Sample records for x-ray spectroscopy analysis

  1. X-ray astronomical spectroscopy

    NASA Technical Reports Server (NTRS)

    Holt, S. S.

    1980-01-01

    The current status of the X-ray spectroscopy of celestial X-ray sources, ranging from nearby stars to distant quasars, is reviewed. Particular emphasis is placed on the role of such spectroscopy as a useful and unique tool in the elucidation of the physical parameters of the sources. The spectroscopic analysis of degenerate and nondegenerate stellar systems, galactic clusters and active galactic nuclei, and supernova remnants is discussed.

  2. 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.

  3. X-ray Echo Spectroscopy

    NASA Astrophysics Data System (ADS)

    Shvyd'ko, Yuri

    2016-02-01

    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 >108 ) with broadband ≃5 - 13 meV dispersing systems are introduced featuring more than 103 signal enhancement. The technique is general, applicable in different photon frequency domains.

  4. 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.

  5. 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.

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

    DOE PAGES

    Miaja-Avila, L.; O'Neil, G. C.; Uhlig, J.; ...

    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 ~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, wemore » 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.« less

  7. X-Ray photoelectron Spectroscopy Applications

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Engelhard, Mark H.; Droubay, Timothy C.; Du, Yingge

    2017-01-03

    With capability for obtaining quantitative elemental composition, chemical and electronic state, and overlayer thickness information from the top ~10 nm of a sample surface, X-ray Photoelectron Spectroscopy (XPS) or Electron Spectroscopy for Chemical Analysis (ESCA) is a versatile and widely used technique for analyzing surfaces. The technique is applied to a host of materials, from insulators to conductors in virtually every scientific field and sub-discipline. More recently, XPS has been extended under in-situ and operando conditions. Following a brief introduction to XPS principles and instrument components, this article exemplifies widely ranging XPS applications in material and life sciences.

  8. Extracting chemical information from high-resolution Kβ X-ray emission spectroscopy

    NASA Astrophysics Data System (ADS)

    Limandri, S.; Robledo, J.; Tirao, G.

    2018-06-01

    High-resolution X-ray emission spectroscopy allows studying the chemical environment of a wide variety of materials. Chemical information can be obtained by fitting the X-ray spectra and observing the behavior of some spectral features. Spectral changes can also be quantified by means of statistical parameters calculated by considering the spectrum as a probability distribution. Another possibility is to perform statistical multivariate analysis, such as principal component analysis. In this work the performance of these procedures for extracting chemical information in X-ray emission spectroscopy spectra for mixtures of Mn2+ and Mn4+ oxides are studied. A detail analysis of the parameters obtained, as well as the associated uncertainties is shown. The methodologies are also applied for Mn oxidation state characterization of double perovskite oxides Ba1+xLa1-xMnSbO6 (with 0 ≤ x ≤ 0.7). The results show that statistical parameters and multivariate analysis are the most suitable for the analysis of this kind of spectra.

  9. Optimizing soft X-ray NEXAFS spectroscopy in the laboratory

    NASA Astrophysics Data System (ADS)

    Mantouvalou, I.; Jonas, A.; Witte, K.; Jung, R.; Stiel, H.; Kanngießer, B.

    2017-05-01

    Near edge X-ray absorption fine structure (NEXAFS) spectroscopy in the soft X-ray range is feasible in the laboratory using laser-produced plasma sources. We present a study using seven different target materials for optimized data analysis. The emission spectra of the materials with atomic numbers ranging from Z = 6 to Z = 79 show distinct differences, rendering the adapted selection of a suitable target material for specialized experiments feasible. For NEXAFS spectroscopy a 112.5 nm thick polyimide film is investigated as a reference exemplifying the superiority of quasi-continuum like emission spectra.

  10. Ultrafast X-Ray Spectroscopy of Conical Intersections

    NASA Astrophysics Data System (ADS)

    Neville, Simon P.; Chergui, Majed; Stolow, Albert; Schuurman, Michael S.

    2018-06-01

    Ongoing developments in ultrafast x-ray sources offer powerful new means of probing the complex nonadiabatically coupled structural and electronic dynamics of photoexcited molecules. These non-Born-Oppenheimer effects are governed by general electronic degeneracies termed conical intersections, which play a key role, analogous to that of a transition state, in the electronic-nuclear dynamics of excited molecules. Using high-level ab initio quantum dynamics simulations, we studied time-resolved x-ray absorption (TRXAS) and photoelectron spectroscopy (TRXPS) of the prototypical unsaturated organic chromophore, ethylene, following excitation to its S2(π π*) state. The TRXAS, in particular, is highly sensitive to all aspects of the ensuing dynamics. These x-ray spectroscopies provide a clear signature of the wave packet dynamics near conical intersections, related to charge localization effects driven by the nuclear dynamics. Given the ubiquity of charge localization in excited state dynamics, we believe that ultrafast x-ray spectroscopies offer a unique and powerful route to the direct observation of dynamics around conical intersections.

  11. CONTIN XPCS: Software for Inverse Transform Analysis of X-Ray Photon Correlation Spectroscopy Dynamics

    PubMed Central

    Narayanan, Suresh; Zhang, Fan; Kuzmenko, Ivan; Ilavsky, Jan

    2018-01-01

    X-ray photon correlation spectroscopy (XPCS) and dynamic light scattering (DLS) both reveal dynamics using coherent scattering, but X-rays permit investigating of dynamics in a much more diverse array of materials. Heterogeneous dynamics occur in many such materials, and we showed how classic tools employed in analysis of heterogeneous DLS dynamics extend to XPCS, revealing additional information that conventional Kohlrausch exponential fitting obscures. This work presents the software implementation of inverse transform analysis of XPCS data called CONTIN XPCS, an extension of traditional CONTIN that accommodates dynamics encountered in equilibrium XPCS measurements. PMID:29875507

  12. CONTIN XPCS: Software for Inverse Transform Analysis of X-Ray Photon Correlation Spectroscopy Dynamics.

    PubMed

    Andrews, Ross N; Narayanan, Suresh; Zhang, Fan; Kuzmenko, Ivan; Ilavsky, Jan

    2018-02-01

    X-ray photon correlation spectroscopy (XPCS) and dynamic light scattering (DLS) both reveal dynamics using coherent scattering, but X-rays permit investigating of dynamics in a much more diverse array of materials. Heterogeneous dynamics occur in many such materials, and we showed how classic tools employed in analysis of heterogeneous DLS dynamics extend to XPCS, revealing additional information that conventional Kohlrausch exponential fitting obscures. This work presents the software implementation of inverse transform analysis of XPCS data called CONTIN XPCS, an extension of traditional CONTIN that accommodates dynamics encountered in equilibrium XPCS measurements.

  13. Solar X-Ray and Gamma-Ray Imaging Spectroscopy

    NASA Astrophysics Data System (ADS)

    Dennis, B. R.; Christe, S. D.; Shih, A. Y.; Holman, G. D.; Emslie, A. G.; Caspi, A.

    2018-02-01

    X-ray and gamma-ray Sun observations from a lunar-based observatory would provide unique information on solar atmosphere thermal and nonthermal processes. EUV and energetic neutral atom imaging spectroscopy would augment the scientific value.

  14. X-ray echo spectroscopy (Conference Presentation)

    NASA Astrophysics Data System (ADS)

    Shvyd'ko, Yuri V.

    2016-09-01

    X-ray echo spectroscopy, a counterpart of neutron spin-echo, was recently introduced [1] to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a point-like 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-meV and 0.02-meV ultra-high-resolution IXS applications (resolving power > 10^8) with broadband 5-13 meV dispersing systems will be presented featuring more than 1000-fold signal enhancement. The technique is general, applicable in different photon frequency domains. [1.] Yu. Shvyd'ko, Phys. Rev. Lett. 116, accepted (2016), arXiv:1511.01526.

  15. X-Ray Spectroscopy of Photoionized Plasmas

    NASA Technical Reports Server (NTRS)

    Kallman, Tim

    2008-01-01

    Spectroscopy allows study of sources on small spatial scales, and can provide detailed diagnostic information about elemental abundances, temperature, density and gas dynamics. For compact sources such as accreting black holes in active galactic nuclei (AGN) and X-ray binaries X-ray spectra provide truly unique insight. Observations using Chandra and XMM have revealed components of gas in these systems which were previously unknown or poorly studied. Interpretation of these data presents modeling and analysis challenges, and requires an understanding of atomic physics, ionization and spectrum formation in a radiation-dominated environment. In this talk I will discuss examples, and how they have contributed to our understanding of accreting sources and the nearby gas.

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

    DOE PAGES

    Kroll, Thomas; Kern, Jan; Kubin, Markus; ...

    2016-09-19

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

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

    PubMed Central

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

    2016-01-01

    X-ray free electron lasers (XFELs) enable unprecedented new ways to study the electronic structure and dynamics of transition metal systems. L-edge absorption spectroscopy is a powerful technique for such studies and the feasibility of this method at XFELs for solutions and solids has been demonstrated. However, the required x-ray bandwidth is an order of magnitude narrower than that of self-amplified spontaneous emission (SASE), and additional monochromatization is needed. Here we compare L-edge x-ray absorption spectroscopy (XAS) of a prototypical transition metal system based on monochromatizing the SASE radiation of the linac coherent light source (LCLS) with a new technique based on self-seeding of LCLS. We demonstrate how L-edge XAS can be performed using the self-seeding scheme without the need of an additional beam line monochromator. We show how the spectral shape and pulse energy depend on the undulator setup and how this affects the x-ray spectroscopy measurements. PMID:27828320

  18. Stimulated x-ray emission spectroscopy in transition metal complexes

    DOE PAGES

    Kroll, Thomas; Weninger, Clemens; Alonso-Mori, Roberto; ...

    2018-03-27

    We report the observation and analysis of the gain curve of amplified Kα X-ray emission from solutions of Mn(II) and Mn(VII) complexes using an X-ray free electron laser to create the 1s core-hole population inversion. We find spectra at amplification levels extending over four orders of magnitude until saturation. We observe bandwidths below the Mn 1s core-hole lifetime broadening in the onset of the stimulated emission. In the exponential amplification regime the resolution corrected spectral width of ~1.7 eV FWHM is constant over three orders of magnitude, pointing to the build-up of transform limited pulses of ~1fs duration. Driving the amplification into saturation leads to broadening and shift of the line. Importantly, the chemical sensitivity of the stimulated X-ray emission to the Mn oxidation state is preserved at power densities ofmore » $$\\sim10 20$$~W/cm 2 for the incoming X-ray pulses. Differences in signal sensitivity and spectral information compared to conventional (spontaneous) X-ray emission spectroscopy are discussed. Our findings build a baseline for nonlinear X-ray spectroscopy for a wide range of transition metal complexes in inorganic chemistry, catalysis and materials science.« less

  19. Stimulated x-ray emission spectroscopy in transition metal complexes

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Kroll, Thomas; Weninger, Clemens; Alonso-Mori, Roberto

    We report the observation and analysis of the gain curve of amplified Kα X-ray emission from solutions of Mn(II) and Mn(VII) complexes using an X-ray free electron laser to create the 1s core-hole population inversion. We find spectra at amplification levels extending over four orders of magnitude until saturation. We observe bandwidths below the Mn 1s core-hole lifetime broadening in the onset of the stimulated emission. In the exponential amplification regime the resolution corrected spectral width of ~1.7 eV FWHM is constant over three orders of magnitude, pointing to the build-up of transform limited pulses of ~1fs duration. Driving the amplification into saturation leads to broadening and shift of the line. Importantly, the chemical sensitivity of the stimulated X-ray emission to the Mn oxidation state is preserved at power densities ofmore » $$\\sim10 20$$~W/cm 2 for the incoming X-ray pulses. Differences in signal sensitivity and spectral information compared to conventional (spontaneous) X-ray emission spectroscopy are discussed. Our findings build a baseline for nonlinear X-ray spectroscopy for a wide range of transition metal complexes in inorganic chemistry, catalysis and materials science.« less

  20. Stimulated X-Ray Emission Spectroscopy in Transition Metal Complexes

    NASA Astrophysics Data System (ADS)

    Kroll, Thomas; Weninger, Clemens; Alonso-Mori, Roberto; Sokaras, Dimosthenis; Zhu, Diling; Mercadier, Laurent; Majety, Vinay P.; Marinelli, Agostino; Lutman, Alberto; Guetg, Marc W.; Decker, Franz-Josef; Boutet, Sébastien; Aquila, Andy; Koglin, Jason; Koralek, Jake; DePonte, Daniel P.; Kern, Jan; Fuller, Franklin D.; Pastor, Ernest; Fransson, Thomas; Zhang, Yu; Yano, Junko; Yachandra, Vittal K.; Rohringer, Nina; Bergmann, Uwe

    2018-03-01

    We report the observation and analysis of the gain curve of amplified K α x-ray emission from solutions of Mn(II) and Mn(VII) complexes using an x-ray free electron laser to create the 1 s core-hole population inversion. We find spectra at amplification levels extending over 4 orders of magnitude until saturation. We observe bandwidths below the Mn 1 s core-hole lifetime broadening in the onset of the stimulated emission. In the exponential amplification regime the resolution corrected spectral width of ˜1.7 eV FWHM is constant over 3 orders of magnitude, pointing to the buildup of transform limited pulses of ˜1 fs duration. Driving the amplification into saturation leads to broadening and a shift of the line. Importantly, the chemical sensitivity of the stimulated x-ray emission to the Mn oxidation state is preserved at power densities of ˜1020 W /cm2 for the incoming x-ray pulses. Differences in signal sensitivity and spectral information compared to conventional (spontaneous) x-ray emission spectroscopy are discussed. Our findings build a baseline for nonlinear x-ray spectroscopy for a wide range of transition metal complexes in inorganic chemistry, catalysis, and materials science.

  1. Photon statistics and speckle visibility spectroscopy with partially coherent X-rays.

    PubMed

    Li, Luxi; Kwaśniewski, Paweł; Orsi, Davide; Wiegart, Lutz; Cristofolini, Luigi; Caronna, Chiara; Fluerasu, Andrei

    2014-11-01

    A new approach is proposed for measuring structural dynamics in materials from multi-speckle scattering patterns obtained with partially coherent X-rays. Coherent X-ray scattering is already widely used at high-brightness synchrotron lightsources to measure dynamics using X-ray photon correlation spectroscopy, but in many situations this experimental approach based on recording long series of images (i.e. movies) is either not adequate or not practical. Following the development of visible-light speckle visibility spectroscopy, the dynamic information is obtained instead by analyzing the photon statistics and calculating the speckle contrast in single scattering patterns. This quantity, also referred to as the speckle visibility, is determined by the properties of the partially coherent beam and other experimental parameters, as well as the internal motions in the sample (dynamics). As a case study, Brownian dynamics in a low-density colloidal suspension is measured and an excellent agreement is found between correlation functions measured by X-ray photon correlation spectroscopy and the decay in speckle visibility with integration time obtained from the analysis presented here.

  2. Chemical speciation using high energy resolution PIXE spectroscopy in the tender X-ray range

    NASA Astrophysics Data System (ADS)

    Kavčič, Matjaž; Petric, Marko; Vogel-Mikuš, Katarina

    2018-02-01

    High energy resolution X-ray emission spectroscopy employing wavelength dispersive (WDS) crystal spectrometers can provide energy resolution on the level of core-hole lifetime broadening of the characteristic emission lines. While crystal spectrometers have been traditionally used in combination with electron excitation for major and minor element analysis, they have been rarely considered in proton induced X-ray emission (PIXE) trace element analysis mainly due to low detection efficiency. Compared to the simplest flat crystal WDS spectrometer the efficiency can be improved by employing cylindrically or even spherically curved crystals in combination with position sensitive X-ray detectors. When such spectrometer is coupled to MeV proton excitation, chemical bonding effects are revealed in the high energy resolution spectra yielding opportunity to extend the analytical capabilities of PIXE technique also towards chemical state analysis. In this contribution we will focus on the high energy resolution PIXE (HR-PIXE) spectroscopy in the tender X-ray range performed in our laboratory with our home-built tender X-ray emission spectrometer. Some general properties of high energy resolution PIXE spectroscopy in the tender X-ray range are presented followed by an example of sulfur speciation in biological tissue illustrating the capabilities as well as limitations of HR-PIXE method used for chemical speciation in the tender X-ray range.

  3. Novel applications of X-ray photoelectron spectroscopy on unsupported nanoparticles

    NASA Astrophysics Data System (ADS)

    Kostko, Oleg; Xu, Bo; Jacobs, Michael I.; Ahmed, Musahid

    X-ray photoelectron spectroscopy (XPS) is a powerful technique for chemical analysis of surfaces. We will present novel results of XPS on unsupported, gas-phase nanoparticles using a velocity-map imaging (VMI) spectrometer. This technique allows for probes of both the surfaces of nanoparticles via XPS as well as their interiors via near edge X-ray absorption fine structure (NEXAFS) spectroscopy. A recent application of this technique has confirmed that arginine's guanidinium group exists in a protonated state even in strongly basic solution. Moreover, the core-level photoelectron spectroscopy can provide information on the effective attenuation length (EAL) of low kinetic energy electrons. This contradictory value is important for determining the probing depth of XPS and in photolithography. A new method for determining EALs will be presented.

  4. X-ray absorption spectroscopy: EXAFS (Extended X-ray Absorption Fine Structure) and XANES (X-ray Absorption Near Edge Structure)

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Alp, E.E.; Mini, S.M.; Ramanathan, M.

    1990-04-01

    The x-ray absorption spectroscopy (XAS) had been an essential tool to gather spectroscopic information about atomic energy level structure in the early decades of this century. It has also played an important role in the discovery and systematization of rare-earth elements. The discovery of synchrotron radiation in 1952, and later the availability of broadly tunable synchrotron based x-ray sources have revitalized this technique since the 1970's. The correct interpretation of the oscillatory structure in the x-ray absorption cross-section above the absorption edge by Sayers et. al. has transformed XAS from a spectroscopic tool to a structural technique. EXAFS (Extended X-raymore » Absorption Fine Structure) yields information about the interatomic distances, near neighbor coordination numbers, and lattice dynamics. An excellent description of the principles and data analysis techniques of EXAFS is given by Teo. XANES (X-ray Absorption Near Edge Structure), on the other hand, gives information about the valence state, energy bandwidth and bond angles. Today, there are about 50 experimental stations in various synchrotrons around the world dedicated to collecting x-ray absorption data from the bulk and surfaces of solids and liquids. In this chapter, we will give the basic principles of XAS, explain the information content of essentially two different aspects of the absorption process leading to EXAFS and XANES, and discuss the source and samples limitations.« less

  5. Recent applications of hard x-ray photoelectron spectroscopy

    DOE PAGES

    Weiland, Conan; Rumaiz, Abdul K.; Pianetta, Piero; ...

    2016-05-05

    Recent applications of hard x-ray photoelectron spectroscopy (HAXPES) demonstrate its many capabilities in addition to several of its limitations. Examples are given, including measurement of buried interfaces and materials under in-situ or in-operando conditions, as well as measurements under x-ray standing-wave and resonant excitation. We also present physical considerations that differentiate HAXPES from photoemission measurements utilizing soft and ultraviolet x rays.

  6. A whole-system approach to x-ray spectroscopy in cargo inspection systems

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Langeveld, Willem G. J.; Gozani, Tsahi; Ryge, Peter

    The bremsstrahlung x-ray spectrum used in high-energy, high-intensity x-ray cargo inspection systems is attenuated and modified by the materials in the cargo in a Z-dependent way. Therefore, spectroscopy of the detected x rays yields information about the Z of the x-rayed cargo material. It has previously been shown that such ZSpectroscopy (Z-SPEC) is possible under certain circumstances. A statistical approach, Z-SCAN (Z-determination by Statistical Count-rate ANalysis), has also been shown to be effective, and it can be used either by itself or in conjunction with Z-SPEC when the x-ray count rate is too high for individual x-ray spectroscopy. Both techniquesmore » require fast x-ray detectors and fast digitization electronics. It is desirable (and possible) to combine all techniques, including x-ray imaging of the cargo, in a single detector array, to reduce costs, weight, and overall complexity. In this paper, we take a whole-system approach to x-ray spectroscopy in x-ray cargo inspection systems, and show how the various parts interact with one another. Faster detectors and read-out electronics are beneficial for both techniques. A higher duty-factor x-ray source allows lower instantaneous count rates at the same overall x-ray intensity, improving the range of applicability of Z-SPEC in particular. Using an intensity-modulated advanced x-ray source (IMAXS) allows reducing the x-ray count rate for cargoes with higher transmission, and a stacked-detector approach may help material discrimination for the lowest attenuations. Image processing and segmentation allow derivation of results for entire objects, and subtraction of backgrounds. We discuss R and D performed under a number of different programs, showing progress made in each of the interacting subsystems. We discuss results of studies into faster scintillation detectors, including ZnO, BaF{sub 2} and PbWO{sub 4}, as well as suitable photo-detectors, read-out and digitization electronics. We discuss high

  7. Hard X-ray imaging spectroscopy of FOXSI microflares

    NASA Astrophysics Data System (ADS)

    Glesener, Lindsay; Krucker, Sam; Christe, Steven; Buitrago-Casas, Juan Camilo; Ishikawa, Shin-nosuke; Foster, Natalie

    2015-04-01

    The ability to investigate particle acceleration and hot thermal plasma in solar flares relies on hard X-ray imaging spectroscopy using bremsstrahlung emission from high-energy electrons. Direct focusing of hard X-rays (HXRs) offers the ability to perform cleaner imaging spectroscopy of this emission than has previously been possible. Using direct focusing, spectra for different sources within the same field of view can be obtained easily since each detector segment (pixel or strip) measures the energy of each photon interacting within that segment. The Focusing Optics X-ray Solar Imager (FOXSI) sounding rocket payload has successfully completed two flights, observing microflares each time. Flare images demonstrate an instrument imaging dynamic range far superior to the indirect methods of previous instruments like the RHESSI spacecraft.In this work, we present imaging spectroscopy of microflares observed by FOXSI in its two flights. Imaging spectroscopy performed on raw FOXSI images reveals the temperature structure of flaring loops, while more advanced techniques such as deconvolution of the point spread function produce even more detailed images.

  8. X-ray-induced photo-chemistry and X-ray absorption spectroscopy of biological samples

    PubMed Central

    George, Graham N.; Pickering, Ingrid J.; Pushie, M. Jake; Nienaber, Kurt; Hackett, Mark J.; Ascone, Isabella; Hedman, Britt; Hodgson, Keith O.; Aitken, Jade B.; Levina, Aviva; Glover, Christopher; Lay, Peter A.

    2012-01-01

    As synchrotron light sources and optics deliver greater photon flux on samples, X-ray-induced photo-chemistry is increasingly encountered in X-ray absorption spectroscopy (XAS) experiments. The resulting problems are particularly pronounced for biological XAS experiments. This is because biological samples are very often quite dilute and therefore require signal averaging to achieve adequate signal-to-noise ratios, with correspondingly greater exposures to the X-ray beam. This paper reviews the origins of photo-reduction and photo-oxidation, the impact that they can have on active site structure, and the methods that can be used to provide relief from X-ray-induced photo-chemical artifacts. PMID:23093745

  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. Pixel detectors for x-ray imaging spectroscopy in space

    NASA Astrophysics Data System (ADS)

    Treis, J.; Andritschke, R.; Hartmann, R.; Herrmann, S.; Holl, P.; Lauf, T.; Lechner, P.; Lutz, G.; Meidinger, N.; Porro, M.; Richter, R. H.; Schopper, F.; Soltau, H.; Strüder, L.

    2009-03-01

    Pixelated semiconductor detectors for X-ray imaging spectroscopy are foreseen as key components of the payload of various future space missions exploring the x-ray sky. Located on the platform of the new Spectrum-Roentgen-Gamma satellite, the eROSITA (extended Roentgen Survey with an Imaging Telescope Array) instrument will perform an imaging all-sky survey up to an X-ray energy of 10 keV with unprecedented spectral and angular resolution. The instrument will consist of seven parallel oriented mirror modules each having its own pnCCD camera in the focus. The satellite born X-ray observatory SIMBOL-X will be the first mission to use formation-flying techniques to implement an X-ray telescope with an unprecedented focal length of around 20 m. The detector instrumentation consists of separate high- and low energy detectors, a monolithic 128 × 128 DEPFET macropixel array and a pixellated CdZTe detector respectively, making energy band between 0.5 to 80 keV accessible. A similar concept is proposed for the next generation X-ray observatory IXO. Finally, the MIXS (Mercury Imaging X-ray Spectrometer) instrument on the European Mercury exploration mission BepiColombo will use DEPFET macropixel arrays together with a small X-ray telescope to perform a spatially resolved planetary XRF analysis of Mercury's crust. Here, the mission concepts and their scientific targets are briefly discussed, and the resulting requirements on the detector devices together with the implementation strategies are shown.

  11. 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.

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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Kojima, Sadaoki, E-mail: kojima-s@ile.osaka-u.ac.jp, E-mail: sfujioka@ile.osaka-u.ac.jp; Ikenouchi, Takahito; Arikawa, Yasunobu

    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{sup 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 resolutionmore » 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 SiO{sub 2} 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.« less

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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Xiang, Dao; Ding, Yuantao; Raubenheimer, Tor

    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 atomicmore » 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.).« less

  14. Photochemically Generated Thiyl Free Radicals Observed by X-ray Absorption Spectroscopy

    DOE PAGES

    Sneeden, Eileen Y.; Hackett, Mark J.; Cotelesage, Julien J. H.; ...

    2017-07-27

    Sulfur-based thiyl radicals are known to be involved in a wide range of chemical and biological processes, but they are often highly reactive, which makes them difficult to observe directly. We report herein X-ray absorption spectra and analysis that support the direct observation of two different thiyl species generated photochemically by X-ray irradiation. The thiyl radical sulfur K-edge X-ray absorption spectra of both species are characterized by a uniquely low energy transition at about 2465 eV, which occurs at a lower energy than any previously observed feature at the sulfur K-edge and corresponds to a 1s → 3p transition tomore » the singly occupied molecular orbital of the free radical. In conclusion, our results constitute the first observation of substantial levels of thiyl radicals generated by X-ray irradiation and detected by sulfur K-edge X-ray absorption spectroscopy.« less

  15. Evaluation of portable Raman spectroscopy and handheld X-ray fluorescence analysis (hXRF) for the direct analysis of glyptics

    NASA Astrophysics Data System (ADS)

    Lauwers, D.; Candeias, A.; Coccato, A.; Mirao, J.; Moens, L.; Vandenabeele, P.

    2016-03-01

    In archaeometry, the advantages of a combined use of Raman spectroscopy and X-ray fluorescence spectroscopy are extensively discussed for applications such as the analysis of paintings, manuscripts, pottery, etc. Here, we demonstrate for the first time the advantage of using both techniques for analysing glyptics. These engraved gemstones or glass materials were originally used as stamps, to identify the owner, for instance on letters, but also on wine vessels. For this research, a set of 64 glyptics (42 Roman glass specimens and 22 modern ones), belonging to the collection of the museum 'Quinta das Cruzes' in Funchal (Madeira, Portugal), was analysed with portable Raman spectroscopy and handheld X-ray fluorescence (hXRF). These techniques were also used to confirm the gemological identification of these precious objects and can give extra information about the glass composition. Raman spectroscopy identifies the molecular composition as well as on the crystalline phases present. On the other hand, hXRF results show that the antique Roman glass samples are characterised with low Pb and Sn levels and that the modern specimens can be discriminated in two groups: lead-based and non-lead-based ones.

  16. Evaluation of portable Raman spectroscopy and handheld X-ray fluorescence analysis (hXRF) for the direct analysis of glyptics.

    PubMed

    Lauwers, D; Candeias, A; Coccato, A; Mirao, J; Moens, L; Vandenabeele, P

    2016-03-15

    In archaeometry, the advantages of a combined use of Raman spectroscopy and X-ray fluorescence spectroscopy are extensively discussed for applications such as the analysis of paintings, manuscripts, pottery, etc. Here, we demonstrate for the first time the advantage of using both techniques for analysing glyptics. These engraved gemstones or glass materials were originally used as stamps, to identify the owner, for instance on letters, but also on wine vessels. For this research, a set of 64 glyptics (42 Roman glass specimens and 22 modern ones), belonging to the collection of the museum 'Quinta das Cruzes' in Funchal (Madeira, Portugal), was analysed with portable Raman spectroscopy and handheld X-ray fluorescence (hXRF). These techniques were also used to confirm the gemological identification of these precious objects and can give extra information about the glass composition. Raman spectroscopy identifies the molecular composition as well as on the crystalline phases present. On the other hand, hXRF results show that the antique Roman glass samples are characterised with low Pb and Sn levels and that the modern specimens can be discriminated in two groups: lead-based and non-lead-based ones. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. Resonant Polarization Spectroscopy for Hot X-ray Plasmas

    DOE PAGES

    Chen, Guo -Xin

    2016-04-28

    X-ray line polarization spectroscopy is a method of choice for probing hot plasma conditions. The precise roles of resonant structures in this method have not been realized and fully understood. With a sophisticated relativistic close coupling Dirac R-matrix calculation of polarized radiation of the quadrupole magnetic M2 line at 2.717 Å in Ba 46+, we revealed the nature of resonant structures in x-ray line polarization spectroscopy. We found that signatures with a heavy resonance forest imprinting on polarization may be used for a sensitive new spectroscopic method. The resonant polarization spectrum was used to determine or constrain the directional beammore » electron distribution of the laboratory Ba plasma. Lastly, our results provide a start of resonant polarization spectroscopy as a method for diagnostics of laboratory, fusion and astrophysical plasma source conditions.« less

  18. Soft X-ray spectroscopy of nanoparticles by velocity map imaging

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Kostko, O.; Xu, B.; Jacobs, M. I.

    Velocity map imaging (VMI), a technique traditionally used to study chemical dynamics in the gas phase, is applied to study X-ray photoemission from aerosol nanoparticles. Soft X-rays from the Advanced Light Source synchrotron, probe a beam of nanoparticles, and the resulting photoelectrons are velocity mapped to obtain their kinetic energy distributions. A new design of the VMI spectrometer is described. The spectrometer is benchmarked by measuring vacuum ultraviolet photoemission from gas phase xenon and squalene nanoparticles followed by measurements using soft X-rays. It is demonstrated that the photoelectron distribution from X-ray irradiated squalene nanoparticles is dominated by secondary electrons. Bymore » scanning the photon energies and measuring the intensities of these secondary electrons, a near edge X-ray absorption fine structure (NEXAFS) spectrum is obtained. The NEXAFS technique is used to obtain spectra of aqueous nanoparticles at the oxygen K edge. By varying the position of the aqueous nanoparticle beam relative to the incident X-ray beam, evidence is presented such that the VMI technique allows for NEXAFS spectroscopy of water in different physical states. Finally, we discuss the possibility of applying VMI methods to probe liquids and solids via X-ray spectroscopy.« less

  19. Soft X-ray spectroscopy of nanoparticles by velocity map imaging

    DOE PAGES

    Kostko, O.; Xu, B.; Jacobs, M. I.; ...

    2017-05-05

    Velocity map imaging (VMI), a technique traditionally used to study chemical dynamics in the gas phase, is applied to study X-ray photoemission from aerosol nanoparticles. Soft X-rays from the Advanced Light Source synchrotron, probe a beam of nanoparticles, and the resulting photoelectrons are velocity mapped to obtain their kinetic energy distributions. A new design of the VMI spectrometer is described. The spectrometer is benchmarked by measuring vacuum ultraviolet photoemission from gas phase xenon and squalene nanoparticles followed by measurements using soft X-rays. It is demonstrated that the photoelectron distribution from X-ray irradiated squalene nanoparticles is dominated by secondary electrons. Bymore » scanning the photon energies and measuring the intensities of these secondary electrons, a near edge X-ray absorption fine structure (NEXAFS) spectrum is obtained. The NEXAFS technique is used to obtain spectra of aqueous nanoparticles at the oxygen K edge. By varying the position of the aqueous nanoparticle beam relative to the incident X-ray beam, evidence is presented such that the VMI technique allows for NEXAFS spectroscopy of water in different physical states. Finally, we discuss the possibility of applying VMI methods to probe liquids and solids via X-ray spectroscopy.« less

  20. Soft X-ray absorption spectroscopy and resonant inelastic X-ray scattering spectroscopy below 100 eV: probing first-row transition-metal M-edges in chemical complexes.

    PubMed

    Wang, Hongxin; Young, Anthony T; Guo, Jinghua; Cramer, Stephen P; Friedrich, Stephan; Braun, Artur; Gu, Weiwei

    2013-07-01

    X-ray absorption and scattering spectroscopies involving the 3d transition-metal K- and L-edges have a long history in studying inorganic and bioinorganic molecules. However, there have been very few studies using the M-edges, which are below 100 eV. Synchrotron-based X-ray sources can have higher energy resolution at M-edges. M-edge X-ray absorption spectroscopy (XAS) and resonant inelastic X-ray scattering (RIXS) could therefore provide complementary information to K- and L-edge spectroscopies. In this study, M2,3-edge XAS on several Co, Ni and Cu complexes are measured and their spectral information, such as chemical shifts and covalency effects, are analyzed and discussed. In addition, M2,3-edge RIXS on NiO, NiF2 and two other covalent complexes have been performed and different d-d transition patterns have been observed. Although still preliminary, this work on 3d metal complexes demonstrates the potential to use M-edge XAS and RIXS on more complicated 3d metal complexes in the future. The potential for using high-sensitivity and high-resolution superconducting tunnel junction X-ray detectors below 100 eV is also illustrated and discussed.

  1. Solid state structural investigations of the bis(chalcone) compound with single crystal X-ray crystallography, DFT, gamma-ray spectroscopy and chemical spectroscopy methods

    NASA Astrophysics Data System (ADS)

    Yakalı, Gül; Biçer, Abdullah; Eke, Canel; Cin, Günseli Turgut

    2018-04-01

    A bis(chalcone), (2E,6E)-2,6-bis((E)-3phenylallidene)cyclohexanone, was characterized by 1H NMR, 13C NMR, FTIR, UV-Vis spectroscopy, gamma-ray spectroscopy and single crystal X- ray structural analysis. The optimized molecular structure of the compound is calculated using DFT/B3LYP with 6-31G (d,p) level. The calculated geometrical parameters are in good agreement with the experimental data obtained from our reported X-ray structure. The powder and single crystal compounds were gama-irradiated using clinical electron linear accelerator and 60Co gamma-ray source, respectively. Spectral studies (1H NMR, 13C NMR, FTIR and UV-Vis) of powder chalcone compound were also investigated before and after irradiation. Depending on the irradiation notable changes were observed in spectral features powder sample. Single crystal X-ray diffraction investigation shows that both unirradiated and irradiated single crystal samples crystallizes in a orthorhombic crystal system in the centrosymmetric space group Pbcn and exhibits an C-H..O intramolecular and intermolecular hydrogen bonds. The crystal packing is stabilised by strong intermolecular bifurcate C-H..O hydrogen bonds and π…π stacking interactions. The asymmetric unit of the title compound contains one-half of a molecule. The other half of the molecule is generated with (1-x,y,-3/2-z) symmetry operator. The molecule is almost planar due to having π conjugated system of chalcones. However, irradiated single crystal compound showed significant changes lattice parameters, crystal volume and density. According to results of gamma-ray spectroscopy, radioactive elements of powder compound which are 123Sb(n,g),124Sb,57Fe(g,p),56Mn, 55Mn(g,n), and 54Mn were determined using photoactivation analysis. However, the most intensive gamma-ray energy signals are 124Sb.

  2. IR Spectroscopy and X-Ray Phase Analysis of the Chemical Composition of Gallstones

    NASA Astrophysics Data System (ADS)

    Pichugina, A. A.; Tsyro, L. V.; Unger, F. G.

    2018-01-01

    The composition of the inorganic and organic parts of gallstones was investigated by x-ray phase analysis and IR spectroscopy. Cholesterol, bilirubin, calcium bilirubinate, calcium carbonate, and calcium hydrogen phosphate are all found in gallstones. The major component is cholesterol. A gallstone was separated into layers and the inorganic part was separated out by annealing. Inorganic compounds were found to predominate in the outer layer of the gallstone, which is related to the mechanism of its formation. The inorganic part contains calcium carbonate, present in both the calcite and waterite modifications.

  3. Characterization of CuHal-intercalated carbon nanotubes with x-ray absorption spectroscopy combined with x-ray photoelectron and resonant photoemission spectroscopies

    NASA Astrophysics Data System (ADS)

    Brzhezinskaya, M.; Generalov, A.; Vinogdradov, A.; Eliseev, A.

    2013-04-01

    Encapsulated single-walled carbon nanotubes (SWCNTs) with inner channels filled by different compounds present the new class of composite materials. Such CNTs give opportunity to form 1D nanocrystals as well as quantum nanowires with new physical and chemical properties inside the tubes. The present study is aimed to characterize the possible chemical interaction between CuHal (Hal=I, Cl, Br) and SWCNTs in CuHal@SWCNTs and electronic structure of the latter using high-resolution near edge X-ray absorption fine structure (NEXAFS) spectroscopy combined with high-resolution X-ray photoelectron spectroscopy and resonant photoemission spectroscopy. The present study has shown that there is a chemical interaction between the filler and π-electron subsystem of CNTs which is accompanied by changes of the atomic and electronic structure of the filler during the encapsulating it inside CNTs.

  4. 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

  5. X-ray absorption fine structure (XAFS) spectroscopy using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Shrivastava, B. D.

    2012-05-01

    The X-ray absorption fine structure (XAFS) spectra are best recorded when a highly intense beam of X-rays from a synchrotron is used along with a good resolution double crystal or curved crystal spectrometer and detectors like ionization chambers, scintillation counters, solid state detectors etc. Several synchrotrons around the world have X-ray beamlines dedicated specifically to XAFS spectroscopy. Fortunately, the Indian synchrotron (Indus-2) at Raja Ramanna Centre for Advanced Technology (RRCAT) at Indore has started operation. A dispersive type EXAFS beamline called BL-8 has been commissioned at this synchrotron and another beamline having double crystal monochromator (DCM) is going to be commissioned shortly. In Indian context, in order that more research workers use these beamlines, the study of XAFS spectroscopy using synchrotron radiation becomes important. In the present work some of the works done by our group on XAFS spectroscopy using synchrotron radiation have been described.

  6. TES X-ray microcalorimeters for X-ray astronomy and material analysis

    NASA Astrophysics Data System (ADS)

    Mitsuda, Kazuhisa

    2016-11-01

    TES X-ray microcalorimeter arrays provide not only high-energy resolution (FWHM < 10eV) in X-ray spectroscopy but also imaging and high-counting-rate capabilities. They are very promising spectrometer for X-ray astronomy and material analysis. In this paper, we report our recent progress. For material analysis, we have fabricated 8 × 8 format array with a fast signal response ( 40 μs) and proved the energy resolution of 5.8 eV FWHM at 5.9 keV. We developed common biasing scheme to reduce number of wirings from room temperature to the cryogenic stage. From measurements using the newly-designed common-bias SQUID array amplifier chips, and from numerical simulations, we demonstrated that signal cross talks due to the common bias is enough small. For space applications, we are developing frequency-division signal multiplexing system. We have fabricated a baseband feedback system and demonstrated that the noise added by the feedback system is about 4 eV FWHM equivalent for 16 ch multiplexing system. The digital to analog converter (DAC) dominates the noise, and needs be reduced by a factor of four for future astronomy missions.

  7. 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.

  8. Alternative difference analysis scheme combining R-space EXAFS fit with global optimization XANES fit for X-ray transient absorption spectroscopy.

    PubMed

    Zhan, Fei; Tao, Ye; Zhao, Haifeng

    2017-07-01

    Time-resolved X-ray absorption spectroscopy (TR-XAS), based on the laser-pump/X-ray-probe method, is powerful in capturing the change of the geometrical and electronic structure of the absorbing atom upon excitation. TR-XAS data analysis is generally performed on the laser-on minus laser-off difference spectrum. Here, a new analysis scheme is presented for the TR-XAS difference fitting in both the extended X-ray absorption fine-structure (EXAFS) and the X-ray absorption near-edge structure (XANES) regions. R-space EXAFS difference fitting could quickly provide the main quantitative structure change of the first shell. The XANES fitting part introduces a global non-derivative optimization algorithm and optimizes the local structure change in a flexible way where both the core XAS calculation package and the search method in the fitting shell are changeable. The scheme was applied to the TR-XAS difference analysis of Fe(phen) 3 spin crossover complex and yielded reliable distance change and excitation population.

  9. X-ray Photoelectron Spectroscopy (XPS), Rutherford Back Scattering (RBS) studies

    NASA Technical Reports Server (NTRS)

    Neely, W. C.; Bozak, M. J.; Williams, J. R.

    1993-01-01

    X-ray photoelectron spectroscopy (XPS), Rutherford Back Scattering (RBS) studies of each of sample received were completed. Since low angle X-ray could not be performed because of instrumentation problems, Auger spectrometry was employed instead. The results of these measurements for each of the samples is discussed in turn.

  10. An upgraded x-ray spectroscopy diagnostic on MST.

    PubMed

    Clayton, D J; Almagri, A F; Burke, D R; Forest, C B; Goetz, J A; Kaufman, M C; O'Connell, R

    2010-10-01

    An upgraded x-ray spectroscopy diagnostic is used to measure the distribution of fast electrons in MST and to determine Z(eff) and the particle diffusion coefficient D(r). A radial array of 12 CdZnTe hard-x-ray detectors measures 10-150 keV Bremsstrahlung from fast electrons, a signature of reduced stochasticity and improved confinement in the plasma. A new Si soft-x-ray detector measures 2-10 keV Bremsstrahlung from thermal and fast electrons. The shaped output pulses from both detector types are digitized and the resulting waveforms are fit with Gaussians to resolve pileup and provide good time and energy resolution. Lead apertures prevent detector saturation and provide a well-known etendue, while lead shielding prevents pickup from stray x-rays. New Be vacuum windows transmit >2 keV x-rays, and additional Al and Be filters are sometimes used to reduce low energy flux for better resolution at higher energies. Measured spectra are compared to those predicted by the Fokker-Planck code CQL3D to deduce Z(eff) and D(r).

  11. Characterization of Colloidal Quantum Dot Ligand Exchange by X-ray Photoelectron Spectroscopy

    NASA Astrophysics Data System (ADS)

    Atewologun, Ayomide; Ge, Wangyao; Stiff-Roberts, Adrienne D.

    2013-05-01

    Colloidal quantum dots (CQDs) are chemically synthesized semiconductor nanoparticles with size-dependent wavelength tunability. Chemical synthesis of CQDs involves the attachment of long organic surface ligands to prevent aggregation; however, these ligands also impede charge transport. Therefore, it is beneficial to exchange longer surface ligands for shorter ones for optoelectronic devices. Typical characterization techniques used to analyze surface ligand exchange include Fourier-transform infrared spectroscopy, x-ray diffraction, transmission electron microscopy, and nuclear magnetic resonance spectroscopy, yet these techniques do not provide a simultaneously direct, quantitative, and sensitive method for evaluating surface ligands on CQDs. In contrast, x-ray photoelectron spectroscopy (XPS) can provide nanoscale sensitivity for quantitative analysis of CQD surface ligand exchange. A unique aspect of this work is that a fingerprint is identified for shorter surface ligands by resolving the regional XPS spectrum corresponding to different types of carbon bonds. In addition, a deposition technique known as resonant infrared matrix-assisted pulsed laser evaporation is used to improve the CQD film uniformity such that stronger XPS signals are obtained, enabling more accurate analysis of the ligand exchange process.

  12. X-ray astronomical spectroscopy

    NASA Technical Reports Server (NTRS)

    Holt, Stephen S.

    1987-01-01

    The contributions of the Goddard group to the history of X-ray astronomy are numerous and varied. One role that the group has continued to play involves the pursuit of techniques for the measurement and interpretation of the X-ray spectra of cosmic sources. The latest development is the selection of the X-ray microcalorimeter for the Advanced X-ray Astrophysics Facility (AXAF) study payload. This technology is likely to revolutionize the study of cosmic X-ray spectra.

  13. Soft X-ray absorption spectroscopy and resonant inelastic X-ray scattering spectroscopy below 100 eV: probing first-row transition-metal M-edges in chemical complexes

    PubMed Central

    Wang, Hongxin; Young, Anthony T.; Guo, Jinghua; Cramer, Stephen P.; Friedrich, Stephan; Braun, Artur; Gu, Weiwei

    2013-01-01

    X-ray absorption and scattering spectroscopies involving the 3d transition-metal K- and L-edges have a long history in studying inorganic and bioinorganic molecules. However, there have been very few studies using the M-edges, which are below 100 eV. Synchrotron-based X-ray sources can have higher energy resolution at M-edges. M-edge X-ray absorption spectroscopy (XAS) and resonant inelastic X-ray scattering (RIXS) could therefore provide complementary information to K- and L-edge spectroscopies. In this study, M 2,3-edge XAS on several Co, Ni and Cu complexes are measured and their spectral information, such as chemical shifts and covalency effects, are analyzed and discussed. In addition, M 2,3-edge RIXS on NiO, NiF2 and two other covalent complexes have been performed and different d–d transition patterns have been observed. Although still preliminary, this work on 3d metal complexes demonstrates the potential to use M-edge XAS and RIXS on more complicated 3d metal complexes in the future. The potential for using high-sensitivity and high-resolution superconducting tunnel junction X-ray detectors below 100 eV is also illustrated and discussed. PMID:23765304

  14. 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.

  15. Kinoform optics applied to X-ray photon correlation spectroscopy.

    PubMed

    Sandy, A R; Narayanan, S; Sprung, M; Su, J-D; Evans-Lutterodt, K; Isakovic, A F; Stein, A

    2010-05-01

    Moderate-demagnification higher-order silicon kinoform focusing lenses have been fabricated to facilitate small-angle X-ray photon correlation spectroscopy (XPCS) experiments. The geometric properties of such lenses, their focusing performance and their applicability for XPCS measurements are described. It is concluded that one-dimensional vertical X-ray focusing via silicon kinoform lenses significantly increases the usable coherent flux from third-generation storage-ring light sources for small-angle XPCS experiments.

  16. Soft x-ray spectroscopy of high pressure liquid.

    PubMed

    Qiao, Ruimin; Xia, Yujian; Feng, Xuefei; Macdougall, James; Pepper, John; Armitage, Kevin; Borsos, Jason; Knauss, Kevin G; Lee, Namhey; Allézy, Arnaud; Gilbert, Benjamin; MacDowell, Alastair A; Liu, Yi-Sheng; Glans, Per-Anders; Sun, Xuhui; Chao, Weilun; Guo, Jinghua

    2018-01-01

    We describe a new experimental technique that allows for soft x-ray spectroscopy studies (∼100-1000 eV) of high pressure liquid (∼100 bars). We achieve this through a liquid cell with a 100 nm-thick Si 3 N 4 membrane window, which is sandwiched by two identical O-rings for vacuum sealing. The thin Si 3 N 4 membrane allows soft x-rays to penetrate, while separating the high-pressure liquid under investigation from the vacuum required for soft x-ray transmission and detection. The burst pressure of the Si 3 N 4 membrane increases with decreasing size and more specifically is inversely proportional to the side length of the square window. It also increases proportionally with the membrane thickness. Pressures > 60 bars could be achieved for 100 nm-thick square Si 3 N 4 windows that are smaller than 65 μm. However, above a certain pressure, the failure of the Si wafer becomes the limiting factor. The failure pressure of the Si wafer is sensitive to the wafer thickness. Moreover, the deformation of the Si 3 N 4 membrane is quantified using vertical scanning interferometry. As an example of the performance of the high-pressure liquid cell optimized for total-fluorescence detected soft x-ray absorption spectroscopy (sXAS), the sXAS spectra at the Ca L edge (∼350 eV) of a CaCl 2 aqueous solution are collected under different pressures up to 41 bars.

  17. Soft x-ray spectroscopy of high pressure liquid

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Qiao, Ruimin; Xia, Yujian; Feng, Xuefei

    Here, we describe a new experimental technique that allows for soft x-ray spectroscopy studies (~100-1000 eV) of high pressure liquid (~100 bars). We achieve this through a liquid cell with a 100 nm-thick Si 3N 4 membrane window, which is sandwiched by two identical O-rings for vacuum sealing. The thin Si 3N 4 membrane allows soft x-rays to penetrate, while separating the high-pressure liquid under investigation from the vacuum required for soft x-ray transmission and detection. The burst pressure of the Si 3N 4 membrane increases with decreasing size and more specifically is inversely proportional to the side length ofmore » the square window. It also increases proportionally with the membrane thickness. Pressures > 60 bars could be achieved for 100 nm-thick square Si 3N 4 windows that are smaller than 65 μm. However, above a certain pressure, the failure of the Si wafer becomes the limiting factor. The failure pressure of the Si wafer is sensitive to the wafer thickness. Moreover, the deformation of the Si 3N 4 membrane is quantified using vertical scanning interferometry. As an example of the performance of the high-pressure liquid cell optimized for total-fluorescence detected soft x-ray absorption spectroscopy (sXAS), the sXAS spectra at the Ca L edge (~350 eV) of a CaCl 2 aqueous solution are collected under different pressures up to 41 bars.« less

  18. Soft x-ray spectroscopy of high pressure liquid

    DOE PAGES

    Qiao, Ruimin; Xia, Yujian; Feng, Xuefei; ...

    2018-01-01

    Here, we describe a new experimental technique that allows for soft x-ray spectroscopy studies (~100-1000 eV) of high pressure liquid (~100 bars). We achieve this through a liquid cell with a 100 nm-thick Si 3N 4 membrane window, which is sandwiched by two identical O-rings for vacuum sealing. The thin Si 3N 4 membrane allows soft x-rays to penetrate, while separating the high-pressure liquid under investigation from the vacuum required for soft x-ray transmission and detection. The burst pressure of the Si 3N 4 membrane increases with decreasing size and more specifically is inversely proportional to the side length ofmore » the square window. It also increases proportionally with the membrane thickness. Pressures > 60 bars could be achieved for 100 nm-thick square Si 3N 4 windows that are smaller than 65 μm. However, above a certain pressure, the failure of the Si wafer becomes the limiting factor. The failure pressure of the Si wafer is sensitive to the wafer thickness. Moreover, the deformation of the Si 3N 4 membrane is quantified using vertical scanning interferometry. As an example of the performance of the high-pressure liquid cell optimized for total-fluorescence detected soft x-ray absorption spectroscopy (sXAS), the sXAS spectra at the Ca L edge (~350 eV) of a CaCl 2 aqueous solution are collected under different pressures up to 41 bars.« less

  19. CONTIN XPCS: software for inverse transform analysis of X-ray photon correlation spectroscopy dynamics

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Andrews, Ross N.; Narayanan, Suresh; Zhang, Fan

    X-ray photon correlation spectroscopy (XPCS) and dynamic light scattering (DLS) reveal materials dynamics using coherent scattering, with XPCS permitting the investigation of dynamics in a more diverse array of materials than DLS. Heterogeneous dynamics occur in many material systems. The authors' recent work has shown how classic tools employed in the DLS analysis of heterogeneous dynamics can be extended to XPCS, revealing additional information that conventional Kohlrausch exponential fitting obscures. The present work describes the software implementation of inverse transform analysis of XPCS data. This software, calledCONTIN XPCS, is an extension of traditionalCONTINanalysis and accommodates the various dynamics encountered inmore » equilibrium XPCS measurements.« less

  20. CONTIN XPCS: software for inverse transform analysis of X-ray photon correlation spectroscopy dynamics

    DOE PAGES

    Andrews, Ross N.; Narayanan, Suresh; Zhang, Fan; ...

    2018-02-01

    X-ray photon correlation spectroscopy (XPCS) and dynamic light scattering (DLS) reveal materials dynamics using coherent scattering, with XPCS permitting the investigation of dynamics in a more diverse array of materials than DLS. Heterogeneous dynamics occur in many material systems. The authors' recent work has shown how classic tools employed in the DLS analysis of heterogeneous dynamics can be extended to XPCS, revealing additional information that conventional Kohlrausch exponential fitting obscures. The present work describes the software implementation of inverse transform analysis of XPCS data. This software, calledCONTIN XPCS, is an extension of traditionalCONTINanalysis and accommodates the various dynamics encountered inmore » equilibrium XPCS measurements.« less

  1. X-ray Absorption and Emission Spectroscopy of CrIII (Hydr)Oxides: Analysis of the K-Pre-Edge Region

    NASA Astrophysics Data System (ADS)

    Frommer, Jakob; Nachtegaal, Maarten; Czekaj, Izabela; Weng, Tsu-Chien; Kretzschmar, Ruben

    2009-10-01

    Pre-edge spectral features below the main X-ray absorption K-edge of transition metals show a pronounced chemical sensitivity and are promising sources of structural information. Nevertheless, the use of pre-edge analysis in applied research is limited because of the lack of definite theoretical peak-assignments. The aim of this study was to determine the factors affecting the chromium K-pre-edge features in trivalent chromium-bearing oxides and oxyhydroxides. The selected phases varied in the degree of octahedral polymerization and the degree of iron-for-chromium substitution in the crystal structure. We investigated the pre-edge fine structure by means of high-energy-resolution fluorescence detected X-ray absorption spectroscopy and by 1s2p resonant X-ray emission spectroscopy. Multiplet theory and full multiple-scattering calculations were used to analyze the experimental data. We show that the chromium K-pre-edge contains localized and nonlocalized transitions. Contributions arising from nonlocalized metal-metal transitions are sensitive to the nearest metal type and to the linkage mode between neighboring metal octahedra. Analyzing these transitions opens up new opportunities for investigating the local coordination environment of chromium in poorly ordered solids of environmental relevance.

  2. Soft X-ray spectroscopy of transition metal compounds: a theoretical perspective

    NASA Astrophysics Data System (ADS)

    Bokarev, S. I.; Hilal, R.; Aziz, S. G.; Kühn, O.

    2017-01-01

    To date, X-ray spectroscopy has become a routine tool that can reveal highly local and element-specific information on the electronic structure of atoms in complex environments. Here, we report on the development of an efficient and versatile theoretical methodology for the treatment of soft X-ray spectra of transition metal compounds based on the multi-configurational self-consistent field electronic structure theory. A special focus is put on the L-edge photon-in/photon-out and photon-in/electron-out processes, i.e. X-ray absorption, resonant inelastic scattering, partial fluorescence yield, and photoelectron spectroscopy, all treated on the same theoretical footing. The investigated systems range from small prototypical coordination compounds and catalysts to aggregates of biomolecules.

  3. X-Ray spectroscopy of cooling flows

    NASA Technical Reports Server (NTRS)

    Prestwich, Andrea

    1996-01-01

    Cooling flows in clusters of galaxies occur when the cooling time of the gas is shorter than the age of the cluster; material cools and falls to the center of the cluster potential. Evidence for short X-ray cooling times comes from imaging studies of clusters and X-ray spectroscopy of a few bright clusters. Because the mass accretion rate can be high (a few 100 solar mass units/year) the mass of material accumulated over the lifetime of a cluster can be as high as 10(exp 12) solar mass units. However, there is little evidence for this material at other wavelengths, and the final fate of the accretion material is unknown. X-ray spectra obtained with the Einstein SSS show evidence for absorption; if confirmed this result would imply that the accretion material is in the form of cool dense clouds. However ice on the SSS make these data difficult to interpret. We obtained ASCA spectra of the cooling flow cluster Abell 85. Our primary goals were to search for multi-temperature components that may be indicative of cool gas; search for temperature gradients across the cluster; and look for excess absorption in the cooling region.

  4. A reaction cell for ambient pressure soft x-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Castán-Guerrero, C.; Krizmancic, D.; Bonanni, V.; Edla, R.; Deluisa, A.; Salvador, F.; Rossi, G.; Panaccione, G.; Torelli, P.

    2018-05-01

    We present a new experimental setup for performing X-ray Absorption Spectroscopy (XAS) in the soft X-ray range at ambient pressure. The ambient pressure XAS setup is fully compatible with the ultra high vacuum environment of a synchrotron radiation spectroscopy beamline end station by means of ultrathin Si3N4 membranes acting as windows for the X-ray beam and seal of the atmospheric sample environment. The XAS detection is performed in total electron yield (TEY) mode by probing the drain current from the sample with a picoammeter. The high signal/noise ratio achievable in the TEY mode, combined with a continuous scanning of the X-ray energies, makes it possible recording XAS spectra in a few seconds. The first results show the performance of this setup to record fast XAS spectra from sample surfaces exposed at atmospheric pressure, even in the case of highly insulating samples. The use of a permanent magnet inside the reaction cell enables the measurement of X-ray magnetic circular dichroism at ambient pressure.

  5. Alternative difference analysis scheme combining R -space EXAFS fit with global optimization XANES fit for X-ray transient absorption spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Zhan, Fei; Tao, Ye; Zhao, Haifeng

    Time-resolved X-ray absorption spectroscopy (TR-XAS), based on the laser-pump/X-ray-probe method, is powerful in capturing the change of the geometrical and electronic structure of the absorbing atom upon excitation. TR-XAS data analysis is generally performed on the laser-on minus laser-off difference spectrum. Here, a new analysis scheme is presented for the TR-XAS difference fitting in both the extended X-ray absorption fine-structure (EXAFS) and the X-ray absorption near-edge structure (XANES) regions.R-space EXAFS difference fitting could quickly provide the main quantitative structure change of the first shell. The XANES fitting part introduces a global non-derivative optimization algorithm and optimizes the local structure changemore » in a flexible way where both the core XAS calculation package and the search method in the fitting shell are changeable. The scheme was applied to the TR-XAS difference analysis of Fe(phen) 3spin crossover complex and yielded reliable distance change and excitation population.« less

  6. 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.

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

    DOE PAGES

    March, Anne Marie; Assefa, Tadesse A.; Bressler, Christian; ...

    2015-02-09

    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. Here 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 formore » time-resolved experiments. Lastly, we discuss technical improvements that will make valence-to-core XES a practical pump–probe technique.« less

  8. Analysis of Ti and TiO2 nanolayers by total reflection X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Kubala-Kukuś, A.; Banaś, D.; Stabrawa, I.; Szary, K.; Sobota, D.; Majewska, U.; Wudarczyk-Moćko, J.; Braziewicz, J.; Pajek, M.

    2018-07-01

    Total reflection X-ray photoelectron spectroscopy (TRXPS) is applied in the analysis of Ti and TiO2 nanolayers deposited on silicon and silicon dioxide substrates. The idea of application of total-reflection phenomenon for exciting X-ray used in the XPS technique is briefly discussed. The experimental setup and measurement conditions for the studied Ti and TiO2 layers are presented. The XPS spectra were registered both for the non-total and total reflection regimes. The survey spectra and C1s, N1s, Ti2p and O1s photoelectron peaks are shown. For energy calibration, the position of C1s photoelectron peak was applied (C-C component, binding energy 284.8 eV). The peak to background ratios are discussed as regards the dependence of the excitation angle. An increase of this ratio for the glancing angle 1°, being below critical angle of the X-ray beam and sample material, results in an improvement of XPS detection limit by factor up to 2. In the case of the Ti nanolayer, additionally, the thickness of the overlayer TiO2 is determined. As an example of applying the TRXPS technique, the analysis of Ti nanolayers implanted by highly charged Xe35+ ions of 280 keV energy is discussed. The Xe3d and O1s photoelectron peaks are presented and discussed.

  9. 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

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

    DOE PAGES

    Picón, A.; Lehmann, C. S.; Bostedt, C.; ...

    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 XeF 2 molecules following X-ray absorption at the Xe site.« less

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

    PubMed

    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

    2016-05-23

    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. 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.

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

    NASA Astrophysics Data System (ADS)

    Mukamel, Shaul

    2017-04-01

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

  13. Elemental-sensitive Detection of the Chemistry in Batteries through Soft X-ray Absorption Spectroscopy and Resonant Inelastic X-ray Scattering.

    PubMed

    Wu, Jinpeng; Sallis, Shawn; Qiao, Ruimin; Li, Qinghao; Zhuo, Zengqing; Dai, Kehua; Guo, Zixuan; Yang, Wanli

    2018-04-17

    Energy storage has become more and more a limiting factor of today's sustainable energy applications, including electric vehicles and green electric grid based on volatile solar and wind sources. The pressing demand of developing high-performance electrochemical energy storage solutions, i.e., batteries, relies on both fundamental understanding and practical developments from both the academy and industry. The formidable challenge of developing successful battery technology stems from the different requirements for different energy-storage applications. Energy density, power, stability, safety, and cost parameters all have to be balanced in batteries to meet the requirements of different applications. Therefore, multiple battery technologies based on different materials and mechanisms need to be developed and optimized. Incisive tools that could directly probe the chemical reactions in various battery materials are becoming critical to advance the field beyond its conventional trial-and-error approach. Here, we present detailed protocols for soft X-ray absorption spectroscopy (sXAS), soft X-ray emission spectroscopy (sXES), and resonant inelastic X-ray scattering (RIXS) experiments, which are inherently elemental-sensitive probes of the transition-metal 3d and anion 2p states in battery compounds. We provide the details on the experimental techniques and demonstrations revealing the key chemical states in battery materials through these soft X-ray spectroscopy techniques.

