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Sample records for x-ray spectroscopy instrumentation

  1. 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.

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

    SciTech Connect

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

    2015-03-03

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

  3. X-ray emission spectroscopy.

    PubMed

    Bergmann, Uwe; Glatzel, Pieter

    2009-01-01

    We describe the chemical information that can be obtained by means of hard X-ray emission spectroscopy (XES). XES is presented as a technique that is complementary to X-ray absorption spectroscopy (XAS) and that provides valuable information with respect to the electronic structure (local charge- and spin-density) as well as the ligand environment of a 3d transition metal. We address non-resonant and resonant XES and present results that were recorded on Mn model systems and the Mn(4)Ca-cluster in the oxygen evolving complex of photosystem II. A brief description of the instrumentation is given with an outlook toward future developments.

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

    NASA Astrophysics Data System (ADS)

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

    2016-04-01

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

  5. X-ray Absorption Spectroscopy

    SciTech Connect

    Yano, Junko; Yachandra, Vittal K.

    2009-07-09

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

  6. Instrument for x-ray absorption spectroscopy with in situ electrical control characterizations

    SciTech Connect

    Huang, Chun-Chao; Chang, Shu-Jui; Yang, Chao-Yao; Tseng, Yuan-Chieh; Chou, Hsiung

    2013-12-15

    We report a synchrotron-based setup capable of performing x-ray absorption spectroscopy and x-ray magnetic circular dichroism with simultaneous electrical control characterizations. The setup can enable research concerning electrical transport, element- and orbital-selective magnetization with an in situ fashion. It is a unique approach to the real-time change of spin-polarized electronic state of a material/device exhibiting magneto-electric responses. The performance of the setup was tested by probing the spin-polarized states of cobalt and oxygen of Zn{sub 1-x}Co{sub x}O dilute magnetic semiconductor under applied voltages, both at low (∼20 K) and room temperatures, and signal variations upon the change of applied voltage were clearly detected.

  7. 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.

  8. 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.

  9. Technology development for soft X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

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

    2016-05-01

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

  10. 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.

  11. X-ray Spectroscopy of Cooling Cluster

    SciTech Connect

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

    2006-01-17

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

  12. Resonant x-ray emission spectroscopy of liquid water: novel instrumentation, high resolution, and the"map" approach

    SciTech Connect

    Weinhardt, L.; Fuchs, O.; Blum, M.; Bär, M.; Weigand, M.; Denlinger, J.D.; Zubavichus, Y.; Zharnikov, M.; Grunze, M.; Heske, C.; Umbach, E.

    2008-06-17

    Techniques to study the electronic structure of liquids are rare. Most recently, resonant x-ray emission spectroscopy (XES) has been shown to be an extremely versatile spectroscopy to study both occupied and unoccupied electronic states for liquids in thermodynamic equilibrium. However, XES requires high-brilliance soft x-ray synchrotron radiation and poses significant technical challenges to maintain a liquid sample in an ultra-high vacuum environment. Our group has therefore developed and constructed a novel experimental setup for the study of liquids, with the long-term goal of investigating the electronic structure of biological systems in aqueous environments. We have developed a flow-through liquid cell in which the liquid is separated from vacuum by a thin Si3N4 or SiC window and which allows a precise control of temperature. This approach has significant advantages compared to static liquids cells used in the past. Furthermore, we have designed a dedicated high-transmission, high-resolution soft x-ray spectrometer. The high transmission makes it possible to measure complete resonant XES"maps" in less than an hour, giving unprecedented detailed insight into the electronic structure of the investigated sample. Using this new equipment we have investigated the electronic structure of liquid water. Furthermore, our XES spectra and maps give information about ultra-fast dissociation on the timescale of the O 1s core hole lifetime, which is strongly affected by the initial state hydrogen bonding configuration.

  13. X-ray spectroscopy of magnetic CVs

    NASA Astrophysics Data System (ADS)

    Matt, Giorgio

    I discuss two topics in X-ray spectroscopy of magnetic CVs: reflection from the white dwarf surface, and opacity effects in the post shock plasma. I also briefly mention future observational perspectives, with particular emphasis on the Constellation X-ray mission.

  14. 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.

  15. European XFEL: Soft X-Ray instrumentation

    SciTech Connect

    Molodtsov, S. L.

    2011-12-15

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

  16. Instrumentation for X-ray Astronomy

    NASA Technical Reports Server (NTRS)

    Ramsey, Brian D.; Austin, Robert A.; Decher, Rudolf

    1994-01-01

    Less than five decades ago, the first X-ray observations of the sky were made using simple devices such as film and geiger counters with crude collimators. These instruments were carried aloft by sounding rockets and made observations lasting only a few minutes at most. Today, orbiting observatories, utilizing high-resolution charged coupled devices (CCD's) at the focus of arc sec optics, have lifetimes measured in years. To maintain the pace of discovery in X-ray astronomy, detectors must continue to evolve into devices of ever increasing sensitivity and sophistication. Further progress depends upon a host of technologies: grazing incidence optics, proportional counters, semiconductors, calorimeters, etc. In this article we present a brief qualitative overview of these technologies and of the principles behind them, as well as some examples of how they are employed in scientific missions for X-ray observations at energies up to 100 keV.

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

    NASA Technical Reports Server (NTRS)

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

    2013-01-01

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

  18. 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.

  19. 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.

  20. Hard x-ray photoelectron spectroscopy and x-ray standing waves

    NASA Astrophysics Data System (ADS)

    Lee, Tien-Lin

    2006-03-01

    Using the brilliant undulator radiation available from the third generation synchrotron sources, hard x-ray photoelectron spectroscopy (HAXPES) has become an emerging field in the recent years. With the excitation energy used in HAXPES one can benefits from the large mean free path of fast electrons (˜ 5 nm for electrons of 6 keV kinetic energy) in probing the bulk electronic properties of materials. For high-resolution studies, photon energy bandwidth narrower than 100 meV is also readily achievable in the hard x-ray range with crystal monochromators. In addition, working with hard x-ray offers the possibility for combining photoelectron spectroscopy with x-ray standing wave (XSW) method. With the high spatial resolution from XSWs, this unique combination can provide site-specific, chemical and electronic information for studying surfaces, buried interfaces, thin films and bulk crystals. In this talk, I will briefly mention some HAXPES experiments detecting electrons up to 14.5 keV [1,2]. I will then sketch the principle of combining XSWs with HAXPES and present results from some recent applications using this combination: (1) chemical state-specific surface structure determination with core-level photoemission, (2) site-specific valence x-ray photoelectron spectroscopy and (3) XSW imaging with core-level photoemission. [1] S. Thiess, C. Kunz, B.C.C. Cowie, T.-L. Lee, M. Renier, and J. Zegenhagen. Solid State Communications 132, 589 (2004) [2] C. Kunz, S. Thiess, B.C.C. Cowie, T.-L. Lee, and J. Zegenhagen, Nuclear Instruments and Methods A 547, 73 (2005).

  1. X-ray instrumentation in astronomy II; Proceedings of the Meeting, San Diego, CA, Aug. 15-17, 1988

    SciTech Connect

    Golub, L.

    1988-01-01

    Various papers on X-ray instrumentation in astronomy are presented. Individual topics addressed include: concentrating hard X-ray collector, advanced X-ray Astrophysics Facility high resolution camera, Fano-noise-limited CCDs, linear CCD with enhanced X-ray quantum efficiency, advances in microchannel plate detectors, X-ray imaging spectroscopy with EEV CCDs, large aperture imaging gas scintillation proportional counter, all-sky monitor for the X-ray Timing Explorer, and miniature satellite technology capabilities for space astronomy. Also discussed are: high-resolution X-ray spectroscopy using microcalorimeters, high-throughput X-ray astrophysics cornerstone, gas mixtures for X-ray proportional counters, transmission grating spectrometer for SPEKTROSAT, efficiency of X-ray reflection gratings, soft X-ray spectrographs for solar observations, observability of coronal variations, Berkeley extreme-UV calibration facility, SURF-II radiometric instrumentation calibration facility, and evaluation of toroidal gratings in the EUV.

  2. 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.

  3. In situ soft X-ray absorption spectroscopy of flames

    NASA Astrophysics Data System (ADS)

    Frank, Jonathan H.; Shavorskiy, Andrey; Bluhm, Hendrik; Coriton, Bruno; Huang, Erxiong; Osborn, David L.

    2014-10-01

    The feasibility of in situ soft X-ray absorption spectroscopy for imaging carbonaceous species in hydrocarbon flames is demonstrated using synchrotron radiation. Soft X-rays are absorbed by core level electrons in all carbon atoms regardless of their molecular structure. Core electron spectroscopy affords distinct advantages over valence spectroscopy, which forms the basis of traditional laser diagnostic techniques for combustion. In core level spectroscopy, the transition linewidths are predominantly determined by the instrument response function and the decay time of the core-hole, which is on the order of a femtosecond. As a result, soft X-ray absorption measurements can be performed in flames with negligible Doppler and collisional broadening. Core level spectroscopy has the further advantage of measuring all carbonaceous species regardless of molecular structure in the far-edge region, whereas near-edge features are molecule specific. Interferences from non-carbon flame species are unstructured and can be subtracted. In the present study, absorption measurements in the carbon K-edge region are demonstrated in low-pressure ( P total = 20-30 Torr) methane jet flames. Two-dimensional imaging of the major carbonaceous species, CH4, CO2, and CO, is accomplished by tuning the synchrotron radiation to the respective carbon K-edge, near-edge X-ray absorption fine structure (NEXAFS) transitions and scanning the burner.

  4. 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.

  5. X-ray resonant Raman spectroscopy

    SciTech Connect

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

    1995-08-01

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

  6. X-ray diffraction: instrumentation and applications.

    PubMed

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

    2015-01-01

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

  7. Hard X-ray imaging spectroscopy of FOXSI microflares

    NASA Astrophysics Data System (ADS)

    Glesener, Lindsay; Krucker, Sam; Christe, Steven; Camilo Buitrago-Casas, Juan; 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. 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 ~106 photons/s, by focusing the produced x-rays with a polycapillary optic. Since the acquisition of x-ray absorption spectra requires the averaging of measurements from >107 laser pulses, we also presentmore » data on the source stability, including single pulse measurements of the x-ray yield and the x-ray spectral shape. In single pulse measurements, the x-ray flux has a measured standard deviation of 8%, where the laser pointing is the main cause of variability. Further, we show that the variability in x-ray spectral shape from single pulses is low, thus justifying the combining of x-rays obtained from different laser pulses into a single spectrum. Finally, we show a static x-ray absorption spectrum of a ferrioxalate solution as detected by a microcalorimeter array. Altogether, our results demonstrate that this water-jet based plasma source is a suitable candidate for laboratory-based time-resolved x-ray absorption spectroscopy experiments.« less

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

    PubMed Central

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

    2015-01-01

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

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

    SciTech Connect

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

    2015-03-02

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

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

    PubMed

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

    2015-03-01

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

  12. Miniaturization in x ray and gamma ray spectroscopy

    NASA Technical Reports Server (NTRS)

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

    1993-01-01

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

  13. X-ray photoelectron spectroscopy in the hard x-ray regime

    NASA Astrophysics Data System (ADS)

    Fadley, Charles S.

    2006-03-01

    Photoelectron spectroscopy is by now a very widely used tool for the study of atoms, molecules, solids, surfaces, and nanoscale structures. Until very recently, the exciting radiation has been limited to the energy range below about 2 keV. However, within the past few years, a few experimental projects have been initiated in which photon energies in the 5-15 keV range are employed. By matching the characteristics of undulator beamlines at third-generation synchrotron radiation sources to the optical properties of the electron spectrometer, it has proven possible to overcome the reduced photoelectric cross sections at such high energies and to study both core and valence electronic levels with resolutions down to ca. 50 meV [1]. Such hard x-ray photoelectron spectroscopy (HXPS or HAXPES) has the advantage of being more bulk sensitive, with electron inelastic attenuation lengths in the 50-150 Angstrom range. In this talk, I will discuss the advantages and disadvantages of this new direction, including highlights from recent work, as well as suggested future avenues for HXPS studies. [1] Nuclear Instruments and Methods A 547, 24 (2005), special issue dedicated to hard x-ray photoelectron spectroscopy, edited by J. Zegenhagen and C. Kunz.

  14. New Developments in Femtosecond Soft X-ray Spectroscopy

    SciTech Connect

    Erko, A.; Firsov, A.; Holldack, K.

    2010-06-23

    Recent instrumentation developments in X-ray spectroscopy for ultra-fast time-resolved measurements with soft X-rays done in HZB Berlin during the last years are described. The significant performance improvements achieved this way are based on Fresnel diffraction from structures being fabricated on a surface of a total externally reflecting mirror. The first type of this spectrometer, an off-axis reflection zone plate, has been implemented at the BESSY Femtoslicing setup and shows on the order of 20 times higher flux in the focal plane compared to the classical grating monochromator beamline. It has proven to serve very precise experiments with a time resolution down to 100 fs on magnetic materials after optical laser pulse excitation.

  15. Suborbital Soft X-Ray Spectroscopy with Gaseous Electron Multipliers

    NASA Astrophysics Data System (ADS)

    Rogers, Thomas D.

    This thesis consists of the design, fabrication, and launch of a sounding rocket payload to observe the spectrum of the soft X-ray emission (0.1-1 keV) from the Cygnus Loop supernova remnant. This instrument, designated the Off-plane Grating Rocket for Extended Source Spectroscopy (OGRESS), was launched from White Sands Missile Range on May 2nd, 2015. The X-ray spectrograph incorporated a wire-grid focuser feeding an array of gratings in the extreme off-plane mount which dispersed the spectrum onto Gaseous Electron Multiplier (GEM) detectors. The gain characteristics of OGRESS's GEM detectors were fully characterized with respect to applied voltage and internal gas pressure, allowing operational settings to be optimized. The GEMs were optimized to operate below laboratory atmospheric pressure, allowing lower applied voltages, thus reducing the risk of both electrical arcing and tearing of the thin detector windows. The instrument recorded 388 seconds of data and found highly uniform count distributions over both detector faces, in sharp contrast to the expected thermal line spectrum. This signal is attributed to X-ray fluorescence lines generated inside the spectrograph. The radiation is produced when thermal ionospheric particles are accelerated into the interior walls of the spectrograph by the high voltages of the detector windows. A fluorescence model was found to fit the flight data better than modeled supernova spectra. Post-flight testing and analysis revealed that electrons produce distinct signal on the detectors which can also be successfully modeled as fluorescence emission.

  16. 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.

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

    NASA Technical Reports Server (NTRS)

    Mori, Shigeyuki; Morales, Wilfredo

    1990-01-01

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

  18. X-ray ferromagnetic resonance spectroscopy

    SciTech Connect

    Boero, G.; Rusponi, S.; Bencok, P.; Popovic, R.S.; Brune, H.; Gambardella, P.

    2005-10-10

    We present a method to measure continuous-wave ferromagnetic resonance (FMR) spectra based on the core-level absorption of circularly polarized x rays. The technique is demonstrated by using a monochromatic x-ray beam incident on an yttrium-iron-garnet sample excited by a microwave field at 2.47 GHz. FMR spectra are obtained by monitoring the x-ray absorption intensity at the photon energy corresponding to the maximum of the magnetic circular dichroism effect at the iron L{sub 2,3} edges as a function of applied magnetic field. The x-ray FMR signal is shown to be energy dependent, which makes the technique element sensitive and opens up new possibilities to perform element-resolved FMR in magnetic alloys and multilayers.

  19. 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.

  20. Current Problems in X-Ray Emission Spectroscopy

    NASA Technical Reports Server (NTRS)

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

    1989-01-01

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

  1. 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.

  2. Tokamak Spectroscopy for X-Ray Astronomy

    NASA Technical Reports Server (NTRS)

    Fournier, Kevin B.; Finkenthal, M.; Pacella, D.; May, M. J.; Soukhanovskii, V.; Mattioli, M.; Leigheb, M.; Rice, J. E.

    2000-01-01

    This paper presents the measured x-ray and Extreme Ultraviolet (XUV) spectra of three astrophysically abundant elements (Fe, Ca and Ne) from three different tokamak plasmas. In every case, each spectrum touches on an issue of atomic physics that is important for simulation codes to be used in the analysis of high spectral resolution data from current and future x-ray telescopes. The utility of the tokamak as a laboratory test bed for astrophysical data is demonstrated. Simple models generated with the HULLAC suite of codes demonstrate how the atomic physics issues studied can affect the interpretation of astrophysical data.

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

    SciTech Connect

    Rubio-Zuazo, Juan; Castro, German R.

    2013-05-15

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

  4. X-ray spectroscopy of manganese clusters

    SciTech Connect

    Grush, M.M. |

    1996-06-01

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

  5. Stimulated X-ray Raman scattering - a critical assessment of the building block of nonlinear X-ray spectroscopy.

    PubMed

    Kimberg, Victor; Sanchez-Gonzalez, Alvaro; Mercadier, Laurent; Weninger, Clemens; Lutman, Alberto; Ratner, Daniel; Coffee, Ryan; Bucher, Maximilian; Mucke, Melanie; Agåker, Marcus; Såthe, Conny; Bostedt, Christoph; Nordgren, Joseph; Rubensson, Jan Erik; Rohringer, Nina

    2016-12-16

    With the invention of femtosecond X-ray free-electron lasers (XFELs), studies of light-induced chemical reaction dynamics and structural dynamics reach a new era, allowing for time-resolved X-ray diffraction and spectroscopy. To ultimately probe coherent electron and nuclear dynamics on their natural time and length scales, coherent nonlinear X-ray spectroscopy schemes have been proposed. In this contribution, we want to critically assess the experimental realisation of nonlinear X-ray spectroscopy at current-day XFEL sources, by presenting first experimental attempts to demonstrate stimulated resonant X-ray Raman scattering in molecular gas targets.

  6. An X-ray diffraction and X-ray absorption spectroscopy joint study of neuroglobin.

    PubMed

    Arcovito, Alessandro; Moschetti, Tommaso; D'Angelo, Paola; Mancini, Giordano; Vallone, Beatrice; Brunori, Maurizio; Della Longa, Stefano

    2008-07-01

    Neuroglobin (Ngb) is a member of the globin family expressed in the vertebrate brain, involved in neuroprotection. A combined approach of X-ray diffraction (XRD) on single crystal and X-ray absorption spectroscopy (XAS) in solution, allows to determine the oxidation state and the structure of the Fe-heme both in the bis-histidine and the CO-bound (NgbCO) states. The overall data demonstrate that under X-ray the iron is photoreduced fairly rapidly, and that the previously reported X-ray structure of ferric Ngb [B. Vallone, K. Nienhaus, M. Brunori, G.U. Nienhaus, Proteins 56 (2004) 85-92] very likely refers to a photoreduced species indistinguishable from the dithionite reduced protein. Results from the XAS analysis of NgbCO in solution are in good agreement with XRD data on the crystal. However prolonged X-ray exposure at 15K determines CO release. This preliminary result paves the way to experiments aimed at the characterization of pentacoordinate ferrous Ngb, the only species competent in binding external ligands such as O2, CO or NO.

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

    NASA Technical Reports Server (NTRS)

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

    2012-01-01

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

  8. Temperature dependent soft x-ray absorption spectroscopy of liquids.

    PubMed

    Meibohm, Jan; Schreck, Simon; Wernet, Philippe

    2014-10-01

    A novel sample holder is introduced which allows for temperature dependent soft x-ray absorption spectroscopy of liquids in transmission mode. The setup is based on sample cells with x-ray transmissive silicon nitride windows. A cooling circuit allows for temperature regulation of the sample liquid between -10 °C and +50 °C. The setup enables to record soft x-ray absorption spectra of liquids in transmission mode with a temperature resolution of 0.5 K and better. Reliability and reproducibility of the spectra are demonstrated by investigating the characteristic temperature-induced changes in the oxygen K-edge x-ray absorption spectrum of liquid water. These are compared to the corresponding changes in the oxygen K-edge spectra from x-ray Raman scattering.

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

    NASA Technical Reports Server (NTRS)

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

    2010-01-01

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

  10. A high-resolution large-acceptance analyzer for X-ray fluorescence and Raman spectroscopy

    SciTech Connect

    Bergmann, Uwe; Cramer, Stephen P.

    2001-08-02

    A newly designed multi-crystal X-ray spectrometer and its applications in the fields of X-ray fluorescence and X-ray Raman spectroscopy are described. The instrument is based on 8 spherically curved Si crystals, each with a 3.5 inch diameter form bent to a radius of 86 cm. The crystals are individually aligned in the Rowland geometry capturing a total solid angle of 0.07 sr. The array is arranged in a way that energy scans can be performed by moving the whole instrument, rather than scanning each crystal by itself. At angles close to back scattering the energy resolution is between 0.3 and 1 eV depending on the beam dimensions at the sample. The instrument is mainly designed for X-ray absorption and fluorescence spectroscopy of transition metals in dilute systems such as metalloproteins. First results of the Mn K{beta} (3p -> 1s) emission in photosystem II are shown. An independent application of the instrument is the technique of X-ray Raman spectroscopy which can address problems similar to those in traditional soft X-ray absorption spectroscopies, and initial results are presented.

