta} phase were distinguished by deconvoluting the XPS spectra of Al2p, V2p and Cr2p core level regions. In addition, it is found that the binding energy of core level electron of alloying elements shifts comparing with that of pure metals, and the fact was interpreted by charge redistribution model. X-ray photoelectron spectroscopy technique could be used to characterize the nano-scale {omega} phase in {beta} alloys. - Highlights: Black-Right-Pointing-Pointer We characterize the {omega} phase in Ti-5553 alloy by XPS. Black-Right-Pointing-Pointer Binding energy of Al2p, V2p and Cr2p electron are different in the {omega} and {beta} phase. Black-Right-Pointing-Pointer Structural difference leads to the binding energy gap.

  7. Near-Edge X-ray Absorption Fine Structure Spectroscopy of Diamondoid Thiol Monolayers on Gold

    SciTech Connect

    Willey, T M; Fabbri, J; Lee, J I; Schreiner, P; Fokin, A A; Tkachenko, B A; Fokina, N A; Dahl, J; Carlson, B; Vance, A L; Yang, W; Terminello, L J; van Buuren, T; Melosh, N

    2007-11-27

    Diamondoids, hydrocarbon molecules with cubic-diamond-cage structures, have unique properties with potential value for nanotechnology. The availability and ability to selectively functionalize this special class of nanodiamond materials opens new possibilities for surface-modification, for high-efficiency field emitters in molecular electronics, as seed crystals for diamond growth, or as robust mechanical coatings. The properties of self-assembled monolayers (SAMs) of diamondoids are thus of fundamental interest for a variety of emerging applications. This paper presents the effects of thiol substitution position and polymantane order on diamondoid SAMs on gold using near-edge X-ray absorption fine structure spectroscopy (NEXAFS) and X-ray photoelectron spectroscopy (XPS). A framework to determine both molecular tilt and twist through NEXAFS is presented and reveals highly ordered diamondoid SAMs, with the molecular orientation controlled by the thiol location. C 1s and S 2p binding energies are lower in adamantane thiol than alkane thiols on gold by 0.67 {+-} 0.05 eV and 0.16 {+-} 0.04 eV respectively. These binding energies vary with diamondoid monolayer structure and thiol substitution position, consistent with different amounts of steric strain and electronic interaction with the substrate. This work demonstrates control over the assembly, in particular the orientational and electronic structure, providing a flexible design of surface properties with this exciting new class of diamond clusters.

  8. X-ray absorption spectroscopy on magnetic nanoscale systems for modern applications

    NASA Astrophysics Data System (ADS)

    Schmitz-Antoniak, Carolin

    2015-06-01

    X-ray absorption spectroscopy facilitated by state-of-the-art synchrotron radiation technology is presented as a powerful tool to study nanoscale systems, in particular revealing their static element-specific magnetic and electronic properties on a microscopic level. A survey is given on the properties of nanoparticles, nanocomposites and thin films covering a broad range of possible applications. It ranges from the ageing effects of iron oxide nanoparticles in dispersion for biomedical applications to the characterisation on a microscopic level of nanoscale systems for data storage devices. In this respect, new concepts for electrically addressable magnetic data storage devices are highlighted by characterising the coupling in a BaTiO3/CoFe2O4 nanocomposite as prototypical model system. But classical magnetically addressable devices are also discussed on the basis of tailoring the magnetic properties of self-assembled ensembles of FePt nanoparticles for data storage and the high-moment material Fe/Cr/Gd for write heads. For the latter cases, the importance is emphasised of combining experimental approaches in x-ray absorption spectroscopy with density functional theory to gain a more fundamental understanding.

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

    PubMed

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

    2016-11-01

    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. PMID:27262277

  10. Measuring surface and grain boundary segregation using wavelength dispersive X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Christien, F.; Le Gall, R.

    2008-07-01

    Electron probe microanalysis (EPMA) using wavelength dispersive X-ray spectroscopy (EPMA-WDS) is applied to the quantification of surface and grain boundary monolayer segregation. The case of sulphur segregation in nickel and nickel alloys is considered. It is evidenced that EPMA-WDS is able to detect submonolayer surface segregation. The sulphur segregation can be accurately quantified from the sulphur Kα line relative intensity (ratio of the intensity measured on the sample and the intensity measured on a standard material) using the Stratagem™ software (analytical modelling of the X-ray emission in a stratified specimen based on the PhiRoZ model). The statistical accuracy of the technique and its detection limit are estimated to be as low as a few percents of a monolayer for reasonable counting times (˜ a few minutes). The advantages and drawbacks of EPMA-WDS with respect to Auger electron spectroscopy (AES) are discussed. The main advantage of EMPA-WDS is that it is almost insensitive to surface contamination and oxidation, which makes it possible to measure surface segregation on samples that have been in contact with atmosphere. The influence of specimen tilt is also discussed. The technique is also applied to the measurement of sulphur segregation on the fracture surface of an iron-nickel alloy sample broken at high temperature. It is thus demonstrated that EPMA-WDS could be a very useful tool for failure analysis in the case of grain boundary fractures.

  11. X-ray emission and photoluminescence spectroscopy of nanostructured silica with implanted copper ions

    NASA Astrophysics Data System (ADS)

    Zatsepin, D. A.; Kortov, V. S.; Kurmaev, É. Z.; Gavrilov, N. V.; Wilks, R. G.; Moewes, A.

    2008-12-01

    Quartz glass samples and compacted SiO2 nanopowders have been studied by x-ray emission (Cu L 2, 3 transition 3 d4 s → 2 p 1/2, 3/2) and photoluminescence spectroscopy following pulsed Cu+ ion implantation (energy, 30 keV; pulse current up to 0.5 A; pulse duration, 400 μs; irradiation doses, 1015, 1016, and 2 × 1017 cm-2). It has been established that ion irradiation gives rise to the formation of glassy and compacted SiO2 samples of nanosized metallic and oxide phases in the structure. An analysis of Cu L x-ray emission spectra has shown that copper nanoparticles are thermodynamically metastable and chemically active because ion beam bombardment transfers them readily to the oxide form. This results from the radiation-stimulated fracture of regular Si-O-Si bonds in amorphous SiO2 and the formation of defective Si-Si bonds, followed by capture of oxygen by copper atoms. The enhanced degree of oxidation of copper ions in SiO2 nanostructured pellets can be reduced by coimplantation and thermal annealing. Optical spectroscopy studies suggest that, in glasses and SiO2 nanostructured pellets, there exist metallic Cu{/n 0} nanoclusters, which at low temperatures exhibit quantum-confined photoluminescence with a characteristic stepped excitation spectrum.

  12. Evolution of Silver Nanoparticles in the Rat Lung Investigated by X-ray Absorption Spectroscopy

    PubMed Central

    2015-01-01

    Following a 6-h inhalation exposure to aerosolized 20 and 110 nm diameter silver nanoparticles, lung tissues from rats were investigated with X-ray absorption spectroscopy, which can identify the chemical state of silver species. Lung tissues were processed immediately after sacrifice of the animals at 0, 1, 3, and 7 days post exposure and the samples were stored in an inert and low-temperature environment until measured. We found that it is critical to follow a proper processing, storage and measurement protocol; otherwise only silver oxides are detected after inhalation even for the larger nanoparticles. The results of X-ray absorption spectroscopy measurements taken in air at 85 K suggest that the dominating silver species in all the postexposure lung tissues were metallic silver, not silver oxide, or solvated silver cations. The results further indicate that the silver nanoparticles in the tissues were transformed from the original nanoparticles to other forms of metallic silver nanomaterials and the rate of this transformation depended on the size of the original nanoparticles. We found that 20 nm diameter silver nanoparticles were significantly modified after aerosolization and 6-h inhalation/deposition, whereas larger, 110 nm diameter nanoparticles were largely unchanged. Over the seven-day postexposure period the smaller 20 nm silver nanoparticles underwent less change in the lung tissue than the larger 110 nm silver nanoparticles. In contrast, silica-coated gold nanoparticles did not undergo any modification processes and remained as the initial nanoparticles throughout the 7-day study period. PMID:25517690

  13. Soft X-Ray Spectroscopy of Glycyl-Glycine Adsorbed on Cu(110) Surface

    NASA Astrophysics Data System (ADS)

    Feyer, V.; Plekan, O.; Lyamayev, V.; Skala, T.; Prince, K. C.; Chab, V.; Tsud, N.; Matolin, V.; Carravetta, V.

    2010-06-01

    Studies of the interaction between organic compounds and surfaces are motivated by their application as bio sensors, and their relevance to biocompatibility of implants and the origin of life. In the present work interaction of the simplest peptide, glycyl-glycine, with the Cu surface has been studied. Multilayer, monolayer and sub-monolayer films of this dipeptide on the clean and oxygen modified Cu(110) surface were prepared by thermal evaporation in high vacuum. The techniques used were soft X-ray photoelectron spectroscopy, near edge X-ray absorption fine structure spectroscopy and density functional theory calculations. By comparing the experimental and theoretical spectra, detailed models of the electronic structure and adsorption geometry for each coverage have been proposed, which are in good agreement with the theoretical calculations. The carboxylic acid group of glycyl-glycine loses hydrogen and the molecule is coordinated via the carboxylate oxygen atoms to the surface. At low coverage the amino group bonds to the surface via a hydrogen atom, while at higher coverage the bonding is via the nitrogen lone pair. The peptide group is not involved in the bonding to the surface.

  14. Core and valence excitations in resonant X-ray spectroscopy using restricted excitation window time-dependent density functional theory

    PubMed Central

    Zhang, Yu; Biggs, Jason D.; Healion, Daniel; Govind, Niranjan; Mukamel, Shaul

    2012-01-01

    We report simulations of X-ray absorption near edge structure (XANES), resonant inelastic X-ray scattering (RIXS) and 1D stimulated X-ray Raman spectroscopy (SXRS) signals of cysteine at the oxygen, nitrogen, and sulfur K and \\documentclass[12pt]{minimal}\\begin{document}$\\textrm {L}_{2,3}$\\end{document}L2,3 edges. Comparison of the simulated XANES signals with experiment shows that the restricted window time-dependent density functional theory is more accurate and computationally less expensive than the static exchange method. Simulated RIXS and 1D SXRS signals give some insights into the correlation of different excitations in the molecule. PMID:23181305

  15. Core and Valence Excitations in Resonant X-ray Spectroscopy using Restricted Excitation Window Time-dependent Density Functional Theory

    SciTech Connect

    Zhang, Yu; Biggs, Jason D.; Healion, Daniel; Govind, Niranjan; Mukamel, Shaul

    2012-11-21

    We report simulations of X-ray absorption near edge structure (XANES), resonant inelastic X-ray scattering (RIXS) and 1D stimulated X-ray Raman spectroscopy (SXRS) signals of cysteine at the oxygen, nitrogen and sulfur K and L2,3 edges. The simulated XANES signals from the restricted window time-dependent density functional theory (REW-TDDFT) and the static exchange (STEX) method are compared with experiments, showing that REW-TDDFT is more accurate and computationally less expensive than STEX. Simulated RIXS and 1D SXRS signals from REW-TDDFT give some insights on the correlation of different excitations in the molecule.

  16. Quantitative spectroscopy of x-ray lines and continua in Tokamaks

    SciTech Connect

    Peacock, N.J.; Barnsley, R.; Lawson, K.D.; Melnick, I.M.; OMullane, M.G.; Singleton, M.A.; Patel, A.

    1997-04-01

    Crystal and synthetic multilayer diffractors, deployed either as flat Bragg reflectors, or curved, as in the Johann configuration, are used to study the spectrum of COMPASS-D and other tokamaks in the wavelength region of 1{endash}100 {Angstrom}. In this article, we concentrate on the measurement of absolute photon fluxes and the derivation of volume emissivities of the lines and continua in the x-ray region. The sensitivities of these instruments to absolute photon flux have been constructed {ital ab initio} from the individual component efficiencies, including published values of the diffractor reflectivities, which have been checked or supplemented by measurements using a double-axis goniometer or from line branching ratios. For those tokamak plasmas, where the elemental abundances and effective ion charge are documented, the x-ray continuum intensity itself has been used as a calibration source to derive absolute instrument sensitivity, in reasonable agreement with the {ital ab initio} method. In the COMPASS-D Tokamak, changes in the effective ion charge state, {ital Z}{sub eff}, have been derived for different operating conditions, from the absolute intensity of the continuum at {approximately}4 {Angstrom}. From the radiances of the line emission, changes in the absolute level of impurities following {open_quotes}boronization{close_quotes} of the vacuum vessel have also been documented. {copyright} {ital 1997 American Institute of Physics.}

  17. Electronic structure measurements of metal-organic solar cell dyes using x-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Johnson, Phillip S.