  14. Probing molecular dynamics in solution with x-ray valence-to-core spectroscopy

    NASA Astrophysics Data System (ADS)

    Doumy, Gilles; March, Anne Marie; Tu, Ming-Feng; Al Haddad, Andre; Southworth, Stephen; Young, Linda; Walko, Donald; Bostedt, Christoph

    2017-04-01

    Hard X-ray spectroscopies are powerful tools for probing the electronic and geometric structure of molecules in complex or disordered systems and have been particularly useful for studying molecules in the solution phase. They are element specific, sensitive to the electronic structure and the local arrangements of surrounding atoms of the element being selectively probed. When combined in a pump-probe scheme with ultrafast lasers, X-ray spectroscopies can be used to track the evolution of structural changes that occur after photoexcitation. Efficient use of hard x-ray radiation coming from high brilliance synchrotrons and upcoming high repetition rate X-ray Free Electron Lasers requires MHz repetition rate lasers and data acquisition systems. High information content Valence-to-Core x-ray emission is directly sensitive to the molecular orbitals involved in photochemistry. We report on recent progress towards fully enabling this photon-hungry technique for the study of time-resolved molecular dynamics, including efficient detection and use of polychromatic x-ray micro-probe at the Advanced Photon Source. Work was supported by the U.S. Department of Energy, Office of Science, Chemical Sciences, Geosciences, and Biosciences Division.

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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Xiao, Y. M., E-mail: yxiao@carnegiescience.edu; Chow, P.; Boman, G.

    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.

  16. 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

  17. Investigation of nanoparticulate silicon as printed layers using scanning electron microscopy, transmission electron microscopy, X-ray absorption spectroscopy and X-ray photoelectron spectroscopy

    DOE PAGES

    Unuigbe, David M.; Harting, Margit; Jonah, Emmanuel O.; ...

    2017-08-21

    The presence of native oxide on the surface of silicon nanoparticles is known to inhibit charge transport on the surfaces. Scanning electron microscopy (SEM) studies reveal that the particles in the printed silicon network have a wide range of sizes and shapes. High-resolution transmission electron microscopy reveals that the particle surfaces have mainly the (111)- and (100)-oriented planes which stabilizes against further oxidation of the particles. X-ray absorption spectroscopy (XANES) and X-ray photoelectron spectroscopy (XPS) measurements at the O 1s-edge have been utilized to study the oxidation and local atomic structure of printed layers of silicon nanoparticles which were milledmore » for different times. XANES results reveal the presence of the +4 (SiO 2) oxidation state which tends towards the +2 (SiO) state for higher milling times. Si 2pXPS results indicate that the surfaces of the silicon nanoparticles in the printed layers are only partially oxidized and that all three sub-oxide, +1 (Si 2O), +2 (SiO) and +3 (Si 2O 3), states are present. The analysis of the change in the sub-oxide peaks of the silicon nanoparticles shows the dominance of the +4 state only for lower milling times.« less

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

    DOE PAGES

    Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; ...

    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. Kβ 1,3 XES spectra of Mn II and Mn 2 III,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

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

    PubMed Central

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

    2012-01-01

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

  20. Analysis of a measurement scheme for ultrafast hole dynamics by few femtosecond resolution X-ray pump-probe Auger spectroscopy.

    PubMed

    Cooper, Bridgette; Kolorenč, Přemysl; Frasinski, Leszek J; Averbukh, Vitali; Marangos, Jon P

    2014-01-01

    Ultrafast hole dynamics created in molecular systems as a result of sudden ionisation is the focus of much attention in the field of attosecond science. Using the molecule glycine we show through ab initio simulations that the dynamics of a hole, arising from ionisation in the inner valence region, evolves with a timescale appropriate to be measured using X-ray pulses from the current generation of SASE free electron lasers. The examined pump-probe scheme uses X-rays with photon energy below the K edge of carbon (275-280 eV) that will ionise from the inner valence region. A second probe X-ray at the same energy can excite an electron from the core to fill the vacancy in the inner-valence region. The dynamics of the inner valence hole can be tracked by measuring the Auger electrons produced by the subsequent refilling of the core hole as a function of pump-probe delay. We consider the feasibility of the experiment and include numerical simulation to support this analysis. We discuss the potential for all X-ray pump-X-ray probe Auger spectroscopy measurements for tracking hole migration.

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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Mascali, David, E-mail: davidmascali@lns.infn.it; Castro, Giuseppe; Celona, Luigi

    2016-02-15

    An experimental campaign aiming to investigate electron cyclotron resonance (ECR) plasma X-ray emission has been recently carried out at the ECRISs—Electron Cyclotron Resonance Ion Sources laboratory of Atomki based on a collaboration between the Debrecen and Catania ECR teams. In a first series, the X-ray spectroscopy was performed through silicon drift detectors and high purity germanium detectors, characterizing the volumetric plasma emission. The on-purpose developed collimation system was suitable for direct plasma density evaluation, performed “on-line” during beam extraction and charge state distribution characterization. A campaign for correlating the plasma density and temperature with the output charge states and themore » 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.« less

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

    NASA Astrophysics Data System (ADS)

    Milne, Chris J.; Pham, Van-Thai; Gawelda, Wojciech; van der Veen, Renske M.; El Nahhas, Amal; Johnson, Steven L.; Beaud, Paul; Ingold, Gerhard; Lima, Frederico; Vithanage, Dimali A.; Benfatto, Maurizio; Grolimund, Daniel; Borca, Camelia; Kaiser, Maik; Hauser, Andreas; Abela, Rafael; Bressler, Christian; Chergui, Majed

    2009-11-01

    The introduction of pump-probe techniques to the field of x-ray absorption spectroscopy (XAS) has allowed the monitoring of both structural and electronic dynamics of disordered systems in the condensed phase with unprecedented accuracy, both in time and in space. We present results on the electronically excited high-spin state structure of an Fe(II) molecular species, [FeII(bpy)3]2+, in aqueous solution, resolving the Fe-N bond distance elongation as 0.2 Å. In addition an analysis technique using the reduced χ2 goodness of fit between FEFF EXAFS simulations and the experimental transient absorption signal in energy space has been successfully tested as a function of excited state population and chemical shift, demonstrating its applicability in situations where the fractional excited state population cannot be determined through other measurements. Finally by using a novel ultrafast hard x-ray 'slicing' source the question of how the molecule relaxes after optical excitation has been successfully resolved using femtosecond XANES.

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

    PubMed

    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 atto-second 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

  4. Quarry identification of historical building materials by means of laser induced breakdown spectroscopy, X-ray fluorescence and chemometric analysis

    NASA Astrophysics Data System (ADS)

    Colao, F.; Fantoni, R.; Ortiz, P.; Vazquez, M. A.; Martin, J. M.; Ortiz, R.; Idris, N.

    2010-08-01

    To characterize historical building materials according to the geographic origin of the quarries from which they have been mined, the relative content of major and trace elements were determined by means of Laser Induced Breakdown Spectroscopy (LIBS) and X-ray Fluorescence (XRF) techniques. 48 different specimens were studied and the entire samples' set was divided in two different groups: the first, used as reference set, was composed by samples mined from eight different quarries located in Seville province; the second group was composed by specimens of unknown provenance collected in several historical buildings and churches in the city of Seville. Data reduction and analysis on laser induced breakdown spectroscopy and X-ray fluorescence measurements was performed using multivariate statistical approach, namely the Linear Discriminant Analysis (LDA), Principal Component Analysis (PCA) and Soft Independent Modeling of Class Analogy (SIMCA). A clear separation among reference sample materials mined from different quarries was observed in Principal Components (PC) score plots, then a supervised soft independent modeling of class analogy classification was trained and run, aiming to assess the provenance of unknown samples according to their elemental content. The obtained results were compared with the provenance assignments made on the basis of petrographical description. This work gives experimental evidence that laser induced breakdown spectroscopy measurements on a relatively small set of elements is a fast and effective method for the purpose of origin identification.

  5. Tracking reaction dynamics in solution by pump-probe X-ray absorption spectroscopy and X-ray liquidography (solution scattering).

    PubMed

    Kim, Jeongho; Kim, Kyung Hwan; Oang, Key Young; Lee, Jae Hyuk; Hong, Kiryong; Cho, Hana; Huse, Nils; Schoenlein, Robert W; Kim, Tae Kyu; Ihee, Hyotcherl

    2016-03-07

    Characterization of transient molecular structures formed during chemical and biological processes is essential for understanding their mechanisms and functions. Over the last decade, time-resolved X-ray liquidography (TRXL) and time-resolved X-ray absorption spectroscopy (TRXAS) have emerged as powerful techniques for molecular and electronic structural analysis of photoinduced reactions in the solution phase. Both techniques make use of a pump-probe scheme that consists of (1) an optical pump pulse to initiate a photoinduced process and (2) an X-ray probe pulse to monitor changes in the molecular structure as a function of time delay between pump and probe pulses. TRXL is sensitive to changes in the global molecular structure and therefore can be used to elucidate structural changes of reacting solute molecules as well as the collective response of solvent molecules. On the other hand, TRXAS can be used to probe changes in both local geometrical and electronic structures of specific X-ray-absorbing atoms due to the element-specific nature of core-level transitions. These techniques are complementary to each other and a combination of the two methods will enhance the capability of accurately obtaining structural changes induced by photoexcitation. Here we review the principles of TRXL and TRXAS and present recent application examples of the two methods for studying chemical and biological processes in solution. Furthermore, we briefly discuss the prospect of using X-ray free electron lasers for the two techniques, which will allow us to keep track of structural dynamics on femtosecond time scales in various solution-phase molecular reactions.

  6. Probing molecular orientations in thin films by x-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Li, Y.; Li, P.; Lu, Z.-H.

    2018-03-01

    A great number of functional organic molecules in active thin-film layers of optoelectronic devices have highly asymmetric structures, such as plate-like, rod-like, etc. This makes molecular orientation an important aspect in thin-films as it can significantly affect both the optical and electrical performance of optoelectronic devices. With a combination of in-situ ultra violet photoelectron spectroscopy (UPS) and x-ray photoelectron spectroscopy (XPS) investigations for organic molecules having a broad range of structural properties, we discovered a rigid connection of core levels and frontier highest occupied molecular orbital levels at organic interfaces. This finding opens up opportunities of using X-ray photoemission spectroscopy as an alternative tool to UPS for providing an easy and unambiguous data interpretation in probing molecular orientations.

  7. Note: application of a pixel-array area detector to simultaneous single crystal X-ray diffraction and X-ray absorption spectroscopy measurements.

    PubMed

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

    2014-04-01

    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 Pr0.67Sr0.33MnO3 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.

  8. Characterization of aluminum nitride based films with high resolution X-ray fluorescence spectroscopy

    NASA Astrophysics Data System (ADS)

    Anagnostopoulos, D. F.; Siozios, A.; Patsalas, P.

    2018-02-01

    X-ray fluorescence spectra of Al based films are measured, using a lab-scale wavelength dispersive flat crystal spectrometer. Various structures of AlN films were studied, like single layered, capped, stratified, nanostructured, crystalline, or amorphous. By optimizing the set-up for enhanced energy resolution and detection efficiency, the measured line shapes of Κα, Kβ, and KLL radiative Auger transitions are shown to be adequately detailed to allow chemical characterization. The chemistry identification is based on the pattern comparison of the emitted line shape from the chemically unknown film and the reference line shapes from standard materials, recorded under identical experimental conditions. The ultimate strength of lab-scale high resolution X-ray fluorescence spectroscopy on film analysis is verified, in cases that ordinary applied techniques like X-ray photoelectron and X-ray diffraction fail, while the characterization refers to the non-destructive determination of the bulk properties of the film and not to its surface, as the probed depth is in the micrometer range.

  9. 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.

  10. High-resolution X-ray emission spectroscopy with transition-edge sensors: present performance and future potential

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Uhlig, J.; Doriese, W. B.; Fowler, J. W.

    2015-04-21

    X-ray emission spectroscopy (XES) is a powerful element-selective tool to analyze the oxidation states of atoms in complex compounds, determine their electronic configuration, and identify unknown compounds in challenging environments. Until now the low efficiency of wavelength-dispersive X-ray spectrometer technology has limited the use of XES, especially in combination with weaker laboratory X-ray sources. More efficient energy-dispersive detectors have either insufficient energy resolution because of the statistical limits described by Fano or too low counting rates to be of practical use. This paper updates an approach to high-resolution X-ray emission spectroscopy that uses a microcalorimeter detector array of superconducting transition-edgemore » sensors (TESs). TES arrays are discussed and compared with conventional methods, and shown under which circumstances they are superior. It is also shown that a TES array can be integrated into a table-top time-resolved X-ray source and a soft X-ray synchrotron beamline to perform emission spectroscopy with good chemical sensitivity over a very wide range of energies.« less

  11. Development of picosecond time-resolved X-ray absorption spectroscopy by high-repetition-rate laser pump/X-ray probe at Beijing Synchrotron Radiation Facility.

    PubMed

    Wang, Hao; Yu, Can; Wei, Xu; Gao, Zhenhua; Xu, Guang Lei; Sun, Da Rui; Li, Zhenjie; Zhou, Yangfan; Li, Qiu Ju; Zhang, Bing Bing; Xu, Jin Qiang; Wang, Lin; Zhang, Yan; Tan, Ying Lei; Tao, Ye

    2017-05-01

    A new setup and commissioning of transient X-ray absorption spectroscopy are described, based on the high-repetition-rate laser pump/X-ray probe method, at the 1W2B wiggler beamline at the Beijing Synchrotron Radiation Facility. A high-repetition-rate and high-power laser is incorporated into the setup with in-house-built avalanche photodiodes as detectors. A simple acquisition scheme was applied to obtain laser-on and laser-off signals simultaneously. The capability of picosecond transient X-ray absorption spectroscopy measurement was demonstrated for a photo-induced spin-crossover iron complex in 6 mM solution with 155 kHz repetition rate.

  12. X-ray magnetic circular dichroism and hard X-ray photoelectron spectroscopy of tetragonal Mn72Ge28 epitaxial thin film

    NASA Astrophysics Data System (ADS)

    Kim, Jinhyeok; Mizuguchi, Masaki; Inami, Nobuhito; Ueno, Tetsuro; Ueda, Shigenori; Takanashi, Koki

    2018-04-01

    An epitaxially grown Mn72Ge28 film with a tetragonal crystal structure was fabricated. It was clarified that the film had a perpendicular magnetization and a high perpendicular magnetic anisotropy energy of 14.3 Merg/cm3. The electronic structure was investigated by X-ray magnetic circular dichroism and hard X-ray photoelectron spectroscopy. The obtained X-ray magnetic circular dichroism spectrum revealed that the Mn orbital magnetic moment governed the magnetocrystalline anisotropy of the Mn72Ge28 film. A doublet structure was observed for the Mn 2p3/2 peak of hard X-ray photoelectron spectrum, indicating the spin exchange interaction between the 2p core-hole and 3d valence electrons.

  13. Probing interfacial characteristics of rubrene/pentacene and pentacene/rubrene bilayers with soft X-ray spectroscopy.

    PubMed

    Seo, J H; Pedersen, T M; Chang, G S; Moewes, A; Yoo, K-H; Cho, S J; Whang, C N

    2007-08-16

    The electronic structure of rubrene/pentacene and pentacene/rubrene bilayers has been investigated using soft X-ray absorption spectroscopy, resonant X-ray emission spectroscopy, and density-functional theory calculations. X-ray absorption and emission measurements reveal that it has been possible to alter the lowest unoccupied and the highest occupied molecular orbital states of rubrene in rubrene/pentacene bilayer. In the reverse case, one gets p* molecular orbital states originating from the pentacene layer. Resonant X-ray emission spectra suggest a reduction in the hole-transition probabilities for the pentacene/rubrene bilayer in comparison to reference pentacene layer. For the rubrenepentacene structure, the hole-transition probability shows an increase in comparison to the rubrene reference. We also determined the energy level alignment of the pentacene-rubrene interface by using X-ray and ultraviolet photoelectron spectroscopy. From these comparisons, it is found that the electronic structure of the pentacene-rubrene interface has a strong dependence on interface characteristics which depends on the order of the layers used.

  14. Nanosecond X-ray Photon Correlation Spectroscopy on Magnetic Skyrmions

    DOE PAGES

    Seaberg, M. H.; Holladay, B.; Lee, J. C. T.; ...

    2017-08-09

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

  15. Nanosecond X-ray Photon Correlation Spectroscopy on Magnetic Skyrmions

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Seaberg, M. H.; Holladay, B.; Lee, J. C. T.

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

  16. X-Ray Spectroscopies of Warm Dense Matter

    NASA Astrophysics Data System (ADS)

    Hoidn, Oliver

    This dissertation provides a perspective on the role of x-ray spectroscopy and diffraction diagnostics in experimental studies of warm dense matter (WDM). The primary focus of the work I discuss is the development of techniques to measure the structure and state variables of laboratory-generated WDM with a view towards both phenomenlogy and placing contraints on theoretical models. I present techniques adapted to two experimental venues for WDM studies: large-scale laser plasma facilities and x-ray free electron lasers. My focus is on the latter, in the context of which I have studied a dose enhancement technique that exploits nonlocal heat transport in nanostructured targets and considered several aspects of optimizing x-ray diffraction measurements. This work came into play in beam runs at the Linac Coherent Light Source (LCLS) in which my group performed x-ray diffraction studies of several materials heated to eV-scale temperatures. The results from these experiments include confirmation of the persistence of long-range crystalline order upon heating of metal oxides to tens of eV temperarures on the 40 fs timescale. One material, MgO, additionally manifested a surprising anomalous early onset in delocalization of valence charge density, contradicting predictions of all models based on either ground state electronic structure or (high-energy density) plasma physics. This particular result outlines a future path for studies of ordered insulators heated to temperatures on the order of the band gap. Such experiments will offer strong tests of electronic strucure theory, implementing a scientific approach that sees measurement of real-space charge density via x-ray diffraction (XRD) as a particularly effectve means to constrain density functional theory (DFT)-based modeling of the solid state/plasma transitional regime.

  17. Pushing x-ray photon correlation spectroscopy beyond the continuous frame rate limit

    DOE PAGES

    Dufresne, Eric M.; Narayanan, Suresh; Sandy, Alec R.; ...

    2016-01-06

    We demonstrate delayed-frame X-ray Photon Correlation Spectroscopy with 120 microsecond time resolution, limited only by sample scattering rates, with a prototype Pixel-array detector capable of taking two image frames separated by 153 ns or less. Although the overall frame rate is currently limited to about 4 frame pairs per second, we easily measured millisecond correlation functions. In conclusion, this technology, coupled to the use of brighter synchrotrons such as Petra III or the NSLS-II should enable X-ray Photon Correlation Spectroscopy on microsecond time scales on a wider variety of materials.

  18. High-order multilayer coated blazed gratings for high resolution soft x-ray spectroscopy

    DOE PAGES

    Voronov, Dmitriy L.; Goray, Leonid I.; Warwick, Tony; ...

    2015-02-17

    A grand challenge in soft x-ray spectroscopy is to drive the resolving power of monochromators and spectrometers from the 10 4 achieved routinely today to well above 10 5. This need is driven mainly by the requirements of a new technique that is set to have enormous impact in condensed matter physics, Resonant Inelastic X-ray Scattering (RIXS). Unlike x-ray absorption spectroscopy, RIXS is not limited by an energy resolution dictated by the core-hole lifetime in the excitation process. Using much higher resolving power than used for normal x-ray absorption spectroscopy enables access to the energy scale of soft excitations inmore » matter. These excitations such as magnons and phonons drive the collective phenomena seen in correlated electronic materials such as high temperature superconductors. RIXS opens a new path to study these excitations at a level of detail not formerly possible. However, as the process involves resonant excitation at an energy of around 1 keV, and the energy scale of the excitations one would like to see are at the meV level, to fully utilize the technique requires the development of monochromators and spectrometers with one to two orders of magnitude higher energy resolution than has been conventionally possible. Here we investigate the detailed diffraction characteristics of multilayer blazed gratings. These elements offer potentially revolutionary performance as the dispersive element in ultra-high resolution x-ray spectroscopy. In doing so, we have established a roadmap for the complete optimization of the grating design. Traditionally 1st order gratings are used in the soft x-ray region, but we show that as in the optical domain, one can work in very high spectral orders and thus dramatically improve resolution without significant loss in efficiency.« less

  19. Calcium in the Oxygen-Evolving Complex: Structural and Mechanistic Role Determined by X-ray Spectroscopy

    PubMed Central

    Yachandra, Vittal K.; Yano, Junko

    2011-01-01

    This review describes the results from X-ray absorption spectroscopy studies that have contributed to an understanding of the role of Ca in the photosynthetic water oxidation reaction. The results include the first Mn, Ca and Sr X-ray spectroscopy studies using Ca or Sr-substituted PS II samples that established the presence of a MnCa heteronuclear structure and its orientation, and the most recent Sr X-ray spectroscopy study using biosynthetically prepared Sr-containing PS II in the various S-states that provide important insights into the requirement for Ca in the mechanism of the Mn4Ca catalytic center. PMID:21524917

  20. Lunar sample analysis. [X-ray photoemission and Auger spectroscopy of lunar glass

    NASA Technical Reports Server (NTRS)

    Housley, R. M.; Grant, R. W.; Cirlin, E. H.

    1979-01-01

    The surface composition of two samples from the highly shocked, glass-coated lunar basalt (12054) and from four glass-coated fragments from the 1-2 mm (14161) fines were examined by X-ray photoemission spectroscopy to determine whether the agglutination process itself is responsible for the difference between their surface and bulk compositions. Auger electron spectroscopy of glass balls from the 15425 and 74001 fines were analyzed to understand the nature, extent, and behavior of volatile phases associated with lunar volcanism. Initial results indicate that (1) volatiles, in the outer few atomic layers sampled, vary considerably from ball to ball; (2) variability over the surface of individual balls is smaller; (3) the dominant volatiles on the balls are S and Zn; and (4) other volatiles commonly observed are P, Cl, and K.

  1. X-ray Emission Line Spectroscopy of Nearby Galaxies

    NASA Astrophysics Data System (ADS)

    Wang, Daniel

    What are the origins of the diffuse soft X-ray emission from non-AGN galaxies? Preliminary analysis of XMM-Newton RGS spectra shows that a substantial fraction of the emission cannot arise from optically-thin thermal plasma, as commonly assumed, and may originate in charge exchange at the interface with neutral gas. We request the support for a comprehensive observing, data analysis, and modeling program to spectroscopically determine the origins of the emission. First, we will use our scheduled XMM-Newton AO-10 368 ks observations of the nearest compact elliptical galaxy M32 to obtain the first spectroscopic calibration of the cumulative soft X-ray emission from the old stellar population and will develop a spectral model for the charge exchange, as well as analysis tools to measure the spatial and kinematic properties of the X-ray line- emitting plasma. Second, we will characterize the truly diffuse emission from the hot plasma and/or its interplay with the neutral gas in a sample of galactic spheroids and active star forming/starburst regions in nearby galaxies observed by XMM-Newton. In particular, we will map out the spatial distributions of key emission lines and measure (or tightly constrain) the kinematics of hot plasma outflows for a few X-ray-emitting regions with high-quality RGS data. For galaxies with insufficient counting statistics in individual emission lines, we will conduct a spectral stacking analysis to constrain the average properties of the X-ray-emitting plasma. We will use the results of these X-ray spectroscopic analyses, together with complementary X-ray CCD imaging/spectral data and observations in other wavelength bands, to test the models of the emission. In addition to the charge exchange, alternative scenarios such as resonance scattering and relic AGN photo-ionization will also be examined for suitable regions. These studies are important to the understanding of the relationship between the diffuse soft X-ray emission and various

  2. Structure of the manganese complex in photosystem II: insights from X-ray spectroscopy.

    PubMed Central

    Yachandra, Vittal K

    2002-01-01

    We have used Mn K-edge absorption and Kbeta emission spectroscopy 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; this technique can be characterized as a Raman process that uses K-edge energies (1s to 4p, ca. 6550 eV) to obtain L-edge-like spectra (2p to 3d, ca. 650 eV). The relevance of these data to the oxidation states and structure of the Mn complex is presented. We have obtained extended X-ray absorption fine structure data from the S(0) and S(3) 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 and 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. PMID:12437873

  3. 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.

  4. X-ray scattering and spectroscopy studies on diesel soot from oxygenated fuel under various engine load conditions

    USGS Publications Warehouse

    Braun, Andreas; Shah, N.; Huggins, Frank E.; Kelly, K.E.; Sarofim, A.; Jacobsen, C.; Wirick, S.; Francis, H.; Ilavsky, J.; Thomas, G.E.; Huffman, G.P.

    2005-01-01

    Diesel soot from reference diesel fuel and oxygenated fuel under idle and load engine conditions was investigated with X-ray scattering and X-ray carbon K-edge absorption spectroscopy. Up to five characteristic size ranges were found. Idle soot was generally found to have larger primary particles and aggregates but smaller crystallites, than load soot. Load soot has a higher degree of crystallinity than idle soot. Adding oxygenates to diesel fuel enhanced differences in the characteristics of diesel soot, or even reversed them. Aromaticity of idle soot from oxygenated diesel fuel was significantly larger than from the corresponding load soot. Carbon near-edge X-ray absorption fine structure (NEXAFS) spectroscopy was applied to gather information about the presence of relative amounts of carbon double bonds (CC, CO) and carbon single bonds (C-H, C-OH, COOH). Using scanning X-ray transmission microspectroscopy (STXM), the relative amounts of these carbon bond states were shown to vary spatially over distances approximately 50 to 100 nm. The results from the X-ray techniques are supported by thermo-gravimetry analysis and high-resolution transmission electron microscopy. ?? 2005 Elsevier Ltd. All rights reserved.

  5. Rolf Mewe: a career devoted to X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Kaastra, Jelle S.; Mewe, Rolf

    2005-06-01

    An overview of the life and work of Rolf Mewe (1935-2004) as an X-ray spectroscopist is given. He was one of the pioneers in the field of X-ray spectroscopy. His work illustrates nicely how this field developed from the early days up to the present high-resolution era. His plasma emission codes, developed by him and collaborators over several decades, is one of the most widely used. His thorough knowledge of the field, as well as his ability and enthousiasm to cooperate with many colleagues, made his career a succes. He will be missed by all of us for his work and personality.

  6. Synchrotron-based ambient pressure X-ray photoelectron spectroscopy of hydrogen and helium

    NASA Astrophysics Data System (ADS)

    Zhong, Jian-Qiang; Wang, Mengen; Hoffmann, William H.; van Spronsen, Matthijs A.; Lu, Deyu; Boscoboinik, J. Anibal

    2018-02-01

    Contrary to popular belief, it is possible to obtain X-ray photoelectron spectra for elements lighter than lithium, namely hydrogen and helium. The literature is plagued with claims of this impossibility, which holds true for lab-based X-ray sources. However, this limitation is merely technical and is related mostly to the low X-ray photoionization cross-sections of the 1s orbitals of hydrogen and helium. In this letter, we show that, using ambient pressure X-ray photoelectron spectroscopy (XPS), a bright-enough X-ray source allows the study of these elusive elements. This has important implications in the understanding of the limitations of one of the most useful techniques in materials science, and moreover, it potentially opens the possibility of using XPS to directly study the most abundant element in the universe.

  7. A Broadband X-Ray Imaging Spectroscopy with High-Angular Resolution: the FORCE Mission

    NASA Technical Reports Server (NTRS)

    Mori, Koji; Tsuru, Takeshi Go; Nakazawac, Kazuhiro; Ueda, Yoshihiro; Okajima, Takashi; Murakami, Hiroshi; Awaki, Hisamitsu; Matsumoto, Hironori; Fukazawai, Yasushi; Tsunemi, Hiroshi; hide

    2016-01-01

    We are proposing FORCE (Focusing On Relativistic universe and Cosmic Evolution) as a future Japan-lead X-ray observatory to be launched in the mid 2020s. Hitomi (ASTRO-H) possesses a suite of sensitive instruments enabling the highest energy-resolution spectroscopy in soft X-ray band, a broadband X-ray imaging spectroscopy in soft and hard X-ray bands, and further high energy coverage up to soft gamma-ray band. FORCE is the direct successor to the broadband X-ray imaging spectroscopy aspect of Hitomi (ASTRO-H) with significantly higher angular resolution. The current design of FORCE defines energy band pass of 1-80 keV with angular resolution of <15" in half-power diameter, achieving a 10 times higher sensitivity above 10 keV compared to any previous missions with simultaneous soft X-ray coverage. Our primary scientific objective is to trace the cosmic formation history by searching for "missing black holes" in various mass-scales: "buried supermassive black holes (SMBHs)" (> 10(exp 4) Stellar Mass) residing in the center of galaxies in a cosmological distance, "intermediate-mass black holes" (10(exp 2)-(10(exp 4) Stellar Mass) acting as the possible seeds from which SMBHs grow, and "orphan stellar-mass black holes" (< 10(exp 2) Stellar Mass) without companion in our Galaxy. In addition to these missing BHs, hunting for the nature of relativistic particles at various astrophysical shocks is also in our scope, utilizing the broadband X-ray coverage with high angular-resolution. FORCE are going to open a new era in these fields. The satellite is proposed to be launched with the Epsilon vehicle that is a Japanese current solid-fuel rocket. FORCE carries three identical pairs of Super-mirror and wide-band X-ray detector. The focal length is currently planned to be 10 m. The silicon mirror with multi-layer coating is our primary choice to achieve lightweight, good angular optics. The detector is a descendant of hard X-ray imager onboard Hitomi (ASTRO-H) replacing its

  8. An alignment method for mammographic X-ray spectroscopy under clinical conditions.

    PubMed

    Miyajima, S; Imagawa, K; Matsumoto, M

    2002-09-01

    This paper describes an alignment method for mammographic X-ray spectroscopy under clinical conditions. A pinhole, a fluorescent screen, a laser device and the case for a detector are used for alignment of the focal spot, a collimator and a detector. The method determines the line between the focal spot and the point of interest in an X-ray field radiographically. The method allows alignment for both central axis and off-axis directions.

  9. Simulated 'On-Line' Wear Metal Analysis of Lubricating Oils by X-Ray Fluorescence Spectroscopy

    NASA Technical Reports Server (NTRS)

    Kelliher, Warren C.; Partos, Richard D.; Nelson, Irina

    1996-01-01

    The objective of this project was to assess the sensitivity of X-ray Fluorescence Spectroscopy (XFS) for quantitative evaluation of metal particle content in engine oil suspensions and the feasibility of real-time, dynamic wear metal analysis. The study was focused on iron as the majority wear metal component. Variable parameters were: particle size, particle concentration and oil velocity. A commercial XFS spectrometer equipped with interchangeable static/dynamic (flow cell) sample chambers was used. XFS spectra were recorded for solutions of Fe-organometallic standard and for a series of DTE oil suspensions of high purity spherical iron particles of 2g, 4g, and 8g diameter, at concentrations from 5 ppm to 5,000 ppm. Real contaminated oil samples from Langley Air Force Base aircraft engines and NASA Langley Research Center wind tunnels were also analyzed. The experimental data conform the reliability of XFS as the analytical method of choice for this project. Intrinsic inadequacies of the instrument for precise analytic work at low metal concentrations were identified as being related to the particular x-ray beam definition, system geometry, and flow-cell materials selection. This work supports a proposal for the design, construction and testing of a conceptually new, miniature XFS spectrometer with superior performance, dedicated to on-line, real-time monitoring of lubricating oils in operating engines. Innovative design solutions include focalization of the incident x-ray beam, non-metal sample chamber, and miniaturization of the overall assembly. The instrument would contribute to prevention of catastrophic engine failures. A proposal for two-year funding has been presented to NASA Langley Research Center Internal Operation Group (IOG) Management, to continue the effort begun by this summer's project.

  10. Synchrotron-based ambient pressure X-ray photoelectron spectroscopy of hydrogen and helium

    DOE PAGES

    Zhong, Jian-Qiang; Wang, Mengen; Hoffmann, William H.; ...

    2018-03-01

    Contrary to popular belief, it is possible to obtain X-ray photoelectron spectra for elements lighter than lithium, namely hydrogen and helium. The literature is plagued with claims of this impossibility, which holds true for lab-based X-ray sources. However, this limitation is merely technical and is related mostly to the low X-ray photoionization cross-sections of the 1s orbitals of hydrogen and helium. Here, we show that, using ambient pressure X-ray photoelectron spectroscopy (XPS), a bright-enough X-ray source allows the study of these elusive elements. This has important implications in the understanding of the limitations of one of the most useful techniquesmore » in materials science, and moreover, it potentially opens the possibility of using XPS to directly study the most abundant element in the universe.« less

  11. Synchrotron-based ambient pressure X-ray photoelectron spectroscopy of hydrogen and helium

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Zhong, Jian-Qiang; Wang, Mengen; Hoffmann, William H.

    Contrary to popular belief, it is possible to obtain X-ray photoelectron spectra for elements lighter than lithium, namely hydrogen and helium. The literature is plagued with claims of this impossibility, which holds true for lab-based X-ray sources. However, this limitation is merely technical and is related mostly to the low X-ray photoionization cross-sections of the 1s orbitals of hydrogen and helium. Here, we show that, using ambient pressure X-ray photoelectron spectroscopy (XPS), a bright-enough X-ray source allows the study of these elusive elements. This has important implications in the understanding of the limitations of one of the most useful techniquesmore » in materials science, and moreover, it potentially opens the possibility of using XPS to directly study the most abundant element in the universe.« less

  12. Investigating the local structure of B-site cations in (1-x)BaTiO3-xBiScO3 and (1-x)PbTiO3-xBiScO3 using X-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Blanchard, Peter E. R.; Grosvenor, Andrew P.

    2018-05-01

    The structural properties of (1-x)BaTiO3-xBiScO3 and (1-x)PbTiO3-xBiScO3 were investigated using powder X-ray diffraction and X-ray absorption spectroscopy. Diffraction measurements confirmed that substituting small amounts of BiScO3 into BaTiO3 initially stabilizes a cubic phase at x = 0.2 before impurity phases begin to form at x = 0.5. BiScO3 substitution also resulted in noticeable changes in the local coordination environment of Ti4+. X-ray absorption near-edge spectroscopy (XANES) analysis showed that replacing Ti4+ with Sc3+ results in an increase in the off-centre displacement of Ti4+ cations. Surprisingly, BiScO3 substitution has no effect on the displacement of the Ti4+ cation in the (1-x)PbTiO3-xBiScO3 solid solution.

  13. Enabling liquid solvent structure analysis using hard x-ray absorption spectroscopy with a transferrable microfluidic reactor

    NASA Astrophysics Data System (ADS)

    Zheng, Jian; Zhang, Wei; Wang, Feng; Yu, Xiao-Ying

    2018-05-01

    In this paper, a vacuum compatible microfluidic device, system for analysis at the liquid vacuum interface, is integrated to hard x-ray absorption spectroscopy to obtain the local structure of K3[Fe(CN)6] in aqueous solutions with three concentrations of 0.5 M, 0.05 M, and 0.005 M. The solutions were sealed in a microchannel 500 µm wide and 300 µm deep in a portable microfluidic device. The Fe K-edge x-ray absorption spectra indicate a presence of Fe(III) in the complex in water, with an octahedral geometry coordinated with 6 C atoms in the first shell with a distance of ~1.92 Å and 6 N atoms in the second shell with a distance of ~3.10 Å. Varying the concentration has no observable influence on the structure of K3[Fe(CN)6]. Our results demonstrate the feasibility of using microfluidic based liquid cells in large synchrotron facilities. Using portable microfludic reactors provides a viable approach to enable multifaceted measurements of liquids in the future.

  14. Enabling liquid solvent structure analysis using hard x-ray absorption spectroscopy with a transferrable microfluidic reactor.

    PubMed

    Zheng, Jian; Zhang, Wei; Wang, Feng; Yu, Xiao-Ying

    2018-05-10

    In this paper, a vacuum compatible microfluidic device, system for analysis at the liquid vacuum interface, is integrated to hard x-ray absorption spectroscopy to obtain the local structure of K 3 [Fe(CN) 6 ] in aqueous solutions with three concentrations of 0.5 M, 0.05 M, and 0.005 M. The solutions were sealed in a microchannel 500 µm wide and 300 µm deep in a portable microfluidic device. The Fe K-edge x-ray absorption spectra indicate a presence of Fe(III) in the complex in water, with an octahedral geometry coordinated with 6 C atoms in the first shell with a distance of ~1.92 Å and 6 N atoms in the second shell with a distance of ~3.10 Å. Varying the concentration has no observable influence on the structure of K 3 [Fe(CN) 6 ]. Our results demonstrate the feasibility of using microfluidic based liquid cells in large synchrotron facilities. Using portable microfludic reactors provides a viable approach to enable multifaceted measurements of liquids in the future.

  15. Enabling liquid solvent structure analysis using hard x-ray absorption spectroscopy with a transferrable microfluidic reactor

    DOE PAGES

    Zheng, Jian; Zhang, Wei; Wang, Feng; ...

    2018-04-11

    In this study, a vacuum compatible microfluidic device, system for analysis at the liquid vacuum interface, is integrated to hard x-ray absorption spectroscopy to obtain the local structure of K 3[Fe(CN) 6] in aqueous solutions with three concentrations of 0.5 M, 0.05 M, and 0.005 M. The solutions were sealed in a microchannel 500 µm wide and 300 µm deep in a portable microfluidic device. The Fe K-edge x-ray absorption spectra indicate a presence of Fe(III) in the complex in water, with an octahedral geometry coordinated with 6 C atoms in the first shell with a distance of ~1.92 Åmore » and 6 N atoms in the second shell with a distance of ~3.10 Å. Varying the concentration has no observable influence on the structure of K 3[Fe(CN) 6]. Our results demonstrate the feasibility of using microfluidic based liquid cells in large synchrotron facilities. Using portable microfludic reactors provides a viable approach to enable multifaceted measurements of liquids in the future.« less

  16. Enabling liquid solvent structure analysis using hard x-ray absorption spectroscopy with a transferrable microfluidic reactor

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Zheng, Jian; Zhang, Wei; Wang, Feng

    In this study, a vacuum compatible microfluidic device, system for analysis at the liquid vacuum interface, is integrated to hard x-ray absorption spectroscopy to obtain the local structure of K 3[Fe(CN) 6] in aqueous solutions with three concentrations of 0.5 M, 0.05 M, and 0.005 M. The solutions were sealed in a microchannel 500 µm wide and 300 µm deep in a portable microfluidic device. The Fe K-edge x-ray absorption spectra indicate a presence of Fe(III) in the complex in water, with an octahedral geometry coordinated with 6 C atoms in the first shell with a distance of ~1.92 Åmore » and 6 N atoms in the second shell with a distance of ~3.10 Å. Varying the concentration has no observable influence on the structure of K 3[Fe(CN) 6]. Our results demonstrate the feasibility of using microfluidic based liquid cells in large synchrotron facilities. Using portable microfludic reactors provides a viable approach to enable multifaceted measurements of liquids in the future.« less

  17. Enabling liquid solvent structure analysis using hard x-ray absorption spectroscopy with a transferrable microfluidic reactor

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Zheng, Jian; Zhang, Wei; Wang, Feng

    In this paper, a vacuum compatible microfluidic device, System for Analysis at the Liquid Vacuum Interface (SALVI), is integrated to hard x-ray absorption spectroscopy (XAS) to obtain the local structure of K3[Fe(CN)6] in aqueous solutions with three concentrations of 0.5 M, 0.05 M, and 0.005 M. The solutions were sealed in a microchannel of 500 μm wide and 300 µm deep in a portable microfluidic device. The Fe K-edge x-ray absorption spectra show that the complex in water is Fe(III). The complex is present with octahedral geometry coordinated with 6 C atoms in the first shell with a distance ofmore » ~1.92 Å and 6 N atoms in the second shell with a distance of ~3.10 Å. Varying the concentration has no observable influence on the structure of K3[Fe(CN)6]. Our results demonstrate the feasibility of using microfluidic based liquid cells in large synchrotron facilities and it is a viable approach to enable multifaceted measurements of liquids in the future.« less

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

    NASA Astrophysics Data System (ADS)

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

    2016-07-01

    We are proposing FORCE (Focusing On Relativistic universe and Cosmic Evolution) as a future Japan-lead Xray observatory to be launched in the mid 2020s. Hitomi (ASTRO-H) possesses a suite of sensitive instruments enabling the highest energy-resolution spectroscopy in soft X-ray band, a broadband X-ray imaging spectroscopy in soft and hard X-ray bands, and further high energy coverage up to soft gamma-ray band. FORCE is the direct successor to the broadband X-ray imaging spectroscopy aspect of Hitomi (ASTRO-H) with significantly higher angular resolution. The current design of FORCE defines energy band pass of 1-80 keV with angular resolution of < 15 in half-power diameter, achieving a 10 times higher sensitivity above 10 keV compared to any previous missions with simultaneous soft X-ray coverage. Our primary scientific objective is to trace the cosmic formation history by searching for "missing black holes" in various mass-scales: "buried supermassive black holes (SMBHs)" (> 104 M⊙) residing in the center of galaxies in a cosmological distance, "intermediate-mass black holes" (102-104 M⊙) acting as the possible seeds from which SMBHs grow, and "orphan stellar-mass black holes" (< 102 M⊙) without companion in our Galaxy. In addition to these missing BHs, hunting for the nature of relativistic particles at various astrophysical shocks is also in our scope, utilizing the broadband X-ray coverage with high angular-resolution. FORCE are going to open a new era in these fields. The satellite is proposed to be launched with the Epsilon vehicle that is a Japanese current solid-fuel rocket. FORCE carries three identical pairs of Super-mirror and wide-band X-ray detector. The focal length is currently planned to be 10 m. The silicon mirror with multi-layer coating is our primary choice to achieve lightweight, good angular optics. The detector is a descendant of hard X-ray imager onboard Hitomi (ASTRO-H) replacing its silicon strip detector with SOI-CMOS silicon pixel

  19. Composition Analysis of III-Nitrides at the Nanometer Scale: Comparison of Energy Dispersive X-ray Spectroscopy and Atom Probe Tomography.

    PubMed

    Bonef, Bastien; Lopez-Haro, Miguel; Amichi, Lynda; Beeler, Mark; Grenier, Adeline; Robin, Eric; Jouneau, Pierre-Henri; Mollard, Nicolas; Mouton, Isabelle; Monroy, Eva; Bougerol, Catherine

    2016-12-01

    The enhancement of the performance of advanced nitride-based optoelectronic devices requires the fine tuning of their composition, which has to be determined with a high accuracy and at the nanometer scale. For that purpose, we have evaluated and compared energy dispersive X-ray spectroscopy (EDX) in a scanning transmission electron microscope (STEM) and atom probe tomography (APT) in terms of composition analysis of AlGaN/GaN multilayers. Both techniques give comparable results with a composition accuracy better than 0.6 % even for layers as thin as 3 nm. In case of EDX, we show the relevance of correcting the X-ray absorption by simultaneous determination of the mass thickness and chemical composition at each point of the analysis. Limitations of both techniques are discussed when applied to specimens with different geometries or compositions.

  20. Microreactor Cells for High-Throughput X-ray Absorption Spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Beesley, Angela; Tsapatsaris, Nikolaos; Weiher, Norbert

    2007-01-19

    High-throughput experimentation has been applied to X-ray Absorption spectroscopy as a novel route for increasing research productivity in the catalysis community. Suitable instrumentation has been developed for the rapid determination of the local structure in the metal component of precursors for supported catalysts. An automated analytical workflow was implemented that is much faster than traditional individual spectrum analysis. It allows the generation of structural data in quasi-real time. We describe initial results obtained from the automated high throughput (HT) data reduction and analysis of a sample library implemented through the 96 well-plate industrial standard. The results show that a fullymore » automated HT-XAS technology based on existing industry standards is feasible and useful for the rapid elucidation of geometric and electronic structure of materials.« less

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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    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 themore » 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.« less

  2. 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.

  3. Infrared x-ray pump-probe spectroscopy of the NO molecule

    NASA Astrophysics Data System (ADS)

    Guimarães, F. F.; Kimberg, V.; Felicíssimo, V. C.; Gel'Mukhanov, F.; Cesar, A.; Ågren, H.

    2005-07-01

    Two color infrared x-ray pump-probe spectroscopy of the NO molecule is studied theoretically and numerically in order to obtain a deeper insight of the underlying physics and of the potential of this suggested technology. From the theoretical investigation a number of conclusions could be drawn: It is found that the phase of the infrared field strongly influences the trajectory of the nuclear wave packet, and hence, the x-ray spectrum. The trajectory experiences fast oscillations with the vibrational frequency with a modulation due to the anharmonicity of the potential. The dependences of the x-ray spectra on the delay time, the duration, and the shape of the pulses are studied in detail. It is shown that the x-ray spectrum keep memory about the infrared phase after the pump field left the system. This memory effect is sensitive to the time of switching-off the pump field and the Rabi frequency. The phase effect takes maximum value when the duration of the x-ray pulse is one-fourth of the infrared field period, and can be enhanced by a proper control of the duration and intensity of the pump pulse. The manifestation of the phase is different for oriented and disordered molecules and depends strongly on the intensity of the pump radiation.

  4. Diamond sensors and polycapillary lenses for X-ray absorption spectroscopy.

    PubMed

    Ravel, B; Attenkofer, K; Bohon, J; Muller, E; Smedley, J

    2013-10-01

    Diamond sensors are evaluated as incident beam monitors for X-ray absorption spectroscopy experiments. These single crystal devices pose a challenge for an energy-scanning experiment using hard X-rays due to the effect of diffraction from the crystalline sensor at energies which meet the Bragg condition. This problem is eliminated by combination with polycapillary lenses. The convergence angle of the beam exiting the lens is large compared to rocking curve widths of the diamond. A ray exiting one capillary from the lens meets the Bragg condition for any reflection at a different energy from the rays exiting adjacent capillaries. This serves to broaden each diffraction peak over a wide energy range, allowing linear measurement of incident intensity over the range of the energy scan. Extended X-ray absorption fine structure data are measured with a combination of a polycapillary lens and a diamond incident beam monitor. These data are of comparable quality to data measured without a lens and with an ionization chamber monitoring the incident beam intensity.

  5. 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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Szlachetko, J.; Institute of Physics, Jan Kochanowski University, 25-406 Kielce; Nachtegaal, M.

    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.

  6. Tenth International Colloquium on UV and X-Ray Spectroscopy of Astrophysical and Laboratory Plasmas

    NASA Astrophysics Data System (ADS)

    Silver, Eric H.; Kahn, Steven M.

    UV and X-ray spectroscopy of astrophysical and laboratory plasmas draws interest from many disciplines. Contributions from international specialists are collected together in this book from a timely recent conference. In astrophysics, the Hubble Space Telescope, Astro 1 and ROSAT observatories are now providing UV and X-ray spectra and images of cosmic sources in unprecedented detail, while the Yohkoh mission recently collected superb data on the solar corona. In the laboratory, the development of ion-trap facilities and novel laser experiments are providing vital new data on high temperature plasmas. Recent innovations in the technology of spectroscopic instrumentation are discussed. These papers constitute an excellent up-to-date review of developments in short-wavelength spectroscopy and offer a solid introduction to its theoretical and experimental foundations. These proceedings give an up-to-date review of developments in short-wavelength spectroscopy and offer a solid introduction to its theoretical and experimental foundations. Various speakers presented some of the first results from the high resolution spectrograph on the Hubble Space Telescope, the high sensitivity far ultraviolet and X-ray spectrometers of the ASTRO 1 Observatory, the imaging X-ray spectrometer on the ROSAT Observatory, and the high resolution solar X-ray spectrometer on Yohkoh. The development of ion trap devices had brought about a revolution in laboratory investigations of atomic processes in highly charged atoms. X-ray laser experiments had not only yielded considerable insight into electron ion interactions in hot dense plasmas, but also demonstrated the versatility of laser plasmas as laboratory X-ray sources. Such measurements also motivated and led to refinements in the development of large-scale atomic and molecular codes. On the instrumental side, the design and development of the next series of very powerful short wavelength observatories had generated a large number of

  7. High-rate x-ray spectroscopy in mammography with a CdTe detector: a digital pulse processing approach.

    PubMed

    Abbene, L; Gerardi, G; Principato, F; Del Sordo, S; Ienzi, R; Raso, G

    2010-12-01

    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. 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. 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. These results make the proposed detection system a very attractive tool for both laboratory research and advanced quality controls in mammography.

  8. Chemical Modification of Graphene Oxide by Nitrogenation: An X-ray Absorption and Emission Spectroscopy Study

    DOE PAGES

    Chuang, Cheng-Hao; Ray, Sekhar C.; Mazumder, Debarati; ...

    2017-02-10

    Nitrogen-doped graphene oxides (GO:N x) were synthesized by a partial reduction of graphene oxide (GO) using urea [CO(NH 2) 2 ]. Their electronic/bonding structures were investigated using X-ray absorption near-edge structure (XANES), valence-band photoemission spectroscopy (VB-PES), X-ray emission spectroscopy (XES) and resonant inelastic X-ray scattering (RIXS). During GO:N x synthesis, different nitrogen-bonding species, such as pyrrolic/graphitic-nitrogen, were formed by replacing of oxygen-containing functional groups. At lower N-content (2.7 at%), pyrrolic-N, owing to surface and subsurface diffusion of C, N and NH is deduced from various X-ray spectroscopies. In contrast, at higher N-content (5.0 at%) graphitic nitrogen was formed in whichmore » each N-atom trigonally bonds to three distinct sp 2 -hybridized carbons with substitution of the N-atoms for C atoms in the graphite layer. Upon nitrogen substitution, the total density of state close to Fermi level is increased to raise the valence-band maximum, as revealed by VB-PES spectra, indicating an electron donation from nitrogen, molecular bonding C/N/O coordination or/and lattice structure reorganization in GO:N x . The well-ordered chemical environments induced by nitrogen dopant are revealed by XANES and RIXS measurements.« less

  9. Deconvolving instrumental and intrinsic broadening in core-shell x-ray spectroscopies

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Fister, T. T.; Seidler, G. T.; Rehr, J. J.

    2007-05-01

    Intrinsic and experimental mechanisms frequently lead to broadening of spectral features in core-shell spectroscopies. For example, intrinsic broadening occurs in x-ray absorption spectroscopy (XAS) measurements of heavy elements where the core-hole lifetime is very short. On the other hand, nonresonant x-ray Raman scattering (XRS) and other energy loss measurements are more limited by instrumental resolution. Here, we demonstrate that the Richardson-Lucy (RL) iterative algorithm provides a robust method for deconvolving instrumental and intrinsic resolutions from typical XAS and XRS data. For the K-edge XAS of Ag, we find nearly complete removal of {approx}9.3 eV full width at half maximum broadeningmore » from the combined effects of the short core-hole lifetime and instrumental resolution. We are also able to remove nearly all instrumental broadening in an XRS measurement of diamond, with the resulting improved spectrum comparing favorably with prior soft x-ray XAS measurements. We present a practical methodology for implementing the RL algorithm in these problems, emphasizing the importance of testing for stability of the deconvolution process against noise amplification, perturbations in the initial spectra, and uncertainties in the core-hole lifetime.« less

  10. STROBE-X: X-ray Timing & Spectroscopy on Dynamical Timescales from Milliseconds to Years

    NASA Technical Reports Server (NTRS)

    Wilson-Hodge, Colleen A.; Ray, P. S.; Maccarone, T; Chakrabarty, D.; Gendreau, K.; Arzoumanian, Z.; Jenke, P.; Ballantyne, D.; Bozzo, E.; Brandt, S.; hide

    2018-01-01

    We describe a probe-class mission concept that provides an unprecedented view of the X-ray sky, performing timing and 0.2-30 keV spectroscopy over timescales from microseconds to years. The Spectroscopic Time-Resolving Observatory for Broadband Energy X-rays (STROBE-X) comprises three primary instruments. The first uses an array of lightweight optics (3-m focal length) that concentrate incident photons onto solid state detectors with CCD-level (85-130 eV) energy resolution, 100 ns time resolution, and low background rates to cover the 0.2-12 keV band. This technology is scaled up from NICER [1], with enhanced optics to take advantage of the longer focal length of STROBE-X. The second uses large-area collimated silicon drift detectors, developed for ESA's LOFT [2], to cover the 2-30 keV band. These two instruments each provide an order of magnitude improvement in effective area compared with its predecessor (NICER and RXTE, respectively). Finally, a sensitive sky monitor triggers pointed observations, provides high duty cycle, high time resolution, high spectral resolution monitoring of the X-ray sky with approx. 20 times the sensitivity of the RXTE ASM, and enables multi-wavelength and multi-messenger studies on a continuous, rather than scanning basis. For the first time, the broad coverage provides simultaneous study of thermal components, non-thermal components, iron lines, and reflection features from a single platform for accreting black holes at all scales. The enormous collecting area allows detailed studies of the dense matter equation of state using both thermal emission from rotation-powered pulsars and harder emission from X-ray burst oscillations. The combination of the wide-field monitor and the sensitive pointed instruments enables observations of potential electromagnetic counterparts to LIGO and neutrino events. Additional extragalactic science, such as high quality spectroscopy of clusters of galaxies and unprecedented timing investigations of

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

    NASA Technical Reports Server (NTRS)

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

    2017-01-01

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

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

    NASA Astrophysics Data System (ADS)

    Wilson-Hodge, Colleen A.; Ray, Paul S.; Gendreau, Keith; Chakrabarty, Deepto; Feroci, Marco; Maccarone, Thomas J.; Arzoumanian, Zaven; Remillard, Ronald A.; Wood, Kent; Griffith, Christopher; Jenke, Peter

    2017-08-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2017-10-01

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

  14. Oxidant K edge x-ray emission spectroscopy of UF 4 and UO 2

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Tobin, J. G.; Yu, S. -W.; Qiao, R.

    The K-Edge (1s) x-ray emission spectroscopy of uranium tetrafluoride and uranium dioxide were compared to each other and to the results of a pair of earlier cluster calculations. Here, using a very simplified approach, it is possible to qualitatively reconstruct the main features of the x-ray emission spectra from the cluster calculation state energies and 2p percentages.

  15. Oxidant K edge x-ray emission spectroscopy of UF 4 and UO 2

    DOE PAGES

    Tobin, J. G.; Yu, S. -W.; Qiao, R.; ...

    2018-01-31

    The K-Edge (1s) x-ray emission spectroscopy of uranium tetrafluoride and uranium dioxide were compared to each other and to the results of a pair of earlier cluster calculations. Here, using a very simplified approach, it is possible to qualitatively reconstruct the main features of the x-ray emission spectra from the cluster calculation state energies and 2p percentages.

  16. X-ray Photoelectron Spectroscopy study of CaV1-xMoxO3-δ

    NASA Astrophysics Data System (ADS)

    Belyakov, S. A.; Kuznetsov, M. V.; Shkerin, S. N.

    2018-06-01

    An investigation was carried out on perovskite-based derivatives of CaV1-xMoxO3-δ using X-ray Photoelectron Spectroscopy (XPS). According to the XRD pattern, the area of homogeneity covers the region from x = 0 to x = 0.6. Wide XPS-peaks of Ca, V, Mo and O are observed, signalling that elements are presented in multiple states. A model for explaining the large chemical shifts of XPS peaks due to different charging effects on different parts of the sample surface is proposed.

  17. The superconducting high-resolution soft X-ray spectrometer at the advanced biological and environmental X-ray facility

    NASA Astrophysics Data System (ADS)

    Friedrich, S.; Drury, O. B.; George, S. J.; Cramer, S. P.

    2007-11-01

    We have built a 36-pixel superconducting tunnel junction X-ray spectrometer for chemical analysis of dilute samples in the soft X-ray band. It offers an energy resolution of ˜10-20 eV FWHM below 1 keV, a solid angle coverage of ˜10 -3, and can be operated at total rates of up to ˜10 6 counts/s. Here, we describe the spectrometer performance in speciation measurements by fluorescence-detected X-ray absorption spectroscopy at the Advanced Biological and Environmental X-ray facility at the ALS synchrotron.

  18. Methods development for diffraction and spectroscopy studies of metalloenzymes at X-ray free-electron lasers

    PubMed Central

    Kern, Jan; Hattne, Johan; Tran, Rosalie; Alonso-Mori, Roberto; Laksmono, Hartawan; Gul, Sheraz; Sierra, Raymond G.; Rehanek, Jens; Erko, Alexei; Mitzner, Rolf; Wernet, Phillip; Bergmann, Uwe; Sauter, Nicholas K.; Yachandra, Vittal; Yano, Junko

    2014-01-01

    X-ray free-electron lasers (XFELs) open up new possibilities for X-ray crystallographic and spectroscopic studies of radiation-sensitive biological samples under close to physiological conditions. To facilitate these new X-ray sources, tailored experimental methods and data-processing protocols have to be developed. The highly radiation-sensitive photosystem II (PSII) protein complex is a prime target for XFEL experiments aiming to study the mechanism of light-induced water oxidation taking place at a Mn cluster in this complex. We developed a set of tools for the study of PSII at XFELs, including a new liquid jet based on electrofocusing, an energy dispersive von Hamos X-ray emission spectrometer for the hard X-ray range and a high-throughput soft X-ray spectrometer based on a reflection zone plate. While our immediate focus is on PSII, the methods we describe here are applicable to a wide range of metalloenzymes. These experimental developments were complemented by a new software suite, cctbx.xfel. This software suite allows for near-real-time monitoring of the experimental parameters and detector signals and the detailed analysis of the diffraction and spectroscopy data collected by us at the Linac Coherent Light Source, taking into account the specific characteristics of data measured at an XFEL. PMID:24914169

  19. The Compton-thick AGN fraction from the deepest X-ray spectroscopy in the CDF-S

    NASA Astrophysics Data System (ADS)

    Corral, A.; Georgantopoulos, I.; Akylas, A.; Ranalli, P.

    2017-10-01

    Highly obscured AGN, especially Compton-thick (CT) AGN, likely play a key role in the galaxy-AGN co-evolution scenario. They would comprise the early stages of AGN activity, preceding the AGN-feedback/star-formation quenching phase, during which most of both the SMBH and galaxy growth take place. However, the actual CT fraction among the AGN population is still largely unconstrained. The most reliable way of confirming the obscured nature of an AGN by X-ray spectroscopy, but very deep observations are needed to extend local analyses to larger distances. We will present the X-ray spectral analysis of the deepest X-ray data obtained to date, the almost 7Ms observation of the Chandra Deep Field South. The unprecedented depth of this survey allow us to carry out reliable spectral analyses down to a flux limit of 10^{-16} erg cm^{-2} s^{-1} in the hard 2-8 keV band. Besides the new deeper X-ray data, our approach also includes the implementation of Bayesian inference in the determination of the CT fraction. Our results favor X-ray background synthesis models which postulate a moderate fraction (25%) of CT objects among the obscured AGN population.

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

    DOE PAGES

    Alonso-Mori, Roberto; Caronna, Chiara; Chollet, Matthieu; ...

    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.

  1. A high-temperature furnace for in situ synchrotron X-ray spectroscopy under controlled atmospheric conditions.

    PubMed

    Eeckhout, Sigrid Griet; Gorges, Bernard; Barthe, Laurent; Pelosi, Orietta; Safonova, Olga; Giuli, Gabriele

    2008-09-01

    A high-temperature furnace with an induction heater coil has been designed and constructed for in situ X-ray spectroscopic experiments under controlled atmospheric conditions and temperatures up to 3275 K. The multi-purpose chamber design allows working in backscattering and normal fluorescence mode for synchrotron X-ray absorption and emission spectroscopy. The use of the furnace is demonstrated in a study of the in situ formation of Cr oxide between 1823 K and 2023 K at logPO(2) values between -10.0 and -11.3 using X-ray absorption near-edge spectroscopy. The set-up is of particular interest for studying liquid metals, alloys and other electrically conductive materials under extreme conditions.

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

    NASA Astrophysics Data System (ADS)

    Pacold, Joseph I.