  11. X-ray spectroscopy to determine line coincidences

    NASA Astrophysics Data System (ADS)

    Burkhalter, P. G.; Charatis, G.; Rockett, P.

    1983-01-01

    X-ray spectroscopy in the 12-15 A region of L-shell lines from selected transition elements was performed in a joint Naval Research Laboratory - KMS Fusion, Inc. experiment. The accurate wavelengths determined in this work will be utilized in selecting potential pumping candidates in future X-ray lasing schemes. Specifically, high-resolution X-ray spectra were collected under controlled geometric and target conditions using both red and green light laser excitation in the KMS Chroma laser. Three groups of X-ray spectra were collected with highly-dispersive X-ray crystals at wavelengths centered at 12.543, 13.781 and 14.458 A corresponding to He- and H-like lines from fluorine. Two specially-designed flat crystal spectrographs employing film shutters were used with pairs of beryl and TAP crystals. The spectra from potential lasant and pump candidates could be recorded on the same spectrogram to aid in identifying X-ray line coincidences. In cases where wavelengths were measured in both the red and green laser work, agreement within 1-3 mA was obtained for the L-series X-ray lines. Within this accuracy range, five L series X-ray lines, mostly 2p-3d transitions from the metals Cr, Mn, and Ni, had wavelength values coincident to K-series lines in fluorine.

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

    NASA Astrophysics Data System (ADS)

    Noda, H.

    2015-09-01

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

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

    SciTech Connect

    Guo, J.-H.

    2005-07-30

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

  14. X-Ray Spectroscopy Using Low Temperature Detectors

    NASA Technical Reports Server (NTRS)

    Porter, Frederick

    2011-01-01

    After several decades of development, a significant amount of the effort in low temperature detectors (LTDs) is concentrated on deploying real-world experiments. This has resulted from a great deal of basic detector physics performed by several generations of students, post-docs, and researchers. One of the most fruitful applications of LTDs is in non-dispersive x-ray spectroscopy. LTD x-ray spectrometers are broadband, efficient, moderately high-resolution, and can handle moderately high count rates. However, they require significantly more power, mass, and infrastructure compared to traditional solid state x-ray spectrometers, and cannot achieve, at least at low energies, the resolving powers achieved with dispersive spectrometers. In several fields, however, LTDs have or will make a significant contribution. In this review, we will discuss x-ray spectroscopy in general, the fields of science where LTDs are making a significant impact, and some of the current and near-term LTD spectrometers.

  15. Combined surface plasmon resonance and X-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Garcia, Miguel Angel; Serrano, Aida; Rodriguez de La Fuente, Oscar; Castro, German R.

    2012-02-01

    We present a system for the excitation and measurement of surface plasmons in metallic films based on the Kretschmann-Raether configuration that can be installed in a synchrotron beamline. The device was mounted an tested in a hard X-ray Absorption beamline, BM25 Spline at ESRF. Whit this device it is possible to carry on experiments combining surface plasmon and X-ray absorption spectroscopies. The surface plasmons can be use to monitor in situ changes induced by the X-rays in the metallic films or the dielectric overlayer. Similarly, the changes in the electronic configuration of the material when surface plasmons are excited can be measured by X-ray absorption spectroscopy. The resolution of the system allows to observe changes in the signals of the order of 10-3 to 10-5 depending on the particular experiment and used configuration. The system is available for experiments at the beamline.

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

    NASA Astrophysics Data System (ADS)

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

    2004-08-01

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

  17. 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.

  18. Photoelectron and X-ray Absorption Spectroscopy Of Pu

    SciTech Connect

    Tobin, J; Chung, B; Schulze, R; Farr, J; Shuh, D

    2003-11-12

    We have performed Photoelectron Spectroscopy and X-Ray Absorption Spectroscopy upon highly radioactive samples of Plutonium at the Advanced Light Source in Berkeley, CA, USA. First results from alpha and delta Plutonium are reported as well as plans for future studies of actinide studies.

  19. Combining scanning probe microscopy and x-ray spectroscopy

    PubMed Central

    2011-01-01

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

  20. X-ray spectroscopy of AGN with the AXAF 'Microcalorimeter'

    NASA Astrophysics Data System (ADS)

    Holt, Stephen S.

    A novel technique for X-ray spectroscopy has been configured as part of the definition payload of the AXAF Observatory. It is basically a calorimeter which, operating at 0.1 K, senses the total conversion of single photoelectrically absorbed X-rays via the differential temperature rise of the absorber. The technique promises to achieve less than 10 eV FWHM with near-unit efficiency simultaneously over the entire AXAF bandpass. This combination of high resolution and high efficiency allows for the possibility of investigating thermal, fluorescent and absorption X-ray line features in many types of X-ray source, including a large sample of active galactic nuclei.

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

    SciTech Connect

    Tobin, J G

    2011-03-17

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

  2. 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.

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

    NASA Technical Reports Server (NTRS)

    Schattenburg, Mark L.

    2004-01-01

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

  4. Proton induced quasi-monochromatic x-ray beams for soft x-ray spectroscopy studies and selective x-ray fluorescence analysis

    SciTech Connect

    Sokaras, D.; Zarkadas, Ch.; Fliegauf, R.; Beckhoff, B.; Karydas, A. G.

    2012-12-15

    We present the analytical features and performance of an x-ray spectroscopy end station of moderate energy resolution operating with proton-induced quasi-monochromatic x-ray beams. The apparatus was designed, installed and operated at the 5.5 MV Tandem VdG Accelerator Laboratory of the Institute of Nuclear Physics, N.C.S.R. 'Demokritos,' Athens. The setup includes a two-level ultrahigh vacuum chamber that hosts in the lower level up to six primary targets in a rotatable holder; there, the irradiation of pure element materials-used as primary targets-with few-MeV high current ({approx}{mu}A) proton beams produces intense quasi-monochromatic x-ray beams of selectable energy. In the chamber's upper level, a six-position rotatable sample holder hosts the targets considered for x-ray spectroscopy studies. The proton-induced x-ray beam, after proper collimation, is guided to the sample position whereas various filters can be also inserted along the beam's path to eliminate the backscattered protons or/and to absorb selectively components of the x-ray beam. The apparatus incorporates an ultrathin window Si(Li) spectrometer (FWHM 136 eV at 5.89 keV) coupled with low-noise electronics capable of efficiently detecting photons down to carbon K{alpha}. Exemplary soft x-ray spectroscopy studies and results of selective x-ray fluorescence analysis are presented.

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

    NASA Astrophysics Data System (ADS)

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

    2010-03-01

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

  6. 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.

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

    PubMed

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

    2011-09-07

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

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

    SciTech Connect

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

    2012-08-15

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

  9. An upgraded x-ray spectroscopy diagnostic on MSTa)

    NASA Astrophysics Data System (ADS)

    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 Zeff and the particle diffusion coefficient Dr. 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 Zeff and Dr.

  10. Advanced X-ray Astrophysics Facility (AXAF) science instruments

    NASA Technical Reports Server (NTRS)

    Winkler, Carl E.; Dailey, Carroll C.; Cumings, Nesbitt P.

    1991-01-01

    The overall AXAF program is summarized, with particular emphasis given to its science instruments. The science objectives established for AXAF are to determine the nature of celestial objects, from normal stars to quasars, to elucidate the nature of the physical processes which take place in and between astronomical objects, and to shed light on the history and evolution of the universe. Attention is given to the AXAF CCD imaging spectrometer, which is to provide spectrally and temporally resolved imaging, or, in conjunction with transmission grating, high-resolution dispersed spectral images of celestial sources. A high-resolution camera, an X-ray spectrometer, and the Bragg Crystal Spectrometer are also discussed.

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

    NASA Astrophysics Data System (ADS)

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

    2015-08-01

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

  12. Soft X-ray spectroscopy of the Cygnus Loop

    NASA Astrophysics Data System (ADS)

    McEntaffer, Randall L.

    My thesis work consisted of the design, fabrication and launch of a sounding rocket payload to observe the spectrum of the soft X-ray emission from the Cygnus Loop supernova remnant. This payload was designated the Cygnus X-ray Emission Spectroscopic Survey (CyXESS) and launched from White Sands Missile Range on November 20th, 2006. The novel X-ray spectrograph incorporated a wire- grid collimator feeding an array of gratings in the extreme off-plane mount which ultimately dispersed the spectrum onto never before flown Gaseous Electron Multiplier (GEM) detectors. This instrument recorded 65 seconds of usable data between 43-49.5 Å in two prominent features. The first feature near 45 Å is dominated by the He-like triplet of O VII in second order with contributions from Mg X and Si IX-Si XII in first order, while the second feature near 47.5 Å is first order S IX and S X. Fits to the spectra give an equilibrium plasma at log( T )=6.2 ( kT e =0.14 keV) and near cosmic abundances. This is consistent with previous observations, which demonstrated that the soft x-ray emission from the Cygnus Loop is dominated by interactions between the initial blast wave with the walls of a precursor formed cavity surrounding the Cygnus Loop.

  13. 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.

  14. Crystal optics for precision x-ray spectroscopy on highly charged ions—conception and proof

    NASA Astrophysics Data System (ADS)

    Beyer, H. F.; Gassner, T.; Trassinelli, M.; Heß, R.; Spillmann, U.; Banaś, D.; Blumenhagen, K.-H.; Bosch, F.; Brandau, C.; Chen, W.; Dimopoulou, Chr; Förster, E.; Grisenti, R. E.; Gumberidze, A.; Hagmann, S.; Hillenbrand, P.-M.; Indelicato, P.; Jagodzinski, P.; Kämpfer, T.; Kozhuharov, Chr; Lestinsky, M.; Liesen, D.; Litvinov, Yu A.; Loetzsch, R.; Manil, B.; Märtin, R.; Nolden, F.; Petridis, N.; Sanjari, M. S.; Schulze, K. S.; Schwemlein, M.; Simionovici, A.; Steck, M.; Stöhlker, Th; Szabo, C. I.; Trotsenko, S.; Uschmann, I.; Weber, G.; Wehrhan, O.; Winckler, N.; Winters, D. F. A.; Winters, N.; Ziegler, E.

    2015-07-01

    The experimental investigation of quantum-electrodydamic contributions to the binding energies of inner shells of highly charged heavy ions requires an accurate spectroscopy in the region of hard x-rays suitable at a limited source strength. For this purpose the focusing compensated asymmetric Laue crystal optics has been developed and a twin-spectrometer assembly has been built and commissioned at the experimental storage ring of the GSI Helmholtzzentrum Darmstadt. We characterize the crystal optics and demonstrate the usefulness of the instrumentation for accurate spectroscopy of both stationary and fast moving x-ray sources. The experimental procedures discussed here may also be applied for other spectroscopic studies where a transition from conventional germanium x-ray detectors to crystal spectrometers seems too demanding because of low source intensity.

  15. Probing deeper by hard x-ray photoelectron spectroscopy

    SciTech Connect

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

    2014-02-03

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

  16. X-ray Photoelectron Spectroscopy of Isolated Nanoparticles.

    PubMed

    Sublemontier, Olivier; Nicolas, Christophe; Aureau, Damien; Patanen, Minna; Kintz, Harold; Liu, Xiaojing; Gaveau, Marc-André; Le Garrec, Jean-Luc; Robert, Emmanuel; Barreda, Flory-Anne; Etcheberry, Arnaud; Reynaud, Cécile; Mitchell, James B; Miron, Catalin

    2014-10-02

    X-ray photoelectron spectroscopy (XPS) is a very efficient and still progressing surface analysis technique. However, when applied to nano-objects, this technique faces drawbacks due to interactions with the substrate and sample charging effects. We present a new experimental approach to XPS based on coupling soft X-ray synchrotron radiation with an in-vacuum beam of free nanoparticles, focused by an aerodynamic lens system. The structure of the Si/SiO2 interface was probed without any substrate interaction or charging effects for silicon nanocrystals previously oxidized in ambient air. Complete characterization of the surface was obtained. The Si 2p core level spectrum reveals a nonabrupt interface.

  17. Soft x-ray spectroscopy of the Vela supernova remnant

    NASA Astrophysics Data System (ADS)

    Zeiger, Benjamin R.

    The CODEX sounding rocket payload was designed and flown to significantly improve spectral resolution of the Vela supernova remnant (SNR) in the soft x-ray (0.1--1.0 keV) bandpass. High spectral resolution (E/Delta E > 40) across its 3.25° x 3.25° field of view would disentangle thermal emission from nonthermal or line emission components to constrain the age when SNRs stop emitting nonthermal x-rays. Relatively recent observations have found significant nonthermal emission from remnants up to several kyr old, but CODEX encountered concurrent problems of higher noise and lower signal than expected, leaving the thermal versus nonthermal question unanswered in the 11 kyr-old Vela SNR. This thesis covers the motivation, design, and post-flight analysis of the CODEX instrument and data from its flight.

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

    NASA Astrophysics Data System (ADS)

    Remillard, Ronald A.

    2016-04-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-09-01

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

  20. 28 CFR 552.13 - X-ray, major instrument, fluoroscope, or surgical intrusion.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

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

  1. 28 CFR 552.13 - X-ray, major instrument, fluoroscope, or surgical intrusion.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

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

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

    Code of Federal Regulations, 2011 CFR

    2011-07-01

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

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

    Code of Federal Regulations, 2014 CFR

    2014-07-01

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

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

    Code of Federal Regulations, 2013 CFR

    2013-07-01

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

  5. 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

  6. Closed source experimental system for soft x-ray spectroscopy of radioactive materials

    SciTech Connect

    Modin, A.; Butorin, S. M.; Vegelius, J.; Olsson, A.; Englund, C.-J.; Andersson, J.; Werme, L.; Nordgren, J.; Kaeaembre, T.; Skarnemark, G.; Burakov, B. E.

    2008-09-15

    An instrumental and experimental setup for soft x-ray spectroscopy meeting the requirements of a closed source for radioactivity is described. The system consists of a vacuum sealed cell containing the sample, mounted on a tubing system to ensure compatibility with most standard manipulators. The soft x rays penetrate a thin x-ray window separating the interior of the cell from the vacuum in the experimental chamber. Our first results for single crystal PuO{sub 2} confirm the feasibility of experiments using the setup. The results are consistent with results of first principles calculations and previously recorded spectra obtained using a standard open source setup. The results show that the closed source experimental system can be used to collect valuable experimental data from radioactive materials.

  7. X-Ray Absorption Spectroscopy of Uranium Dioxide

    SciTech Connect

    Tobin, J G

    2010-12-10

    After the CMMD Seminar by Sung Woo Yu on the subject of the x-ray spectroscopy of UO2, there arose some questions concerning the XAS of UO2. These questions can be distilled down to these three issues: (1) The validity of the data; (2) The monchromator energy calibration; and (3) The validity of XAS component of the figure shown. The following will be shown: (1) The data is valid; (2) It is possible to calibrate the monchromator; and (3) The XAS component of the above picture is correct. The remainder of this document is in three sections, corresponding to these three issues.

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

    SciTech Connect

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

    2009-12-11

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

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

    NASA Astrophysics Data System (ADS)

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

    2011-10-01

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

  10. 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

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

    SciTech Connect

    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. 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 ions during the fragmentation of XeF2 molecules following X-ray absorption at the Xe site.

  12. 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.

  13. 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 XeF2 molecules following X-ray absorption at the Xe site.« less

  14. Hubbard Model Approach to X-ray Spectroscopy

    NASA Astrophysics Data System (ADS)

    Ahmed, Towfiq

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

  15. Individual heteroatom identification with X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

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

    2016-04-01

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

  16. 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.

  17. CUBIC - A non-dispersive Diffuse X-ray Background spectrometer. [Cosmic Unresolved X-ray Background Instrument

    NASA Technical Reports Server (NTRS)

    Burrows, David N.; Skinner, Mark A.; Antunes, Alexander J. D.; Catalano, Mark A.; Cocklin, Eric J.; Engel, Leland G.; Entingh, Timothy J.; Garmire, Gordon P.; Green, Roland; Kelly, Douglas A.

    1992-01-01

    The Cosmic Unresolved X-ray Background Instrument using CCDs (CUBIC) is designed to obtain spectral observations of the Diffuse X-ray Background (DXRB) with moderate spectral resolution over the energy range 0.2-10 keV, using mechanically-collimated CCDs. At this time, it is the only planned satellite payload devoted to the study of the spectrum of the DXRB. Over the anticipated 3 year lifetime of the satellite, CUBIC will be able to study up to 50 percent of the sky with 5 x 5 deg spatial resolution for the subkilovolt Galactic diffuse background, and with 10 x 10 deg spatial resolution for the extragalactic diffuse background above 2 keV. CUBIC will obtain high quality nondispersive spectra of soft X-ray emission from the interstellar medium, supernova remnants, and some bright sources, and will make a sensitive seach for line emission or other features in the extragalactic cosmic X-ray background from 2-10 keV.

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

    SciTech Connect

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

    1996-06-01

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

  19. 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

  20. X-Ray Spectroscopy of the Liquid Water Surface

    NASA Astrophysics Data System (ADS)

    Saykally, Richard

    2004-03-01

    We have developed a new experiment for probing molecular details of liquid-vapor interfaces of volatile substances and their solutions under equilibrium conditions. Electronic and geometric structures of interfacial molecules are probed by EXAFS and NEXAFS methods in the soft X-ray region, using the Advanced Light Source, Berkeley, CA. Liquids are introduced into a high vacuum environment through the use of liquid microjets, which have been characterized independently by Raman spectroscopy. Detection of ions and electrons produced by the Auger avalanche probe the bulk and surface regions of the microjet, respectively, as a result of their different escape depths. Our first efforts involved a comparative study of the interfaces of water and methanol, wherein we detailed the first observation of surface relaxation for a liquid. Analysis of EXAFS data yielded a 6distance at the water interface, whereas a 5was found for methanol. NEXAFS measurements, interpreted in terms of density functional theory simulations, indicate a large population of interfacial water molecules having two free OH bonds ("acceptor only molecules"). This complements the "single donor" species identified in sum frequency generation experiments. These results are supported by recent theoretical calculations. For methanol and other simple alcohols, the data indicate that free alkyl groups extend into the vapor part of the interface. Preliminary results for aqueous solutions, as well as for other pure liquids, have been obtained and are presently under analysis. REFERENCES 1. K.R. Wilson, R.D. Schaller, B.S. Rude, T. Catalano, D.T. Co, J.D. Bozek, and R.J. Saykally, "Surface relaxation in liquid water and methanol studied by X-ray absorption spectroscopy," J. Chem. Phys 117,7738(2002). 2. K.R. Wilson, M. Cavalleri, B.S. Rude, R.D. Schaller, A. Nilsson, L.G.M. Pettersson, N. Goldman, T. Catalano, J.D. Bozek, and R.J. Saykally, "Characterization of hydrogen bond acceptor molecules at the water surface

  1. Laboratory-based high pressure X-ray photoelectron spectroscopy: A novel and flexible reaction cell approach

    NASA Astrophysics Data System (ADS)

    Kerherve, Gwilherm; Regoutz, Anna; Bentley, David; Hood, Colin; Feeley, Keith; Knight, Stewart; Robson, Anthony; Turner, Craig; Singh, Nick; Pontefract, John; Åhlund, John; Kahk, Juhan M.; Villar-Garcia, Ignacio J.; Payne, David J.

    2017-03-01

    The last 10-15 years have witnessed a resurgence in the application of high pressure X-ray photoelectron spectroscopy, mainly through the development of new electron energy analyser designs and the utilization of high-brilliance synchrotron radiation sources. To continue this expansion of the technique, it is crucial that instruments are developed for the home-laboratory, considering that this is where the vast majority of traditional ultra-high vacuum (UHV) X-ray photoelectron spectroscopy is performed. The research presented here introduces a new addition to the field, an instrument capable of performing spectroscopy measurements from UHV to high pressure (25 mbar), achieved using a retractable and modular reaction cell design. The ease of use, stability (of analyser, X-ray source, and gas delivery, etc.), and overall capability of the instrument will be demonstrated.