    The focus of this thesis is twofold: to report the results of X-ray absorption studies of metal-organic dye molecules for dye-sensitized solar cells and to provide a basic training manual on X-ray absorption spectroscopy techniques and data analysis. The purpose of our research on solar cell dyes is to work toward an understanding of the factors influencing the electronic structure of the dye: the choice of the metal, its oxidation state, ligands, and cage structure. First we study the effect of replacing Ru in several common dye structures by Fe. First-principles calculations and X-ray absorption spectroscopy at the C 1s and N 1s edges are combined to investigate transition metal dyes in octahedral and square planar N cages. Octahedral molecules are found to have a downward shift in the N 1s-to-pi* transition energy and an upward shift in C 1s-to-pi* transition energy when Ru is replaced by Fe, explained by an extra transfer of negative charge from Fe to the N ligands compared to Ru. For the square planar molecules, the behavior is more complex because of the influence of axial ligands and oxidation state. Next the crystal field parameters for a series of phthalocyanine and porphyrins dyes are systematically determined using density functional calculations and atomic multiplet calculations with polarization-dependent X-ray absorption spectra. The polarization dependence of the spectra provides information on orbital symmetries which ensures the determination of the crystal field parameters is unique. A uniform downward scaling of the calculated crystal field parameters by 5-30% is found to be necessary to best fit the spectra. This work is a part of the ongoing effort to design and test new solar cell dyes. Replacing the rare metal Ru with abundant metals like Fe would be a significant advance for dye-sensitized solar cells. Understanding the effects of changing the metal centers in these dyes in terms of optical absorption, charge transfer, and electronic

  18. Micro-x-ray fluorescence, micro-x-ray absorption spectroscopy, and micro-x-ray diffraction investigation of lead speciation after the addition of different phosphorus amendments to a smelter-contaminated soil.

    PubMed

    Baker, Lucas R; Pierzynski, Gary M; Hettiarachchi, Ganga M; Scheckel, Kirk G; Newville, Matthew

    2014-03-01

    The stabilization of Pb on additions of P to contaminated soils and mine spoil materials has been well documented. It is clear from the literature that different P sources result in different efficacies of Pb stabilization in the same contaminated material. We hypothesized that the differences in the efficacy of Pb stabilization in contaminated soils on fluid or granular P amendment addition is due to different P reaction processes in and around fertilizer granules and fluid droplets. We used a combination of several synchrotron-based techniques (i.e., spatially resolved micro-X-ray fluorescence, micro-X-ray absorption near-edge structure spectroscopy, and micro-X-ray diffraction) to speciate Pb at two incubation times in a smelter-contaminated soil on addition of several fluid and granular P amendments. The results indicated that the Pb phosphate mineral plumbogummite was an intermediate phase of pyromorphite formation. Additionally, all fluid and granular P sources were able to induce Pb phosphate formation, but fluid phosphoric acid (PA) was the most effective with time and distance from the treatment. Granular phosphate rock and triple super phosphate (TSP) amendments reacted to generate Pb phosphate minerals, with TSP being more effective at greater distances from the point of application. As a result, PA and TSP were the most effective P amendments at inducing Pb phosphate formation, but caution needs to be exercised when adding large amounts of soluble P to the environment.

  19. Energy Dispersive X-Ray and Electrochemical Impedance Spectroscopies for Performance and Corrosion Analysis of PEMWEs

    NASA Astrophysics Data System (ADS)

    Steen, S. M., Iii; Zhang, F.-Y.

    2014-11-01

    Proton exchange membrane water electrolyzers (PEMWEs) are a promising energy storage technology due to their high efficiency, compact design, and ability to be used in a renewable energy system. Before they are able to make a large commercial impact, there are several hurdles facing the technology today. Two powerful techniques for both in-situ and ex- situ characterizations to improve upon their performance and better understand their corrosion are electrochemical impedance spectroscopy and energy dispersive x-ray spectroscopy, respectively. In this paper, the authors use both methods in order to characterize the anode gas diffusion layer (GDL) in a PEMWE cell and better understand the corrosion that occurs in the oxygen electrode during electrolysis.

  20. Uses of Auger and x ray photoelectron spectroscopy in the study of adhesion and friction

    NASA Technical Reports Server (NTRS)

    Miyoshi, Kazuhisa

    1990-01-01

    Three studies are described characterizing the possible contributions of surface science to tribology. These include surface contamination formed by the interaction of a surface with the environment, contaminants obtained with diffusion of compounds, and surface chemical changes resulting from selective thermal evaporation. Surface analytical tools such as Auger electron spectroscopy (AES) and x ray photoelectron spectroscopy (XPS) incorporated directly into adhesion and friction systems are primarily used to define the nature of tribological surfaces before and after tribological experimentation and to characterize the mechanism of solid-to-solid interaction. Emphasis is on fundamental studies involving the role of surfaces in controlling the adhesion and friction properties of materials emerging as a result of the surface analyses. The materials which were studied include metals and ceramics such as elemental metals, amorphous alloys (metallic glasses), and silicon-based ceramics.

  1. Development of intelligent control system for X-ray streak camera in diagnostic instrument manipulator

    NASA Astrophysics Data System (ADS)

    Pei, Chengquan; Wu, Shengli; Tian, Jinshou; Liu, Zhen; Fang, Yuman; Gao, Guilong; Liang, Lingliang; Wen, Wenlong

    2015-11-01

    An intelligent control system for an X ray streak camera in a diagnostic instrument manipulator (DIM) is proposed and implemented, which can control time delay, electric focusing, image gain adjustment, switch of sweep voltage, acquiring environment parameters etc. The system consists of 16 A/D converters and 16 D/A converters, a 32-channel general purpose input/output (GPIO) and two sensors. An isolated DC/DC converter with multi-outputs and a single mode fiber were adopted to reduce the interference generated by the common ground among the A/D, D/A and I/O. The software was designed using graphical programming language and can remotely access the corresponding instrument from a website. The entire intelligent control system can acquire the desirable data at a speed of 30 Mb/s and store it for later analysis. The intelligent system was implemented on a streak camera in a DIM and it shows a temporal resolution of 11.25 ps, spatial distortion of less than 10% and dynamic range of 279:1. The intelligent control system has been successfully used in a streak camera to verify the synchronization of multi-channel laser on the Inertial Confinement Fusion Facility.

  2. Atmospheric Electron-induced X-Ray Spectrometer (AEXS) Instrument Development

    NASA Technical Reports Server (NTRS)

    Urgiles, E.; Wilcox, J. Z.; Toda, R.; Crisp, J.; George, T.

    2005-01-01

    Introduction: This paper describes the progress in data acquisition and establishing the observational capability of the AEXS instrument. The AEXS is a miniature instrument[1-4] based on the excitation of characteristic X-Ray Fluorescence (XRF) and luminescence spectra using a focused electron beam which enables nondestructive evaluation of sample surfaces in planetary ambient atmospheres. In situ operation is obtained through the use of a thin electron transmissive membrane to isolate the vacuum of the AEXS source from the outside ambient atmosphere. Thus eliminating the need for a vacuum pumped sample chamber as is common in all laboratory SEM s. The transmitted electrons impinge on the sample exciting XRF spectra from the irradiated spot on in-situ or collected samples with sub-mm to cm-scale spatial resolution at Mars atmospheric pressure. The AEXS system (Fig 1) consists of a high-energy (>10keV) electron gun encapsulated by the isolation membrane, an XRF detection and analyzer system, and a high voltage power supply. The XRF data are analyzed to determine the elemental abundance for the irradiated spots. The approach to demonstrating a proof of concept of the AEXS has been through 1) demonstrating the viability of microfabricated membranes, 2) assembling AEXS setups with increasingly integrated functional components, and 3) simulating the AEXS observational capabilities. The development of the instrument is described in detail in the poster paper[4] at this conference. This paper focuses on describing the progress of the AEXS instrument to acquire XRF data and using commercially available software to analyze the data streams and determine the accuracy, precision and resolution of the analysis compared to the certified elemental abundance.

  3. Characterization of metalloproteins by high-throughput X-ray absorption spectroscopy.

    PubMed

    Shi, Wuxian; Punta, Marco; Bohon, Jen; Sauder, J Michael; D'Mello, Rhijuta; Sullivan, Mike; Toomey, John; Abel, Don; Lippi, Marco; Passerini, Andrea; Frasconi, Paolo; Burley, Stephen K; Rost, Burkhard; Chance, Mark R

    2011-06-01

    High-throughput X-ray absorption spectroscopy was used to measure transition metal content based on quantitative detection of X-ray fluorescence signals for 3879 purified proteins from several hundred different protein families generated by the New York SGX Research Center for Structural Genomics. Approximately 9% of the proteins analyzed showed the presence of transition metal atoms (Zn, Cu, Ni, Co, Fe, or Mn) in stoichiometric amounts. The method is highly automated and highly reliable based on comparison of the results to crystal structure data derived from the same protein set. To leverage the experimental metalloprotein annotations, we used a sequence-based de novo prediction method, MetalDetector, to identify Cys and His residues that bind to transition metals for the redundancy reduced subset of 2411 sequences sharing <70% sequence identity and having at least one His or Cys. As the HT-XAS identifies metal type and protein binding, while the bioinformatics analysis identifies metal- binding residues, the results were combined to identify putative metal-binding sites in the proteins and their associated families. We explored the combination of this data with homology models to generate detailed structure models of metal-binding sites for representative proteins. Finally, we used extended X-ray absorption fine structure data from two of the purified Zn metalloproteins to validate predicted metalloprotein binding site structures. This combination of experimental and bioinformatics approaches provides comprehensive active site analysis on the genome scale for metalloproteins as a class, revealing new insights into metalloprotein structure and function.

  4. Characterization of Metalloproteins by High-throughput X-ray Absorption Spectroscopy

    SciTech Connect

    W Shi; M Punta; J Bohon; J Sauder; R DMello; M Sullivan; J Toomey; D Abel; M Lippi; et al.

    2011-12-31

    High-throughput X-ray absorption spectroscopy was used to measure transition metal content based on quantitative detection of X-ray fluorescence signals for 3879 purified proteins from several hundred different protein families generated by the New York SGX Research Center for Structural Genomics. Approximately 9% of the proteins analyzed showed the presence of transition metal atoms (Zn, Cu, Ni, Co, Fe, or Mn) in stoichiometric amounts. The method is highly automated and highly reliable based on comparison of the results to crystal structure data derived from the same protein set. To leverage the experimental metalloprotein annotations, we used a sequence-based de novo prediction method, MetalDetector, to identify Cys and His residues that bind to transition metals for the redundancy reduced subset of 2411 sequences sharing <70% sequence identity and having at least one His or Cys. As the HT-XAS identifies metal type and protein binding, while the bioinformatics analysis identifies metal-binding residues, the results were combined to identify putative metal-binding sites in the proteins and their associated families. We explored the combination of this data with homology models to generate detailed structure models of metal-binding sites for representative proteins. Finally, we used extended X-ray absorption fine structure data from two of the purified Zn metalloproteins to validate predicted metalloprotein binding site structures. This combination of experimental and bioinformatics approaches provides comprehensive active site analysis on the genome scale for metalloproteins as a class, revealing new insights into metalloprotein structure and function.

  5. Characterization and speciation of mercury-bearing mine wastes using X-ray absorption spectroscopy

    USGS Publications Warehouse

    Kim, C.S.; Brown, Gordon E.; Rytuba, J.J.