    Luminescent materials play important roles in energy sciences, through solid state lighting and possible applications in solar energy utilization, and in biomedical research and applications, such as in immunoassays and fluorescence microscopy. The initial excitation of a luminescent material leads to a sequence of transitions between excited states, ideally ending with the emission of one or more optical-wavelength photons. It is essential to understand the microscopic physics of this excited state cascade in order to rationally design materials with high quantum efficiencies or with other fine-tuning of materials response. While optical-wavelength spectroscopies have unraveled many details of the energy transfer pathways in luminescent materials, significant questions remain open for many lanthanide-based luminescent materials. For organometallic dyes in particular, quantum yields remain limited in comparison with inorganic phosphors. This dissertation reports on a research program of synchrotron x-ray studies of the excited state electronic structure and energy-relaxation cascade in trivalent lanthanide phosphors and dyes. To this end, one of the primary results presented here is the first time-resolved x-ray absorption near edge spectroscopy studies of the transient 4f excited states in lanthanide-activated luminescent dyes and phosphors. This is a new application of time-resolved x-ray absorption spectroscopy that makes it possible to directly observe and, to some extent, quantify intramolecular nonradiative energy transfer processes. We find a transient increase in 4f spectral weight associated with an excited state confined to the 4f shell of trivalent Eu. This result implies that it is necessary to revise the current theoretical understanding of 4f excitation in trivalent lanthanide activators: either transient 4f-5d mixing effects are much stronger than previously considered, or else the lanthanide 4f excited state has an unexpectedly large contribution

  3. Characterization of Sb-doped Bi(2)UO(6) solid solutions by X-ray diffraction and X-ray absorption spectroscopy.

    PubMed

    Misra, N L; Yadav, A K; Dhara, Sangita; Mishra, S K; Phatak, Rohan; Poswal, A K; Jha, S N; Sinha, A K; Bhattacharyya, D

    2013-01-01

    The preparation and characterization of Sb-doped Bi(2)UO(6) solid solutions, in a limited composition range, is reported for the first time. The solid solutions were prepared by solid-state reactions of Bi(2)O(3), Sb(2)O(3) and U(3)O(8) in the required stoichiometry. The reaction products were characterized by X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) measurements at the Bi and U L(3) edges. The XRD patterns indicate the precipitation of additional phases in the samples when Sb doping exceeds 4 at%. The chemical shifts of the Bi absorption edges in the samples, determined from the XANES spectra, show a systematic variation only up to 4 at% of Sb doping and support the results of XRD measurements. These observations are further supported by the local structure parameters obtained by analysis of the EXAFS spectra. The local structure of U is found to remain unchanged upon Sb doping indicating that Sb(+3) ions replace Bi(+3) during the doping of Bi(2)UO(6) by Sb.

  4. Low Dose X-Ray Speckle Visibility Spectroscopy Reveals Nanoscale Dynamics in Radiation Sensitive Ionic Liquids

    NASA Astrophysics Data System (ADS)

    Verwohlt, Jan; Reiser, Mario; Randolph, Lisa; Matic, Aleksandar; Medina, Luis Aguilera; Madsen, Anders; Sprung, Michael; Zozulya, Alexey; Gutt, Christian

    2018-04-01

    X-ray radiation damage provides a serious bottleneck for investigating microsecond to second dynamics on nanometer length scales employing x-ray photon correlation spectroscopy. This limitation hinders the investigation of real time dynamics in most soft matter and biological materials which can tolerate only x-ray doses of kGy and below. Here, we show that this bottleneck can be overcome by low dose x-ray speckle visibility spectroscopy. Employing x-ray doses of 22-438 kGy and analyzing the sparse speckle pattern of count rates as low as 6.7 ×10-3 per pixel, we follow the slow nanoscale dynamics of an ionic liquid (IL) at the glass transition. At the prepeak of nanoscale order in the IL, we observe complex dynamics upon approaching the glass transition temperature TG with a freezing in of the alpha relaxation and a multitude of millisecond local relaxations existing well below TG . We identify this fast relaxation as being responsible for the increasing development of nanoscale order observed in ILs at temperatures below TG .

  5. Analysis of heterogeneous gallstones using laser-induced breakdown spectroscopy (LIBS) and wavelength dispersive X-ray fluorescence (WD-XRF).

    PubMed

    Jaswal, Brij Bir S; Kumar, Vinay; Sharma, Jitendra; Rai, Pradeep K; Gondal, Mohammed A; Gondal, Bilal; Singh, Vivek K

    2016-04-01

    Laser-induced breakdown spectroscopy (LIBS) is an emerging analytical technique with numerous advantages such as rapidity, multi-elemental analysis, no specific sample preparation requirements, non-destructiveness, and versatility. It has been proven to be a robust elemental analysis tool attracting interest because of being applied to a wide range of materials including biomaterials. In this paper, we have performed spectroscopic studies on gallstones which are heterogeneous in nature using LIBS and wavelength dispersive X-ray fluorescence (WD-XRF) techniques. It has been observed that the presence and relative concentrations of trace elements in different kind of gallstones (cholesterol and pigment gallstones) can easily be determined using LIBS technique. From the experiments carried out on gallstones for trace elemental mapping and detection, it was found that LIBS is a robust tool for such biomedical applications. The stone samples studied in the present paper were classified using the Fourier transform infrared (FTIR) spectroscopy. WD-XRF spectroscopy has been applied for the qualitative and quantitative analysis of major and trace elements present in the gallstone which was compared with the LIBS data. The results obtained in the present paper show interesting prospects for LIBS and WD-XRF to study cholelithiasis better.

  6. 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.

  7. X-ray Spectroscopy of a TDE

    NASA Astrophysics Data System (ADS)

    Kochanek, Christopher

    2017-09-01

    Tidal disruption events (TDE), where supermassive black holes destroy stars to produce accretion flares, are of great current observational and theoretical interest. Here we propose a four epoch HRC/LETG X-ray spectroscopic ``movie'' of a TDE spread over the first 40 days of an X-ray bright TDE, including any discovered by our ASAS-SN survey, supported and extended by higher cadence Swift XRT/UVOT observations over the first 100 days. For this next X-ray bright TDE, we will measure the evolution of the X-ray emission (luminosity/temperature) from the hot accretion disk, the emission reprocessed by the debris into UV/optical, and use X-ray absorption (or emission) features to look at the abundances and the evolution of the kinematics and ionization parameter.

  8. Analysis of doping concentration and composition in wide bandgap AlGaN:Si by wavelength dispersive x-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Kusch, Gunnar; Mehnke, Frank; Enslin, Johannes; Edwards, Paul R.; Wernicke, Tim; Kneissl, Michael; Martin, Robert W.

    2017-03-01

    Detailed knowledge of the dopant concentration and composition of wide band gap Al x Ga{}1-x{{N}} layers is of crucial importance for the fabrication of ultra violet light emitting diodes. This paper demonstrates the capabilities of wavelength dispersive x-ray (WDX) spectroscopy in accurately determining these parameters and compares the results with those from high resolution x-ray diffraction (HR-XRD) and secondary ion mass spectrometry (SIMS). WDX spectroscopy has been carried out on different silicon-doped wide bandgap Al x Ga{}1-x{{N}} samples (x between 0.80 and 1). This study found a linear increase in the Si concentration with the SiH4/group-III ratio, measuring Si concentrations between 3× {10}18 cm-3 and 2.8× {10}19 cm-3, while no direct correlation between the AlN composition and the Si incorporation ratio was found. Comparison between the composition obtained by WDX and by HR-XRD showed very good agreement in the range investigated, while comparison of the donor concentration between WDX and SIMS found only partial agreement, which we attribute to a number of effects.

  9. Identification of Uranyl Minerals Using Oxygen K-Edge X Ray Absorption Spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Ward, Jesse D.; Bowden, Mark E.; Resch, Charles T.

    2016-03-01

    Uranium analysis is consistently needed throughout the fuel cycle, from mining to fuel fabrication to environmental monitoring. Although most of the world’s uranium is immobilized as pitchblende or uraninite, there exists a plethora of secondary uranium minerals, nearly all of which contain the uranyl cation. Analysis of uranyl compounds can provide clues as to a sample’s facility of origin and chemical history. X-ray absorption spectroscopy is one technique that could enhance our ability to identify uranium minerals. Although there is limited chemical information to be gained from the uranium X-ray absorption edges, recent studies have successfully used ligand NEXAFS tomore » study the physical chemistry of various uranium compounds. This study extends the use of ligand NEXAFS to analyze a suite of uranium minerals. We find that major classes of uranyl compounds (carbonate, oxyhydroxide, silicate, and phosphate) exhibit characteristic lineshapes in the oxygen K-edge absorption spectra. As a result, this work establishes a library of reference spectra that can be used to classify unknown uranyl minerals.« less

  10. Development of polycapillary x-ray optics for x-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Adams, Bernhard W.; Attenkofer, Klaus; Bond, Justin L.; Craven, Christopher A.; Cremer, Till; O'Mahony, Aileen; Minot, Michael J.; Popecki, Mark A.

    2016-09-01

    Bundles of hollow glass capillaries can be tapered to produce quasi-focusing x-ray optics. These optics are known as Kumakhov lenses. These optics are interesting for lab-based sources because they can be used to collimate and concentrate x-rays originating from a point, such as a laser focus or an electron-beam focus in a microtube.

  11. Distinct charge dynamics in battery electrodes revealed by in situ and operando soft X-ray spectroscopy

    PubMed Central

    Liu, Xiaosong; Wang, Dongdong; Liu, Gao; Srinivasan, Venkat; Liu, Zhi; Hussain, Zahid; Yang, Wanli

    2013-01-01

    Developing high-performance batteries relies on material breakthroughs. During the past few years, various in situ characterization tools have been developed and have become indispensible in studying and the eventual optimization of battery materials. However, soft X-ray spectroscopy, one of the most sensitive probes of electronic states, has been mainly limited to ex situ experiments for battery research. Here we achieve in situ and operando soft X-ray absorption spectroscopy of lithium-ion battery cathodes. Taking advantage of the elemental, chemical and surface sensitivities of soft X-rays, we discover distinct lithium-ion and electron dynamics in Li(Co1/3Ni1/3Mn1/3)O2 and LiFePO4 cathodes in polymer electrolytes. The contrast between the two systems and the relaxation effect in LiFePO4 is attributed to a phase transformation mechanism, and the mesoscale morphology and charge conductivity of the electrodes. These discoveries demonstrate feasibility and power of in situ soft X-ray spectroscopy for studying integrated and dynamic effects in batteries. PMID:24100759

  12. Electronic Structure of the Organic Semiconductor Alq3 (aluminum tris-8-hydroxyquinoline) from Soft X-ray Spectroscopies and Density Functional Theory Calculations

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    DeMasi, A.; Piper, L; Zhang, Y

    2008-01-01

    The element-specific electronic structure of the organic semiconductor aluminum tris-8-hydroxyquinoline (Alq3) has been studied using a combination of resonant x-ray emission spectroscopy, x-ray photoelectron spectroscopy, x-ray absorption spectroscopy, and density functional theory (DFT) calculations. Resonant and nonresonant x-ray emission spectroscopy were used to measure directly the carbon, nitrogen and oxygen 2p partial densities of states in Alq3, and good agreement was found with the results of DFT calculations. Furthermore, resonant x-ray emission at the carbon K-edge is shown to be able to measure the partial density of states associated with individual C sites. Finally, comparison of previous x-ray emission studiesmore » and the present data reveal the presence of clear photon-induced damage in the former.« less

  13. Electronic structure of the organic semiconductor Alq3 (aluminum tris-8-hydroxyquinoline) from soft x-ray spectroscopies and density functional theory calculations.

    PubMed

    DeMasi, A; Piper, L F J; Zhang, Y; Reid, I; Wang, S; Smith, K E; Downes, J E; Peltekis, N; McGuinness, C; Matsuura, A

    2008-12-14

    The element-specific electronic structure of the organic semiconductor aluminum tris-8-hydroxyquinoline (Alq(3)) has been studied using a combination of resonant x-ray emission spectroscopy, x-ray photoelectron spectroscopy, x-ray absorption spectroscopy, and density functional theory (DFT) calculations. Resonant and nonresonant x-ray emission spectroscopy were used to measure directly the carbon, nitrogen and oxygen 2p partial densities of states in Alq(3), and good agreement was found with the results of DFT calculations. Furthermore, resonant x-ray emission at the carbon K-edge is shown to be able to measure the partial density of states associated with individual C sites. Finally, comparison of previous x-ray emission studies and the present data reveal the presence of clear photon-induced damage in the former.

  14. Trace elemental analysis of school chalk using energy dispersive X-ray florescence spectroscopy (ED-XRF)

    NASA Astrophysics Data System (ADS)

    Maruthi, Y. A.; Das, N. Lakshmana; Ramprasad, S.; Ram, S. S.; Sudarshan, M.

    2015-08-01

    The present studies focus the quantitative analysis of elements in school chalk to ensure the safety of its use. The elements like Calcium (Ca), Aluminum (Al), Iron (Fe), Silicon (Si) and Chromium (Cr) were analyzed from settled chalk dust samples collected from five classrooms (CD-1) and also from another set of unused chalk samples collected from local market (CD-2) using Energy Dispersive X-Ray florescence(ED-XRF) spectroscopy. Presence of these elements in significant concentrations in school chalk confirmed that, it is an irritant and occupational hazard. It is suggested to use protective equipments like filtered mask for mouth, nose and chalk holders. This study also suggested using the advanced mode of techniques like Digital boards, marker boards and power point presentations to mitigate the occupational hazard for classroom chalk

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

    NASA Astrophysics Data System (ADS)

    Wilson-Hodge, Colleen A.; Ray, Paul S.; Gendreau, Keith; Chakrabarty, Deepto; Feroci, Marco; Maccarone, Tom; Arzoumanian, Zaven; Remillard, Ronald A.; Wood, Kent; Griffith, Christopher; STROBE-X Collaboration

    2017-01-01

    We describe a proposed probe-class mission concept that will provide an unprecedented view of the X-ray sky, performing timing and spectroscopy over a broad band (0.2-30 keV) probing timescales from microseconds to years. The Spectroscopic Time-Resolving Observatory for Broadband Energy X-rays (STROBE-X) comprises two primary instruments. The soft band (0.2-12 keV) will be covered by an array of lightweight optics (3-m focal length) that concentrate incident photons onto small solid state detectors with CCD-level (85-130 eV) energy resolution, 100 ns time resolution, and low background rates. This technology, fully developed for NICER, would be scaled up with enhanced optics to take advantage of the longer focal length of STROBE-X. The harder band (2 to at least 30 keV) would be covered by large-area collimated silicon drift detectors,developed for the European LOFT mission concept. Each instrument would provide an order of magnitude improvement in effective area compared with its predecessor (NICER in the soft band and RXTE in the hard band). A sensitive sky monitor would act as a trigger for pointed observations, provide high duty cycle, high time resolution, high spectral resolution monitoring of the X-ray sky with ~20 times the sensitivity of the RXTE ASM, and enable multi-wavelength and multi-messenger studies on a continuous, rather than scanning basis.The broad coverage will enable thermal components, non-thermal components, iron lines, and reflection features to be studied simultaneously from a single platform for the first time in accreting black holes at all scales. The enormous collecting area will enable studies of the dense matter equation of state using both soft thermal emission from rotation-powered pulsars and harder emission from X-ray burst oscillations. Revolutionary science, such as high quality spectroscopy of clusters of galaxies and unprecedented timing investigations of active galactic nuclei, would also be obtained.We describe the mission

  16. 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

  17. Extended x-ray absorption fine structure spectroscopy and x-ray absorption near edge spectroscopy study of aliovalent doped ceria to correlate local structural changes with oxygen vacancies clustering

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Shirbhate, S. C.; Acharya, S. A., E-mail: saha275@yahoo.com; Yadav, A. K.

    2016-04-04

    This study provides atomic scale insight to understand the role of aliovalent dopants on oxygen vacancies clustering and dissociation mechanism in ceria system in order to enhance the performance of oxy-ion conductor. Dopants induced microscale changes in ceria are probed by extended X-ray absorption fine structure spectroscopy, X-ray absorption near edge spectra, and Raman spectroscopy. The results are explored to establish a correlation between atomic level structural changes (coordination number, interatomic spacing) → formation of dimer and trimer type cation-oxygen vacancies defect complex (intrinsic and extrinsic) → dissociation of oxygen vacancies from defect cluster → ionic conductivity temperature. It ismore » a strategic approach to understand key physics of ionic conductivity mechanism in order to reduce operating temperature of electrolytes for intermediate temperature (300–450 °C) electrochemical devices for the first time.« less

  18. PyXRF: Python-based X-ray fluorescence analysis package

    NASA Astrophysics Data System (ADS)

    Li, Li; Yan, Hanfei; Xu, Wei; Yu, Dantong; Heroux, Annie; Lee, Wah-Keat; Campbell, Stuart I.; Chu, Yong S.

    2017-09-01

    We developed a python-based fluorescence analysis package (PyXRF) at the National Synchrotron Light Source II (NSLS-II) for the X-ray fluorescence-microscopy beamlines, including Hard X-ray Nanoprobe (HXN), and Submicron Resolution X-ray Spectroscopy (SRX). This package contains a high-level fitting engine, a comprehensive commandline/ GUI design, rigorous physics calculations, and a visualization interface. PyXRF offers a method of automatically finding elements, so that users do not need to spend extra time selecting elements manually. Moreover, PyXRF provides a convenient and interactive way of adjusting fitting parameters with physical constraints. This will help us perform quantitative analysis, and find an appropriate initial guess for fitting. Furthermore, we also create an advanced mode for expert users to construct their own fitting strategies with a full control of each fitting parameter. PyXRF runs single-pixel fitting at a fast speed, which opens up the possibilities of viewing the results of fitting in real time during experiments. A convenient I/O interface was designed to obtain data directly from NSLS-II's experimental database. PyXRF is under open-source development and designed to be an integral part of NSLS-II's scientific computation library.

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

    PubMed

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

    2017-06-14

    Modern X-ray spectroscopy has proven itself as a robust tool for probing the electronic structure of atoms in complex environments. Despite working on energy scales that are much larger than those corresponding to nuclear motions, taking nuclear dynamics and the associated nuclear correlations into account may be of importance for X-ray spectroscopy. Recently, we have developed an efficient protocol to account for nuclear dynamics in X-ray absorption and resonant inelastic X-ray scattering spectra [Karsten et al., J. Phys. Chem. Lett. 8, 992 (2017)], based on ground state molecular dynamics accompanied with state-of-the-art calculations of electronic excitation energies and transition dipoles. Here, we present an alternative derivation of the formalism and elaborate on the developed simulation protocol using gas phase and bulk water as examples. The specific spectroscopic features stemming from the nuclear motions are analyzed and traced down to the dynamics of electronic energy gaps and transition dipole correlation functions. The observed tendencies are explained on the basis of a simple harmonic model, and the involved approximations are discussed. The method represents a step forward over the conventional approaches that treat the system in full complexity and provides a reasonable starting point for further improvements.

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

    NASA Astrophysics Data System (ADS)

    Karsten, Sven; Bokarev, Sergey I.; Aziz, Saadullah G.; Ivanov, Sergei D.; Kühn, Oliver

    2017-06-01

    Modern X-ray spectroscopy has proven itself as a robust tool for probing the electronic structure of atoms in complex environments. Despite working on energy scales that are much larger than those corresponding to nuclear motions, taking nuclear dynamics and the associated nuclear correlations into account may be of importance for X-ray spectroscopy. Recently, we have developed an efficient protocol to account for nuclear dynamics in X-ray absorption and resonant inelastic X-ray scattering spectra [Karsten et al., J. Phys. Chem. Lett. 8, 992 (2017)], based on ground state molecular dynamics accompanied with state-of-the-art calculations of electronic excitation energies and transition dipoles. Here, we present an alternative derivation of the formalism and elaborate on the developed simulation protocol using gas phase and bulk water as examples. The specific spectroscopic features stemming from the nuclear motions are analyzed and traced down to the dynamics of electronic energy gaps and transition dipole correlation functions. The observed tendencies are explained on the basis of a simple harmonic model, and the involved approximations are discussed. The method represents a step forward over the conventional approaches that treat the system in full complexity and provides a reasonable starting point for further improvements.

  1. X ray photoelectron spectroscopy (XPS) analysis of Photosensitive ZrO2 array

    NASA Astrophysics Data System (ADS)

    Li, Y.; Zhao, G.; Zhu, R.; Kou, Z.

    2018-03-01

    Based on organic zirconium source as the starting material, by adding chemical modifiers which are made up with photosensitive ZrO2 sol. A uniformed ZrO2 array dot was fabricated with a mean diameter of around 800 nm. By using UV-vis spectra and X-ray photoelectron spectroscopy analysis method, studies the photosensitive ZrO2 gel film of photochemical reaction process and the photosensitive mechanism, to determine the zirconium atom centered chelate structure, reaction formed by metal chelate Zr atom for the center, and to establish the molecular model of the chelate. And studied the ultraviolet light in the process of the variation of the XPS spectra, Zr3d5/2 to 184.9 eV corresponding to the binding energy of the as the combination of state peak gradually reduce; By combining with the status of Zr-O peak gradually increase; The strength of the peak is gradually decline. This suggests that in the process of ultraviolet light photo chemical reaction happened. This study is of great significance to the micro fabrication of ZrO2 array not only to the memory devices but also to the optical devices.

  2. Chemical Modification of Graphene Oxide by Nitrogenation: An X-ray Absorption and Emission Spectroscopy Study

    NASA Astrophysics Data System (ADS)

    Chuang, Cheng-Hao; Ray, Sekhar C.; Mazumder, Debarati; Sharma, Surbhi; Ganguly, Abhijit; Papakonstantinou, Pagona; Chiou, Jau-Wern; Tsai, Huang-Ming; Shiu, Hung-Wei; Chen, Chia-Hao; Lin, Hong-Ji; Guo, Jinghua; Pong, Way-Faung

    2017-02-01

    Nitrogen-doped graphene oxides (GO:Nx) were synthesized by a partial reduction of graphene oxide (GO) using urea [CO(NH2)2]. Their electronic/bonding structures were investigated using X-ray absorption near-edge structure (XANES), valence-band photoemission spectroscopy (VB-PES), X-ray emission spectroscopy (XES) and resonant inelastic X-ray scattering (RIXS). During GO:Nx synthesis, different nitrogen-bonding species, such as pyrrolic/graphitic-nitrogen, were formed by replacing of oxygen-containing functional groups. At lower N-content (2.7 at%), pyrrolic-N, owing to surface and subsurface diffusion of C, N and NH is deduced from various X-ray spectroscopies. In contrast, at higher N-content (5.0 at%) graphitic nitrogen was formed in which each N-atom trigonally bonds to three distinct sp2-hybridized carbons with substitution of the N-atoms for C atoms in the graphite layer. Upon nitrogen substitution, the total density of state close to Fermi level is increased to raise the valence-band maximum, as revealed by VB-PES spectra, indicating an electron donation from nitrogen, molecular bonding C/N/O coordination or/and lattice structure reorganization in GO:Nx. The well-ordered chemical environments induced by nitrogen dopant are revealed by XANES and RIXS measurements.

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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    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). Themore » 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.« less

  4. The characterization of Cr secondary oxide phases in ZnO films studied by X-ray spectroscopy and photoemission spectroscopy

    NASA Astrophysics Data System (ADS)

    Chiou, J. W.; Chang, S. Y.; Huang, W. H.; Chen, Y. T.; Hsu, C. W.; Hu, Y. M.; Chen, J. M.; Chen, C.-H.; Kumar, K.; Guo, J.-H.

    2011-03-01

    X-ray absorption near-edge structure (XANES), X-ray emission spectroscopy (XES), and X-ray photoemission spectroscopy (XPS) were used to characterize the Cr secondary oxide phases in ZnO films that had been prepared using a co-sputtering method. Analysis of the Cr L3,2-edge XANES spectra reveals that the intensity of white-line features decreases subtly as the sputtering power increases, indicating that the occupation of Cr 3 d orbitals increases with Cr concentration in (Zn, Cr)O films. The O K-edge spectra show that the intensity of XANES features of (Zn, Cr)O films is lower than those of ZnO film, suggesting enhanced occupation of O 2 p-derived states through O 2 p-Cr 3 d hybridization. The XES and XPS spectra indicate that the line shapes in the valence band of (Zn, Cr)O films are quite different from those of ZnO and that the Cr 2O 3 phase dominates the spinel structure of (Zn, Cr)O films increasingly as the Cr sputtering power is increased. Over all results suggest that the non-ferromagnetic behavior of (Zn, Cr)O films can be attributed to the dominant presence of Cr 2O 3, whereas the bulk comprise phase segregations of Cr 2O 3 and/or ZnCr 2O 4, which results them the most stable TM-doped ZnO material against etching.

  5. Near- and Extended-Edge X-Ray-Absorption Fine-Structure Spectroscopy Using Ultrafast Coherent High-Order Harmonic Supercontinua

    NASA Astrophysics Data System (ADS)

    Popmintchev, Dimitar; Galloway, Benjamin R.; Chen, Ming-Chang; Dollar, Franklin; Mancuso, Christopher A.; Hankla, Amelia; Miaja-Avila, Luis; O'Neil, Galen; Shaw, Justin M.; Fan, Guangyu; Ališauskas, Skirmantas; Andriukaitis, Giedrius; Balčiunas, Tadas; Mücke, Oliver D.; Pugzlys, Audrius; Baltuška, Andrius; Kapteyn, Henry C.; Popmintchev, Tenio; Murnane, Margaret M.

    2018-03-01

    Recent advances in high-order harmonic generation have made it possible to use a tabletop-scale setup to produce spatially and temporally coherent beams of light with bandwidth spanning 12 octaves, from the ultraviolet up to x-ray photon energies >1.6 keV . Here we demonstrate the use of this light for x-ray-absorption spectroscopy at the K - and L -absorption edges of solids at photon energies near 1 keV. We also report x-ray-absorption spectroscopy in the water window spectral region (284-543 eV) using a high flux high-order harmonic generation x-ray supercontinuum with 109 photons/s in 1% bandwidth, 3 orders of magnitude larger than has previously been possible using tabletop sources. Since this x-ray radiation emerges as a single attosecond-to-femtosecond pulse with peak brightness exceeding 1026 photons/s /mrad2/mm2/1 % bandwidth, these novel coherent x-ray sources are ideal for probing the fastest molecular and materials processes on femtosecond-to-attosecond time scales and picometer length scales.

  6. Cosmic X-ray physics

    NASA Technical Reports Server (NTRS)

    Mccammon, D.; Cox, D. P.; Kraushaar, W. L.; Sanders, W. T.

    1986-01-01

    The analysis of the beryllium-filtered data from Flight 17.020 was completed. The data base provided by the Wisconsin diffuse X-ray sky survey is being analyzed by correlating the B and C band emission with individual velocity components of neutral hydrogen. Work on a solid state detector to be used in high resolution spectroscopy of diffuse or extend X-ray sources is continuing. A series of 21 cm observations was completed. A paper on the effects of process parameter variation on the reflectivity of sputter-deposited tungsten-carvon multilayers was published.

  7. Ray-trace analysis of glancing-incidence X-ray optical systems

    NASA Technical Reports Server (NTRS)

    Foreman, J. W., Jr.; Cardone, J. M.

    1976-01-01

    The results of a ray-trace analysis of several glancing-incidence X-ray optical systems are presented. The object of the study was threefold. First, the vignetting characteristics of the S-056 X-ray telescope were calculated using experimental data to determine mirror reflectivities. Second, a small Wolter Type I X-ray telescope intended for possible use in the Geostationary Operational Environmental Satellite program was designed and ray traced. Finally, a ray-trace program was developed for a Wolter-Schwarzschild X-ray telescope.

  8. Trace elemental analysis of school chalk using energy dispersive X-ray florescence spectroscopy (ED-XRF)

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Maruthi, Y. A., E-mail: ymjournal2014@gmail.com; Das, N. Lakshmana, E-mail: nldas9@gmail.com; Ramprasad, S., E-mail: ramprasadsurakala@gmail.com

    The present studies focus the quantitative analysis of elements in school chalk to ensure the safety of its use. The elements like Calcium (Ca), Aluminum (Al), Iron (Fe), Silicon (Si) and Chromium (Cr) were analyzed from settled chalk dust samples collected from five classrooms (CD-1) and also from another set of unused chalk samples collected from local market (CD-2) using Energy Dispersive X-Ray florescence(ED-XRF) spectroscopy. Presence of these elements in significant concentrations in school chalk confirmed that, it is an irritant and occupational hazard. It is suggested to use protective equipments like filtered mask for mouth, nose and chalk holders.more » This study also suggested using the advanced mode of techniques like Digital boards, marker boards and power point presentations to mitigate the occupational hazard for classroom chalk.« less

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

    NASA Astrophysics Data System (ADS)

    Sindhupakorn, Bura; Thienpratharn, Suwittaya; Kidkhunthod, Pinit

    2017-10-01

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

  10. 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.

  11. Monitoring the recrystallisation of amorphous xylitol using Raman spectroscopy and wide-angle X-ray scattering.

    PubMed

    Palomäki, Emmi; Ahvenainen, Patrik; Ehlers, Henrik; Svedström, Kirsi; Huotari, Simo; Yliruusi, Jouko

    2016-07-11

    In this paper we present a fast model system for monitoring the recrystallization of quench-cooled amorphous xylitol using Raman spectroscopy and wide-angle X-ray scattering. The use of these two methods enables comparison between surface and bulk crystallization. Non-ordered mesoporous silica micro-particles were added to the system in order to alter the rate of crystallization of the amorphous xylitol. Raman measurements showed that adding silica to the system increased the rate of surface crystallization, while X-ray measurements showed that the rate of bulk crystallization decreased. Using this model system it is possible to measure fast changes, which occur in minutes or within a few hours. Raman-spectroscopy and wide-angle X-ray scattering were found to be complementary techniques when assessing surface and bulk crystallization of amorphous xylitol. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Pt and Ru X-ray absorption spectroscopy of PtRu anode catalysts in operating direct methanol fuel cells.

    PubMed

    Stoupin, Stanislav; Chung, Eun-Hyuk; Chattopadhyay, Soma; Segre, Carlo U; Smotkin, Eugene S

    2006-05-25

    In situ X-ray absorption spectroscopy, ex situ X-ray fluorescence, and X-ray powder diffraction enabled detailed core analysis of phase segregated nanostructured PtRu anode catalysts in an operating direct methanol fuel cell (DMFC). No change in the core structures of the phase segregated catalyst was observed as the potential traversed the current onset potential of the DMFC. The methodology was exemplified using a Johnson Matthey unsupported PtRu (1:1) anode catalyst incorporated into a DMFC membrane electrode assembly. During DMFC operation the catalyst is essentially metallic with half of the Ru incorporated into a face-centered cubic (FCC) Pt alloy lattice and the remaining half in an amorphous phase. The extended X-ray absorption fine structure (EXAFS) analysis suggests that the FCC lattice is not fully disordered. The EXAFS indicates that the Ru-O bond lengths were significantly shorter than those reported for Ru-O of ruthenium oxides, suggesting that the phases in which the Ru resides in the catalysts are not similar to oxides.

  13. X-ray Fluorescence Holography: Principles, Apparatus, and Applications

    NASA Astrophysics Data System (ADS)

    Hayashi, Kouichi; Korecki, Pawel

    2018-06-01

    X-ray fluorescence holography (XFH) is an atomic structure determination technique that combines the capabilities of X-ray diffraction and X-ray fluorescence spectroscopy. It provides a unique means of gaining fully three-dimensional information about the local atomic structure and lattice site positions of selected elements inside compound samples. In this work, we discuss experimental and theoretical aspects that are essential for the efficient recording and analysis of X-ray fluorescence holograms and review the most recent advances in XFH. We describe experiments performed with brilliant synchrotron radiation as well as with tabletop setups that employ conventional X-ray tubes.

  14. Preparation and characterization of polymer layer systems for validation of 3D Micro X-ray fluorescence spectroscopy

    NASA Astrophysics Data System (ADS)

    Schaumann, Ina; Malzer, Wolfgang; Mantouvalou, Ioanna; Lühl, Lars; Kanngießer, Birgit; Dargel, Rainer; Giese, Ulrich; Vogt, Carla

    2009-04-01

    For the validation of the quantification of the newly-developed method of 3D Micro X-ray fluorescence spectroscopy (3D Micro-XRF) samples with a low average Z matrix and minor high Z elements are best suited. In a light matrix the interferences by matrix effects are minimized so that organic polymers are appropriate as basis for analytes which are more easily detected by X-ray fluorescence spectroscopy. Polymer layer systems were assembled from single layers of ethylene-propylene-diene rubber (EPDM) filled with changing concentrations of silica and zinc oxide as inorganic additives. Layer thicknesses were in the range of 30-150 μm. Before the analysis with 3D Micro-XRF all layers have been characterized by scanning micro-XRF with regard to filler dispersion, by infrared microscopy and light microscopy in order to determine the layer thicknesses and by ICP-OES to verify the concentration of the X-ray sensitive elements in the layers. With the results obtained for stacked polymer systems the validity of the analytical quantification model for the determination of stratified materials by 3D Micro-XRF could be demonstrated.

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

    NASA Astrophysics Data System (ADS)

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

    2017-09-01

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

  16. New developments in fabrication of high-energy-resolution analyzers for inelastic x-ray spectroscopy.

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Said, A. H.; Sinn, H.; Divan, R.

    2011-05-01

    In this work new improvements related to the fabrication of spherical bent analyzers for 1 meV energy-resolution inelastic X-ray scattering spectroscopy are presented. The new method includes the use of a two-dimensional bender to achieve the required radius of curvature for X-ray analyzers. The advantage of this method is the ability to monitor the focus during bending, which leads to higher-efficiency analyzers.

  17. The CAT-ACT Beamline at ANKA: A new high energy X-ray spectroscopy facility for CATalysis and ACTinide research

    NASA Astrophysics Data System (ADS)

    Zimina, A.; Dardenne, K.; Denecke, M. A.; Grunwaldt, J. D.; Huttel, E.; Lichtenberg, H.; Mangold, S.; Pruessmann, T.; Rothe, J.; Steininger, R.; Vitova, T.

    2016-05-01

    A new hard X-ray beamline for CATalysis and ACTinide research has been built at the synchrotron radiation facility ANKA. The beamline design is dedicated to X-ray spectroscopy, including ‘flux hungry’ photon-in/photon-out and correlative techniques with a special infrastructure for radionuclide and catalysis research. The CAT-ACT beamline will help serve the growing need for high flux/hard X-ray spectroscopy in these communities. The design, the first spectra and the current status of this project are reported.

  18. Clocking Femtosecond Collisional Dynamics via Resonant X-Ray Spectroscopy

    NASA Astrophysics Data System (ADS)

    van den Berg, Q. Y.; Fernandez-Tello, E. V.; Burian, T.; Chalupský, J.; Chung, H.-K.; Ciricosta, O.; Dakovski, G. L.; Hájková, V.; Hollebon, P.; Juha, L.; Krzywinski, J.; Lee, R. W.; Minitti, M. P.; Preston, T. R.; de la Varga, A. G.; Vozda, V.; Zastrau, U.; Wark, J. S.; Velarde, P.; Vinko, S. M.

    2018-02-01

    Electron-ion collisional dynamics is of fundamental importance in determining plasma transport properties, nonequilibrium plasma evolution, and electron damage in diffraction imaging applications using bright x-ray free-electron lasers (FELs). Here we describe the first experimental measurements of ultrafast electron impact collisional ionization dynamics using resonant core-hole spectroscopy in a solid-density magnesium plasma, created and diagnosed with the Linac Coherent Light Source x-ray FEL. By resonantly pumping the 1 s →2 p transition in highly charged ions within an optically thin plasma, we have measured how off-resonance charge states are populated via collisional processes on femtosecond time scales. We present a collisional cross section model that matches our results and demonstrates how the cross sections are enhanced by dense-plasma effects including continuum lowering. Nonlocal thermodynamic equilibrium collisional radiative simulations show excellent agreement with the experimental results and provide new insight on collisional ionization and three-body-recombination processes in the dense-plasma regime.

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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Klysubun, Wantana; Kidkhunthod, Pinit; Tarawarakarn, Pongjakr

    2017-04-04

    The SUT-NANOTEC-SLRI beamline was constructed in 2012 as the flagship of the SUT-NANOTEC-SLRI Joint Research Facility for Synchrotron Utilization, co-established by Suranaree University of Technology (SUT), National Nanotechnology Center (NANOTEC) and Synchrotron Light Research Institute (SLRI). It is an intermediate-energy X-ray absorption spectroscopy (XAS) beamline at SLRI. The beamline delivers an unfocused monochromatic X-ray beam of tunable photon energy (1.25–10 keV). The maximum normal incident beam size is 13 mm (width) × 1 mm (height) with a photon flux of 3 × 10 8to 2 × 10 10 photons s -1(100 mA) -1varying across photon energies. Details of the beamlinemore » and XAS instrumentation are described. To demonstrate the beamline performance,K-edge XANES spectra of MgO, Al 2O 3, S 8, FeS, FeSO 4, Cu, Cu 2O and CuO, and EXAFS spectra of Cu and CuO are presented.« less

  20. Investigation of periodically driven systems by x-ray absorption spectroscopy using asynchronous data collection mode

    NASA Astrophysics Data System (ADS)

    Singh, H.; Donetsky, D.; Liu, J.; Attenkofer, K.; Cheng, B.; Trelewicz, J. R.; Lubomirsky, I.; Stavitski, E.; Frenkel, A. I.

    2018-04-01

    We report the development, testing, and demonstration of a setup for modulation excitation spectroscopy experiments at the Inner Shell Spectroscopy beamline of National Synchrotron Light Source - II. A computer algorithm and dedicated software were developed for asynchronous data processing and analysis. We demonstrate the reconstruction of X-ray absorption spectra for different time points within the modulation pulse using a model system. This setup and the software are intended for a broad range of functional materials which exhibit structural and/or electronic responses to the external stimulation, such as catalysts, energy and battery materials, and electromechanical devices.

  1. Portable total reflection x-ray fluorescence analysis in the identification of unknown laboratory hazards

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Liu, Ying, E-mail: liu.ying.48r@st.kyoto-u.ac.jp; Imashuku, Susumu; Sasaki, Nobuharu

    In this study, a portable total reflection x-ray fluorescence (TXRF) spectrometer was used to analyze unknown laboratory hazards that precipitated on exterior surfaces of cooling pipes and fume hood pipes in chemical laboratories. With the aim to examine the accuracy of TXRF analysis for the determination of elemental composition, analytical results were compared with those of wavelength-dispersive x-ray fluorescence spectrometry, scanning electron microscope and energy-dispersive x-ray spectrometry, energy-dispersive x-ray fluorescence spectrometry, inductively coupled plasma atomic emission spectrometry, x-ray diffraction spectrometry (XRD), and x-ray photoelectron spectroscopy (XPS). Detailed comparison of data confirmed that the TXRF method itself was not sufficient tomore » determine all the elements (Z > 11) contained in the samples. In addition, results suggest that XRD should be combined with XPS in order to accurately determine compound composition. This study demonstrates that at least two analytical methods should be used in order to analyze the composition of unknown real samples.« less

  2. Structural studies of homoisoflavonoids: NMR spectroscopy, X-ray diffraction, and theoretical calculations

    NASA Astrophysics Data System (ADS)

    Sievänen, Elina; Toušek, Jaromír; Lunerová, Kamila; Marek, Jaromír; Jankovská, Dagmar; Dvorská, Margita; Marek, Radek

    2010-08-01

    In this article we present a detailed structural investigation for five homoisoflavonoids, molecules important from the pharmacological point of view. For studying the electron distribution as well as its influence on the physicochemical properties, NMR spectroscopy, X-ray diffraction, and theoretical calculations have been used. Nuclear magnetic shieldings obtained by using DFT calculations for optimized molecular geometries are correlated with the experimentally determined chemical shifts. The theoretical data are well in agreement with the experimental values. The single crystal X-ray structures of homoisoflavonoid derivatives 1, 3, and 4 have been solved. The molecular geometries and crystal packing determined by X-ray diffraction are used for characterizing the intermolecular interactions. Electron distribution is crucial for the stability of radicals and hence the antioxidant efficiency of flavonoid structures. The hydrogen bonding governs the formation of complexes of homoisoflavonoids with biological targets.

  3. 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

  4. Inter-diffusion of copper and hafnium as studied by x-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Pearson, Justin; Chourasia, A. R.

    The Cu/Hf interface has been characterized by x-ray photoelectron spectroscopy. Thin films (thicknesses ranging from 100 nm to 150 nm) of hafnium were deposited on a silicon substrate. About 80 nm of copper was then deposited on such samples. The e-beam method was used for the deposition. The samples were annealed for 30 min at temperatures of 100, 200, 300, 400, and 500°C. The inter-diffusion of copper and hafnium was investigated by sequential sputter depth profiling and x-ray photoelectron spectroscopy. The interdiffusion in each case was analyzed by the Matano-Boltzmann's procedure using the Fick's second law. The interdiffusion coefficients and the width of the interface as determined from the data have been correlated with the annealing temperature. Supported by Organized Research, TAMU-Commerce.

  5. 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.

  6. Photon-in photon-out hard X-ray spectroscopy at the Linac Coherent Light Source

    DOE PAGES

    Alonso-Mori, Roberto; Sokaras, Dimosthenis; Zhu, Diling; ...

    2015-04-15

    X-ray free-electron lasers (FELs) have opened unprecedented possibilities to study the structure and dynamics of matter at an atomic level and ultra-fast timescale. Many of the techniques routinely used at storage ring facilities are being adapted for experiments conducted at FELs. In order to take full advantage of these new sources several challenges have to be overcome. They are related to the very different source characteristics and its resulting impact on sample delivery, X-ray optics, X-ray detection and data acquisition. Here it is described how photon-in photon-out hard X-ray spectroscopy techniques can be applied to study the electronic structure andmore » its dynamics of transition metal systems with ultra-bright and ultra-short FEL X-ray pulses. In particular, some of the experimental details that are different compared with synchrotron-based setups are discussed and illustrated by recent measurements performed at the Linac Coherent Light Source.« less

  7. Hydrothermal Diamond Anvil Cell (HDAC): From Visual Observation to X-ray Absorption Spectroscopy

    NASA Astrophysics Data System (ADS)

    Bassett, W. A.; Mibe, K.

    2006-05-01

    A fluid sample contained in a Re gasket between two diamond anvils can be subjected to pressures up to 2.5 GPa and temperatures up to 1200°C in a resistively heated hydrothermal diamond anvil cell (HDAC). Thermocouples are used to measure temperature. The constant-volume sample chamber permits isochoric measurements that can be used to determine pressure from the equation of state of H2O and to map phases and properties in P-T space. A movie of reactions between K-feldspar and water up to 2.5 GPa and 880°C illustrates the use of visual observations for mapping coexisting solution, melt, and solid phases. X-ray absorption spectroscopy of ZnBr2 in solution up to 500°C and 500 MPa shows hydrogen bond breaking in the hydration shells of the ZnBr42- and Br- ions with increasing temperature. In other studies the stability field of ikaite (CaCO3·6H2O) has been mapped by visual observation and Raman spectroscopy; the phases of montmorillonite have been mapped by X-ray diffraction; and the leaching of Pb from zircon has been measured by X-ray microprobe.

  8. Remote X-Ray Diffraction and X-Ray Fluorescence Analysis on Planetary Surfaces

    NASA Technical Reports Server (NTRS)

    Blake, David F.; DeVincenzi, D. (Technical Monitor)

    1999-01-01

    The legacy of planetary X-ray Diffraction (XRD) and X-ray Fluorescence (XRF) began in 1960 when W. Parish proposed an XRD instrument for deployment on the moon. The instrument was built and flight qualified, but the Lunar XRD program was cancelled shortly before the first human landing in 1969. XRF chemical data have been collected in situ by surface landers on Mars (Viking 1 & 2, Pathfinder) and Venus (Venera 13 & 14). These highly successful experiments provide critical constraints on our current understanding of surface processes and planetary evolution. However, the mineralogy, which is more critical to planetary surface science than simple chemical analysis, will remain unknown or will at best be imprecisely constrained until X-ray diffraction (XRD) data are collected. Recent progress in X-ray detector technology allows the consideration of simultaneous XRD (mineralogic analysis) and high-precision XRF (elemental analysis) in systems miniaturized to the point where they can be mounted on fixed landers or small robotic rovers. There is a variety of potential targets for XRD/XRF equipped landers within the solar system, the most compelling of which are the poles of the moon, the southern highlands of Mars and Europa.

  9. Dual crystal x-ray spectrometer at 1.8 keV for high repetition-rate single-photon counting spectroscopy experiments

    DOE PAGES

    Gamboa, E. J.; Bachmann, B.; Kraus, D.; ...

    2016-08-01

    The recent development of high-repetition rate x-ray free electron lasers (FEL), makes it possible to perform x-ray scattering and emission spectroscopy measurements from thin foils or gasses heated to high-energy density conditions by integrating over many experimental shots. Since the expected signal may be weaker than the typical CCD readout noise over the region-of-interest, it is critical to the success of this approach to use a detector with high-energy resolution so that single x-ray photons may be isolated. We describe a dual channel x-ray spectrometer developed for the Atomic and Molecular Optics endstation at the Linac Coherent Light Source (LCLS)more » for x-ray spectroscopy near the K-edge of aluminum. The spectrometer is based on a pair of curved PET (002) crystals coupled to a single pnCCD detector which simultaneously measures x-ray scattering and emission in the forward and backward directions. Furthermore, the signals from single x-ray photons are accumulated permitting continuous single-shot acquisition at 120 Hz.« less

  10. Data reduction and analysis for the graphite crystal X-ray spectrometer and polarimeter experiment flown aboard OSO-8 spacecraft

    NASA Technical Reports Server (NTRS)

    Novick, R.

    1980-01-01

    The documentation and software programs developed for the reception, initial processing (quickbook), and production analysis of data obtained by solar X-ray spectroscopy, stellar spectroscopy, and X-ray polarimetry experiments on OSO-8 are listed. The effectiveness and sensitivity of the Bragg crystal scattering instruments used are assessed. The polarization data polarimetric data obtained shows that some X-ray sources are polarized and that a larger polarimeter of this type is required to perform the measurements necessary to fully understand the physics of X-ray sources. The scanning Bragg crystal spectrometer was ideally suited for studying rapidly changing solar conditions. Observations of the Crab Nebula and pulsar, Cyg X-1, Cyg X-2, Cyg X-3, Sco X-1, Cen X-3, and Her X-1 are discussed as well as of 4U1656-53 and 4U1820-30. Evidence was obtained for iron line emission from Cyg X-3.

  11. High resolution X- and gamma-ray spectroscopy of cosmic X-ray sources

    NASA Technical Reports Server (NTRS)

    Lin, R. P.

    1983-01-01

    A high resolution X-ray spectrometer and large area phoswich detector were designed and co-aligned in a common elevation mounting in order to measure solar and cosmic X-ray and gamma ray emission in the 13 to 600 KeV energy range from a balloon. The instrument is described and results obtained for the Crab Nebula, the supernova remnant Cas A, and the Sun are discussed and analyzed.

  12. Plasma synthesis, Mössbauer spectroscopy and X-ray diffraction studies of nanosized iron oxides

    NASA Astrophysics Data System (ADS)

    Paneva, Daniela; Zaharieva, Katerina; Grabis, Janis; Mitov, Ivan; Vissokov, Gheorghi

    2010-06-01

    In this article synthesis and study of iron oxide nanopowders are described. The synthesis of sample 1 and sample 2—iron oxides—was carried out by electric arc plasma cutting of ordinary steel. The sample 3 was prepared by evaporation of Fe2O3/FeO mixture in radio-frequency nitrogen plasma. The characterization of the as prepared iron oxide nanoproducts was achieved by means of Mössbauer spectroscopy and X-ray diffraction analysis. The presence of different phases of iron oxide with a basic phase Fe3 - xO4 (magnetite), additional Fe1 - xO (wüstite) and α or γ-Fe2O3 (hematite or maghemite) with superparamagnetic particles for sample 1 and sample 2 and Fe3 - xO4 (magnetite) for sample 3 is observed.

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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Kühl, Frank-Christian, E-mail: Frank-christian.kuehl@mail.de; Müller, Matthias, E-mail: matthias.mueller@llg-ev.de; Schellhorn, Meike

    2016-07-15

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

  14. Annealing induced atomic rearrangements on (Ga,In) (N,As) probed by hard X-ray photoelectron spectroscopy and X-ray absorption fine structure.

    PubMed

    Ishikawa, Fumitaro; Higashi, Kotaro; Fuyuno, Satoshi; Morifuji, Masato; Kondow, Masahiko; Trampert, Achim

    2018-04-13

    We study the effects of annealing on (Ga 0.64 ,In 0.36 ) (N 0.045 ,As 0.955 ) using hard X-ray photoelectron spectroscopy and X-ray absorption fine structure measurements. We observed surface oxidation and termination of the N-As bond defects caused by the annealing process. Specifically, we observed a characteristic chemical shift towards lower binding energies in the photoelectron spectra related to In. This phenomenon appears to be caused by the atomic arrangement, which produces increased In-N bond configurations within the matrix, as indicated by the X-ray absorption fine structure measurements. The reduction in the binding energies of group-III In, which occurs concomitantly with the atomic rearrangements of the matrix, causes the differences in the electronic properties of the system before and after annealing.

  15. X-Ray Absorption near Edge Structure Spectroscopy of Nanodiamonds from the Allende Meteorite

    NASA Technical Reports Server (NTRS)

    Flynn, G. J.; Keller, L. P.; Hill, H.; Jacobsen, C.; Wirick, S.

    2000-01-01

    Carbon X-ray Absorption Near Edge Structure Spectroscopy shows Allende DM nanodiamonds have two pre-edge peaks, consistent with other small diamonds, but fail to show a diamond exciton which is seen in 3.6 nm diamond thin films.

  16. X-ray Weak Broad-line Qquasars: Absorption or Intrinsic X-ray Weakness

    NASA Technical Reports Server (NTRS)

    Mushotzky, Richard (Technical Monitor); Risaliti, Guida

    2005-01-01

    XMM observations of X-ray weak quasars have been performed during 2003 and 2004. The data for all the observations have become available in 2004 (there has been a delay of several months on the initial schedule, due to high background flares which contaminated the observations: as a consequence, most of them had to be rescheduled). We have reduced and analyzed all the data, and obtained interesting scientific results. Out of the eight sources, 4 are confirmed to be extremely X-ray weak, in agreement with the results of previous Chandra observations. 3 sources are confined to be highly variable both in flux (by factor 20-50) and in spectral properties (dramatic changes in spectral index). For both these groups of objects we are completing a publication: 1) For the X-ray weak sources, a paper is submitted with a complete analysis of the X-ray spectra both from Chandra and XMM-Newton, and a comparison with optical and near-IR photometry obtained from all-sky surveys. Possible models for the unusual spectral energy distribution of these sources are also presented. 2) For the variable sources, a paper is being finalized where the X-ray spectra obtained with XMM-Newton are compared with previous X-ray observations and with observations at other wavelengths. It is shown that these sources are high luminosity and extreme cases of the highly variable class of narrow-line Seyfert Is. In order to further understand the nature of these X-ray weak quasars, we submitted proposals for spectroscopy at optical and infrared telescopes. We obtained time at the TNG 4 meter telescope for near-IR observations and at the Hobby-Eberly Telescope for optical high-resolution spectroscopy. These observations have been performed in early 2004. They will complement the XMM data and will lead to understanding of whether the X-ray weakness of these sources is an intrinsic property or is due to absorption by circum-nuclear material. The infrared spectra of the variable sources have been already

  17. 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.

  18. Photometric, Spectroscopic, and X-ray Analysis of the Cool Algol BD+05 706

    NASA Astrophysics Data System (ADS)

    Torres, G.; Mader, J.; Marschall, L. A.; Neuhaeuser, R.; Duffy, A. S.

    2000-12-01

    BD+05 706 is an example of a rare class of a dozen or so interacting binaries called ``cool Algols", in which both components of the system are late-type stars. By contrast, the ``classical Algols" are systems in which the star transfering mass is of late spectral type, but the mass gainer is much hotter. BD+05 706 was shown previously to be eclipsing (Marschall, Torres & Neuhaeuser 1998, BAAS, 30, 835). In this paper we report our complete analysis of BVRI light curves for the system obtained at Gettysburg College Observatory, together with spectroscopy from the Harvard-Smithsonian Center for Astrophysics reported previously (Torres, Neuhaeuser & Wichmann 1998, AJ, 115, 2028), and X-ray observations obtained with the ROSAT satellite. Our light curve analysis indicates the presence of spots, most likely on the more massive, active component (primary), which change from season to season. Our results confirm the semi-detached nature of the system, and combined with the spectroscopy they have allowed us to obtain the most precise absolute masses and radii for any object of this class. Our X-ray light curve for BD+05 706 shows the primary eclipse clearly, but no sign of a secondary eclipse, confirming that the primary is the active star. Strong X-ray flares are also visible.

  19. 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).

  20. X-ray Emission Spectroscopy of Biomimetic Mn Coordination Complexes.

    PubMed

    Jensen, Scott C; Davis, Katherine M; Sullivan, Brendan; Hartzler, Daniel A; Seidler, Gerald T; Casa, Diego M; Kasman, Elina; Colmer, Hannah E; Massie, Allyssa A; Jackson, Timothy A; Pushkar, Yulia

    2017-06-15

    Understanding the function of Mn ions in biological and chemical redox catalysis requires precise knowledge of their electronic structure. X-ray emission spectroscopy (XES) is an emerging technique with a growing application to biological and biomimetic systems. Here, we report an improved, cost-effective spectrometer used to analyze two biomimetic coordination compounds, [Mn IV (OH) 2 (Me 2 EBC)] 2+ and [Mn IV (O)(OH)(Me 2 EBC)] + , the second of which contains a key Mn IV ═O structural fragment. Despite having the same formal oxidation state (Mn IV ) and tetradentate ligands, XES spectra from these two compounds demonstrate different electronic structures. Experimental measurements and DFT calculations yield different localized spin densities for the two complexes resulting from Mn IV -OH conversion to Mn IV ═O. The relevance of the observed spectroscopic changes is discussed for applications in analyzing complex biological systems such as photosystem II. A model of the S 3 intermediate state of photosystem II containing a Mn IV ═O fragment is compared to recent time-resolved X-ray diffraction data of the same state.

  1. Clocking Femtosecond Collisional Dynamics via Resonant X-Ray Spectroscopy

    DOE PAGES

    van den Berg, Q. Y.; Fernandez-Tello, E. V.; Burian, T.; ...

    2018-02-01

    Electron-ion collisional dynamics is of fundamental importance in determining plasma transport properties, nonequilibrium plasma evolution, and electron damage in diffraction imaging applications using bright x-ray free-electron lasers (FELs). Here in this paper, we describe the first experimental measurements of ultrafast electron impact collisional ionization dynamics using resonant core-hole spectroscopy in a solid-density magnesium plasma, created and diagnosed with the Linac Coherent Light Source x-ray FEL. By resonantly pumping the 1s → 2p transition in highly charged ions within an optically thin plasma, we have measured how off-resonance charge states are populated via collisional processes on femtosecond time scales. We presentmore » a collisional cross section model that matches our results and demonstrates how the cross sections are enhanced by dense-plasma effects including continuum lowering. Nonlocal thermodynamic equilibrium collisional radiative simulations show excellent agreement with the experimental results and provide new insight on collisional ionization and three-body-recombination processes in the dense-plasma regime.« less

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

    NASA Astrophysics Data System (ADS)

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

    2017-04-01

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

  3. X-ray absorption spectroscopy investigations on oxidized Ni/Au contacts to p-GaN.

    PubMed

    Jan, J C; Asokan, K; Chiou, J W; Pong, W F; Tseng, P K; Chen, L C; Chen, F R; Lee, J F; Wu, J S; Lin, H J; Chen, C T

    2001-03-01

    X-ray absorption spectroscopy was used to investigate the electronic structure of as-deposited and oxidized Ni/Au contacts to p-GaN and to elucidate the mechanism responsible for low impedance. X-ray absorption near edge spectra of Ni K- and L3,2-edges clearly indicate formation of NiO on the sample surface after annealing. The reason for low impedance may be attributed to increase in hole concentration and existence of p-NiO layer on the surface.

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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Cahill, A. D., E-mail: adc87@cornell.edu; Hoyt, C. L., E-mail: adc87@cornell.edu; Shelkovenko, T. A., E-mail: adc87@cornell.edu

    2014-12-15

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

  5. Ultrafast X-Ray Absorption Spectroscopy of Isochorically Heated Warm Dense Matter

    NASA Astrophysics Data System (ADS)

    Engelhorn, Kyle Craig

    This dissertation will present a series of new tools, together with new techniques, focused on the understanding of warm and dense matter. We report on the development of a high time resolution and high detection efficiency x-ray camera. The camera is integrated with a short pulse laser and an x-ray beamline at the Advanced Light Source synchrotron. This provides an instrument for single shot, broadband x-ray absorption spectroscopy of warm and dense matter with 2 picosecond time resolution. Warm and dense matter is created by isochorically heating samples of known density with an ultrafast optical laser pulse, and X-ray absorption spectroscopy probes the unoccupied electronic density of states before the onset of hydrodynamic expansion and electron-ion equilibrium is reached. Measured spectra from a variety of materials are compared with first principle molecular dynamics and density functional theory calculations. In heated silicon dioxide spectra, two novel pre-edge features are observed, a peak below the band gap and absorption within the band gap, while a reduction was observed in the features above the edge. From consideration of the calculated spectra, the peak below the gap is attributed to valence electrons that have been promoted to the conduction band, the absorption within the gap is attributed to broken Si-O bonds, and the reduction above the edge is attributed to an elevated ionic temperature. In heated copper spectra, a time-dependent shift and broadening of the absorption edge are observed, consistent with and elevated electron temperature. The temporal evolution of the electronic temperature is accurately determined by fitting the measured spectra with calculated spectra. The electron-ion equilibration is studied with a two-temperature model. In heated nickel spectra, a shift of the absorption edge is observed. This shift is found to be inconsistent with calculated spectra and independent of incident laser fluence. A shift of the chemical potential

  6. The X-ray Astronomy Recovery Mission

    NASA Astrophysics Data System (ADS)

    Tashiro, M.; Kelley, R.

    2017-10-01

    On 25 March 2016, the Japanese 6th X-ray astronomical satellite ASTRO-H (Hitomi), launched on February 17, lost communication after a series of mishap in its attitude control system. In response to the mishap the X-ray astronomy community and JAXA analyzed the direct and root cause of the mishap and investigated possibility of a recovery mission with the international collaborator NASA and ESA. Thanks to great effort of scientists, agencies, and governments, the X-ray Astronomy Recovery Mission (XARM) are proposed. The recovery mission is planned to resume high resolution X-ray spectroscopy with imaging realized by Hitomi under the international collaboration in the shortest time possible, simply by focusing one of the main science goals of Hitomi Resolving astrophysical problems by precise high-resolution X-ray spectroscopy'. XARM will carry a 6 x 6 pixelized X-ray micro-calorimeter on the focal plane of an X-ray mirror assembly, and an aligned X-ray CCD camera covering the same energy band and wider field of view, but no hard X-ray or soft gamma-ray instruments are onboard. In this paper, we introduce the science objectives, mission concept, and schedule of XARM.

  7. Revealing hole trapping in zinc oxide nanoparticles by time-resolved X-ray spectroscopy

    DOE PAGES

    Penfold, Thomas J.; Szlachetko, Jakub; Santomauro, Fabio G.; ...

    2018-02-02

    Nanostructures of transition metal oxides (TMO), such as ZnO, have attracted considerable interest for solar-energy conversion and photocatalysis. For the latter, trapping of charge carriers has an essential role. The probing of electron trapping in the conduction band of room temperature photoexcited TMOs has recently become possible owing to the emergence of time-resolved element-sensitive methods, such as X-ray spectroscopy. However, because the valence band of TMOs is dominated by the oxygen 2p orbitals,holes have so far escaped observation. Herein we use a novel dispersive X-ray emission spectrometer combined with X-ray absorption spectroscopy to directly probe the charge carrier relaxation andmore » trapping pro-cesses in ZnO nanoparticles after above band-gap photoexcitation. Here, our results, supported by simulations, demonstrate that within our temporal resolution of 80 ps, photo-excited holes are trapped at singly charged oxygen vacancies, turning them into doubly charged vacancies, which causes an outward displacement by approximately 15% of the four surrounding Zn atoms away from the central vacancy. These traps recombine radiatively with the delocalised electrons of the conduction band yielding the commonly observed green luminescence. This identification of the hole traps and their evolution provides new insight for future developments of TMO-based nanodevices.« less

  8. Revealing hole trapping in zinc oxide nanoparticles by time-resolved X-ray spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Penfold, Thomas J.; Szlachetko, Jakub; Santomauro, Fabio G.