  2. X-Ray Imaging-Spectroscopy of Abell 1835

    NASA Technical Reports Server (NTRS)

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

    2000-01-01

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

  3. heterojunction interface investigated by X-ray photoemission spectroscopy

    NASA Astrophysics Data System (ADS)

    Lin, Lingyan; Yu, Jinling; Cheng, Shuying; Lu, Peimin; Lai, Yunfeng; Lin, Sile; Zhao, Pengyi

    2014-09-01

    The band alignment at the In2S3/Cu2ZnSnS4 heterojunction interface is investigated by X-ray photoemission spectroscopy. In2S3 is thermally evaporated onto the contamination-free polycrystalline Cu2ZnSnS4 surface prepared by magnetron sputtering. The valence band offset is measured to be 0.46 ± 0.1 eV, which matches well with the valance band offset value 0.49 eV calculated using "transitivity" method. The conduction band offset is determined to be 0.82 ± 0.1 eV, indicating a `type I' band alignment at the heterojunction interface.

  4. The Constellation-X Spectroscopy X-Ray Telescope

    NASA Technical Reports Server (NTRS)

    Petre, Robert; Content, David; Lehan, John; O'Dell, Stephen; Owens, Scott; Podgorsky, William; Stewart, Jeff; Zhang, William

    2004-01-01

    The status of technology development for the Constellation-X Spectroscopy X-ray Telescope (SXT) mirror is presented. The SXT mirror combines a large (1.6 m) aperture with modest (12 arc sec half power diameter) angular resolution and low mass (750 kg). The overall collecting area, larger than 9,600 square cm at 0.25 keV, requires high throughput, and thus nesting of a substantial number of thin reflectors. A phased development program is underway to develop reflectors, mounting and alignment approaches, and metrology techniques for components and the mirror has a whole. The latest results in all these areas are summarized, along with an overview of results of optical testing of reflector performance.

  5. The LNLS soft X-ray spectroscopy beamline.

    PubMed

    Tolentino, H; Compagnon-Cailhol, V; Vicentin, F C; Abbate, M

    1998-05-01

    The soft X-ray spectroscopy beamline installed at a bending-magnet source at the LNLS is described. The optics are designed to cover energies from 800 to 4000 eV with good efficiency. The focusing element is a gold-coated toroidal mirror with an angle of incidence of 17 mrad. The UHV double-crystal monochromator has three pairs of crystals, Si (111), InSb (111) and beryl (101;0), that can be selected by a sliding movement. The UHV workstation is equipped with an ion gun, an electron gun, an electron analyser, LEED optics, an open channeltron and a photodiode array. This beamline is intended for photoemission, photoabsorption, reflectivity and dichroism experiments.

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

    NASA Technical Reports Server (NTRS)

    Wheeler, D. R.

    1980-01-01

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

  7. VUV and soft x-ray spectroscopy of actinides

    SciTech Connect

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

    2004-01-01

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

  8. Imide photodissociation investigated by X-ray absorption spectroscopy.

    PubMed

    Johnson, Phillip S; Cook, Peter L; Liu, Xiaosong; Yang, Wanli; Bai, Yiqun; Abbott, Nicholas L; Himpsel, F J

    2012-06-21

    X-ray absorption spectroscopy is used to investigate the photodissociation of the imides PMDI (pyromellitic diimide) and SSMCC (sulfosuccinimidyl 4-(N-maleimidomethyl) cyclohexane-1-carboxylate). PMDI contains only one type of imide, and its photodissociation can be explained by a simple conversion from imide to a mix of imine and nitrile after desorption of the oxygens from the imide. SSMCC contains two different imides. One reacts like PMDI, the other in a more complex multistep process. Eventually, N(2) is formed in the bulk of the sample at high radiation density. The sequence of reactions is inferred from the π* peaks in total electron yield and fluorescence yield absorption spectra at the N 1s and O 1s edges. First-order rate equations are used to model the evolution of the peak areas versus radiation dose.

  9. Investigating DNA Radiation Damage Using X-Ray Absorption Spectroscopy

    PubMed Central

    Czapla-Masztafiak, Joanna; Szlachetko, Jakub; Milne, Christopher J.; Lipiec, Ewelina; Sá, Jacinto; Penfold, Thomas J.; Huthwelker, Thomas; Borca, Camelia; Abela, Rafael; Kwiatek, Wojciech M.

    2016-01-01

    The biological influence of radiation on living matter has been studied for years; however, several questions about the detailed mechanism of radiation damage formation remain largely unanswered. Among all biomolecules exposed to radiation, DNA plays an important role because any damage to its molecular structure can affect the whole cell and may lead to chromosomal rearrangements resulting in genomic instability or cell death. To identify and characterize damage induced in the DNA sugar-phosphate backbone, in this work we performed x-ray absorption spectroscopy at the P K-edge on DNA irradiated with either UVA light or protons. By combining the experimental results with theoretical calculations, we were able to establish the types and relative ratio of lesions produced by both UVA and protons around the phosphorus atoms in DNA. PMID:27028640

  10. Hard x ray/microwave spectroscopy of solar flares

    NASA Technical Reports Server (NTRS)

    Gary, Dale E.

    1992-01-01

    The joint study of hard x ray and microwave observations of solar flares is extremely important because the two complementary ways of viewing the accelerated electrons yield information that cannot be obtained using hard x rays or microwaves alone. The microwaves can provide spatial information lacking in the hard x rays, and the x ray data can give information on the energy distribution of electrons that remove ambiguities in the radio data. A prerequisite for combining the two data-sets, however, is to first understand which range of microwave frequencies correlate best with the hard x rays. This SMM Guest Investigator grant enabled us to combine multi-frequency OVRO data with calibrated hard x ray data to shed light on the relationship between the two emissions. In particular, the questions of which microwave frequencies correspond to which hard x ray energies, and what is the corresponding energy of the electrons that produce both types of emission are investigated.

  11. X-ray mapping in electron-beam instruments.

    PubMed

    Friel, John J; Lyman, Charles E

    2006-02-01

    This review traces the development of X-ray mapping from its beginning 50 years ago through current analysis procedures that can reveal otherwise obscure elemental distributions and associations. X-ray mapping or compositional imaging of elemental distributions is one of the major capabilities of electron beam microanalysis because it frees the operator from the necessity of making decisions about which image features contain elements of interest. Elements in unexpected locations, or in unexpected association with other elements, may be found easily without operator bias as to where to locate the electron probe for data collection. X-ray mapping in the SEM or EPMA may be applied to bulk specimens at a spatial resolution of about 1 microm. X-ray mapping of thin specimens in the TEM or STEM may be accomplished at a spatial resolution ranging from 2 to 100 nm, depending on specimen thickness and the microscope. Although mapping has traditionally been considered a qualitative technique, recent developments demonstrate the quantitative capabilities of X-ray mapping techniques. Moreover, the long-desired ability to collect and store an entire spectrum at every pixel is now a reality, and methods for mining these data are rapidly being developed.

  12. Instrumentation for Microfabrication with Deep X-ray Lithography

    NASA Astrophysics Data System (ADS)

    Pantenburg, F. J.

    2007-01-01

    Deep X-ray lithography for microfabrication is performed at least at ten synchrotron radiation centers worldwide. The characteristic energies of these sources range from 1.4 keV up to 8 keV, covering mask making capabilities, deep X-ray lithography up to ultra deep x-ray lithography of several millimeters resist thickness. Limitations in deep X-ray lithography arise from hard X-rays in the SR-spectrum leading to adhesion losses of resist lines after the developing process, as well as heat load due to very high fluxes leading to thermal expansion of mask and resist during exposure and therefore to microstructure distortion. Considering the installations at ANKA as an example, the advantages of mirrors and central beam stops for DXRL are presented. Future research work will concentrate on feature sizes much below 1 μm, while the commercialization of DXRL goes in the direction of massive automation, including parallel exposures of several samples in a very wide SR-fan, developing and inspection.

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

    SciTech Connect

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

    2015-07-15

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

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

    SciTech Connect

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

    2011-12-31

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

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

    SciTech Connect

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

    2011-05-01

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

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

    PubMed Central

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

    2011-01-01

    The research philosophy and new capabilities installed at NSLS beamline X26-C to support electronic absorption and Raman spectroscopies coupled with X-ray diffraction are reviewed. This beamline is dedicated full time to multidisciplinary studies with goals that include revealing the relationship between the electronic and atomic structures in macromolecules. The beamline instrumentation has been fully integrated such that optical absorption spectra and X-ray diffraction images are interlaced. Therefore, optical changes induced by X-ray exposure can be correlated with X-ray diffraction data collection. The installation of Raman spectroscopy into the beamline is also briefly reviewed. Data are now routinely generated almost simultaneously from three complementary types of experiments from the same sample. The beamline is available now to the NSLS general user population. PMID:21525643

  17. The focal plane assembly for the Athena X-ray Integral Field Unit instrument

    NASA Astrophysics Data System (ADS)

    Jackson, B. D.; van Weers, H.; van der Kuur, J.; den Hartog, R.; Akamatsu, H.; Argan, A.; Bandler, S. R.; Barbera, M.; Barret, D.; Bruijn, M. P.; Chervenak, J. A.; Dercksen, J.; Gatti, F.; Gottardi, L.; Haas, D.; den Herder, J.-W.; Kilbourne, C. A.; Kiviranta, M.; Lam-Trong, T.; van Leeuwen, B.-J.; Macculi, C.; Piro, L.; Smith, S. J.

    2016-07-01

    This paper summarizes a preliminary design concept for the focal plane assembly of the X-ray Integral Field Unit on the Athena spacecraft, an imaging microcalorimeter that will enable high spectral resolution imaging and point-source spectroscopy. The instrument's sensor array will be a 3840-pixel transition edge sensor (TES) microcalorimeter array, with a frequency domain multiplexed SQUID readout system allowing this large-format sensor array to be operated within the thermal constraints of the instrument's cryogenic system. A second TES detector will be operated in close proximity to the sensor array to detect cosmic rays and secondary particles passing through the sensor array for off-line coincidence detection to identify and reject events caused by the in-orbit high-energy particle background. The detectors, operating at 55 mK, or less, will be thermally isolated from the instrument cryostat's 2 K stage, while shielding and filtering within the FPA will allow the instrument's sensitive sensor array to be operated in the expected environment during both on-ground testing and in-flight operation, including straylight from the cryostat environment, low-energy photons entering through the X-ray aperture, low-frequency magnetic fields, and high-frequency electric fields.

  18. High-efficiency blazed transmission gratings for high-resolution soft x-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Heilmann, Ralf K.; Bruccoleri, Alexander R.; Schattenburg, Mark L.

    2015-09-01

    High-resolution spectroscopy of astrophysical sources is the key to gaining a quantitative understanding of the history, dynamics, and current conditions of the cosmos. A large-area (> 1,000 cm2), high resolving power (R = λ/Δλ> 3000) soft x-ray grating spectrometer (XGS) that covers the lines of C, N, O, Ne and Fe ions is the ideal tool to address a number of high-priority science questions from the 2010 Decadal Survey, such as the connection between super-massive black holes and large-scale structure via cosmic feedback, the evolution of large- scale structure, the behavior of matter at high densities, and the conditions close to black holes. While no grating missions or instruments are currently approved, an XGS aboard a potential future X-ray Surveyor could easily surpass the above performance metrics. To improve the chances for future soft x-ray grating spectroscopy missions or instruments, grating technology has to progress and advance to higher Technology Readiness Levels (TRLs). To that end we have developed Critical-Angle Transmission (CAT) gratings that combine the advantages of blazed reflection gratings (high efficiency, use of higher diffraction orders) with those of conventional transmission gratings (low mass, relaxed alignment tolerances and temperature requirements, high transparency at higher energies). A CAT grating-based spectrometer can provide performance 1-2 orders of magnitude better than current grating instruments on Chandra and Newton-XMM with minimal resource requirements. At present we have fabricated large-area freestanding CAT gratings with narrow integrated support structures from silicon-on- insulator wafers using advanced lithography and a combination of deep reactive-ion and wet etching. Our latest x-ray test results show record high absolute diffraction efficiencies in blazed orders in excess of 30% with room for improvement.

  19. Fast CCD camera for x-ray photon correlation spectroscopy and time-resolved x-ray scattering and imaging

    NASA Astrophysics Data System (ADS)

    Falus, P.; Borthwick, M. A.; Mochrie, S. G. J.

    2004-11-01

    A new, fast x-ray detector system is presented for high-throughput, high-sensitivity, time-resolved, x-ray scattering and imaging experiments, most especially x-ray photon correlation spectroscopy (XPCS). After a review of the architectures of different CCD chips and a critical examination of their suitability for use in a fast x-ray detector, the new detector hardware is described. In brief, its principal component is an inexpensive, commercial camera—the SMD1M60—originally designed for optical applications, and modified for use as a direct-illumination x-ray detector. The remainder of the system consists of two Coreco Imaging PC-DIG frame grabber boards, located inside a Dell Power-edge 6400 server. Each frame grabber sits on its own PCI bus and handles data from 2 of the CCD's 4 taps. The SMD1M60 is based on a fast, frame-transfer, 4-tap CCD chip, read out at12-bit resolution at frame rates of up to 62 Hz for full frame readout and up to 500 Hz for one-sixteenth frame readout. Experiments to characterize the camera's suitability for XPCS and small-angle x-ray scattering (SAXS) are presented. These experiments show that single photon events are readily identified, and localized to within a pixel index or so. This is a sufficiently fine spatial resolution to maintain the speckle contrast at an acceptable value for XPCS measurements. The detective quantum efficiency of the SMD1M60 is 49% for directly-detected 6.3 keV x rays. The effects of data acquisition strategies that permit near-real-time data compression are also determined and discussed. Overall, the SMD1M60 detector system represents a major improvement in the technology for time-resolved x-ray experiments, that require an area detector with time-resolutions in few-milliseconds-to-few-seconds range, and it should have wide applications, extending beyond XPCS.

  20. Al0.2Ga0.8As X-ray photodiodes for X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Whitaker, M. D. C.; Lioliou, G.; Butera, S.; Barnett, A. M.

    2016-12-01

    Three custom-made Al0.2Ga0.8As p-i-n mesa X-ray photodiodes (200 μm diameter, 3 μm i layer) were electrically characterised and investigated for their response to illumination with soft X-rays from an 55Fe radioisotope X-ray source (Mn Kα = 5.9 keV; Mn Kβ = 6.49 keV). The AlGaAs photodiodes were shown to be suitable for photon counting X-ray spectroscopy at room temperature. When coupled to a custom-made low-noise charge-sensitive preamplifier, a mean energy resolution (as quantified by the full width at half maximum of the 5.9 keV photopeak) of 1.24 keV was measured at room temperature. Parameters such as the depletion width (1.92 μm at 10 V), charge trapping noise (61.7 e- rms ENC at 5 V, negligible at 10 V) and the electronic noise components (known dielectric noise (63.4 e- rms), series white noise (27.7 e- rms), parallel white noise (9.5 e- rms) and 1/f series noise (2.2 e- rms) at 10 V reverse bias) affecting the achieved energy resolution were computed. The estimated charge trapping noise and mean energy resolution were compared to similar materials (e.g. Al0.8Ga0.2As) previously reported, and discussed. These results are the first demonstration of photon counting X-ray spectroscopy with Al0.2Ga0.8As reported to date.

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

    SciTech Connect

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

    2016-02-15

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

  2. Depth-Resolved X-ray Absorption Spectroscopy by Means of Grazing Emission X-ray Fluorescence.

    PubMed

    Kayser, Yves; Sá, Jacinto; Szlachetko, Jakub

    2015-11-03

    Grazing emission X-ray fluorescence (GEXRF) is well suited for nondestructive elemental-sensitive depth-profiling measurements on samples with nanometer-sized features. By varying the grazing emission angle under which the X-ray fluorescence signal is detected, the probed depth range can be tuned from a few to several hundred nanometers. The dependence of the XRF intensity on the grazing emission angle can be assessed in a sequence of measurements or in a scanning-free approach using a position-sensitive area detector. Hereafter, we will show that the combination of scanning-free GEXRF and fluorescence detected X-ray absorption spectroscopy (XAS) allows for depth-resolved chemical speciation measurements with nanometer-scale accuracy. While the conventional grazing emission geometry is advantageous to minimize self-absorption effects, the use of a scanning-free setup makes the sequential scanning of the grazing emission angles obsolete and paves the way toward time-resolved depth-sensitive XAS measurements. The presented experimental approach was applied to study the surface oxidation of an Fe layer on the top of bulk Si and of a Ge bulk sample. Thanks to the penetrating properties and the insensitivity toward the electric conduction properties of the incident and emitted X-rays, the presented experimental approach is well suited for in situ sample surface studies in the nanometer regime.

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

    NASA Astrophysics Data System (ADS)

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

    2016-02-01

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

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

    SciTech Connect

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

    2011-07-01

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

  5. Multi-speckle X-ray photon correlation spectroscopy in the ultra-small-angle X-ray scattering range

    PubMed Central

    Möller, Johannes; Chushkin, Yuriy; Prevost, Sylvain; Narayanan, Theyencheri

    2016-01-01

    Multi-speckle X-ray photon correlation spectroscopy (XPCS) measurements in the ultra-small-angle range are performed using a long pinhole collimation instrument in combination with two-dimensional photon-counting and high-sensitivity imaging detectors. The feasibility of the presented setup to measure dynamics on different time and length scales pertinent to colloidal systems is shown. This setup offers new research opportunities, such as for example in the investigation of non-equilibrium dynamics in optically opaque, complex systems over length scales from tens of nanometres to several micrometres. In addition, due to the short duration of the X-ray exposure involved in the ultra-small-angle range, possible radiation-induced effects are alleviated. Furthermore, the performance of two different detectors, a photon-counting Pilatus 300K and an integrating FReLoN CCD, are compared, and their applicability for accurate XPCS measurements is demonstrated. PMID:27359141

  6. Software System for the Calibration of X-Ray Measuring Instruments

    NASA Astrophysics Data System (ADS)

    Gaytán-Gallardo, E.; Tovar-Muñoz, V. M.; Cruz-Estrada, P.; Vergara-Martínez, F. J.; Rivero-Gutiérrez, T.

    2006-09-01

    A software system that facilities the calibration of X-ray measuring instruments used in medical applications is presented. The Secondary Standard Dosimetry Laboratory (SSDL) of the Nuclear Research National Institute in México (ININ in Spanish), supports activities concerning with ionizing radiations in medical area. One of these activities is the calibration of X-ray measuring instruments, in terms of air kerma or exposure by substitution method in an X-ray beam at a point where the rate has been determined by means of a standard ionization chamber. To automatize this process, a software system has been developed, the calibration system is composed by an X-ray unit, a Dynalizer IIIU X-ray meter by RADCAL, a commercial data acquisition card, the software system and the units to be tested and calibrated. A quality control plan has been applied in the development of the software system, ensuring that quality assurance procedures and standards are being followed.

  7. Kr X-ray spectroscopy to diagnose NIF ICF implosions

    NASA Astrophysics Data System (ADS)

    Dasgupta, A.; Ouart, N.; Giuliani, J. L.; Clark, R. W.; Schneider, M. B.; Scott, H. A.; Chen, H.; Ma, T.; Apruzese, J. P.

    2016-10-01

    X ray spectroscopy is used on the NIF to diagnose the plasma conditions in the ignition target in indirect drive ICF implosions. High-energy emission spectra from mid to high atomic number elements can provide estimates of electron temperature near stagnation of an ICF implosion. A platform is being developed at NIF where small traces of krypton are used as a dopant to the fuel gas for spectroscopic diagnostics using krypton line emissions. The fraction of krypton dopant was varied in the experiments and was selected so as not to perturb the implosion. Simulations of the krypton spectra using a 1 in 104 atomic fraction of krypton in direct-drive exploding pusher with a range of electron temperatures and densities show discrepancies when different atomic models are used. We use our non-LTE atomic model with a detailed fine-structure level atomic structure and collisional-radiative rates to investigate the krypton spectra at the same conditions. Synthetic spectra are generated with a detailed multi-frequency radiation transport scheme from the emission regions of interest to analyze the experimental data and compare and contrast with the existing simulations at LLNL. Work supported by DOE/NNSA and under the auspices of DOE by LLNL under Contract # DE-AC52-07NA27344.

  8. X-ray Absorption Spectroscopy of the Rare Earth orthophosphates

    SciTech Connect

    Shuh, D.K.; Terminello, L.J.; Boatner, L.A.; Abraham, M.M.

    1993-06-01

    X-ray Absorption Spectroscopy (XAS) of the Rare Earth (RE) 3d levels yields sharp peaks near the edges as a result of strong, quasi-atomic 3d{sup 10}4f{sup n} {yields} 3d-{sup 9}4f{sup n+1} transitions and these transitions exhibit a wealth of spectroscopic features. The XAS measurements of single crystal REPO{sub 4} (RE = La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Er) at the 3d edge were performed in the total yield mode at beam line 8-2 at the Stanford Synchrotron Radiation Laboratory (SSRL). The XAS spectra of the RE ions in the orthophosphate matrix generally resemble the XAS of the corresponding RE metal. This is not unexpected and emphasizes the major contribution of the trivalent state to the electronic transitions at the RE 3d edges. These spectra unequivocally identify the transitions originating from well-characterized RE cores and correlate well with previous theoretical investigations.