    2000-01-01

    Mining of mercury deposits located in the California Coast Range has resulted in the release of mercury to the local environment and water supplies. The solubility, transport, and potential bioavailability of mercury are controlled by its chemical speciation, which can be directly determined for samples with total mercury concentrations greater than 100 mg kg-1 (ppm) using X-ray absorption spectroscopy (XAS). This technique has the additional benefits of being non-destructive to the sample, element-specific, relatively sensitive at low concentrations, and requiring minimal sample preparation. In this study, Hg L(III)-edge extended X-ray absorption fine structure (EXAFS) spectra were collected for several mercury mine tailings (calcines) in the California Coast Range. Total mercury concentrations of samples analyzed ranged from 230 to 1060 ppm. Speciation data (mercury phases present and relative abundances) were obtained by comparing the spectra from heterogeneous, roasted (calcined) mine tailings samples with a spectral database of mercury minerals and sorbed mercury complexes. Speciation analyses were also conducted on known mixtures of pure mercury minerals in order to assess the quantitative accuracy of the technique. While some calcine samples were found to consist exclusively of mercuric sulfide, others contain additional, more soluble mercury phases, indicating a greater potential for the release of mercury into solution. Also, a correlation was observed between samples from hot-spring mercury deposits, in which chloride levels are elevated, and the presence of mercury-chloride species as detected by the speciation analysis. The speciation results demonstrate the ability of XAS to identify multiple mercury phases in a heterogeneous sample, with a quantitative accuracy of ??25% for the mercury-containing phases considered. Use of this technique, in conjunction with standard microanalytical techniques such as X-ray diffraction and electron probe microanalysis

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

    SciTech Connect

    Lawniczak-Jablonska, K. |; Jia, J.J.; Underwood, J.H.

    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.

  7. Testing the theory of colliding winds: the periastron passage of 9 Sagittarii. I. X-ray and optical spectroscopy

    NASA Astrophysics Data System (ADS)

    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

  8. The design and application of an in-laboratory diffraction-enhanced x-ray imaging instrument

    SciTech Connect

    Nesch, Ivan; Fogarty, Daniel P.; Tzvetkov, Tochko; Reinhart, Benjamin; Walus, A. Charles; Khelashvili, Gocha; Muehleman, Carol; Chapman, Dean

    2009-09-15

    We describe the design and application of a new in-laboratory diffraction-enhanced x-ray imaging (DEXI) instrument that uses a nonsynchrotron, conventional x-ray source to image the internal structure of an object. In the work presented here, a human cadaveric thumb is used as a test-sample to demonstrate the imaging capability of our instrument. A 22 keV monochromatic x-ray beam is prepared using a mismatched, two-crystal monochromator; a silicon analyzer crystal is placed in a parallel crystal geometry with the monochromator allowing both diffraction-enhanced imaging and multiple-imaging radiography to be performed. The DEXI instrument was found to have an experimentally determined spatial resolution of 160{+-}7 {mu}m in the horizontal direction and 153{+-}7 {mu}m in the vertical direction. As applied to biomedical imaging, the DEXI instrument can detect soft tissues, such as tendons and other connective tissues, that are normally difficult or impossible to image via conventional x-ray techniques.

  9. X-ray absorption spectroscopy of lithium sulfur battery reaction intermediates

    NASA Astrophysics Data System (ADS)

    Wujcik, Kevin; Pascal, Tod; Prendergast, David; Balsara, Nitash

    2015-03-01

    Lithium sulfur batteries have a theoretical energy density nearly five times greater than current lithium ion battery standards, but questions still remain regarding the reaction pathways through which soluble lithium polysulfide (Li2Sx, ``x'' ranging from 2 to 8) reaction intermediates are formed. Complicating spectroelectrochemical approaches to elucidate redox pathways is the challenge of obtaining spectral standards for individual Li2Sx species. Lithium polysulfides cannot be isolated as individual component and exist only in solution as a distribution of different Li2Sx molecules formed via disproportionation reactions (e.g. 2Li2S4 goes to Li2S3 + Li2S5). X-ray absorption spectroscopy (XAS) at the sulfur K-edge has recently been employed as a technique to study Li-S chemistry. We have recently obtained XAS standards for individual Li2Sx species via first principles DFT simulations and the excited electron and core hole approach. Here, experimental sulfur K-edge XAS of Li2Sx species dissolved in poly(ethylene oxide) are compared to spectra obtained from analogous theoretical calculations. The impact that polysulfide solution concentration and the presence of other lithium salts (e.g. LiNO3) have on X-ray spectra of Li2Sx species is explored via experiment and theory.

  10. High-resolution x-ray absorption spectroscopy studies of metal compounds in neurodegenerative brain tissue

    SciTech Connect

    Collingwood, J.F.; Mikhaylova, A.; Davidson, M.R.; Batich, C.; Streit, W.J.; Eskin, T.; Terry, J.; Barrea, R.; Underhill, R.S.; Dobson, J.

    2008-06-16

    Fluorescence mapping and microfocus X-ray absorption spectroscopy are used to detect, locate and identify iron biominerals and other inorganic metal accumulations in neurodegenerative brain tissue at sub-cellular resolution (< 5 microns). Recent progress in developing the technique is reviewed. Synchrotron X-rays are used to map tissue sections for metals of interest, and XANES and XAFS are used to characterize anomalous concentrations of the metals in-situ so that they can be correlated with tissue structures and disease pathology. Iron anomalies associated with biogenic magnetite, ferritin and haemoglobin are located and identified in an avian tissue model with a pixel resolution {approx} 5 microns. Subsequent studies include brain tissue sections from transgenic Huntington's mice, and the first high-resolution mapping and identification of iron biominerals in human Alzheimer's and control autopsy brain tissue. Technical developments include use of microfocus diffraction to obtain structural information about biominerals in-situ, and depositing sample location grids by lithography for the location of anomalies by conventional microscopy. The combined techniques provide a breakthrough in the study of both intra- and extra-cellular iron compounds and related metals in tissue. The information to be gained from this approach has implications for future diagnosis and treatment of neurodegeneration, and for our understanding of the mechanisms involved.

  11. High-resolution x-ray absorption spectroscopy studies of metal compounds in neurodegenerative brain tissue

    NASA Astrophysics Data System (ADS)

    Collingwood, J. F.; Mikhaylova, A.; Davidson, M. R.; Batich, C.; Streit, W. J.; Eskin, T.; Terry, J.; Barrea, R.; Underhill, R. S.; Dobson, J.

    2005-01-01

    Fluorescence mapping and microfocus X-ray absorption spectroscopy are used to detect, locate and identify iron biominerals and other inorganic metal accumulations in neurodegenerative brain tissue at sub-cellular resolution (<5 microns). Recent progress in developing the technique is reviewed. Synchrotron X-rays are used to map tissue sections for metals of interest, and XANES and XAFS are used to characterise anomalous concentrations of the metals in-situ so that they can be correlated with tissue structures and disease pathology. Iron anomalies associated with biogenic magnetite, ferritin and haemoglobin are located and identified in an avian tissue model with a pixel resolution ~5 microns. Subsequent studies include brain tissue sections from transgenic Huntington's mice, and the first high-resolution mapping and identification of iron biominerals in human Alzheimer's and control autopsy brain tissue. Technical developments include use of microfocus diffraction to obtain structural information about biominerals in-situ, and depositing sample location grids by lithography for the location of anomalies by conventional microscopy. The combined techniques provide a breakthrough in the study of both intra- and extra-cellular iron compounds and related metals in tissue. The information to be gained from this approach has implications for future diagnosis and treatment of neurodegeneration, and for our understanding of the mechanisms involved.

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

    PubMed Central

    Pichler, Thomas; Ayala, Paola

    2015-01-01

    Summary 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. PMID:25671162

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

    SciTech Connect

    Andrews, J.C. |

    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.

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

    SciTech Connect

    Himpsel, Franz J.

    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.

  15. X-ray absorption spectroscopy of iron at multimegabar pressures in laser shock experiments

    NASA Astrophysics Data System (ADS)

    Harmand, M.; Ravasio, A.; Mazevet, S.; Bouchet, J.; Denoeud, A.; Dorchies, F.; Feng, Y.; Fourment, C.; Galtier, E.; Gaudin, J.; Guyot, F.; Kodama, R.; Koenig, M.; Lee, H. J.; Miyanishi, K.; Morard, G.; Musella, R.; Nagler, B.; Nakatsutsumi, M.; Ozaki, N.; Recoules, V.; Toleikis, S.; Vinci, T.; Zastrau, U.; Zhu, D.; Benuzzi-Mounaix, A.

    2015-07-01

    Taking advantage of the new opportunities provided by x-ray free electron laser (FEL) sources when coupled to a long laser pulse as available at the Linear Coherent Light Source (LCLS), we have performed x-ray absorption near-edge spectroscopy (XANES) of laser shock compressed iron up to 420 GPa (±50 ) and 10 800 K (±1390 ). Visible diagnostics coupled with hydrodynamic simulations were used to infer the thermodynamical conditions along the Hugoniot and the release adiabat. A modification of the pre-edge feature at 7.12 keV in the XANES spectra is observed above pressures of 260 GPa along the Hugoniot. Comparing with ab initio calculations and with previous laser-heated diamond cell data, we propose that such changes in the XANES pre-edge could be a signature of molten iron. This interpretation then suggests that iron is molten at pressures and temperatures higher than 260 GPa (±29 ) and 5680 K (±700 ) along the principal Fe Hugoniot.

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

    PubMed

    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.

  17. X-ray absorption spectroscopy as a probe of dissolved polysulfides in lithium sulfur batteries

    NASA Astrophysics Data System (ADS)

    Pascal, Tod; Prendergast, David

    2015-03-01

    There has been enormous interest lately in lithium sulfur batteries, since they have 5 times the theoretical capacity of lithium ion batteries. Large-scale adoption of this technology has been hampered by numerous shortcomings, chiefly the poor utilization of the active cathode material and rapid capacity fading during cycling. Overcoming these limitations requires methods capable of identifying and quantifying the products of the poorly understood electrochemical reactions. One recent advance has been the use of X-ray absorption spectroscopy (XAS), an element-specific probe of the unoccupied energy levels around an excited atom upon absorption of an X-ray photon, to identify the reaction products and intermediates. In this talk, we'll present first principles molecular dynamics and spectral simulations of dissolved lithium polysulfide species, showing how finite temperature dynamics, molecular geometry, molecular charge state and solvent environment conspire to determine the peak positions and intensity of the XAS. We'll present a spectral analysis of the radical (-1e charge) species, and reveal a unique low energy feature that can be used to identify these species from their more common dianion (-2e charge) counterparts.

  18. High-resolution X-ray spectroscopy: the coming-of-age

    NASA Astrophysics Data System (ADS)

    Kaastra, J.

    2016-06-01

    Since the launch of Chandra and XMM-Newton, high-resolution X-ray spectra of cosmic sources of all kinds have become available. These spectra have resulted in major scientific breakthroughs. However, due to the techniques used, in general high-quality spectra can only be obtained for the brightest few sources of each class. Moreover, except for the most compact extended sources, like cool core clusters, grating spectra are limited to point sources. ASTRO-H makes another major step forward, in yielding for the first time high-quality spectra of extended sources, and improved spectral sensitivity in the Fe-K band. With the launch of Athena, X-ray spectroscopy will become mature. It allows us to extend the investigations from the few handful of brightest sources of each category to a large number of sources far away in space and time, or to get high time-resolution, high-spectral resolution spectra of bright time variable sources.

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

    USGS Publications Warehouse

    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.

  20. Mossbauer spectroscopy and X-ray diffraction of samples from the Santa Catharina iron meteorite

    NASA Technical Reports Server (NTRS)

    Roy-Poulsen, H.; Clarke, R. S., Jr.; Jensen, G. B.; Knudsen, J. M.; Larsen, L.; Roy-Poulsen, N. O.; Vistisen, L.

    1984-01-01

    Conversion electron Mossbauer spectroscopy (CEMS) of samples from the Santa Catharina iron meteorite shows the presence of the ordered iron-nickel phase with 50% Ni, tetrataenite, and of the paramagnetic iron-nickel phase with 25% Ni. The FeNi phase with 50% Ni amounts to 70% of the iron-nickel alloys. Futhermore, the CEM spectra show the presence of small peaks from one or more spinel compounds. These small peaks are more pronounced when regions near the rim of the samples are analyzed. The X-ray diffraction of different areas of the samples, both optically dark and optically light areas, shows the presence of a diffraction pattern from a single f.c.c. lattice with a lattice parameter of a=3.58A This means that the two different Fe-Ni phases seen in the CEMS analysis occupy the same lattice. The X-ray photographs also show the presence of super-structure reflections from the ordered FeNi phase, and that the orientation of the f.c.c. lattice is the same within the whole sample.