    Nanostructures of transition metal oxides (TMO), such as ZnO, have attracted considerable interest for solar-energy conversion and photocatalysis. For the latter, trapping of charge carriers has an essential role. The probing of electron trapping in the conduction band of room temperature photoexcited TMOs has recently become possible owing to the emergence of time-resolved element-sensitive methods, such as X-ray spectroscopy. However, because the valence band of TMOs is dominated by the oxygen 2p orbitals,holes have so far escaped observation. Herein we use a novel dispersive X-ray emission spectrometer combined with X-ray absorption spectroscopy to directly probe the charge carrier relaxation andmore » trapping pro-cesses in ZnO nanoparticles after above band-gap photoexcitation. Here, our results, supported by simulations, demonstrate that within our temporal resolution of 80 ps, photo-excited holes are trapped at singly charged oxygen vacancies, turning them into doubly charged vacancies, which causes an outward displacement by approximately 15% of the four surrounding Zn atoms away from the central vacancy. These traps recombine radiatively with the delocalised electrons of the conduction band yielding the commonly observed green luminescence. This identification of the hole traps and their evolution provides new insight for future developments of TMO-based nanodevices.« less

  9. New Optimizations of Microcalorimeter Arrays for High-Resolution Imaging X-ray Spectroscopy

    NASA Astrophysics Data System (ADS)

    Kilbourne, Caroline

    We propose to continue our successful research program in developing arrays of superconducting transition-edge sensors (TES) for x-ray astrophysics. Our standard 0.3 mm TES pixel achieves better than 2.5-eV resolution, and we now make 32x32 arrays of such pixels. We have also achieved better than 1-eV resolution in smaller pixels, and promising performance in a range of position-sensitive designs. We propose to continue to advance the designs of both the single-pixel and position-sensitive microcalorimeters so that we can produce arrays suitable for several x-ray spectroscopy observatories presently in formulation. We will also investigate various array and pixel optimizations such as would be needed for large arrays for surveys, large- pixel arrays for diffuse soft x-ray measurements, or sub-arrays of fast pixels optimized for neutron-star burst spectroscopy. In addition, we will develop fabrication processes for integrating sub-arrays with very different pixel designs into a monolithic focal-plane array to simplify the design of the focal-plane assembly and make feasible new detector configurations such as the one currently baselined for AXSIO. Through a series of measurements on test devices, we have improved our understanding of the weak-link physics governing the observed resistive transitions in TES detectors. We propose to build on that work and ultimately use the results to improve the immunity of the detector to environmental magnetic fields, as well as its fundamental performance, in each of the targeted optimizations we are developing.

  10. Use of portable X-ray fluorescence spectroscopy and geostatistics for health risk assessment.

    PubMed

    Yang, Meng; Wang, Cheng; Yang, Zhao-Ping; Yan, Nan; Li, Feng-Ying; Diao, Yi-Wei; Chen, Min-Dong; Li, Hui-Ming; Wang, Jin-Hua; Qian, Xin

    2018-05-30

    Laboratory analysis of trace metals using inductively coupled plasma (ICP) spectroscopy is not cost effective, and the complex spatial distribution of soil trace metals makes their spatial analysis and prediction problematic. Thus, for the health risk assessment of exposure to trace metals in soils, portable X-ray fluorescence (PXRF) spectroscopy was used to replace ICP spectroscopy for metal analysis, and robust geostatistical methods were used to identify spatial outliers in trace metal concentrations and to map trace metal distributions. A case study was carried out around an industrial area in Nanjing, China. The results showed that PXRF spectroscopy provided results for trace metal (Cu, Ni, Pb and Zn) levels comparable to ICP spectroscopy. The results of the health risk assessment showed that Ni posed a higher non-carcinogenic risk than Cu, Pb and Zn, indicating a higher priority of concern than the other elements. Sampling locations associated with adverse health effects were identified as 'hotspots', and high-risk areas were delineated from risk maps. These 'hotspots' and high-risk areas were in close proximity to and downwind from petrochemical plants, indicating the dominant role of industrial activities as the major sources of trace metals in soils. The approach used in this study could be adopted as a cost-effective methodology for screening 'hotspots' and priority areas of concern for cost-efficient health risk management. Copyright © 2018 Elsevier Inc. All rights reserved.

  11. Speciation of metal(loid)s in environmental samples by X-ray absorption spectroscopy: a critical review.

    PubMed

    Gräfe, Markus; Donner, Erica; Collins, Richard N; Lombi, Enzo

    2014-04-25

    Element specificity is one of the key factors underlying the widespread use and acceptance of X-ray absorption spectroscopy (XAS) as a research tool in the environmental and geo-sciences. Independent of physical state (solid, liquid, gas), XAS analyses of metal(loid)s in complex environmental matrices over the past two decades have provided important information about speciation at environmentally relevant interfaces (e.g. solid-liquid) as well as in different media: plant tissues, rhizosphere, soils, sediments, ores, mineral process tailings, etc. Limited sample preparation requirements, the concomitant ability to preserve original physical and chemical states, and independence from crystallinity add to the advantages of using XAS in environmental investigations. Interpretations of XAS data are founded on sound physical and statistical models that can be applied to spectra of reference materials and mixed phases, respectively. For spectra collected directly from environmental matrices, abstract factor analysis and linear combination fitting provide the means to ascertain chemical, bonding, and crystalline states, and to extract quantitative information about their distribution within the data set. Through advances in optics, detectors, and data processing, X-ray fluorescence microprobes capable of focusing X-rays to micro- and nano-meter size have become competitive research venues for resolving the complexity of environmental samples at their inherent scale. The application of μ-XANES imaging, a new combinatorial approach of X-ray fluorescence spectrometry and XANES spectroscopy at the micron scale, is one of the latest technological advances allowing for lateral resolution of chemical states over wide areas due to vastly improved data processing and detector technology. Copyright © 2014. Published by Elsevier B.V.

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

    NASA Technical Reports Server (NTRS)

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

    2012-01-01

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

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

    DOE PAGES

    Lassalle-Kaiser, Benedikt; Gul, Sheraz; Kern, Jan; ...

    2017-05-02

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

  14. VETA-I x ray test analysis

    NASA Technical Reports Server (NTRS)

    Brissenden, R. J. V.; Chartas, G.; Freeman, M. D.; Hughes, J. P.; Kellogg, E. M.; Podgorski, W. A.; Schwartz, D. A.; Zhao, P.

    1992-01-01

    This interim report presents some definitive results from our analysis of the VETA-I x-ray testing data. It also provides a description of the hardware and software used in the conduct of the VETA-I x-ray test program performed at the MSFC x-ray Calibration Facility (XRCF). These test results also serve to supply data and information to include in the TRW final report required by DPD 692, DR XC04. To provide an authoritative compendium of results, we have taken nine papers as published in the SPIE Symposium, 'Grazing Incidence X-ray/EUV Optics for Astronomy and Projection Lithography' and have reproduced them as the content of this report.

  15. Simultaneous Femtosecond X-ray Spectroscopy and Diffraction of Photosystem II at Room Temperature

    PubMed Central

    Kern, Jan; Alonso-Mori, Roberto; Tran, Rosalie; Hattne, Johan; Gildea, Richard J.; Echols, Nathaniel; Glöckner, Carina; Hellmich, Julia; Laksmono, Hartawan; Sierra, Raymond G.; Lassalle-Kaiser, Benedikt; Koroidov, Sergey; Lampe, Alyssa; Han, Guangye; Gul, Sheraz; DiFiore, Dörte; Milathianaki, Despina; Fry, Alan R.; Miahnahri, Alan; Schafer, Donald W.; Messerschmidt, Marc; Seibert, M. Marvin; Koglin, Jason E.; Sokaras, Dimosthenis; Weng, Tsu-Chien; Sellberg, Jonas; Latimer, Matthew J.; Grosse-Kunstleve, Ralf W.; Zwart, Petrus H.; White, William E.; Glatzel, Pieter; Adams, Paul D.; Bogan, Michael J.; Williams, Garth J.; Boutet, Sébastien; Messinger, Johannes; Zouni, Athina; Sauter, Nicholas K.; Yachandra, Vittal K.; Bergmann, Uwe; Yano, Junko

    2013-01-01

    Intense femtosecond X-ray pulses produced at the Linac Coherent Light Source (LCLS) were used for simultaneous X-ray diffraction (XRD) and X-ray emission spectroscopy (XES) of microcrystals of Photosystem II (PS II) at room temperature. This method probes the overall protein structure and the electronic structure of the Mn4CaO5 cluster in the oxygen-evolving complex of PS II. XRD data are presented from both the dark state (S1) and the first illuminated state (S2) of PS II. Our simultaneous XRD/XES study shows that the PS II crystals are intact during our measurements at the LCLS, not only with respect to the structure of PS II, but also with regard to the electronic structure of the highly radiation sensitive Mn4CaO5 cluster, opening new directions for future dynamics studies. PMID:23413188

  16. Simultaneous femtosecond X-ray spectroscopy and diffraction of photosystem II at room temperature.

    PubMed

    Kern, Jan; Alonso-Mori, Roberto; Tran, Rosalie; Hattne, Johan; Gildea, Richard J; Echols, Nathaniel; Glöckner, Carina; Hellmich, Julia; Laksmono, Hartawan; Sierra, Raymond G; Lassalle-Kaiser, Benedikt; Koroidov, Sergey; Lampe, Alyssa; Han, Guangye; Gul, Sheraz; Difiore, Dörte; Milathianaki, Despina; Fry, Alan R; Miahnahri, Alan; Schafer, Donald W; Messerschmidt, Marc; Seibert, M Marvin; Koglin, Jason E; Sokaras, Dimosthenis; Weng, Tsu-Chien; Sellberg, Jonas; Latimer, Matthew J; Grosse-Kunstleve, Ralf W; Zwart, Petrus H; White, William E; Glatzel, Pieter; Adams, Paul D; Bogan, Michael J; Williams, Garth J; Boutet, Sébastien; Messinger, Johannes; Zouni, Athina; Sauter, Nicholas K; Yachandra, Vittal K; Bergmann, Uwe; Yano, Junko

    2013-04-26

    Intense femtosecond x-ray pulses produced at the Linac Coherent Light Source (LCLS) were used for simultaneous x-ray diffraction (XRD) and x-ray emission spectroscopy (XES) of microcrystals of photosystem II (PS II) at room temperature. This method probes the overall protein structure and the electronic structure of the Mn4CaO5 cluster in the oxygen-evolving complex of PS II. XRD data are presented from both the dark state (S1) and the first illuminated state (S2) of PS II. Our simultaneous XRD-XES study shows that the PS II crystals are intact during our measurements at the LCLS, not only with respect to the structure of PS II, but also with regard to the electronic structure of the highly radiation-sensitive Mn4CaO5 cluster, opening new directions for future dynamics studies.

  17. In-vivo analysis of the uptake process of heavy metals through maize roots by using synchrotron X-ray fluorescence spectroscopy

    NASA Astrophysics Data System (ADS)

    Hwang, Bae Geun; Lee, Sang Joon; Gil, Kyehwan

    2016-12-01

    The uptake of heavy metals by plants has been receiving much attention for crop contamination and phytoremediation. We employed synchrotron X-ray fluorescence (XRF) spectroscopy for an in-vivo analysis of heavy-metal uptake through a strand of maize root. A focused X-ray beam of 2.5 × 2.5 μm2 in physical dimensions was scanned along horizontal lines of the maize root at intervals of 3 μm at the 4B X-ray micro-diffraction beamline of the Pohang Accelerator Laboratory (PAL). Time-resolved mapping of the fluorescence intensities from multiple metallic elements in the root tissues provided information about the radial distributions of heavy-metal elements and their temporal variations. The concentrated core stream of heavy-metal elements spread radially up to roughly 500 μm, corresponding to 40 % of the root diameter. The absorption characteristics of three heavy metals, Cr, Mn and Ni, and their physiological features were analyzed. The absolute concentrations and the contents of the heavy-metal elements in the tested maize roots were quantitatively evaluated by using the calibration curve obtained from reference samples with preset concentrations. The uptake quantities of the tested heavy-metal elements are noticeably different, although their molecular weights are similar. This study should be helpful for understanding plant physiology related with heavy-metal uptake.

  18. Component analyses of urinary nanocrystallites of uric acid stone formers by combination of high-resolution transmission electron microscopy, fast Fourier transformation, energy dispersive X-ray spectroscopy, X-ray diffraction and Fourier transform infrared spectroscopy.

    PubMed

    Sun, Xin-Yuan; Xue, Jun-Fa; Xia, Zhi-Yue; Ouyang, Jian-Ming

    2015-06-01

    This study aimed to analyse the components of nanocrystallites in urines of patients with uric acid (UA) stones. X-ray diffraction (XRD), Fourier transform infrared spectroscopy, high-resolution transmission electron microscopy (HRTEM), fast Fourier transformation (FFT) of HRTEM, and energy dispersive X-ray spectroscopy (EDS) were performed to analyse the components of these nanocrystallites. XRD and FFT showed that the main component of urinary nanocrystallites was UA, which contains a small amount of calcium oxalate monohydrate and phosphates. EDS showed the characteristic absorption peaks of C, O, Ca and P. The formation of UA stones was closely related to a large number of UA nanocrystallites in urine. A combination of HRTEM, FFT, EDS and XRD analyses could be performed accurately to analyse the components of urinary nanocrystallites.

  19. X-ray and synchrotron methods in studies of cultural heritage sites

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Koval’chuk, M. V.; Yatsishina, E. B.; Blagov, A. E.

    2016-09-15

    X-ray and synchrotron methods that are most widely used in studies of cultural heritage objects (including archaeological sites)—X-ray diffraction analysis, X-ray spectroscopy, and visualization techniques— have been considered. The reported examples show high efficiency and informativeness of natural science studies when solving most diverse problems of archaeology, history, the study of art, museology, etc.

  20. Capillary Optics Based X-Ray Micro-Imaging Elemental Analysis

    NASA Astrophysics Data System (ADS)

    Hampai, D.; Dabagov, S. B.; Cappuccio, G.; Longoni, A.; Frizzi, T.; Cibin, G.

    2010-04-01

    A rapidly developed during the last few years micro-X-ray fluorescence spectrometry (μXRF) is a promising multi-elemental technique for non-destructive analysis. Typically it is rather hard to perform laboratory μXRF analysis because of the difficulty of producing an original small-size X-ray beam as well as its focusing. Recently developed for X-ray beam focusing polycapillary optics offers laboratory X-ray micro probes. The combination of polycapillary lens and fine-focused micro X-ray tube can provide high intensity radiation flux on a sample that is necessary in order to perform the elemental analysis. In comparison to a pinhole, an optimized "X-ray source-op tics" system can result in radiation density gain of more than 3 orders by the value. The most advanced way to get that result is to use the confocal configuration based on two X-ray lenses, one for the fluorescence excitation and the other for the detection of secondary emission from a sample studied. In case of X-ray capillary microfocusing a μXRF instrument designed in the confocal scheme allows us to obtain a 3D elemental mapping. In this work we will show preliminary results obtained with our prototype, a portable X-ray microscope for X-ray both imaging and fluorescence analysis; it enables μXRF elemental mapping simultaneously with X-ray imaging. A prototype of compact XRF spectrometer with a spatial resolution less than 100 μm has been designed.

  1. X-ray texture analysis of paper coating pigments and the correlation with chemical composition analysis

    NASA Astrophysics Data System (ADS)

    Roine, J.; Tenho, M.; Murtomaa, M.; Lehto, V.-P.; Kansanaho, R.

    2007-10-01

    The present research experiments the applicability of x-ray texture analysis in investigating the properties of paper coatings. The preferred orientations of kaolin, talc, ground calcium carbonate, and precipitated calcium carbonate particles used in four different paper coatings were determined qualitatively based on the measured crystal orientation data. The extent of the orientation, namely, the degree of the texture of each pigment, was characterized quantitatively using a single parameter. As a result, the effect of paper calendering is clearly seen as an increase on the degree of texture of the coating pigments. The effect of calendering on the preferred orientation of kaolin was also evident in an independent energy dispersive spectrometer analysis on micrometer scale and an electron spectroscopy for chemical analysis on nanometer scale. Thus, the present work proves x-ray texture analysis to be a potential research tool for characterizing the properties of paper coating layers.

  2. An x ray scatter approach for non-destructive chemical analysis of low atomic numbered elements

    NASA Technical Reports Server (NTRS)

    Ross, H. Richard

    1993-01-01

    A non-destructive x-ray scatter (XRS) approach has been developed, along with a rapid atomic scatter algorithm for the detection and analysis of low atomic-numbered elements in solids, powders, and liquids. The present method of energy dispersive x-ray fluorescence spectroscopy (EDXRF) makes the analysis of light elements (i.e., less than sodium; less than 11) extremely difficult. Detection and measurement become progressively worse as atomic numbers become smaller, due to a competing process called 'Auger Emission', which reduces fluorescent intensity, coupled with the high mass absorption coefficients exhibited by low energy x-rays, the detection and determination of low atomic-numbered elements by x-ray spectrometry is limited. However, an indirect approach based on the intensity ratio of Compton and Rayleigh scattered has been used to define light element components in alloys, plastics and other materials. This XRS technique provides qualitative and quantitative information about the overall constituents of a variety of samples.

  3. X-ray diagnostics of massive star winds

    NASA Astrophysics Data System (ADS)

    Oskinova, L. M.; Ignace, R.; Huenemoerder, D. P.

    2017-11-01

    Observations with powerful X-ray telescopes, such as XMM-Newton and Chandra, significantly advance our understanding of massive stars. Nearly all early-type stars are X-ray sources. Studies of their X-ray emission provide important diagnostics of stellar winds. High-resolution X-ray spectra of O-type stars are well explained when stellar wind clumping is taking into account, providing further support to a modern picture of stellar winds as non-stationary, inhomogeneous outflows. X-ray variability is detected from such winds, on time scales likely associated with stellar rotation. High-resolution X-ray spectroscopy indicates that the winds of late O-type stars are predominantly in a hot phase. Consequently, X-rays provide the best observational window to study these winds. X-ray spectroscopy of evolved, Wolf-Rayet type, stars allows to probe their powerful metal enhanced winds, while the mechanisms responsible for the X-ray emission of these stars are not yet understood.

  4. ID16B: a hard X-ray nanoprobe beamline at the ESRF for nano-analysis

    PubMed Central

    Martínez-Criado, Gema; Villanova, Julie; Tucoulou, Rémi; Salomon, Damien; Suuronen, Jussi-Petteri; Labouré, Sylvain; Guilloud, Cyril; Valls, Valentin; Barrett, Raymond; Gagliardini, Eric; Dabin, Yves; Baker, Robert; Bohic, Sylvain; Cohen, Cédric; Morse, John

    2016-01-01

    Within the framework of the ESRF Phase I Upgrade Programme, a new state-of-the-art synchrotron beamline ID16B has been recently developed for hard X-ray nano-analysis. The construction of ID16B was driven by research areas with major scientific and societal impact such as nanotechnology, earth and environmental sciences, and bio-medical research. Based on a canted undulator source, this long beamline provides hard X-ray nanobeams optimized mainly for spectroscopic applications, including the combination of X-ray fluorescence, X-ray diffraction, X-ray excited optical luminescence, X-ray absorption spectroscopy and 2D/3D X-ray imaging techniques. Its end-station re-uses part of the apparatus of the earlier ID22 beamline, while improving and enlarging the spectroscopic capabilities: for example, the experimental arrangement offers improved lateral spatial resolution (∼50 nm), a larger and more flexible capability for in situ experiments, and monochromatic nanobeams tunable over a wider energy range which now includes the hard X-ray regime (5–70 keV). This paper describes the characteristics of this new facility, short-term technical developments and the first scientific results. PMID:26698084

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

    NASA Astrophysics Data System (ADS)

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

    2018-01-01

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

  6. Elemental profiling of laser cladded multilayer coatings by laser induced breakdown spectroscopy and energy dispersive X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Lednev, V. N.; Sdvizhenskii, P. A.; Filippov, M. N.; Grishin, M. Ya.; Filichkina, V. A.; Stavertiy, A. Ya.; Tretyakov, R. S.; Bunkin, A. F.; Pershin, S. M.

    2017-09-01

    Multilayer tungsten carbide wear resistant coatings were analyzed by laser induced breakdown spectroscopy (LIBS) and energy dispersive X-ray (EDX) spectroscopy. Coaxial laser cladding technique was utilized to produce tungsten carbide coating deposited on low alloy steel substrate with additional inconel 625 interlayer. EDX and LIBS techniques were used for elemental profiling of major components (Ni, W, C, Fe, etc.) in the coating. A good correlation between EDX and LIBS data was observed while LIBS provided additional information on light element distribution (carbon). A non-uniform distribution of tungsten carbide grains along coating depth was detected by both LIBS and EDX. In contrast, horizontal elemental profiling showed a uniform tungsten carbide particles distribution. Depth elemental profiling by layer-by-layer LIBS analysis was demonstrated to be an effective method for studying tungsten carbide grains distribution in wear resistant coating without any sample preparation.

  7. Origin of Pressure-induced Superconducting Phase in K xFe 2-ySe 2 studied by Synchrotron X-ray Diffraction and Spectroscopy

    DOE PAGES

    Yamamoto, Yoshiya; Yamaoka, Hitoshi; Tanaka, Masashi; ...

    2016-08-08

    Pressure dependence of the electronic and crystal structures of K xFe 2–ySe 2, which has pressure-induced two superconducting domes of SC I and SC II, was investigated by x-ray emission spectroscopy and diffraction. X-ray diffraction data show that compressibility along the c-axis changes around 12 GPa, where a new superconducting phase of SC II appears. This suggests a possible tetragonal to collapsed tetragonal phase transition. X-ray emission spectroscopy data also shows the change in the electronic structure around 12 GPa. These results can be explained by the scenario that the two SC domes under pressure originate from the change ofmore » Fermi surface topology. Lastly, our results here show the pronounced increase of the density of states near the Fermi surface under pressure with a structural phase transition, which can help address our fundamental understanding for the appearance of the SC II phase.« less

  8. X-ray photoelectron spectroscopy for characterization of wood surfaces in adhesion studies

    Treesearch

    James F. Beecher; Charles R. Frihart

    2005-01-01

    X-ray photoelectron spectroscopy (XPS) is one of a set of tools that have been used to characterize wood surfaces. Among the advantages of XPS are surface sensitivity, identification of nearly all elements, and frequently, discrimination of bonding states. For these reasons, XPS seemed to be an appropriate tool to help explain the differences in bond strength under wet...

  9. Atomic Data in X-Ray Astrophysics

    NASA Technical Reports Server (NTRS)

    Brickhouse, N. S.

    2000-01-01

    With the launches of the Chandra X-ray Observatory (CXO) and the X-ray Multimirror Mission (XMM) and the upcoming launch of the Japanese mission ASTRO-E, high resolution X-ray spectroscopy of cosmic sources has begun. Early, deep observations of three stellar coronal sources will provide not only invaluable calibration data, but will also give us benchmarks for the atomic data under collisional equilibrium conditions. Analysis of the Chandra X-ray Observatory data, and data from other telescopes taken simultaneously, for these stars is ongoing as part of the Emission Line Project. Goals of the Emission Line Project are: (1) to determine and verify accurate and robust diagnostics and (2) to identify and prioritize issues in fundamental spectroscopy which will require further theoretical and/or laboratory work. The Astrophysical Plasma Emission Database will be described in some detail, as it is introducing standardization and flexibility into X-ray spectral modeling. Spectral models of X-ray astrophysical plasmas can be generally classified as dominated by either collisional ionization or by X-ray photoionization. While the atomic data needs for spectral models under these two types of ionization are significantly different, there axe overlapping data needs, as I will describe. Early results from the Emission Line Project benchmarks are providing an invaluable starting place, but continuing work to improve the accuracy and completeness of atomic data is needed. Additionally, we consider the possibility that some sources will require that both collisional ionization and photoionization be taken into account, or that time-dependent ionization be considered. Thus plasma spectral models of general use need to be computed over a wide range of physical conditions.

  10. Combined use of infrared and hard X-ray microprobes for spectroscopy-based neuroanatomy

    NASA Astrophysics Data System (ADS)

    Surowka, A. D.; Ziomber, A.; Czyzycki, M.; Migliori, A.; Pieklo, L.; Kasper, K.; Szczerbowska-Boruchowska, M.

    2018-05-01

    Understanding the pathological triggers that affect the structural and physiological integrity of biochemical milieu of neurons is crucial to extend our knowledge on brain disorders, that are in many circumstances hardly treatable. Over recently, by using sophisticated hyperspectral micro-imaging modalities, it has been placed within our reach to get an insight into high fidelity histological details along with corresponding biochemical information in a label-free fashion, without using any additional chemical fixatives. However, in order to push forwards extensive application of these methods in the clinical arena, it is viable to make further iterations in novel data analysis protocols in order to boost their sensitivity. Therefore, in our study we proposed a new combined approach utilizing both benchtop Fourier transform infrared (FTIR) and synchrotron X-ray fluorescence (SR-XRF) micro-spectroscopies coupled with multivariate data clustering using the K-means algorithm for combined molecular and elemental micro-imaging, so that these complimentary analytical tools could be used for delineating between various brain structures based on their biochemical composition. By utilizing mid-IR transmission FTIR experiments, the biochemical composition in terms of lipids, proteins and phosphodiesters became accessible. In turn, the SR-XRF experiment was carried out at the advanced IAEA X-ray spectrometry station at Elettra Sincrotrone Trieste. By measuring in vacuum and by using the primary exciting X-ray beam, monochromatized to 10.5 keV, we took advantage of accessing the characteristic X-ray lines of a variety of elements ranging from carbon to zinc. Herein, we can report that the developed methodology has high specificity for label-free discriminating between lipid- and protein-rich brain tissue areas.

  11. 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).

  12. NuSTAR Hard X-Ray Survey of the Galactic Center Region I: Hard X-Ray Morphology and Spectroscopy of the Diffuse Emission

    NASA Astrophysics Data System (ADS)

    Mori, Kaya; Hailey, Charles J.; Krivonos, Roman; Hong, Jaesub; Ponti, Gabriele; Bauer, Franz; Perez, Kerstin; Nynka, Melania; Zhang, Shuo; Tomsick, John A.; Alexander, David M.; Baganoff, Frederick K.; Barret, Didier; Barrière, Nicolas; Boggs, Steven E.; Canipe, Alicia M.; Christensen, Finn E.; Craig, William W.; Forster, Karl; Giommi, Paolo; Grefenstette, Brian W.; Grindlay, Jonathan E.; Harrison, Fiona A.; Hornstrup, Allan; Kitaguchi, Takao; Koglin, Jason E.; Luu, Vy; Madsen, Kristen K.; Mao, Peter H.; Miyasaka, Hiromasa; Perri, Matteo; Pivovaroff, Michael J.; Puccetti, Simonetta; Rana, Vikram; Stern, Daniel; Westergaard, Niels J.; Zhang, William W.; Zoglauer, Andreas

    2015-12-01

    We present the first sub-arcminute images of the Galactic Center above 10 keV, obtained with NuSTAR. NuSTAR resolves the hard X-ray source IGR J17456-2901 into non-thermal X-ray filaments, molecular clouds, point sources, and a previously unknown central component of hard X-ray emission (CHXE). NuSTAR detects four non-thermal X-ray filaments, extending the detection of their power-law spectra with Γ ˜ 1.3-2.3 up to ˜50 keV. A morphological and spectral study of the filaments suggests that their origin may be heterogeneous, where previous studies suggested a common origin in young pulsar wind nebulae (PWNe). NuSTAR detects non-thermal X-ray continuum emission spatially correlated with the 6.4 keV Fe Kα fluorescence line emission associated with two Sgr A molecular clouds: MC1 and the Bridge. Broadband X-ray spectral analysis with a Monte-Carlo based X-ray reflection model self-consistently determined their intrinsic column density (˜1023 cm-2), primary X-ray spectra (power-laws with Γ ˜ 2) and set a lower limit of the X-ray luminosity of Sgr A* flare illuminating the Sgr A clouds to LX ≳ 1038 erg s-1. Above ˜20 keV, hard X-ray emission in the central 10 pc region around Sgr A* consists of the candidate PWN G359.95-0.04 and the CHXE, possibly resulting from an unresolved population of massive CVs with white dwarf masses MWD ˜ 0.9 M⊙. Spectral energy distribution analysis suggests that G359.95-0.04 is likely the hard X-ray counterpart of the ultra-high gamma-ray source HESS J1745-290, strongly favoring a leptonic origin of the GC TeV emission.

  13. Analysis of nutrition-relevant trace elements in human blood and serum by means of total reflection X-ray fluorescence (TXRF) spectroscopy

    NASA Astrophysics Data System (ADS)

    Stosnach, Hagen; Mages, Margarete

    2009-04-01

    In clinical service laboratories, one of the most common analytical tasks with regard to inorganic traces is the determination of the nutrition-relevant elements Fe, Cu, Zn, and Se. Because of the high numbers of samples and the commercial character of these analyses, a time-consuming sample preparation must be avoided. In this presentation, the results of total reflection X-ray fluorescence measurements with a low-power system and different sample preparation procedures are compared with those derived from analysis with common methods like Atomic Absorption Spectroscopy (AAS) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS). The results of these investigations indicate that the optimal total reflection X-ray fluorescence analysis of the nutrition-relevant elements Fe, Cu, Zn, and Se can be performed by preparing whole blood and serum samples after dilution with ultrapure water and transferring 10 μl of internally standardized sample to an unsiliconized quartz glass sample carrier with subsequent drying in a laboratory oven. Suitable measurement time was found to be 600 s. The enhanced sample preparation by means of microwave or open digestion, in parts combined with cold plasma ashing, led to an improvement of detection limits by a factor of 2 for serum samples while for whole blood samples an improvement was only observed for samples prepared by means of microwave digestion. As the matrix elements P, S, Cl, and for whole blood Fe have a major influence on the detection limits, most probably a further enhancement of analytical quality requires the removal of the organic matrix. However, for the routine analysis of the nutrition-relevant elements, the dilution preparation was found to be sufficient.

  14. Differentiation of dental restorative materials combining energy-dispersive X-ray fluorescence spectroscopy and post-mortem CT.

    PubMed

    Merriam, Tim; Kaufmann, Rolf; Ebert, Lars; Figi, Renato; Erni, Rolf; Pauer, Robin; Sieberth, Till

    2018-06-01

    Today, post-mortem computed tomography (CT) is routinely used for forensic identification. Mobile energy-dispersive X-ray fluorescence (EDXRF) spectroscopy of a dentition is a method of identification that has the potential to be easier and cheaper than CT, although it cannot be used with every dentition. In challenging cases, combining both techniques could facilitate the process of identification and prove to be advantageous over chemical analyses. Nine dental restorative material brands were analyzed using EDXRF spectroscopy. Their differentiability was assessed by comparing each material's x-ray fluorescence spectrum and then comparing the spectra to previous research investigating differentiability in CT. To verify EDXRF's precision and accuracy, select dental specimens underwent comparative electron beam excited x-ray spectroscopy (EDS) scans, while the impact of the restorative surface area was studied by scanning a row of dental specimens with varying restorative surface areas (n = 10). EDXRF was able to differentiate all 36 possible pairs of dental filling materials; however, dual-energy CT was only able to differentiate 33 out of 36. The EDS scans showed correlating x-ray fluorescence peaks on the x-ray spectra compared to our EDXRF. In addition, the surface area showed no influence on the differentiability of the dental filling materials. EDXRF has the potential to facilitate corpse identification by differentiating and comparing restorative materials, providing more information compared to post-mortem CT alone. Despite not being able to explicitly identify a brand without a control sample or database, its fast and mobile use could accelerate daily routines or mass victim identification processes. To achieve this goal, further development of EDXRF scanners for this application and further studies evaluating the method within a specific routine need to be performed.

  15. Charge and Spin-State Characterization of Cobalt Bis( o-dioxolene) Valence Tautomers Using Co Kβ X-ray Emission and L-Edge X-ray Absorption Spectroscopies

    DOE PAGES

    Liang, H. Winnie; Kroll, Thomas; Nordlund, Dennis; ...

    2016-12-30

    The valence tautomeric states of Co(phen)(3,5-DBQ) 2 and Co(tmeda)(3,5-DBQ) 2, where 3,5-DBQ is either the semiquinone (SQ –) or catecholate (Cat 2–) form of 3,5-di- tert-butyl-1,2-benzoquinone, have been examined by a series of cobalt-specific X-ray spectroscopies. In this work, we have utilized the sensitivity of 1s3p X-ray emission spectroscopy (Kβ XES) to the oxidation and spin states of 3d transition-metal ions to determine the cobalt-specific electronic structure of valence tautomers. A comparison of their Kβ XES spectra with the spectra of cobalt coordination complexes with known oxidation and spin states demonstrates that the low-temperature valence tautomer can be described asmore » a low-spin Co III configuration and the high-temperature valence tautomer as a high-spin Co II configuration. This conclusion is further supported by Co L-edge X-ray absorption spectroscopy (L-edge XAS) of the high-temperature valence tautomers and ligand-field atomic-multiplet calculations of the Kβ XES and L-edge XAS spectra. In conclusion, the nature and strength of the magnetic exchange interaction between the cobalt center and SQ – in cobalt valence tautomers is discussed in view of the effective spin at the Co site from Kβ XES and the molecular spin moment from magnetic susceptibility measurements.« less

  16. Charge and Spin-State Characterization of Cobalt Bis( o-dioxolene) Valence Tautomers Using Co Kβ X-ray Emission and L-Edge X-ray Absorption Spectroscopies

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Liang, H. Winnie; Kroll, Thomas; Nordlund, Dennis

    The valence tautomeric states of Co(phen)(3,5-DBQ) 2 and Co(tmeda)(3,5-DBQ) 2, where 3,5-DBQ is either the semiquinone (SQ –) or catecholate (Cat 2–) form of 3,5-di- tert-butyl-1,2-benzoquinone, have been examined by a series of cobalt-specific X-ray spectroscopies. In this work, we have utilized the sensitivity of 1s3p X-ray emission spectroscopy (Kβ XES) to the oxidation and spin states of 3d transition-metal ions to determine the cobalt-specific electronic structure of valence tautomers. A comparison of their Kβ XES spectra with the spectra of cobalt coordination complexes with known oxidation and spin states demonstrates that the low-temperature valence tautomer can be described asmore » a low-spin Co III configuration and the high-temperature valence tautomer as a high-spin Co II configuration. This conclusion is further supported by Co L-edge X-ray absorption spectroscopy (L-edge XAS) of the high-temperature valence tautomers and ligand-field atomic-multiplet calculations of the Kβ XES and L-edge XAS spectra. In conclusion, the nature and strength of the magnetic exchange interaction between the cobalt center and SQ – in cobalt valence tautomers is discussed in view of the effective spin at the Co site from Kβ XES and the molecular spin moment from magnetic susceptibility measurements.« less

  17. Analysis of electronic structure of amorphous InGaZnO/SiO{sub 2} interface by angle-resolved X-ray photoelectron spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Ueoka, Y.; Ishikawa, Y.; Maejima, N.

    2013-10-28

    The electronic structures of amorphous indium gallium zinc oxide (a-IGZO) on a SiO{sub 2} layers before and after annealing were observed by constant final state X-ray photoelectron spectroscopy (CFS-XPS) and X-ray adsorption near-edge structure spectroscopy (XANES). From the results of angle-resolved CFS-XPS, the change in the electronic state was clearly observed in the a-IGZO bulk rather than in the a-IGZO/SiO{sub 2} interface. This suggests that the electronic structures of the a-IGZO bulk strongly affected the thin-film transistor characteristics. The results of XANES indicated an increase in the number of tail states upon atmospheric annealing (AT). We consider that the increasemore » in the number of tail states decreased the channel mobility of AT samples.« less

  18. Counting-loss correction for X-ray spectroscopy using unit impulse pulse shaping.

    PubMed

    Hong, Xu; Zhou, Jianbin; Ni, Shijun; Ma, Yingjie; Yao, Jianfeng; Zhou, Wei; Liu, Yi; Wang, Min

    2018-03-01

    High-precision measurement of X-ray spectra is affected by the statistical fluctuation of the X-ray beam under low-counting-rate conditions. It is also limited by counting loss resulting from the dead-time of the system and pile-up pulse effects, especially in a high-counting-rate environment. In this paper a detection system based on a FAST-SDD detector and a new kind of unit impulse pulse-shaping method is presented, for counting-loss correction in X-ray spectroscopy. The unit impulse pulse-shaping method is evolved by inverse deviation of the pulse from a reset-type preamplifier and a C-R shaper. It is applied to obtain the true incoming rate of the system based on a general fast-slow channel processing model. The pulses in the fast channel are shaped to unit impulse pulse shape which possesses small width and no undershoot. The counting rate in the fast channel is corrected by evaluating the dead-time of the fast channel before it is used to correct the counting loss in the slow channel.

  19. X-ray photoelectron spectroscopy study of excimer laser treated alumina films

    NASA Astrophysics Data System (ADS)

    Georgiev, D. G.; Kolev, K.; Laude, L. D.; Mednikarov, B.; Starbov, N.

    1998-01-01

    Amorphous alumina layers are deposited on a single crystal Si substrate by a e-gun evaporation technique. These films are then thermally annealed in oxygen to be crystallized and, further, irradiated with an excimer laser beam. At each stage of the film preparation, an x-ray photoelectron spectroscopy analysis is performed at the film surface and in depth, upon ion beam grinding. Results give evidence for the formation of an aluminosilicate upon thermal annealing of the film in oxygen. At the surface itself, this compound is observed to decompose upon excimer laser irradiation at energy densities exceeding 1.75 J/cm2, giving rise to free Si atoms and SiO2, however with complete disappearance of Al atoms. Model photochemical reactions are proposed to explain such transformations.

  20. X-ray absorption spectroscopy characterization of embedded and extracted nano-oxides

    DOE PAGES

    Stan, Tiberiu; Sprouster, David J.; Ofan, Avishai; ...

    2016-12-29

    Here, the chemistries and structures of both embedded and extracted Ysingle bondTisingle bondO nanometer-scale oxides in a nanostructured ferritic alloy (NFA) were probed by x-ray absorption spectroscopy (XAS). Y 2Ti 2O 7 is the primary embedded phase, while the slightly larger extracted oxides are primarily Y 2TiO 5. Analysis of the embedded nano-oxides is difficult partly due to the multiple Ti environments associated with different oxides and those still residing in matrix lattice sites. Thus, bulk extraction followed by selective filtration was used to isolate the larger Y 2TiO 5 oxides for XAS, while the smaller predominant embedded phase Ymore » 2Ti 2O 7 oxides passed through the filters and were analyzed using the log-ratio method.« less

  1. Reactor for tracking catalyst nanoparticles in liquid at high temperature under a high-pressure gas phase with X-ray absorption spectroscopy.

    PubMed

    Nguyen, Luan; Tao, Franklin Feng

    2018-02-01

    Structure of catalyst nanoparticles dispersed in liquid phase at high temperature under gas phase of reactant(s) at higher pressure (≥5 bars) is important for fundamental understanding of catalytic reactions performed on these catalyst nanoparticles. Most structural characterizations of a catalyst performing catalysis in liquid at high temperature under gas phase at high pressure were performed in an ex situ condition in terms of characterizations before or after catalysis since, from technical point of view, access to the catalyst nanoparticles during catalysis in liquid phase at high temperature under high pressure reactant gas is challenging. Here we designed a reactor which allows us to perform structural characterization using X-ray absorption spectroscopy including X-ray absorption near edge structure spectroscopy and extended X-ray absorption fine structure spectroscopy to study catalyst nanoparticles under harsh catalysis conditions in terms of liquid up to 350 °C under gas phase with a pressure up to 50 bars. This reactor remains nanoparticles of a catalyst homogeneously dispersed in liquid during catalysis and X-ray absorption spectroscopy characterization.

  2. X-ray emission spectroscopy of biomimetic Mn coordination complexes

    DOE PAGES

    Jensen, Scott C.; Davis, Katherine M.; Sullivan,

    2017-05-19

    Understanding the function of Mn ions in biological and chemical redox catalysis requires precise knowledge of their electronic structure. X-ray emission spectroscopy (XES) is an emerging technique with a growing application to biological and biomimetic systems. Here, we report an improved, cost-effective spectrometer used to analyze two biomimetic coordination compounds, [Mn IV(OH) 2(Me 2EBC)] 2+ and [Mn IV(O)(OH)(Me 2EBC)] +, the second of which contains a key Mn IV=O structural fragment. Despite having the same formal oxidation state (Mn IV) and tetradentate ligands, XES spectra from these two compounds demonstrate different electronic structures. Experimental measurements and DFT calculations yield differentmore » localized spin densities for the two complexes resulting from Mn IV–OH conversion to Mn IV=O. The relevance of the observed spectroscopic changes is discussed for applications in analyzing complex biological systems such as photosystem II. In conclusion, a model of the S 3 intermediate state of photosystem II containing a Mn IV=O fragment is compared to recent time-resolved X-ray diffraction data of the same state.« less

  3. Single- and double-core-hole ion emission spectroscopy of transient neon plasmas produced by ultraintense x-ray laser pulses

    NASA Astrophysics Data System (ADS)

    Gao, Cheng; Zeng, Jiaolong; Yuan, Jianmin

    2016-02-01

    Single-core-hole (SCH) and double-core-hole (DCH) spectroscopy is investigated systematically for neon gas in the interaction with ultraintense x-ray pulses with photon energy from 937 eV to 2000 eV. A time-dependent rate equation, implemented in detailed level accounting approximation, is utilized to study the dynamical evolution of the level population and emission properties of the laser-produced highly transient plasmas. The plasma-density effects on level populations and charge-state distribution are demonstrated with an x-ray photon energy of 2000 eV. It is shown that atomic number density of relevant experiment is about 1 × 1018 cm-3, which is comparable to a recent experiment. At this density, we systematically investigate the emissivity of the transient neon plasmas. For laser photon energy in the range 937-1360 eV, resonant absorptions (RA) of 1s\\to {np} (n≥slant 2) transitions play important roles in time evolution of the population and DCH emission spectroscopy. The RA effects are illustrated in detail for an x-ray pulse of 944 eV photon energy, which creates the 1s\\to 2p RA from the SCH states (1s2{s}22{p}4, 1s2s2p5, and 1s2p6) of Ne3+. After averaging over the space and time distribution of x-ray pulse, DCH emission spectroscopy is studied at x-ray photon energies of 937, 944, 955, 968, 980, and 990 eV, where there exist 1s\\to 2p resonances from SCH states of Ne2+-Ne7+. The processes with producing DCH states are discussed. For x-ray photon energy larger than 1360 eV, no RA exist and transient plasmas show different features in the DCH spectroscopy.

  4. Monte Carlo simulation of X-ray imaging and spectroscopy experiments using quadric geometry and variance reduction techniques

    NASA Astrophysics Data System (ADS)

    Golosio, Bruno; Schoonjans, Tom; Brunetti, Antonio; Oliva, Piernicola; Masala, Giovanni Luca

    2014-03-01

    The simulation of X-ray imaging experiments is often performed using deterministic codes, which can be relatively fast and easy to use. However, such codes are generally not suitable for the simulation of even slightly more complex experimental conditions, involving, for instance, first-order or higher-order scattering, X-ray fluorescence emissions, or more complex geometries, particularly for experiments that combine spatial resolution with spectral information. In such cases, simulations are often performed using codes based on the Monte Carlo method. In a simple Monte Carlo approach, the interaction position of an X-ray photon and the state of the photon after an interaction are obtained simply according to the theoretical probability distributions. This approach may be quite inefficient because the final channels of interest may include only a limited region of space or photons produced by a rare interaction, e.g., fluorescent emission from elements with very low concentrations. In the field of X-ray fluorescence spectroscopy, this problem has been solved by combining the Monte Carlo method with variance reduction techniques, which can reduce the computation time by several orders of magnitude. In this work, we present a C++ code for the general simulation of X-ray imaging and spectroscopy experiments, based on the application of the Monte Carlo method in combination with variance reduction techniques, with a description of sample geometry based on quadric surfaces. We describe the benefits of the object-oriented approach in terms of code maintenance, the flexibility of the program for the simulation of different experimental conditions and the possibility of easily adding new modules. Sample applications in the fields of X-ray imaging and X-ray spectroscopy are discussed. Catalogue identifier: AERO_v1_0 Program summary URL:http://cpc.cs.qub.ac.uk/summaries/AERO_v1_0.html Program obtainable from: CPC Program Library, Queen’s University, Belfast, N. Ireland

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

    NASA Technical Reports Server (NTRS)

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

    2009-01-01

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

  6. Summary: Update to ASTM guide E 1523 to charge control and charge referencing techniques in x-ray photoelectron spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Baer, D.R.

    2005-05-01

    An updated version of the American Society for Testing and Materials (ASTM) guide E 1523 to the methods to charge control and charge referencing techniques in x-ray photoelectron spectroscopy has been released by ASTM [Annual Book of ASTM Standards Surface Analysis (American Society for Testing and Materials, West Conshohocken, PA, 2004), Vol. 03.06]. The guide is meant to acquaint x-ray photoelectron spectroscopy (XPS) users with the various charge control and charge referencing techniques that are and have been used in the acquisition and interpretation of XPS data from surfaces of insulating specimens. The current guide has been expanded to includemore » new references as well as recommendations for reporting information on charge control and charge referencing. The previous version of the document had been published in 1997 [D. R. Baer and K. D. Bomben, J. Vac. Sci. Technol. A 16, 754 (1998)].« less

  7. Insights into electron and ion acceleration and transport from x-ray and gamma-ray imaging spectroscopy

    NASA Astrophysics Data System (ADS)

    Hurford, Gordon J.; Krucker, Samuel

    The previous solar maximum has featured high resolution imaging/spectroscopy observations at hard x-ray and gamma-ray energies by the Reuven Ramaty High Energy Solar/Spectroscopic Imager (RHESSI). Highlights of these observations will be reviewed, along with their impli-cations for our understanding of ion and electron acceleration and transport processes. The results to date have included new insights into the location of the acceleration region and the thick target model, a new appreciation of the significance of x-ray albedo, observation of coronal gamma-ray sources and their implications for electron trapping, and indications of differences in the acceleration and transport between electrons and ions. The role of RHESSI's observational strengths and weaknesses in determining the character of its scientific results will also be discussed and used to identify what aspects of the acceleration and transport processes must await the next generation of instrumentation. The extent to which new instrumentation now under development, such as Solar Orbiter/STIX, GRIPS, and FOXSI, can address these open issues will be outlined.

  8. NuSTAR HARD X-RAY SURVEY OF THE GALACTIC CENTER REGION. I. HARD X-RAY MORPHOLOGY AND SPECTROSCOPY OF THE DIFFUSE EMISSION

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Mori, Kaya; Hailey, Charles J.; Perez, Kerstin

    2015-12-01

    We present the first sub-arcminute images of the Galactic Center above 10 keV, obtained with NuSTAR. NuSTAR resolves the hard X-ray source IGR J17456–2901 into non-thermal X-ray filaments, molecular clouds, point sources, and a previously unknown central component of hard X-ray emission (CHXE). NuSTAR detects four non-thermal X-ray filaments, extending the detection of their power-law spectra with Γ ∼ 1.3–2.3 up to ∼50 keV. A morphological and spectral study of the filaments suggests that their origin may be heterogeneous, where previous studies suggested a common origin in young pulsar wind nebulae (PWNe). NuSTAR detects non-thermal X-ray continuum emission spatially correlated with the 6.4more » keV Fe Kα fluorescence line emission associated with two Sgr A molecular clouds: MC1 and the Bridge. Broadband X-ray spectral analysis with a Monte-Carlo based X-ray reflection model self-consistently determined their intrinsic column density (∼10{sup 23} cm{sup −2}), primary X-ray spectra (power-laws with Γ ∼ 2) and set a lower limit of the X-ray luminosity of Sgr A* flare illuminating the Sgr A clouds to L{sub X} ≳ 10{sup 38} erg s{sup −1}. Above ∼20 keV, hard X-ray emission in the central 10 pc region around Sgr A* consists of the candidate PWN G359.95–0.04 and the CHXE, possibly resulting from an unresolved population of massive CVs with white dwarf masses M{sub WD} ∼ 0.9 M{sub ⊙}. Spectral energy distribution analysis suggests that G359.95–0.04 is likely the hard X-ray counterpart of the ultra-high gamma-ray source HESS J1745–290, strongly favoring a leptonic origin of the GC TeV emission.« less

  9. Metalloprotein structures at ambient conditions and in real-time: biological crystallography and spectroscopy using X-ray free electron lasers

    DOE PAGES

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

    2015-09-02

    We have studied the structure of enzymes and the chemistry at the catalytic sites, intensively and have acquired an understanding of the atomic-scale chemistry which requires a new approach beyond steady state X-ray crystallography and X-ray spectroscopy at cryogenic temperatures. Following the dynamic changes in the geometric and electronic structure of metallo-enzymes at ambient conditions, while overcoming the severe X-ray-induced changes to the redox active catalytic center, is key for deriving reaction mechanisms. Such studies become possible by the intense and ultra-short femtosecond (fs) X-ray pulses from an X-ray free electron laser (XFEL) by acquiring a signal before the samplemore » is destroyed. Our review describes the recent and pioneering uses of XFELs to study the protein structure and dynamics of metallo-enzymes using crystallography and scattering, as well as the chemical structure and dynamics of the catalytic complexes (charge, spin, and covalency) using spectroscopy during the reaction to understand the electron-transfer processes and elucidate the mechanism.« less

  10. Metalloprotein structures at ambient conditions and in real-time: biological crystallography and spectroscopy using X-ray free electron lasers

    DOE Office of Scientific and Technical Information (OSTI.GOV)

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

    We have studied the structure of enzymes and the chemistry at the catalytic sites, intensively and have acquired an understanding of the atomic-scale chemistry which requires a new approach beyond steady state X-ray crystallography and X-ray spectroscopy at cryogenic temperatures. Following the dynamic changes in the geometric and electronic structure of metallo-enzymes at ambient conditions, while overcoming the severe X-ray-induced changes to the redox active catalytic center, is key for deriving reaction mechanisms. Such studies become possible by the intense and ultra-short femtosecond (fs) X-ray pulses from an X-ray free electron laser (XFEL) by acquiring a signal before the samplemore » is destroyed. Our review describes the recent and pioneering uses of XFELs to study the protein structure and dynamics of metallo-enzymes using crystallography and scattering, as well as the chemical structure and dynamics of the catalytic complexes (charge, spin, and covalency) using spectroscopy during the reaction to understand the electron-transfer processes and elucidate the mechanism.« less

  11. X ray spectra of X Per. [oso-8 observations

    NASA Technical Reports Server (NTRS)

    Becker, R. H.; Boldt, E. A.; Holt, S. S.; Pravdo, S. H.; Robinson-Saba, J.; Serlemitsos, P. J.; Swank, J. H.

    1978-01-01

    The cosmic X-ray spectroscopy experiment on OSO-8 observed X Per for twenty days during two observations in Feb. 1976 and Feb. 1977. The spectrum of X Per varies in phase with its 13.9 min period, hardening significantly at X-ray minimum. Unlike other X-ray binary pulsar spectra, X Per's spectra do not exhibit iron line emission or strong absorption features. The data show no evidence for a 22 hour periodicity in the X-ray intensity of X Per. These results indicate that the X-ray emission from X Per may be originating from a neutron star in a low density region far from the optically identified Be star.

  12. Atomic Data Needs for X-Ray Astronomy

    NASA Technical Reports Server (NTRS)

    Kallman, Timothy; White, Nicholas E. (Technical Monitor)

    1999-01-01

    This publication contains written versions of most of the invited talks presented at the workshop on Atomic Data Needs for X-ray Astronomy which was held at NASA's Goddard Space Flight Center on December 16-1 7 1999. The idea of hosting such a workshop emerged from an imminent need to update and complete current atomic datasets in anticipation of a new era of high quality X-ray spectra starting with the launching of Chandra and XMM-Newton observatories. At first, our vision of the workshop was of a short and limited attendance event, given the specialization of the topic. But it, was soon realized, from the response to the first workshop announcement, that the topic was of much interest, to researchers working in X-ray spectra (physicists and astronomers). As a result, the workshop grew to approximately 120 participants from several countries. The kind of atomic data that interests us are those parameters needed for analysis and modeling of spectra shortward of about about 100 A and relevant to ionic species of astronomical interest. The physical mechanisms of interest in the formation of spectra include photoionization. collisional ionization, recombination (radiative and dielectronic). collisional excitation (by electrons and protons). and radiative deexcitation. Unique to X-ray spectroscopy are the ionization and excitation processes from inner-closed shells. in addition to the challenges in interpret,ing the medium resolution (epsilon/delta epsilon is about 0.05 - 0.1) data obtained by current X-ray astronomy experiments. Line wavelengths are of interest too, particularly owing to the high resolution spectra from the new experiments. The workshop was divided into five major areas: Observational Spectroscopy, Theoretical Calculations of Atomic Data, Laboratory Measurements of Atomic Parameters. Spectra Modeling, and Atomic Databases. One comforting finding from the work shop is that the enthusiasm felt by X-ray astronomers about the new observational missions

  13. Single and double core-hole ion emission spectroscopy of transient neon plasmas produced by ultraintense x-ray laser pulses

    NASA Astrophysics Data System (ADS)

    Gao, Cheng; Zeng, Jiaolong; Yuan, Jianmin

    2016-05-01

    Single core-hole (SCH) and double core-hole (DCH) spectroscopy is investigated systematically for neon gas in the interaction with ultraintense x-ray pulses with photon energy from 937 eV to 2000 eV. A time-dependent rate equation, implemented in the detailed level accounting approximation, is utilized to study the dynamical evolution of the level population and emission properties of the laser-produced highly transient plasmas. The plasma density effects on level populations are demonstrated with an x-ray photon energy of 2000 eV. For laser photon energy in the range of 937 - 1360 eV, resonant absorptions (RA) of 1s-np (n> = 2) transitions play important roles in time evolution of the population and DCH emission spectroscopy. For x-ray photon energy larger than 1360 eV, no RA exist and transient plasmas show different features in the DCH spectroscopy.

  14. REDSoX: Monte-Carlo ray-tracing for a soft x-ray spectroscopy polarimeter

    NASA Astrophysics Data System (ADS)

    Günther, Hans M.; Egan, Mark; Heilmann, Ralf K.; Heine, Sarah N. T.; Hellickson, Tim; Frost, Jason; Marshall, Herman L.; Schulz, Norbert S.; Theriault-Shay, Adam

    2017-08-01

    X-ray polarimetry offers a new window into the high-energy universe, yet there has been no instrument so far that could measure the polarization of soft X-rays (about 17-80 Å) from astrophysical sources. The Rocket Experiment Demonstration of a Soft X-ray Polarimeter (REDSoX Polarimeter) is a proposed sounding rocket experiment that uses a focusing optic and splits the beam into three channels. Each channel has a set of criticalangle transmission (CAT) gratings that disperse the x-rays onto a laterally graded multilayer (LGML) mirror, which preferentially reflects photons with a specific polarization angle. The three channels are oriented at 120 deg to each other and thus measure the three Stokes parameters: I, Q, and U. The period of the LGML changes with position. The main design challenge is to arrange the gratings so that they disperse the spectrum in such a way that all rays are dispersed onto the position on the multi-layer mirror where they satisfy the local Bragg condition despite arriving on the mirror at different angles due to the converging beam from the focusing optics. We present a polarimeteric Monte-Carlo ray-trace of this design to assess non-ideal effects from e.g. mirror scattering or the finite size of the grating facets. With mirror properties both simulated and measured in the lab for LGML mirrors of 80-200 layers we show that the reflectivity and the width of the Bragg-peak are sufficient to make this design work when non-ideal effects are included in the simulation. Our simulations give us an effective area curve, the modulation factor and the figure of merit for the REDSoX polarimeter. As an example, we simulate an observation of Mk 421 and show that we could easily detect a 20% linear polarization.

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

    NASA Astrophysics Data System (ADS)

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

    2012-01-01

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

  16. Gamma ray spectroscopy in astrophysics. [conferences

    NASA Technical Reports Server (NTRS)

    Cline, T. L. (Editor); Ramaty, R. (Editor)

    1978-01-01

    Experimental and theoretical aspects of gamma ray spectroscopy in high energy astrophysics are discussed. Line spectra from solar, stellar, planetary, and cosmic gamma rays are examined as well as HEAO investigations, the prospects of a gamma ray observatory, and follow-on X-ray experiments in space.

  17. Investigation of the nanoscale two-component ZnS-ZnO heterostructures by means of HR-TEM and X-ray based analysis

    NASA Astrophysics Data System (ADS)

    Pankin, I. A.; Polozhentsev, O. E.; Soldatov, M. A.; Bugaev, A. L.; Tsaturyan, A.; Lomachenko, K. A.; Guda, A. A.; Budnyk, A. P.; Lamberti, C.; Soldatov, A. V.

    2018-06-01

    This article is devoted to the spectroscopic characterization of ZnS-ZnO nanoscale heterostructures synthesized by the microwave-assisted solvothermal method. The synthesized samples were investigated by means of X-ray powder diffraction (XRPD), high energy resolution fluorescence detected X-ray absorption near-edge-structure (HERFD-XANES) spectroscopy, valence-to-core X-ray emission spectroscopy (VtC-XES) and high resolution transmission electron microscopy (HR-TEM) as well as energy dispersive X-ray spectroscopy (EDX). The average crystallite size estimated by the broadening of XRPD peaks increases from 2.7 nm to 3.7 nm in the temperature range from 100 °C to 150 °C. HR-TEM images show that nanoparticles are arranged in aggregates with the 60-200 nm size. Theoretical estimation shows that the systems synthesized at higher temperatures more prone to the agglomeration. The full profile Reitveld analysis of XRPD data reveals the formation of hexagonal zinc sulfide structure, whereas electron diffraction data reveal also the formation of cubic zinc sulfide and claim the polymorphous character of the system. High energy resolution Zn K-edge XANES data unambiguously demonstrate the presence of a certain amount of the zinc oxide which is likely to have an amorphous structure and could not be detected by XRPD. Qualitative analysis of XANES data allows deriving ZnS/ZnO ratio as a function of synthesis temperature. EDX analysis depicts homogeneous distribution of ZnS and amorphous ZnO phases across the conglomerates. A complementary element-selective valence to core X-ray emission spectroscopy evidences formation of two-component system and confirms estimations of ZnS/ZnO fractions obtained by linear combination fit of XANES data.

  18. Analysis of RNA structure using small-angle X-ray scattering

    PubMed Central

    Cantara, William A.; Olson, Erik D.; Musier-Forsyth, Karin

    2016-01-01

    In addition to their role in correctly attaching specific amino acids to cognate tRNAs, aminoacyl-tRNA synthetases (aaRS) have been found to possess many alternative functions and often bind to and act on other nucleic acids. In contrast to the well-defined 3D structure of tRNA, the structures of many of the other RNAs recognized by aaRSs have not been solved. Despite advances in the use of X-ray crystallography (XRC), nuclear magnetic resonance (NMR) spectroscopy and cryo-electron microscopy (cryo-EM) for structural characterization of biomolecules, significant challenges to solving RNA structures still exist. Recently, small-angle X-ray scattering (SAXS) has been increasingly employed to characterize the 3D structures of RNAs and RNA-protein complexes. SAXS is capable of providing low-resolution tertiary structure information under physiological conditions and with less intensive sample preparation and data analysis requirements than XRC, NMR and cryo-EM. In this article, we describe best practices involved in the process of RNA and RNA-protein sample preparation, SAXS data collection, data analysis, and structural model building. PMID:27777026

  19. High-Resolution Spectroscopy with the Chandra X-ray Observatory

    ScienceCinema

    Canizares, Claude R. [MIT, Cambridge, Massachusetts, United States

    2017-12-09

    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.