  9. ITER core imaging X-ray spectroscopy: Atomic physics issues

    NASA Astrophysics Data System (ADS)

    Beiersdorfer, P.; Clementson, J.; Widmann, K.; Bitter, M.; Hill, K. W.; Johnson, D.; Barnsley, R.; Chung, H. K.; Safronova, U. I.

    2017-03-01

    The Core Imaging X-Ray Spectrometer (CIXS) will be employed for measurements of the ion temperature and of the toroidal rotation velocity, Ti and vϕ, respectively, as a function of the radius of ITER plasmas. The diagnostic is based on precision determinations of the Doppler broadening, centroid shift, and intensity of the lines of highly ionized heavy impurities using a curved Bragg crystal spectral disperser and imager. The ions under consideration for the diagnostic are those of tungsten, krypton, xenon, iron, and argon. A detailed discussion is given of the need for atomic physics experiments and calculations involving the primary diagnostic lines and their collisional and dielectronic satellites. Such experiments and calculations define the instrument parameters, determine the diagnostic uncertainties, and provide paths for extending the diagnostic capabilities to measure impurity concentrations, electron temperature, and ion transport parameters. Enabling the diagnostic to measure radially dependent ion transport coefficients, in particular, requires a large amount of high-quality atomic data in the form of reliable excitation, ionization, and recombination rate coefficients as well as ionization balance calculations which make use of these data. Because core imaging spectrometers are being developed and implemented on present-day magnetic fusion devices, much of the atomic data are already needed and can be tested in the analysis of existing spectra recorded by these diagnostics.

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

    ERIC Educational Resources Information Center

    Baker, A. D.; And Others

    1980-01-01

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

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

    SciTech Connect

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

    1997-04-01

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

  12. Electrochemical discharge of nanocrystalline magnetite: structure analysis using X-ray diffraction and X-ray absorption spectroscopy.

    PubMed

    Menard, Melissa C; Takeuchi, Kenneth J; Marschilok, Amy C; Takeuchi, Esther S

    2013-11-14

    Magnetite (Fe3O4) is an abundant, low cost, environmentally benign material with potential application in batteries. Recently, low temperature coprecipitation methods have enabled preparation of a series of nanocrystalline magnetite samples with a range of crystallite sizes. Electrochemical cells based on Li/Fe3O4 show a linear increase in capacity with decreasing crystallite size at voltages ≥1.2 V where a 2× capacity improvement relative to commercial (26.2 nm) magnetite is observed. In this report, a combination of X-ray powder diffraction (XRD) and X-ray absorption spectroscopy (XAS) is used to measure magnetite structural changes occurring upon electrochemical reduction, with parent Fe3O4 crystallite size as a variable. Notably, XAS provides evidence of metallic iron formation at high levels of electrochemical reduction.

  13. Spectroscopy of six X-ray-selected BL Lacertae candidates

    SciTech Connect

    Margon, B.; Boroson, T.A.; Chanan, G.A.; Thompson, I.B.; Schneider, D.P.

    1986-11-01

    Results of a continuing program aimed at extending the small list of X-ray-selected BL Lac objects are reported. High-quality spectra have been obtained of six faint blue objects that lie within the positional error boxes of X-ray sources discovered serendipitously by the Einstein Observatory. Three of the objects are found to be previously uncataloged low-red-shift quasi-stellar objects, including one formerly suggested as BL Lac candidate. Two are faint galactic stars, while the final object has a featureless spectrum, and thus remains a candidate. Although X-ray selection may ultimately be an effective means of discovering faint BL Lac objects, such sources are evidently rare at the X-ray flux levels attainable by the Einstein Observatory. 15 references.

  14. UV-Visible Absorption Spectroscopy Enhanced X-ray Crystallography at Synchrotron and X-ray Free Electron Laser Sources.

    PubMed

    Cohen, Aina E; Doukov, Tzanko; Soltis, Michael S

    2016-01-01

    This review describes the use of single crystal UV-Visible Absorption micro-Spectrophotometry (UV-Vis AS) to enhance the design and execution of X-ray crystallography experiments for structural investigations of reaction intermediates of redox active and photosensitive proteins. Considerations for UV-Vis AS measurements at the synchrotron and associated instrumentation are described. UV-Vis AS is useful to verify the intermediate state of an enzyme and to monitor the progression of reactions within crystals. Radiation induced redox changes within protein crystals may be monitored to devise effective diffraction data collection strategies. An overview of the specific effects of radiation damage on macromolecular crystals is presented along with data collection strategies that minimize these effects by combining data from multiple crystals used at the synchrotron and with the X-ray free electron laser.

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

    DOE PAGES

    Dakovski, Georgi L.; Heimann, Philip; Holmes, Michael; ...

    2015-04-02

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

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

    SciTech Connect

    Collins, Michael L; Havrilla, George J

    2009-01-01

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

  17. Hitomi X-ray Astronomy Satellite: Power of High-Resolution Spectroscopy

    NASA Astrophysics Data System (ADS)

    Odaka, Hirokazu; Aff001

    2017-01-01

    Hitomi (ASTRO-H) is an X-ray observatory developed by an international collaboration led by JAXA. An X-ray microcalorimeter onboard this satellite has opened a new window of high-resolution spectroscopy with an unprecedented energy resolution of 5 eV (FWHM) at 6 keV. The spacecraft was launched on February 17, 2016 from Tanegashima Island, Japan, and we completed initial operations including deployment of the hard X-ray imagers on the extensible optical bench. All scientific instruments had successfully worked until the sudden loss of the mission on March 26. We have obtained a spectrum showing fully resolved emission lines through the first-light observation of the Perseus Cluster. The line-of-sight velocity dispersion of 164 +/- 10 km s-1 reveals the quiescent environment of intracluster medium at the cluster core, implying that measured cluster mass requires little correction for the turbulent pressure. We also discuss observations to the Galactic Center which could be performed with Hitomi.

  18. Development of spatially resolved high resolution x-ray spectroscopy for fusion and light-source research

    NASA Astrophysics Data System (ADS)

    Lu, J.; Hill, K. W.; Bitter, M.; Delgado-Aparicio, L.; Pablant, N. A.; Efthimion, P.; Beiersdorfer, P.; Chen, H.; Widmann, K.; Sanchez del Rio, M.

    2014-09-01

    One dimensional spatially resolved high resolution x-ray spectroscopy with spherically bent crystals and 2D pixelated detectors is an established technique on magnetic confinement fusion (MCF) experiments world wide for Doppler measurements of spatial profiles of plasma ion temperature and flow velocity. This technique is being further developed for diagnosis of High Energy Density Physics (HEDP) plasmas at laser-plasma facilities and synchrotron/x-ray free electron laser (XFEL) facilities. Useful spatial resolution (micron scale) of such small-scale plasma sources requires magnification, because of the finite pixel size of x-ray CCD detectors (13.5 μm). A von-Hamos like spectrometer using spherical crystals is capable of magnification, as well as uniform sagittal focusing across the full x-ray spectrum, and is being tested in laboratory experiments using a tungsten-target microfocus (5-10 μm) x-ray tube and 13-μm pixel x-ray CCD. A spatial resolution better than 10 μm has been demonstrated. Good spectral resolution is indicated by small differences (0.02 - 0.1 eV) of measured line widths with best available published natural line widths. Progress and status of HEDP measurements and the physics basis for these diagnostics are presented. A new type of x-ray crystal spectrometer with a convex spherically bent crystal is also reported. The status of testing of a 2D imaging microscope using matched pairs of spherical crystals with x rays will also be presented. The use of computational x-ray optics codes in development of these instrumental concepts is addressed.

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

    PubMed

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

    2013-06-07

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

  20. 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

  1. Combining X-ray and neutron crystallography with spectroscopy

    PubMed Central

    Smith, Oliver

    2017-01-01

    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. PMID:28177310

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

    SciTech Connect

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

    2006-01-01

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

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

    SciTech Connect

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

    2012-04-15

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

  4. 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

  5. Evaluating Superconducting YBCO Film Properties Using X-Ray Photoelectron Spectroscopy (Postprint)

    DTIC Science & Technology

    2012-02-01

    AFRL-RZ-WP-TP-2012-0093 EVALUATING SUPERCONDUCTING YBCO FILM PROPERTIES USING X-RAY PHOTOELECTRON SPECTROSCOPY (POSTPRINT) Paul N. Barnes...2012 Conference Paper Postprint 01 January 2002 – 01 January 2004 4. TITLE AND SUBTITLE EVALUATING SUPERCONDUCTING YBCO FILM PROPERTIES USING X-RAY

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

    NASA Astrophysics Data System (ADS)

    Pacold, Joseph I.

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

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

    PubMed

    Sun, Tianxi; Liu, Zhiguo; Wang, Guangfu; Ma, Yongzhong; Peng, Song; Sun, Weiyuan; Li, Fangzuo; Sun, Xuepeng; Ding, Xunliang

    2014-12-01

    A confocal micro X-ray fluorescence (MXRF) spectrometer based on polycapillary X-ray optics was used for the identification of paint layers. The performance of the confocal MXRF was studied. Multilayered paint fragments of a car were analyzed nondestructively to demonstrate that this confocal MXRF instrument could be used in the discrimination of the various layers in multilayer paint systems.

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

    SciTech Connect

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

    2015-04-15

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

  9. 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.

  10. White Dwarf Mass Estimation with X-ray Spectroscopy

    NASA Astrophysics Data System (ADS)

    Hayashi, T.

    2017-03-01

    I present X-ray spectral modeling of intermediate polars (IPs) and its application to Suzaku satellite data. The intrinsic thermal X-rays are modeled by integrating the plasma emissions of various temperatures in the post-shock accretion column (PSAC). The physical quantity distributions for the thermal spectral model is calculated from quasi-one-dimensional hydrodynamics. The PSAC calculation includes especially the dipolar geometry and variation of the specific accretion rate. The X-ray reflection from the white dwarf (WD) is modeled by a Monte Carlo simulation. In this simulation, the PSAC irradiates a cool, neutral and spherical WD with the various thermal spectra from the corresponding positions in the PSAC according to the thermal spectral model. The coherent and incoherent scattering, the photoelectric absorption, and Kα and Kβ re-emission of iron and nickel are taken into account for the photons arriving at the WD. The constructed X-ray spectral model is applied to EX Hya and V1223 Sgr, finding 0.65+0.11 –0.12 M⊙ and 0.91+0.08–0.03 M⊙, respectively. Their specific accretion rates are estimated at 0.069+0.33–0.045 g cm–2 s-1 and > 2 g cm–2 s-1, respectively, while the reflecting angles are 78.0–1.6+1.4 deg and 66.2+2.5–2.3 deg, respectively.

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

    NASA Astrophysics Data System (ADS)

    Hixson, Holly Gwyndolen

    1997-08-01

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

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

    SciTech Connect

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

    2012-03-13

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

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

    SciTech Connect

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

    2007-08-15

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

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

    NASA Astrophysics Data System (ADS)

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

    2004-09-01

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

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

    SciTech Connect

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

    2013-04-15

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

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

    PubMed

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

    2016-04-01

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

  17. X-ray spectroscopy of photoionized plasmas in astrophysics.

    NASA Astrophysics Data System (ADS)

    Kunieda, H.

    Among astrophysical objects, active galactic nuclei (AGN) are good examples of photoionized plasmas illuminated by central bright sources. X-rays emerging from such plasmas are observed by ASCA. In soft X-rays, emission lines are observed from He-like Ca, Ar, S, Si, and Mg, whose ionization temperature are much higher than the electron temperature. From some Sy I's, an absorption feature due to O VII/O VIII was found, which suggests it ionized (warm) absorber. Such a warm absorber has been identified by emission lines seen by EUVE. A common spectral feature of Sy I's is the iron K emission line. ASCA discovered broad line feature due to gravitational and Doppler effects of reprocessor on the accretion disk around a massive black hole.

  18. Recent upgrades to MST's soft-x-ray spectroscopy diagnostic

    NASA Astrophysics Data System (ADS)

    Pandya, M. D.; Scherer, A. C.; Clark, J.; Dubois, A. M.; Almagri, A. F.; Chapman, B. E.

    2016-10-01

    In MST RFP plasmas, electron energization during tearing mode reconnection events was recently observed via soft-x-ray (sxr) emission. X-ray measurements from 3-25 keV during these short-lived (< 100 μs) events were achieved with a detector consisting of an avalanche photodiode and a 20 ns Gaussian shaping amplifier (GSA) whose output was digitized at 500 MHz. A radially resolved measurement of x-ray emission from 2-10 keV can also be made with an existing array of six Amptek XR-100CR sxr detectors, each comprised of a Si photodiode, a charge-sensitive preamplifier, a thermoelectric cooler, and a Cremat GSA CR-200-500ns having a pulse FWHM of about 1200 ns. One upgrade to this system entails a CR-200-25ns GSA which will reduce the FWHM to 60 ns. The digitization rate is also increased from 60 MHz to 240 MHz, sufficient to resolve a 60 ns Gaussian pulse. The upgrade will also incorporate improved shielding from IGBT switching noise arising from MST's Bt and Bp programmable power supplies. Housing the detector assembly within Compac-SRF-series enclosures attenuates noise at 20 MHz by 80 dB. Initial measurements will be presented. Work supported by US DOE.

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

    NASA Astrophysics Data System (ADS)

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

    2017-01-01

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

  20. 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.

  1. 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

  2. High Resolution X-Ray Spectroscopy with a Microcalorimeter

    SciTech Connect

    Norrell, J.; Anderson, I.

    2005-01-01

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

  3. X-ray spectroscopy of hot white dwarfs

    NASA Astrophysics Data System (ADS)

    Adamczak, Jens

    2010-10-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-08-01

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

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

    DOE PAGES

    Chollet, Matthieu; Alonso-Mori, Roberto; Cammarata, Marco; ...

    2015-04-21

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

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

    PubMed

    Kowalska, Joanna; DeBeer, Serena

    2015-06-01

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

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

    PubMed Central

    2015-01-01

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

  8. The USA experiment on the Argos Satellite: A low cost instrument for timing x-ray binaries

    SciTech Connect

    Wood, K.S.; Fritz, G.; Hertz, P.; Johnson, W.N.; Lovelette, M.N.; Wolff, M.T. ); Bloom, E.; Godfrey, G.; Hanson, J.; Michelson, P.; Taylor, R.; Wen, H. )

    1994-07-05

    The Unconventional Stellar Aspect (USA) experiment to be launched in September 1995 on the Advanced Research and Global Observations Satellite (ARGOS) is a low-cost, quick---yet scientifically ambitious---x-ray timing experiment. It is designed for the dual purpose of scientific research in x-ray timing and time resolved spectroscopy and also for exploration of applications of x-ray sensor technology. Bright galactic x-ray binaries are used simultaneously for both scientific and applied objectives.

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

    NASA Astrophysics Data System (ADS)

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

    2017-01-01

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

  10. X-ray spectroscopy of the SSME plume

    NASA Technical Reports Server (NTRS)

    Olive, Dan F.

    1988-01-01

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

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

    SciTech Connect

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

    2011-08-16

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

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

    NASA Astrophysics Data System (ADS)

    Zhao, W.; Chu, W. S.; Yang, F. F.; Yu, M. J.; Chen, D. L.; Guo, X. Y.; Zhou, D. W.; Shi, N.; Marcelli, A.; Niu, L. W.; Teng, M. K.; Gong, W. M.; Benfatto, M.; Wu, Z. Y.

    2007-09-01

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

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

    PubMed

    Chergui, Majed

    2016-05-01

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

  14. 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

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

    NASA Astrophysics Data System (ADS)

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

    2012-11-01

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

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

    PubMed

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

    2012-11-01

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

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

    SciTech Connect

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

    2012-11-15

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

  18. Science Instruments for the Advanced X-Ray Astrophysics Facility (AXAF)

    NASA Technical Reports Server (NTRS)

    Winkler, Carl E.; Cumings, Nesbitt P.; Randolph, Joseph L.; Talley, Drayton H.

    1993-01-01

    The AXAF program has undergone major changes since the Announcement of Opportunity was extended by NASA Headquarters in 1983. The Science Instruments (SI's) for AXAF have also experienced several design changes since they were competitively selected in 1985. Moreover, two separate complementary missions are now being baselined for AXAF; one is designated AXAF-I for imaging and will include the high precision Wolter type I optics, and the other is called AXAF-S for spectroscopy. The resulting less-costly AXAF will still be superior to any previous x-ray observatories. Both missions continue to be managed. AXAF-I contains two focal plane SI's, the High Resolution Camera (HRC), and the AXAF Charge-Coupled Device (CCD) imaging spectrometer (ACIS), as well as the High-Energy Transmission Grating Spectrometer (HETGS) and the Low-Energy Transmission Grating Spectrometer (LETGS). Optics/Cryogenics Division (BECD). AXAF-S features only one focal plane SI, the X-Ray Spectrometer (XRS). The grazing incidence mirrors for this mission are mainly to provide a large collecting area and to concentrate these x-ray photons onto the XRS detector. Precise focusing, although preferred, is of secondary importance. Nested conical foil mirrors are currently baselined; however, replicated imaging optics are being evaluated for collecting efficiency and cost. AXAF-S is scheduled to be launched in late 1999. It has been designated as an MSFC in-house project. In addition to overall management, MSFC is fully responsible for the design, development, integration, and test of the complete AXAF-S observatory, including the XRS which will be furnished by the Goddard Space Flight Center (GSFC). Together, AXAF-I and AXAF-S constitute the third of NASA's series of Great Observatories, joining the Hubble space telescope (HST) and the Gamma-Ray Observatory (GRO) which are already operational. The develop- ment, launch, and operation of the Space InfraRed Telescope Facility (SIRTF) will follow later to

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

    NASA Astrophysics Data System (ADS)

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

    2010-06-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2017-03-01

    Current inertial confinement fusion experiments on the National Ignition Facility (NIF) [G. H. Miller, E. I. Moses, and C. R. Wuest, Opt. Eng. 43, 2841 (2004)] are attempting to demonstrate thermonuclear ignition using x-ray drive by imploding spherical targets containing hydrogen-isotope fuel in the form of a thin cryogenic layer surrounding a central volume of fuel vapor [J. Lindl, Phys. Plasmas 2, 3933 (1995)]. The fuel is contained within a plastic ablator layer with small concentrations of one or more mid-Z elements, e.g., Ge or Cu. The capsule implodes, driven by intense x-ray emission from the inner surface of a hohlraum enclosure irradiated by the NIF laser, and fusion reactions occur in the central hot spot near the time of peak compression. Ignition will occur if the hot spot within the compressed fuel layer attains a high-enough areal density to retain enough of the reaction product energy to reach nuclear reaction temperatures within the inertial hydrodynamic disassembly time of the fuel mass [J. Lindl, Phys. Plasmas 2, 3933 (1995)]. The primary purpose of the ablator dopants is to shield the ablator surface adjacent to the DT ice from heating by the hohlraum x-ray drive [S. W. Haan et al., Phys. Plasmas 18, 051001 (2011)]. Simulations predicted that these dopants would produce characteristic K-shell emission if ablator material mixed into the hot spot [B. A. Hammel et al., High Energy Density Phys. 6, 171 (2010)]. In NIF ignition experiments, emission and absorption features from these dopants appear in x-ray spectra measured with the hot-spot x-ray spectrometer in Supersnout II [S. P. Regan et al., "Hot-Spot X-Ray Spectrometer for the National Ignition Facility," to be submitted to Review of Scientific Instruments]. These include K-shell emission lines from the hot spot (driven primarily by inner-shell collisional ionization and dielectronic recombination) and photoionization edges, fluorescence, and absorption lines caused by the absorption of the

  1. Magnetic x-ray linear dichroism in the photoelectron spectroscopy of ultrathin magnetic alloy films

    NASA Astrophysics Data System (ADS)

    Tobin, J. G.; Goodman, K. W.; Mankey, G. J.; Willis, R. F.; Denlinger, J. D.; Rotenberg, E.; Warwick, A.

    1996-04-01

    The magnetic structure of nanoscale alloy films has been probed using the magnetic x-ray linear dichroism in photoelectron spectroscopy. FeNi and CoFe epitaxial films were grown on Cu(001), in situ and using molecular beam epitaxy techniques. The magnetic x-ray linear dichroism measurements were made at the Spectromicroscopy Facility of the Third Generation Advanced Light Source. Because soft x-rays were used to generate photoemission from the 3p core levels, both elemental selectivity and magnetic sensitivity were achieved simultaneously.

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

    SciTech Connect

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

    1997-04-01

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

  3. 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.