  1. Americium characterization by X-ray fluorescence and absorption spectroscopy in plutonium uranium mixed oxide

    NASA Astrophysics Data System (ADS)

    Degueldre, Claude; Cozzo, Cedric; Martin, Matthias; Grolimund, Daniel; Mieszczynski, Cyprian

    2013-06-01

    Plutonium uranium mixed oxide (MOX) fuels are currently used in nuclear reactors. The actinides in these fuels need to be analyzed after irradiation for assessing their behaviour with regard to their environment and the coolant. In this work the study of the atomic structure and next-neighbour environment of Am in the (Pu,U)O2 lattice in an irradiated (60 MW d kg-1) MOX sample was performed employing micro-X-ray fluorescence (µ-XRF) and micro-X-ray absorption fine structure (µ-XAFS) spectroscopy. The chemical bonds, valences and stoichiometry of Am (˜0.66 wt%) are determined from the experimental data gained for the irradiated fuel material examined in its peripheral zone (rim) of the fuel. In the irradiated sample Am builds up as Am3+ species within an [AmO8]13- coordination environment (e.g. >90%) and no (<10%) Am(IV) or (V) can be detected in the rim zone. The occurrence of americium dioxide is avoided by the redox buffering activity of the uranium dioxide matrix.

  2. The Chemistry os Spent Nuclear Fuel From X-Ray Absorption Spectroscopy

    SciTech Connect

    F.A. Fortner; A.J. Kropf; J.C. Cunnane

    2006-09-21

    Present and future nuclear fuel cycles will require an understanding of the complex chemistry of trace fission products and transuranium actinides in spent nuclear fuel (SNF). Because of the unique analytical challenges presented by SNF to the materials scientist, many of its fundamental physical and chemical properties remain poorly understood, especially on the microscopic scale. Such an understanding of the chemical states of radionuclides in SNF would benefit development of technologies for fuel monitoring, fuel performance improvement and modeling, fuel reprocessing, and spent fuel storage and disposal. We have recently demonstrated the use of synchrotron x-ray absorption spectroscopy (XAS) to examine crystal chemical properties of actinides and fission products in extracted specimens of SNF. Information obtained includes oxidation state, chemical bond coordination, and quantitative elemental concentration and distribution. We have also used XAS in a scanning mode to obtain x-ray spectral micrographs with resolution approaching 1 micron. A brief overview of the technique will be presented, along with findings on uranium, plutonium, neptunium, technetium, and molybdenum in commercial PWR SNF specimens.

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

    PubMed

    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.

  4. Detrended fluctuation analysis in x-ray photon correlation spectroscopy for determining coarsening dynamics in alloys

    SciTech Connect

    Stadler, Lorenz-M.; Sepiol, Bogdan; Pfau, Bastian; Vogl, Gero; Kantelhardt, Jan W.; Weinkamer, Richard

    2006-10-15

    We study the dynamics of precipitate coarsening in phase-separating alloys at late stages of phase separation by x-ray photon correlation spectroscopy (XPCS). For analyzing time series of fluctuating speckle intensities from small-angle scattering of coherent x rays, the method of detrended fluctuation analysis (DFA), which is ideal for determining power-law correlations, is applied. We discuss the application of DFA with respect to XPCS data by means of simulated time series. In particular, the effects of different signal-to-noise ratios are examined. Results from measurements of the two model systems Al-6 at. % Ag at 140 deg. C and Al-9 at. % Zn at 0 deg. C are presented. Since the DFA effectively removes adulterating trends in the data, quantitative agreement with Monte Carlo simulations is obtained. It is verified that two different coarsening mechanisms are predominant in the two systems--coarsening either by diffusion of single atoms or by movement of whole precipitates.

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

    NASA Astrophysics Data System (ADS)

    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

    2015-01-01

    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.

  6. Digital x-ray processing electronics for fluorescence EXAFS and spectroscopy

    NASA Astrophysics Data System (ADS)

    Hubbard, B.; Warburton, W. K.; Zhou, C. Z.

    1996-09-01

    We have developed a digital x-ray processor (DXP) for x-ray fluorescence spectroscopy, implemented in a 4-channel CAMAC module, which accepts inputs of either polarity from reset or tail preamplifiers, and outputs one spectrum per channel. Digital trapezoidal shaping and efficient pileup rejection are implemented in dedicated logic, with programmable peaking times from 0.5 to 20 msec. The energy resolution is comparable to good analog units at equivalent peaking times. A maximum input count rate (ICR) of 500,000 cps per channel can be accomodated at a peaking time of 0.5 msec. A digital signal processor on each channel is used to collect the data, apply corrections, and update the spectrum. The capabilities of the DXP prototype at high rates was tested at SSRL. Using an Ortec single-element germanium detector, the resolution was seen to degrade somewhat with increasing ICR above 150,000 cps, due to effects that we are still investigating. Collaborating with Hewlett-Packard and SSRL, the DXP was also used with a Kevex Si(Li) detector for trace element detection on silicon wafers in comparison with Kevex readout electronics. At 4 msec peaking time, DXP's resolution was slightly worse (10-15 eV) due to some excess noise pickup, though the background levels in the spectra were essentially identical in the two systems and the DXP's maximum count rate was several times higher.

  7. Biomedical and agricultural applications of energy dispersive X-ray spectroscopy in electron microscopy.

    PubMed

    Wyroba, Elżbieta; Suski, Szymon; Miller, Karolina; Bartosiewicz, Rafał

    2015-09-01

    Energy dispersive X-ray spectroscopy (EDS) in electron microscopy has been widely used in many research areas since it provides precise information on the chemical composition of subcellular structures that may be correlated with their high resolution images. In EDS the characteristic X-rays typical of each element are analyzed and the new detectors - an example of which we describe - allow for setting precisely the area of measurements and acquiring signals as a point analysis, as a linescan or in the image format of the desired area. Mapping of the elements requires stringent methods of sample preparation to prevent redistribution/loss of the elements as well as elimination of the risk of overlapping spectra. Both qualitative and quantitative analyses may be performed at a low probe current suitable for thin biological samples. Descriptions of preparation techniques, drawbacks and precautions necessary to obtain reliable results are provided, including data on standards, effects of specimen roughness and quantification. Data on EPMA application in different fields of biomedical and agricultural studies are reviewed. In this review we refer to recent EDS/EPMA applications in medical diagnostics, studies on air pollution and agrochemicals as well as on plant models used to monitor the environment.

  8. Probing hot-electron effects in wide area plasmonic surfaces using X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Ayas, Sencer; Cupallari, Andi; Dana, Aykutlu

    2014-12-01

    Plasmon enhanced hot carrier formation in metallic nanostructures increasingly attracts attention due to potential applications in photodetection, photocatalysis, and solar energy conversion. Here, hot-electron effects in nanoscale metal-insulator-metal (MIM) structures are investigated using a non-contact X-ray photoelectron spectroscopy based technique using continuous wave X-ray and laser excitations. The effects are observed through shifts of the binding energy of the top metal layer upon excitation with lasers of 445, 532, and 650 nm wavelength. The shifts are polarization dependent for plasmonic MIM grating structures fabricated by electron beam lithography. Wide area plasmonic MIM surfaces fabricated using a lithography free route by the dewetting of evaporated Ag on HfO2 exhibit polarization independent optical absorption and surface photovoltage. Using a simple model and making several assumptions about the magnitude of the photoemission current, the responsivity and external quantum efficiency of wide area plasmonic MIM surfaces are estimated as 500 nA/W and 11 × 10-6 for 445 nm illumination.

  9. Diagnosis of pusher-fuel mix in spherical implosions using x-ray spectroscopy (invited)

    NASA Astrophysics Data System (ADS)

    Keane, C. J.; Cook, R. C.; Dittrich, T. R.; Hammel, B. A.; Levedahl, W. K.; Landen, O. L.; Langer, S.; Munro, D. H.; Scott, H. A.

    1995-01-01

    Of primary concern in next generation inertial confinement fusion (ICF) implosion experiments is Rayleigh-Taylor (RT) instability of the pusher-fuel interface occurring upon acceleration and deceleration of the pusher. This results in mixing of hot fuel with cold pusher material. One method of diagnosing mix in this case is to place spectroscopic dopants both in the capsule fuel region and the innermost region of the capsule wall adjacent to the fuel. As the degree of pusher/fuel mix is increased (typically through placement of controlled perturbations on the outer surface of the capsule) the pusher dopant x-ray emission increases relative to that of the fuel dopant. Experiments of this type using indirectly driven implosions have been carried out on Nova. In this paper we describe some of the important physics issues underlying spectral line formation in these targets and discuss how they are manifested in the modeling and interpretation of experimental data. The importance of radiative transfer as well as high density plasma phenomena such as continuum lowering and Stark broadening is demonstrated. We provide an overview of recent Nova hydrodynamic instability experiments and discuss how the level of instability growth implicit in a given capsule design impacts the diagnosis of mix through x-ray spectroscopy.

  10. High-resolution X-ray spectroscopy of four active galaxies - Probing the intercloud medium

    NASA Astrophysics Data System (ADS)

    Lum, Kenneth S. K.; Canizares, Claude R.; Markert, Thomas H.; Arnaud, Keith A.

    1990-07-01

    The focal plane crystal spectrometer (FPCS) on the Einstein Observatory has been used to perform a high-resolution spectroscopic search for oxygen X-ray line emission from four active galaxies: Fairall 9, Mrk 421, Mrk 501, and PKS 0548 - 322. Specifically, O VIII Ly-alpha and Ly-beta, whose unredshifted energies are 653 and 775 eV, respectively, were sought. No narrow-line emission was detected within the energy bands searched. Upper limits are calculated on the line flux from these sources of 30 eV equivalent width and use a photoionization model to place corresponding upper limits on the densities of diffuse gas surrounding the active nuclei. The upper limits on gas density range from about 0.02-50/cu cm and probe various radial distances from the central source. This is the first time high-resolution X-ray spectroscopy has been used to place constraints on the intercloud medium in active galaxies.

  11. Millisecond Kinetics of Nanocrystal Cation Exchange UsingMicrofluidic X-ray Absorption Spectroscopy

    SciTech Connect

    Chan, Emory M.; Marcus, Matthew A.; Fakra, Sirine; Elnaggar,Mariam S.; Mathies, Richard A.; Alivisatos, A. Paul

    2007-05-07

    We describe the use of a flow-focusing microfluidic reactorto measure the kinetics of theCdSe-to-Ag2Se nanocrystal cation exchangereaction using micro-X-ray absorption spectroscopy (mu XAS). The smallmicroreactor dimensions facilitate the millisecond mixing of CdSenanocrystal and Ag+ reactant solutions, and the transposition of thereaction time onto spatial coordinates enables the in situ observation ofthe millisecond reaction with mu XAS. XAS spectra show the progression ofCdSe nanocrystals to Ag2Se over the course of 100 ms without the presenceof long-lived intermediates. These results, along with supporting stoppedflow absorption experiments, suggest that this nanocrystal cationexchange reaction is highly efficient and provide insight into how thereaction progresses in individual particles. This experiment illustratesthe value and potential of in situ microfluidic X-ray synchrotrontechniques for detailed studies of the millisecond structuraltransformations of nanoparticles and other solution-phase reactions inwhich diffusive mixing initiates changes in local bond structures oroxidation states.

  12. A multi-channel monolithic Ge detector system for fluorescence x-ray absorption spectroscopy

    SciTech Connect

    Bucher, J.J.; Allen, P.G.; Edelstein, N.M.; Shuh, D.K.; Madden, N.W.; Cork, C.; Luke, P.; Pehl, D.; Malone, D.