  20. X-ray spectroscopy of the mixed morphology supernova remnant W 28 with XMM-Newton

    NASA Astrophysics Data System (ADS)

    Nakamura, Ryoko; Bamba, Aya; Ishida, Manabu; Yamazaki, Ryo; Tatematsu, Ken'ichi; Kohri, Kazunori; Pühlhofer, Gerd; Wagner, Stefan J.; Sawada, Makoto

    2014-06-01

    We report on spatially resolved X-ray spectroscopy of the north-eastern part of the mixed morphology supernova remnant (SNR) W 28 with XMM-Newton. The observed field of view includes a prominent and twisted shell emission forming the edge of this SNR as well as part of the center-filled X-ray emission brightening toward the south-west edge of the field of view. The shell region spectra are in general represented by an optically thin thermal plasma emission in collisional ionization equilibrium with a temperature of ˜ 0.3 keV and a density of ˜ 10 cm-3, which is much higher than the density obtained for inner parts. In contrast, we detected no significant X-ray flux from one of the TeV γ-ray peaks with an upper-limit flux of 2.1 × 10-14 erg cm-2 s-1 in the 2-10 keV band. The large flux ratio of TeV to X-ray, larger than 16, and the spatial coincidence of the molecular cloud and the TeV γ-ray emission site indicate that the TeV γ-ray of W 28 is π0-decay emission originating from collisions between accelerated protons and molecular cloud protons. Comparing the spectrum in the TeV band and the X-ray upper limit, we obtained a weak upper limit on the magnetic field strength B ≲ 1500 μG.

  1. Visible micro-Raman spectroscopy of single human mammary epithelial cells exposed to x-ray radiation.

    PubMed

    Delfino, Ines; Perna, Giuseppe; Lasalvia, Maria; Capozzi, Vito; Manti, Lorenzo; Camerlingo, Carlo; Lepore, Maria

    2015-03-01

    A micro-Raman spectroscopy investigation has been performed in vitro on single human mammary epithelial cells after irradiation by graded x-ray doses. The analysis by principal component analysis (PCA) and interval-PCA (i-PCA) methods has allowed us to point out the small differences in the Raman spectra induced by irradiation. This experimental approach has enabled us to delineate radiation-induced changes in protein, nucleic acid, lipid, and carbohydrate content. In particular, the dose dependence of PCA and i-PCA components has been analyzed. Our results have confirmed that micro-Raman spectroscopy coupled to properly chosen data analysis methods is a very sensitive technique to detect early molecular changes at the single-cell level following exposure to ionizing radiation. This would help in developing innovative approaches to monitor radiation cancer radiotherapy outcome so as to reduce the overall radiation dose and minimize damage to the surrounding healthy cells, both aspects being of great importance in the field of radiation therapy.

  2. X-Ray Spectroscopy of the Nearby, Classical T Tauri Star TW Hydrae

    NASA Astrophysics Data System (ADS)

    Kastner, Joel H.; Huenemoerder, David P.; Schulz, Norbert S.; Weintraub, David A.

    1999-11-01

    We present ASCA and ROSAT X-ray observations of the classical T Tauri star TW Hya, the namesake of a small association that, at a distance of ~50 pc, represents the nearest known region of recent star formation. Analysis of ASCA and ROSAT spectra indicates characteristic temperatures of ~1.7 and ~9.7 MK for the X-ray-emitting region(s) of TW Hya, with emission lines of highly ionized Fe dominating the spectrum at energies of ~1 keV. The X-ray data show variations in X-ray flux on timescales of <~1 hr as well as indications of changes in the X-ray-absorbing column on timescales of several years, suggesting that flares and variable obscuration are responsible for the large-amplitude optical variability of TW Hya on short and long timescales, respectively. Comparison with model calculations suggests that TW Hya produces sufficient hard X-ray flux to produce significant ionization of molecular gas within its circumstellar disk; such X-ray ionization may regulate both protoplanetary accretion and protoplanetary chemistry.

  3. 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

  4. Revealing the electronic structure of LiC 6 by soft X-ray spectroscopy

    DOE PAGES

    Zhang, L.; Li, X.; Augustsson, A.; ...

    2017-03-09

    The electronic structure of LiC 6 has been investigated in this paper by soft X-ray absorption and emission spectroscopies. The results reveal that upon full lithiation of graphite, the Li 2s electrons are transferred into the carbon π* states in a near rigid-band behavior, resulting in the increased density of states near E F and the shift of σ* states to lower energies. Finally, in addition, the resonant inelastic X-ray scattering spectra of LiC 6 do not show strong dispersive features as that of graphite, indicating that the crystal momentum is not conserved during the scattering process due to themore » delocalization of electrons in the intermediate state.« less

  5. Optics for coherent X-ray applications

    PubMed Central

    Yabashi, Makina; Tono, Kensuke; Mimura, Hidekazu; Matsuyama, Satoshi; Yamauchi, Kazuto; Tanaka, Takashi; Tanaka, Hitoshi; Tamasaku, Kenji; Ohashi, Haruhiko; Goto, Shunji; Ishikawa, Tetsuya

    2014-01-01

    Developments of X-ray optics for full utilization of diffraction-limited storage rings (DLSRs) are presented. The expected performance of DLSRs is introduced using the design parameters of SPring-8 II. To develop optical elements applicable to manipulation of coherent X-rays, advanced technologies on precise processing and metrology were invented. With propagation-based coherent X-rays at the 1 km beamline of SPring-8, a beryllium window fabricated with the physical-vapour-deposition method was found to have ideal speckle-free properties. The elastic emission machining method was utilized for developing reflective mirrors without distortion of the wavefronts. The method was further applied to production of diffraction-limited focusing mirrors generating the smallest spot size in the sub-10 nm regime. To enable production of ultra-intense nanobeams at DLSRs, a low-vibration cooling system for a high-heat-load monochromator and advanced diagnostic systems to characterize X-ray beam properties precisely were developed. Finally, new experimental schemes for combinative nano-analysis and spectroscopy realised with novel X-ray optics are discussed. PMID:25177986

  6. Optics for coherent X-ray applications.

    PubMed

    Yabashi, Makina; Tono, Kensuke; Mimura, Hidekazu; Matsuyama, Satoshi; Yamauchi, Kazuto; Tanaka, Takashi; Tanaka, Hitoshi; Tamasaku, Kenji; Ohashi, Haruhiko; Goto, Shunji; Ishikawa, Tetsuya

    2014-09-01

    Developments of X-ray optics for full utilization of diffraction-limited storage rings (DLSRs) are presented. The expected performance of DLSRs is introduced using the design parameters of SPring-8 II. To develop optical elements applicable to manipulation of coherent X-rays, advanced technologies on precise processing and metrology were invented. With propagation-based coherent X-rays at the 1 km beamline of SPring-8, a beryllium window fabricated with the physical-vapour-deposition method was found to have ideal speckle-free properties. The elastic emission machining method was utilized for developing reflective mirrors without distortion of the wavefronts. The method was further applied to production of diffraction-limited focusing mirrors generating the smallest spot size in the sub-10 nm regime. To enable production of ultra-intense nanobeams at DLSRs, a low-vibration cooling system for a high-heat-load monochromator and advanced diagnostic systems to characterize X-ray beam properties precisely were developed. Finally, new experimental schemes for combinative nano-analysis and spectroscopy realised with novel X-ray optics are discussed.

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

    NASA Technical Reports Server (NTRS)

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

    2011-01-01

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

  8. Determination of copper binding in Pseudomonas putida CZ1 by chemical modifications and X-ray absorption spectroscopy.

    PubMed

    Chen, XinCai; Shi, JiYan; Chen, YingXu; Xu, XiangHua; Chen, LiTao; Wang, Hui; Hu, TianDou

    2007-03-01

    Previously performed studies have shown that Pseudomonas putida CZ1 biomass can bind an appreciable amount of Cu(II) and Zn(II) ions from aqueous solutions. The mechanisms of Cu- and Zn-binding by P. putida CZ1 were ascertained by chemical modifications of the biomass followed by Fourier transform infrared and X-ray absorption spectroscopic analyses of the living or nonliving cells. A dramatic decrease in Cu(II)- and Zn(II)-binding resulted after acidic methanol esterification of the nonliving cells, indicating that carboxyl functional groups play an important role in the binding of metal to the biomaterial. X-ray absorption spectroscopy was used to determine the speciation of Cu ions bound by living and nonliving cells, as well as to elucidate which functional groups were involved in binding of the Cu ions. The X-ray absorption near-edge structure spectra analysis showed that the majority of the Cu was bound in both samples as Cu(II). The fitting results of Cu K-edge extended X-ray absorption fine structure spectra showed that N/O ligands dominated in living and nonliving cells. Therefore, by combining different techniques, our results indicate that carboxyl functional groups are the major ligands responsible for the metal binding in P. putida CZ1.

  9. The use of C-near edge X-ray absorption fine structure spectroscopy for the elaboration of chemistry in lignocellulosics

    Treesearch

    Lucian A. Lucia; Hiroki Nanko; Alan W. Rudie; Doug G. Mancosky; Sue Wirick

    2006-01-01

    The research presented elucidates the oxidation chemistry occurring in hydrogen peroxide bleached kraft pulp fibers by employing carbon near edge x-ray absorption fine structure spectroscopy (C-NEXAFS). C-NEXAFS is a soft x-ray technique that selectively interrogates atomic moieties using photoelectrons (Xrays) of variable energies. The X1A beam line at the National...

  10. Novel visualization studies of lignocellulosic oxidation chemistry by application of C-near edge X-ray absorption fine structure spectroscopy

    Treesearch

    Douglas G. Mancosky; Lucian A. Lucia; Hiroki Nanko; Sue Wirick; Alan W. Rudie; Robert Braun

    2005-01-01

    The research presented herein is the first attempt to probe the chemical nature of lignocellulosic samples by the application of carbon near edge X-ray absorption fine structure spectroscopy (C-NEXAFS). C-NEXAFS is a soft X-ray technique that principally provides selective interrogation of discrete atomic moieties using photoelectrons of variable energies. The X1A beam...

  11. Femtosecond time-resolved X-ray absorption spectroscopy of anatase TiO2 nanoparticles using XFEL

    PubMed Central

    Obara, Yuki; Ito, Hironori; Ito, Terumasa; Kurahashi, Naoya; Thürmer, Stephan; Tanaka, Hiroki; Katayama, Tetsuo; Togashi, Tadashi; Owada, Shigeki; Yamamoto, Yo-ichi; Karashima, Shutaro; Nishitani, Junichi; Yabashi, Makina; Suzuki, Toshinori; Misawa, Kazuhiko

    2017-01-01

    The charge-carrier dynamics of anatase TiO2 nanoparticles in an aqueous solution were studied by femtosecond time-resolved X-ray absorption spectroscopy using an X-ray free electron laser in combination with a synchronized ultraviolet femtosecond laser (268 nm). Using an arrival time monitor for the X-ray pulses, we obtained a temporal resolution of 170 fs. The transient X-ray absorption spectra revealed an ultrafast Ti K-edge shift and a subsequent growth of a pre-edge structure. The edge shift occurred in ca. 100 fs and is ascribed to reduction of Ti by localization of generated conduction band electrons into shallow traps of self-trapped polarons or deep traps at penta-coordinate Ti sites. Growth of the pre-edge feature and reduction of the above-edge peak intensity occur with similar time constants of 300–400 fs, which we assign to the structural distortion dynamics near the surface. PMID:28713842

  12. Probing Chemical Bonding in Uranium Dioxide by Means of High-Resolution X-ray Absorption Spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Butorin, Sergei M.; Modin, Anders; Vegelius, Johan R.

    Here, a systematic X-ray absorption study at the U 3d, 4d, and 4f edges of UO 2 was performed, and the data were analyzed within framework of the Anderson impurity model. By applying the high-energy-resolution fluorescence-detection (HERFD) mode of X-ray absorption spectroscopy (XAS) at the U 3d 3/2 edge and conducting the XAS measurements at the shallower U 4f levels, fine details of the XAS spectra were resolved resulting from reduced core-hole lifetime broadening. This multiedge study enabled a far more effective analysis of the electronic structure at the U sites and characterization of the chemical bonding and degree ofmore » the 5f localization in UO 2. The results support the covalent character of UO 2 and do not agree with the suggestions of rather ionic bonding in this compound as expressed in some publications.« less

  13. Probing Chemical Bonding in Uranium Dioxide by Means of High-Resolution X-ray Absorption Spectroscopy

    DOE PAGES

    Butorin, Sergei M.; Modin, Anders; Vegelius, Johan R.; ...

    2016-11-30

    Here, a systematic X-ray absorption study at the U 3d, 4d, and 4f edges of UO 2 was performed, and the data were analyzed within framework of the Anderson impurity model. By applying the high-energy-resolution fluorescence-detection (HERFD) mode of X-ray absorption spectroscopy (XAS) at the U 3d 3/2 edge and conducting the XAS measurements at the shallower U 4f levels, fine details of the XAS spectra were resolved resulting from reduced core-hole lifetime broadening. This multiedge study enabled a far more effective analysis of the electronic structure at the U sites and characterization of the chemical bonding and degree ofmore » the 5f localization in UO 2. The results support the covalent character of UO 2 and do not agree with the suggestions of rather ionic bonding in this compound as expressed in some publications.« less

  14. Anionic and cationic redox and interfaces in batteries: Advances from soft X-ray absorption spectroscopy to resonant inelastic scattering

    NASA Astrophysics Data System (ADS)

    Yang, Wanli; Devereaux, Thomas P.

    2018-06-01

    Recent advances in battery science and technology have triggered both the challenges and opportunities on studying the materials and interfaces in batteries. Here, we review the recent demonstrations of soft X-ray spectroscopy for studying the interfaces and electrode materials. The focus of this review is on the recently developed mapping of resonant inelastic X-ray scattering (mRIXS) as a powerful probe of battery chemistry with superior sensitivity. Six different channels of soft X-ray absorption spectroscopy (sXAS) are introduced for different experimental purposes. Although conventional sXAS channels remain effective tools for quantitative analysis of the transition-metal states and surface chemistry, we elaborate the limitations of sXAS in both cationic and anionic redox studies. Particularly, based on experimental findings in various electrodes, we show that sXAS is unreliable for studying oxygen redox. We then demonstrate the mRIXS as a reliable technique for fingerprinting oxygen redox and summarize several crucial observations. We conclude that mRIXS is the tool-of-choice to study both the practical issue on reversibility of oxygen redox and the fundamental nature of bulk oxygen states. We hope this review clarifies the popular misunderstanding on oxygen sXAS results of oxide electrodes, and establishes a reliable technique for detecting oxygen redox through mRIXS.

  15. High resolution x-ray absorption and emission spectroscopy of Li x CoO2 single crystals as a function delithiation

    NASA Astrophysics Data System (ADS)

    Simonelli, L.; Paris, E.; Iwai, C.; Miyoshi, K.; Takeuchi, J.; Mizokawa, T.; Saini, N. L.

    2017-03-01

    The effect of delithiation in Li x CoO2 is studied by high resolution Co K-edge x-ray absorption and x-ray emission spectroscopy. Polarization dependence of the x-ray absorption spectra on single crystal samples is exploited to reveal information on the anisotropic electronic structure. We find that the electronic structure of Li x CoO2 is significantly affected by delithiation in which the Co ions oxidation state tending to change from 3+  to 4+. The Co intersite (intrasite) 4p-3d hybridization suffers a decrease (increase) by delithiation. The unoccupied 3d t 2g orbitals with a 1g symmetry, containing substantial O 2p character, hybridize isotropically with Co 4p orbitals and likely to have itinerant character unlike anisotropically hybridized 3d e g orbitals. Such a peculiar electronic structure could have significant effect on the mobility of Li in Li x CoO2 cathode and hence the battery characteristics.

  16. Application toward Confocal Full-Field Microscopic X-ray Absorption Near Edge Structure Spectroscopy.

    PubMed

    Tack, Pieter; Vekemans, Bart; Laforce, Brecht; Rudloff-Grund, Jennifer; Hernández, Willinton Y; Garrevoet, Jan; Falkenberg, Gerald; Brenker, Frank; Van Der Voort, Pascal; Vincze, Laszlo

    2017-02-07

    Using X-ray absorption near edge structure (XANES) spectroscopy, information on the local chemical structure and oxidation state of an element of interest can be acquired. Conventionally, this information can be obtained in a spatially resolved manner by scanning a sample through a focused X-ray beam. Recently, full-field methods have been developed to obtain direct 2D chemical state information by imaging a large sample area. These methods are usually in transmission mode, thus restricting the use to thin and transmitting samples. Here, a fluorescence method is displayed using an energy-dispersive pnCCD detector, the SLcam, characterized by measurement times far superior to what is generally applicable. Additionally, this method operates in confocal mode, thus providing direct 3D spatially resolved chemical state information from a selected subvolume of a sample, without the need of rotating a sample. The method is applied to two samples: a gold-supported magnesia catalyst (Au/MgO) and a natural diamond containing Fe-rich inclusions. Both samples provide XANES spectra that can be overlapped with reference XANES spectra, allowing this method to be used for fingerprinting and linear combination analysis of known XANES reference compounds.

  17. X-ray photoelectron spectroscopy of select multi-layered transition metal carbides (MXenes)

    DOE PAGES

    Halim, Joseph; Cook, Kevin M.; Naguib, Michael; ...

    2015-12-01

    A detailed high resolution X-ray photoelectron spectroscopy (XPS) analysis is presented in this work for select MXenes—a recently discovered family of two-dimensional (2D) carbides and carbonitrides. Given their 2D nature, understanding their surface chemistry is paramount. Thus we identify and quantify the surface groups present before, and after, sputter-cleaning as well as freshly prepared vs. aged multi-layered cold pressed discs. The nominal compositions of the MXenes studied here are Ti 3C 2T x, Ti 2CT x, Ti 3CNTx, Nb 2CT x and Nb 4C 3T x, where T represents surface groups that this work attempts to quantify. In all themore » cases, the presence of three surface terminations, single bondO, single bondOH and single bondF, in addition to OH-terminations relatively strongly bonded to H 2O molecules, was confirmed. Moreover, from XPS peak fits, it was possible to establish the average sum of the negative charges of the terminations for the aforementioned MXenes. Based on this work, it is now possible to quantify the nature of the surface terminations. This information can, in turn, be used to better design and tailor these novel 2D materials for various applications.« less

  18. X-ray diffraction, IR spectroscopy and thermal characterization of partially hydrolyzed guar gum.

    PubMed

    Mudgil, Deepak; Barak, Sheweta; Khatkar, B S

    2012-05-01

    Guar gum was hydrolyzed using cellulase from Aspergillus niger at 5.6 pH and 50°C temperature. Hydrolyzed guar gum sample was characterized using Fourier transform infrared spectroscopy, differential scanning calorimetry, thermogravimetric analysis, X-ray diffraction, dilute solution viscometry and rotational viscometry. Viscometry analysis of native guar gum showed a molecular weight of 889742.06, whereas, after enzymatic hydrolysis, the resultant product had a molecular weight of 7936.5. IR spectral analysis suggests that after enzymatic hydrolysis of guar gum there was no major transformation of functional group. Thermal analysis revealed no major change in thermal behavior of hydrolyzed guar gum. It was shown that partial hydrolysis of guar gum could be achieved by inexpensive and food grade cellulase (Aspergillus niger) having commercial importance and utilization as a functional soluble dietary fiber for food industry. Copyright © 2012 Elsevier B.V. All rights reserved.

  19. Spectra of cosmic X-ray sources

    NASA Technical Reports Server (NTRS)

    Holt, S. S.; Mccray, R.

    1982-01-01

    X-ray measurements provide the most direct probes of astrophysical environments with temperatures exceeding one million K. Progress in experimental research utilizing dispersive techniques (e.g., Bragg and grating spectroscopy) is considerably slower than that in areas utilizing photometric techniques, because of the relative inefficiency of the former for the weak X-ray signals from celestial sources. As a result, the term "spectroscopy" as applied to X-ray astronomy has traditionally satisfied a much less restrictive definition (in terms of resolving power) than it has in other wavebands. Until quite recently, resolving powers of order unity were perfectly respectable, and still provide (in most cases) the most useful spectroscopic data. In the broadest sense, X-ray photometric measurements are spectroscopic, insofar as they represent samples of the overall electromagnetic continua of celestial objects.

  20. 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

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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Kroner, Anna B., E-mail: anna.kroner@diamond.ac.uk; Gilbert, Martin; Duller, Graham

    2016-07-27

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

  2. Combining X-ray and neutron crystallography with spectroscopy.

    PubMed

    Kwon, Hanna; Smith, Oliver; Raven, Emma Lloyd; Moody, Peter C E

    2017-02-01

    X-ray protein crystallography has, through the determination of the three-dimensional structures of enzymes and their complexes, been essential to the understanding of biological chemistry. However, as X-rays are scattered by electrons, the technique has difficulty locating the presence and position of H atoms (and cannot locate H + ions), knowledge of which is often crucially important for the understanding of enzyme mechanism. Furthermore, X-ray irradiation, through photoelectronic effects, will perturb the redox state in the crystal. By using single-crystal spectrophotometry, reactions taking place in the crystal can be monitored, either to trap intermediates or follow photoreduction during X-ray data collection. By using neutron crystallography, the positions of H atoms can be located, as it is the nuclei rather than the electrons that scatter neutrons, and the scattering length is not determined by the atomic number. Combining the two techniques allows much greater insight into both reaction mechanism and X-ray-induced photoreduction.

  3. Investigation of the Structural Stability of Ion-Implanted Gd 2Ti 2-xSn xO 7 Pyrochlore-Type Oxides by Glancing Angle X-ray Absorption Spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Aluri, Esther Rani; Hayes, John R.; Walker, James D.S.

    2016-03-24

    Rare-earth titanate and stannate pyrochlore-type oxides have been investigated in the past for the sequestration of nuclear waste elements because of their resistance to radiation-induced structural damage. In order to enhance this property, it is necessary to understand the effect of radioactive decay of the incorporated actinide elements on the local chemical environment. In this study, Gd 2Ti 2–xSn xO 7 materials have been implanted with Au– ions to simulate radiation-induced structural damage. Glancing angle X-ray absorption near-edge spectroscopy (GA-XANES), glancing angle X-ray absorption fine structure (GA-EXAFS) analysis, and powder X-ray diffraction have been used to investigate changes in themore » local coordination environment of the metal atoms in the damaged surface layer. Examination of GA-XANES/EXAFS spectra from the implanted Gd 2Ti 2–xSn xO 7 materials collected at various glancing angles allowed for an investigation of how the local coordination environment around the absorbing atoms changed at different depths in the damaged surface layer. This study has shown the usefulness of GA-XANES to the examination of ion-implanted materials and has suggested that Gd 2Ti 2–xSn xO 7 becomes more susceptible to ion-beam-induced structural damage with increasing Sn concentration.« less

  4. Cosmic X-ray physics

    NASA Technical Reports Server (NTRS)

    Mccammon, D.; Cox, D. P.; Kraushaar, W. L.; Sanders, W. T.

    1985-01-01

    A progress report of research activities carried out in the area of cosmic X-ray physics is presented. The Diffuse X-ray Spectrometer DXS which has been flown twice as a rocket payload is described. The observation times proved to be too small for meaningful X-ray data to be obtained. Data collection and reduction activities from the Ultra-Soft X-ray background (UXT) instrument are described. UXT consists of three mechanically-collimated X-ray gas proportional counters with window/filter combinations which allow measurements in three energy bands, Be (80-110 eV), B (90-187 eV), and O (e84-532 eV). The Be band measurements provide an important constraint on local absorption of X-rays from the hot component of the local interstellar medium. Work has also continued on the development of a calorimetric detector for high-resolution spectroscopy in the 0.1 keV - 8keV energy range.

  5. Sulfur Speciation in Biochars by Very High Resolution Benchtop Kα X-ray Emission Spectroscopy.

    PubMed

    Holden, William M; Seidler, Gerald T; Cheah, Singfoong

    2018-05-30

    The analytical chemistry of sulfur-containing materials poses substantial technical challenges, especially due to the limitations of 33 S NMR and the time-intensive preparations required for wet-chemistry analyses. A number of prior studies have found that synchrotron-based X-ray absorption near edge structure (XANES) measurements can give detailed speciation of sulfur chemistry in such cases. However, due to the obvious access limitations, synchrotron XANES of sulfur cannot be part of routine analytical practice across the chemical sciences community. Here, in a study of the sulfur chemistry in biochars, we compare and contrast the chemical inferences available from synchrotron XANES with that given by benchtop, extremely high resolution wavelength-dispersive X-ray fluorescence (WD-XRF) spectroscopy, also often called X-ray emission spectroscopy (XES). While the XANES spectra have higher total information content, often giving differentiation between different moieties having the same oxidation state, the lower sensitivity of the S Kα XES to coordination and local structure provides pragmatic benefit for the more limited goal of quantifying the S oxidation state distribution. Within that constrained metric, we find good agreement between the two methods. As the sulfur concentrations were as low as 150 ppm, these measurements provide proof-of-principle for characterization of the sulfur chemistry of biochars and potential applications to other areas such as soils, batteries, catalysts, and fossil fuels and their combustion products.

  6. Chemical potential shift in organic field-effect transistors identified by soft X-ray operando nano-spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Nagamura, Naoka, E-mail: NAGAMURA.Naoka@nims.go.jp; Kitada, Yuta; Honma, Itaru

    2015-06-22

    A chemical potential shift in an organic field effect transistor (OFET) during operation has been revealed by soft X-ray operando nano-spectroscopy analysis performed using a three-dimensional nanoscale electron-spectroscopy chemical analysis system. OFETs were fabricated using ultrathin (3 ML or 12 nm) single-crystalline C10-DNBDT-NW films on SiO{sub 2} (200 nm)/Si substrates with a backgate electrode and top source/drain Au electrodes, and C 1s line profiles under biasing at the backgate and drain electrodes were measured. When applying −30 V to the backgate, there is C 1s core level shift of 0.1 eV; this shift can be attributed to a chemical potential shift correspondingmore » to band bending by the field effect, resulting in p-type doping.« less

  7. Research relative to high energy astrophysics. [large area modular array of reflectors, X-ray spectroscopy, and thermal control

    NASA Technical Reports Server (NTRS)

    Gorenstein, P.

    1984-01-01

    Various parameters which affect the design of the proposed large area modular array of reflectors (LAMAR) are considered, including thermal control, high resolution X-ray spectroscopy, pointing control, and mirror performance. The LAMAR instrument is to be a shuttle-launched X-ray observatory to carry out cosmic X-ray investigations. The capabilities of LAMAR are enumerated. Angular resolution performance of the mirror module prototype was measured to be 30 sec of ARC for 50% of the power. The LAMAR thermal pre-collimator design concepts and test configurations are discussed in detail.

  8. Application of X-ray photoelectron spectroscopy to the analysis of stainless-steel welding aerosols

    NASA Astrophysics Data System (ADS)

    Tandon, R. K.; Payling, R.; Chenhall, B. E.; Crisp, P. T.; Ellis, J.; Baker, R. S.

    1985-02-01

    Aerosol particles ("fume") from manual metal arc welding of stainless steel with E316L-16 electrodes were analysed by X-ray photoelectron spectroscopy. The inherent complexity of the particles required the use of a wide range of experimental techniques. These included IR spectrophotometry, TGA/DTA, XRF, XRD, AAS and electron microprobe analysis. The surface of the fume particles comprised ≈ 50 at% NaF and KF, ≈ 8 at.% soluble (probably K) chromate, ≈ 30 at% SiO 2 and several at.% transition-metal oxides, hydroxides or silicates. The fluorides and chromates were removed by washing to reveal a surface which was predominantly SiO 2 (≈ 60 at%) with the remainder comprising of transition-metal oxides, silicates and fluorides. Approximately 6 at% F remained on the surface of the water-washed particles, presumably as transition-metal fluoro-complexes. The water-soluble fraction of the fume contained K +, Na +, F - and CrO 2-4 ions in the mole ratio 5:5:4:3. When aerosol particles are deposited in lung tissues, water-soluble constituents would be expected to dissolve rapidly. In view of the suspected carcinogenicity of stainless steel welding fume, a bio-medical study of the combined effects of F - and CrO 2-4 ions on lung tissue is warranted.

  9. Structural investigations of Pu{sup III} phosphate by X-ray diffraction, MAS-NMR and XANES spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Popa, Karin; Raison, Philippe E., E-mail: philippe.raison@ec.europa.eu; Martel, Laura

    2015-10-15

    PuPO{sub 4} was prepared by a solid state reaction method and its crystal structure at room temperature was solved by powder X-ray diffraction combined with Rietveld refinement. High resolution XANES measurements confirm the +III valence state of plutonium, in agreement with valence bond derivation. The presence of the americium (as β{sup −} decay product of plutonium) in the +III oxidation state was determined based on XANES spectroscopy. High resolution solid state {sup 31}P NMR agrees with the XANES results and the presence of a solid-solution. - Graphical abstract: A full structural analysis of PuPO{sub 4} based on Rietveld analysis ofmore » room temperature X-ray diffraction data, XANES and MAS NMR measurements was performed. - Highlights: • The crystal structure of PuPO{sub 4} monazite is solved. • In PuPO{sub 4} plutonium is strictly trivalent. • The presence of a minute amount of Am{sup III} is highlighted. • We propose PuPO{sub 4} as a potential reference material for spectroscopic and microscopic studies.« less

  10. 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.

  11. Synchrotron X-ray microscopy and spectroscopy analysis of iron in hemochromatosis liver and intestines

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Ko, J .Y. Peter; Sham, Tsun-Kong; Chakrabarti, Subrata

    2009-12-01

    Hemochromatosis is a genetic disorder that causes body to store excess iron in organs such as heart or liver. Distribution of iron, as well as copper, zinc and calcium, and chemical identity of iron in hemochromatosis liver and intestine were investigated by X-ray microprobe experiments, which consist of X-ray microscopy and micro-X-ray absorption fine structure. Our results show that iron concentration in hemochromatosis liver tissue is high, while much less Fe is found in intestinal tissue. Moreover, chemical identity of Fe in hemochromatosis liver can be identified. X-ray microprobe experiments allows for examining elemental distribution at an excellent spatial resolution.more » Moreover, chemical identity of element of interest can be obtained.« less

  12. 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.

  13. X-ray absorption spectroscopy study of Gd3+-loaded ultra-short carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Ma, Q.; Jebb, M.; Tweedle, M. F.; Wilson, L. J.

    2013-04-01

    We present an x-ray absorption spectroscopy study of the local structure around the Gd3+ion loaded in ultra short (20-100 nm) carbon nanotubes (GNTs). X-ray Gd L3 absorption near edge structure data shows that the 31.2-μM GNT suspension exhibits a clear characteristic of hydration at the [GdOn] cluster. Extended x-ray absorption fine structure data show that the Gd3+ ion is coordinated by about 9 oxygen ions and that this first coordination shell exhibits an asymmetry similar to that found in triclinic Gd-acetate or Gd[C2H3O2]3·4H2O or GdAc. After correction for the asymmetry using the cumulant of the third order, the Gd-O bond distance is found to be 2.345 Å, instead of 2.406 Å for a symmetrical (or Gaussian) distribution. It is shorter than that in the Gd-containing MRI contrast agents currently in clinical uses. This may account in part for high proton relaxivity observed for the GNT suspension.

  14. Monitoring Ultrafast Chemical Dynamics by Time-Domain X-ray Photo- and Auger-Electron Spectroscopy.

    PubMed

    Gessner, Oliver; Gühr, Markus

    2016-01-19

    The directed flow of charge and energy is at the heart of all chemical processes. Extraordinary efforts are underway to monitor and understand the concerted motion of electrons and nuclei with ever increasing spatial and temporal sensitivity. The element specificity, chemical sensitivity, and temporal resolution of ultrafast X-ray spectroscopy techniques hold great promise to provide new insight into the fundamental interactions underlying chemical dynamics in systems ranging from isolated molecules to application-like devices. Here, we focus on the potential of ultrafast X-ray spectroscopy techniques based on the detection of photo- and Auger electrons to provide new fundamental insight into photochemical processes of systems with various degrees of complexity. Isolated nucleobases provide an excellent testing ground for our most fundamental understanding of intramolecular coupling between electrons and nuclei beyond the traditionally applied Born-Oppenheimer approximation. Ultrafast electronic relaxation dynamics enabled by the breakdown of this approximation is the major component of the nucleobase photoprotection mechanisms. Transient X-ray induced Auger electron spectroscopy on photoexcited thymine molecules provides atomic-site specific details of the extremely efficient coupling that converts potentially bond changing ultraviolet photon energy into benign heat. In particular, the time-dependent spectral shift of a specific Auger band is sensitive to the length of a single bond within the molecule. The X-ray induced Auger transients show evidence for an electronic transition out of the initially excited state within only ∼200 fs in contrast to theoretically predicted picosecond population trapping behind a reaction barrier. Photoinduced charge transfer dynamics between transition metal complexes and semiconductor nanostructures are of central importance for many emerging energy and climate relevant technologies. Numerous demonstrations of photovoltaic and

  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. Band alignment of SiO2/(AlxGa1-x)2O3 (0 ≤ x ≤ 0.49) determined by X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Feng, Zhaoqing; Feng, Qian; Zhang, Jincheng; Li, Xiang; Li, Fuguo; Huang, Lu; Chen, Hong-Yan; Lu, Hong-Liang; Hao, Yue

    2018-03-01

    In this work, we report the investigation of the band alignment of SiO2/(AlxGa1-x)2O3 (0 ≤ x ≤ 0.49) utilizing the high resolution X-ray photoelectron spectroscopy (XPS) measurements. The single crystallinity and orientation of β-(AlxGa1-x)2O3 films grown on sapphire by pulsed laser deposition were studied with the high resolution X-ray diffraction. The Ga 2p3/2 and Si 2p core-level spectra as well as valence band spectra were used in the analysis of band alignment. As the mole fraction x of Al increases from 0 to 0.49, the bandgap and conduction band offset values of SiO2/(AlxGa1-x)2O3 increases from 4.9 to 5.6 eV and from 1.5 to 2.1 eV, respectively, while that of valence band offset decreases from 2.2 to 0.9 eV. From the results obtained, the energy band diagram of the studied SiO2/(AlxGa1-x)2O3 (0 ≤ x ≤ 0.49) interfaces is found to be of type I. Energy band lineups of SiO2/(AlxGa1-x)2O3 were thus determined which can be used as for Ga2O3 based power device technology.

  17. Background radiation in inelastic X-ray scattering and X-ray emission spectroscopy. A study for Johann-type spectrometers

    NASA Astrophysics Data System (ADS)

    Paredes Mellone, O. A.; Bianco, L. M.; Ceppi, S. A.; Goncalves Honnicke, M.; Stutz, G. E.

    2018-06-01

    A study of the background radiation in inelastic X-ray scattering (IXS) and X-ray emission spectroscopy (XES) based on an analytical model is presented. The calculation model considers spurious radiation originated from elastic and inelastic scattering processes along the beam paths of a Johann-type spectrometer. The dependence of the background radiation intensity on the medium of the beam paths (air and helium), analysed energy and radius of the Rowland circle was studied. The present study shows that both for IXS and XES experiments the background radiation is dominated by spurious radiation owing to scattering processes along the sample-analyser beam path. For IXS experiments the spectral distribution of the main component of the background radiation shows a weak linear dependence on the energy for the most cases. In the case of XES, a strong non-linear behaviour of the background radiation intensity was predicted for energy analysis very close to the backdiffraction condition, with a rapid increase in intensity as the analyser Bragg angle approaches π / 2. The contribution of the analyser-detector beam path is significantly weaker and resembles the spectral distribution of the measured spectra. Present results show that for usual experimental conditions no appreciable structures are introduced by the background radiation into the measured spectra, both in IXS and XES experiments. The usefulness of properly calculating the background profile is demonstrated in a background subtraction procedure for a real experimental situation. The calculation model was able to simulate with high accuracy the energy dependence of the background radiation intensity measured in a particular XES experiment with air beam paths.

  18. Frontiers of X-Ray Astronomy

    NASA Astrophysics Data System (ADS)

    Fabian, Andrew C.; Pounds, Kenneth A.; Blandford, Roger D.

    2004-07-01

    Preface; 1. Forty years on from Aerobee 150: a personal perspective K. Pounds; 2. X-ray spectroscopy of astrophysical plasmas S. M. Kahn, E. Behar, A. Kinkhabwala and D. W. Savin; 3. X-rays from stars M. Gudel; 4. X-ray observations of accreting white-dwarf systems M. Cropper, G. Ramsay, C. Hellier, K. Mukai, C. Mauche and D. Pandel; 5. Accretion flows in X-ray binaries C. Done; 6. Recent X-ray observations of supernova remnants C. R. Canizares; 7. Luminous X-ray sources in spiral and star-forming galaxies M. Ward; 8. Cosmological constraints from Chandra observations of galaxy clusters S. W. Allen; 9. Clusters of galaxies: a cosmological probe R. Mushotzky; 10. Obscured active galactic nuclei: the hidden side of the X-ray Universe G. Matt; 11. The Chandra Deep Field-North Survey and the cosmic X-ray background W. N. Brandt, D. M. Alexander, F. E. Bauer and A. E. Hornschemeier; 12. Hunting the first black holes G. Hasinger; 13. X-ray astronomy in the new millennium: a summary R. D. Blandford.

  19. The Cambridge-Cambridge X-ray Serendipity Survey: I X-ray luminous galaxies

    NASA Technical Reports Server (NTRS)

    Boyle, B. J.; Mcmahon, R. G.; Wilkes, B. J.; Elvis, M.

    1994-01-01

    We report on the first results obtained from a new optical identification program of 123 faint X-ray sources with S(0.5-2 keV) greater than 2 x 10(exp -14) erg/s/sq cm serendipitously detected in ROSAT PSPC pointed observations. We have spectroscopically identified the optical counterparts to more than 100 sources in this survey. Although the majority of the sample (68 objects) are QSO's, we have also identified 12 narrow emission line galaxies which have extreme X-ray luminosities (10(exp 42) less than L(sub X) less than 10(exp 43.5) erg/s). Subsequent spectroscopy reveals them to be a mixture of star-burst galaxies and Seyfert 2 galaxies in approximately equal numbers. Combined with potentially similar objects identified in the Einstein Extended Medium Sensitivity Survey, these X-ray luminous galaxies exhibit a rate of cosmological evolution, L(sub X) varies as (1 + z)(exp 2.5 +/- 1.0), consistent with that derived for X-ray QSO's. This evolution, coupled with the steep slope determined for the faint end of the X-ray luminosity function (Phi(L(sub X)) varies as L(sub X)(exp -1.9)), implies that such objects could comprise 15-35% of the soft (1-2 keV) X-ray background.

  20. Lu.sub.1-xI.sub.3:Ce.sub.x-a scintillator for gamma-ray spectroscopy and time-of-flight pet

    DOEpatents

    Shah, Kanai S [Newton, MA

    2008-02-12

    The present invention includes very fast scintillator materials including lutetium iodide doped with Cerium (Lu.sub.1-xI.sub.3:Ce.sub.x; LuI.sub.3:Ce). The LuI.sub.3 scintillator material has surprisingly good characteristics including high light output, high gamma-ray stopping efficiency, fast response, low cost, good proportionality, and minimal afterglow that the material is useful for gamma-ray spectroscopy, medical imaging, nuclear and high energy physics research, diffraction, non-destructive testing, nuclear treaty verification and safeguards, and geological exploration.

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

    DOE PAGES

    Lehmkühler, Felix; Kwaśniewski, Paweł; Roseker, Wojciech; ...

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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Lehmkühler, Felix; Kwaśniewski, Paweł; Roseker, Wojciech

    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

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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Albert, Felicie

    2016-10-12

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

  4. X-ray Raman spectroscopy of lithium-ion battery electrolyte solutions in a flow cell.

    PubMed

    Ketenoglu, Didem; Spiekermann, Georg; Harder, Manuel; Oz, Erdinc; Koz, Cevriye; Yagci, Mehmet C; Yilmaz, Eda; Yin, Zhong; Sahle, Christoph J; Detlefs, Blanka; Yavaş, Hasan

    2018-03-01

    The effects of varying LiPF 6 salt concentration and the presence of lithium bis(oxalate)borate additive on the electronic structure of commonly used lithium-ion battery electrolyte solvents (ethylene carbonate-dimethyl carbonate and propylene carbonate) have been investigated. X-ray Raman scattering spectroscopy (a non-resonant inelastic X-ray scattering method) was utilized together with a closed-circle flow cell. Carbon and oxygen K-edges provide characteristic information on the electronic structure of the electrolyte solutions, which are sensitive to local chemistry. Higher Li + ion concentration in the solvent manifests itself as a blue-shift of both the π* feature in the carbon edge and the carbonyl π* feature in the oxygen edge. While these oxygen K-edge results agree with previous soft X-ray absorption studies on LiBF 4 salt concentration in propylene carbonate, carbon K-edge spectra reveal a shift in energy, which can be explained with differing ionic conductivities of the electrolyte solutions.

  5. Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

    NASA Astrophysics Data System (ADS)

    Gaudin, J.; Fourment, C.; Cho, B. I.; Engelhorn, K.; Galtier, E.; Harmand, M.; Leguay, P. M.; Lee, H. J.; Nagler, B.; Nakatsutsumi, M.; Ozkan, C.; Störmer, M.; Toleikis, S.; Tschentscher, Th; Heimann, P. A.; Dorchies, F.

    2014-04-01

    The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called ``molecular movie'' within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level of the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes.

  6. Combined use of atomic force microscopy, X-ray photoelectron spectroscopy, and secondary ion mass spectrometry for cell surface analysis.

    PubMed

    Dague, Etienne; Delcorte, Arnaud; Latgé, Jean-Paul; Dufrêne, Yves F

    2008-04-01

    Understanding the surface properties of microbial cells is a major challenge of current microbiological research and a key to efficiently exploit them in biotechnology. Here, we used three advanced surface analysis techniques with different sensitivity, probing depth, and lateral resolution, that is, in situ atomic force microscopy, X-ray photoelectron spectroscopy, and secondary ion mass spectrometry, to gain insight into the surface properties of the conidia of the human fungal pathogen Aspergillus fumigatus. We show that the native ultrastructure, surface protein and polysaccharide concentrations, and amino acid composition of three mutants affected in hydrophobin production are markedly different from those of the wild-type, thereby providing novel insight into the cell wall architecture of A. fumigatus. The results demonstrate the power of using multiple complementary techniques for probing microbial cell surfaces.

  7. Synthesis, high-resolution NMR spectroscopic analysis, and single-crystal X-ray diffraction of isoxazoline tetracycles.

    PubMed

    Fascio, Mirta L; Alvarez-Larena, Angel; D'Accorso, Norma B

    2002-11-29

    Three isoxazoline tetracycles were obtained enantiomerically pure by intramolecular 1,3-dipolar cycloaddition. The characterization of the new compounds was performed by high-resolution 1H and 13C NMR spectroscopy. The relative configuration of the new chiral centers was determined by NOESY experiments and confirmed by single-crystal X-ray structural analysis.

  8. Depth resolved compositional analysis of aluminium oxide thin film using non-destructive soft x-ray reflectivity technique

    NASA Astrophysics Data System (ADS)

    Sinha, Mangalika; Modi, Mohammed H.

    2017-10-01

    In-depth compositional analysis of 240 Å thick aluminium oxide thin film has been carried out using soft x-ray reflectivity (SXR) and x-ray photoelectron spectroscopy technique (XPS). The compositional details of the film is estimated by modelling the optical index profile obtained from the SXR measurements over 60-200 Å wavelength region. The SXR measurements are carried out at Indus-1 reflectivity beamline. The method suggests that the principal film region is comprised of Al2O3 and AlOx (x = 1.6) phases whereas the interface region comprised of SiO2 and AlOx (x = 1.6) mixture. The soft x-ray reflectivity technique combined with XPS measurements explains the compositional details of principal layer. Since the interface region cannot be analyzed with the XPS technique in a non-destructive manner in such a case the SXR technique is a powerful tool for nondestructive compositional analysis of interface region.

  9. Characterization of the LCLS “nanosecond two-bunch” mode for x-ray speckle visibility spectroscopy experiments

    DOE PAGES

    Sun, Yanwen; Zhu, Diling; Song, Sanghoon; ...

    2017-05-23

    The generation of two X-ray pulses with tunable nanosecond scale time separations has recently been demonstrated at the Linac Coherent Light Source using an accelerator based technique. This approach offers the opportunity to extend X-ray Photon Correlation Spectroscopy techniques to the yet unexplored regime of nanosecond timescales by means of X-ray Speckle Visibility Spectroscopy. As the two pulses originate from two independent Spontaneous Amplified Stimulated Emission processes, the beam properties fluctuate from pulse pair to pulse pair, but as well between the individual pulses within a pair. However, two-pulse XSVS experiments require the intensity of the individual pulses to bemore » either identical in the ideal case, or with a accurately known intensity ratio. We present the design and performances of a non-destructive intensity diagnostic based on measurement of scattering from a transparent target using a high-speed photo-detector. Individual pulses within a pulse pair with time delays as short as 0.7 ns can be resolved. Moreover, using small angle coherent scattering, we characterize the averaged spatial overlap of the focused pulse pairs. Furthermore, the multi-shot average-speckle contrasts from individual pulses and pulse pairs are compared.« less

  10. X-ray photoelectron spectroscopy and atomic force microscopy characterization of the effects of etching Zn xCd 1- xTe surfaces

    NASA Astrophysics Data System (ADS)

    George, M. A.; Azoulay, M.; Jayatirtha, H. N.; Burger, A.; Collins, W. E.; Silberman, E.

    1993-10-01

    X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM) was used for the first time to characterize the chemical composition of modified surfaces of Zn xCd 1- xTe single crystals. These surface treatments were selected for their relevance to device preparation procedures. The XPS peaks indicated an increase of the tellurium and a depletion of the cadmium concentrations upon etching in bromine methanol solution. AFM revealed the formation of pronounced Te inclusions. Higher x values correlated with a decrease in residual bromine left on the surface, while cut and polished samples had higher oxide concentrations and increased bromination of the surface than cleaved samples.

  11. Broadband high resolution X-ray spectral analyzer

    DOEpatents

    Silver, Eric H.; Legros, Mark; Madden, Norm W.; Goulding, Fred; Landis, Don

    1998-01-01

    A broad bandwidth high resolution x-ray fluorescence spectrometer has a performance that is superior in many ways to those currently available. It consists of an array of 4 large area microcalorimeters with 95% quantum efficiency at 6 keV and it produces x-ray spectra between 0.2 keV and 7 keV with an energy resolution of 7 to 10 eV. The resolution is obtained at input count rates per array element of 10 to 50 Hz in real-time, with analog pulse processing and thermal pile-up rejection. This performance cannot be matched by currently available x-ray spectrometers. The detectors are incorporated into a compact and portable cryogenic refrigerator system that is ready for use in many analytical spectroscopy applications as a tool for x-ray microanalysis or in research applications such as laboratory and astrophysical x-ray and particle spectroscopy.

  12. Broadband high resolution X-ray spectral analyzer

    DOEpatents

    Silver, E.H.; Legros, M.; Madden, N.W.; Goulding, F.; Landis, D.

    1998-07-07

    A broad bandwidth high resolution X-ray fluorescence spectrometer has a performance that is superior in many ways to those currently available. It consists of an array of 4 large area microcalorimeters with 95% quantum efficiency at 6 keV and it produces X-ray spectra between 0.2 keV and 7 keV with an energy resolution of 7 to 10 eV. The resolution is obtained at input count rates per array element of 10 to 50 Hz in real-time, with analog pulse processing and thermal pile-up rejection. This performance cannot be matched by currently available X-ray spectrometers. The detectors are incorporated into a compact and portable cryogenic refrigerator system that is ready for use in many analytical spectroscopy applications as a tool for X-ray microanalysis or in research applications such as laboratory and astrophysical X-ray and particle spectroscopy. 6 figs.

  13. X-ray magnetic circular dichroism measured at the Fe K-edge with a reduced intrinsic broadening: x-ray absorption spectroscopy versus resonant inelastic x-ray scattering measurements

    NASA Astrophysics Data System (ADS)

    Juhin, Amélie; Sainctavit, Philippe; Ollefs, Katharina; Sikora, Marcin; Filipponi, Adriano; Glatzel, Pieter; Wilhelm, Fabrice; Rogalev, Andrei

    2016-12-01

    X-ray magnetic circular dichroism is measured at the Fe K pre-edge in yttrium iron garnet using two different procedures that allow reducing the intrinsic broadening due to the 1s corehole lifetime. First, deconvolution of XMCD data measured in total fluorescence yield (TFY) with an extremely high signal-to-noise ratio enables a factor of 2.4 to be gained in the XMCD intensity. Ligand field multiplet calculations performed with different values of intrinsic broadening show that deconvolving such high quality XMCD data is similar to reducing the lifetime broadening from a 1s corehole to a 2p corehole. Second, MCD is measured by resonant inelastic x-ray scattering spectroscopy as a function of incident energy and emission energy. Selection of a fixed emission energy, instead of using the TFY, allows enhancing the MCD intensity up to a factor of  ˜4.7. However, this significantly changes the spectral shape of the XMCD signal, which cannot be interpreted any more as an absorption spectrum.

  14. A study of mercuric iodide near melting using differential scanning calorimetry, Raman spectroscopy and X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Burger, A.; Morgan, S.; Jiang, H.; Silberman, E.; Schieber, M.; Van Den Berg, L.; Keller, L.; Wagner, C. N. J.

    1989-11-01

    High-temperature studies of mercuric iodide (HgI2) involving differential scanning calorimetry (DSC), Raman spectroscopy and X-ray powder diffraction have failed to confirm the existence of a red-colored tetragonal high-temperature phase called α'-HgI2 reported by S.N. Toubektsis et al. [J. Appl. Phys. 58 (1988) 2070] using DSC measurements. The multiple DSC peaks near melting reported by Toubektsis are found by the present authors only if the sample is heated in a stainless-steel container. Using a Pyrex container or inserting a platinum foil between the HgI2 and the stainless-steel container yields only one sharp, single DSC peak at the melting point. The nonexistence of the α' phase is confirmed by high-temperature X-ray diffraction and Raman spectroscopy performed in the vicinity of the melting point. These methods clearly, indicate the existence of only the yellow orthorhombic β-HgI2 phase. The experimental high-temperature DSC, Raman and X-ray diffraction data are presented and discussed.

  15. Saccharose solid matrix embedded proteins: a new method for sample preparation for X-ray absorption spectroscopy.

    PubMed

    Ascone, I; Sabatucci, A; Bubacco, L; Di Muro, P; Salvato, B

    2000-01-01

    In this study, solid samples of hemoglobin and hemocyanin have been prepared by embedding the proteins into a saccharose-based matrix. These materials have been developed specifically for specimens for X-ray absorption spectroscopy (XAS). The preservation of protein conformation and active site organization was tested, making comparisons between the solid and the corresponding liquid samples, using resonance Raman, infra red, fluorescence and XAS. The XAS spectra of irradiated solid and liquid samples were then compared, and the preservation of biological activity of the proteins during both preparation procedure and X-ray irradiation was assessed. In all cases, the measurements clearly demonstrate that protein solid samples are both structurally and functionally quite well preserved, much better than those in the liquid state. The saccharose matrix provides an excellent protection against X-ray damages, allowing for longer exposure to the X-ray beam. Moreover, the demonstrated long-term stability of samples permits their preparation and storage in optimal conditions, allowing for the repetition of data collection with the same sample in several experimental sessions. The very high protein concentration that can be reached results in a significantly better signal-to-noise ratio, particularly useful for high molecular weight proteins with a low metal-to-protein ratio. On the bases of the above-mentioned results, we propose the new method as a standard procedure for the preparation of biological samples to be used for XAS spectroscopy.

  16. Electronic structure change of NiS2- x Se x in the metal-insulator transition probed by X-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Jeong, Jinwon; Park, Kyung Ja; Cho, En-Jin; Noh, Han-Jin; Kim, Sung Baek; Kim, Hyeong-Do

    2018-01-01

    The electronic structure change of NiS2- x Se x as a function of Se concentration x has been studied by Ni L-edge X-ray absorption spectroscopy (XAS). The XAS spectra show distinct features in Ni L 3 edge, indicating whether the system is insulating or metallic. These features can be semi-quantitatively explained within the framework of the configurational interaction cluster model (CICM). In the S-rich region, relatively large charge-transfer energy (Δ 5 eV) from ligand p to Ni 3 d states and a little small p- d hybridization strength ( V pdσ 1.1 eV) can reproduce the experimental spectra in the CICM calculation, and vice versa in the Se-rich region. Our analysis result is consistent with the Zaanen-Sawatzky-Allen scheme that the systems in S-rich side ( x ≤ 0.5) are a charge transfer insulator. However, it also requires that the Δ value must change abruptly in spite of the small change of x near x = 0.5. As a possible microscopic origin, we propose a percolation scenario where a long range connection of Ni[(S,Se)2]6 octahedra with Se-Se dimers plays a key role to gap closure.

  17. Adaptive design of an X-ray magnetic circular dichroism spectroscopy experiment with Gaussian process modelling

    NASA Astrophysics Data System (ADS)

    Ueno, Tetsuro; Hino, Hideitsu; Hashimoto, Ai; Takeichi, Yasuo; Sawada, Masahiro; Ono, Kanta

    2018-01-01

    Spectroscopy is a widely used experimental technique, and enhancing its efficiency can have a strong impact on materials research. We propose an adaptive design for spectroscopy experiments that uses a machine learning technique to improve efficiency. We examined X-ray magnetic circular dichroism (XMCD) spectroscopy for the applicability of a machine learning technique to spectroscopy. An XMCD spectrum was predicted by Gaussian process modelling with learning of an experimental spectrum using a limited number of observed data points. Adaptive sampling of data points with maximum variance of the predicted spectrum successfully reduced the total data points for the evaluation of magnetic moments while providing the required accuracy. The present method reduces the time and cost for XMCD spectroscopy and has potential applicability to various spectroscopies.

  18. Analysis of the Central X-ray Source in DG Tau

    NASA Astrophysics Data System (ADS)

    Schneider, P. Christian; Schmitt, Jürgen H. M. M.

    As a stellar X-ray source DG Tau shows two rather unusual features: A resolved X-ray jet [2] and an X-ray spectrum best described by two thermal components with different absorbing column densities, a so called "two-absorber X-ray (TAX)" morphology [1, 2]. In an effort to understand the properties of the central X-ray source in DG Tau a detailed position analysis was carried out.

  19. Summary: Update to ASTM Guide E 1523 to Charge Control and Charge Referencing Techniques in X-ray Photoelectron Spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Baer, Donald R.

    2005-04-22

    An updated version of the ASTM guide E1523 to the methods to charge control and charge referencing techniques in x-ray photoelectron spectroscopy has been released by ASTM. The guide is meant to acquaint x-ray photoelectron spectroscopy (XPS) users with the various charge control and charge referencing techniques that are and have been used in the acquisition and interpretation of XPS data from surfaces of insulating specimens. The current guide has been expanded to include new references as well as recommendations for reporting information on charge control and charge referencing. The previous version of the document had been published in 1997.

  20. Sulfur Speciation in Biochars by Very High Resolution Benchtop Ka X-Ray Emission Spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Cheah, Singfoong; Holden, William M.; Seidler, Gerald T.

    The analytical chemistry of sulfur-containing materials poses substantial technical challenges, especially due to the limitations of 33S NMR and the time-intensive preparations required for wet-chemistry analyses. A number of prior studies have found that synchrotron-based X-ray absorption near edge structure (XANES) measurements can give detailed speciation of sulfur chemistry in such cases. However, due to the obvious access limitations, synchrotron XANES of sulfur cannot be part of routine analytical practice across the chemical sciences community. Here, in a study of the sulfur chemistry in biochars, we compare and contrast the chemical inferences available from synchrotron XANES with that given bymore » benchtop, extremely high resolution wavelength-dispersive X-ray fluorescence (WD-XRF) spectroscopy, also often called X-ray emission spectroscopy (XES). While the XANES spectra have higher total information content, often giving differentiation between different moieties having the same oxidation state, the lower sensitivity of the S Ka XES to coordination and local structure provides pragmatic benefit for the more limited goal of quantifying the S oxidation state distribution. Within that constrained metric, we find good agreement between the two methods. As the sulfur concentrations were as low as 150 ppm, these measurements provide proof-of-principle for characterization of the sulfur chemistry of biochars and potential applications to other areas such as soils, batteries, catalysts, and fossil fuels and their combustion products.« less

  1. Quantification of rapid environmental redox processes with quick-scanning x-ray absorption spectroscopy (Q-XAS)

    PubMed Central

    Ginder-Vogel, Matthew; Landrot, Gautier; Fischel, Jason S.; Sparks, Donald L.

    2009-01-01

    Quantification of the initial rates of environmental reactions at the mineral/water interface is a fundamental prerequisite to determining reaction mechanisms and contaminant transport modeling and predicting environmental risk. Until recently, experimental techniques with adequate time resolution and elemental sensitivity to measure initial rates of the wide variety of environmental reactions were quite limited. Techniques such as electron paramagnetic resonance and Fourier transform infrared spectroscopies suffer from limited elemental specificity and poor sensitivity to inorganic elements, respectively. Ex situ analysis of batch and stirred-flow systems provides high elemental sensitivity; however, their time resolution is inadequate to characterize rapid environmental reactions. Here we apply quick-scanning x-ray absorption spectroscopy (Q-XAS), at sub-second time-scales, to measure the initial oxidation rate of As(III) to As(V) by hydrous manganese(IV) oxide. Using Q-XAS, As(III) and As(V) concentrations were determined every 0.98 s in batch reactions. The initial apparent As(III) depletion rate constants (t < 30 s) measured with Q-XAS are nearly twice as large as rate constants measured with traditional analytical techniques. Our results demonstrate the importance of developing analytical techniques capable of analyzing environmental reactions on the same time scale as they occur. Given the high sensitivity, elemental specificity, and time resolution of Q-XAS, it has many potential applications. They could include measuring not only redox reactions but also dissolution/precipitation reactions, such as the formation and/or reductive dissolution of Fe(III) (hydr)oxides, solid-phase transformations (i.e., formation of layered-double hydroxide minerals), or almost any other reaction occurring in aqueous media that can be measured using x-ray absorption spectroscopy. PMID:19805269

  2. Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

    PubMed Central

    Gaudin, J.; Fourment, C.; Cho, B. I.; Engelhorn, K.; Galtier, E.; Harmand, M.; Leguay, P. M.; Lee, H. J.; Nagler, B.; Nakatsutsumi, M.; Ozkan, C.; Störmer, M.; Toleikis, S.; Tschentscher, Th; Heimann, P. A.; Dorchies, F.

    2014-01-01

    The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called “molecular movie” within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level of the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes. PMID:24740172

  3. Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

    DOE PAGES

    Gaudin, J.; Fourment, C.; Cho, B. I.; ...

    2014-04-17

    The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called “molecular movie” within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level ofmore » the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes.« less

  4. Effect of Pressure on Valence and Structural Properties of YbFe 2 Ge 2 Heavy Fermion Compound—A Combined Inelastic X-ray Spectroscopy, X-ray Diffraction, and Theoretical Investigation

    DOE PAGES

    Kumar, Ravhi S.; Svane, Axel; Vaitheeswaran, Ganapathy; ...

    2015-10-19

    We measured the crystal structure and the Yb valence of the YbFe 2Ge 2 heavy fermion compound at room temperature and under high pressures using high-pressure powder X-ray diffraction and X-ray absorption spectroscopy via both partial fluorescence yield and resonant inelastic X-ray emission techniques. Moreover, the measurements are complemented by first-principles density functional theoretical calculations using the self-interaction corrected local spin density approximation investigating in particular the magnetic structure and the Yb valence. Finally, while the ThCr 2Si 2-type tetragonal (I4/mmm) structure is stable up to 53 GPa, the X-ray emission results show an increase of the Yb valence frommore » v = 2.72(2) at ambient pressure to v = 2.93(3) at ~9 GPa, where at low temperature a pressure-induced quantum critical state was reported.« less

  5. 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.