  4. An instrument for in situ coherent x-ray studies of metal-organic vapor phase epitaxy of III-nitrides.

    PubMed

    Ju, Guangxu; Highland, Matthew J; Yanguas-Gil, Angel; Thompson, Carol; Eastman, Jeffrey A; Zhou, Hua; Brennan, Sean M; Stephenson, G Brian; Fuoss, Paul H

    2017-03-01

    We describe an instrument that exploits the ongoing revolution in synchrotron sources, optics, and detectors to enable in situ studies of metal-organic vapor phase epitaxy (MOVPE) growth of III-nitride materials using coherent x-ray methods. The system includes high-resolution positioning of the sample and detector including full rotations, an x-ray transparent chamber wall for incident and diffracted beam access over a wide angular range, and minimal thermal sample motion, giving the sub-micron positional stability and reproducibility needed for coherent x-ray studies. The instrument enables surface x-ray photon correlation spectroscopy, microbeam diffraction, and coherent diffraction imaging of atomic-scale surface and film structure and dynamics during growth, to provide fundamental understanding of MOVPE processes.

  5. An instrument for in situ coherent x-ray studies of metal-organic vapor phase epitaxy of III-nitrides

    NASA Astrophysics Data System (ADS)

    Ju, Guangxu; Highland, Matthew J.; Yanguas-Gil, Angel; Thompson, Carol; Eastman, Jeffrey A.; Zhou, Hua; Brennan, Sean M.; Stephenson, G. Brian; Fuoss, Paul H.

    2017-03-01

    We describe an instrument that exploits the ongoing revolution in synchrotron sources, optics, and detectors to enable in situ studies of metal-organic vapor phase epitaxy (MOVPE) growth of III-nitride materials using coherent x-ray methods. The system includes high-resolution positioning of the sample and detector including full rotations, an x-ray transparent chamber wall for incident and diffracted beam access over a wide angular range, and minimal thermal sample motion, giving the sub-micron positional stability and reproducibility needed for coherent x-ray studies. The instrument enables surface x-ray photon correlation spectroscopy, microbeam diffraction, and coherent diffraction imaging of atomic-scale surface and film structure and dynamics during growth, to provide fundamental understanding of MOVPE processes.

  6. X-ray Raman spectroscopy of carbon in asphaltene: light element characterization with bulk sensitivity.

    PubMed

    Bergmann, U; Mullins, O C; Cramer, S P

    2000-06-01

    X-ray Raman spectra of the carbon K-edge have been recorded using 6.461 keV radiation for a petroleum asphaltene. By comparison with coronene, graphite, and paraffin standards, the asphaltene spectrum is seen to be composed of contributions from saturated and aromatic carbon species. The information contained in the carbon K-edge was extracted with bulk (approximately 1 mm) sensitivity, because the Raman method used hard X-rays. This helps alleviate concerns about surface artifacts that frequently occur with soft X-ray spectroscopy of light elements. X-ray Raman spectroscopy shows great potential for characterization of light elements in fuels, catalysts, and other complex materials under chemically relevant conditions.

  7. Multidimensional resonant nonlinear spectroscopy with coherent broadband x-ray pulses

    NASA Astrophysics Data System (ADS)

    Bennett, Kochise; Zhang, Yu; Kowalewski, Markus; Hua, Weijie; Mukamel, Shaul

    2016-12-01

    New x-ray free electron laser (XFEL) and high harmonic generation (HHG) light sources are capable of generating short and intense pulses that make x-ray nonlinear spectroscopy possible. Multidimensional spectroscopic techniques, which have long been used in the nuclear magnetic resonance, infrared, and optical regimes to probe the electronic structure and nuclear dynamics of molecules by sequences of short pulses with variable delays, can thus be extended to the attosecond x-ray regime. This opens up the possibility of probing core-electronic structure and couplings, the real-time tracking of impulsively created valence-electronic wavepackets and electronic coherences, and monitoring ultrafast processes such as nonadiabatic electron-nuclear dynamics near conical-intersection crossings. We survey various possible types of multidimensional x-ray spectroscopy techniques and demonstrate the novel information they can provide about molecules.

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

    NASA Astrophysics Data System (ADS)

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

    2012-08-01

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

  9. Solving the Structure of Reaction Intermediates by Time-Resolved Synchrotron X-ray Absorption Spectroscopy

    SciTech Connect

    Wang, Q.; Hanson, J; Frenkel, A

    2008-01-01

    We present a robust data analysis method of time-resolved x-ray absorption spectroscopy experiments suitable for chemical speciation and structure determination of reaction intermediates. Chemical speciation is done by principal component analysis (PCA) of the time-resolved x-ray absorption near-edge structure data. Structural analysis of intermediate phases is done by theoretical modeling of their extended x-ray absorption fine-structure data isolated by PCA. The method is demonstrated using reduction and reoxidation of Cu-doped ceria catalysts where we detected reaction intermediates and measured fine details of the reaction kinetics. This approach can be directly adapted to many time-resolved x-ray spectroscopy experiments where new rapid throughput data collection and analysis methods are needed.

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

    SciTech Connect

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

    2007-10-26

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

  11. Arcus: An X-ray Grating Spectroscopy Mission

    NASA Astrophysics Data System (ADS)

    Smith, Randall K.; Arcus Collaboration

    2016-01-01

    We present the design and scientific motivation for Arcus, an X-ray grating spectrometer mission to be proposed to NASA as a MIDEX in 2016. This mission will observe structure formation at and beyond the edges of clusters and galaxies, feedback from supermassive black holes, the structure of the interstellar medium and the formation and evolution of stars. Key mission design parameters are R~3000 and >700 cm^2 of effective area at the crucial O VII and O VIII lines, with the full bandpass going from ~10-50Å. Arcus will use the silicon pore optics proposed for ESA's Athena mission, paired with off-plane gratings being developed at the University of Iowa and combined with MIT/Lincoln Labs CCDs.

  12. 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.

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

    SciTech Connect

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

    2014-04-15

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

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

    SciTech Connect

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

    1983-09-15

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

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

    NASA Technical Reports Server (NTRS)

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

    2014-01-01

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

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

    SciTech Connect

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

    2007-11-11

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

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

    SciTech Connect

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

    2008-10-22

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

  18. Capturing Transient Electronic and Molecular Structures in Liquids by Picosecond X-Ray Absorption Spectroscopy

    SciTech Connect

    Gawelda, W.; Pham, V. T.; El Nahhas, A.; Kaiser, M.; Zaushitsyn, Y.; Bressler, C.; Chergui, M.; Johnson, S. L.; Grolimund, D.; Abela, R.; Hauser, A.

    2007-02-02

    We describe an advanced setup for time-resolved x-ray absorption fine structure (XAFS) Spectroscopy with picosecond temporal resolution. It combines an intense femtosecond laser source synchronized to the x-ray pulses delivered into the microXAS beamline of the Swiss Light Source (SLS). The setup is applied to measure the short-lived high-spin geometric structure of photoexcited aqueous Fe(bpy)3 at room temperature.

  19. 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

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

    NASA Astrophysics Data System (ADS)

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

    2016-09-01

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

  1. Investigation of surface structure with X-ray absorption and electron emission spectroscopies

    NASA Astrophysics Data System (ADS)

    Pauli, Mark Daniel

    The use of electron spectromicroscopy for the study of the chemical composition and electronic properties of surfaces, overlayers, and interfaces has become widely accepted. Improvements to the optics of instruments such as the X-ray photo electron emission microscope have pushed spectroscopic microscopies into the realm of very high spatial resolution, at and below 1 micrometer [1]. Coupled with the high spectral resolution available from third generation synchrotron sources, this spatial resolution allows the measurement of micro-X-ray absorption near-edge spectra in addition to the more typical electron emission spectra and diffraction patterns. Complementary to the experimental developments is the development of improved theoretical methods for computational modeling of X-ray absorption and emission spectroscopies. In the field of tribochemistry, zinc dialkyl dithiophosphate (ZDDP) has long been a topic of much study. ZDDP is widely used as an anti-wear additive in engine oils and there is interest in determining the decomposition products of ZDDP that provide this protection against friction. An analysis of X-ray absorption near-edge spectra of thermal films from ZDDP samples is presented, including a comparison of the Zinc L-edge spectra with model calculations [2]. It was found essential to carry out self-consistent calculations of the electronic structure for the modeling. For the techniques of electron diffraction, a new method for a full multiple-scattering calculation of diffraction patterns from crystals with two-dimensional periodicity parallel to the surface is presented [3]. The calculation makes use of Helmholtz's reciprocity principle to compute the path-reversed process of the back propagation of a photoelectron from the position of a distant detector to that of the emitting atom. Early application is demonstrated with simulations of 64 eV M2,3VV and 914 eV L 2,3VV Auger electron diffraction from a Cu(001) surface. The functionality of the path

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

    NASA Astrophysics Data System (ADS)

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

    2015-12-01

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

  3. Probing electrode/electrolyte interfaces in situ by X-ray spectroscopies: old methods, new tricks.

    PubMed

    Wu, Cheng Hao; Weatherup, Robert S; Salmeron, Miquel B

    2015-11-11

    Electrode/electrolyte interfaces play a vital role in various electrochemical systems, but in situ characterization of such buried interfaces remains a major challenge. Several efforts to develop techniques or to modify existing techniques to study such interfaces are showing great promise to overcome this challenge. Successful examples include electrochemical scanning tunneling microscopy (EC-STM), surface-sensitive vibrational spectroscopies, environmental transmission electron microscopy (E-TEM), and surface X-ray scattering. Other techniques such as X-ray core-level spectroscopies are element-specific and chemical-state-specific, and are being widely applied in materials science research. Herein we showcase four types of newly developed strategies to probe electrode/electrolyte interfaces in situ with X-ray core-level spectroscopies. These include the standing wave approach, the meniscus approach, and two liquid cell approaches based on X-ray photoelectron spectroscopy and soft X-ray absorption spectroscopy. These examples demonstrate that with proper modifications, many ultra-high-vacuum based techniques can be adapted to study buried electrode/electrolyte interfaces and provide interface-sensitive, element- and chemical-state-specific information, such as solute distribution, hydrogen-bonding network, and molecular reorientation. At present, each method has its own specific limitations, but all of them enable in situ and operando characterization of electrode/electrolyte interfaces that can provide important insights into a variety of electrochemical systems.

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

    NASA Astrophysics Data System (ADS)

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

    2015-11-01

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

  5. Design and Operation of a High Pressure Reaction Cell for in situ X-ray Absorption Spectroscopy

    SciTech Connect

    Bare,S.; Yang, N.; Kelly, S.; Mickelson, G.; Modica, F.

    2007-01-01

    X-ray absorption spectroscopy measurements of catalytic reactions have been instrumental in advancing the understanding of catalytic processes. These measurements require an in situ catalysis reaction cell with unique properties. Here we describe the design and initial operation of an in situ/operando catalysis reaction cell for transmission X-ray absorption spectroscopy measurements. The cell is designed: to be an ideal catalytic reactor with no mass transfer effects; to give the same conversion and selectivity under similar space velocities as standard laboratory micro-reactors; to be operational temperatures up to 600 {sup o}C and pressures up to 14 bar; to be X-ray transparent allowing XAS measurement to be collected in transmission for all elements with Z {>=} 23 (vanadium K-edge at 5.5 keV); to measure the actual catalyst bed temperature; to not use o-ring seals, or water cooling; to be robust, compact, easy to assemble, and use, and relatively low cost to produce. The heart of the cell is fabricated from an X-ray transparent beryllium tube that forms a plug flow reactor. XAFS data recorded during the reduction of a Re/{gamma}-A{sub 2}O{sub 3} catalyst as a function of hydrogen pressure from 0.05 to 8 bar, and from a Pt-Sn/{gamma}-A{sub 2}O{sub 3} catalyst during n-heptane reforming are given as initial examples of the versatility of the reactor.

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

    NASA Technical Reports Server (NTRS)

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

    2012-01-01

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

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

    NASA Technical Reports Server (NTRS)

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

    2012-01-01

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

  8. Application of an X-ray Fluorescence Instrument to Helicopter Wear Debris Analysis

    DTIC Science & Technology

    2008-04-01

    Application of an X-ray Fluorescence Instrument to Helicopter Wear Debris Analysis Andrew Becker Air Vehicles Division...instrument to determine the composition of wear debris collected from helicopter magnetic chip detectors and oil filters. The Twin-X XRF (assessed in this...report) is a commercially produced bench-top XRF and has not previously been applied to wear debris analysis of Australian Defence Force aircraft

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

    NASA Astrophysics Data System (ADS)

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

    2007-11-01

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

  10. X-ray Spectroscopy of Directly Driven Cylindrical Implosions

    NASA Astrophysics Data System (ADS)

    Haynes, D.; Hooper, C.; Delamater, N.; Barnes, C.; Oertel, J.; Pollak, G.; Tubbs, D.; Watt, R.; Boehly, T.; Bradley, D.; Jaanimagi, P.; Knauer, J.

    1998-11-01

    X-ray spectra from a chlorinated polystyrene marker layer in a series of directly driven cylindrical implosions are presented and analyzed. The 4μm thick, 500μm long C_8H_6Cl2 (1.42g/cc) annular spectroscopic tracer layer is centrally located on the interior surface of the 20μm thick, 2250μm long polystyrene (1.044g/cc) 860μ m inner diameter cylindrical shell. The shell is filled with polystyrene foam (60mg/cc).(Barnes, C. W., et al.) 1998, to be published in Rev. Sci. Instrum., Tubbs, D. L., et al. 1998, to be published in Lasers and Particle Beams The implosions are driven by 50 beams of the OMEGA Laser facility. The temperature and density sensitive K-shell Cl spectra are recorded by a time-resolved spectrograph, and compared to calculated spectra in order to infer the evolution of electron temperature and density in the marker layer.(This work was performed under the auspices of the U. S. Department of Energy by the Los Alamos National Laboratory under contract No. W-7405-Eng-36)

  11. Picosecond and femtosecond X-ray absorption spectroscopy of molecular systems.

    PubMed

    Chergui, Majed

    2010-03-01

    The need to visualize molecular structure in the course of a chemical reaction, a phase transformation or a biological function has been a dream of scientists for decades. The development of time-resolved X-ray and electron-based methods is making this true. X-ray absorption spectroscopy is ideal for the study of structural dynamics in liquids, because it can be implemented in amorphous media. Furthermore, it is chemically selective. Using X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) in laser pump/X-ray probe experiments allows the retrieval of the local geometric structure of the system under study, but also the underlying photoinduced electronic structure changes that drive the structural dynamics. Recent developments in picosecond and femtosecond X-ray absorption spectroscopy applied to molecular systems in solution are reviewed: examples on ultrafast photoinduced processes such as intramolecular electron transfer, low-to-high spin change, and bond formation are presented.

  12. High-resolution structure of the photosynthetic Mn4Ca catalyst from X-ray spectroscopy.

    PubMed

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

    2008-03-27

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

  13. Experimental setup for high resolution x-ray spectroscopy of solids and liquid samples

    NASA Astrophysics Data System (ADS)

    Yin, Zhong; Rajković, Ivan; Raiser, Dirk; Scholz, Mirko; Techert, Simone

    2013-09-01

    Here we present a next-generation experimental setup for high-resolution X-ray spectroscopy of solid and liquid samples in the soft X-ray region to elucidate the complex molecular structures of (bio)chemical systems. The setup consists of a main target chamber, a target holder for either solid samples or a liquid jet delivery system, and a high-resolution soft X-ray grating spectrometer. This setup is in commissioning at PETRA III, presently one of the most brilliant storage ring based X-ray radiation sources in the world. The newly designed grazing incidence grating spectrometer is utilized for high-resolution measurement in the XUV range from 1 nm up to 6 nm.

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

    NASA Astrophysics Data System (ADS)

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

    2009-12-01

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

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

    SciTech Connect

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

    2010-05-01

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

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

    SciTech Connect

    Kanter, E.P.

    1996-08-01

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

  17. A sample holder for soft x-ray absorption spectroscopy of liquids in transmission mode.

    PubMed

    Schreck, Simon; Gavrila, Gianina; Weniger, Christian; Wernet, Philippe

    2011-10-01

    A novel sample holder for soft x-ray absorption spectroscopy of liquids in transmission mode based on sample cells with x-ray transparent silicon nitride membranes is introduced. The sample holder allows for a reliable preparation of ultrathin liquid films with an adjustable thickness in the nm-μm range. This enables measurements of high quality x-ray absorption spectra of liquids in transmission mode, as will be shown for the example of liquid H(2)O, aqueous solutions of 3d-transition metal ions and alcohol-water mixtures. The fine structure of the x-ray absorption spectra is not affected by the sample thickness. No effects of the silicon nitride membranes were observed in the spectra. It is shown how an inhomogeneous thickness of the sample affects the spectra and how this can be avoided.

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

    NASA Astrophysics Data System (ADS)

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

    2016-10-01

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

  19. RASOR: an advanced instrument for soft x-ray reflectivity and diffraction.

    PubMed

    Beale, T A W; Hase, T P A; Iida, T; Endo, K; Steadman, P; Marshall, A R; Dhesi, S S; van der Laan, G; Hatton, P D

    2010-07-01

    We report the design and construction of a novel soft x-ray diffractometer installed at Diamond Light Source. The beamline endstation RASOR is constructed for general users and designed primarily for the study of single crystal diffraction and thin film reflectivity. The instrument is comprised of a limited three circle (theta, 2theta, and chi) diffractometer with an additional removable rotation (phi) stage. It is equipped with a liquid helium cryostat, and post-scatter polarization analysis. Motorized motions are provided for the precise positioning of the sample onto the diffractometer center of rotation, and for positioning the center of rotation onto the x-ray beam. The functions of the instrument have been tested at Diamond Light Source, and initial test measurements are provided, demonstrating the potential of the instrument.

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

    NASA Astrophysics Data System (ADS)

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

    2016-11-01

    Hard X-ray photoelectron spectroscopy (HAXPES) using an excitation energy range of 2 keV to 6 keV in combination with Fe K- and S K-edge XANES, measured simultaneously in total electron (TEY) and partial fluorescence yield (PFY) modes, have been applied to study near-surface regions of natural polycrystalline pyrite FeS2 and pyrrhotite Fe1-xS before and after etching treatments in an acidic ferric chloride solution. It was found that the following near-surface regions are formed owing to the preferential release of iron from oxidized metal sulfide lattices: (i) a thin, no more than 1-4 nm in depth, outer layer containing polysulfide species, (ii) a layer exhibiting less pronounced stoichiometry deviations and low, if any, concentrations of polysulfide, the composition and dimensions of which vary for pyrite and pyrrhotite and depend on the chemical treatment, and (iii) an extended almost stoichiometric underlayer yielding modified TEY XANES spectra, probably, due to a higher content of defects. We suggest that the extended layered structure should heavily affect the near-surface electronic properties, and processes involving the surface and interfacial charge transfer.

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

    SciTech Connect

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

    2012-05-10

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

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

    SciTech Connect

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

    2014-07-21

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

  3. 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.

  4. A Laboratory Scale Critical-Dimension Small-Angle X-ray Scattering Instrument

    SciTech Connect

    Ho, Derek L.; Wang Chengqing; Lin, Eric K.; Jones, Ronald L.; Wu Wenli

    2007-09-26

    New methods for critical dimension (CD) measurements may be needed to enable the detailed characterization of nanoscale structures produced in the semiconductor industry and for nanotechnology applications. In earlier work, small angle x-ray scattering (SAXS) measurements with synchrotron sources have shown promise in meeting several grand challenges for CD metrology. However, it is not practical to depend upon x-ray synchrotron sources, which are large national facilities with limitations in the number of available instruments. To address this problem, a laboratory scale SAXS instrument for critical dimension measurements on periodic nanoscale patterns has been designed, installed, and tested. The system possesses two configurations, SAXS and ultra-small-angle x-ray scattering (USAXS), with a radiation target of either copper or molybdenum. With these configurations, the instrument is capable of accessing scattering angles that probe length scales ranging from ca. 0.5 nm to 2 {mu}m. In this work, we compare CD-SAXS measurements taken from a synchrotron-based SAXS at the Advanced Photon Source of the Argonne National Laboratory with those from the National Institute of Standards and Technology laboratory-scale SAXS instrument. The results from standard line/space gratings possessing periodic line-space patterns with CDs of tens to hundreds of nanometers show that the laboratory-scale system can quantitatively measure parameters, such as the pitch, line width, height, line-width roughness and sidewall angle. These results show that laboratory-scale measurements are feasible and can be used for research and development purposes or to assist calibration of optical scatterometry and CD-scanning electron microscopy instruments. The primary limitation of the measurement is that the data collection rate is unacceptably slow for production metrology because of the significantly lower x-ray beam fluxes currently available.

  5. A cosmic and solar X-ray and gamma-ray instrument for a scout launch

    NASA Technical Reports Server (NTRS)

    Forrest, D. J.; Vestrand, W. T.; Chupp, E. L.