    1995-03-01

    Construction and performance of a monolithic quad-pixel Ge detector for fluorescence x-ray absorption spectroscopy (XAS) at synchrotron radiation sources are described. The detector semiconductor element has an active surface area of 4.0 cm{sup 2} which is electrically separated into four 1.0 cm{sup 2} pixels, with little interfacial dead volume. Spatial response of the array shows that cross-talk between adjacent pixels is < 10% for 5.9 keV photons that fall within 0.5 mm of the pixel boundaries. The detector electronics system uses pre-amplifiers built at LBNL with commercial Tennelec Model TC 244 amplifiers. Using an {sup 55}Fe test source (MnK{sub {alpha}}, 5.9 keV), energy resolution of better than 200 eV is achieved with a 4 {mu}sec peaking time. At 0.5 {mu}sec peaking time, pulse pileup results in a 75% throughput efficiency for an incoming count rate of 100 kHz. Initial XAS fluoresncece measurements at the beamline 4 wiggler end stations at SSRL show that the detector system has several advantages over commercial x-ray spectrometers for low-concentration counting.

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

    PubMed

    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. PMID:24101232

  14. Optical Metrology for the Segmented Optics on the Constellation-X Spectroscopy X-Ray Telescope

    NASA Technical Reports Server (NTRS)

    Content, David; Colella, David; Fleetwood, Charles; Hadjimichael, Theo; Lehan, John; McMann, Joseph; Reid, Paul; Saha, Timo; Wright, Geraldine; Zhang, William

    2004-01-01

    We present the metrology requirements and metrology implementation necessary to prove out the reflector technology for the Constellation X(C-X) spectroscopy X-ray telescope (SXT). This segmented, 1.6m diameter highly nested Wolter-1 telescope presents many metrology and alignment challenges. In particular, these mirrors have a stringent imaging error budget as compared to their intrinsic stiffness; This is required for Constellation-X to have sufficient effective area with the weight requirement. This has implications for the metrology that can be used. A variety of contract and noncontact optical profiling and interferometric methods are combined to test the formed glass substrates before replication and the replicated reflector segments.The reflectors are tested both stand-alone and in-situ in an alignment tower.Some of these methods have not been used on prior X-ray telescopes and some are feasible only because of the segmented approach used on the SXT. Methods discussed include high precision coordinate measurement machines using very low force or optical probe axial interferometric profiling azimuthal circularity profiling and use of advanced null optics such as conical computer generated hologram (CGHs).

  15. Electronic structure of Au-Ta alloys:. An X-ray spectroscopy study

    NASA Astrophysics Data System (ADS)

    Kuhn, M.; Sammynaiken, R.; Sham, T. K.

    1998-07-01

    Au-Ta alloys with the compositions of AuTa, AuTa 2 and AuTa 3, prepared by quenching from the melt, has been studied with X-ray diffraction, photoelectron spectroscopy (XPS) and X-ray absorption near-edge structure (XANES) measurements. It was found that while AuTa 3 is a single-phase solid solution, AuTa 2 and AuTa have mixed phases and that the Au and Ta 4f levels of the alloys shift to higher binding energy, relative to the pure metal; this is accompanied by a narrowing of the Au 5d component of the alloy d-band, which moves away from the Fermi level. This observation is interpreted in terms of a charge compensation model in which Au loses d charge but is overcompensated by s-p charge gain, resulting in a small net charge flow from Ta to Au. The observed Ta 4f binding energy shift is as predicted by electronegativity and indicates charge depletion at the Ta site. The notion of d charge depletion at both Au and Ta sites upon alloying is confirmed independently by XANES measurements which showed that the L 2,3 edge whiteline intensity for both Au and Ta increases as they become more dilute in the host, indicating an increase in d hole count. The experimental results compare favorably with a recent linear-augmented Slater-type-orbital (LASTO) calculations. The implications of these results are discussed.

  16. Probing hot-electron effects in wide area plasmonic surfaces using X-ray photoelectron spectroscopy

    SciTech Connect

    Ayas, Sencer; Cupallari, Andi; Dana, Aykutlu

    2014-12-01

    Plasmon enhanced hot carrier formation in metallic nanostructures increasingly attracts attention due to potential applications in photodetection, photocatalysis, and solar energy conversion. Here, hot-electron effects in nanoscale metal-insulator-metal (MIM) structures are investigated using a non-contact X-ray photoelectron spectroscopy based technique using continuous wave X-ray and laser excitations. The effects are observed through shifts of the binding energy of the top metal layer upon excitation with lasers of 445, 532, and 650 nm wavelength. The shifts are polarization dependent for plasmonic MIM grating structures fabricated by electron beam lithography. Wide area plasmonic MIM surfaces fabricated using a lithography free route by the dewetting of evaporated Ag on HfO{sub 2} exhibit polarization independent optical absorption and surface photovoltage. Using a simple model and making several assumptions about the magnitude of the photoemission current, the responsivity and external quantum efficiency of wide area plasmonic MIM surfaces are estimated as 500 nA/W and 11 × 10{sup −6} for 445 nm illumination.

  17. A Suborbital Payload for Soft X-ray Spectroscopy of Extended Sources

    NASA Astrophysics Data System (ADS)

    Oakley, Phillip Henry Howard

    This thesis details the intent, design and results of an X-ray suborbital rocket payload whose scientific target was the Cygnus Loop Supernova Remnant. The payload consists of wire grid collimators, off-plane gratings arrays and gaseous electron multiplier (GEM) detectors. The system was designed for measurements in the 17-107 Å bandpass with a resolution up to ∼ 60 (λ=Δλ). This instrument was christened the Extended X-ray Off-plane Spectrometer (EXOS) and was launched on a Terrier-Black Brant rocket on November 13th, 2009 from White Sands Missile Range and obtained 340 seconds of useable scientific data. The emission is dominated by O VII and O VIII, including the He-like O VII triplet at ∼22 Å. Another feature at ∼45 Å is composed primarily of Si XI and Si XII. The best-fit model to this spectrum is an equilibrium plasma model at a temperature of log(T) = 6.4 (0.23 keV).

  18. Electronic Structures of Uranium Compounds Studied by Soft X-ray Photoelectron Spectroscopy

    NASA Astrophysics Data System (ADS)

    Fujimori, Shin-ichi; Takeda, Yukiharu; Okane, Tetsuo; Saitoh, Yuji; Fujimori, Atsushi; Yamagami, Hiroshi; Haga, Yoshinori; Yamamoto, Etsuji; Ōnuki, Yoshichika

    2016-06-01

    The electronic structures of uranium-based compounds have been studied by photoelectron spectroscopy with soft X-ray synchrotron radiation. Angle-resolved photoelectron spectroscopy with soft X-rays has made it possible to directly observe their bulk band structures and Fermi surfaces. It has been shown that the band structures and Fermi surfaces of itinerant compounds such as UB2, UN, and UFeGa5 are quantitatively described by a band-structure calculation treating all U 5f electrons as itinerant. Furthermore, the overall electronic structures of heavy-fermion compounds such as UPd2Al3, UNi2Al3, and URu2Si2 are also explained by a band-structure calculation, although some disagreements exist, which might originate from the electron correlation effect. This suggests that the itinerant description of U 5f states is an appropriate starting point for the description of their electronic structures. The situation is similar for ferromagnetic superconductors such as UGe2, URhGe, UCoGe, and UIr, although the complications from their low-symmetry crystal structures make it more difficult to describe their detailed electronic structures. The local electronic structures of the uranium site have been probed by core-level photoelectron spectroscopy with soft X-rays. The comparisons of core-level spectra of heavy-fermion compounds with typical itinerant and localized compounds suggest that the local electronic structures of most itinerant and heavy-fermion compounds are close to the U 5f3 configuration except for UPd2Al3 and UPt3. The core-level spectrum of UPd2Al3 has similarities to those of both itinerant and localized compounds, suggesting that it is located at the boundary between the itinerant and localized states. Moreover, the spectrum of UPt3 is very close to that of the localized compound UPd3, suggesting that it is nearly localized, although there are narrow quasi-particle bands in the vicinity of EF.

  19. Planetary and satellite x ray spectroscopy: A new window on solid-body composition by remote sensing

    NASA Technical Reports Server (NTRS)

    Chenette, D. L.; Wolcott, R. W.; Selesnick, R. S.

    1993-01-01

    The rings and most of the satellites of the outer planets orbit within the radiation belts of their parent bodies. This is an environment with intense fluxes of energetic electrons. As a result, these objects are strong emitters of X-rays. The characteristic X-ray lines from these bodies depend on atomic composition, but they are not sensitive to how the material is arranged in compounds or mixtures. X-ray fluorescence spectral analysis has demonstrated its unique value in the laboratory as a qualitative and quantitative analysis tool. This technique has yet to be fully exploited in a planetary instrument for remote sensing. The characteristic X-ray emissions provide atomic relative abundances. These results are complementary to the molecular composition information obtained from IR, visible, and UV emission spectra. The atomic relative abundances are crucial to understanding the formation and evolution of these bodies. They are also crucial to the proper interpretation of the molecular composition results from the other sensors. The intensities of the characteristic X-ray emissions are sufficiently strong to be measured with an instrument of modest size. Recent developments in X-ray detector technologies and electronic miniaturization have made possible space-flight X-ray imaging and nonimaging spectrometers of high sensitivity and excellent energy resolution that are rugged enough to survive long-duration space missions. Depending on the application, such instruments are capable of resolving elemental abundances of elements from carbon through iron. At the same time, by measuring the bremsstrahlung intensity and energy spectrum, the characteristics of the source electron flux can be determined. We will discuss these concepts, including estimated source strengths, and will describe a small instrument capable of providing this unique channel of information for future planetary missions. We propose to build this instrument using innovative electronics packaging

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

    SciTech Connect

    Butorin, S.M.; Guo, J.; Magnuson, M.

    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.

  1. Local Structure Determination of Carbon/Nickel Ferrite Composite Nanofibers Probed by X-ray Absorption Spectroscopy.

    PubMed

    Nilmoung, Sukunya; Kidkhunthod, Pinit; Maensiri, Santi

    2015-11-01

    Carbon/NiFe2O4 composite nanofibers have been successfully prepared by electrospinning method using a various concentration solution of Ni and Fe nitrates dispersed into polyacrylonitride (PAN) solution in N,N' dimethylformamide. The phase and mophology of PAN/NiFe2O4 composite samples were characterized and investigated by X-ray diffraction and scanning electron microscopy. The magnetic properties of the prepared samples were measured at ambient temperature by a vibrating sample magnetometer. It is found that all composite samples exhibit ferromagnetism. This could be local-structurally explained by the existed oxidation states of Ni2+ and Fe3+ in the samples. Moreover, local environments around Ni and Fe ions could be revealed by X-ray absorption spectroscopy (XAS) measurement including X-ray absorption near edge structure (XANES) and Extended X-ray absorption fine structure (EXAFS).

  2. Distribution and speciation of bromine in mammalian tissue and fluids by X-ray fluorescence imaging and X-ray absorption spectroscopy.

    PubMed

    Ceko, Melanie J; Hummitzsch, Katja; Hatzirodos, Nicholas; Bonner, Wendy; James, Simon A; Kirby, Jason K; Rodgers, Raymond J; Harris, Hugh H

    2015-05-01

    Bromine is one of the most abundant and ubiquitous trace elements in the biosphere and until recently had not been shown to perform any essential biological function in animals. A recent study demonstrated that bromine is required as a cofactor for peroxidasin-catalysed formation of sulfilimine crosslinks in Drosophila. In addition, bromine dietary deficiency is lethal in Drosophila, whereas bromine replenishment restores viability. The aim of this study was to examine the distribution and speciation of bromine in mammalian tissues and fluids to provide further insights into the role and function of this element in biological systems. In this study we used X-ray fluorescence (XRF) imaging and inductively coupled plasma-mass spectrometry (ICP-MS) to examine the distribution of bromine in bovine ovarian tissue samples, follicular fluid and aortic serum, as well as human whole blood and serum and X-ray absorption spectroscopy (XAS) to identify the chemical species of bromine in a range of mammalian tissue (bovine, ovine, porcine and murine), whole blood and serum samples (bovine, ovine, porcine, murine and human), and marine samples (salmon (Salmo salar), kingfish (Seriola lalandi) and Scleractinian coral). Bromine was found to be widely distributed across all tissues and fluids examined. In the bovine ovary in particular it was more concentrated in the sub-endothelial regions of arterioles. Statistical comparison of the near-edge region of the X-ray absorption spectra with a library of bromine standards led to the conclusion that the major form of bromine in all samples analysed was bromide.