  6. High-pressure studies with x-rays using diamond anvil cells

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Shen, Guoyin; Mao, Ho Kwang

    2016-11-22

    Pressure profoundly alters all states of matter. The symbiotic development of ultrahigh-pressure diamond anvil cells, to compress samples to sustainable multi-megabar pressures; and synchrotron x-ray techniques, to probe materials' properties in situ, has enabled the exploration of rich high-pressure (HP) science. In this article, we first introduce the essential concept of diamond anvil cell technology, together with recent developments and its integration with other extreme environments. We then provide an overview of the latest developments in HP synchrotron techniques, their applications, and current problems, followed by a discussion of HP scientific studies using x-rays in the key multidisciplinary fields. Thesemore » HP studies include: HP x-ray emission spectroscopy, which provides information on the filled electronic states of HP samples; HP x-ray Raman spectroscopy, which probes the HP chemical bonding changes of light elements; HP electronic inelastic x-ray scattering spectroscopy, which accesses high energy electronic phenomena, including electronic band structure, Fermi surface, excitons, plasmons, and their dispersions; HP resonant inelastic x-ray scattering spectroscopy, which probes shallow core excitations, multiplet structures, and spin-resolved electronic structure; HP nuclear resonant x-ray spectroscopy, which provides phonon densities of state and time-resolved Mössbauer information; HP x-ray imaging, which provides information on hierarchical structures, dynamic processes, and internal strains; HP x-ray diffraction, which determines the fundamental structures and densities of single-crystal, polycrystalline, nanocrystalline, and non-crystalline materials; and HP radial x-ray diffraction, which yields deviatoric, elastic and rheological information. Integrating these tools with hydrostatic or uniaxial pressure media, laser and resistive heating, and cryogenic cooling, has enabled investigations of the structural, vibrational, electronic, and

  7. High-pressure studies with x-rays using diamond anvil cells

    NASA Astrophysics Data System (ADS)

    Shen, Guoyin; Mao, Ho Kwang

    2017-01-01

    Pressure profoundly alters all states of matter. The symbiotic development of ultrahigh-pressure diamond anvil cells, to compress samples to sustainable multi-megabar pressures; and synchrotron x-ray techniques, to probe materials’ properties in situ, has enabled the exploration of rich high-pressure (HP) science. In this article, we first introduce the essential concept of diamond anvil cell technology, together with recent developments and its integration with other extreme environments. We then provide an overview of the latest developments in HP synchrotron techniques, their applications, and current problems, followed by a discussion of HP scientific studies using x-rays in the key multidisciplinary fields. These HP studies include: HP x-ray emission spectroscopy, which provides information on the filled electronic states of HP samples; HP x-ray Raman spectroscopy, which probes the HP chemical bonding changes of light elements; HP electronic inelastic x-ray scattering spectroscopy, which accesses high energy electronic phenomena, including electronic band structure, Fermi surface, excitons, plasmons, and their dispersions; HP resonant inelastic x-ray scattering spectroscopy, which probes shallow core excitations, multiplet structures, and spin-resolved electronic structure; HP nuclear resonant x-ray spectroscopy, which provides phonon densities of state and time-resolved Mössbauer information; HP x-ray imaging, which provides information on hierarchical structures, dynamic processes, and internal strains; HP x-ray diffraction, which determines the fundamental structures and densities of single-crystal, polycrystalline, nanocrystalline, and non-crystalline materials; and HP radial x-ray diffraction, which yields deviatoric, elastic and rheological information. Integrating these tools with hydrostatic or uniaxial pressure media, laser and resistive heating, and cryogenic cooling, has enabled investigations of the structural, vibrational, electronic, and

  8. 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

  9. Site partitioning of Cr3+ in the trichroic alexandrite BeAl2O4:Cr3+ crystal: contribution from x-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Bordage, Amélie; Rossano, Stéphanie; Horn, Adolf Heinrich; Fuchs, Yves

    2012-06-01

    X-ray absorption spectroscopy measurements at the Cr K-edge of a trichroic crystal of alexandrite BeAl2O4:Cr3+ for different orientations of the crystal with respect to the polarization and direction of the x-ray incident beam have been performed. Analysis of the experimental spectra with the help of first-principles calculations of x-ray absorption spectra allowed us to estimate the proportion of chromium Cr3+ cations among the two different octahedral sites of the alexandrite structure (70% in the Cs site-30% in the Ci site). The methodology presented in this work opens up new possibilities in the field of mineralogy for the study of complex minerals containing several sites potentially occupied by several transition elements or for solid solutions.

  10. Report on the 18th International Conference on X-ray and Inner-Shell Processes (X99).

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Gemmell, D. S.; Physics

    2000-01-01

    The 18th conference of the series served as a forum for discussing fundamental issues in the field of x-ray and inner-shell processes and their application in various disciplines of science and technology. Special emphasis was given to the opportunities offered by modern synchrotron x-ray sources. The program included plenary talks, progress reports and poster presentations relating to new developments in the field of x-ray and inner-shell processes. The range of topics included: X-ray interactions with atoms, molecules, clusters, surfaces and solids; Decay processes for inner-shell vacancies; X-ray absorption and emission spectroscopy - Photoionization processes; Phenomena associated with highly charged ionsmore » and collisions with energetic particles; Electron-spin and -momentum spectroscopy; X-ray scattering and spectroscopy in the study of magnetic systems; Applications in materials science, biology, geosciences, and other disciplines; Elastic and inelastic x-ray scattering processes in atoms and molecules; Threshold phenomena (post-collision interaction, resonant Raman processes, etc.); Nuclear absorption and scattering of x-rays; 'Fourth-generation' x-ray sources; Processes exploiting the polarization and coherence properties of x-ray beams; Developments in experimental techniques (x-ray optics, temporal techniques, detectors); Microscopy, spectromicroscopy, and various imaging techniques; Non-linear processes and x-ray lasers; Ionization and excitation induced by charged particles and by x-rays; and Exotic atoms (including 'hollow' atoms and atoms that contain 'exotic' particles).« less

  11. Scanning electron microscopy and X-ray energy dispersive spectroscopy - useful tools in the analysis of pharmaceutical products

    NASA Astrophysics Data System (ADS)

    Sarecka-Hujar, Beata; Balwierz, Radoslaw; Ostrozka-Cieslik, Aneta; Dyja, Renata; Lukowiec, Dariusz; Jankowski, Andrzej

    2017-11-01

    The quality of the drug, its purity and identification of degradation products provide the highest quality of pharmaceutical products. The energy dispersive spectroscopy (EDS) method analyses the percentage of each element form as well as their distribution, and morphological characteristics of the drug form. We analysed the usefulness of EDS method in testing orally disintegrating tablets (ODT) with trimetazidine hydrochloride with high resolution scanning electron microscopy (SEM, SUPRA25 Carl Zeiss company) with spectrophotometer equipped with an X-ray energy dispersion (EDAX Company). The samples of the analysed tablets were imaged after applying conductive layers of gold on their surface. In the EDS analysis the compositions of each sample of the obtained tablets were observed to be virtually identical. The differences in the content of carbon and oxygen came from differences in the composition of particular tablets. The presence of gold in the composition resulted from the sputtering the surface of tablets with gold during the analysis. Knowing the composition of the tablet, SEM-EDS method helps to locate and identify the impurities and degradation products of the compounds, leading to a better understanding of the mechanisms of their formation.

  12. X-Ray Weak Broad-Line Quasars: Absorption or Intrinsic X-Ray Weakness

    NASA Technical Reports Server (NTRS)

    Risaliti, Guido; Mushotzky, Richard F. (Technical Monitor)

    2004-01-01

    XMM observations of X-ray weak quasars have been performed during 2003. The data for all but the last observation are now available (there has been a delay of several months on the initial schedule, due to high background flares which contaminated the observations: as a consequence, most of them had to be rescheduled). We have reduced and analyzed these data, and obtained interesting preliminary scientific results. Out of the eight sources, 4 are confirmed to be extrimely X-ray weak, in agreement with the results of previous Chandra observations. 3 sources are confirmed to be highly variable both in flux (by factors 20-50) and in spectral properties (dramatic changes in spectral index). For both these groups of objects, an article is in preparation. Preliminary results have been presented at an international workshop on AGN surveys in December 2003, in Cozumel (Mexico). In order to further understand the nature of these X-ray weak quasars, we submitted proposals for spectroscopy at optical and infrared telescopes. We obtained time at the TNG 4 meter telescope for near-IR observations, and at the Hobby-Eberly Telescope for optical high-resolution spectroscopy. These observations will be performed in early 2004, and will complement the XMM data, in order to understand whether the X-ray weakness of these sources is an intrinsic property or is due to absorption by circumnuclear material.

  13. 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.

  14. GSFC Contributions to the NATO X-ray Astronomy Institute, Erice, July 1979. [X-ray spectra of supernova remants, galactic X-ray sources, active galactic nuclei, and clusters of galaxies

    NASA Technical Reports Server (NTRS)

    Holt, S. S.; Mushotzky, R. F.

    1979-01-01

    An overview of X-ray astronomical spectroscopy in general is presented and results obtained by HEAO 1 and 2 as well as earlier spacecraft are examined. Particular emphasis is given to the spectra of supernova remnants; galactic binary X-ray sources, cataclysmic variables, bulges, pulsars, and stars; the active nuclei of Seyfert 1 galaxy, BL Lac, and quasars; the diffuse X-ray background; and galactic clusters.

  15. TOPICAL REVIEW: Human soft tissue analysis using x-ray or gamma-ray techniques

    NASA Astrophysics Data System (ADS)

    Theodorakou, C.; Farquharson, M. J.

    2008-06-01

    This topical review is intended to describe the x-ray techniques used for human soft tissue analysis. X-ray techniques have been applied to human soft tissue characterization and interesting results have been presented over the last few decades. The motivation behind such studies is to provide improved patient outcome by using the data obtained to better understand a disease process and improve diagnosis. An overview of theoretical background as well as a complete set of references is presented. For each study, a brief summary of the methodology and results is given. The x-ray techniques include x-ray diffraction, x-ray fluorescence, Compton scattering, Compton to coherent scattering ratio and attenuation measurements. The soft tissues that have been classified using x-rays or gamma rays include brain, breast, colon, fat, kidney, liver, lung, muscle, prostate, skin, thyroid and uterus.

  16. Mössbauer spectroscopy and X-ray diffraction analyses of clayey samples used as ceramic sourcing materials, in Peru

    NASA Astrophysics Data System (ADS)

    Quille, Rubén; Bustamante, Ángel; Palomino, Ybar

    2011-11-01

    The ceramic industry is an important area of economic activity in the Ayacucho Region, in particular in the District of Quinua. As a consequence, there is a huge demand for clay to produce ceramic pastes in that region. This paper reports on results concerning the mineralogical characterization of four clayey samples, which were collected MAA and SPQA from the area Pampa de La Quinua with geographic coordinates 13° 02' 49″ S 74° 08' 03″ W, CE1M and CE2M from the Quinua locality 13° 03' 07″ S 74° 08' 31″ W, both in the District of Quinua, Province of Huamanga, Ayacucho, Peru. The chemical and mineralogical characterization of these samples was carried out with powder X-ray diffraction detecting quartz, albite, montmorillonite, kaolinite and glauconite mineral phases, Mössbauer spectroscopy detected iron in kaolinite, glauconite and montmorillonite minerals. Chemical analysis was performed through scanning electron microscopy and energy dispersive X-ray spectroscopy. Data obtained from the combination of these techniques provided relevant information about the morphology, chemical composition, and the mineralogy of samples.

  17. Crystallography with online optical and X-ray absorption spectroscopies demonstrates an ordered mechanism in copper nitrite reductase.

    PubMed

    Hough, Michael A; Antonyuk, Svetlana V; Strange, Richard W; Eady, Robert R; Hasnain, S Samar

    2008-04-25

    Nitrite reductases are key enzymes that perform the first committed step in the denitrification process and reduce nitrite to nitric oxide. In copper nitrite reductases, an electron is delivered from the type 1 copper (T1Cu) centre to the type 2 copper (T2Cu) centre where catalysis occurs. Despite significant structural and mechanistic studies, it remains controversial whether the substrates, nitrite, electron and proton are utilised in an ordered or random manner. We have used crystallography, together with online X-ray absorption spectroscopy and optical spectroscopy, to show that X-rays rapidly and selectively photoreduce the T1Cu centre, but that the T2Cu centre does not photoreduce directly over a typical crystallographic data collection time. Furthermore, internal electron transfer between the T1Cu and T2Cu centres does not occur, and the T2Cu centre remains oxidised. These data unambiguously demonstrate an 'ordered' mechanism in which electron transfer is gated by binding of nitrite to the T2Cu. Furthermore, the use of online multiple spectroscopic techniques shows their value in assessing radiation-induced redox changes at different metal sites and demonstrates the importance of ensuring the correct status of redox centres in a crystal structure determination. Here, optical spectroscopy has shown a very high sensitivity for detecting the change in T1Cu redox state, while X-ray absorption spectroscopy has reported on the redox status of the T2Cu site, as this centre has no detectable optical absorption.

  18. Identifying anthropogenic uranium compounds using soft X-ray near-edge absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Ward, Jesse D.; Bowden, Mark; Tom Resch, C.; Eiden, Gregory C.; Pemmaraju, C. D.; Prendergast, David; Duffin, Andrew M.

    2017-01-01

    Uranium ores mined for industrial use are typically acid-leached to produce yellowcake and then converted into uranium halides for enrichment and purification. These anthropogenic chemical forms of uranium are distinct from their mineral counterparts. The purpose of this study is to use soft X-ray absorption spectroscopy to characterize several common anthropogenic uranium compounds important to the nuclear fuel cycle. Chemical analyses of these compounds are important for process and environmental monitoring. X-ray absorption techniques have several advantages in this regard, including element-specificity, chemical sensitivity, and high spectral resolution. Oxygen K-edge spectra were collected for uranyl nitrate, uranyl fluoride, and uranyl chloride, and fluorine K-edge spectra were collected for uranyl fluoride and uranium tetrafluoride. Interpretation of the data is aided by comparisons to calculated spectra. The effect of hydration state on the sample, a potential complication in interpreting oxygen K-edge spectra, is discussed. These compounds have unique spectral signatures that can be used to identify unknown samples.

  19. Identifying anthropogenic uranium compounds using soft X-ray near-edge absorption spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Ward, Jesse D.; Bowden, Mark; Tom Resch, C.

    2017-01-01

    Uranium ores mined for industrial use are typically acid-leached to produce yellowcake and then converted into uranium halides for enrichment and purification. These anthropogenic chemical forms of uranium are distinct from their mineral counterparts. The purpose of this study is to use soft X-ray absorption spectroscopy to characterize several common anthropogenic uranium compounds important to the nuclear fuel cycle. Non-destructive chemical analyses of these compounds is important for process and environmental monitoring and X-ray absorption techniques have several advantages in this regard, including element-specificity, chemical sensitivity, and high spectral resolution. Oxygen K-edge spectra were collected for uranyl nitrate, uranyl fluoride,more » and uranyl chloride, and fluorine K-edge spectra were collected for uranyl fluoride and uranium tetrafluoride. Interpretation of the data is aided by comparisons to calculated spectra. These compounds have unique spectral signatures that can be used to identify unknown samples.« less

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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Andrews, J.C.

    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 IImore » 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.« less

  1. An Energy Dispersive X-ray Spectroscopy Analysis of Elemental Changes of a Persimmon Phytobezoar Dissolved in Coca-Cola.

    PubMed

    Iwamuro, Masaya; Urata, Haruo; Higashi, Reiji; Nakagawa, Masahiro; Ishikawa, Shin; Shiraha, Hidenori; Okada, Hiroyuki

    To investigate the mechanism of phytobezoar dissolution by Coca-Cola(®), persimmon phytobezoar pieces removed from a 60-year-old Japanese woman were analyzed by energy dispersive X-ray spectroscopy. The amount of calcium significantly decreased after dissolution treatment using Coca-Cola(®), suggesting a potential contribution of calcium to dissolution mechanisms. Moreover, immersion in Coca-Cola(®) for 120 hours on the exterior surface revealed that Coca-Cola(®) did not permeate persimmon phytobezoars. This is the first study to investigate the mechanisms of persimmon phytobezoar permeability and dissolution induced by Coca-Cola(®).

  2. Disentangling atomic-layer-specific x-ray absorption spectra by Auger electron diffraction spectroscopy

    NASA Astrophysics Data System (ADS)

    Matsui, Fumihiko; Matsushita, Tomohiro; Kato, Yukako; Hashimoto, Mie; Daimon, Hiroshi

    2009-11-01

    In order to investigate the electronic and magnetic structures of each atomic layer at subsurface, we have proposed a new method, Auger electron diffraction spectroscopy, which is the combination of x-ray absorption spectroscopy (XAS) and Auger electron diffraction (AED) techniques. We have measured a series of Ni LMM AED patterns of the Ni film grown on Cu(001) surface for various thicknesses. Then we deduced a set of atomic-layer-specific AED patterns in a numerical way. Furthermore, we developed an algorithm to disentangle XANES spectra from different atomic layers using these atomic-layer-specific AED patterns. Surface and subsurface core level shift were determined for each atomic layer.

  3. High-temperature cuprate superconductors studied by x-ray Compton scattering and positron annihilation spectroscopies

    NASA Astrophysics Data System (ADS)

    Barbiellini, Bernardo

    2013-06-01

    The bulk Fermi surface in an overdoped (x = 0.3) single crystal of La2-xSrxCuO4 has been observed by using x-ray Compton scattering. This momentum density technique also provides a powerful tool for directly seeing what the dopant Sr atoms are doing to the electronic structure of La2CuO4. Because of wave function effects, positron annihilation spectroscopy does not yield a strong signature of the Fermi surface in extended momentum space, but it can be used to explore the role of oxygen defects in the reservoir layers for promoting high temperature superconductivity.

  4. Elucidating light-induced charge accumulation in an artificial analogue of methane monooxygenase enzymes using time-resolved X-ray absorption spectroscopy

    DOE PAGES

    Moonshiram, Dooshaye; Picon, Antonio; Vazquez-Mayagoitia, Alvaro; ...

    2017-02-08

    Here, we report the use of time-resolved X-ray absorption spectroscopy in the ns–μs time scale to track the light induced two electron transfer processes in a multi-component photocatalytic system, consisting of [Ru(bpy) 3] 2+/ a diiron(III,III) model/triethylamine. EXAFS analysis with DFT calculations confirms the structural configurations of the diiron(III,III) and reduced diiron(II,II) states.

  5. Elucidating light-induced charge accumulation in an artificial analogue of methane monooxygenase enzymes using time-resolved X-ray absorption spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Moonshiram, Dooshaye; Picon, Antonio; Vazquez-Mayagoitia, Alvaro

    Here, we report the use of time-resolved X-ray absorption spectroscopy in the ns–μs time scale to track the light induced two electron transfer processes in a multi-component photocatalytic system, consisting of [Ru(bpy) 3] 2+/ a diiron(III,III) model/triethylamine. EXAFS analysis with DFT calculations confirms the structural configurations of the diiron(III,III) and reduced diiron(II,II) states.

  6. A sealable ultrathin window sample cell for the study of liquids by means of soft X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Grötzsch, D.; Streeck, C.; Nietzold, C.; Malzer, W.; Mantouvalou, I.; Nutsch, A.; Dietrich, P.; Unger, W.; Beckhoff, B.; Kanngießer, B.

    2017-12-01

    A new sample cell concept for the analysis of liquids or solid-liquid interfaces using soft X-ray spectroscopy is presented, which enables the complete sealing of the cell as well as the transport into vacuum via, for example, a load-lock system. The cell uses pressure monitoring and active as well as passive pressure regulation systems, thereby facilitating the full control over the pressure during filling, sealing, evacuation, and measurement. The cell design and sample preparation as well as the crucial sealing procedure are explained in detail. As a first proof-of-principle experiment, successful nitrogen K-edge fluorescence yield near-edge X-ray absorption fine structure experiments of a biomolecular solution are presented. For this purpose, it is shown that the careful evaluation of all involved parameters, such as window type or photon flux, is desirable for optimizing the experimental result.

  7. Development of a micro-X-ray fluorescence system based on polycapillary X-ray optics for non-destructive analysis of archaeological objects

    NASA Astrophysics Data System (ADS)

    Cheng, Lin; Ding, Xunliang; Liu, Zhiguo; Pan, Qiuli; Chu, Xuelian

    2007-08-01

    A new micro-X-ray fluorescence (micro-XRF) system based on rotating anode X-ray generator and polycapillary X-ray optics has been set up in XOL Lab, BNU, China, in order to be used for analysis of archaeological objects. The polycapillary X-ray optics used here can focus the primary X-ray beam down to tens of micrometers in diameter that allows for non-destructive and local analysis of sub-mm samples with minor/trace level sensitivity. The analytical characteristics and potential of this micro-XRF system in archaeological research are discussed. Some described uses of this instrument include studying Chinese ancient porcelain.

  8. Observational techniques for solar flare gamma-rays, hard X-rays, and neutrons

    NASA Technical Reports Server (NTRS)

    Lin, Robert P.

    1989-01-01

    The development of new instrumentation and techniques for solar hard X-ray, gamma ray and neutron observations from spacecraft and/or balloon-borne platforms is examined. The principal accomplishments are: (1) the development of a two segment germanium detector which is near ideal for solar hard X-ray and gamma ray spectroscopy; (2) the development of long duration balloon flight techniques and associated instrumentation; and (3) the development of innovative new position sensitive detectors for hard X-ray and gamma rays.

  9. 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

  10. Bright Linearly and Circularly Polarized Extreme Ultraviolet and Soft X-ray High Harmonics for Absorption Spectroscopy

    NASA Astrophysics Data System (ADS)

    Fan, Tingting

    High harmonic generation (HHG) is an extreme nonlinear optical process. When implemented in a phase-matched geometry, HHG coherent upconverts femtosecond laser light into coherent "X-ray laser" beams, while retaining excellent spatial and temporal coherence, as well as the polarization state of the driving laser. HHG has a tabletop footprint, with femtosecond to attosecond time resolution, combined with nanometer spatial resolution. As a consequence of these unique capabilities, HHG is now being widely adopted for use in molecular spectroscopy and imaging, materials science, as well as nanoimaging in general. In the first half of this thesis, I demonstrate high flux linearly polarized soft X-ray HHG, driven by a single-stage 10-mJ Ti:sapphire regenerative amplifier at a repetition rate of 1 kHz. I first down-converted the laser to 1.3 mum using an optical parametric amplifier, before up-converting it into the soft X-ray region using HHG in a high-pressure, phase-matched, hollow waveguide geometry. The resulting optimally phase-matched broadband spectrum extends to 200 eV, with a soft X-ray photon flux of > 106 photons/pulse/1% bandwidth at 1 kHz, corresponding to > 109 photons/s/1% bandwidth, or approximately a three orders-of-magnitude increase compared with past work. Using this broad bandwidth X-ray source, I demonstrated X-ray absorption spectroscopy of multiple elements and transitions in molecules in a single spectrum, with a spectral resolution of 0.25 eV, and with the ability to resolve the near edge fine structure. In the second half of this thesis, I discuss how to generate the first bright circularly polarized (CP) soft X-ray HHG and also use them to implement the first tabletop X-ray magnetic circular dichroism (XMCD) measurements. Using counter-rotating CP lasers at 1.3 mum and 0.79 mum, I generated CPHHG with photon energies exceeding 160 eV. The harmonic spectra emerge as a sequence of closely spaced pairs of left and right CP peaks, with energies

  11. 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.

  12. X-ray And EUV Spectroscopy Of Highly Charged Tungsten Ions

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Biedermann, Christoph; Radtke, Rainer

    2009-09-10

    The Berlin EBIT has been established by the Max-Planck-Institut fuer Plasmaphysik to generate atomic physics data in support of research in the field of controlled nuclear fusion, by measuring the radiation from highly charged ions in the x-ray, extreme ultraviolet and visible spectral ranges and providing valuable diagnostics for high temperature plasmas. In future fusion devices, for example ITER, currently being constructed at Cadarache, France, the plasma facing components will be armored with high-Z materials, most likely tungsten, due to the favorable properties of this element. At the same time the tremendous radiation cooling of these high-Z materials represents amore » threat to fusion and obliges one to monitor carefully the radiation. With EBIT a selected ensemble of ions in specific charge states can be produced, stored and excited for spectroscopic investigations. Employing this technique, we have for example resolved the wide structure observed around 5 nm at the ASDEX Upgrade tokamak as originating from E1-transitions into the open 4d shell of tungsten ions in charge states 25+ to 37+ producing a band-like emission pattern. Further, these ions emit well-separated M1 lines in the EUV range around 65 nm suitable for plasma diagnostics. Kr-like to Cr-like tungsten ions (38+ to 50+) show strong soft-x-ray lines in the range 0.5 to 2 and 5 to 15 nm. Lines of even higher charged tungsten ions, up to Ne-like W{sup 64+}, abundant in the core plasma of present and future fusion test devices, have been investigated with high resolution Bragg-crystal spectroscopy at 0.13 nm. Recently, x-ray spectroscopic measurements of the dielectronic recombination LMn resonances of W{sup 60+} to W{sup 67+} ions have been preformed and compare well with atomic structure calculations.« less

  13. Markov Chain Monte Carlo Joint Analysis of Chandra X-Ray Imaging Spectroscopy and Sunyaev-Zel'dovich Effect Data

    NASA Technical Reports Server (NTRS)

    Bonamente, Massimillano; Joy, Marshall K.; Carlstrom, John E.; Reese, Erik D.; LaRoque, Samuel J.

    2004-01-01

    X-ray and Sunyaev-Zel'dovich effect data can be combined to determine the distance to galaxy clusters. High-resolution X-ray data are now available from Chandra, which provides both spatial and spectral information, and Sunyaev-Zel'dovich effect data were obtained from the BIMA and Owens Valley Radio Observatory (OVRO) arrays. We introduce a Markov Chain Monte Carlo procedure for the joint analysis of X-ray and Sunyaev- Zel'dovich effect data. The advantages of this method are the high computational efficiency and the ability to measure simultaneously the probability distribution of all parameters of interest, such as the spatial and spectral properties of the cluster gas and also for derivative quantities such as the distance to the cluster. We demonstrate this technique by applying it to the Chandra X-ray data and the OVRO radio data for the galaxy cluster A611. Comparisons with traditional likelihood ratio methods reveal the robustness of the method. This method will be used in follow-up paper to determine the distances to a large sample of galaxy cluster.

  14. Quaternary ammonium oxidative demethylation: X-ray crystallographic, resonance Raman, and UV-visible spectroscopic analysis of a Rieske-type demethylase.

    PubMed

    Daughtry, Kelly D; Xiao, Youli; Stoner-Ma, Deborah; Cho, Eunsun; Orville, Allen M; Liu, Pinghua; Allen, Karen N

    2012-02-08

    Herein, the structure resulting from in situ turnover in a chemically challenging quaternary ammonium oxidative demethylation reaction was captured via crystallographic analysis and analyzed via single-crystal spectroscopy. Crystal structures were determined for the Rieske-type monooxygenase, stachydrine demethylase, in the unliganded state (at 1.6 Å resolution) and in the product complex (at 2.2 Å resolution). The ligand complex was obtained from enzyme aerobically cocrystallized with the substrate stachydrine (N,N-dimethylproline). The ligand electron density in the complex was interpreted as proline, generated within the active site at 100 K by the absorption of X-ray photon energy and two consecutive demethylation cycles. The oxidation state of the Rieske iron-sulfur cluster was characterized by UV-visible spectroscopy throughout X-ray data collection in conjunction with resonance Raman spectra collected before and after diffraction data. Shifts in the absorption band wavelength and intensity as a function of absorbed X-ray dose demonstrated that the Rieske center was reduced by solvated electrons generated by X-ray photons; the kinetics of the reduction process differed dramatically for the liganded complex compared to unliganded demethylase, which may correspond to the observed turnover in the crystal.

  15. 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

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

    DOE PAGES

    Ye, Yifan; Kawase, Ayako; Song, Min-Kyu; ...

    2016-01-11

    The X-ray absorption spectroscopy technique has been applied to study different stages of the lithium/sulfur (Li/S) cell life cycle. We investigated how speciation of S in Li/S cathodes changes upon the introduction of CTAB (cetyltrimethylammonium bromide, CH 3(CH 2) 15N+(CH 3) 3Br₋) and with charge/discharge cycling. The introduction of CTAB changes the synthesis reaction pathway dramatically due to the interaction of CTAB with the terminal S atoms of the polysulfide ions in the Na 2S x solution. For the cycled Li/S cell, the loss of electrochemically active sulfur and the accumulation of a compact blocking insulating layer of unexpected sulfurmore » reaction products on the cathode surface during the charge/discharge processes make the capacity decay. Lastly, a modified coin cell and a vacuum-compatible three-electrode electro-chemical cell have been introduced for further in-situ/in-operando studies.« less

  17. Simultaneous broadband observations and high-resolution X-ray spectroscopy of the transitional millisecond pulsar PSR J1023+0038

    NASA Astrophysics Data System (ADS)

    Coti Zelati, F.; Campana, S.; Braito, V.; Baglio, M. C.; D'Avanzo, P.; Rea, N.; Torres, D. F.

    2018-03-01

    We report on the first simultaneous XMM-Newton, NuSTAR, and Swift observations of the transitional millisecond pulsar PSR J1023+0038 in the X-ray active state. Our multi-wavelength campaign allowed us to investigate with unprecedented detail possible spectral variability over a broad energy range in the X-rays, as well as correlations and lags among emissions in different bands. The soft and hard X-ray emissions are significantly correlated, with no lags between the two bands. On the other hand, the X-ray emission does not correlate with the UV emission. We refine our model for the observed mode switching in terms of rapid transitions between a weak propeller regime and a rotation-powered radio pulsar state, and report on a detailed high-resolution X-ray spectroscopy using all XMM-Newton Reflection Grating Spectrometer data acquired since 2013. We discuss our results in the context of the recent discoveries on the system and of the state of the art simulations on transitional millisecond pulsars, and show how the properties of the narrow emission lines in the soft X-ray spectrum are consistent with an origin within the accretion disc.

  18. An x-ray absorption spectroscopy study of Ni-Mn-Ga shape memory alloys.

    PubMed

    Sathe, V G; Dubey, Aditi; Banik, Soma; Barman, S R; Olivi, L

    2013-01-30

    The austenite to martensite phase transition in Ni-Mn-Ga ferromagnetic shape memory alloys was studied by extended x-ray absorption fine structure (EXAFS) and x-ray absorption near-edge structure (XANES) spectroscopy. The spectra at all the three elements', namely, Mn, Ga and Ni, K-edges in several Ni-Mn-Ga samples (with both Ni and Mn excess) were analyzed at room temperature and low temperatures. The EXAFS analysis suggested a displacement of Mn and Ga atoms in opposite direction with respect to the Ni atoms when the compound transforms from the austenite phase to the martensite phase. The first coordination distances around the Mn and Ga atoms remained undisturbed on transition, while the second and subsequent shells showed dramatic changes indicating the presence of a modulated structure. The Mn rich compounds showed the presence of antisite disorder of Mn and Ga. The XANES results showed remarkable changes in the unoccupied partial density of states corresponding to Mn and Ni, while the electronic structure of Ga remained unperturbed across the martensite transition. The post-edge features in the Mn K-edge XANES spectra changed from a double peak like structure to a flat peak like structure upon phase transition. The study establishes strong correlation between the crystal structure and the unoccupied electronic structure in these shape memory alloys.

  19. Angularly resolved X-ray photoelectron spectroscopy investigation of PTFE after prolonged space exposure

    NASA Technical Reports Server (NTRS)

    Dalins, I.; Karimi, M.

    1992-01-01

    Monochromatized angularly resolved X-ray photoelectron spectroscopy (ARXPS) was used to study PTFE (Teflon) that had been exposed to an earth orbital environment for approximately six years. The primary interest of the research is on a very reactive component of this environment (atomic oxygen) which, because of the typical orbital velocities of a spacecraft, impinge on exposed surfaces with 5 eV energy. This presentation deals with the method of analysis, the findings as they pertain to a rather complex carbon, oxygen, and fluorine XPS peak analysis, and the character of the valence bands. An improved bias referencing method, based on ARXPS, is also demonstrated for evaluating specimen charging effects. It was found that the polymer molecule tends to resist the atomic oxygen attack by reorienting itself, so that the most electronegative CF3 groups are facing the incoming hyperthermal oxygen atoms. The implications of these findings to ground-based laboratory studies are discussed.

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

    DOE PAGES

    Wright, Joshua T.; Su, Dong; van Buuren, Tony; ...

    2014-08-21

    Here, 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. 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 anmore » octahedrally coordinated (impurity) phase. With decreasing particle sizes, the impurity phase increases, suggesting that small QDs can be difficult to dope.« less

  1. Electromagnetic diagnostics of ECR-Ion Sources plasmas: optical/X-ray imaging and spectroscopy

    NASA Astrophysics Data System (ADS)

    Mascali, D.; Castro, G.; Altana, C.; Caliri, C.; Mazzaglia, M.; Romano, F. P.; Leone, F.; Musumarra, A.; Naselli, E.; Reitano, R.; Torrisi, G.; Celona, L.; Cosentino, L. G.; Giarrusso, M.; Gammino, S.

    2017-12-01

    Magnetoplasmas in ECR-Ion Sources are excited from gaseous elements or vapours by microwaves in the range 2.45-28 GHz via Electron Cyclotron Resonance. A B-minimum, magnetohydrodynamic stable configuration is used for trapping the plasma. The values of plasma density, temperature and confinement times are typically ne= 1011-1013 cm-3, 01 eVX-ray domain. Fast Silicon Drift detectors with high energy resolution of 125 eV at 5.9 keV have been used for the characterization of plasma emission at 02X-ray pin-hole camera technique has allowed space resolved X-ray spectroscopy with a spatial resolution down to 30 μm and an energy resolution down to 140 eV at 5.9 keV . In parallel, imaging in the optical range and spectroscopic measurements have been carried out. Relative abundances of H/H2 atoms/molecules in the plasmas have been measured for different values of neutral pressure, microwave power and magnetic field profile (they are critical for high-power proton sources).

  2. On the Electronic Structure of Cu Chlorophyllin and Its Breakdown Products: A Carbon K-Edge X-ray Absorption Spectroscopy Study.

    PubMed

    Witte, Katharina; Mantouvalou, Ioanna; Sánchez-de-Armas, Rocío; Lokstein, Heiko; Lebendig-Kuhla, Janina; Jonas, Adrian; Roth, Friedrich; Kanngießer, Birgit; Stiel, Holger

    2018-02-15

    Using near-edge X-ray absorption fine structure (NEXAFS) spectroscopy, the carbon backbone of sodium copper chlorophyllin (SCC), a widely used chlorophyll derivative, and its breakdown products are analyzed to elucidate their electronic structure and physicochemical properties. Using various sample preparation methods and complementary spectroscopic methods (including UV/Vis, X-ray photoelectron spectroscopy), a comprehensive insight into the SCC breakdown process is presented. The experimental results are supported by density functional theory calculations, allowing a detailed assignment of characteristic NEXAFS features to specific C bonds. SCC can be seen as a model system for the large group of porphyrins; thus, this work provides a novel and detailed description of the electronic structure of the carbon backbone of those molecules and their breakdown products. The achieved results also promise prospective optical pump/X-ray probe investigations of dynamic processes in chlorophyll-containing photosynthetic complexes to be analyzed more precisely.

  3. High-Resolution Detector For X-Ray Diffraction

    NASA Technical Reports Server (NTRS)

    Carter, Daniel C.; Withrow, William K.; Pusey, Marc L.; Yost, Vaughn H.

    1988-01-01

    Proposed x-ray-sensitive imaging detector offers superior spatial resolution, counting-rate capacity, and dynamic range. Instrument based on laser-stimulated luminescence and reusable x-ray-sensitive film. Detector scans x-ray film line by line. Extracts latent image in film and simultaneously erases film for reuse. Used primarily for protein crystallography. Principle adapted to imaging detectors for electron microscopy and fluorescence spectroscopy and general use in astronomy, engineering, and medicine.

  4. High resolution X- and gamma-ray spectroscopy of solar flares

    NASA Technical Reports Server (NTRS)

    Lin, R. P.

    1984-01-01

    A balloon-borne X- and gamma-ray instrument was developed, fabricated, and flown. This instrument has the highest energy resolution of any instrument flown to date for measurements of solar and cosmic X-ray and gamma-ray emission in the 13 to 600 keV energy range. The purpose of the solar measurements was to study electron acceleration and solar flare energy release processes. The cosmic observations were to search for cyclotron line features from neutron stars and for low energy gamma-ray lines from nucleosynthesis. The instrument consists of four 4 cm diameter, 1.3 cm thick, planar intrinsic germanium detectors cooled by liquid nitrogen and surrounded by CsI and NaI anti-coincidence scintillation crystals. A graded z collimator limited the field of view to 3 deg x 6 deg and a gondola pointing system provided 0.3 deg pointing accuracy. A total of four flights were made with this instrument. Additional funding was obtained from NSF for the last three flights, which had primarily solar objectives. A detailed instrument description is given. The main scientific results and the data analysis are discussed. Current work and indications for future work are summarized. A bibliography of publications resulting from this work is given.

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

    PubMed Central

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

    2010-01-01

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

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

    PubMed

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

    2014-12-11

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

  7. X-ray Fluorescence Spectroscopy: the Potential of Astrophysics-developed Techniques

    NASA Astrophysics Data System (ADS)

    Elvis, M.; Allen, B.; Hong, J.; Grindlay, J.; Kraft, R.; Binzel, R. P.; Masterton, R.

    2012-12-01

    X-ray fluorescence from the surface of airless bodies has been studied since the Apollo X-ray fluorescence experiment mapped parts of the lunar surface in 1971-1972. That experiment used a collimated proportional counter with a resolving power of ~1 and a beam size of ~1degree. Filters separated only Mg, Al and SI lines. We review progress in X-ray detectors and imaging for astrophysics and show how these advances enable much more powerful use of X-ray fluorescence for the study of airless bodies. Astrophysics X-ray instrumentation has developed enormously since 1972. Low noise, high quantum efficiency, X-ray CCDs have flown on ASCA, XMM-Newton, the Chandra X-ray Observatory, Swift and Suzaku, and are the workhorses of X-ray astronomy. They normally span 0.5 to ~8 keV with an energy resolution of ~100 eV. New developments in silicon based detectors, especially individual pixel addressable devices, such as CMOS detectors, can withstand many orders of magnitude more radiation than conventional CCDs before degradation. The capability of high read rates provides dynamic range and temporal resolution. Additionally, the rapid read rates minimize shot noise from thermal dark current and optical light. CMOS detectors can therefore run at warmer temperatures and with ultra-thin optical blocking filters. Thin OBFs mean near unity quantum efficiency below 1 keV, thus maximizing response at the C and O lines.such as CMOS detectors, promise advances. X-ray imaging has advanced similarly far. Two types of imager are now available: specular reflection and coded apertures. X-ray mirrors have been flown on the Einstein Observatory, XMM-Newton, Chandra and others. However, as X-ray reflection only occurs at small (~1degree) incidence angles, which then requires long focal lengths (meters), mirrors are not usually practical for planetary missions. Moreover the field of view of X-ray mirrors is comparable to the incident angle, so can only image relatively small regions. More useful

  8. 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

  9. X-ray Diffraction Gratings for Astrophysics

    NASA Astrophysics Data System (ADS)

    Paerels, Frits

    2010-12-01

    Over the past year, we have celebrated the tenth anniversary of the Chandra and XMM-Newton X-ray observatories. Both carry powerful, novel diffraction grating spectrometers, which have opened true X-ray spectroscopy for astrophysics. I will describe the design and operation of these instruments, as the background to some of the beautiful results they have produced. But these designs do not exhaust the versatility and essential simplicity of diffraction grating spectrometers, and I will discuss applications for the International X-ray Observatory IXO.

  10. Argon content of the Martian atmosphere at the Viking 1 landing site - Analysis by X-ray fluorescence spectroscopy

    NASA Technical Reports Server (NTRS)

    Clark, B. C.; Toulmin, P., III; Rose, H. J., Jr.; Baird, A. K.; Keil, K.

    1976-01-01

    Spectra provided by the Viking 1 X-ray fluorescence spectrometer operating in the calibration mode (without a soil sample in the analysis chamber) were analyzed to determine the argon content of the Martian atmosphere at the landing site. This was found to be less than or equal to 0.15 millibar, or not more than 2% by volume, consistent with data obtained by the entry mass spectrometer and by the mass spectrometer on the lander. It is anticipated that analysis of the K content of surface samples using X-ray fluorescence data will provide information on the evolution of the atmosphere, since most atmospheric argon is apparently produced by decay of K-40.

  11. Combining theory and experiment for X-ray absorption spectroscopy and resonant X-ray scattering characterization of polymers

    DOE PAGES

    Su, Gregory M.; Cordova, Isvar A.; Brady, Michael A.; ...

    2016-07-04

    We present that an improved understanding of fundamental chemistry, electronic structure, morphology, and dynamics in polymers and soft materials requires advanced characterization techniques that are amenable to in situ and operando studies. Soft X-ray methods are especially useful in their ability to non-destructively provide information on specific materials or chemical moieties. Analysis of these experiments, which can be very dependent on X-ray energy and polarization, can quickly become complex. Complementary modeling and predictive capabilities are required to properly probe these critical features. Here, we present relevant background on this emerging suite of techniques. Finally, we focus on how the combinationmore » of theory and experiment has been applied and can be further developed to drive our understanding of how these methods probe relevant chemistry, structure, and dynamics in soft materials.« less

  12. 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.

  13. Nonresonant valence-to-core x-ray emission spectroscopy of niobium

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Ravel, Bruce; Kropf, A. Jeremy; Yang, Dali

    The valence-to-core (V2C) portion of x-ray emission spectroscopy (XES) measures the electron states close to the Fermi level. These states are involved in bonding, thus providing a measure of the chemistry of the material. For this paper, we show the V2C XES spectra for several niobium compounds. The Kβ" peak in the V2C XES results from the transition of a ligand 2s electron into the 1s core-hole of the niobium, a transition allowed by hybridization with the niobium 4p . This location in energy of this weak peak shows a strong ligand dependence, thus providing a sensitive probe of themore » ligand environment about the niobium.« less

  14. Nonresonant valence-to-core x-ray emission spectroscopy of niobium

    DOE PAGES

    Ravel, Bruce; Kropf, A. Jeremy; Yang, Dali; ...

    2018-03-23

    The valence-to-core (V2C) portion of x-ray emission spectroscopy (XES) measures the electron states close to the Fermi level. These states are involved in bonding, thus providing a measure of the chemistry of the material. For this paper, we show the V2C XES spectra for several niobium compounds. The Kβ" peak in the V2C XES results from the transition of a ligand 2s electron into the 1s core-hole of the niobium, a transition allowed by hybridization with the niobium 4p . This location in energy of this weak peak shows a strong ligand dependence, thus providing a sensitive probe of themore » ligand environment about the niobium.« less

  15. Biological X-ray absorption spectroscopy (BioXAS): a valuable tool for the study of trace elements in the life sciences.

    PubMed

    Strange, Richard W; Feiters, Martin C

    2008-10-01

    Using X-ray absorption spectroscopy (XAS) the binding modes (type and number of ligands, distances and geometry) and oxidation states of metals and other trace elements in crystalline as well as non-crystalline samples can be revealed. The method may be applied to biological systems as a 'stand-alone' technique, but it is particularly powerful when used alongside other X-ray and spectroscopic techniques and computational approaches. In this review, we highlight how biological XAS is being used in concert with crystallography, spectroscopy and computational chemistry to study metalloproteins in crystals, and report recent applications on relatively rare trace elements utilised by living organisms and metals involved in neurodegenerative diseases.

  16. 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.

  17. The Athena X-ray Integral Field Unit (X-IFU)

    NASA Astrophysics Data System (ADS)

    Pajot, F.; Barret, D.; Lam-Trong, T.; den Herder, J.-W.; Piro, L.; Cappi, M.; Huovelin, J.; Kelley, R.; Mas-Hesse, J. M.; Mitsuda, K.; Paltani, S.; Rauw, G.; Rozanska, A.; Wilms, J.; Barbera, M.; Douchin, F.; Geoffray, H.; den Hartog, R.; Kilbourne, C.; Le Du, M.; Macculi, C.; Mesnager, J.-M.; Peille, P.

    2018-04-01

    The X-ray Integral Field Unit (X-IFU) of the Advanced Telescope for High-ENergy Astrophysics (Athena) large-scale mission of ESA will provide spatially resolved high-resolution X-ray spectroscopy from 0.2 to 12 keV, with 5^' ' } pixels over a field of view of 5 arc minute equivalent diameter and a spectral resolution of 2.5 eV (FWHM) up to 7 keV. The core scientific objectives of Athena drive the main performance parameters of the X-IFU. We present the current reference configuration of the X-IFU, and the key issues driving the design of the instrument.

  18. X-ray photoemission study of NiS2-xSex (x=0.0 1.2)

    NASA Astrophysics Data System (ADS)

    Krishnakumar, S. R.; Sarma, D. D.

    2003-10-01

    Electronic structure of NiS2-xSex system has been investigated for various compositions (x) using x-ray photoemission spectroscopy. An analysis of the core-level as well as the valence-band spectra of NiS2 in conjunction with many-body cluster calculations provides a quantitative description of the electronic structure of this compound. With increasing Se content, the on-site Coulomb correlation strength (U) does not change, while the bandwidth W of the system increases, driving the system from a covalent insulating state to a pd-metallic state.

  19. CAT-ACT-A new highly versatile x-ray spectroscopy beamline for catalysis and radionuclide science at the KIT synchrotron light facility ANKA.

    PubMed

    Zimina, A; Dardenne, K; Denecke, M A; Doronkin, D E; Huttel, E; Lichtenberg, H; Mangold, S; Pruessmann, T; Rothe, J; Spangenberg, Th; Steininger, R; Vitova, T; Geckeis, H; Grunwaldt, J-D

    2017-11-01

    CAT-ACT-the hard X-ray beamline for CATalysis and ACTinide/radionuclide research at the KIT synchrotron radiation facility ANKA-is dedicated to X-ray spectroscopy, including "flux hungry" photon-in/photon-out and correlative techniques and combines state-of-the-art optics with a unique infrastructure for radionuclide and catalysis research. Measurements can be performed at photon energies varying between 3.4 keV and 55 keV, thus encompassing the actinide M- and L-edge or potassium K-edge up to the K-edges of the lanthanide series such as cerium. Well-established X-ray absorption fine structure spectroscopy in transmission and fluorescence detection modes is available in combination with high energy-resolution X-ray emission spectroscopy or X-ray diffraction techniques. The modular beamline design with two alternately operated in-line experimental stations enables sufficient flexibility to adapt sample environments and detection systems to many scientific challenges. The ACT experimental station focuses on various aspects of nuclear waste disposal within the mission of the Helmholtz association to contribute to the solution of one of the greatest scientific and social challenges of our time-the safe disposal of heat producing, highly radioactive waste forms from nuclear energy production. It augments present capabilities at the INE-Beamline by increasing the flux and extending the energy range into the hard X-ray regime. The CAT experimental station focuses on catalytic materials, e.g., for energy-related and exhaust gas catalysis. Characterization of catalytically active materials under realistic reaction conditions and the development of in situ and operando cells for sample environments close to industrial reactors are essential aspects at CAT.

  20. CAT-ACT—A new highly versatile x-ray spectroscopy beamline for catalysis and radionuclide science at the KIT synchrotron light facility ANKA

    NASA Astrophysics Data System (ADS)

    Zimina, A.; Dardenne, K.; Denecke, M. A.; Doronkin, D. E.; Huttel, E.; Lichtenberg, H.; Mangold, S.; Pruessmann, T.; Rothe, J.; Spangenberg, Th.; Steininger, R.; Vitova, T.; Geckeis, H.; Grunwaldt, J.-D.

    2017-11-01

    CAT-ACT—the hard X-ray beamline for CATalysis and ACTinide/radionuclide research at the KIT synchrotron radiation facility ANKA—is dedicated to X-ray spectroscopy, including "flux hungry" photon-in/photon-out and correlative techniques and combines state-of-the-art optics with a unique infrastructure for radionuclide and catalysis research. Measurements can be performed at photon energies varying between 3.4 keV and 55 keV, thus encompassing the actinide M- and L-edge or potassium K-edge up to the K-edges of the lanthanide series such as cerium. Well-established X-ray absorption fine structure spectroscopy in transmission and fluorescence detection modes is available in combination with high energy-resolution X-ray emission spectroscopy or X-ray diffraction techniques. The modular beamline design with two alternately operated in-line experimental stations enables sufficient flexibility to adapt sample environments and detection systems to many scientific challenges. The ACT experimental station focuses on various aspects of nuclear waste disposal within the mission of the Helmholtz association to contribute to the solution of one of the greatest scientific and social challenges of our time—the safe disposal of heat producing, highly radioactive waste forms from nuclear energy production. It augments present capabilities at the INE-Beamline by increasing the flux and extending the energy range into the hard X-ray regime. The CAT experimental station focuses on catalytic materials, e.g., for energy-related and exhaust gas catalysis. Characterization of catalytically active materials under realistic reaction conditions and the development of in situ and operando cells for sample environments close to industrial reactors are essential aspects at CAT.

  1. Analysis of solar X-ray data

    NASA Technical Reports Server (NTRS)

    Teske, R. G.

    1972-01-01

    Type III solar bursts occurring in the absence of solar flares were observed to be accompanied by weak X-radiation. The energy scale of an OSO-3 soft X-ray ion chamber was assessed using realistic theoretical X-ray spectra. Relationships between soft solar X-rays and solar activity were investigated. These included optical studies, the role of the Type III acceleration mechanism in establishing the soft X-ray source volume, H alpha flare intensity variations, and gross magnetic field structure.

  2. Bismuth@US-tubes as a Potential Contrast Agent for X-ray Imaging Applications

    PubMed Central

    Rivera, Eladio J.; Tran, Lesa A.; Hernández-Rivera, Mayra; Yoon, Diana; Mikos, Antonios G.; Rusakova, Irene A.; Cheong, Benjamin Y.; Cabreira-Hansen, Maria da Graça; Willerson, James T.; Perin, Emerson C.; Wilson, Lon J.

    2013-01-01

    The encapsulation of bismuth as BiOCl/Bi2O3 within ultra-short (ca. 50 nm) single-walled carbon nanocapsules (US-tubes) has been achieved. The Bi@US-tubes have been characterized by high-resolution transmission electron microscopy (HR-TEM), energy-dispersive X-ray spectroscopy (EDS), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy. Bi@US-tubes have been used for intracellular labeling of pig bone marrow-derived mesenchymal stem cells (MSCs) to show high X-ray contrast in computed tomography (CT) cellular imaging for the first time. The relatively high contrast is achieved with low bismuth loading (2.66% by weight) within the US-tubes and without compromising cell viability. X-ray CT imaging of Bi@US-tubes-labeled MSCs showed a nearly two-fold increase in contrast enhancement when compared to unlabeled MSCs in a 100 kV CT clinical scanner. The CT signal enhancement from the Bi@US-tubes is 500 times greater than polymer-coated Bi2S3 nanoparticles and several-fold that of any clinical iodinated contrast agent (CA) at the same concentration. Our findings suggest that the Bi@US-tubes can be used as a potential new class of X-ray CT agent for stem cell labeling and possibly in vivo tracking. PMID:24288589

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

    PubMed

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

    1997-01-01

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

  4. Probing the CZTS/CdS heterojunction utilizing photoelectrochemistry and x-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Turnbull, Matthew J.; Vaccarello, Daniel; Wong, Jonathan; Yiu, Yun Mui; Sham, Tsun-Kong; Ding, Zhifeng

    2018-04-01

    The importance of renewable resources is becoming more and more influential on research due to the depletion of fossil fuels. Cost-effective ways of harvesting solar energy should also be at the forefront of these investigations. Cu2ZnSnS4 (CZTS) solar cells are well within the frame of these goals, and a thorough understanding of how they are made and processed synthetically is crucial. The CZTS/CdS heterojunction was examined using photoelectrochemistry and synchrotron radiation (SR) spectroscopy. These tools provided physical insights into this interface that was formed by the electrophoretic deposition of CZTS nanocrystals and chemical bath deposition (CBD) of CdS for the respective films. It was discovered that CBD induced a change in the local and long range environment of the Zn in the CZTS lattice, which was detrimental to the photoresponse. X-ray absorption near-edge structures and extended X-ray absorption fine structures (EXAFSs) of the junction showed that this change was at an atomic level and was associated with the coordination of oxygen to zinc. This was confirmed through FEFF fitting of the EXAFS and through IR spectroscopy. It was found that this change in both photoresponse and the Zn coordination can be reversed with the use of low temperature annealing. Investigating CZTS through SR techniques provides detailed structural information of minor changes from the zinc perspective.

  5. Preferred site occupation of 3 d atoms in NixF e4 -xN (x =1 and 3) films revealed by x-ray absorption spectroscopy and magnetic circular dichroism

    NASA Astrophysics Data System (ADS)

    Takata, Fumiya; Ito, Keita; Takeda, Yukiharu; Saitoh, Yuji; Takanashi, Koki; Kimura, Akio; Suemasu, Takashi

    2018-02-01

    X-ray absorption spectroscopy (XAS) and x-ray magnetic circular dichroism measurements were performed at the Ni and Fe L2 ,3 absorption edges for N ixF e4 -xN (x =1 and 3) epitaxial films. Spectral line-shape analysis and element-specific magnetic moment evaluations are presented. Shoulders at approximately 2 eV above the Ni L2 ,3 main peaks in the XAS spectrum of N i3FeN were interpreted to originate from hybridization of orbitals between Ni 3 d at face-centered (II) sites and N 2 p at body-centered sites, while such features were missing in NiF e3N film. Similar shoulders were observed at Fe L2 ,3 edges in both films. These results indicate that the orbitals of Ni atoms did not hybridize with those of N atoms in the NiF e3N film. Hence, Ni atoms preferentially occupied corner (I) sites, where the hybridization was weak because of the relatively long distance between Ni at I sites and N atoms. The relatively large magnetic moment deduced from sum-rule analysis of NiF e3N also showed a good agreement with the presence of Ni atoms at I sites.

  6. X-ray Absorption Spectroscopy Study of the Effect of Rh doping in Sr2IrO4

    PubMed Central

    Sohn, C. H.; Cho, Deok-Yong; Kuo, C.-T.; Sandilands, L. J.; Qi, T. F.; Cao, G.; Noh, T. W.

    2016-01-01

    We investigate the effect of Rh doping in Sr2IrO4 using X-ray absorption spectroscopy (XAS). We observed appearance of new electron-addition states with increasing Rh concentration (x in Sr2Ir1−xRhxO4) in accordance with the concept of hole doping. The intensity of the hole-induced state is however weak, suggesting weakness of charge transfer (CT) effect and Mott insulating ground states. Also, Ir Jeff = 1/2 upper Hubbard band shifts to lower energy as x increases up to x = 0.23. Combined with optical spectroscopy, these results suggest a hybridisation-related mechanism, in which Rh doping can weaken the (Ir Jeff = 1/2)–(O 2p) orbital hybridisation in the in-planar Rh-O-Ir bond networks. PMID:27025538

  7. X-Ray Spectral Diagnostics of Gamma-Ray Burst Environments.

    PubMed

    Paerels; Kuulkers; Heise; Liedahl

    2000-05-20

    Recently, detection of discrete features in the X-ray afterglow spectra of GRB 970508 and GRB 970828 was reported. The most natural interpretation of these features is that they are redshifted Fe K emission complexes. The identification of the line emission mechanism has drastic implications for the inferred mass of radiating material and hence the nature of the burst site. X-ray spectroscopy provides a direct observational constraint on these properties of gamma-ray bursters. We briefly discuss how these constraints arise in the context of an application to the spectrum of GRB 970508.

  8. The X-ray Absorber in the X-ray Transient NLS1 WPVS 007

    NASA Astrophysics Data System (ADS)

    Grupe, Dirk

    This proposal is for a funding request for an approved XMM-Newton observations of the X-ray transient Narrow-Line Seyfert 1 galaxy WPVS 007. The request is for 4 month of salary for the PI for one year in order to do the data analysis, publish the results, and attend an international AGN meeting. XMM will observe WPVS 007 in June 2010 simultaneously with HST, Chandra, and Swift. The goal is to establish a tight connection between the UV broad absorption line troughs found in FUSE observations and the strong partial covering absorber feature found by Swift. WPVS 007 showed a dramatic transformation into a Broad Absorption line QSO like AGN between a 1996 HST observation and a 2003 FUSE observation. Several Swift monitoring observations have suggested that the absorber may have started to disappear. Therefore it is crucial for our HST COS UV spectroscopy to know what the status of the X-ray absorber is. The XMM observation will provide a well-exposed X-ray spectrum even if WPVS 007 will be in a low flux state. This spectrum will enable us to put constraints on the absorption column density and covering fraction of the partial covering absorber.

  9. X-ray verification of an optically aligned off-plane grating module

    NASA Astrophysics Data System (ADS)

    Donovan, Benjamin D.; McEntaffer, Randall L.; Tutt, James H.; DeRoo, Casey T.; Allured, Ryan; Gaskin, Jessica A.; Kolodziejczak, Jeffery J.

    2018-01-01

    Off-plane x-ray reflection gratings are theoretically capable of achieving high resolution and high diffraction efficiencies over the soft x-ray bandpass, making them an ideal technology to implement on upcoming x-ray spectroscopy missions. To achieve high effective area, these gratings must be aligned into grating modules. X-ray testing was performed on an aligned grating module to assess the current optical alignment methods. Results indicate that the grating module achieved the desired alignment for an upcoming x-ray spectroscopy suborbital rocket payload with modest effective area and resolving power. These tests have also outlined a pathway towards achieving the stricter alignment tolerances of future x-ray spectrometer payloads, which require improvements in alignment metrology, grating fabrication, and testing techniques.

  10. Towards ultrafast dynamics with split-pulse X-ray photon correlation spectroscopy at free electron laser sources

    DOE PAGES

    Roseker, W.; Hruszkewycz, S. O.; Lehmkuhler, F.; ...

    2018-04-27

    One of the important challenges in condensed matter science is to understand ultrafast, atomic-scale fluctuations that dictate dynamic processes in equilibrium and non-equilibrium materials. Here, we report an important step towards reaching that goal by using a state-of-the-art perfect crystal based split-and-delay system, capable of splitting individual X-ray pulses and introducing femtosecond to nanosecond time delays. We show the results of an ultrafast hard X-ray photon correlation spectroscopy experiment at LCLS where split X-ray pulses were used to measure the dynamics of gold nanoparticles suspended in hexane. We show how reliable speckle contrast values can be extracted even from verymore » low intensity free electron laser (FEL) speckle patterns by applying maximum likelihood fitting, thus demonstrating the potential of a split-and-delay approach for dynamics measurements at FEL sources. This will enable the characterization of equilibrium and, importantly also reversible non-equilibrium processes in atomically disordered materials.« less

  11. Towards ultrafast dynamics with split-pulse X-ray photon correlation spectroscopy at free electron laser sources

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Roseker, W.; Hruszkewycz, S. O.; Lehmkuhler, F.

    One of the important challenges in condensed matter science is to understand ultrafast, atomic-scale fluctuations that dictate dynamic processes in equilibrium and non-equilibrium materials. Here, we report an important step towards reaching that goal by using a state-of-the-art perfect crystal based split-and-delay system, capable of splitting individual X-ray pulses and introducing femtosecond to nanosecond time delays. We show the results of an ultrafast hard X-ray photon correlation spectroscopy experiment at LCLS where split X-ray pulses were used to measure the dynamics of gold nanoparticles suspended in hexane. We show how reliable speckle contrast values can be extracted even from verymore » low intensity free electron laser (FEL) speckle patterns by applying maximum likelihood fitting, thus demonstrating the potential of a split-and-delay approach for dynamics measurements at FEL sources. This will enable the characterization of equilibrium and, importantly also reversible non-equilibrium processes in atomically disordered materials.« less

  12. Internal standards in fluorescent X-ray spectroscopy1 1 Publication authorized by the Director, U.S. Geological Survey.

    USGS Publications Warehouse

    Adler, I.; Axelrod, J.M.

    1955-01-01

    The use of internal standards in the analysis of ores and minerals of widely-varying matrix by means of fluorescent X-ray spectroscopy is frequently the most practical approach. Internal standards correct for absorption and enhancement effects except when an absorption edge falls between the comparison lines or a very strong emission line falls between the absorption edges responsible for the comparison lines. Particle size variations may introduce substantial errors. One method of coping with the particle size problem is grinding the sample with an added abrasive. ?? 1955.