    1988-01-01

    An overview is presented for a set of simple and robust X-ray and gamma ray instruments which have both cosmic and solar objectives. The primary solar scientific objective is the study of the beaming of energetic electrons and ions in solar flares. The instrument will measure spectra and polarization of flare emissions up to 10 MeV. At X-ray energies both the directly emitted flux and the reflected albedo flux will be measured with a complement of six X-ray sensors. Each of these detectors will have a different high Z filter selected to optimize both the energy resolution and high rate capabilities in the energy band 10 to 300 keV. At energies greater than 100 keV seven 7.6 x 7.6 cm NaI and a set of 30 concentric plastic scattering detectors will record the spectra and polarization of electron bremsstrahlung and nuclear gamma rays. All of the components of the instrument are in existence and have passed flight tests for earlier space missions. The instrument will use a spinning solar oriented Scout spacecraft. The NaI detectors will act as a self-modulating gamma ray detector for cosmic sources in a broad angular band which lies at 90 degrees to the Sun-Earth vector and hence will scan the entire sky in 6 months.

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

    PubMed

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

    2016-01-19

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

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

    SciTech Connect

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

    2015-06-24

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

  8. Firing of Clays Studied by X-ray Diffraction and Mössbauer Spectroscopy

    NASA Astrophysics Data System (ADS)

    Häusler, W.

    2004-06-01

    Three bentonites of varying purity were fired in air under controlled conditions up to 1300°C in an attempt to provide data for the assessment of firing techniques used in prehistoric pottery making. X-ray diffraction of samples heated at increasing temperatures allows to study the mineral transformations, the breakdown of the clay structure and the formation of new minerals in the high-temperature region. Mössbauer spectroscopy reveals the change of valence state and of the environment of the iron atoms on heating. Non iron-bearing minerals are only accessible by X-ray diffraction, while iron-containing oxidic and amorphous phases may be difficult to detect, due to poor crystallinity and small particle size. The combination of X-ray diffraction and Mössbauer spectroscopy therefore has a considerable potential in the study of the chemical and physical transformations occurring in pottery clays during firing.

  9. Nuclear Dynamical Correlation Effects in X-ray Spectroscopy from a Theoretical Time-Domain Perspective.

    PubMed

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

    2017-03-02

    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 focus on nuclear dynamical correlation effects in X-ray spectra and develop a rigorous time-correlation function method employing ground state classical molecular dynamics simulations. The importance of nuclear correlation phenomena is demonstrated by comparison against the results from the conventional sampling approach performed on the same data set for gas phase water. In contrast to the first-order absorption, second-order resonant inelastic scattering spectra exhibit pronounced fingerprints of nuclear motions. The developed methodology is not biased to a particular electronic structure method and, owing to its generality, can be applied to, e.g., X-ray photoelectron and Auger spectroscopies.

  10. 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.

    2016-12-01

    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.

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

    NASA Technical Reports Server (NTRS)

    Marshall, J.; Keaten, R.

    1999-01-01

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

  12. A Positional X-ray Instrumentation Test Stand For Beam-Line Experiments

    NASA Astrophysics Data System (ADS)

    Nikoleyczik, Jonathan; Prieskorn, Z.; Burrows, D. N.; Falcone, A.

    2014-01-01

    A multi-axis, motion controlled test stand has been built in the PSU 47 m X-ray beam-line for the purpose of testing X-ray instrumentation and mirrors using parallel rays. The test stand is capable of translation along two axes and rotation about two axes with motorized fine position control. The translation stages have a range of motion of 200 mm with a movement accuracy of ± 2.5 microns. Rotation is accomplished with a two-axis gimbal which can rotate 360° about one axis and 240° about another; movement with ± 35 arcsecond accuracy are achieved in both axes. The position and status are monitored using a LabView program. An XCalibr source with multiple target materials is used as an X-ray source and can produce multiple lines between 0.8 and 8 keV. Some sample spectra are shown from a Si-PIN diode detector. This system is well suited for testing X-ray mirror segments which are currently being developed.

  13. Instrumental limits to our knowledge of the X-ray sky

    NASA Astrophysics Data System (ADS)

    Guainazzi, Matteo

    2014-08-01

    In the last decade, performances of X-ray detectors have improved over all parameter spaces (throughput, energy and spatial resolution, timing). However, the quality of our science is only as good as the quality our instruments' calibration. Measurements of X-ray observables in celestial sources are increasingly limited by systematic rather then by statistical errors. Unfortunately, all attempts at defining X-ray "standard candles" have proven unsuccessful so far. The energy scale can be still absolutely calibrated through emission lines produced by atomic transitions in on-board or astrophysical calibration sources. Likewise, timing accuracy can be estimated using fast rotators such as the Crab pulsar. On the other hand, uncertainties at the level of the order of 10% (and more) affect the absolute flux calibration. These "cross-calibration" uncertainties are energy-dependent, thus implying uncertainties on spectral measurements. I present in this talk the calibration and cross-calibration status of historical and operational X-ray detectors. Efforts to monitor, document and improve the cross-calibration status are carried out primarily by the IACHEC (International Astronomical Consortium for High Energy Calibration: http://web.mit.edu/iachec/). I will also briefly discuss the impact that these uncertainties (may) have on fields as diverse as the measurements of spin in accreting black holes, and the determination of cosmological parameters through surveys of galaxy clusters.

  14. Ab initio simulation of diffractometer instrumental function for high-resolution X-ray diffraction.

    PubMed

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

    2015-06-01

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

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

    NASA Technical Reports Server (NTRS)

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

    1994-01-01

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

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

    SciTech Connect

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

    2007-08-01

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

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

    PubMed

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

    2016-11-01

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

  18. Status of the X-Ray Absorption Spectroscopy (XAS) Beamline at the Australian Synchrotron

    NASA Astrophysics Data System (ADS)

    Glover, C.; McKinlay, J.; Clift, M.; Barg, B.; Boldeman, J.; Ridgway, M.; Foran, G.; Garret, R.; Lay, P.; Broadbent, A.

    2007-02-01

    We present herein the current status of the X-ray Absorption Spectroscopy (XAS) Beamline at the 3 GeV Australian Synchrotron. The optical design and performance, details of the insertion device (Wiggler), end station capabilities and construction and commissioning timeline are given.

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

    SciTech Connect

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

    2007-11-07

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

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

    SciTech Connect

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

    1988-01-01

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

  1. LISA: the Italian CRG beamline for x-ray Absorption Spectroscopy at ESRF

    NASA Astrophysics Data System (ADS)

    d'Acapito, F.; Trapananti, A.; Puri, A.

    2016-05-01

    LISA is the acronym of Linea Italiana per la Spettroscopia di Assorbimento di raggi X (Italian beamline for X-ray Absorption Spectroscopy) and is the upgrade of the former GILDA beamline installed on the BM08 bending magnet port of European Synchrotron Radiation Facility (ESRF). Within this contribution a full description of the project is provided.

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

    PubMed Central

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

    2014-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-08-01

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

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

    DOE 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. Kβ1,3 XES spectra of MnII and Mn2III,IV complexes at room temperature were collected using a wavelength dispersive spectrometer and femtosecond X-ray pulses with an individual dose of up to >100 MGy. The spectra were found in agreement with undamaged spectra collected at low dose using synchrotron radiation. Our results demonstrate that the intact electronic structure of redox active transition metal compounds in different oxidation states can be characterized with this shot-by-shot method. This opens the door for studying the chemical dynamics of metal catalytic sites by following reactions under functional conditions. Furthermore, the technique can be combined with X-ray diffraction to simultaneously obtain the geometric structure of the overall protein and the local chemistry of active metal sites and is expected to prove valuable for understanding the mechanism of important metalloproteins, such as photosystem II.« less

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

    SciTech Connect

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

    2012-11-05

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

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

    PubMed

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

    2015-07-01

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

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

    SciTech Connect

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

    2015-07-15

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

  8. Revealing the electronic structure of LiC6 by soft X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Zhang, L.; Li, X.; Augustsson, A.; Lee, C. M.; Rubensson, J.-E.; Nordgren, J.; Ross, P. N.; Guo, J.-H.

    2017-03-01

    The electronic structure of LiC6 has been investigated 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 EF and the shift of σ* states to lower energies. In addition, the resonant inelastic X-ray scattering spectra of LiC6 do not show strong dispersive features as that of graphite, indicating that the crystal momentum is not conserved during the scattering process due to the delocalization of electrons in the intermediate state.

  9. Hard x-ray photoelectron spectroscopy of chalcopyrite solar cell components

    NASA Astrophysics Data System (ADS)

    Gloskovskii, A.; Jenkins, C. A.; Ouardi, S.; Balke, B.; Fecher, G. H.; Dai, X.-F.; Gruhn, T.; Johnson, B.; Lauermann, I.; Caballero, R.; Kaufmann, C. A.; Felser, C.

    2012-02-01

    Hard x-ray photoelectron spectroscopy is used to examine the partial density of states of Cu(In,Ga)Se2 (CIGSe), a semiconducting component of solar cells. The investigated, thin Cu(In,Ga)Se2 films were produced by multi-stage co-evaporation. Details of the measured core level and valence band spectra are compared to the calculated density of states. The semiconducting type electronic structure of Cu(In,Ga)Se2 is clearly resolved in the hard x-ray photoelectron spectra.

  10. Crystal spectroscopy of X-ray synchrotron source brightness

    NASA Astrophysics Data System (ADS)

    Als-Nielsen, Jens; Kjaer, Kristian

    1992-12-01

    Photon intensities in a monochromatic beam obtained by a horizontal Bragg reflection of synchrotron radiation by a monochromator crystal are compared for the three perfect crystals: silicon and germanium in symmetric (111) reflection and Diamond (C∗) in asymmetric (111) transmission geometry. Consistent results are obtained within relative bandwidths spanning a factor of 50 from Si(333) to Ge(111) and within a wavelength range form 0.4 Å to 1.6 Å. Results using a mosaic Be crystal within the same wavelength range depend in this work on a model of the mosaicity of the Be crystal. However, if the reflectivity of the Be crystal is determined experimentally for a few selected wavelengths, it is not necessary to invoke a mosaic model and a Be crystal may serve the purpose of characterizing the synchrotron beam as well as a perfect crystal. Thin diamond and beryllium crystals in transmission are particularly convenient for spectroscopy of very powerful beams from third generation synchrotron sources, because these low-Z elements absorb only a tiny fraction of the beam power.

  11. Time and space resolved spectroscopy of x-ray laser experiments

    SciTech Connect

    Ceglio, N.M.

    1986-04-01

    We report experimental data from one of the first of this new generation of instruments designed specifically for laboratory x-ray laser diagnosis. Representative TGSS-EM data are presented from three different x-ray laser inversion schemes: collisional excitation of neon-like selenium (lambda approx. = 206, 209A); resonant photoexcitation of hydrogen-like fluorine (lambda = 81A); and recombination of hydrogen-like magnesium (lambda approx. = 130A). The data illustrate the measurement capabilities of the TGSS-EM and provide insight to the dynamics and emission characteristics of this new class of laser produced plasmas.

  12. Photodissociation Structural Dynamics of TrirutheniumDodecacarbonyl Investigated by X-ray Transient Absorption Spectroscopy

    NASA Astrophysics Data System (ADS)

    Harpham, Michael R.; Stickrath, Andrew, B.; Zhang, Xiaoyi,; Huang, Jier; Mara, Michael W.; Chen, Lin X.; Liu, Di-Jia

    2013-10-01

    The molecular and electronic structures of the transient intermediates generated from the photolysis of trirutheniumdodecacarbonyl, Ru3(CO)12, by ultrafast UV (351 nm) laser excitation were investigated using X-ray transient absorption (XTA) spectroscopy. The electronic configuration change and nuclear rearrangement after the dissociation of carbonyls were observed at ruthenium K-edge X-ray absorption near edge structure and X-ray absorption fine structure spectra. Analysis of XTA data, acquired after 100, 200, and 400 ps and 300 ns time delay following the photoexcitation, identified the presence of three intermediate species with Ru3(CO)10 being the most dominating one. The results set an example of applying XTA in capturing both transient electronic and nuclear configurations in metal clusters simulating catalysts in chemical reactions.

  13. IN SITU STUDIES OF CORROSION USING X-RAY ABSORPTION NEAR SPECTROSCOPY (XANES)

    SciTech Connect

    ISAACS, H.S.; SCHMUKI, P.; VIRTANEN, S.

    2001-03-25

    Applications of x-ray absorption near-edge spectroscopy (XANES) and the design of cells for in situ corrosion studies are reviewed. Passive films studies require very thin metal or alloy layers be used having a thickness of the order of the films formed because of penetration of the x-ray beam into the metal substrate. The depth of penetration in water also limits the thickness of solutions that can be used because of water reduces the x-ray intensity. Solution thickness must also be limited in studies of conversion layer formation studies because the masking of the Cr in solution. Illustrative examples are taken from the anodic behavior of Al-Cr alloys, the growth of passive films on Fe and stainless steels, and the formation of chromate conversion layers on Al.

  14. 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.

  15. 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.

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

    PubMed Central

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

    2015-01-01

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

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

    SciTech Connect

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

    2015-11-27

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

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

    SciTech Connect

    Citron, Robert; Kropf, A.J.

    2008-01-01

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

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

    PubMed Central

    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

    2017-01-01

    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. PMID:28186190

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

    PubMed

    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

    2017-02-10

    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 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:Nx. The well-ordered chemical environments induced by nitrogen dopant are revealed by XANES and RIXS measurements.

  1. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-11-01

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

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

    SciTech Connect

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

    2009-06-30

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

  4. An alpha particle instrument with alpha, proton, and X-ray modes for planetary chemical analyses

    NASA Technical Reports Server (NTRS)

    Economou, T. E.; Turkevich, A. L.

    1976-01-01

    The interaction of alpha particles with matter is employed in a compact instrument that could provide rather complete in-situ chemical analyses of surfaces and thin atmospheres of extraterrestrial bodies. The instrument is a miniaturized and improved version of the Surveyor lunar instrument. The backscattering of alpha particles and (alpha, p) reactions provide analytical data on the light elements (carbon-iron). An X-ray mode that detects the photons produced by the alpha sources provides sensitivity and resolution for the chemical elements heavier than about silicon. The X-rays are detected by semiconductor detectors having a resolution between 150 and 250 eV at 5.9 keV. Such an instrument can identify and determine with good accuracy 99 percent of the atoms (except hydrogen) in rocks. For many trace elements, the detecting sensitivity is a few ppm. Auxiliary sources could be used to enhance the sensitivities for elements of special interest. The instrument could probably withstand the acceleration involved in semi-hard landings.

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

    PubMed

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

    2015-01-01

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

  6. Electronic ground states of Fe2(+) and Co2(+) as determined by x-ray absorption and x-ray magnetic circular dichroism spectroscopy.

    PubMed

    Zamudio-Bayer, V; Hirsch, K; Langenberg, A; Ławicki, A; Terasaki, A; V Issendorff, B; Lau, J T

    2015-12-28

    The (6)Π electronic ground state of the Co2 (+) diatomic molecular cation has been assigned experimentally by x-ray absorption and x-ray magnetic circular dichroism spectroscopy in a cryogenic ion trap. Three candidates, (6)Φ, (8)Φ, and (8)Γ, for the electronic ground state of Fe2 (+) have been identified. These states carry sizable orbital angular momenta that disagree with theoretical predictions from multireference configuration interaction and density functional theory. Our results show that the ground states of neutral and cationic diatomic molecules of 3d transition elements cannot generally be assumed to be connected by a one-electron process.

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

    NASA Astrophysics Data System (ADS)

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

    2011-12-01

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

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

    NASA Astrophysics Data System (ADS)

    McCammon, Dan

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

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

    NASA Astrophysics Data System (ADS)

    Church, Jonathan R.

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

  10. 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.

  11. Fabrication and testing of off-plane gratings for future x-ray spectroscopy missions

    NASA Astrophysics Data System (ADS)

    DeRoo, Casey T.

    Soft X-ray spectroscopy is a useful observational tool, offering information about high-temperature (106 - 107 K) astrophysical plasmas and providing useful characterizations of a number of energetic systems, including accreting young stars, cosmic filaments between galaxies, and supermassive black holes. In order to yield high resolution spectra with good signal-to-noise, however, soft X-ray spectrometers must realize improvements in resolving power and effective area through the development of high performance gratings. Off-plane reflection gratings offer the capability to work at high dispersions with excellent throughput, and are a viable candidate technology for future X-ray spectroscopy missions. The off-plane geometry requires a customizable grating meeting distinct fabrication requirements, and a process for producing gratings meeting these requirements has been developed. These fabricated gratings have been evaluated for performance in terms of resolution and diffraction efficiency. Furthermore, these gratings have been conceptually implemented in a soft X-ray spectrometer, the Off-Plane Grating Rocket Experiment (OGRE), whose optical design provides a template for future missions to achieve high performance within a small payload envelope.

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

    PubMed

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

    2016-10-14

    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.

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

    NASA Astrophysics Data System (ADS)

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

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

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

    SciTech Connect

    Peele, A. G.

    1999-12-15

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

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

    SciTech Connect

    Wang, Xin

    1996-12-01

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

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

    SciTech Connect

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

    1997-08-01

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

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

    SciTech Connect

    Hamad, Kimberly Sue

    2000-01-01

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

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

    SciTech Connect

    Yachandra, Vittal K.

    2002-04-02

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

  19. The x-ray polarimeter instrument on board the Polarimeter for Relativistic Astrophysical X-ray Sources (PRAXyS) mission

    NASA Astrophysics Data System (ADS)

    Hill, J. E.; Black, J. K.; Jahoda, K.; Tamagawa, T.; Iwakiri, W.; Kitaguchi, T.; Kubota, M.; Kaaret, P.; McCurdy, R.; Miles, D. M.; Okajima, T.; Soong, Y.; Olsen, L.; Sparr, L.; Mosely, S. J.; Nolan, D.

    2016-07-01

    The Polarimeter for Relativistic Astrophysical X-ray Sources (PRAXyS) is one of three Small Explorer (SMEX) missions selected by NASA for Phase A study. The PRAXyS observatory carries an X-ray Polarimeter Instrument (XPI) capable of measuring the linear polarization from a variety of high energy sources, including black holes, neutron stars, and supernova remnants. The XPI is comprised of two identical mirror-Time Projection Chamber (TPC) polarimeter telescopes with a system effective area of 124 cm2 at 3 keV, capable of photon limited observations for sources as faint as 1 mCrab. The XPI is built with well-established technologies. This paper will describe the performance of the XPI flight mirror with the engineering test unit polarimeter.

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

    NASA Technical Reports Server (NTRS)

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

    1997-01-01

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

  1. Large Area X-ray Proportional Counter (LAXPC) instrument onboard ASTROSAT

    NASA Astrophysics Data System (ADS)

    Yadav, J. S.; Agrawal, P. C.; Antia, H. M.; Chauhan, Jai Verdhan; Dedhia, Dhiraj; Katoch, Tilak; Madhwani, P.; Manchanda, R. K.; Misra, Ranjeev; Pahari, Mayukh; Paul, B.; Shah, Parag

    2016-07-01

    ASTROSAT, India's first dedicated astronomy space mission was launched on September 28, 2015. The Large Area X-ray Proportional Counter (LAXPC) is one of the major payloads on ASTROSAT. A cluster of three co-aligned identical LAXPC detectors provide large area of collection .The large detection volume (15 cm depth) filled with mixture of xenon gas (90(%) and methane (10%) at 2 atmospheres pressure, results in detection efficiency greater than 50%, above 30 keV. The LAXPC instrument is best suited for X-ray timing and spectral studies. It will provide the largest effective area in 3-80 keV range among all the satellite missions flown so far worldwide and will remain so for the next 5-10 years. The LAXPC detectors have been calibrated using radioactive sources in the laboratory. GEANT4 simulation for LAXPC detectors was carried out to understand detector background and its response. The LAXPC instrument became fully operational on 19th October 2015 for the first time in space. We have performed detector calibration in orbit. The LAXPC instrument is functioning well and has achieved all detector parameters proposed initially. In this paper, we will describe LAXPC detector calibration in lab as well as in orbit along with first results.

  2. Multilayer graphene stacks grown by different methods-thickness measurements by X-ray diffraction, Raman spectroscopy and optical transmission

    SciTech Connect

    Tokarczyk, M. Kowalski, G.; Kępa, H.; Grodecki, K.; Drabińska, A.; Strupiński, W.

    2013-12-15

    X-ray diffraction, Raman spectroscopy and Optical absorption estimates of the thickness of graphene multi layer stacks (number of graphene layers) are presented for three different growth techniques. The objective of this work was focused on comparison and reconciliation of the two already widely used methods for thickness estimates (Raman and Absorption) with the calibration of the X-ray method as far as Scherer constant K is concerned and X-ray based Wagner-Aqua extrapolation method.