  3. Distribution and speciation of bromine in mammalian tissue and fluids by X-ray fluorescence imaging and X-ray absorption spectroscopy.

    PubMed

    Ceko, Melanie J; Hummitzsch, Katja; Hatzirodos, Nicholas; Bonner, Wendy; James, Simon A; Kirby, Jason K; Rodgers, Raymond J; Harris, Hugh H

    2015-05-01

    Bromine is one of the most abundant and ubiquitous trace elements in the biosphere and until recently had not been shown to perform any essential biological function in animals. A recent study demonstrated that bromine is required as a cofactor for peroxidasin-catalysed formation of sulfilimine crosslinks in Drosophila. In addition, bromine dietary deficiency is lethal in Drosophila, whereas bromine replenishment restores viability. The aim of this study was to examine the distribution and speciation of bromine in mammalian tissues and fluids to provide further insights into the role and function of this element in biological systems. In this study we used X-ray fluorescence (XRF) imaging and inductively coupled plasma-mass spectrometry (ICP-MS) to examine the distribution of bromine in bovine ovarian tissue samples, follicular fluid and aortic serum, as well as human whole blood and serum and X-ray absorption spectroscopy (XAS) to identify the chemical species of bromine in a range of mammalian tissue (bovine, ovine, porcine and murine), whole blood and serum samples (bovine, ovine, porcine, murine and human), and marine samples (salmon (Salmo salar), kingfish (Seriola lalandi) and Scleractinian coral). Bromine was found to be widely distributed across all tissues and fluids examined. In the bovine ovary in particular it was more concentrated in the sub-endothelial regions of arterioles. Statistical comparison of the near-edge region of the X-ray absorption spectra with a library of bromine standards led to the conclusion that the major form of bromine in all samples analysed was bromide. PMID:25675086

  4. A unique 30 Tesla single-solenoid pulsed magnet instrument for x-ray studies

    NASA Astrophysics Data System (ADS)

    Islam, Zahirul; Capatina, Dana; Ruff, Jacob; Das, Ritesh; Nojiri, Hiroyuki; Narumi, Yasuo

    2011-03-01

    We present a dual-cryostat pulsed-magnet instrument at the Advanced Photon Source (APS) with unique capabilities. The dual-cryostat independently cools the solenoid (Tohoku design) using liquid nitrogen and the sample using a closed-cycle refrigerator, respectively. Liquid nitrogen (LN) cooling allows a repetition rate of seven minutes for peak fields of 30 Tesla. The system is unique in that the LN cryostat incorporates a double-funnel vacuum tube passing through the solenoid's bore preserving the entire angular range allowed by the magnet. This scheme is advantageous in that it allows the applied magnetic field to be parallel to the scattering plane complementing typical split-pair magnets with fields normal to the scattering plane. Performance of the coils along with preliminary x-ray diffraction and spectroscopic studies will be presented. Use of the APS is supported by the U. S. DOE, Office of Science, under Contract No. DE-AC02-06CH11357. The work was supported in part by ICC-IMR, Tohoku University.

  5. Testing of High-Resolution SI and GE Analyzers for X-Ray Raman Scattering and X-Ray Emission Spectroscopy

    SciTech Connect

    Reynolds, K.W.; Bergmann, U.

    2005-01-01

    A project at Stanford Linear Accelerator Center (SLAC) is currently underway for the building of a new multi-crystal x-ray spectrometer that will be used to probe the fundamental structures of light elements, including water, as well as 3d transition metals, such as metalloproteins, in dilute systems. Experimentation for determining the focal lengths for the prospective high-resolution, spherically-curved silicon (Si) and germanium (Ge) analyzers for the instrument and the energy resolutions at their respective focal points is described. The focal lengths of the Si and Ge analyzers being sampled were found by minimizing the focal size made from a diffused helium-neon (HeNe) gas laser operating at 632 nm (0.95 meV). Afterwards, the energy resolutions were determined by using synchrotron radiation (SR), in the range from 6-16 keV energies. The experiments were performed at Beamline 10-2 at the Stanford Synchrotron Radiation Laboratory (SSRL), a division of SLAC. This data, along with the energies of the incident beams, was used to determine which samples are most effective at focusing x-rays to the highest spatial and energy resolution. Sample Si (440)A, with a focal length of 1015.2 mm, had the best energy resolution. Furthermore, a new multi-crystal goniometer was tested and commissioned. As part of this work, the device was prealigned into Rowland geometry, in order to facilitate the process of finding a single high-energy resolution x-ray focus for all 7 analyzers.

  6. Low-cost virtual instrumentation system of an energy-dispersive X-ray spectrometer for a scanning electron microscope

    PubMed Central

    Lei, Junfeng; Zeng, Libo; Liu, Ronggui; Liu, Juntang; Zhang, Zelan

    2002-01-01

    The paper describes an energy-dispersive X-ray spectrometer for a scanning electron microscope (SEM-EDXS). It was constructed using the new architecture of a virtual instrument (VI), which is low-cost, space-saving, fast and flexible way to develop the instrument. Computer-aided teaching (CAT) was used to develop the instrument and operation rather than a traditional instrument technique. The VI was designed using the object-oriented program language C++ and compact programmable logical devices (CPLD). These include spectra collection and processing, quantitative analysis and X-ray-intensity distribution analysis. The procedure is described in detail. The VI system gives an e¡ective and user-friendly human interface for the whole analytical task. Some examples are described. PMID:18924732

  7. High-rate x-ray spectroscopy in mammography with a CdTe detector: A digital pulse processing approach

    SciTech Connect

    Abbene, L.; Gerardi, G.; Principato, F.; Del Sordo, S.; Ienzi, R.; Raso, G.

    2010-12-15

    Purpose:Direct measurement of mammographic x-ray spectra under clinical conditions is a difficult task due to the high fluence rate of the x-ray beams as well as the limits in the development of high resolution detection systems in a high counting rate environment. In this work we present a detection system, based on a CdTe detector and an innovative digital pulse processing (DPP) system, for high-rate x-ray spectroscopy in mammography. Methods: The DPP system performs a digital pile-up inspection and a digital pulse height analysis of the detector signals, digitized through a 14-bit, 100 MHz digitizer, for x-ray spectroscopy even at high photon counting rates. We investigated on the response of the digital detection system both at low (150 cps) and at high photon counting rates (up to 500 kcps) by using monoenergetic x-ray sources and a nonclinical molybdenum anode x-ray tube. Clinical molybdenum x-ray spectrum measurements were also performed by using a pinhole collimator and a custom alignment device. Results: The detection system shows excellent performance up to 512 kcps with an energy resolution of 4.08% FWHM at 22.1 keV. Despite the high photon counting rate (up to 453 kcps), the molybdenum x-ray spectra, measured under clinical conditions, are characterized by a low number of pile-up events. The agreement between the attenuation curves and the half value layer values, obtained from the measured spectra, simulated spectra, and from the exposure values directly measured with an ionization chamber, also shows the accuracy of the measurements. Conclusions: These results make the proposed detection system a very attractive tool for both laboratory research and advanced quality controls in mammography.

  8. X-ray absorption spectroscopy study in the BaFe2As2 family

    NASA Astrophysics Data System (ADS)

    Koh, Yoonyoung; Kim, Yeongkwan; Yang, Wanli; Kim, Changyoung

    2012-02-01

    One of the representative Fe-based superconductor families, BaFe2As2 (Tc =38K) is a semimetal with the same number of hole and electron carriers, and is in a spin density wave state below 139K. It has been reported that various types of ``doped'' BaFe2As2 systems can obtained by substitution of Ba, Fe, and As atoms. However, an important issue has been recently raised regarding whether each type of substitution indeed induces effective charge doping or not. It is essential to clarify whether each type of substitution indeed induce an effective doping in BaFe2As2 system. To clarify the carrier doping issue, we performed high resolution X-ray absorption spectroscopy experiment on Ba(Fe,Co)2As2, Ba(Fe,Ru)2As2, BaFe2(As,P)2 which are representative ``doped'' BaFe2As2 systems.

  9. Electronic topological transition in zinc under pressure: An x-ray absorption spectroscopy study

    NASA Astrophysics Data System (ADS)

    Aquilanti, G.; Trapananti, A.; Minicucci, M.; Liscio, F.; Twaróg, A.; Principi, E.; Pascarelli, S.

    2007-10-01

    Zinc metal has been studied at high pressure using x-ray absorption spectroscopy. In order to investigate the role of the different degrees of hydrostaticity on the occurrence of structural anomalies following the electronic topological transition, two pressure transmitting media have been used. Results show that the electronic topological transition, if it exists, does not induce an anomaly in the local environment of compressed Zn as a function of hydrostatic pressure and any anomaly must be related to a loss of hydrostaticity of the pressure transmitting medium. The near-edge structures of the spectra, sensitive to variations in the electronic density of states above the Fermi level, do not show any evidence of electronic transition whatever pressure transmitting medium is used.

  10. X-ray absorption spectroscopy to probe interfacial issues in photolithography.

    SciTech Connect

    Angelopoulos, Marie (IBM, T.J. Watson Research Center, Yorktown Heights, NY); Lenhart, Joseph Ludlow; Wu, Wen-li (National Institute of Standards and Technology, Gaithersburg, MD); Sambasivan, Sharadha (National Institute of Standards and Technology, Gaithersburg, MD); Fischer, Daniel A. (National Institute of Standards and Technology, Gaithersburg, MD); Jones, Ronald L. (National Institute of Standards and Technology, Gaithersburg, MD); Soles, Christopher L. (National Institute of Standards and Technology, Gaithersburg, MD); Lin, Eric K. (National Institute of Standards and Technology, Gaithersburg, MD); Goldfarb, Dario L. (IBM, T.J. Watson Research Center, Yorktown Heights, NY)

    2003-03-01

    We utilize near edge X-ray absorption fine structure spectroscopy (NEXASFS) to provide detailed chemical insight into two interfacial problems facing sub-100 nm patterning. First, chemically amplified photo-resists are sensitive to surface phenomenon, which causes deviations in the pattern profile near the interface. Striking examples include T-topping, closure, footing, and undercutting. NEXAFS was used to examine surface segregation of a photo-acid generator at the resist/air interface and to illustrate that the surface extent of deprotection in a model resist film can be different than the bulk extent of deprotection. Second, line edge roughness becomes increasingly critical with shrinking patterns, and may be intimately related to the line edge deprotection profile. A NEXAFS technique to surface depth profile for compositional gradients is described with the potential to provide chemical information about the resist line edge.

  11. A novel X-ray photoelectron spectroscopy study of the Al/SiO2 interface

    NASA Technical Reports Server (NTRS)

    Hecht, M. H.; Vasquez, R. P.; Grunthaner, F. J.; Zamani, N.; Maserjian, J.

    1985-01-01

    The nondestructive measurement of the chemical and physical characteristics of the interface between bulk SiO2 and thick aluminum films is reported. Both X-ray phototelectron spectroscopy (XPS) and electrical measurements of unannealed, resistively evaporated Al films on thermal SiO2 indicate an atomically abrupt interface. Post metallization annealing at 450 C induces reduction of the SiO2 by the aluminum, at a rate consistent with the bulk reaction rate. The XPS measurement is performed from the SiO2 side after the removal of the Si substrate with XeF2 gas and thinning of the SiO2 layer with HF:ETOH. This represents a powerful new approach to the study of metal-insulator and related interfaces.

  12. Melting of iron determined by X-ray absorption spectroscopy to 100 GPa

    PubMed Central

    Aquilanti, Giuliana; Trapananti, Angela; Karandikar, Amol; Kantor, Innokenty; Marini, Carlo; Mathon, Olivier; Pascarelli, Sakura; Boehler, Reinhard

    2015-01-01

    Temperature, thermal history, and dynamics of Earth rely critically on the knowledge of the melting temperature of iron at the pressure conditions of the inner core boundary (ICB) where the geotherm crosses the melting curve. The literature on this subject is overwhelming, and no consensus has been reached, with a very large disagreement of the order of 2,000 K for the ICB temperature. Here we report new data on the melting temperature of iron in a laser-heated diamond anvil cell to 103 GPa obtained by X-ray absorption spectroscopy, a technique rarely used at such conditions. The modifications of the onset of the absorption spectra are used as a reliable melting criterion regardless of the solid phase from which the solid to liquid transition takes place. Our results show a melting temperature of iron in agreement with most previous studies up to 100 GPa, namely of 3,090 K at 103 GPa. PMID:26371317

  13. X-ray photoelectron spectroscopy study of radiofrequency-sputtered refractory compound steel interfaces

    NASA Technical Reports Server (NTRS)

    Wheeler, D. R.; Brainard, W. A.