  13. Catalysis of GTP Hydrolysis by Small GTPases at Atomic Detail by Integration of X-ray Crystallography, Experimental, and Theoretical IR Spectroscopy*

    PubMed Central

    Rudack, Till; Jenrich, Sarah; Brucker, Sven; Vetter, Ingrid R.; Gerwert, Klaus; Kötting, Carsten

    2015-01-01

    Small GTPases regulate key processes in cells. Malfunction of their GTPase reaction by mutations is involved in severe diseases. Here, we compare the GTPase reaction of the slower hydrolyzing GTPase Ran with Ras. By combination of time-resolved FTIR difference spectroscopy and QM/MM simulations we elucidate that the Mg2+ coordination by the phosphate groups, which varies largely among the x-ray structures, is the same for Ran and Ras. A new x-ray structure of a Ran·RanBD1 complex with improved resolution confirmed this finding and revealed a general problem with the refinement of Mg2+ in GTPases. The Mg2+ coordination is not responsible for the much slower GTPase reaction of Ran. Instead, the location of the Tyr-39 side chain of Ran between the γ-phosphate and Gln-69 prevents the optimal positioning of the attacking water molecule by the Gln-69 relative to the γ-phosphate. This is confirmed in the RanY39A·RanBD1 crystal structure. The QM/MM simulations provide IR spectra of the catalytic center, which agree very nicely with the experimental ones. The combination of both methods can correlate spectra with structure at atomic detail. For example the FTIR difference spectra of RasA18T and RanT25A mutants show that spectral differences are mainly due to the hydrogen bond of Thr-25 to the α-phosphate in Ran. By integration of x-ray structure analysis, experimental, and theoretical IR spectroscopy the catalytic center of the x-ray structural models are further refined to sub-Å resolution, allowing an improved understanding of catalysis. PMID:26272610

  14. Development of a krypton-doped gas symmetry capsule platform for x-ray spectroscopy of implosion cores on the NIF.

    PubMed

    Ma, T; Chen, H; Patel, P K; Schneider, M B; Barrios, M A; Casey, D T; Chung, H-K; Hammel, B A; Berzak Hopkins, L F; Jarrott, L C; Khan, S F; Lahmann, B; Nora, R; Rosenberg, M J; Pak, A; Regan, S P; Scott, H A; Sio, H; Spears, B K; Weber, C R

    2016-11-01

    The electron temperature at stagnation of an ICF implosion can be measured from the emission spectrum of high-energy x-rays that pass through the cold material surrounding the hot stagnating core. Here we describe a platform developed on the National Ignition Facility where trace levels of a mid-Z dopant (krypton) are added to the fuel gas of a symcap (symmetry surrogate) implosion to allow for the use of x-ray spectroscopy of the krypton line emission.

  15. Development of a krypton-doped gas symmetry capsule platform for x-ray spectroscopy of implosion cores on the NIF

    NASA Astrophysics Data System (ADS)

    Ma, T.; Chen, H.; Patel, P. K.; Schneider, M. B.; Barrios, M. A.; Casey, D. T.; Chung, H.-K.; Hammel, B. A.; Berzak Hopkins, L. F.; Jarrott, L. C.; Khan, S. F.; Lahmann, B.; Nora, R.; Rosenberg, M. J.; Pak, A.; Regan, S. P.; Scott, H. A.; Sio, H.; Spears, B. K.; Weber, C. R.

    2016-11-01

    The electron temperature at stagnation of an ICF implosion can be measured from the emission spectrum of high-energy x-rays that pass through the cold material surrounding the hot stagnating core. Here we describe a platform developed on the National Ignition Facility where trace levels of a mid-Z dopant (krypton) are added to the fuel gas of a symcap (symmetry surrogate) implosion to allow for the use of x-ray spectroscopy of the krypton line emission.

  16. 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. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. X-ray absorption fine structure and X-ray excited optical luminescence studies of II-VI semiconducting nanostructures

    NASA Astrophysics Data System (ADS)

    Murphy, Michael Wayne

    2010-06-01

    Various II-VI semiconducting nanomaterials such as ZnO-ZnS nanoribbons (NRs), CdSxSe1-x nanostructures, ZnS:Mn NRs, ZnS:Mn,Eu nanoprsims (NPs), ZnO:Mn nanopowders, and ZnO:Co nanopowders were synthesized for study. These materials were characterized by techniques such as scanning electron microscopy, transmission electron microscopy, element dispersive X-ray spectroscopy, selected area electron diffraction, and X-ray diffraction. The electronic and optical properties of these nanomaterials were studied by X-ray absorption fine structure (XAFS) spectroscopy and X-ray excited optical luminescence (XEOL) techniques, using tuneable soft X-rays from a synchrotron light source. The complementary nature ofthe XAFS and XEOL techniques give site, element and chemical specific measurements which allow a better understanding of the interplay and role of each element in the system. Chemical vapour deposition (CVD) of ZnS powder in a limited oxygen environment resulted in side-by-side biaxial ZnO-ZnS NR heterostructures. The resulting NRs contained distinct wurtzite ZnS and wurtzite ZnO components with widths of 10--100 nm and 20 --500 nm, respectively and a uniform interface region of 5-15 nm. XAFS and XEOL measurements revealed the luminescence of ZnO-ZnS NRs is from the ZnO component. The luminescence of CdSxSe1-x nanostructures is shown to be dependent on the S to Se ratio, with the band-gap emission being tunable between that of pure CdS and CdSe. Excitation of the CdSxSe 1-x nanostructures by X-ray in XEOL has revealed new de-excitation channels which show a defect emission band not seen by laser excitation. CVD of Mn2+ doped ZnS results in nanostructures with luminescence dominated by the yellow Mn2+ emission due to energy transfer from the ZnS host to the Mn dopant sites. The addition of EuCl3 to the reactants in the CVD process results in a change in morphology from NR to NP. Zn1-xMnxO and Zn1-xCOxO nanopowders were prepared by sol-gel methods at dopant concentrations

  18. X-ray induced dimerization of cinnamic acid: Time-resolved inelastic X-ray scattering study

    NASA Astrophysics Data System (ADS)

    Inkinen, Juho; Niskanen, Johannes; Talka, Tuomas; Sahle, Christoph J.; Müller, Harald; Khriachtchev, Leonid; Hashemi, Javad; Akbari, Ali; Hakala, Mikko; Huotari, Simo

    2015-11-01

    A classic example of solid-state topochemical reactions is the ultraviolet-light induced photodimerization of α-trans-cinnamic acid (CA). Here, we report the first observation of an X-ray-induced dimerization of CA and monitor it in situ using nonresonant inelastic X-ray scattering spectroscopy (NRIXS). The time-evolution of the carbon core-electron excitation spectra shows the effects of two X-ray induced reactions: dimerization on a short time-scale and disintegration on a long time-scale. We used spectrum simulations of CA and its dimerization product, α-truxillic acid (TA), to gain insight into the dimerization effects. From the time-resolved spectra, we extracted component spectra and time-dependent weights corresponding to CA and TA. The results suggest that the X-ray induced dimerization proceeds homogeneously in contrast to the dimerization induced by ultraviolet light. We also utilized the ability of NRIXS for direct tomography with chemical-bond contrast to image the spatial progress of the reactions in the sample crystal. Our work paves the way for other time-resolved studies on chemical reactions using inelastic X-ray scattering.

  19. The soft x-ray beamline at Frascati Labs

    NASA Astrophysics Data System (ADS)

    Cinque, Gianfelice; Burattini, Emilio; Grilli, Antonio; Dabagov, Sultan

    2005-08-01

    DAΦNE-Light is the Synchrotron Radiation laboratory at the Laboratori Nazionali di Frascati (LNF)1. Three beamlines were commissioned since spring 2003 to exploit parasitically the intense photon emission from DAΦNE, the 0.5 1 GeV storage ring routinely circulating over 1 A of electrons. The soft X-ray beamline utilizes a wiggler source and, by a double-crystal fixed-exit monochromator, it is operational in the distinguishing energy window 1.5 - 4 keV range to be extended from the "water window" toward 6 keV. At present, the research activity is focused on X-ray Absorption Spectroscopy (XAS): precisely, X-ray Absorption Near Edge Spectroscopy (XANES) on the inner electronic levels of light elements and transition metals from Al to Ge and both d- and f-shells of higher Z atoms. Preliminary tests of X-ray imaging have been performed in view of applying different focusing optics, namely policapillary systems in trasmission and/or bent mica diffractor in back-reflection, for X-ray microscopy and spectromicroscopy experiments. The use of polycapillary systems (lenses, halflenses, capillaries) for studying features of radiation transportation by such structures (X-ray channelling, focusing, bending, etc.) has been planned.

  20. HIGH-RESOLUTION X-RAY SPECTROSCOPY REVEALS THE SPECIAL NATURE OF WOLF-RAYET STAR WINDS

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Oskinova, L. M.; Hamann, W.-R.; Gayley, K. G.

    We present the first high-resolution X-ray spectrum of a putatively single Wolf-Rayet (WR) star. 400 ks observations of WR 6 by the XMM-Newton telescope resulted in a superb quality high-resolution X-ray spectrum. Spectral analysis reveals that the X-rays originate far out in the stellar wind, more than 30 stellar radii from the photosphere, and thus outside the wind acceleration zone where the line-driving instability (LDI) could create shocks. The X-ray emitting plasma reaches temperatures up to 50 MK and is embedded within the unshocked, 'cool' stellar wind as revealed by characteristic spectral signatures. We detect a fluorescent Fe line atmore » Almost-Equal-To 6.4 keV. The presence of fluorescence is consistent with a two-component medium, where the cool wind is permeated with the hot X-ray emitting plasma. The wind must have a very porous structure to allow the observed amount of X-rays to escape. We find that neither the LDI nor any alternative binary scenario can explain the data. We suggest a scenario where X-rays are produced when the fast wind rams into slow 'sticky clumps' that resist acceleration. Our new data show that the X-rays in single WR star are generated by some special mechanism different from the one operating in the O-star winds.« less

  1. X-Tip: a New Tool for Nanoscience or How to Combine X-Ray Spectroscopies to Local Probe Analysis

    NASA Astrophysics Data System (ADS)

    Olivier, Dhez; Mario, Rodrigues; Fabio, Comin; Roberto, Felici; Joel, Chevrier

    2007-01-01

    With the advent of nanoscale science, the need of tools able to image samples and bring the region of interest to the X-ray beam is essential. We show the possibility of using the high resolution imaging capability of a scanning probe microscope to image and align a sample relative to the X-ray beam, as well as the possibility to record the photoelectrons emitted by the sample.

  2. Water analysis via portable X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Pearson, Delaina; Chakraborty, Somsubhra; Duda, Bogdan; Li, Bin; Weindorf, David C.; Deb, Shovik; Brevik, Eric; Ray, D. P.

    2017-01-01

    Rapid, in-situ elemental water analysis would be an invaluable tool in studying polluted and/or salt-impacted waters. Analysis of water salinity has commonly used electrical conductance (EC); however, the identity of the elements responsible for the salinity are not revealed using EC. Several studies have established the viability of using portable X-ray fluorescence (PXRF) spectrometry for elemental data analysis of soil, sediment, and other matrices. However, the accuracy of PXRF is known to be affected while scanning moisture-laden soil samples. This study used PXRF elemental data in water samples to predict water EC. A total of 256 water samples, from 10 different countries were collected and analyzed via PXRF, inductively coupled plasma atomic emission spectroscopy (ICP-AES), and a digital salinity bridge. The PXRF detected some elements more effectively than others, but overall results indicated that PXRF can successfully predict water EC via quantifying Cl in water samples (validation R2 and RMSE of 0.77 and 0.95 log μS cm-1, respectively). The findings of this study elucidated the potential of PXRF for future analysis of pollutant and/or metal contaminated waters.

  3. p-Type dopant incorporation and surface charge properties of catalyst-free GaN nanowires revealed by micro-Raman scattering and X-ray photoelectron spectroscopy.

    PubMed

    Wang, Q; Liu, X; Kibria, M G; Zhao, S; Nguyen, H P T; Li, K H; Mi, Z; Gonzalez, T; Andrews, M P

    2014-09-07

    Micro-Raman scattering and X-ray photoelectron spectroscopy were employed to investigate Mg-doped GaN nanowires. With the increase of Mg doping level, pronounced Mg-induced local vibrational modes were observed. The evolution of longitudinal optical phonon-plasmon coupled mode, together with detailed X-ray photoelectron spectroscopy studies, show that the near-surface region of nanowires can be transformed from weakly n-type to p-type with the increase of Mg doping.

  4. X-ray Photoelectron Spectroscopy Analysis of Gold Surfaces after Removal of Thiolated DNA Oligomers by Ultraviolet/Ozone Treatment

    PubMed Central

    Mirsaleh-Kohan, Nasrin; Bass, Andrew D.; Sanche, Léon

    2012-01-01

    Well ordered films of molecular DNA can be formed by the attachment of thiolated DNA oligonucleotides to a supporting gold substrate. The gold substrate represents a significant fraction of the total cost of preparing such films and it is thus important to determine whether such substrates can be reused. Here we investigate with X-ray Photoelectron Spectroscopy the suitability of UV/ozonolysis previously employed to remove alkanethiols from gold, for removing 40-mer, single and double stranded synthetic DNA. We find that while UV/O3 can indeed remove thiolated DNA from gold slides, the treatment times required permit the implantation of additional organic contaminants. PMID:20000594

  5. X-ray photoelectron spectroscopy analysis of gold surfaces after removal of thiolated DNA oligomers by ultraviolet/ozone treatment.

    PubMed

    Mirsaleh-Kohan, Nasrin; Bass, Andrew D; Sanche, Léon

    2010-05-04

    Well-ordered films of molecular DNA can be formed by the attachment of thiolated DNA oligonucleotides to a supporting gold substrate. The gold substrate represents a significant fraction of the total cost of preparing such films, and it is thus important to determine whether such substrates can be reused. Here, we investigate with X-ray photoelectron spectroscopy the suitability of UV/ozonolysis previously employed to remove alkanethiols from gold, for removing 40-mer, single- and double-stranded synthetic DNA. We find that while UV/O(3) can indeed remove thiolated DNA from gold slides, the treatment times required permit the implantation of additional organic contaminants.

  6. An X-ray absorption spectroscopy study of the inversion degree in zinc ferrite nanocrystals dispersed on a highly porous silica aerogel matrix.

    PubMed

    Carta, D; Marras, C; Loche, D; Mountjoy, G; Ahmed, S I; Corrias, A

    2013-02-07

    The structural properties of zinc ferrite nanoparticles with spinel structure dispersed in a highly porous SiO(2) aerogel matrix were compared with a bulk zinc ferrite sample. In particular, the details of the cation distribution between the octahedral (B) and tetrahedral (A) sites of the spinel structure were determined using X-ray absorption spectroscopy. The analysis of both the X-ray absorption near edge structure and the extended X-ray absorption fine structure indicates that the degree of inversion of the zinc ferrite spinel structures varies with particle size. In particular, in the bulk microcrystalline sample, Zn(2+) ions are at the tetrahedral sites and trivalent Fe(3+) ions occupy octahedral sites (normal spinel). When particle size decreases, Zn(2+) ions are transferred to octahedral sites and the degree of inversion is found to increase as the nanoparticle size decreases. This is the first time that a variation of the degree of inversion with particle size is observed in ferrite nanoparticles grown within an aerogel matrix.

  7. Lu.sub.1-xI.sub.3:Ce.sub.x--a scintillator for gamma ray spectroscopy and time-of-flight PET

    DOEpatents

    Shah, Kanai S.

    2007-02-06

    The present invention concerns very fast scintillator materials comprising lutetium iodide doped with Cerium (Lu.sub.1-xI.sub.3:Ce.sub.x; LuI.sub.3:Ce). The LuI.sub.3 scintillator material has surprisingly good characteristics including high light output, high gamma ray stopping efficiency, fast response, low cost, good proportionality, and minimal afterglow that the material is useful for gamma ray spectroscopy, medical imaging, nuclear and high energy physics research, diffraction, non-destructive testing, nuclear treaty verification and safeguards, and geological exploration. The timing resolution of the scintillators of the present invention provide compositions capable of resolving the position of an annihilation event within a portion of a human body cross-section.

  8. Innovative diffraction gratings for high-resolution resonant inelastic soft x-ray scattering spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Voronov, D.L.; Warwick, T.; Gullikson, E. M.

    2016-07-27

    High-resolution Resonant Inelastic X-ray Scattering (RIXS) requires diffraction gratings with very exacting characteristics. The gratings should provide both very high dispersion and high efficiency which are conflicting requirements and extremely challenging to satisfy in the soft x-ray region for a traditional grazing incidence geometry. To achieve high dispersion one should increase the groove density of a grating; this however results in a diffraction angle beyond the critical angle range and results in drastic efficiency loss. The problem can be solved by use of multilayer coated blazed gratings (MBG). In this work we have investigated the diffraction characteristics of MBGs viamore » numerical simulations and have developed a procedure for optimization of grating design for a multiplexed high resolution imaging spectrometer for RIXS spectroscopy to be built in sector 6 at the Advanced Light Source (ALS). We found that highest diffraction efficiency can be achieved for gratings optimized for 4{sup th} or 5{sup th} order operation. Fabrication of such gratings is an extremely challenging technological problem. We present a first experimental prototype of these gratings and report its performance. High order and high line density gratings have the potential to be a revolutionary new optical element that should have great impact in the area of soft x-ray RIXS.« less

  9. X-Ray Calorimeter Arrays for Astrophysics

    NASA Technical Reports Server (NTRS)

    Kilbourne, Caroline A.

    2009-01-01

    High-resolution x-ray spectroscopy is a powerful tool for studying the evolving universe. The grating spectrometers on the XMM and Chandra satellites started a new era in x-ray astronomy, but there remains a need for instrumentation that can provide higher spectral resolution with high throughput in the Fe-K band (around 6 keV) and can enable imaging spectroscopy of extended sources, such as supernova remnants and galaxy clusters. The instrumentation needed is a broad-band imaging spectrometer - basically an x-ray camera that can distinguish tens of thousands of x-ray colors. The potential benefits to astrophysics of using a low-temperature calorimeter to determine the energy of an incident x-ray photon via measurement of a small change in temperature was first articulated by S. H. Moseley over two decades ago. In the time since, technological progress has been steady, though full realization in an orbiting x-ray telescope is still awaited. A low-temperature calorimeter can be characterized by the type of thermometer it uses, and three types presently dominate the field. The first two types are temperature-sensitive resistors - semiconductors in the metal-insulator transition and superconductors operated in the superconducting-normal transition. The third type uses a paramagnetic thermometer. These types can be considered the three generations of x-ray calorimeters; by now each has demonstrated a resolving power of 2000 at 6 keV, but only a semiconductor calorimeter system has been developed to spaceflight readiness. The Soft X-ray Spectrometer on Astro-H, expected to launch in 2013, will use an array of silicon thermistors with I-IgTe x-ray absorbers that will operate at 50 mK. Both the semiconductor and superconductor calorimeters have been implemented in small arrays, kilo-pixel arrays of the superconducting calorimeters are just now being produced, and it is anticipated that much larger arrays will require the non-dissipative advantage of magnetic thermometers.

  10. Origin of Pressure-induced Superconducting Phase in KxFe2-ySe2 studied by Synchrotron X-ray Diffraction and Spectroscopy

    NASA Astrophysics Data System (ADS)

    Yamamoto, Yoshiya; Yamaoka, Hitoshi; Tanaka, Masashi; Okazaki, Hiroyuki; Ozaki, Toshinori; Takano, Yoshihiko; Lin, Jung-Fu; Fujita, Hidenori; Kagayama, Tomoko; Shimizu, Katsuya; Hiraoka, Nozomu; Ishii, Hirofumi; Liao, Yen-Fa; Tsuei, Ku-Ding; Mizuki, Jun'Ichiro

    2016-08-01

    Pressure dependence of the electronic and crystal structures of KxFe2-ySe2, which has pressure-induced two superconducting domes of SC I and SC II, was investigated by x-ray emission spectroscopy and diffraction. X-ray diffraction data show that compressibility along the c-axis changes around 12 GPa, where a new superconducting phase of SC II appears. This suggests a possible tetragonal to collapsed tetragonal phase transition. X-ray emission spectroscopy data also shows the change in the electronic structure around 12 GPa. These results can be explained by the scenario that the two SC domes under pressure originate from the change of Fermi surface topology. Our results here show the pronounced increase of the density of states near the Fermi surface under pressure with a structural phase transition, which can help address our fundamental understanding for the appearance of the SC II phase.

  11. X-ray photoelectron spectroscopy analysis for the chemical impact of solvent addition rate on electromagnetic shielding effectiveness of HCl-doped polyaniline nanopowders

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Tantawy, Hesham Ramzy; Aston, D. Eric, E-mail: aston@uidaho.edu; Kengne, Blaise-Alexis F.

    2015-11-07

    An in-depth analysis of the chemical functionality in HCl-doped polyaniline (PANI) nanopowders is discussed through interpretations of x-ray photoelectron spectra. The distinctions between three PANI sample types, produced under varied synthesis conditions, are compared on the basis correlations between newly collected electron spectra for chemical analysis (or also x-ray photoelectron spectroscopy) and electromagnetic (EM) shielding effectiveness (SE) within two frequency bands (100–1500 MHz and ∼2–14 GHz). The findings are discussed with reference to previous data analysis of electrical conductivities and Raman and UV-vis spectra analyzed from replicates of the same PANI nanopowders, where only the 8–12 GHz range for SE was tested.more » They further corroborate previous results for limited-solvent conditions that enhance EM shielding. The three nanopowder types show distinctive differences in polaron, bipolaron, and polar lattice contributions. The collective findings describe the chemical connections between controlling and, most importantly, limiting the available solvent for polymerization with simultaneously doping and how it is that the newly developed solvent-limited approach for HCl-PANI nanopowders provides better shielding than traditionally solvent-rich methods by having more extended and perhaps even faster polaron delocalization than other PANI-based products. The maximum oxidation (50%) and doping (49%) levels obtained in the solvent-free nanopowders also produced the highest SE values of 37.3 ± 3.7 dB (MHz band) and 68.6 ± 4.6 dB (GHz band)« less

  12. SMART-X: Square Meter, Arcsecond Resolution Telescope for X-rays

    NASA Astrophysics Data System (ADS)

    Vikhlinin, Alexey; SMART-X Collaboration

    2013-04-01

    SMART-X is a concept for a next-generation X-ray observatory with large-area, 0.5" angular resolution grazing incidence adjustable X-ray mirrors, high-throughput critical angle transmission gratings, and X-ray microcalorimeter and CMOS-based imager in the focal plane. High angular resolution is enabled by new technology based on controlling the shape of mirror segments using thin film piezo actuators deposited on the back surface. Science applications include observations of growth of supermassive black holes since redshifts of ~10, ultra-deep surveys over 10's of square degrees, galaxy assembly at z=2-3, as well as new opportunities in the high-resolution X-ray spectroscopy and time domains. We also review the progress in technology development, tests, and mission design over the past year.

  13. In Situ X-ray Absorption Near-Edge Structure Spectroscopy of ZnO Nanowire Growth During Chemical Bath Deposition

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    McPeak, Kevin M.; Becker, Matthew A.; Britton, Nathan G.

    2010-12-03

    Chemical bath deposition (CBD) offers a simple and inexpensive route to deposit semiconductor nanostructures, but lack of fundamental understanding and control of the underlying chemistry has limited its versatility. Here we report the first use of in situ X-ray absorption spectroscopy during CBD, enabling detailed investigation of both reaction mechanisms and kinetics of ZnO nanowire growth from zinc nitrate and hexamethylenetetramine (HMTA) precursors. Time-resolved X-ray absorption near-edge structure (XANES) spectra were used to quantify Zn(II) speciation in both solution and solid phases. ZnO crystallizes directly from [Zn(H{sub 2}O){sub 6}]{sup 2+} without long-lived intermediates. Using ZnO nanowire deposition as an example,more » this study establishes in situ XANES spectroscopy as an excellent quantitative tool to understand CBD of nanomaterials.« less

  14. Catalysts at work: From integral to spatially resolved X-ray absorption spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Grunwaldt, Jan-Dierk; Kimmerle, Bertram; Baiker, Alfons

    2009-09-25

    Spectroscopic studies on heterogeneous catalysts have mostly been done in an integral mode. However, in many cases spatial variations in catalyst structure can occur, e.g. during impregnation of pre-shaped particles, during reaction in a catalytic reactor, or in microstructured reactors as the present overview shows. Therefore, spatially resolved molecular information on a microscale is required for a comprehensive understanding of theses systems, partly in ex situ studies, partly under stationary reaction conditions and in some cases even under dynamic reaction conditions. Among the different available techniques, X-ray absorption spectroscopy (XAS) is a well-suited tool for this purpose as the differentmore » selected examples highlight. Two different techniques, scanning and full-field X-ray microscopy/tomography, are described and compared. At first, the tomographic structure of impregnated alumina pellets is presented using full-field transmission microtomography and compared to the results obtained with a scanning X-ray microbeam technique to analyse the catalyst bed inside a catalytic quartz glass reactor. On the other hand, by using XAS in scanning microtomography, the structure and the distribution of Cu(0), Cu(I), Cu(II) species in a Cu/ZnO catalyst loaded in a quartz capillary microreactor could be reconstructed quantitatively on a virtual section through the reactor. An illustrating example for spatially resolved XAS under reaction conditions is the partial oxidation of methane over noble metal-based catalysts. In order to obtain spectroscopic information on the spatial variation of the oxidation state of the catalyst inside the reactor XAS spectra were recorded by scanning with a micro-focussed beam along the catalyst bed. Alternatively, full-field transmission imaging was used to efficiently determine the distribution of the oxidation state of a catalyst inside a reactor under reaction conditions. The new technical approaches together with

  15. Monitoring long-range electron transfer pathways in proteins by stimulated attosecond broadband X-ray Raman spectroscopy

    DOE PAGES

    Zhang, Yu; Biggs, Jason D.; Govind, Niranjan; ...

    2014-10-09

    In this study, long-range electron transfer (ET) plays a key role in many biological energy conversion and synthesis processes. We show that nonlinear spectroscopy with attosecond X-ray pulses provides a real time movie of the evolving oxidation states and electron densities around atoms, and can probe these processes with high spatial and temporal resolution. This is demonstrated in a simulation study of the stimulated X-ray Raman (SXRS) signals in Re-modified azurin, which had long served as a benchmark for long-range ET in proteins. Nonlinear SXRS signals are sensitive to the local electronic structure and should offer a novel window formore » long-range ET.« less

  16. 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.

  17. Feasibility study of total reflection X-ray fluorescence analysis using a liquid metal jet X-ray tube

    NASA Astrophysics Data System (ADS)

    Maderitsch, A.; Smolek, S.; Wobrauschek, P.; Streli, C.; Takman, P.

    2014-09-01

    Total reflection X-ray spectroscopy (TXRF) is a powerful analytical technique for qualitative and quantitative analysis of trace and ultratrace elements in a sample with lower limits of detection (LLDs) of pg/g to ng/g in concentration and absolute high fg levels are attainable. Several X-ray sources, from low power (few W), 18 kW rotating anodes to synchrotron radiation, are in use for the excitation and lead accordingly to their photon flux delivered on the sample the detection limits specified. Not only the power, but also the brilliance and focal shape are of importance for TXRF. A microfocus of 50-100 μm spot size or the line focus of diffraction tubes is best suited. Excillum developed a new approach in the design of a source: the liquid metal jet anode. In this paper the results achieved with this source are described. A versatile TXRF spectrometer with vacuum chamber designed at Atominstitut was used for the experiments. A multilayer monochromator selecting the intensive Ga-Kα radiation was taken and the beam was collimated by 50 μm slits. Excellent results regarding geometric beam stability, high fluorescence intensities and low background were achieved leading to detection limits in the high fg range for Ni. A 100 mm2 silicon drift detector (SDD) collimated to 80 mm2 was used to collect the fluorescence radiation. The results from measurements on single element samples are presented.

  18. Molybdenum X-Ray Absorption Edges from 200 – 20,000 eV, The Benefits of Soft X-Ray Spectroscopy for Chemical Speciation

    PubMed Central

    George, Simon J.; Drury, Owen B.; Fu, Juxia; Friedrich, Stephan; Doonan, Christian J.; George, Graham N.; White, Jonathan M.; Young, Charles G.; Cramer, Stephen P.

    2009-01-01

    We have surveyed the chemical utility of the near-edge structure of molybdenum x-ray absorption edges from the hard x-ray K-edge at 20,000 eV down to the soft x-ray M4,5-edges at ~230 eV. We compared, for each edge, the spectra of two tetrahedral anions, MoO4 and MoS42-. We used three criteria for assessing near-edge structure of each edge: (i) the ratio of the observed chemical shift between MoO42- and MoS42- and the linewidth, (ii) the chemical information from analysis of the near-edge structure and (iii) the ease of measurement using fluorescence detection. Not surprisingly, the K-edge was by far the easiest to measure, but it contained the least information. The L2,3-edges, although harder to measure, had benefits with regard to selection rules and chemical speciation in that they had both a greater chemical shift as well as detailed lineshapes which could be theoretically analyzed in terms of Mo ligand field, symmetry, and covalency. The soft x-ray M2,3-edges were perhaps the least useful, in that they were difficult to measure using fluorescence detection and had very similar information content to the corresponding L2,3-edges. Interestingly, the soft x-ray, low energy (~230 eV) M4,5-edges had greatest potential chemical sensitivity and using our high resolution superconducting tunnel junction (STJ) fluorescence detector they appear to be straightforward to measure. The spectra were amenable to analysis using both the TT-multiplet approach and FEFF. The results using FEFF indicate that the sharp near-edge peaks arise from 3d → 5p transitions, while the broad edge structure has predominately 3d → 4f character. A proper understanding of the dependence of these soft x-ray spectra on ligand field and site geometry is necessary before a complete assessment of the utility of the Mo M4,5-edges can be made. This work includes crystallographic characterization of sodium tetrathiomolybdate. PMID:19041140

  19. Soft x-ray absorption spectroscopy of metalloproteins and high-valent metal-complexes at room temperature using free-electron lasers

    PubMed Central

    Kubin, Markus; Kern, Jan; Gul, Sheraz; Kroll, Thomas; Chatterjee, Ruchira; Löchel, Heike; Fuller, Franklin D.; Sierra, Raymond G.; Quevedo, Wilson; Weniger, Christian; Rehanek, Jens; Firsov, Anatoly; Laksmono, Hartawan; Weninger, Clemens; Alonso-Mori, Roberto; Nordlund, Dennis L.; Lassalle-Kaiser, Benedikt; Glownia, James M.; Krzywinski, Jacek; Moeller, Stefan; Turner, Joshua J.; Minitti, Michael P.; Dakovski, Georgi L.; Koroidov, Sergey; Kawde, Anurag; Kanady, Jacob S.; Tsui, Emily Y.; Suseno, Sandy; Han, Zhiji; Hill, Ethan; Taguchi, Taketo; Borovik, Andrew S.; Agapie, Theodor; Messinger, Johannes; Erko, Alexei; Föhlisch, Alexander; Bergmann, Uwe; Mitzner, Rolf; Yachandra, Vittal K.; Yano, Junko; Wernet, Philippe

    2017-01-01

    X-ray absorption spectroscopy at the L-edge of 3d transition metals provides unique information on the local metal charge and spin states by directly probing 3d-derived molecular orbitals through 2p-3d transitions. However, this soft x-ray technique has been rarely used at synchrotron facilities for mechanistic studies of metalloenzymes due to the difficulties of x-ray-induced sample damage and strong background signals from light elements that can dominate the low metal signal. Here, we combine femtosecond soft x-ray pulses from a free-electron laser with a novel x-ray fluorescence-yield spectrometer to overcome these difficulties. We present L-edge absorption spectra of inorganic high-valent Mn complexes (Mn ∼ 6–15 mmol/l) with no visible effects of radiation damage. We also present the first L-edge absorption spectra of the oxygen evolving complex (Mn4CaO5) in Photosystem II (Mn < 1 mmol/l) at room temperature, measured under similar conditions. Our approach opens new ways to study metalloenzymes under functional conditions. PMID:28944255

  20. Soft x-ray absorption spectroscopy of metalloproteins and high-valent metal-complexes at room temperature using free-electron lasers

    DOE PAGES

    Kubin, Markus; Kern, Jan; Gul, Sheraz; ...

    2017-09-01

    X-ray absorption spectroscopy at the L-edge of 3d transition metals provides unique information on the local metal charge and spin states by directly probing 3d-derived molecular orbitals through 2p-3d transitions. But, this soft x-ray technique has been rarely used at synchrotron facilities for mechanistic studies of metalloenzymes due to the difficulties of x-ray-induced sample damage and strong background signals from light elements that can dominate the low metal signal. Here, we combine femtosecond soft x-ray pulses from a free-electron laser with a novel x-ray fluorescence-yield spectrometer to overcome these difficulties. We present L-edge absorption spectra of inorganic high-valent Mn complexesmore » (Mn ~ 6-15 mmol/l) with no visible effects of radiation damage. We then present the first L-edge absorption spectra of the oxygen evolving complex (Mn 4 CaO 5 ) in Photosystem II (Mn < 1 mmol/l) at room temperature, measured under similar conditions. Our approach opens new ways to study metalloenzymes under functional conditions.« less

  1. Studies by Near Edge X-ray Absorption Spectroscopies of Bonding Dynamics at the Graphene/Guanine Interface - A Proposal for High Mobility, Organic Graphene Field Effect Transistors

    DTIC Science & Technology

    2015-07-01

    AFRL-AFOSR-UK-TR-2015-0034 Studies by Near Edge X-ray Absorption Spectroscopies of Bonding Dynamics at the Graphene /Guanine...Interface – A Proposal for High Mobility, Organic Graphene Field Effect Transistors Eva Campo BANGOR UNIVERSITY COLLEGE ROAD BANGOR...April 2015 4. TITLE AND SUBTITLE Studies by Near Edge X-ray Absorption Spectroscopies of Bonding Dynamics at the Graphene /Guanine Interface - A

  2. Development of a krypton-doped gas symmetry capsule platform for x-ray spectroscopy of implosion cores on the NIF

    DOE PAGES

    Ma, T.; Chen, H.; Patel, P. K.; ...

    2016-08-18

    The electron temperature at stagnation of an ICF implosion can be measured from the emission spectrum of high-energy x-rays that pass through the cold material surrounding the hot stagnating core. We describe a platform developed on the National Ignition Facility where trace levels of a mid-Z dopant (krypton) are added to the fuel gas of a symcap (symmetry surrogate) implosion to allow for the use of x-ray spectroscopy of the krypton line emission.Published by AIP Publishing

  3. Examining the ground layer of St. Anthony from Padua 19th century oil painting by Raman spectroscopy, scanning electron microscopy and X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Vančo, Ľubomír; Kadlečíková, Magdaléna; Breza, Juraj; Čaplovič, Ľubomír; Gregor, Miloš

    2013-01-01

    In this paper we studied the material composition of the ground layer of a neoclassical painting. We used Raman spectroscopy (RS) as a prime method. Thereafter scanning electron microscopy combined with energy dispersive spectroscopy (SEM-EDS) and X-ray powder diffraction (XRD) were employed as complementary techniques. The painting inspected was of the side altar in King St. Stephen's Church in Galanta (Slovakia), signed and dated by Jos. Chr. Mayer 1870. Analysis was carried out on both covered and uncovered ground layers. Four principal compounds (barite, lead white, calcite, dolomite) and two minor compounds (sphalerite, quartz) were identified. This ground composition is consistent with the 19th century painting technique used in Central Europe consisting of white pigments and white fillers. Transformation of lead white occurred under laser irradiation. Subdominant Raman peaks of the components were measured. The observed results elucidate useful partnership of RS and SEM-EDS measurements supported by X-ray powder diffraction as well as possibilities and limitations of non-destructive analysis of covered lower layers by RS.

  4. Next generation of pnCCDs for X-ray spectroscopy and imaging

    NASA Astrophysics Data System (ADS)

    Meidinger, Norbert; Andritschke, Robert; Hälker, Olaf; Hartmann, Robert; Herrmann, Sven; Holl, Peter; Lutz, Gerhard; Kimmel, Nils; Schaller, Gerhard; Schnecke, Martina; Schopper, Florian; Soltau, Heike; Strüder, Lothar

    2006-11-01

    A special type of charge-coupled device, the pnCCD, has been developed in the nineties as focal-plane detector for the X-ray astronomy mission XMM-Newton of the European Space Agency. The pnCCD detector has been in operation since the satellite launch in 1999. It is performing up to date spectroscopy of X-rays in combination with imaging and high time resolution. The excellent performance of the flight camera is still maintained; in particular, the energy resolution has been nearly constant since launch. In order to satisfy the requirements of future X-ray astronomy missions as well as those of ground-based experiments, a new type of pnCCD has been developed. The ‘frame store pnCCD’ shows various optimizations in device design and fabrication process. Devices with up to 256×512 pixels have been fabricated in 2004 and recently tested. Simultaneously, a programmable analog signal processor for the readout of the CCD signals, the DUO CAMEX, has been developed. The readout noise of the new detector has a value of 2 electrons ENC which is less than half of the figure of the XMM-Newton pnCCD. We measured an energy resolution that is close to the theoretical limit given by the Fano noise. In particular the low-energy response of the new devices was substantially improved. The quantum efficiency for X-rays is at least 90% in the entire energy band from 0.3 keV up to 11 keV. This is due to the ultra-thin photon entrance window as well as the full depletion of the 450 μm thick back-illuminated pnCCD. The position resolution is better than the pixel sizes of 75 μm×75 μm or 51 μm×51 μm because the signal charge is spread over up to four pixels which allows a more accurate event position determination. ‘Out of time’ events are substantially reduced to the order of 0.1% by operating the pnCCD in frame store mode. Higher operating temperatures, e.g. -20 °C, are possible due to the smaller thermally generated dark-current level of the new devices and the operation

  5. Ultra-Small-Angle X-ray Scattering – X-ray Photon Correlation Spectroscopy Studies of Incipient Structural Changes in Amorphous Calcium Phosphate Based Dental Composites

    PubMed Central

    Zhang, F.; Allen, A.J.; Levine, L.E.; Espinal, L.; Antonucci, J.M.; Skrtic, D.; O’Donnell, J.N.R.; Ilavsky, J.

    2012-01-01

    The local structural changes in amorphous calcium phosphate (ACP) based dental composites were studied under isothermal conditions using both static, bulk measurement techniques and a recently developed methodology based on combined ultra-small angle X-ray scattering – X-ray photon correlation spectroscopy (USAXS-XPCS), which permits a dynamic approach. While results from conventional bulk measurements do not show clear signs of structural change, USAXS-XPCS results reveal unambiguous evidence for local structural variations on a similar time scale to that of water loss in the ACP fillers. A thermal-expansion based simulation indicates that thermal behavior alone does not account for the observed dynamics. Together, these results suggest that changes in the water content of ACP affect the composite morphology due to changes in ACP structure that occur without an amorphous-to-crystalline conversion. It is also noted that biomedical materials research could benefit greatly from USAXS-XPCS, a dynamic approach. PMID:22374649

  6. Comparison of two portable solid state detectors with an improved collimation and alignment device for mammographic x-ray spectroscopy.

    PubMed

    Bottigli, U; Golosio, B; Masala, G L; Oliva, P; Stumbo, S; Delogu, P; Fantacci, M E; Abbene, L; Fauci, F; Raso, G

    2006-09-01

    We describe a portable system for mammographic x-ray spectroscopy, based on a 2 X 2 X 1 mm3 cadmium telluride (CdTe) solid state detector, that is greatly improved over a similar system based on a 3 X 3 X 2 mm3 cadmium zinc telluride (CZT) solid state detector evaluated in an earlier work. The CdTe system utilized new pinhole collimators and an alignment device that facilitated measurement of mammographic x-ray spectra. Mammographic x-ray spectra acquired by each system were comparable. Half value layer measurements obtained using an ion chamber agreed closely with those derived from the x-ray spectra measured by either detector. The faster electronics and other features of the CdTe detector allowed its use with a larger pinhole collimator than could be used with the CZT detector. Additionally, the improved pinhole collimator and alignment features of the apparatus permitted much more rapid setup for acquisition of x-ray spectra than was possible on the system described in the earlier work. These improvements in detector technology, collimation and ease of alignment, as well as low cost, make this apparatus attractive as a tool for both laboratory research and advanced mammography quality control.

  7. New Worlds / New Horizons Science with an X-ray Astrophysics Probe

    NASA Technical Reports Server (NTRS)

    Smith, Randall K.; Bookbinder, Jay A.; Hornschemeier, Ann E.; Bandler, Simon; Brandt, W. N.; Hughes, John P.; McCammon, Dan; Matsumoto, Hironori; Mushotzky, Richard; Osten, Rachel A.; hide

    2014-01-01

    In 2013 NASA commenced a design study for an X-ray Astrophysics Probe to address the X-ray science goals and program prioritizations of the Decadal Survey New World New Horizons (NWNH) with a cost cap of approximately $1B. Both the NWNH report and 2011 NASA X-ray mission concept study found that high-resolution X-ray spectroscopy performed with an X-ray microcalorimeter would enable the most highly rated NWNH X-ray science. Here we highlight some potential science topics, namely: 1) a direct, strong-field test of General Relativity via the study of accretion onto black holes through relativistic broadened Fe lines and their reverberation in response to changing hard X-ray continuum, 2) understanding the evolution of galaxies and clusters by mapping temperatures, abundances and dynamics in hot gas, 3) revealing the physics of accretion onto stellar-mass black holes from companion stars and the equation of state of neutron stars through timing studies and time-resolved spectroscopy of X-ray binaries and 4) feedback from AGN and star formation shown in galaxy-scale winds and jets. In addition to these high-priority goals, an X-ray astrophysics probe would be a general-purpose observatory that will result in invaluable data for other NWNH topics such as stellar astrophysics, protostars and their impact on protoplanetary systems, X-ray spectroscopy of transient phenomena such as high-z gamma-ray bursts and tidal capture of stars by massive black holes, and searches for dark matter decay.

  8. Incorporation of Trace Elements in Ancient and Modern Human Bone: An X-Ray Absorption Spectroscopy Study

    NASA Astrophysics Data System (ADS)

    Pingitore, N. E.; Cruz-Jimenez, G.; Price, T. D.

    2001-12-01

    X-ray absorption spectroscopy (XAS) affords the opportunity to probe the atomic environment of trace elements in human bone. We are using XAS to investigate the mode(s) of incorporation of Sr, Zn, Pb, and Ba in both modern and ancient (and thus possibly altered) human and animal bone. Because burial and diagenesis may add trace elements to bone, we performed XAS analysis on samples of pristine contemporary and ancient, buried human and animal bone. We assume that deposition of these elements during burial occurs by processes distinct from those in vivo, and this will be reflected in their atomic environments. Archaeologists measure strontium in human and animal bone as a guide to diet. Carnivores show lower Sr/Ca ratios than their herbivore prey due to discrimination against Sr relative to Ca up the food chain. In an initial sample suite no difference was observed between modern and buried bone. Analysis of additional buried samples, using a more sensitive detector, revealed significant differences in the distance to the second and third neighbors of the Sr in some of the buried samples. Distances to the first neighbor, oxygen, were similar in all samples. Zinc is also used in paleo-diet studies. Initial x-ray absorption spectroscopy of a limited suite of bones did not reveal any differences between modern and buried samples. This may reflect the limited number of samples examined or the low levels of Zn in typical aqueous solutions in soils. Signals from barium and lead were too low to record useful XAS spectra. Additional samples will be studied for Zn, Ba, and Pb. We conducted our XAS experiments on beam lines 4-1 and 4-3 at the Stanford Synchrotron Radiation Laboratory. Data were collected in the fluorescence mode, using a Lytle detector and appropriate filter, and a solid state, 13-element Ge-detector.

  9. Advanced X-ray Astrophysics Facility (AXAF): An overview

    NASA Technical Reports Server (NTRS)

    Weisskopf, M. C.; ODell, S. L.; Elsner, R. F.; VanSpeybroeck, L. P.

    1995-01-01

    The Advanced X-ray Astrophysics Facility (AXAF) is the x-ray component of NASA's Great Observatories. To be launched in late 1998, AXAF will provide unprecedented capabilities for high-resolution imaging, spectrometric imaging, and high-resolution disperse spectroscopy, over the x-ray band from about 0.1 keV to 10 keV. With these capabilities, AXAF observations will address many of the outstanding questions in astronomy, astrophysics, and cosmology.

  10. Rapid Mapping of Lithiation Dynamics in Transition Metal Oxide Particles with Operando X-ray Absorption Spectroscopy.

    PubMed

    Nowack, Lea; Grolimund, Daniel; Samson, Vallerie; Marone, Federica; Wood, Vanessa

    2016-02-24

    Since the commercialization of lithium ion batteries (LIBs), layered transition metal oxides (LiMO2, where M = Co, Mn, Ni, or mixtures thereof) have been materials of choice for LIB cathodes. During cycling, the transition metals change their oxidation states, an effect that can be tracked by detecting energy shifts in the X-ray absorption near edge structure (XANES) spectrum. X-ray absorption spectroscopy (XAS) can therefore be used to visualize and quantify lithiation kinetics in transition metal oxide cathodes; however, in-situ measurements are often constrained by temporal resolution and X-ray dose, necessitating compromises in the electrochemistry cycling conditions used or the materials examined. We report a combined approach to reduce measurement time and X-ray exposure for operando XAS studies of lithium ion batteries. A highly discretized energy resolution coupled with advanced post-processing enables rapid yet reliable identification of the oxidation state. A full-field microscopy setup provides sub-particle resolution over a large area of battery electrode, enabling the oxidation state within many transition metal oxide particles to be tracked simultaneously. Here, we apply this approach to gain insights into the lithiation kinetics of a commercial, mixed-metal oxide cathode material, nickel cobalt aluminium oxide (NCA), during (dis)charge and its degradation during overcharge.

  11. Rapid Mapping of Lithiation Dynamics in Transition Metal Oxide Particles with Operando X-ray Absorption Spectroscopy

    PubMed Central

    Nowack, Lea; Grolimund, Daniel; Samson, Vallerie; Marone, Federica; Wood, Vanessa

    2016-01-01

    Since the commercialization of lithium ion batteries (LIBs), layered transition metal oxides (LiMO2, where M = Co, Mn, Ni, or mixtures thereof) have been materials of choice for LIB cathodes. During cycling, the transition metals change their oxidation states, an effect that can be tracked by detecting energy shifts in the X-ray absorption near edge structure (XANES) spectrum. X-ray absorption spectroscopy (XAS) can therefore be used to visualize and quantify lithiation kinetics in transition metal oxide cathodes; however, in-situ measurements are often constrained by temporal resolution and X-ray dose, necessitating compromises in the electrochemistry cycling conditions used or the materials examined. We report a combined approach to reduce measurement time and X-ray exposure for operando XAS studies of lithium ion batteries. A highly discretized energy resolution coupled with advanced post-processing enables rapid yet reliable identification of the oxidation state. A full-field microscopy setup provides sub-particle resolution over a large area of battery electrode, enabling the oxidation state within many transition metal oxide particles to be tracked simultaneously. Here, we apply this approach to gain insights into the lithiation kinetics of a commercial, mixed-metal oxide cathode material, nickel cobalt aluminium oxide (NCA), during (dis)charge and its degradation during overcharge. PMID:26908198

  12. Rapid Mapping of Lithiation Dynamics in Transition Metal Oxide Particles with Operando X-ray Absorption Spectroscopy

    NASA Astrophysics Data System (ADS)

    Nowack, Lea; Grolimund, Daniel; Samson, Vallerie; Marone, Federica; Wood, Vanessa

    2016-02-01

    Since the commercialization of lithium ion batteries (LIBs), layered transition metal oxides (LiMO2, where M = Co, Mn, Ni, or mixtures thereof) have been materials of choice for LIB cathodes. During cycling, the transition metals change their oxidation states, an effect that can be tracked by detecting energy shifts in the X-ray absorption near edge structure (XANES) spectrum. X-ray absorption spectroscopy (XAS) can therefore be used to visualize and quantify lithiation kinetics in transition metal oxide cathodes; however, in-situ measurements are often constrained by temporal resolution and X-ray dose, necessitating compromises in the electrochemistry cycling conditions used or the materials examined. We report a combined approach to reduce measurement time and X-ray exposure for operando XAS studies of lithium ion batteries. A highly discretized energy resolution coupled with advanced post-processing enables rapid yet reliable identification of the oxidation state. A full-field microscopy setup provides sub-particle resolution over a large area of battery electrode, enabling the oxidation state within many transition metal oxide particles to be tracked simultaneously. Here, we apply this approach to gain insights into the lithiation kinetics of a commercial, mixed-metal oxide cathode material, nickel cobalt aluminium oxide (NCA), during (dis)charge and its degradation during overcharge.

  13. The X-Ray Binary Population of the Nearby Dwarf Starburst Galaxy IC 10: Variable and Transient X-Ray Sources

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Laycock, Silas; Cappallo, Rigel; Williams, Benjamin F.

    We have monitored the Cassiopeia dwarf galaxy (IC 10) in a series of 10 Chandra ACIS-S observations to capture its variable and transient X-ray source population, which is expected to be dominated by High Mass X-ray Binaries (HMXBs). We present a sample of 21 X-ray sources that are variable between observations at the 3 σ level, from a catalog of 110 unique point sources. We find four transients (flux variability ratio greater than 10) and a further eight objects with ratios >5. The observations span the years 2003–2010 and reach a limiting luminosity of >10{sup 35} erg s{sup −1}, providingmore » sensitivity to X-ray binaries in IC 10 as well as flare stars in the foreground Milky Way. The nature of the variable sources is investigated from light curves, X-ray spectra, energy quantiles, and optical counterparts. The purpose of this study is to discover the composition of the X-ray binary population in a young starburst environment. IC 10 provides a sharp contrast in stellar population age (<10 My) when compared to the Magellanic Clouds (40–200 My) where most of the known HMXBs reside. We find 10 strong HMXB candidates, 2 probable background Active Galactic Nuclei, 4 foreground flare-stars or active binaries, and 5 not yet classifiable sources. Complete classification of the sample requires optical spectroscopy for radial velocity analysis and deeper X-ray observations to obtain higher S/N spectra and search for pulsations. A catalog and supporting data set are provided.« less

  14. Physics of Accretion in X-Ray Binaries

    NASA Technical Reports Server (NTRS)

    Vrtilek, Saeqa D.

    2004-01-01

    This project consists of several related investigations directed to the study of mass transfer processes in X-ray binaries. Models developed over several years incorporating highly detailed physics will be tested on a balanced mix of existing data and planned observations with both ground and space-based observatories. The extended time coverage of the observations and the existence of {\\it simultaneous} X-ray, ultraviolet, and optical observations will be particularly beneficial for studying the accretion flows. These investigations, which take as detailed a look at the accretion process in X-ray binaries as is now possible, test current models to their limits, and force us to extend them. We now have the ability to do simultaneous ultraviolet/X-ray/optical spectroscopy with HST, Chandra, XMM, and ground-based observatories. The rich spectroscopy that these Observations give us must be interpreted principally by reference to detailed models, the development of which is already well underway; tests of these essential interpretive tools are an important product of the proposed investigations.

  15. Revealing electronic structure changes in Chevrel phase cathodes upon Mg insertion using X-ray absorption spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Wan, Liwen F.; Wright, Joshua; Perdue, Brian R.

    Following previous work predicting the electronic response of the Chevrel phase Mo6S8 upon Mg insertion (Thole et al., Phys. Chem. Chem. Phys., 2015, 17, 22548), we provide the experimental proof, evident in X-ray absorption spectroscopy, to illustrate the charge compensation mechanism of the Chevrel phase compound during Mg insertion and de-insertion processes.

  16. Doing Solar Science With Extreme-ultraviolet and X-ray High Resolution Imaging Spectroscopy

    NASA Astrophysics Data System (ADS)

    Doschek, G. A.

    2005-12-01

    In this talk I will demonstrate how high resolution extreme-ultraviolet (EUV) and/or X-ray imaging spectroscopy can be used to provide unique information for solving several current key problems of the solar atmosphere, e.g., the morphology and reconnection site of solar flares, the structure of the transition region, and coronal heating. I will describe the spectra that already exist relevant to these problems and what the shortcomings of the data are, and how an instrument such as the Extreme-ultraviolet Imaging Spectrometer (EIS) on Solar-B as well as other proposed spectroscopy missions such as NEXUS and RAM will improve on the existing observations. I will discuss a few particularly interesting properties of the spectra and atomic data for highly ionized atoms that are important for the science problems.

  17. Effects of sulfation level on the desulfation behavior of pre-sulfated Pt BaO/Al2O3 lean NOx trap catalysts: a combined H2 Temperature-Programmed Reaction, in-situ sulfur K-edge X-ray Absorption Near-Edge Spectroscopy, X-ray Photoelectron Spectroscopy, and Time-Resolved X-ray Diffraction Study

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Kim, Do Heui; Szanyi, Janos; Kwak, Ja Hun

    2009-04-03

    Desulfation by hydrogen of pre-sulfated Pt(2wt%) BaO(20wt%)/Al2O3 with various sulfur loading (S/Ba = 0.12, 0.31 and 0.62) were investigated by combining H2 temperature programmed reaction (TPRX), x-ray photoelectron spectroscopy (XPS), in-situ sulfur K-edge x-ray absorption near-edge spectroscopy (XANES), and synchrotron time-resolved x-ray diffraction (TR-XRD) techniques. We find that the amount of H2S desorbed during the desulfation in the H2 TPRX experiments is not proportional to the amount of initial sulfur loading. The results of both in-situ sulfur K-edge XANES and TR-XRD show that at low sulfur loadings, sulfates were transformed to a BaS phase and remained in the catalyst, rathermore » than being removed as H2S. On the other hand, when the deposited sulfur level exceeded a certain threshold (at least S/Ba = 0.31) sulfates were reduced to form H2S, and the relative amount of the residual sulfide species in the catalyst was much less than at low sulfur loading. Unlike samples with high sulfur loading (e.g., S/Ba = 0.62), H2O did not promote the desulfation for the sample with S/Ba of 0.12, implying that the formed BaS species originating from the reduction of sulfates at low sulfur loading are more stable to hydrolysis. The results of this combined spectroscopy investigation provide clear evidence to show that sulfates at low sulfur loadings are less likely to be removed as H2S and have a greater tendency to be transformed to BaS on the material, leading to the conclusion that desulfation behavior of Pt BaO/Al2O3 lean NOx trap catalysts is markedly dependent on the sulfation levels.« less

  18. Spectroscopy of X-ray Photoionized Plasmas in the Laboratory

    NASA Astrophysics Data System (ADS)

    Liedahl, Duane A.; Loisel, Guillaume; Bailey, James E.; Nagayama, Taisuke; Hansen, Stephanie B.; Rochau, Gregory; Fontes, Christopher J.; Mancini, Roberto; Kallman, Timothy R.

    2018-06-01

    The physical processes operating in astrophysical plasmas --- heating, cooling, ionization, recombination, level population kinetics, and radiation transport --- are all accessible to observation in the laboratory. What distinguishes X-ray photoionized plasmas from the more common case of high-temperature collisionally-ionized plasmas is the elevated level of importance of the radiation/matter interaction. The advent of laboratory facilities with the capability to generate high-powered X-ray sources has provided the means by which to study this interaction, which is also fundamental to active galactic nuclei and other accretion-powered objects. We discuss recent and ongoing experiments, with an emphasis on X-ray spectroscopic measurements of silicon plasmas obtained at the Sandia Z Pulsed Power Facility.

  19. Direct determination of oxidation state of gold deposits in metal-reducing bacterium Shewanella algae using X-ray absorption near-edge structure spectroscopy (XANES).

    PubMed

    Konishi, Yasuhiro; Tsukiyama, Takeshi; Saitoh, Norizoh; Nomura, Toshiyuki; Nagamine, Shinsuke; Takahashi, Yoshio; Uruga, Tomoya

    2007-06-01

    X-ray absorption near-edge structure spectroscopy (XANES) was successfully employed to determine the gold valence in the metal-reducing bacterium Shewanella algae after exposure to a 1 mM aqueous HAuCl4 solution for 10-120 min. XANES spectra revealed the oxidation state of gold in the bacterial cells to be Au(0) without any contribution from Au(III), demonstrating that S. algae cells can reduce AuCl4- ions to elemental gold. Transmission electron microscopy (TEM) and energy dispersive X-ray (EDX) analysis confirmed that gold nanoparticles 5-15 nm in size were deposited in the periplasmic space of the bacterial cells; a preferable, cell surface location for the easy recovery of biogenic nanoparticles.

  20. Characterization of pentavalent and hexavalent americium complexes in nitric acid using X-ray absorption fine structure spectroscopy and first-principles modeling

    DOE PAGES

    Riddle, Catherine; Czerwinski, Kenneth; Kim, Eunja; ...

    2016-01-18

    We studied the speciation of pentavalent and hexavalent americium (Am) complexes in nitric acidicby X-ray absorption fine structure spectroscopy (XAFS), UV-visible spectroscopy, and density functional theory (DFT). Extended x-ray absorption fine structure (EXAFS) and x-ray absorption near edge structure (XANES) results were consistent with the presence of a mixture of AmO 2 + and AmO 2 2+ with only a small amount AmO 2 present. The resulting average bond distances we found were 1.71 Å for Am=O and 2.44 Å for Am-O. All-electron scalar relativistic calculations were also carried out using DFT to predict the equilibrium geometries and properties ofmore » the AmO 2 + and AmO 2 2+ aquo complexes. Calculated bond distances for the Am(VI) complex are in reasonable agreement with EXAFS data and the computed energy gaps between frontier molecular orbitals suggest a slightly higher kinetic stability and chemical hardness of Am(VI) compared to Am(V).« less

  1. 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. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

  2. Elemental content of enamel and dentin after bleaching of teeth (a comparative study between laser-induced breakdown spectroscopy and x-ray photoelectron spectroscopy)

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Imam, H.; Ahmed, Doaa; Eldakrouri, Ashraf

    2013-06-21

    The elemental content of the superficial and inner enamel as well as that of dentin was analyzed using laser-induced breakdown spectroscopy (LIBS) and x-ray photoelectron spectroscopy (XPS) of bleached and unbleached tooth specimens. It is thus clear from the spectral analysis using both the LIBS and XPS technique that elemental changes (though insignificant within the scopes of this study) of variable intensities do occur on the surface of the enamel and extend deeper to reach dentin. The results of the LIBS revealed a slight reduction in the calcium levels in the bleached compared to the control specimens in all themore » different bleaching groups and in both enamel and dentin. The good correlation found between the LIBS and XPS results demonstrates the possibility of LIBS technique for detection of minor loss in calcium and phosphorus in enamel and dentin.« less

  3. Studies of x-ray localization and thickness dependence in atomic-scale elemental mapping by STEM energy-dispersive x-ray spectroscopy using single-frame scanning method

    DOE PAGES

    Lu, Ping; Moya, Jaime M.; Yuan, Renliang; ...

    2018-03-01

    The delocalization of x-ray signals limits the spatial resolution in atomic-scale elemental mapping by scanning transmission electron microscopy (STEM) using energy-dispersive x-ray spectroscopy (EDS). In this study, using a SrTiO 3 [001] single crystal, we show that the x-ray localization to atomic columns is strongly dependent on crystal thickness, and a thin crystal is critical for improving the spatial resolution in atomic-scale EDS mapping. A single-frame scanning technique is used in this study instead of the multiple-frame technique to avoid peak broadening due to tracking error. The strong thickness dependence is realized by measuring the full width at half maximamore » (FWHM) as well as the peak-to-valley (P/V) ratio of the EDS profiles for Ti K and Sr K+L, obtained at several crystal thicknesses. A FWHM of about 0.16 nm and a P/V ratio of greater than 7.0 are obtained for Ti K for a crystal thickness of less than 20 nm. In conclusion, with increasing crystal thickness, the FWHM and P/V ratio increases and decreases, respectively, indicating the advantage of using a thin crystal for high-resolution EDS mapping.« less

  4. Studies of x-ray localization and thickness dependence in atomic-scale elemental mapping by STEM energy-dispersive x-ray spectroscopy using single-frame scanning method

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Lu, Ping; Moya, Jaime M.; Yuan, Renliang

    The delocalization of x-ray signals limits the spatial resolution in atomic-scale elemental mapping by scanning transmission electron microscopy (STEM) using energy-dispersive x-ray spectroscopy (EDS). In this study, using a SrTiO 3 [001] single crystal, we show that the x-ray localization to atomic columns is strongly dependent on crystal thickness, and a thin crystal is critical for improving the spatial resolution in atomic-scale EDS mapping. A single-frame scanning technique is used in this study instead of the multiple-frame technique to avoid peak broadening due to tracking error. The strong thickness dependence is realized by measuring the full width at half maximamore » (FWHM) as well as the peak-to-valley (P/V) ratio of the EDS profiles for Ti K and Sr K+L, obtained at several crystal thicknesses. A FWHM of about 0.16 nm and a P/V ratio of greater than 7.0 are obtained for Ti K for a crystal thickness of less than 20 nm. In conclusion, with increasing crystal thickness, the FWHM and P/V ratio increases and decreases, respectively, indicating the advantage of using a thin crystal for high-resolution EDS mapping.« less

  5. Studies of x-ray localization and thickness dependence in atomic-scale elemental mapping by STEM energy-dispersive x-ray spectroscopy using single-frame scanning method.