  3. Direct Determination of Oxidation States of Uranium in Mixed-Valent Uranium Oxides Using Total Reflection X-ray Fluorescence X-ray Absorption Near-Edge Spectroscopy.

    PubMed

    Sanyal, Kaushik; Khooha, Ajay; Das, Gangadhar; Tiwari, M K; Misra, N L

    2017-01-03

    Total reflection X-ray fluorescence (TXRF)-based X-ray absorption near-edge spectroscopy has been used to determine the oxidation state of uranium in mixed-valent U3O8 and U3O7 uranium oxides. The TXRF spectra of the compounds were measured using variable X-ray energies in the vicinity of the U L3 edge in the TXRF excitation mode at the microfocus beamline of the Indus-2 synchrotron facility. The TXRF-based X-ray absorption near-edge spectroscopy (TXRF-XANES) spectra were deduced from the emission spectra measured using the energies below and above the U L3 edge in the XANES region. The data processing using TXRF-XANES spectra of U(IV), U(V), and U(VI) standard compounds revealed that U present in U3O8 is a mixture of U(V) and U(VI), whereas U in U3O7 is mixture of U(IV) and U(VI). The results obtained in this study are similar to that reported in literature using the U M edge. The present study has demonstrated the possibility of application of TXRF for the oxidation state determination and elemental speciation of radioactive substances in a nondestructive manner with very small amount of sample requirement.

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

    PubMed

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

    2012-10-01

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

  5. Toward femtosecond X-ray spectroscopy at the Advanced Light Source

    NASA Astrophysics Data System (ADS)

    Chong, Henry Herng Wei

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

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

    SciTech Connect

    Chong, Henry Herng Wei

    2004-01-01

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

  7. Total reflection X-ray photoelectron spectroscopy as a semiconductor lubricant elemental analysis method

    NASA Astrophysics Data System (ADS)

    Alshehabi, Abbas; Sasaki, Nobuharu; Kawai, Jun

    2015-12-01

    Photoelectron spectra from a typical hard disk storage media device (HDD) were measured at total reflection and non-total reflection at unburnished, acetone-cleaned, and argon-sputtered conditions. F, O, N, and C usually making the upper layer of a typical hard disk medium were detected. Enhancement of the photoelectron emission of the fluorocarbon lubricant was observed at total reflection. Pt and Co were only found by non-total X-ray photoelectron spectroscopy (XPS) because they are constituents of a deeper region than the top and interface regions. Argon-sputtered, ultrasonic acetone-cleaned, and unburnished top layers were compared at total and non-total reflection conditions. Total reflection X-ray photoelectron spectroscopy (TRXPS) is demonstrated to be a powerful tool for storage media lubrication layer chemical state analysis, reliable for industrial quality control application , and reproducible.

  8. Direction dependent diffusion of aligned magnetic rods by means of x-ray photon correlation spectroscopy.

    PubMed

    Wagner, Joachim; Märkert, Christian; Fischer, Birgit; Müller, Leonard

    2013-01-25

    Rodlike hematite particles in suspension align perpendicular to an external magnetic field due to a negative anisotropy of their magnetic susceptibility Δχ. The diffusion tensor consists of two principal constants D(∥) and D(⊥) for the diffusion parallel and perpendicular to the long particle axis. X-ray photon correlation spectroscopy is capable of probing the diffusive motion in optically opaque suspensions of rodlike hematite particles parallel to the direction of the scattering vector Q. Choosing Q parallel or perpendicular to the direction of an external magnetic field H the direction dependent intermediate scattering function is measured by means of x-ray photon correlation spectroscopy. From the intermediate scattering function in both directions the principal diffusion constants D(∥) and D(⊥) are determined. The ratio D(∥)/D(⊥) increases with increasing aspect ratio of the particles and can be described via a rescaled theoretical approach for prolate ellipsoids of revolution.

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

    SciTech Connect

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

    2009-05-27

    Water oxidation to dioxygen in photosynthesis is catalyzed by a Mn{sub 4}Ca cluster with O bridging in Photosystem II (PS II) of plants, algae and cyanobacteria. A variety of spectroscopic methods have been applied to analyzing the participation of the complex. X-ray spectroscopy is particularly useful because it is element-specific, and because it can reveal important structural features of the complex with high accuracy and identify the participation of Mn in the redox chemistry. Following a brief history of the application of X-ray spectroscopy to PS II, an overview of newer results will be presented and a description of the present state of our knowledge based on this approach.

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

    SciTech Connect

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

    2015-07-15

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

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

    NASA Technical Reports Server (NTRS)

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

    2005-01-01

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

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

    SciTech Connect

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

    2014-10-15

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-07-01

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

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

    PubMed

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

    2014-10-01

    A new liquid flow-cell designed for electronic structure investigations at the liquid-solid interface by soft X-ray absorption and emission spectroscopy is presented. A thin membrane serves simultaneously as a substrate for the working electrode and solid state samples as well as for separating the liquid from the surrounding vacuum conditions. In combination with counter and reference electrodes this approach allows in-situ studies of electrochemical deposition processes and catalytic reactions at the liquid-solid interface in combination with potentiostatic measurements. As model system in-situ monitoring of the deposition process of Co metal from a 10 mM CoCl2 aqueous solution by X-ray absorption and emission spectroscopy is presented.

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

    SciTech Connect

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

    2007-04-05

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

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

    NASA Astrophysics Data System (ADS)

    Karunaratne, V. N. C.

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

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

    SciTech Connect

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

    2009-10-01

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

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

    SciTech Connect

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

    2008-01-22

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

  19. Synchrotron X-ray Powder Diffraction and Absorption Spectroscopy in Pulsed Magnetic Fields with Milliseconds Duration

    NASA Astrophysics Data System (ADS)

    Vanacken, J.; Detlefs, C.; Mathon, O.; Frings, P.; Duc, F.; Lorenzo, J. E.; Nardone, M.; Billette, J.; Zitouni, A.; Dominguez, M.-C.; Herczeg, J.; Bras, W.; Moshchalkov, V. V.; Rikken, G.

    2007-03-01

    X-ray Powder Diffraction and X-ray Absorption Spectroscopy experiments (WAS) and X-ray magnetic circular dichroism (XMCD) experiments were carried out at the ESRF DUBBLE beam line (BM26) and at the energy dispersive beam line (ID24), respectively. A mobile pulse generator, developed at the LNCMP, delivered 110kJ to the load coil, which was sufficient to generate peak fields of 30T with a rise time of about 5 ms. A liquid He flow cryostat allowed us to vary the sample temperature accurately between 4.2K and 300K. Powder diffraction patterns of TbVO4 were recorded in a broad temperature range using 21 keV monochromatic X-rays and using an on-line image plate detector. We observed the suppression of the Jahn-Teller structural distortion in TbVO4 due to the high magnetic pulsed field. XAS spectra could be measured and finite XMCD signals, directly proportional to the magnetic moment on the Gd absorber atom, were measured in thin Gd foils. Thanks to its element and orbital selectivity, XMCD proofs to be very useful in probing the magnetic properties and due to the strong brilliance of the synchrotron beam, the signals can be measured even in the ms range.

  20. Undistorted X-ray Absorption Spectroscopy Using s-Core-Orbital Emissions.

    PubMed

    Golnak, Ronny; Xiao, Jie; Atak, Kaan; Unger, Isaak; Seidel, Robert; Winter, Bernd; Aziz, Emad F

    2016-05-12

    Detection of secondary emissions, fluorescence yield (FY), or electron yield (EY), originating from the relaxation processes upon X-ray resonant absorption has been widely adopted for X-ray absorption spectroscopy (XAS) measurements when the primary absorption process cannot be probed directly in transmission mode. Various spectral distortion effects inherent in the relaxation processes and in the subsequent transportation of emitted particles (electron or photon) through the sample, however, undermine the proportionality of the emission signals to the X-ray absorption coefficient. In the present study, multiple radiative (FY) and nonradiative (EY) decay channels have been experimentally investigated on a model system, FeCl3 aqueous solution, at the excitation energy of the Fe L-edge. The systematic comparisons between the experimental spectra taken from various decay channels, as well as the comparison with the theoretically simulated Fe L-edge XA spectrum that involves only the absorption process, indicate that the detection of the Fe 3s → 2p partial fluorescence yield (PFY) gives rise to the true Fe L-edge XA spectrum. The two key characteristics generalized from this particular decay channel-zero orbital angular momentum (i.e., s orbital) and core-level emission-set a guideline for obtaining undistorted X-ray absorption spectra in the future.

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

    NASA Astrophysics Data System (ADS)

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

    2015-07-01

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

  2. Analysis of some Nigerian solid mineral ores by energy-dispersive X-ray fluorescence spectroscopy

    NASA Astrophysics Data System (ADS)

    Obiajunwa, E. I.

    2001-11-01

    Determination of major, minor and trace elements in some Nigerian solid mineral ores by energy-dispersive X-ray fluorescence (EDXRF) spectroscopy is described. Concentration values of major, minor and trace elements for Z>18 are reported. The mineral ores studied include (i) tantalite-coloumbite minerals, (ii) bismuth minerals and (iii) lead minerals. The accuracy and precision of the technique for chemical analysis was assured by analysing the geological standards mica-Fe (biotite) and NBS 278 (obsidian).

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

    SciTech Connect

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

    1992-01-01

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

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

    SciTech Connect

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

    1992-10-01

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

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

    SciTech Connect

    Paesler, M.; Sayers, D.

    1988-12-01

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

  6. An X-Ray Photoelectron Spectroscopy (XPS) Study of Activated Carbons Impregnated with some Organocopper Complexes,

    DTIC Science & Technology

    1993-10-01

    AD-A282 721 l lllllll a Dfene Defence nationals AN X.RAY PHOTOELECTRON SPECTROSCOPY (XPS) STUDY OF ACTIVATED CARBONS IMPREGNATED WITH SOME... ammoniacal solution as a carrier into which all impregnants (except TEDA) were dissolved. Without a suitable carrier, and with the inherent low vapor...and will not be repeated here. All five complexes were synthesized at DREO using known methods. 2 2.2 IMPREGNATING PROCEDURES Two impregnating

  7. Soft X-Ray Spectroscopy of the Cygnus Loop Supernova Remnant

    NASA Astrophysics Data System (ADS)

    McEntaffer, R. L.; Cash, W.

    2008-06-01

    The Cygnus X-Ray Emission Spectroscopic Survey (CyXESS) sounding rocket payload was launched from White Sands Missile Range on 2006 November 20 and obtained a high-resolution spectrum of the Cygnus Loop supernova remnant in the soft X-ray. The novel X-ray spectrograph incorporated a wire-grid collimator feeding an array of gratings in the extreme off-plane mount that ultimately dispersed the spectrum onto gaseous electron multiplier (GEM) detectors. This instrument recorded 65 s of usable data between 43 and 49.5 Å in two prominent features. The first feature near 45 Å is dominated by the He-like triplet of O VII in second order with contributions from Mg X and Si IX-Si XII in first order, while the second feature near 47.5 Å is first-order S IX and S X. Fits to the spectra give an equilibrium plasma at log (T) = 6.2 (kTe = 0.14 keV) and near cosmic abundances. This is consistent with previous observations, which demonstrated that the soft X-ray emission from the Cygnus Loop is dominated by interactions between the initial blast wave and the walls of a precursor-formed cavity surrounding the Cygnus Loop and that this interaction can be described using equilibrium conditions.

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

    NASA Astrophysics Data System (ADS)

    Stout, Kevin D.; Masterson, Rebecca A.

    2014-08-01

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

  9. Micro X-ray Fluorescence Imaging in a Tabletop Full Field-X-ray Fluorescence Instrument and in a Full Field-Particle Induced X-ray Emission End Station.

    PubMed

    Romano, Francesco Paolo; Caliri, Claudia; Cosentino, Luigi; Gammino, Santo; Mascali, David; Pappalardo, Lighea; Rizzo, Francesca; Scharf, Oliver; Santos, Hellen Cristine

    2016-10-08

    A full field-X-ray camera (FF-XRC) was developed for performing the simultaneous mapping of chemical elements with a high lateral resolution. The device is based on a conventional CCD detector coupled to a straight shaped polycapillary. Samples are illuminated at once with a broad primary beam that can consist of X-rays or charged particles in two different analytical setups. The characteristic photons induced in the samples are guided by the polycapillary to the detector allowing the elemental imaging without the need for scanning. A single photon counting detection operated in a multiframe acquisition mode and a processing algorithm developed for event hitting reconstruction have enabled one to use the CCD as a high energy resolution X-ray detector. A novel software with a graphical user interface (GUI) programmed in Matlab allows full control of the device and the real-time imaging with a region-of-interest (ROI) method. At the end of the measurement, the software produces spectra for each of the pixels in the detector allowing the application of a least-squares fitting with external analytical tools. The FF-XRC is very compact and can be installed in different experimental setups. This work shows the potentialities of the instrument in both a full field-micro X-ray fluorescence (FF-MXRF) tabletop device and in a full field-micro particle induced X-ray emission (FF-MPIXE) end-station operated with an external proton beam. Some examples of applications are given as well.

  10. The high-energy celestial X-ray instrument on board OSO-8

    NASA Technical Reports Server (NTRS)

    Dennis, B. R.; Frost, K. J.; Lencho, R. J.; Orwig, L. E.

    1977-01-01

    The 20 keV-3 MeV celestial X-ray detector on the OSO-8 is described. The primary objectives of this instrument are to measure the energy spectrum of cosmic X-ray sources above 20 keV and to search for time variations, both periodic and irregular, in the intensity of the sources detected. The detector consists of two optically isolated central crystals shielded by a large, active collimator. The sensitive area is 27.5 sq cm and the field-of-view is 5 deg FWHM. The instrument is mounted in the wheel section of OSO-8 with the axis of its field of view offset by 5 deg from the negative spin axis of the wheel. The minimum detectable intensity of a point source which is brought to within 5 deg of the negative spin axis for greater than one day is about 10 to the minus fifth power photons/sq cm-sec at 100 keV.

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

    NASA Technical Reports Server (NTRS)

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

    2007-01-01

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

  12. Cryogen-free operation of the Soft X-ray Spectrometer instrument

    NASA Astrophysics Data System (ADS)

    Sneiderman, Gary A.; Shirron, Peter J.; Fujimoto, Ryuichi; Bialas, Thomas G.; Boyce, Kevin R.; Chiao, Meng P.; DiPirro, Michael J.; Eckart, Megan E.; Hartz, Leslie; Ishisaki, Yoshitaka; Kelley, Richard L.; Kilbourne, Caroline A.; Masters, Candace; McCammon, Dan; Mitsuda, Kazuhisa; Noda, Hirofumi; Porter, Frederick S.; Szymkowiak, Andrew E.; Takei, Yoh; Tsujimoto, Masahiro; Yoshida, Seiji

    2016-07-01

    The Soft X-ray Spectrometer (SXS) is the first space-based instrument to implement redundancy in the operation of a sub-Kelvin refrigerator. The SXS cryogenic system consists of a superfluid helium tank and a combination of Stirling and Joule-Thompson (JT) cryocoolers that support the operation of a 3-stage adiabatic demagnetization refrigerator (ADR). When liquid helium is present, the x-ray microcalorimeter detectors are cooled to their 50 mK operating temperature by two ADR stages, which reject their heat directly to the liquid at 1.1 K. When the helium is depleted, all three ADR stages are used to accomplish detector cooling while rejecting heat to the JT cooler operating at 4.5 K. Compared to the simpler helium mode operation, the cryogen-free mode achieves the same instrument performance by controlling the active cooling devices within the cooling system differently. These include the three ADR stages and four active heat switches, provided by NASA, and five cryocoolers, provided by JAXA. Development and verification details of this capability are presented within this paper and offer valuable insights into the challenges, successes, and lessons that can benefit other missions, particularly those employing cryogen-free cooling systems.

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

    PubMed

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

    2016-03-15

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

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

    NASA Astrophysics Data System (ADS)

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

    1999-09-01

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

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

    NASA Technical Reports Server (NTRS)

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

    1999-01-01

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

  16. Isotope and temperature effects in liquid water probed by x-ray absorption and resonant x-ray emission spectroscopy.

    PubMed

    Fuchs, O; Zharnikov, M; Weinhardt, L; Blum, M; Weigand, M; Zubavichus, Y; Bär, M; Maier, F; Denlinger, J D; Heske, C; Grunze, M; Umbach, E

    2008-01-18

    High-resolution x-ray absorption and emission spectra of liquid water exhibit a strong isotope effect. Further, the emission spectra show a splitting of the 1b1 emission line, a weak temperature effect, and a pronounced excitation-energy dependence. They can be described as a superposition of two independent contributions. By comparing with gas phase, ice, and NaOH/NaOD, we propose that the two components are governed by the initial state hydrogen bonding configuration and ultrafast dissociation on the time scale of the O 1s core hole decay.

  17. An XPS (X-Ray Photoelectron Spectroscopy) Study of the Composition of Thin Polyimide Films Formed by Vapor Deposition.

    DTIC Science & Technology

    1987-07-15

    Deposition, volycrystalline ? Silver, 0xidianiline (ODA), Benzenetetracarboxylic anhydride (PMDA), .- imidization, polymer , in situ, X-ray Photoelectron...imidization reaction leading to polymer formation was followed in situ with X-ray Photoelectron Spectroscopy. The uncertainties inherent in a...is an important polymer for application in solid state electronic technology because of its favorable dielectric properties and high thermal

  18. Non-conventional applications of a noninvasive portable X-ray diffraction/fluorescence instrument

    NASA Astrophysics Data System (ADS)

    Chiari, Giacomo; Sarrazin, Philippe; Heginbotham, Arlen

    2016-11-01

    Noninvasive techniques have become widespread in the cultural heritage analytical domain. The popular handheld X-ray fluorescence (XRF) devices give the elemental composition of all the layers that X-rays can penetrate, but no information on how atoms are bound together or at which depth they are located. A noninvasive portable X-ray powder diffraction/X-ray fluorescence (XRD/XRF) device may offer a solution to these limitations, since it can provide information on the composition of crystalline materials. This paper introduces applications of XRD beyond simple phase recognition. The two fundamental principles for XRD are: (1) the crystallites should be randomly oriented, to ensure proper intensity to all the diffraction peaks, and (2) the material should be positioned exactly in the focal plane of the instrument, respecting its geometry, as any displacement of the sample would results in 2 θ shifts of the diffraction peaks. In conventional XRD, the sample is ground and set on the properly positioned sample holder. Using a noninvasive portable instrument, these two requirements are seldom fulfilled. The position, size and orientation of a given crystallite within a layered structure depend on the object itself. Equation correlating the displacement (distance from the focal plane) versus peak shift (angular difference in 2 θ from the standard value) is derived and used to determine the depth at which a given substance is located. The quantitative composition of two binary Cu/Zn alloys, simultaneously present, was determined measuring the cell volume and using Vegard's law. The analysis of the whole object gives information on the texture and possible preferred orientations of the crystallites, which influences the peak intensity. This allows for the distinction between clad and electroplated daguerreotypes in the case of silver and between ancient and modern gilding for gold. Analyses of cross sections can be carried out successfully. Finally, beeswax, used in

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

    NASA Astrophysics Data System (ADS)

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

    2015-07-01

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

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

    SciTech Connect

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

    1997-04-01

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

  1. Analytical performance of benchtop total reflection X-ray fluorescence instrumentation for multielemental analysis of wine samples

    NASA Astrophysics Data System (ADS)

    Dalipi, Rogerta; Marguí, Eva; Borgese, Laura; Bilo, Fabjola; Depero, Laura E.

    2016-06-01

    Recent technological improvements have led to a widespread adoption of benchtop total reflection X-ray fluorescence systems (TXRF) for analysis of liquid samples. However, benchtop TXRF systems usually present limited sensitivity compared with high-scale instrumentation which can restrict its application in some fields. The aim of the present work was to evaluate and compare the analytical capabilities of two TXRF systems, equipped with low power Mo and W target X-ray tubes, for multielemental analysis of wine samples. Using the Mo-TXRF system, the detection limits for most elements were one order of magnitude lower than those attained using the W-TXRF system. For the detection of high Z elements like Cd and Ag, however, W-TXRF remains a very good option due to the possibility of K-Lines detection. Accuracy and precision of the obtained results have been evaluated analyzing spiked real wine samples and comparing the TXRF results with those obtained by inductively coupled plasma emission spectroscopy (ICP-OES). In general, good agreement was obtained between ICP-OES and TXRF results for the analysis of both red and white wine samples except for light elements (i.e., K) which TXRF concentrations were underestimated. However, a further achievement of analytical quality of TXRF results can be achieved if wine analysis is performed after dilution of the sample with de-ionized water.