    1978-01-01

    Radiofrequency sputtering was used to deposit Mo2C, Mo2B5, and MoSi2 coatings on 440C steel substrates. Both sputter etched and preoxidized substrates were used, and the films were deposited with and without a substrate bias of -300 V. The composition of the coatings was measured as a function of depth by X-ray photoelectron spectroscopy combined with argon ion etching. In the interfacial region there was evidence that bias produced a graded interface in Mo2B5 but not in Mo2C. Oxides of iron and of all film constituents except carbon were presented in all cases but the iron oxide concentration was higher and the layer thicker on the preoxidized substrates. The film and iron oxides were mixed in the MoSi2 and Mo2C films but layered in the Mo2B5 film. The presence of mixed oxides correlates with enhanced film adhesion.

  14. Zinc ligands in the metal hyperaccumulator Thlaspi caerulescens as determined using X-ray absorption spectroscopy

    SciTech Connect

    Salt, D.E.; Prince, R.C.; Baker, A.J.M.; Raskin, I.; Pickering, I.J.

    1999-03-01

    Using the noninvasive technique of X-ray absorption spectroscopy (XAS), the authors have been able to determine the ligand environment of Zn in different tissues of the Zn-hyperaccumulator Thlaspi caerulescens. The majority of intracellular Zn in roots of T. caerulescens was found to be coordinated with histidine. In the xylem sap Zn was found to be transported mainly as the free hydrated Zn{sup 2+} cation with a smaller proportion coordinated with organic acids. In the shoots, Zn coordination occurred mainly via organic acids, with a smaller proportion present as the hydrated cation and coordinated with histidine and the cell wall. Their data suggest that histidine plays an important role in Zn homeostasis in the roots, whereas organic acids are involved in xylem transport and Zn storage in shoots.

  15. Studies of Y-Ba-Cu-O single crystals by x-ray absorption spectroscopy

    SciTech Connect

    Krol, A.; Ming, Z.H.; Kao, Y.H.; Nuecker, N.; Roth, G.; Fink, J.; Smith, G.C.; Erband, A.; Mueller-Vogt, G.; Karpinski, J.; Kaldis, E.; Schoenmann, K.

    1992-02-01

    The symmetry and density of unoccupied states of YBa{sub 2}Cu{sub 3}O{sub 7} YBa{sub 2}Cu{sub 4}O{sub 8} have been investigated by orientation dependent x-ray absorption spectroscopy on the O 1s edge using a bulk-sensitive fluorescence-yield-detection method. It has been found that the O 2p holes are distributed equally between the CuO{sub 2} planes and CuO chains and that the partial density of unoccupied O 2p states in the CuO{sub 2} planes are identical in both systems investigated. The upper Hubbard band has been observed in the planes but not in the chains in both systems. 18 refs.

  16. Studies of fluorine in catalysts with ultrasoft X-ray absorption spectroscopy

    SciTech Connect

    Davis, S.M. ); Meitzner, G.D. ); Fischer, D.A. ); Gland, J. )

    1993-08-01

    The structures of fluorine-doped alumina catalyst powders have been studied by fluorescence yield ultrasoft X-ray absorption spectroscopy. The results presented here demonstrate that important local structural information can be obtained by the technique. It is established that fluoride ions are substituted for oxygen in alumina at low concentration of adsorbed fluorine. For doping levels larger than those required for saturation of the monolayer, the authors observed AlF[sub 3]-like features in the radial structure function. These results are in agreement with previous observations of bulk AlF[sub 3] in aluminas with high levels of fluorine doping. The fluorescence yield method is well suited for determining structures of a wide range of ceramic materials. 22 refs., 4 figs.

  17. Melting of iron determined by X-ray absorption spectroscopy to 100 GPa.

    PubMed

    Aquilanti, Giuliana; Trapananti, Angela; Karandikar, Amol; Kantor, Innokenty; Marini, Carlo; Mathon, Olivier; Pascarelli, Sakura; Boehler, Reinhard

    2015-09-29

    Temperature, thermal history, and dynamics of Earth rely critically on the knowledge of the melting temperature of iron at the pressure conditions of the inner core boundary (ICB) where the geotherm crosses the melting curve. The literature on this subject is overwhelming, and no consensus has been reached, with a very large disagreement of the order of 2,000 K for the ICB temperature. Here we report new data on the melting temperature of iron in a laser-heated diamond anvil cell to 103 GPa obtained by X-ray absorption spectroscopy, a technique rarely used at such conditions. The modifications of the onset of the absorption spectra are used as a reliable melting criterion regardless of the solid phase from which the solid to liquid transition takes place. Our results show a melting temperature of iron in agreement with most previous studies up to 100 GPa, namely of 3,090 K at 103 GPa.

  18. Surface properties of SmB6 from x-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Heming, N.; Treske, U.; Knupfer, M.; Büchner, B.; Inosov, D. S.; Shitsevalova, N. Y.; Filipov, V. B.; Krause, S.; Koitzsch, A.

    2014-11-01

    We have investigated the properties of cleaved SmB6 single crystals by x-ray photoelectron spectroscopy. At low temperatures and freshly cleaved samples a surface core level shift is observed which vanishes when the temperature is increased. A Sm valence between 2.5 and 2.6 is derived from the relative intensities of the Sm2 + and Sm3 + multiplets. The B/Sm intensity ratio obtained from the core levels is always larger than the stoichiometric value. Possible reasons for this deviation are discussed. The B 1s signal shows an unexpected complexity: An anomalous low energy component appears with increasing temperature and is assigned to the formation of a suboxide at the surface. While several interesting intrinsic and extrinsic properties of the SmB6 surface are elucidated in this manuscript, no clear indication of a trivial mechanism for the prominent surface conductivity is found.

  19. Determination of InN/Diamond Heterojunction Band Offset by X-ray Photoelectron Spectroscopy

    PubMed Central

    2011-01-01

    Diamond is not only a free standing highly transparent window but also a promising carrier confinement layer for InN based devices, yet little is known of the band offsets in InN/diamond system. X-ray photoelectron spectroscopy was used to measure the energy discontinuity in the valence band offset (VBO) of InN/diamond heterostructure. The value of VBO was determined to be 0.39 ± 0.08 eV and a type-I heterojunction with a conduction band offset (CBO) of 4.42 ± 0.08 eV was obtained. The accurate determination of VBO and CBO is important for the application of III-N alloys based electronic devices. PMID:27502672

  20. X-Ray absorption spectroscopy investigation of 1-alkyl-3-methylimidazolium bromide salts

    SciTech Connect

    D'Angelo, Paola; Zitolo, Andrea; Migliorati, Valentina; Bodo, Enrico; Caminiti, Ruggero; Aquilanti, Giuliana; Hazemann, Jean Louis; Testemale, Denis; Mancini, Giordano

    2011-08-21

    X-ray absorption spectroscopy (XAS) has been used to unveil the bromide ion local coordination structure in 1-alkyl-3-methylimidazolium bromide [C{sub n}mim]Br ionic liquids (ILs) with different alkyl chains. The XAS spectrum of 1-ethyl-3-methylimidazolium bromide has been found to be different from those of the other members of the series, from the butyl to the decyl derivatives, that have all identical XAS spectra. This result indicates that starting from 1-buthyl-3-methylimidazolium bromide the local molecular arrangement around the bromide anion is the same independently from the length of the alkyl chain, and that the imidazolium head groups in the liquid ILs with long alkyl chains assume locally the same orientation as in the [C{sub 4}mim]Br crystal. With this study we show that the XAS technique is an effective direct tool for unveiling the local structural arrangements around selected atoms in ILs.

  1. The hydrogen bond in ice probed by soft x-ray spectroscopy and density functional theory

    SciTech Connect

    Nilsson, A.; Ogasawara, H.; Cavalleri, M.; Nordlund, D.; Nyberg, M.; Wernet, Ph.; Pettersson, L.G.M.

    2005-04-15

    We combine photoelectron and x-ray absorption spectroscopy with density functional theory to derive a molecular orbital picture of the hydrogen bond in ice. We find that the hydrogen bond involves donation and back-donation of charge between the oxygen lone pair and the O-H antibonding orbitals on neighboring molecules. Together with internal s-p rehybridization this minimizes the repulsive charge overlap of the connecting oxygen and hydrogen atoms, which is essential for a strong attractive electrostatic interaction. Our joint experimental and theoretical results demonstrate that an electrostatic model based on only charge induction from the surrounding medium fails to properly describe the internal charge redistributions upon hydrogen bonding.

  2. Compositional analysis of Ceramic Glaze by Laser Induced Breakdown Spectroscopy and Energy Dispersive X-Ray

    NASA Astrophysics Data System (ADS)

    Khedr, A.; Abdel-kareem, O.; Elnabi, S. H.; Harith, M. A.

    2011-09-01

    Laser induced breakdown spectroscopy (LIBS) has been applied for the analysis of Egyptian Islamic glaze ceramic sample. The sample dating back to Fatimid period (969-1169AD), and collected from Al-Fustat excavation store in Cairo. The analysis of contaminated pottery sample has been performed to draw mapping for the elemental compositions by LIBS technique. LIBS measurements have been done by the fundamental wavelength (1064 nm) of Nd: YAG laser for the elemental analysis and performing the cleaning processes of the pottery sample. In addition, complementary analyses were carried out by scanning electron microscopy linked with energy dispersive X-ray microanalysis (SEM/EDX) to obtain verification of chemical results. The morphological surfaces before and after cleaning has been done by Optical Microscopy (OM).

  3. An x ray photoelectron spectroscopy study of Au(x)In(y) alloys

    NASA Technical Reports Server (NTRS)

    Jayne, Douglas T.; Fatemi, Navid S.; Weizer, Victor G.

    1990-01-01

    Four gold-indium alloys were studied by x ray photoelectron spectroscopy. The binding energies and intensity ratios of the Au 4f7/2 and In 3d5/2 core levels were determined for the bulk alloy compositions of Au(10 percent In), Au3In, AuIn, and AuIn2. These values were determined for the native oxides on the materials, for the surfaces prepared by ion bombardment to remove the oxide and for surfaces scraped in-situ with a ceramic tool to expose the bulk composition. These results furnish calibration values that allow determination of the composition of thin films of this alloy system. In addition the binding energies add to the data base for understanding the effect of alloying on core level binding energies. As an illustration, these results are used to determine the composition of a series of alloy films formed by incongruent evaporation of an alloy charge.

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

    NASA Astrophysics Data System (ADS)

    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.

  5. X-ray photoelectron spectroscopy study of chemically-etched Nd-Ce-Cu-O surfaces

    NASA Technical Reports Server (NTRS)

    Vasquez, R. P.; Gupta, A.; Kussmaul, A.

    1991-01-01

    Acetic acid, Br2, and HCl solutions are investigated for removing insulating species from Nd(1.85)Ce(0.15)CuO(4-delta) (NCCO) thin film surfaces. X-ray photoelectron spectroscopy (XPS) shows that the HCl etch is most effective, yielding O 1s spectra comparable to those obtained from samples cleaned in vacuum and a clear Fermi edge in the valence band region. Reduction and oxidation reversibly induces and eliminates, respectively, Fermi level states for undoped samples, but has no clearly observable effect on the XPS spectra for doped samples. Reactivity to air is much less for NCCO compared to hole superconductors, which is attributed to the lack of reactive alkaline earth elements in NCCO.