    PubMed

    Lu, Ping; Moya, Jaime M; Yuan, Renliang; Zuo, Jian Min

    2018-03-01

    The delocalization of x-ray signals limits the spatial resolution in atomic-scale elemental mapping by scanning transmission electron microscopy (STEM) using energy-dispersive x-ray spectroscopy (EDS). In this study, using a SrTiO 3 [001] single crystal, we show that the x-ray localization to atomic columns is strongly dependent on crystal thickness, and a thin crystal is critical for improving the spatial resolution in atomic-scale EDS mapping. A single-frame scanning technique is used in this study instead of the multiple-frame technique to avoid peak broadening due to tracking error. The strong thickness dependence is realized by measuring the full width at half maxima (FWHM) as well as the peak-to-valley (P/V) ratio of the EDS profiles for Ti K and Sr K + L, obtained at several crystal thicknesses. A FWHM of about 0.16 nm and a P/V ratio of greater than 7.0 are obtained for Ti K for a crystal thickness of less than 20 nm. With increasing crystal thickness, the FWHM and P/V ratio increases and decreases, respectively, indicating the advantage of using a thin crystal for high-resolution EDS mapping. Published by Elsevier B.V.

  6. Effects of Sulfation Level on the Desulfation Behavior of Presulfated Pt-BaO/Al2O3 Lean NOx Trap Catalysts: A Combined H2 Temperature-Programmed Reaction, in Situ Sulfur K-Edge X-ray Absorption Near-Edge Spectroscopy, X-ray Photoelectron Spectroscopy, and Time-Resolved X-ray Diffraction Study

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Kim, D.H.; Hanson, J.; Szanyi, J.

    2009-04-30

    Desulfation by hydrogen of presulfated Pt (2 wt %)-BaO(20 wt %)/Al{sub 2}O{sub 3} with various sulfur loading (S/Ba = 0.12, 0.31, and 0.62) were investigated by combining H{sub 2} temperature programmed reaction (TPRX), X-ray photoelectron spectroscopy (XPS), in situ sulfur K-edge X-ray absorption near-edge spectroscopy (XANES), and synchrotron time-resolved X-ray diffraction (TR-XRD) techniques. We find that the amount of H{sub 2}S desorbed during the desulfation in the H{sub 2} TPRX experiments is not proportional to the amount of initial sulfur loading. The results of both in situ sulfur K-edge XANES and TR-XRD show that at low sulfur loadings, sulfates weremore » transformed to a BaS phase and remained in the catalyst rather than being removed as H{sub 2}S. On the other hand, when the deposited sulfur level exceeded a certain threshold (at least S/Ba = 0.31) sulfates were reduced to form H{sub 2}S, and the relative amount of the residual sulfide species in the catalyst was much less than at low sulfur loading. Unlike samples with high sulfur loading (e.g., S/Ba = 0.62), H{sub 2}O did not promote the desulfation for the sample with S/Ba of 0.12, implying that the formed BaS species originating from the reduction of sulfates at low sulfur loading are more stable to hydrolysis. The results of this combined spectroscopy investigation provide clear evidence to show that sulfates at low sulfur loadings are less likely to be removed as H{sub 2}S and have a greater tendency to be transformed to BaS on the material, leading to the conclusion that desulfation behavior of Pt-BaO/Al{sub 2}O{sub 3} lean NO{sub x} trap catalysts is markedly dependent on the sulfation levels.« less

  7. Electronic structure and magnetic properties of the half-metallic ferrimagnet Mn2VAl probed by soft x-ray spectroscopies

    NASA Astrophysics Data System (ADS)

    Nagai, K.; Fujiwara, H.; Aratani, H.; Fujioka, S.; Yomosa, H.; Nakatani, Y.; Kiss, T.; Sekiyama, A.; Kuroda, F.; Fujii, H.; Oguchi, T.; Tanaka, A.; Miyawaki, J.; Harada, Y.; Takeda, Y.; Saitoh, Y.; Suga, S.; Umetsu, R. Y.

    2018-01-01

    We have studied the electronic structure of ferrimagnetic Mn2VAl single crystals by means of soft x-ray absorption spectroscopy (XAS), x-ray absorption magnetic circular dichroism (XMCD), and resonant soft x-ray inelastic scattering (RIXS). We have successfully observed the XMCD signals for all the constituent elements. The Mn L2 ,3 XAS and XMCD spectra are reproduced by spectral simulations based on density-functional theory, indicating the itinerant character of the Mn 3 d states. On the other hand, the V 3 d electrons are rather localized since the ionic model can qualitatively explain the V L2 ,3 XAS and XMCD spectra. This picture is consistent with local d d excitations revealed by the V L3 RIXS.

  8. Pump-Flow-Probe X-Ray Absorption Spectroscopy as a Tool for Studying Intermediate States of Photocatalytic Systems.

    PubMed

    Smolentsev, Grigory; Guda, Alexander; Zhang, Xiaoyi; Haldrup, Kristoffer; Andreiadis, Eugen; Chavarot-Kerlidou, Murielle; Canton, Sophie E; Nachtegaal, Maarten; Artero, Vincent; Sundstrom, Villy

    2013-08-29

    A new setup for pump-flow-probe X-ray absorption spectroscopy has been implemented at the SuperXAS beamline of the Swiss Light Source. It allows recording X-ray absorption spectra with a time resolution of tens of microseconds and high detection efficiency for samples with sub-mM concentrations. A continuous wave laser is used for the photoexcitation, with the distance between laser and X-ray beams and velocity of liquid flow determining the time delay, while the focusing of both beams and the flow speed define the time resolution. This method is compared with the alternative measurement technique that utilizes a 1 kHz repetition rate laser and multiple X-ray probe pulses. Such an experiment was performed at beamline 11ID-D of the Advanced Photon Source. Advantages, limitations and potential for improvement of the pump-flow-probe setup are discussed by analyzing the photon statistics. Both methods, with Co K-edge probing were applied to the investigation of a cobaloxime-based photo-catalytic reaction. The interplay between optimizing for efficient photoexcitation and time resolution as well as the effect of sample degradation for these two setups are discussed.

  9. Pump-Flow-Probe X-Ray Absorption Spectroscopy as a Tool for Studying Intermediate States of Photocatalytic Systems

    PubMed Central

    Smolentsev, Grigory; Guda, Alexander; Zhang, XIaoyi; Haldrup, Kristoffer; Andreiadis, Eugen; Chavarot-Kerlidou, Murielle; Canton, Sophie E.; Nachtegaal, Maarten; Artero, Vincent; Sundstrom, Villy

    2014-01-01

    A new setup for pump-flow-probe X-ray absorption spectroscopy has been implemented at the SuperXAS beamline of the Swiss Light Source. It allows recording X-ray absorption spectra with a time resolution of tens of microseconds and high detection efficiency for samples with sub-mM concentrations. A continuous wave laser is used for the photoexcitation, with the distance between laser and X-ray beams and velocity of liquid flow determining the time delay, while the focusing of both beams and the flow speed define the time resolution. This method is compared with the alternative measurement technique that utilizes a 1 kHz repetition rate laser and multiple X-ray probe pulses. Such an experiment was performed at beamline 11ID-D of the Advanced Photon Source. Advantages, limitations and potential for improvement of the pump-flow-probe setup are discussed by analyzing the photon statistics. Both methods, with Co K-edge probing were applied to the investigation of a cobaloxime-based photo-catalytic reaction. The interplay between optimizing for efficient photoexcitation and time resolution as well as the effect of sample degradation for these two setups are discussed. PMID:24443663

  10. Catalysis of GTP hydrolysis by small GTPases at atomic detail by integration of X-ray crystallography, experimental, and theoretical IR spectroscopy.

    PubMed

    Rudack, Till; Jenrich, Sarah; Brucker, Sven; Vetter, Ingrid R; Gerwert, Klaus; Kötting, Carsten

    2015-10-02

    Small GTPases regulate key processes in cells. Malfunction of their GTPase reaction by mutations is involved in severe diseases. Here, we compare the GTPase reaction of the slower hydrolyzing GTPase Ran with Ras. By combination of time-resolved FTIR difference spectroscopy and QM/MM simulations we elucidate that the Mg(2+) coordination by the phosphate groups, which varies largely among the x-ray structures, is the same for Ran and Ras. A new x-ray structure of a Ran·RanBD1 complex with improved resolution confirmed this finding and revealed a general problem with the refinement of Mg(2+) in GTPases. The Mg(2+) coordination is not responsible for the much slower GTPase reaction of Ran. Instead, the location of the Tyr-39 side chain of Ran between the γ-phosphate and Gln-69 prevents the optimal positioning of the attacking water molecule by the Gln-69 relative to the γ-phosphate. This is confirmed in the RanY39A·RanBD1 crystal structure. The QM/MM simulations provide IR spectra of the catalytic center, which agree very nicely with the experimental ones. The combination of both methods can correlate spectra with structure at atomic detail. For example the FTIR difference spectra of RasA18T and RanT25A mutants show that spectral differences are mainly due to the hydrogen bond of Thr-25 to the α-phosphate in Ran. By integration of x-ray structure analysis, experimental, and theoretical IR spectroscopy the catalytic center of the x-ray structural models are further refined to sub-Å resolution, allowing an improved understanding of catalysis. © 2015 by The American Society for Biochemistry and Molecular Biology, Inc.

  11. In situ study of an oxidation reaction on a Pt/C electrode by ambient pressure hard X-ray photoelectron spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Takagi, Yasumasa, E-mail: ytakagi@ims.ac.jp; Uemura, Yohei; Yokoyama, Toshihiko

    2014-09-29

    We have constructed an ambient pressure X-ray photoelectron spectroscopy instrument that uses hard X-ray radiation at the high-performance undulator beamline BL36XU of SPring-8. The dependence of the Au 4f peak intensity from Au foil on the ambient N{sub 2} pressure was measured. At a photon energy of 7.94 keV, the Au 4f peak intensity maintained 40% at 3000 Pa compared with that at high vacuum. We designed a polymer electrolyte fuel cell that allows us to perform X-ray photoelectron spectroscopy measurements of an electrode under working conditions. The oxidized Pt peaks were observed in the Pt 3d{sub 5/2} level of Pt nanoparticlesmore » in the cathode, and the peaks clearly depended on the applied voltage between the anode and cathode. Our apparatus can be applied as a valuable in situ tool for the investigation of the electronic states and adsorbed species of polymer electrolyte fuel cell electrode catalysts under the reaction conditions.« less

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

    NASA Astrophysics Data System (ADS)

    Lee, Eunsook; Kim, D. H.; Kang, J.-S.; Kim, Kyung Hyun; Kim, Pil; Baik, Jaeyoon; Shin, H. J.

    2014-11-01

    The electronic structures of molecule-based nanoparticles, such as biomineralized Helicobacter pylori ferritin (Hpf), Heme, and RbCo[Fe(CN)6]H2O (RbCoFe) Prussian blue analogue, have been investigated by employing photoemission spectroscopy and soft X-ray absorption spectroscopy. Fe ions are found to be nearly trivalent in Hpf and Heme nanoparticles, which provides evidence that the amount of magnetite (Fe3O4) should be negligible in the Hpf core and that the biomineralization of Fe oxides in the high-Fe-bound-state Hpf core arises from a hematite-like formation. On the other hand, Fe ions are nearly divalent and Co ions are Co2+-Co3+ mixed-valent in RbCoFe. Therefore this finding suggests that the mechanism of the photo-induced transition in RbCoFe Prussian blue analogue is not a simple spin-state transition of Fe2+-Co3+ → Fe3+-Co2+. It is likely that Co2+ ions have the high-spin configuration while Fe2+ ions have the low-spin configuration.

  13. X-ray induced dimerization of cinnamic acid: Time-resolved inelastic X-ray scattering study

    PubMed Central

    Inkinen, Juho; Niskanen, Johannes; Talka, Tuomas; Sahle, Christoph J.; Müller, Harald; Khriachtchev, Leonid; Hashemi, Javad; Akbari, Ali; Hakala, Mikko; Huotari, Simo

    2015-01-01

    A classic example of solid-state topochemical reactions is the ultraviolet-light induced photodimerization of α-trans-cinnamic acid (CA). Here, we report the first observation of an X-ray-induced dimerization of CA and monitor it in situ using nonresonant inelastic X-ray scattering spectroscopy (NRIXS). The time-evolution of the carbon core-electron excitation spectra shows the effects of two X-ray induced reactions: dimerization on a short time-scale and disintegration on a long time-scale. We used spectrum simulations of CA and its dimerization product, α-truxillic acid (TA), to gain insight into the dimerization effects. From the time-resolved spectra, we extracted component spectra and time-dependent weights corresponding to CA and TA. The results suggest that the X-ray induced dimerization proceeds homogeneously in contrast to the dimerization induced by ultraviolet light. We also utilized the ability of NRIXS for direct tomography with chemical-bond contrast to image the spatial progress of the reactions in the sample crystal. Our work paves the way for other time-resolved studies on chemical reactions using inelastic X-ray scattering. PMID:26568420

  14. The Physics of Accretion in X-Ray Binaries

    NASA Technical Reports Server (NTRS)

    Vrtilek, S.; Oliversen, Ronald (Technical Monitor)

    2001-01-01

    This project consists of several related investigations directed to the study of mass transfer processes in X-ray binaries. Models developed over several years incorporating highly detailed physics will be tested on a balanced mix of existing data and planned observations with both ground and space-based observatories. The extended time coverage of the observations and the existence of simultaneous X-ray, ultraviolet, and optical observations will be particularly beneficial for studying the accretion flows. These investigations, which take as detailed a look at the accretion process in X-ray binaries as is now possible, test current models to their limits, and force us to extend them. We now have the ability to do simultaneous ultraviolet/X-ray/optical spectroscopy with HST, Chandra, XMM, and ground-based observatories. The rich spectroscopy that these observations give us must be interpreted principally by reference to detailed models, the development of which is already well underway; tests of these essential interpretive tools are an important product of the proposed investigations.

  15. In Situ Mineralogical Analysis of Planetary Materials Using X-Ray Diffraction and X-Ray Fluorescence

    NASA Technical Reports Server (NTRS)

    Sarrazin, P.; Blake, D.; Vaniman, D.; Chang, Sherwood (Technical Monitor)

    1996-01-01

    Remote observations of Mars have led scientists to believe that its early climate was similar to that of the early Earth, having had abundant liquid water and a dense atmosphere. One of the most fascinating questions of recent times is whether simple bacterial life developed on Mars (as it did on the Earth) during this early element period. Analyses of SNC meteorites have broadened considerably our knowledge of the chemistry of certain types of Martian rocks, underscoring the tantalizing possibility of early hydrothermal systems and even of ancient bacterial life. Detailed analyses of SNC meteorites in Terrestrial laboratories utilize the most sophisticated organic, isotopic and microscopic techniques in existence. Indeed; it is unlikely that the key biogenic indicators used in McKay et al (ibid) could be identified by a remote instrument on the surface of Mars. As a result, it is probable that any robotic search for evidence of an ancient Martian biosphere will have as its focus the identification of key minerals in likely host rocks rather than the direct detection of organic or isotopic biomarkers. Even on a sample return mission, mineralogical screening will be utilized to choose the most likely candidate rocks. X-ray diffraction (XRD) is the only technique that can provide a direct determination of the crystal structures of the phases present within a sample. When many different crystalline phases are present, quantitative analysis is better constrained if used in conjunction with a determination of elemental composition, obtainable by X-ray fluorescence (XRF) using the same X-ray source as for XRD. For planetary surface analysis, a remote instrument combining XRD and XRF could be used for mineralogical characterization of both soils and rocks. We are designing a remote XRD/XRF instrument with this objective in mind. The instrument concept pays specific attention to constraints in sample preparation, weight, volume, power, etc. Based on the geometry of a

  16. Determination of minor and trace elements in kidney stones by x-ray fluorescence analysis

    NASA Astrophysics Data System (ADS)

    Srivastava, Anjali; Heisinger, Brianne J.; Sinha, Vaibhav; Lee, Hyong-Koo; Liu, Xin; Qu, Mingliang; Duan, Xinhui; Leng, Shuai; McCollough, Cynthia H.

    2014-03-01

    The determination of accurate material composition of a kidney stone is crucial for understanding the formation of the kidney stone as well as for preventive therapeutic strategies. Radiations probing instrumental activation analysis techniques are excellent tools for identification of involved materials present in the kidney stone. In particular, x-ray fluorescence (XRF) can be very useful for the determination of minor and trace materials in the kidney stone. The X-ray fluorescence measurements were performed at the Radiation Measurements and Spectroscopy Laboratory (RMSL) of department of nuclear engineering of Missouri University of Science and Technology and different kidney stones were acquired from the Mayo Clinic, Rochester, Minnesota. Presently, experimental studies in conjunction with analytical techniques were used to determine the exact composition of the kidney stone. A new type of experimental set-up was developed and utilized for XRF analysis of the kidney stone. The correlation of applied radiation source intensity, emission of X-ray spectrum from involving elements and absorption coefficient characteristics were analyzed. To verify the experimental results with analytical calculation, several sets of kidney stones were analyzed using XRF technique. The elements which were identified from this techniques are Silver (Ag), Arsenic (As), Bromine (Br), Chromium (Cr), Copper (Cu), Gallium (Ga), Germanium (Ge), Molybdenum (Mo), Niobium (Nb), Rubidium (Rb), Selenium (Se), Strontium (Sr), Yttrium (Y), Zirconium (Zr). This paper presents a new approach for exact detection of accurate material composition of kidney stone materials using XRF instrumental activation analysis technique.

  17. X-Ray Astronomy Research at the Marshall Space Flight Center

    NASA Technical Reports Server (NTRS)

    Austin, Robert A.

    1999-01-01

    For at least twenty years, NASA's Marshall Space Flight Center (MSFC) has played a major role in the development of X-ray astronomy in the United States. MSFC scientists and engineers are currently involved in a wide range of programs which will contribute to the growth of X-ray astronomy well into the next century. Areas of activity include calibration of X-ray astronomy instrumentation using Marshall's world-class X-ray Calibration Facility (XRCF), development of high-throughput, replicated X-ray optics, X-ray detector development, balloon-based X-ray astronomy, and analysis of Active Galactic Nuclei (AGNs) and clusters of galaxies. Recent milestones include the successful calibration of NASA's premier X-ray Astronomy Satellite - AXAF (recently renamed Chandra), a balloon flight of a large area (1000 sq cm) micro-strip proportional counter, and work on a hard X-ray (30-100 keV) telescope called HERO, capable of high quality spectroscopy and imaging through the use of grazing incidence optics and an Imaging Gas Scintillation Proportional Counter (IGSPC). In my presentation, I will provide a general overview of our research and facilities. I will conclude with a more detailed discussion of our High Energy Replicated Optics (HERO) program and plans for long duration (>100 days) balloon flights which will take place in the near future.

  18. Handbook Of X-ray Astronomy

    NASA Astrophysics Data System (ADS)

    Arnaud, Keith A.; Smith, R. K.; Siemiginowska, A.; Edgar, R. J.; Grant, C. E.; Kuntz, K. D.; Schwartz, D. A.

    2011-09-01

    This poster advertises a book to be published in September 2011 by Cambridge University Press. Written for graduate students, professional astronomers and researchers who want to start working in this field, this book is a practical guide to x-ray astronomy. The handbook begins with x-ray optics, basic detector physics and CCDs, before focussing on data analysis. It introduces the reduction and calibration of x-ray data, scientific analysis, archives, statistical issues and the particular problems of highly extended sources. The book describes the main hardware used in x-ray astronomy, emphasizing the implications for data analysis. The concepts behind common x-ray astronomy data analysis software are explained. The appendices present reference material often required during data analysis.

  19. Simulating Valence-to-Core X-ray Emission Spectroscopy of Transition Metal Complexes with Time-Dependent Density Functional Theory.

    PubMed

    Zhang, Yu; Mukamel, Shaul; Khalil, Munira; Govind, Niranjan

    2015-12-08

    Valence-to-core (VtC) X-ray emission spectroscopy (XES) has emerged as a powerful technique for the structural characterization of complex organometallic compounds in realistic environments. Since the spectrum represents electronic transitions from the ligand molecular orbitals to the core holes of the metal centers, the approach is more chemically sensitive to the metal-ligand bonding character compared with conventional X-ray absorption techniques. In this paper we study how linear-response time-dependent density functional theory (LR-TDDFT) can be harnessed to simulate K-edge VtC X-ray emission spectra reliably. LR-TDDFT allows one to go beyond the single-particle picture that has been extensively used to simulate VtC-XES. We consider seven low- and high-spin model complexes involving chromium, manganese, and iron transition metal centers. Our results are in good agreement with experiment.

  20. In Situ Solid-State Reactions Monitored by X-ray Absorption Spectroscopy: Temperature-Induced Proton Transfer Leads to Chemical Shifts.

    PubMed

    Stevens, Joanna S; Walczak, Monika; Jaye, Cherno; Fischer, Daniel A

    2016-10-24

    The dramatic colour and phase alteration with the solid-state, temperature-dependent reaction between squaric acid and 4,4'-bipyridine has been probed in situ with X-ray absorption spectroscopy. The electronic and chemical sensitivity to the local atomic environment through chemical shifts in the near-edge X-ray absorption fine structure (NEXAFS) revealed proton transfer from the acid to the bipyridine base through the change in nitrogen protonation state in the high-temperature form. Direct detection of proton transfer coupled with structural analysis elucidates the nature of the solid-state process, with intermolecular proton transfer occurring along an acid-base chain followed by a domino effect to the subsequent acid-base chains, leading to the rapid migration along the length of the crystal. NEXAFS thereby conveys the ability to monitor the nature of solid-state chemical reactions in situ, without the need for a priori information or long-range order. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Resonant soft X-ray scattering for polymer materials

    DOE PAGES

    Liu, Feng; Brady, Michael A.; Wang, Cheng

    2016-04-16

    Resonant Soft X-ray Scattering (RSoXS) was developed within the last few years, and the first dedicated resonant soft X-ray scattering beamline for soft materials was constructed at the Advanced Light Source, LBNL. RSoXS combines soft X-ray spectroscopy with X-ray scattering and thus offers statistical information for 3D chemical morphology over a large length scale range from nanometers to micrometers. Using RSoXS to characterize multi-length scale soft materials with heterogeneous chemical structures, we have demonstrated that soft X-ray scattering is a unique complementary technique to conventional hard X-ray and neutron scattering. Its unique chemical sensitivity, large accessible size scale, molecular bondmore » orientation sensitivity with polarized X-rays, and high coherence have shown great potential for chemically specific structural characterization for many classes of materials.« less

  2. Searching for outflows in ultraluminous X-ray sources through high-resolution X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Kosec, P.; Pinto, C.; Fabian, A. C.; Walton, D. J.

    2018-02-01

    Ultraluminous X-ray sources (ULXs) are non-nuclear point sources exceeding the Eddington luminosity of a 10 M⊙ black hole. Modern consensus for a majority of the ULX population is that they are powered by stellar-mass black holes or neutron stars accreting well above the Eddington limit. Theoretical models of super-Eddington accretion predict existence of powerful outflows of moderately ionized gas at mildly relativistic velocities. So far, these winds have been found in three systems: NGC 1313 X-1, NGC 5408 X-1 and NGC 55 ULX. In this work, we create a sample of all ULXs with usable archival high-resolution X-ray data, with 10 sources in total, in which we aim to find more signatures of outflows. We perform Gaussian line scans to find any narrow spectral signatures, and physical wind model scans where possible. We tentatively identify an outflow in NGC 5204 X-1, blueshifted to 0.34c, which produces emission features with a total significance of at least 3σ. Next we compare ULXs with similar hardness ratios. Holmberg IX X-1 shows absorption features that could be associated with a photoionized outflowing absorber, similar to that seen in NGC 1313 X-1. The spectrum of Holmberg II X-1 possesses features similar to NGC 5408 X-1 and NGC 6946 X-1 shows O VIII rest-frame emission. All other sources from the sample also show tentative evidence of spectral features in their high-resolution spectra. Further observations with the XMM-Newton and Chandra gratings will place stronger constraints. Future missions like XARM and Athena will be able to detect them at larger distances and increase our sample.

  3. Experimental Results and Modeling of Low-Heat-Capacity TES Microcalorimeters for Soft-X-ray Spectroscopy

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Eckart, Megan E.; NASA Postdoctoral Program Fellow; Adams, Joseph S.

    2009-12-16

    Transition-edge-sensor (TES) X-ray microcalorimeters have mostly been targeted at mid-band energies from 0.05-10 keV and high energies to above 100 keV. However, many other optimizations are possible. Here we present results from devices optimized for soft X-ray applications. For spectroscopy below 1 keV, the X-ray stopping power and heat capacity (C) of the TES itself are high enough that we can omit a separate absorber. The resulting devices have low C and the best-achievable energy resolution should be under 1 eV. We are interested in pursuing such devices primarily for astrophysical applications and laboratory astrophysics at LLNL's Electron-Beam Ion Trap.more » To this end, we have studied arrays in which 'bare' TESs are interspersed with broad-band pixels that have absorbers. By extending the absorbers to cover the area where the leads contact the low-energy pixels, we have eliminated a significant source of non-Gaussian detector response. The bare devices are in a different regime from our typical devices in that C is ten times lower and the conductance to the bath is four times lower. We have explored this regime through simultaneous fitting of noise and impedance data. These data cannot be fit by the simple model we employ to describe our typical broad-band devices. In this contribution we present X-ray spectra and the results from modeling.« less

  4. Ambient-Pressure X-ray Photoelectron Spectroscopy to Characterize the Solid/Liquid Interface: Probing the Electrochemical Double Layer

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Favaro, Marco; Liu, Zhi; Crumlin, Ethan J.

    Ambient-pressure X-ray photoelectron spectroscopy (APXPS) has contributed greatly to a wide range of research fields, including environmental science, catalysis, and electrochemistry, to name a few. The use of this technique at synchrotron facilities primarily focused on probing the solid/gas interface; however, it quickly advanced to the probing of liquid/vapor interfaces and solid/liquid interfaces through an X-ray-transparent window. Most recently, combining APXPS with “Tender” X-rays (~2.5 keV to 8 keV) on beamline 9.3.1 at the Advanced Light Source in Lawrence Berkeley National Laboratory (which can generate photoelectrons with much longer inelastic mean free paths) has enabled us to probe the solid/liquidmore » interface without needing a window. This innovation allows us to probe interfacial chemistries of electrochemically controlled solid/liquid interfaces undergoing charge transfer reactions. Lastly, these advancements have transitioned APXPS from a traditional surface science tool to an essential interface science technique.« less

  5. Ambient-Pressure X-ray Photoelectron Spectroscopy to Characterize the Solid/Liquid Interface: Probing the Electrochemical Double Layer

    DOE PAGES

    Favaro, Marco; Liu, Zhi; Crumlin, Ethan J.

    2017-03-31

    Ambient-pressure X-ray photoelectron spectroscopy (APXPS) has contributed greatly to a wide range of research fields, including environmental science, catalysis, and electrochemistry, to name a few. The use of this technique at synchrotron facilities primarily focused on probing the solid/gas interface; however, it quickly advanced to the probing of liquid/vapor interfaces and solid/liquid interfaces through an X-ray-transparent window. Most recently, combining APXPS with “Tender” X-rays (~2.5 keV to 8 keV) on beamline 9.3.1 at the Advanced Light Source in Lawrence Berkeley National Laboratory (which can generate photoelectrons with much longer inelastic mean free paths) has enabled us to probe the solid/liquidmore » interface without needing a window. This innovation allows us to probe interfacial chemistries of electrochemically controlled solid/liquid interfaces undergoing charge transfer reactions. Lastly, these advancements have transitioned APXPS from a traditional surface science tool to an essential interface science technique.« less

  6. Ultrafast time-resolved X-ray absorption spectroscopy of ferrioxalate photolysis with a laser plasma X-ray source and microcalorimeter array

    DOE PAGES

    O’Neil, Galen C.; Miaja-Avila, Luis; Joe, Young Il; ...

    2017-02-17

    The detailed pathways of photoactivity on ultrafast time scales are a topic of contemporary interest. Using a tabletop apparatus based on a laser plasma X-ray source and an array of cryogenic microcalorimeter X-ray detectors, we measured a transient X-ray absorption spectrum during the ferrioxalate photoreduction reaction. With these high-efficiency detectors, we observe the Fe K edge move to lower energies and the amplitude of the extended X-ray absorption fine structure reduce, consistent with a photoreduction mechanism in which electron transfer precedes disassociation. We provide quantitative limits on the Fe–O bond length change. Lastly, we review potential improvements to our measurementmore » technique, highlighting the future potential of tabletop X-ray science using microcalorimeter sensors.« less

  7. Ultrafast time-resolved X-ray absorption spectroscopy of ferrioxalate photolysis with a laser plasma X-ray source and microcalorimeter array

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    O’Neil, Galen C.; Miaja-Avila, Luis; Joe, Young Il

    The detailed pathways of photoactivity on ultrafast time scales are a topic of contemporary interest. Using a tabletop apparatus based on a laser plasma X-ray source and an array of cryogenic microcalorimeter X-ray detectors, we measured a transient X-ray absorption spectrum during the ferrioxalate photoreduction reaction. With these high-efficiency detectors, we observe the Fe K edge move to lower energies and the amplitude of the extended X-ray absorption fine structure reduce, consistent with a photoreduction mechanism in which electron transfer precedes disassociation. We provide quantitative limits on the Fe–O bond length change. Lastly, we review potential improvements to our measurementmore » technique, highlighting the future potential of tabletop X-ray science using microcalorimeter sensors.« less

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

    DOE PAGES

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

    2017-01-17

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

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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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

  10. 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.

  11. X-RAY SPECTROSCOPY OF THE HIGH-MASS X-RAY BINARY PULSAR CENTAURUS X-3 OVER ITS BINARY ORBIT

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Naik, Sachindra; Ali, Zulfikar; Paul, Biswajit, E-mail: snaik@prl.res.in

    2011-08-20

    We present a comprehensive spectral analysis of the high-mass X-ray binary (HMXB) pulsar Centaurus X-3 with the Suzaku observatory covering nearly one orbital period. The light curve shows the presence of extended dips which are rarely seen in HMXBs. These dips are seen up to as high as {approx}40 keV. The pulsar spectra during the eclipse, out-of-eclipse, and dips are found to be well described by a partial covering power-law model with high-energy cutoff and three Gaussian functions for 6.4 keV, 6.7 keV, and 6.97 keV iron emission lines. The dips in the light curve can be explained by themore » presence of an additional absorption component with high column density and covering fraction, the values of which are not significant during the rest of the orbital phases. The iron line parameters during the dips and eclipse are significantly different compared to those during the rest of the observation. During the dips, the iron line intensities are found to be lesser by a factor of 2-3 with a significant increase in the line equivalent widths. However, the continuum flux at the corresponding orbital phase is estimated to be lesser by more than an order of magnitude. Similarities in the changes in the iron line flux and equivalent widths during the dips and eclipse segments suggest that the dipping activity in Cen X-3 is caused by an obscuration of the neutron star by dense matter, probably structures in the outer region of the accretion disk, as in the case of dipping low-mass X-ray binaries.« less

  12. An X-ray absorption spectroscopy study of the interactions of Ni2+ with yeast enolase.

    PubMed

    Wang, S; Scott, R A; Lebioda, L; Zhou, Z H; Brewer, J M

    1995-05-15

    An x-ray absorption spectroscopy (XAS) study was carried out at pH 7.6 on solutions of Ni2+ and yeast enolase depleted of its physiological cofactor (Mg2+) in the presence or absence of substrate/product, the very strongly bound competitive inhibitor 2-phosphonoacetohydroxamate and Mg2+. Both "conformational" and "catalytic" Ni2+ are distorted octahedral in coordination, in agreement with several spectroscopic studies but in contrast to the coordination in the crystal at pH 6.0. The data are consistent with direct coordination of what must be the catalytic Ni2+ to the phosphate of the substrate, in agreement with some previous data but in disagreement with recent interpretations by other workers. The ligands around the metal ions obtained from the x-ray structure give simulated XAS spectra in good agreement with the observed spectra.

  13. Future prospects for high resolution X-ray spectrometers

    NASA Technical Reports Server (NTRS)

    Canizares, C. R.

    1981-01-01

    Capabilities of the X-ray spectroscopy payloads were compared. Comparison of capabilities of AXAF in the context of the science to be achieved is reported. The Einstein demonstrated the tremendous scientific power of spectroscopy to probe deeply the astrophysics of all types of celestial X-ray source. However, it has limitations in sensitivity and resolution. Each of the straw man instruments has a sensitivity that is at least an order of magnitude better than that of the Einstein FPSC. The AXAF promises powerful spectral capability.

  14. Electronic structure of transition metal-cysteine complexes from X-ray absorption spectroscopy.

    PubMed

    Leung, Bonnie O; Jalilehvand, Farideh; Szilagyi, Robert K

    2008-04-17

    The electronic structures of HgII, NiII, CrIII, and MoV complexes with cysteine were investigated by sulfur K-edge X-ray absorption near-edge structure (XANES) spectroscopy and density functional theory. The covalency in the metal-sulfur bond was determined by analyzing the intensities of the electric-dipole allowed pre-edge features appearing in the XANES spectra below the ionization threshold. Because of the well-defined structures of the selected cysteine complexes, the current work provides a reference set for further sulfur K-edge XAS studies of bioinorganic active sites with transition metal-sulfur bonds from cysteine residues as well as more complex coordination compounds with thiolate ligands.

  15. NASA's Future X-ray Missions: From Constellation-X to Generation-X

    NASA Technical Reports Server (NTRS)

    Hornschemeier, A.

    2006-01-01

    Among the most important topics in modern astrophysics are the formation and evolution of supermassive black holes in concert with galaxy bulges, the nature of the dark energy equation of state, and the self-regulating symmetry imposed by both stellar and AGN feedback. All of these topics are readily addressed with observations at X-ray wavelengths. NASA's next major X-ray observatory is Constellation-X, which is being developed to perform spatially resolved high-resolution X-ray spectroscopy. Con-X will directly measure the physical properties of material near black holes' last stable orbits and the absolute element abundances and velocities of hot gas in clusters of galaxies. The Con-X mission will be described, as well as its successor, Generation-X (anticipated to fly approx.1 decade after Con-X). After describing these missions and their driving science areas, the talk will focus on areas in which Chandra observing programs may enable science with future X-ray observatories. These areas include a possible ultra-deep Chandra imaging survey as an early Universe pathfinder, a large program to spatially resolve the hot intracluster medium of massive clusters to aid dark energy measurements, and possible deep spectroscopic observations to aid in preparatory theoretical atomic physics work needed for interpreting Con-X spectra.

  16. Lab-based ambient pressure X-ray photoelectron spectroscopy from past to present

    NASA Astrophysics Data System (ADS)

    Arble, Chris; Jia, Meng; Newberg, John T.

    2018-05-01

    Chemical interactions which occur at a heterogeneous interface between a gas and substrate are critical in many technological and natural processes. Ambient pressure X-ray photoelectron spectroscopy (AP-XPS) is a powerful spectroscopy tool that is inherently surface sensitive, elemental and chemical specific, with the ability to probe sample surfaces in the presence of a gas phase. In this review, we discuss the evolution of lab-based AP-XPS instruments, from the first development by Siegbahn and coworkers up through modern day systems. A comprehensive overview is given of heterogeneous experiments investigated to date via lab-based AP-XPS along with the different instrumental metrics that affect the quality of sample probing. We conclude with a discussion of future directions for lab-based AP-XPS, highlighting the efficacy for this in-demand instrument to continue to expand in its ability to significantly advance our understanding of surface chemical processes under in situ conditions in a technologically multidisciplinary setting.

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

    NASA Astrophysics Data System (ADS)

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

    2004-03-01

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

  18. Evidence of Mott physics in iron pnictides from x-ray spectroscopy

    DOE PAGES

    Lafuerza, S.; Gretarsson, H.; Hardy, F.; ...

    2017-07-24

    The existence of large instantaneous local magnetic moments in paramagnetic phases is a direct signature of Mott localization. In order to track the doping evolution of fluctuating local moments in iron-based superconductors, we jointly use two fast probes, x-ray emission and absorption spectroscopies. Exploring K- and Cr-hole-doped BaF e 2 A s 2 , we also find a systematic increase in the local moment with hole-doping, in contrast with inelastic neutron scattering measurements, which suggest an opposite trend. The results support the theoretical scenario in which a Mott insulating state that would be realized for half-filled conduction bands has anmore » influence throughout the phase diagram of these iron pnictides.« less

  19. Valence band offset of β-Ga2O3/wurtzite GaN heterostructure measured by X-ray photoelectron spectroscopy.

    PubMed

    Wei, Wei; Qin, Zhixin; Fan, Shunfei; Li, Zhiwei; Shi, Kai; Zhu, Qinsheng; Zhang, Guoyi

    2012-10-10

    A sample of the β-Ga2O3/wurtzite GaN heterostructure has been grown by dry thermal oxidation of GaN on a sapphire substrate. X-ray diffraction measurements show that the β-Ga2O3 layer was formed epitaxially on GaN. The valence band offset of the β-Ga2O3/wurtzite GaN heterostructure is measured by X-ray photoelectron spectroscopy. It is demonstrated that the valence band of the β-Ga2O3/GaN structure is 1.40 ± 0.08 eV.

  20. A novel spinal kinematic analysis using X-ray imaging and vicon motion analysis: a case study.

    PubMed

    Noh, Dong K; Lee, Nam G; You, Joshua H

    2014-01-01

    This study highlights a novel spinal kinematic analysis method and the feasibility of X-ray imaging measurements to accurately assess thoracic spine motion. The advanced X-ray Nash-Moe method and analysis were used to compute the segmental range of motion in thoracic vertebra pedicles in vivo. This Nash-Moe X-ray imaging method was compared with a standardized method using the Vicon 3-dimensional motion capture system. Linear regression analysis showed an excellent and significant correlation between the two methods (R2 = 0.99, p < 0.05), suggesting that the analysis of spinal segmental range of motion using X-ray imaging measurements was accurate and comparable to the conventional 3-dimensional motion analysis system. Clinically, this novel finding is compelling evidence demonstrating that measurements with X-ray imaging are useful to accurately decipher pathological spinal alignment and movement impairments in idiopathic scoliosis (IS).

  1. On the Detectability of CO Molecules in the Interstellar Medium via X-Ray Spectroscopy

    NASA Technical Reports Server (NTRS)

    Joachimi, Katerine; Gatuzz, Efrain; Garcia, Javier; Kallman, Timothy R.

    2016-01-01

    We present a study of the detectability of CO molecules in the Galactic interstellar medium using high-resolution X-ray spectra obtained with the XMM-Newton Reflection Grating Spectrometer. We analysed 10 bright low mass X-ray binaries (LMXBs) to study the CO contribution in their line of sights. A total of 25 observations were fitted with the ISMabs X-ray absorption model which includes photoabsorption cross-sections for Oi, Oii, Oiii and CO. We performed a Monte Carlo (MC) simulation analysis of the goodness of fit in order to estimate the significance of the CO detection. We determine that the statistical analysis prevents a significant detection of CO molecular X-ray absorption features, except for the lines of sight towards XTE J1718-330 and 4U 1636-53. In the case of XTE J1817-330, this is the first report of the presence of CO along its line of sight. Our results reinforce the conclusion that molecules have a minor contribution to the absorption features in the O K-edge spectral region. We estimate a CO column density lower limit to perform a significant detection with XMM-Newton of N(CO) greater than 6 x 10(exp 16) per sq cm for typical exposure times.

  2. Analysis of Microflares from the Second Sounding Rocket Flight of the Focusing Optics X-ray Solar Imager (FOXSI-2)

    NASA Astrophysics Data System (ADS)

    Vievering, J. T.; Glesener, L.; Krucker, S.; Christe, S.; Buitrago-Casas, J. C.; Ishikawa, S. N.; Ramsey, B.; Takahashi, T.; Watanabe, S.

    2016-12-01

    Observations of the sun in hard x-rays can provide insight into many solar phenomena which are not currently well-understood, including the mechanisms behind particle acceleration in flares. Currently, RHESSI is the only solar-dedicated spacecraft observing in the hard x-ray regime. Though RHESSI has greatly added to our knowledge of flare particle acceleration, the method of rotation modulation collimators is limited in sensitivity and dynamic range. By instead using a direct imaging technique, the structure and evolution of even small flares and active regions can be investigated in greater depth. FOXSI (Focusing Optics X-ray Solar Imager), a hard x-ray instrument flown on two sounding rocket campaigns, seeks to achieve these improved capabilities by using focusing optics for solar observations in the 4-20 keV range. During the second of the FOXSI flights, flown on December 11, 2014, two microflares were observed, estimated as GOES class A0.5 and A2.5 (upper limits). Preliminary analysis of these two flares will be presented, including imaging spectroscopy, light curves, and photon spectra. Through this analysis, we investigate the capabilities of FOXSI in enhancing our knowledge of smaller-scale solar events.

  3. Optically detected X-ray absorption spectroscopy measurements as a means of monitoring corrosion layers on copper.

    PubMed

    Dowsett, Mark G; Adriaens, Annemie; Jones, Gareth K C; Poolton, Nigel; Fiddy, Steven; Nikitenko, Sergé

    2008-11-15

    XANES and EXAFS information is conventionally measured in transmission through the energy-dependent absorption of X-rays or by observing X-ray fluorescence, but secondary fluorescence processes, such as the emission of electrons and optical photons (e.g., 200-1000 nm), can also be used as a carrier of the XAS signatures, providing complementary information such as improved surface specificity. Where the near-visible photons have a shorter range in a material, the data will be more surface specific. Moreover, optical radiation may escape more readily than X-rays through liquid in an environmental cell. Here, we describe a first test of optically detected X-ray absorption spectroscopy (ODXAS) for monitoring electrochemical treatments on copper-based alloys, for example, heritage metals. Artificially made corrosion products deposited on a copper substrate were analyzed in air and in a 1% (w/v) sodium sesquicarbonate solution to simulate typical conservation methods for copper-based objects recovered from marine environments. The measurements were made on stations 7.1 and 9.2 MF (SRS Daresbury, UK) using the mobile luminescence end station (MoLES), supplemented by XAS measurements taken on DUBBLE (BM26 A) at the ESRF. The ODXAS spectra usually contain fine structure similar to that of XAS spectra measured in X-ray fluorescence. Importantly, for the compounds examined, the ODXAS is significantly more surface specific, and >98% characteristic of thin surface layers of 0.5-1.5-microm thickness in cases where X-ray measurements are dominated by the substrate. However, EXAFS and XANES from broadband optical measurements are superimposed on a high background due to other optical emission modes. This produces statistical fluctuations up to double what would be expected from normal counting statistics because the data retain the absolute statistical fluctuation in the original raw count, while losing up to 70% of their magnitude when background is removed. The problem may be

  4. High Resolution X-ray Spectroscopy and Star Formation: HETG Observations of the Pre-Main Sequence Stellar Cluster IC 348

    NASA Astrophysics Data System (ADS)

    Principe, David; Huenemoerder, David P.; Schulz, Norbert; Kastner, Joel H.; Weintraub, David; Preibisch, Thomas

    2018-01-01

    We present Chandra High Energy Transmission Grating (HETG) observations of the ∼3 Myr old pre-main sequence (pre-MS) stellar cluster IC 348. With 400-500 cluster members at a distance of ∼300 pc, IC 348 is an ideal target to observe a large number of X-ray sources in a single pointing and is thus an extremely efficient use of Chandra-HETG. High resolution X-ray spectroscopy offers a means to investigate detailed spectral characteristic of X-ray emitting plasmas and their surrounding environments. We present preliminary results where we compare X-ray spectral signatures (e.g., luminosity, temperature, column density, abundance) of the X-ray brightest pre-MS stars in IC 348 with spectral type, multiwavelength signatures of accretion, and the presence of circumstellar disks at multiple stages of pre-MS stellar evolution. Assuming all IC 348 members formed from the same primordial molecular cloud, any disparity between coronal abundances of individual members, as constrained by the identification and strength of emission lines, will constrain the source(s) of coronal chemical evolution at a stage of pre-MS evolution vital to the formation of planets.

  5. Discovery of Spatial and Spectral Structure in the X-Ray Emission from the Crab Nebula

    NASA Technical Reports Server (NTRS)

    Weisskopf, Martin C.; Hester, J. Jeff; Tennant, Allyn F.; Elsner, Ronald F.; Schulz, Norbert S.; Marshall, Herman L.; Karovska, Margarita; Nichols, Joy S.; Swartz, Douglas A.; Kolodziejczak, Jeffery J.

    2000-01-01

    The Chandra X-Ray Observatory observed the Crab Nebula and pulsar during orbital calibration. Zeroth-order images with the High-Energy Transmission Grating (HETG) readout by the Advanced Charge Coupled Devices (CCD) Imaging Spectrometer spectroscopy array (ACIS-S) show a striking richness of X-ray structure at a resolution comparable to that of the best ground-based visible-light observations. The HETG-ACIS-S images reveal, for the first time, an X-ray inner ring within the X-ray torus, the suggestion of a hollow-tube structure for the torus, and X-ray knots along the inner ring and (perhaps) along the inward extension of the X-ray jet. Although complicated by instrumental effects and the brightness of the Crab Nebula, the spectrometric analysis shows systematic variations of the X-ray spectrum throughout the nebula.

  6. Discovery of Spatial and Spectral Structure in the X-Ray Emission from the Crab Nebula.

    PubMed

    Weisskopf; Hester; Tennant; Elsner; Schulz; Marshall; Karovska; Nichols; Swartz; Kolodziejczak; O'Dell

    2000-06-20

    The Chandra X-Ray Observatory observed the Crab Nebula and pulsar during orbital calibration. Zeroth-order images with the High-Energy Transmission Grating (HETG) readout by the Advanced CCD Imaging Spectrometer spectroscopy array (ACIS-S) show a striking richness of X-ray structure at a resolution comparable to that of the best ground-based visible-light observations. The HETG-ACIS-S images reveal, for the first time, an X-ray inner ring within the X-ray torus, the suggestion of a hollow-tube structure for the torus, and X-ray knots along the inner ring and (perhaps) along the inward extension of the X-ray jet. Although complicated by instrumental effects and the brightness of the Crab Nebula, the spectrometric analysis shows systematic variations of the X-ray spectrum throughout the nebula.

  7. Topics in Astrophysical X-Ray and Gamma Ray Spectroscopy. Ph.D. Thesis - Maryland Univ.

    NASA Technical Reports Server (NTRS)

    Bussard, R. W.

    1978-01-01

    A number of topics relating to astrophysical observations that have already been made or are currently planned of spectral features, mostly emission lines, in the X-ray and gamma ray region of the electromagnetic spectrum are investigated. These topics include: the production of characteristic X-ray and gamma ray lines by nonthermal ions, spectral features induced by processes occurring in strong magnetic fields, and the positron annihilation line at 0.5 MeV. The rate of X-ray production at 6.8 keV by the 2p to 1s transition in fast hydrogen- and helium-like iron ions, following both electron capture to excited levels and collisional excitation is calculated. The cross section for electron-ion Coulomb collisions in strong fields is also calculated.

  8. Study of Cr(VI) adsorption onto magnetite nanoparticles using synchrotron-based X-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Chen, Yen-Hua; Liu, Dian-Yu; Lee, Jyh-Fu

    2018-04-01

    In this study, the efficiency of Cr(VI) adsorption onto nano-magnetite was examined by batch experiments, and the Cr(VI) adsorption mechanism was investigated using synchrotron-based X-ray absorption spectroscopy. Magnetite nanoparticles with a mean diameter of 10 nm were synthesized using an inexpensive and simple co-precipitation method. It shows a saturation magnetization of 54.3 emu/g, which can be recovered with an external magnetic field. The adsorption data fitted the Langmuir adsorption isotherm well, implying a monolayer adsorption behavior of Cr(VI) onto nano-magnetite. X-ray absorption spectroscopy results indicate that the adsorption mechanism involves electron transfer between Fe(II) in nano-magnetite (Fe2+OFe3+ 2O3) and Cr(VI) to transform into Cr(III), which may exist as an Fe(III)-Cr(III) mixed solid phase. Moreover, the Cr(III)/Cr(VI) ratio in the final products can be determined by the characteristic pre-edge peak area of Cr(VI) in the Cr K-edge spectrum. These findings suggest that nano-magnetite is effective for Cr(VI) removal from wastewater because it can transform highly poisonous Cr(VI) species into nontoxic Cr(III) compounds, which are highly insoluble and immobile under environmental conditions.

  9. Energy dispersive X-ray analysis on an absolute scale in scanning transmission electron microscopy.

    PubMed

    Chen, Z; D'Alfonso, A J; Weyland, M; Taplin, D J; Allen, L J; Findlay, S D

    2015-10-01

    We demonstrate absolute scale agreement between the number of X-ray counts in energy dispersive X-ray spectroscopy using an atomic-scale coherent electron probe and first-principles simulations. Scan-averaged spectra were collected across a range of thicknesses with precisely determined and controlled microscope parameters. Ionization cross-sections were calculated using the quantum excitation of phonons model, incorporating dynamical (multiple) electron scattering, which is seen to be important even for very thin specimens. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. X-rays from Magnetic B-type Stars

    NASA Astrophysics Data System (ADS)

    Fletcher, Corinne; Petit, Véronique; Caballero-Nieves, Saida Maria; Nazé, Yaël; Owocki, Stan; Wade, Gregg; Cohen, David; Townsend, Richard; David-Uraz, Alexandre; Shultz, Matt

    2018-01-01

    Recent surveys have found that ~10% of OB-type stars host strong (~1kG), mostly dipolar magnetic fields. The prominent idea describing the interaction between the stellar winds and the magnetic field is the magnetically confined wind shock model. In this model, the ionized wind material is forced to move along the closed magnetic field loops and collides at the magnetic equator creating a shock. As the shocked material cools radiatively it will emit X-rays. Therefore, X-ray spectroscopy is a key tool in detecting and characterizing the wind material confined by the magnetic fields of these stars. Some of these magnetic B-type stars are found to have very short rotational periods. The effects of the rapid rotation on the X-ray production within the magnetosphere have yet to be explored in detail. The added centrifugal force is predicted to cause faster wind outflows along the field lines, which could lead to higher shock temperatures and harder X-rays. However, this is not observed in all rapidly rotating magnetic B-type stars. In order to address this question from a theoretical point of view, we use the X-ray Analytical Dynamical Magnetosphere model, developed for slow rotators and implement the physics of rapid rotation. Using X-ray spectroscopy from ESA’s XMM-Newton space telescope, we observed 5 rapidly rotating B-types stars to add to the previous list of observations. Comparing the observed X-ray luminosity and hardness ratio to that predicted by the XADM allows us to determine the role an added centrifugal acceleration plays in the magnetospheres of these stars.

  11. Measuring the Dust Grains and Distance to X Persei Via Its X-ray Halo

    NASA Astrophysics Data System (ADS)

    Smith, Randall

    2006-09-01

    We propose to observe the X-ray halo of the high mass X-ray binary pulsar X Per to measure interstellar dust grains along the line of sight (LOS) and to determine the distance to X Per. The X-ray halo is formed by scattering from grains along the LOS, which for X Per appear to be concentrated in one molecular cloud. Unlike many other X-ray halo observations, this low-absorption high-latitude sightline is well-characterized from absorption spectroscopy done with HST, Copernicus, and FUSE. This halo observation will measure the distance to the cloud and the dust size distribution in it. We will also be able to determine the distance to X Per by measuring the time delayed pulses in the X-ray halo.

  12. Chemical imaging analysis of the brain with X-ray methods

    NASA Astrophysics Data System (ADS)

    Collingwood, Joanna F.; Adams, Freddy

    2017-04-01

    Cells employ various metal and metalloid ions to augment the structure and the function of proteins and to assist with vital biological processes. In the brain they mediate biochemical processes, and disrupted metabolism of metals may be a contributing factor in neurodegenerative disorders. In this tutorial review we will discuss the particular role of X-ray methods for elemental imaging analysis of accumulated metal species and metal-containing compounds in biological materials, in the context of post-mortem brain tissue. X-rays have the advantage that they have a short wavelength and can penetrate through a thick biological sample. Many of the X-ray microscopy techniques that provide the greatest sensitivity and specificity for trace metal concentrations in biological materials are emerging at synchrotron X-ray facilities. Here, the extremely high flux available across a wide range of soft and hard X-rays, combined with state-of-the-art focusing techniques and ultra-sensitive detectors, makes it viable to undertake direct imaging of a number of elements in brain tissue. The different methods for synchrotron imaging of metals in brain tissues at regional, cellular, and sub-cellular spatial resolution are discussed. Methods covered include X-ray fluorescence for elemental imaging, X-ray absorption spectrometry for speciation imaging, X-ray diffraction for structural imaging, phase contrast for enhanced contrast imaging and scanning transmission X-ray microscopy for spectromicroscopy. Two- and three-dimensional (confocal and tomographic) imaging methods are considered as well as the correlation of X-ray microscopy with other imaging tools.

  13. ATHENA, ARTEMIS, HEPHAESTUS: data analysis for X-ray absorption spectropscopy using IFEFFIT

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Ravel, B.; Newville, M.; UC)

    2010-07-20

    A software package for the analysis of X-ray absorption spectroscopy (XAS) data is presented. This package is based on the IFEFFIT library of numerical and XAS algorithms and is written in the Perl programming language using the Perl/Tk graphics toolkit. The programs described here are: (i) ATHENA, a program for XAS data processing, (ii) ARTEMIS, a program for EXAFS data analysis using theoretical standards from FEFF and (iii) HEPHAESTUS, a collection of beamline utilities based on tables of atomic absorption data. These programs enable high-quality data analysis that is accessible to novices while still powerful enough to meet the demandsmore » of an expert practitioner. The programs run on all major computer platforms and are freely available under the terms of a free software license.« less

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

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Butterworth, A.L.; Becker, N.; Gainsforth, Z.

    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 synchrotronmore » 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

  15. X-ray Photoelectron Spectroscopy Study of Argon-Plasma-Treated Fluoropolymers

    NASA Technical Reports Server (NTRS)

    Golub, Morton A.; Lopata, Eugene S.; Finney, Lorie S.

    1994-01-01

    Films of poly(tetrafluoroethylene) (PTFE) and of a tetrafluoroethylene-perfluoroalkyl vinyl ether (approximately 49:1) copolymer (PFA) were exposed to a radio-frequency argon plasma and then examined by X-ray photoelectron spectroscopy (XPS). The use of fluoropolymer films nearly free of surface hydrocarbon contamination as well as the use of a monochromatized X-ray source for XPS removed two factors contributing to conflicting reports on the effect of exposure time on the fluorine-to-carbon (F/C) and oxygen-to-carbon (O/C) ratios for several Ar-plasma-treated fluoropolymers. Contrary to literature indications, a common pattern was found for PTFE and PFA: a moderate decrease in F/C ratio (from 1.99 to 1.40, and from 1.97 to 1.57, respectively), together with a moderate increase in O/C ratio (from negligible to about 0.10, and from 0.012 to about O.10, respectively) at very short exposures, after which the F/C ratios remained essentially constant on prolonged exposures, while the O/C ratios for PTFE and PFA leveled off at 0.11 and 0.15, respectively. The XPS C(sub 1s), spectra for these polymers exposed to the Ar plasma for 20 min were similar and presented, besides a prominent peak at 292.0 eV (CF2,) and a minor peak at 294.0 or 294.1 eV (CF3), a composite band of four curve-resolved peaks (approximately 285-290 eV) representing various CH, CC, CO, CN, and CF functionalities.

  16. Lu1-xI3:Cex--A Scintillator for gamma ray spectroscopy and time-of-flight PET

    DOEpatents

    Shah, Kanai S [Newton, MA

    2009-03-17

    The present invention concerns very fast scintillator materials comprising lutetium iodide doped with Cerium Lu.sub.1-xI.sub.3:Ce.sub.x; LuI.sub.3:Ce). The LuI.sub.3 scintillator material has surprisingly good characteristics including high light output, high gamma ray stopping efficiency, fast response, low cost, good proportionality, and minimal afterglow that the material is useful for gamma ray spectroscopy, medical imaging, nuclear and high energy physics research, diffraction, non-destructive testing, nuclear treaty verification and safeguards, and geological exploration. The timing resolution of the scintillators of the present invention provide compositions capable of resolving the position of an annihilation event within a portion of a human body cross-section.

  17. Magnetic x-ray dichroism in ultrathin epitaxial films

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Tobin, J.G.; Goodman, K.W.; Cummins, T.R.

    1997-04-01

    The authors have used Magnetic X-ray Linear Dichroism (MXLD) and Magnetic X-ray Circular Dichroism (MXCD) to study the magnetic properties of epitaxial overlayers in an elementally specific fashion. Both MXLD and MXCD Photoelectron Spectroscopy were performed in a high resolution mode at the Spectromicroscopy Facility of the ALS. Circular Polarization was obtained via the utilization of a novel phase retarder (soft x-ray quarter wave plate) based upon transmission through a multilayer film. The samples were low temperature Fe overlayers, magnetic alloy films of NiFe and CoNi, and Gd grown on Y. The authors results include a direct comparison of highmore » resolution angle resolved Photoelectron Spectroscopy performed in MXLD and MXCD modes as well as structural studies with photoelectron diffraction.« less

  18. Auger electron spectroscopy and x-ray photoelectron spectroscopy of the biocorrosion of copper by Gum Arabic, BCS and Pseudomonas atlantica exopolymer

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Jolley, J.G.; Geesey, G.G.; Hankins, M.R.

    1987-01-01

    Thin films (3.4 nm) of copper on germanium substrates were exposed to 10% Gum Arabic aqueous solution, 1% BCS (aqueous and simulated sea water solutions) and 0.5% Pseudomonas atlantica exopolymer (aqueous and simulated sea water solutions). Pre- and post-exposure characterization were done by Auger electron spectroscopy and x-ray photoelectron spectroscopy. Ancillary graphite furnace atomic absorption spectroscopy was used to monitor the removal process of the copper thin film from the germanium substrate. Results indicate that the copper was oxidized by the Gum Arabic and BCS, and some was removed from the Cu/Ge interface by all three polymers and incorporated intomore » the polymer matrix. Thus biocorrosion of copper was exhibited by the Gum Arabic, BCS and Pseudomonas atlantica exopolymer. 14 refs., 4 figs., 3 tabs.« less

  19. Growth, characterization and estimation of lattice strain and size in CdS nanoparticles: X-ray peak profile analysis

    NASA Astrophysics Data System (ADS)

    Solanki, Rekha Garg; Rajaram, Poolla; Bajpai, P. K.

    2018-05-01

    This work is based on the growth, characterization and estimation of lattice strain and crystallite size in CdS nanoparticles by X-ray peak profile analysis. The CdS nanoparticles were synthesized by a non-aqueous solvothermal method and were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman and UV-visible spectroscopy. XRD confirms that the CdS nanoparticles have the hexagonal structure. The Williamson-Hall (W-H) method was used to study the X-ray peak profile analysis. The strain-size plot (SSP) was used to study the individual contributions of crystallite size and lattice strain from the X-rays peaks. The physical parameters such as strain, stress and energy density values were calculated using various models namely, isotropic strain model, anisotropic strain model and uniform deformation energy density model. The particle size was estimated from the TEM images to be in the range of 20-40 nm. The Raman spectrum shows the characteristic optical 1LO and 2LO vibrational modes of CdS. UV-visible absorption studies show that the band gap of the CdS nanoparticles is 2.48 eV. The results show that the crystallite size estimated from Scherrer's formula, W-H plots, SSP and the particle size calculated by TEM images are approximately similar.

  20. Calibration of X-Ray Observatories

    NASA Technical Reports Server (NTRS)

    Weisskopf, Martin C.; L'Dell, Stephen L.

    2011-01-01

    Accurate calibration of x-ray observatories has proved an elusive goal. Inaccuracies and inconsistencies amongst on-ground measurements, differences between on-ground and in-space performance, in-space performance changes, and the absence of cosmic calibration standards whose physics we truly understand have precluded absolute calibration better than several percent and relative spectral calibration better than a few percent. The philosophy "the model is the calibration" relies upon a complete high-fidelity model of performance and an accurate verification and calibration of this model. As high-resolution x-ray spectroscopy begins to play a more important role in astrophysics, additional issues in accurately calibrating at high spectral resolution become more evident. Here we review the challenges of accurately calibrating the absolute and relative response of x-ray observatories. On-ground x-ray testing by itself is unlikely to achieve a high-accuracy calibration of in-space performance, especially when the performance changes with time. Nonetheless, it remains an essential tool in verifying functionality and in characterizing and verifying the performance model. In the absence of verified cosmic calibration sources, we also discuss the notion of an artificial, in-space x-ray calibration standard. 6th