  6. Structural analysis of sulfur in natural rubber using X-ray absorption near-edge spectroscopy.

    PubMed

    Pattanasiriwisawa, Wanwisa; Siritapetawee, Jaruwan; Patarapaiboolchai, Orasa; Klysubun, Wantana

    2008-09-01

    X-ray absorption near-edge spectroscopy (XANES) has been applied to natural rubber in order to study the local environment of sulfur atoms in sulfur crosslinking structures introduced in the vulcanization process. Different types of chemical accelerators in conventional, semi-efficient and efficient vulcanization systems were investigated. The experimental results show the good sensitivity and reproducibility of XANES to characterize the local geometry and electronic environment of the sulfur K-shell under various conditions of vulcanization and non-vulcanization of natural rubber. Several applications of XANES in this study demonstrate an alternative way of identifying sulfur crosslinks in treated natural rubber based on differences in their spectra and oxidation states. PMID:18728323

  7. X-Ray Absorption Spectroscopy Of Thin Foils Irradiated By An Ultra-short Laser Pulse

    NASA Astrophysics Data System (ADS)

    Renaudin, P.; Lecherbourg, L.; Blancard, C.; Cossé, P.; Faussurier, G.; Audebert, P.; Bastiani-Ceccotti, S.; Geindre, J.-P.; Shepherd, R.

    2007-08-01

    Point-projection K-shell absorption spectroscopy has been used to measure absorption spectra of transient plasma created by an ultra-short laser pulse. The 1s-2p and 1s-3p absorption lines of weakly ionized aluminum and the 2p-3d absorption lines of bromine were measured over an extended range of densities in a low-temperature regime. Independent plasma characterization was obtained using frequency domain interferometry diagnostic (FDI) that allows the interpretation of the absorption spectra in terms of spectral opacities. Assuming local thermodynamic equilibrium, spectral opacity calculations have been performed using the density and temperature inferred from the FDI diagnostic to compare to the measured absorption spectra. A good agreement is obtained when non-equilibrium effects due to non-stationary atomic physics are negligible at the x-ray probe time.

  8. The Anderson-Condon-Shortley Site in X-ray Spectroscopies of Solids

    NASA Astrophysics Data System (ADS)

    Delley, Bernard; Uldry, Anne-Christine

    2014-03-01

    Electronic structures of compounds involving open d- and f- shell are studied frequently by X-ray and electron spectroscopies. The excitation, especially core excitation, is localized on a single site makes this the problem of impurity site states interacting with the continuum of bands. on the other hande, the electron-electron interaction whithin the d- or f- shell leads to a multiplet problem as addressed long ago for isolated atoms. Building on our easy to use program multiX (*), which treats an atom in a general crystal field environment without symmetry analysis, we now address the interaction of this atomic entity with the band continuum. The crossover from atomic to bandlike spectra is the focus of interest. We discuss experimental examples where available and accessible to our methods. Swiss SNF grant 200021-129970 is gratefully acknowledged.

  9. Band alignment at memristive metal-oxide interfaces investigated by hard x-ray photoemission spectroscopy

    NASA Astrophysics Data System (ADS)

    Lenser, C.; Köhl, A.; Patt, M.; Schneider, C. M.; Waser, R.; Dittmann, R.

    2014-09-01

    The electronic structure and band alignment at metal/oxide interfaces for nonvolatile memory applications are investigated by hard x-ray photoelectron spectroscopy (HAXPES) and DC transport measurements, using acceptor doped SrTiO3 as a model memristive oxide. Metal-insulator-metal (MIM) structures with a noble metal (Pt) top electrode form a Schottky barrier and exhibit rectifying properties, while a reactive metal (Ti) as top electrode shows symmetric I(V) characteristics and a flat band situation at the interface. The transition from rectifying to ohmic I(V) relations with increasing Ti thickness is discussed with respect to the electrochemical reaction at the interface, the band alignment at the electrode/oxide interface, and the slope of the energy bands across the MIM structure.

  10. X-ray emission spectroscopy and density functional study of CO/Fe(100)

    SciTech Connect

    Gladh, J.; Oeberg, H.; Li, Jibiao; Ljungberg, M. P.; Matsuda, A.; Pettersson, L. G. M.; Oestroem, H.; Ogasawara, H.; Nilsson, A.

    2012-01-21

    We report x-ray emission and absorption spectroscopy studies of the electronic structure of the predissociative {alpha}{sub 3} phase of CO bound at hollow sites of Fe(100) as well as of the on-top bound species in the high-coverage {alpha}{sub 1} phase. The analysis is supported by density functional calculations of structures and spectra. The bonding of ''lying down'' CO in the hollow site is well described in terms of {pi} to {pi}* charge transfer made possible through bonding interaction also at the oxygen in the minority spin-channel. The on-top CO in the mixed, high-coverage {alpha}{sub 1} phase is found to be tilted due to adsorbate-adsorbate interaction, but still with bonding mainly characteristic of ''vertical'' on-top adsorbed CO similar to other transition-metal surfaces.

  11. Ge doped HfO{sub 2} thin films investigated by x-ray absorption spectroscopy

    SciTech Connect

    Miotti, Leonardo; Bastos, Karen P.; Lucovsky, Gerald; Radtke, Claudio; Nordlund, Dennis

    2010-07-15

    The stability of the tetragonal phase of Ge doped HfO{sub 2} thin films on Si(100) was investigated. Hf(Ge)O{sub 2} films with Ge atomic concentrations varying from 0% to 15% were deposited by remote plasma chemical vapor deposition. The atomic structure on the oxide after rapid thermal annealing was investigated by x-ray absorption spectroscopy of the O and Ge K edges and by Rutherford backscattering spectrometry. The authors found that Ge concentrations as low as 5 at. % effectively stabilize the tetragonal phase of 5 nm thick Hf(Ge)O{sub 2} on Si and that higher concentrations are not stable to rapid thermal annealing at temperatures above 750 deg. C.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

  14. X-ray absorption/emission line spectroscopy of the Galactic hot gaseous halo

    NASA Astrophysics Data System (ADS)

    Wang, Daniel

    2016-04-01

    There is an ongoing debate as to whether or not the Milky Way is surrounded by a large-scale, massive corona. Vastly different conclusions as to its extent and mass have been drawn from existing studies based on X-ray absorption and/or emission line spectroscopy. I will discuss my assessment of this issue, focusing on various uncertainties and potential problems in the present data, analyses, results, and interpretations.In particular, I will examine how different assumptions about the temperature distribution of the corona affect the inference of its physical scale. I will also discuss the external perspectives of galactic coronae obtained form observing nearby highly-inclined disk galaxies.

  15. [Surface and interface analysis of PTCDA/ITO using X-ray photoelectron spectroscopy (XPS)].

    PubMed

    Ou, Gu-ping; Song, Zhen; Gui, Wen-ming; Zhang, Fu-jia

    2006-04-01

    X-ray photoelectron spectroscopy (XPS) of surface and interface of PTCDA/ITO in PTCDA/p-Si organic-on-inorganic photoelectric detector was investigated. From C1s fine spectrum we found that the binding energy of C atoms in perylene rings was 284.6 eV; and the binding energy of C atoms in acid radical was 288.7 eV; moreover, some C atoms were oxidized by O atoms from ITO. The binding energy of O atoms in C=O bonds and C-O-C bonds was 531.5 and 533.4 eV, respectively. At the interface, the peak of high binding energy in C1s spectrum disappeared, and the main peak shifted toward lower binding energy.

  16. The irradiation of ammonia ice studied by near edge x-ray absorption spectroscopy

    SciTech Connect

    Parent, Ph.; Bournel, F.; Lasne, J.; Laffon, C.; Carniato, S.; Lacombe, S.; Strazzulla, G.; Gardonio, S.; Lizzit, S.; Kappler, J.-P.; Joly, L.

    2009-10-21

    A vapor-deposited NH{sub 3} ice film irradiated at 20 K with 150 eV photons has been studied with near-edge x-ray absorption fine structure (NEXAFS) spectroscopy at the nitrogen K-edge. Irradiation leads to the formation of high amounts (12%) of molecular nitrogen N{sub 2}, whose concentration as a function of the absorbed energy has been quantified to 0.13 molecule/eV. The stability of N{sub 2} in solid NH{sub 3} has been also studied, showing that N{sub 2} continuously desorbs between 20 and 95 K from the irradiated ammonia ice film. Weak concentrations (<1%) of other photoproducts are also detected. Our NEXAFS simulations show that these features own to NH{sub 2}, N{sub 2}H{sub 2}, and N{sub 3}{sup -}.

  17. Sodium Chloride Diffusion during Muscle Salting Evidenced by Energy-Dispersive X-ray Spectroscopy Imaging.

    PubMed

    Filgueras, Rénata; Peyrin, Frédéric; Vénien, Annie; Hénot, Jean Marc; Astruc, Thierry

    2016-01-27

    To better understand the relationship between the muscle structure and NaCl transfers in meat, we used energy-dispersive X-ray spectroscopy (EDS) coupled with scanning electron microscopy (SEM) to analyze brined and dry-salted rat muscles. The muscles were freeze-dried to avoid the delocalization of soluble ions that happens in regular dehydration through a graded series of ethanol. Na and Cl maps were superimposed on SEM images to combine the muscle structure and NaCl diffusion. Brining causes rapid diffusion of NaCl through the tissue. Most brine diffuses in a linear front from the muscle surface, but a small proportion enters through the perimysium network. The muscle area penetrated by brine shows heterogeneous patterns of NaCl retention, with some connective tissue islets containing more NaCl than other parts of perimysium. NaCl penetration is considerably slower after dry salting than after brining.

  18. Measurement of barrier height of Pd on diamond (100) surface by X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Li, F. N.; Liu, J. W.; Zhang, J. W.; Wang, X. L.; Wang, W.; Liu, Z. C.; Wang, H. X.

    2016-05-01

    Barrier height (VBH) values for Pd/hydrogen-terminated diamond (H-diamond) and Pd/oxygen-terminated diamond (O-diamond) have been investigated by X-ray photoelectron spectroscopy technique. H-diamond and O-diamond have been formed on the same diamond (100) layer grown by microwave plasma-enhanced chemical vapor deposition on which Pd layers have been evaporated. The VBH values for Pd/H-diamond and Pd/O-diamond are determined to be -0.27 eV and 1.73 eV, respectively. It indicates that Pd is a suitable metal for ohmic and Schottky contacts on H-diamond and O-diamond, respectively. The experimental ΦBH values are in good agreement with the theoretical calculation results.

  19. X-ray absorption spectroscopy in electrical fields: An element-selective probe of atomic polarization

    NASA Astrophysics Data System (ADS)

    Ney, V.; Wilhelm, F.; Ollefs, K.; Rogalev, A.; Ney, A.

    2016-01-01

    We have studied a range of polar and nonpolar materials using x-ray absorption near-edge spectroscopy (XANES) in external electric fields. An energy shift of the XANES by a few meV/kV is found which scales linearly with the applied voltage, thus being reminiscent of the linear Stark effect. This is corroborated by the consistent presence of this energy shift in polar thin films and bulk crystals and its absence in nonpolar materials as well as in conducting films. The observed energy shift of the XANES is different between two atomic species in one specimen and appears to scale linearly with the atomic number of the studied element. Therefore, XANES in electrical fields opens the perspective to study atomic polarization with element specificity in a range of functional materials.

  20. Orientation of a monolayer of dipolar molecules on graphene from X-ray absorption spectroscopy.

    PubMed

    Johnson, Phillip S; Huang, Changshui; Kim, Myungwoong; Safron, Nathaniel S; Arnold, Michael S; Wong, Bryan M; Gopalan, Padma; Himpsel, F J

    2014-03-11

    Recently, single-walled carbon nanotubes as well as graphene functionalized with azobenzene chromophores have drawn attention for applications in optoelectronics due to their ability to undergo cis-trans isomerization when exposed to light. The electronic properties of the nanocarbon materials at these unconventional interfaces can be tailored by gaining structural insight into the organic monolayers at the molecular level. In this work, we use polarization-dependent X-ray absorption spectroscopy to probe the orientation of three chromophores on graphene, all identical except for their terminal groups. All three terminal groups (methyl, nitro, and nitrile) are well-oriented, with a tilt angle of about 30° from the substrate for the shared azobenzene group. Density functional theory calculations are in good agreement with experimental results and give two similar, stable configurations for the orientation of these molecules on graphene.