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

    PubMed

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

    2010-01-01

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

  3. Caliste-SO X-ray micro-camera for the STIX instrument on-board Solar Orbiter space mission

    NASA Astrophysics Data System (ADS)

    Meuris, A.; Hurford, G.; Bednarzik, M.; Limousin, O.; Gevin, O.; Le Mer, I.; Martignac, J.; Horeau, B.; Grimm, O.; Resanovic, R.; Krucker, S.; Orleański, P.

    2012-12-01

    The Spectrometer Telescope for Imaging X-rays (STIX) is an instrument on the Solar-Orbiter space mission that performs hard X-ray imaging spectroscopy of solar flares. It consists of 32 collimators with grids and 32 spectrometer units called Caliste-SO for indirect Fourier-transform imaging. Each Caliste-SO device integrates a 1 cm2 CdTe pixel sensor with a low-noise low-power analog front-end ASIC and circuits for supply regulation and filtering. The ASIC named IDeF-X HD is designed by CEA/Irfu (France) whereas CdTe-based semiconductor detectors are provided by the Laboratory for Micro- and Nanotechnology, Paul Scherrer Institute (Switzerland). The design of the hybrid, based on 3D Plus technology (France), is well suited for STIX spectroscopic requirements (1 keV FWHM at 6 keV, 4 keV low-level threshold) and system constraints (4 W power and 5 kg mass). The performance of the sub-assemblies and the design of the first Caliste-SO prototype are presented.

  4. Multiple pre-edge structures in Cu K -edge x-ray absorption spectra of high- Tc cuprates revealed by high-resolution x-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Gougoussis, C.; Rueff, J.-P.; Calandra, M.; D'Astuto, M.; Jarrige, I.; Ishii, H.; Shukla, A.; Yamada, I.; Azuma, M.; Takano, M.

    2010-06-01

    Using high-resolution x-ray absorption spectroscopy and state-of-the-art electronic structure calculations we demonstrate that the pre-edge region at the Cu K edge of high- Tc cuprates is composed of several excitations invisible in standard x-ray absorption spectra. We consider in detail the case of Ca2-xCuO2Cl2 and show that the many pre-edge excitations (two for c -axis polarization, four for in-plane polarization and out-of-plane incident x-ray momentum) are dominated by off-site transitions and intersite hybridization. This demonstrates the relevance of approaches beyond the single-site model for the description of the pre edges of correlated materials. Finally, we show the occurrence of a doubling of the main edge peak that is most visible when the polarization is along the c axis. This doubling, that has not been seen in any previous absorption data in cuprates, is not reproduced by first-principles calculations. We suggest that this peak is due to many-body charge-transfer excitations while all the other visible far-edge structures are single particle in origin. Our work indicates that previous interpretations of the Cu K -edge x-ray absorption spectra in high- Tc cuprates can be profitably reconsidered.

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

    NASA Astrophysics Data System (ADS)

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

    2011-12-01

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

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

    PubMed Central

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

    2012-01-01

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

  7. 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

  8. Calcium in the oxygen-evolving complex: structural and mechanistic role determined by X-ray spectroscopy.

    PubMed

    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 Mn(4)Ca catalytic center.

  9. Nm-scale spatial resolution x-ray imaging with MLL nanofocusing optics: instrumentational requirements and challenges

    SciTech Connect

    Nazaretski, E.; Yan, H.; Lauer, K.; Huang, X.; Xu, W.; Kalbfleisch, S.; Yan, Hui; Li, Li; Bouet, N.; Zhou, J.; Shu, D.; Conley, R.; Chu, Y. S.

    2016-08-30

    The Hard X-ray Nanoprobe (HXN) beamline at NSLS-II has been designed and constructed to enable imaging experiments with unprecedented spatial resolution and detection sensitivity. The HXN X-ray Microscope is a key instrument for the beamline, providing a suite of experimental capabilities which includes scanning fluorescence, diffraction, differential phase contrast and ptychography utilizing Multilayer Laue Lenses (MLL) and zoneplate (ZP) as nanofocusing optics. In this paper, we present technical requirements for the MLL-based scanning microscope, outline the development concept and present first ~15 x 15 nm2 spatial resolution x-ray fluorescence images.

  10. Algorithms for a hand-held miniature x-ray fluorescence analytical instrument

    SciTech Connect

    Elam, W.T.; Newman, D.; Ziemba, F.

    1998-12-31

    The purpose of this joint program was to provide technical assistance with the development of a Miniature X-ray Fluorescence (XRF) Analytical Instrument. This new XRF instrument is designed to overcome the weaknesses of spectrometers commercially available at the present time. Currently available XRF spectrometers (for a complete list see reference 1) convert spectral information to sample composition using the influence coefficients technique or the fundamental parameters method. They require either a standard sample with composition relatively close to the unknown or a detailed knowledge of the sample matrix. They also require a highly-trained operator and the results often depend on the capabilities of the operator. In addition, almost all existing field-portable, hand-held instruments use radioactive sources for excitation. Regulatory limits on such sources restrict them such that they can only provide relatively weak excitation. This limits all current hand-held XRF instruments to poor detection limits and/or long data collection times, in addition to the licensing requirements and disposal problems for radioactive sources. The new XRF instrument was developed jointly by Quantrad Sensor, Inc., the Naval Research Laboratory (NRL), and the Department of Energy (DOE). This report describes the analysis algorithms developed by NRL for the new instrument and the software which embodies them.

  11. 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.

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

    PubMed

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

    2007-07-15

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

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

    SciTech Connect

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

    2015-06-22

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

  14. The X-ray Microcalorimeter Spectrometer (XMS): A Reference Cryogenic Instrument Design for Constellation-X

    NASA Technical Reports Server (NTRS)

    Whitehouse, Paul L.

    2003-01-01

    Constellation-X, a mission now belonging to the Beyond Einstein initiative, is being planned to inherit the x-ray sky from Chandra, XMM-Newton and Astro-E. The first two of four observatories in the constellation will be launched together in 2013 and followed a year later by the launch of the remaining two. The four will independently orbit the Sun-Earth Lagrange point L2. An instrument compliment resides in the Focal Plane Module (FPM) of each observatory 10 m from the Optics Module and consists of three Hard X-ray Telescope (HXT) detectors, a Reflection Grating Spectrometer (RGS) focal plane CCD camera and an X-ray Microcalorimeter Spectrometer (XMS). Instrument awards are scheduled for early 2006. The reference detector for XMS is a 32 x 32 array of microcalorimetric superconducting Transition Edge Sensors (TES). Each pixel casts a variable resistance in a SQUID based multiplexed readout circuit which is coupled to series SQUID arrays for amplification and finally read out by external electronics. A multi-stage continuous ADR will provide the stable 50 mK desired for the TES array and a stable 1 K for the series SQUID arrays while also lifting thermal parasitic and inefficiency loads to a 6 K cryocooler interface. The 6 K cryocooler is expected to emerge from the joint-project Advanced Cryocooler Technology Development Program (ACTDP) in which Constellation-X is an active participant. Project Pre-Formulation activities are marked by extensive technology development necessitating early, but realistic, thermal and cooling load requirements for ADR and ACTDP-cryocooler design points. Such requirements are driven by the encompassing XMS cryostat and ultimately by the thermal environment imposed by the FPM. It is further desired that the XMS instrument be able to operate on its side in the laboratory, with a warm vacuum shell, during an extensive calibration regime. It is that reference system design of the XMS instrument (microcalorimeter, ADR, cryocooler and

  15. X-ray Spectroscopy and Diffraction at HPCAT - An Integrated High Pressure Synchrotron Facility

    NASA Astrophysics Data System (ADS)

    Mao, H.; Hemley, R. J.; Hausermann, D.; Hu, M.; Meng, Y.; Somayazulu, M.

    2002-05-01

    High Pressure Collaborative Access Team (HPCAT) is a new facility dedicated for high-pressure research using the high-energy synchrotron beams at the Advanced Photon Source for in-situ investigations of crystallographic, elastic, rheologic, electronic, and magnetic properties of solids, liquids, and amorphous materials at high P and simultaneous high T or cryogenic T. The HPCAT high-brilliance undulator beamline is optimized for a full range of high-pressure x-ray spectroscopy. For instance, nuclear resonant inelastic scattering measures phonon densities of state of Fe-containing samples that yield valuable information on acoustic wave velocity, elasticity, elastic anisotropy, and thermodynamic quantities (vibrational energy, heat capacity, entropy, Debye temperature, and Gr\\x81neisen parameter) of materials at high pressures. Nuclear resonant x-ray forward scattering measures M”ssbauer spectra in the time domain that yield information on magnetism, site occupancy, oxidation states, and the Lamb-M”ssbauer coefficient of Fe. Resonant inelastic x-ray scattering measures element-specific electronic transitions. The medium-resolution (10-100 meV) non-resonant x-ray inelastic scattering measures electronic energies and dispersions that yield information on plasmons, excitons, electronic band structures, and chemical bondings, and high-resolution (<10 meV) inelastic scattering measures phonon dispersions that yield information on acoustic wave velocity and elasticity as a function of crystallographic orientation. X-ray emission spectroscopy yields information on valence electrons and spin states of d-electrons. A diamond branch monochromator diverts a full-intensity undulator monochromatic beam at energies up to 35 keV for full-time x-ray diffraction studies of crystallography, phase transitions, and equations of state in a side station without affecting the simultaneous operation of the main undualtor beamline. The HPCAT bending-magnet beamline is divided into two

  16. Identifying anthropogenic uranium compounds using soft X-ray near-edge absorption spectroscopy

    SciTech Connect

    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. 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, 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.

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

    SciTech Connect

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

    2014-08-21

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

  18. The nature of arsenic in uranium mill tailings by X-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Cutler, J. N.; Chen, N.; Jiang, D. T.; Demopoulos, G. P.; Jia, Y.; Rowson, J. W.

    2003-05-01

    In order to understand the evolving world of environmental issues, the ability to characterize and predict the stability and bioavailability of heavy métal contaminants in mine waste is becoming increasingly more important. X-ray Absorption Near Edge Structure (XANES) and Extended X-ray Absorption Fine Structure (EXAFS) spectroscopies were used to characterize a series of synthetic and natural samples associated with mine tailings processing. XANES was shown to be excellent as a tool to rapidly differentiate oxidation states of arsenic within the samples. The EXAFS spectra provided information on the mineralogy of the precipitated raffinate and tailings and showed that these samples are composed of a mixture of amorphous ferric arsenates, adsorbed arsenates and a mixture of other poorly ordered arsenates.

  19. 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.

  20. X-ray laser-induced photoelectron spectroscopy for single-state measurements

    NASA Astrophysics Data System (ADS)

    Nelson, A. J.; Dunn, J.; van Buuren, T.; Hunter, J.

    2004-12-01

    We demonstrate single-shot x-ray laser-induced time-of-flight photoelectron spectroscopy on metal and semiconductor surfaces with picosecond time resolution. Our compact multipulse terawatt tabletop x-ray laser source provides the necessary high photon flux (>1012/pulse), monochromaticity, picosecond pulse duration, and coherence for probing ultrafast changes in the chemical and electronic structure of these materials. Static valence band and shallow core-level photoemission spectra are presented for ambient temperature polycrystalline Cu foils and Ge(100). Surface contamination was removed by UV ozone cleaning prior to analysis. The ultrafast nature of this technique lends itself to true single-state measurements of shocked and heated materials.

  1. X-Ray Laser Induced Photoelectron Spectroscopy for Single-State Measurements

    SciTech Connect

    Nelson, A J; Dunn, J; van Buuren, T; Hunter, J

    2004-07-14

    We demonstrate single-shot x-ray laser induced time-of-flight photoelectron spectroscopy on metal and semiconductor surfaces with picosecond time resolution. The LLNL COMET compact tabletop x-ray laser source provides the necessary high photon flux (>10{sup 12}/pulse), monochromaticity, picosecond pulse duration, and coherence for probing ultrafast changes in the chemical and electronic structure of these materials. Static valence band and shallow core-level photoemission spectra are presented for ambient temperature polycrystalline Cu foils and Ge(100). Surface contamination was removed by UV ozone cleaning prior to analysis. The ultrafast nature of this technique lends itself to true single-state measurements of shocked and heated materials.

  2. Detection, identification and mapping of iron anomalies in brain tissue using X-ray absorption spectroscopy

    SciTech Connect

    Mikhaylova, A.; Davidson, M.; Toastmann, H.; Channell, J.E.T.; Guyodo, Y.; Batich, C.; Dobson, J.

    2008-06-16

    This work describes a novel method for the detection, identification and mapping of anomalous iron compounds in mammalian brain tissue using X-ray absorption spectroscopy. We have located and identified individual iron anomalies in an avian tissue model associated with ferritin, biogenic magnetite and haemoglobin with a pixel resolution of less than 5 {micro}m. This technique represents a breakthrough in the study of both intra- and extra-cellular iron compounds in brain tissue. The potential for high-resolution iron mapping using microfocused X-ray beams has direct application to investigations of the location and structural form of iron compounds associated with human neurodegenerative disorders - a problem which has vexed researchers for 50 years.

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

    SciTech Connect

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

    2015-06-21

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

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

    PubMed Central

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

    2016-01-01

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

  5. Electronic structure of warm dense copper studied by ultrafast x-ray absorption spectroscopy.

    PubMed

    Cho, B I; Engelhorn, K; Correa, A A; Ogitsu, T; Weber, C P; Lee, H J; Feng, J; Ni, P A; Ping, Y; Nelson, A J; Prendergast, D; Lee, R W; Falcone, R W; Heimann, P A

    2011-04-22

    We use time-resolved x-ray absorption spectroscopy to investigate the unoccupied electronic density of states of warm dense copper that is produced isochorically through the absorption of an ultrafast optical pulse. The temperature of the superheated electron-hole plasma, which ranges from 4000 to 10 000 K, was determined by comparing the measured x-ray absorption spectrum with a simulation. The electronic structure of warm dense copper is adequately described with the high temperature electronic density of state calculated by the density functional theory. The dynamics of the electron temperature is consistent with a two-temperature model, while a temperature-dependent electron-phonon coupling parameter is necessary.

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

    NASA Astrophysics Data System (ADS)

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

    2015-03-01

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

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

    SciTech Connect

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

    2015-03-15

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

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

    PubMed

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

    2013-02-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-09-01

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

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

    SciTech Connect

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

    2014-12-01

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

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

    SciTech Connect

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

    1997-09-01

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

  12. Structural studies of PCU-hydrazones: NMR spectroscopy, X-ray diffractions, and DFT calculations

    NASA Astrophysics Data System (ADS)

    Veljković, Jelena; Šekutor, Marina; Molčanov, Krešimir; Lo, Rabindranath; Ganguly, Bishwajit; Mlinarić-Majerski, Kata

    2011-06-01

    In this article we present a detailed structural investigation for the configurational isomers of PCU-hydrazones. The structural characterization of these hydrazones was performed using NMR spectroscopy, X-ray diffraction analysis and theoretical calculations. The single crystal X-ray structures of PCU-hydrazones 6B and 6C have been solved and used to conclusively confirm the characterization obtained via NMR spectra of a particular isomer. Nuclear magnetic shielding values calculated for 6A-C using DFT calculations were correlated with the experimentally determined chemical shifts. The computed results were found to be in good agreement with the observed 13C NMR values. The computed NMR results helped to ascertain the isomers of PCU-hydrazones 4A-C.

  13. Microcalorimeters for High Resolution X-Ray Spectroscopy of Laboratory and Astrophysical Plasmas

    NASA Technical Reports Server (NTRS)

    Silver, E.; Flowers, Bobby J. (Technical Monitor)

    2003-01-01

    The proposal has three major objectives. The first focuses on advanced neutron-transmutation-doped (NTD)-based microcalorimeter development. Our goal is to develop an array of microcalorimeters with sub- 5 eV energy resolution that can operate with pile-up-free throughput of at least 100 Hz per pixel. The second objective is to establish our microcalorimeter as an essential x-ray diagnostic for laboratory astrophysics studies. We propose to develop a dedicated microcalorimeter spectrometer for the EBIT (electron beam ion trap). This instrument will incorporate the latest detector and cryogenic technology that we have available. The third objective is to investigate innovative ideas related to possible flight opportunities. These include compact, long lived cryo-systems, ultra-low temperature cold stages, low mass and low power electronics, and novel assemblies of thin windows with high x-ray transmission.

  14. Theoretical calculations and instrument development and test characterization of low intensity X-ray imaging devices

    NASA Technical Reports Server (NTRS)

    Ferguson, G.; Lewis, M.; Harval, R.; Anderson, J.; Brown, S.

    1978-01-01

    The characteristics of the Lixiscope when excited by X-rays produced by conventional electrically powered X-ray generators are explored to determine the optimum X-ray spectrum and mode of operation of the generator, which yields satisfactory Lixiscope images of medical and industrial specimens.

  15. Demonstration of a time-resolved x-ray scattering instrument utilizing the full-repetition rate of x-ray pulses at the Pohang Light Source

    NASA Astrophysics Data System (ADS)

    Jo, Wonhyuk; Eom, Intae; Landahl, Eric C.; Lee, Sooheyong; Yu, Chung-Jong

    2016-03-01

    We report on the development of a new experimental instrument for time-resolved x-ray scattering (TRXS) at the Pohang Light Source (PLS-II). It operates with a photon energy ranging from 5 to 18 keV. It is equipped with an amplified Ti:sappahire femtosecond laser, optical diagnostics, and laser beam delivery for pump-probe experiments. A high-speed single-element detector and high trigger-rate oscilloscope are used for rapid data acquisition. While this instrument is capable of measuring sub-nanosecond dynamics using standard laser pump/x-ray probe techniques, it also takes advantage of the dense 500 MHz standard fill pattern in the PLS-II storage ring to efficiently record nano-to-micro-second dynamics simultaneously. We demonstrate this capability by measuring both the (fast) impulsive strain and (slower) thermal recovery dynamics of a crystalline InSb sample following intense ultrafast laser excitation. Exploiting the full repetition rate of the storage ring results in a significant improvement in data collection rates compared to conventional bunch-tagging methods.

  16. Thermal and magnetic anomalies of α-iron: an exploration by extended x-ray absorption fine structure spectroscopy and synchrotron x-ray diffraction.

    PubMed

    Boccato, Silvia; Sanson, Andrea; Kantor, Innokenty; Mathon, Olivier; Dyadkin, Vadim; Chernyshov, Dmitry; Carnera, Alberto; Pascarelli, Sakura

    2016-09-07

    The local structure and dynamics of α-iron have been investigated by extended x-ray absorption fine structure (EXAFS) spectroscopy and x-ray diffraction (XRD) in order to shed light on some thermal and magnetic anomalies observed in the last decades. The quantitative EXAFS analysis of the first two coordination shells reveals a peculiar local vibrational dynamics of α-iron: the second neighbor distance exhibits anharmonicity and vibrational anisotropy larger than the first neighbor distance. We search for possible distortions of the bcc structure to justify the unexplained magnetostriction anomalies of α-iron and provide a value for the maximum dislocation of the central Fe atom. No thermal anomalies have been detected from the current XRD data. On the contrary, an intriguing thermal anomaly at about 150 K, ascribed to a stiffening of the Fe-Fe bonds, was found by EXAFS.

  17. Thermal and magnetic anomalies of α-iron: an exploration by extended x-ray absorption fine structure spectroscopy and synchrotron x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Boccato, Silvia; Sanson, Andrea; Kantor, Innokenty; Mathon, Olivier; Dyadkin, Vadim; Chernyshov, Dmitry; Carnera, Alberto; Pascarelli, Sakura

    2016-09-01

    The local structure and dynamics of α-iron have been investigated by extended x-ray absorption fine structure (EXAFS) spectroscopy and x-ray diffraction (XRD) in order to shed light on some thermal and magnetic anomalies observed in the last decades. The quantitative EXAFS analysis of the first two coordination shells reveals a peculiar local vibrational dynamics of α-iron: the second neighbor distance exhibits anharmonicity and vibrational anisotropy larger than the first neighbor distance. We search for possible distortions of the bcc structure to justify the unexplained magnetostriction anomalies of α-iron and provide a value for the maximum dislocation of the central Fe atom. No thermal anomalies have been detected from the current XRD data. On the contrary, an intriguing thermal anomaly at about 150 K, ascribed to a stiffening of the Fe-Fe bonds, was found by EXAFS.

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

    NASA Astrophysics Data System (ADS)

    Blagoev, K.; Grozeva, M.; Malcheva, G.; Neykova, S.

    2013-01-01

    The paper presents the results of the application of laser induced breakdown spectroscopy, X-ray fluorescence spectrometry, and X-ray powder diffraction in assessing the chemical and phase composition of white clay decorative ceramic tiles from the medieval archaeological site of Veliki Preslav, a Bulgarian capital in the period 893-972 AC, well-known for its original ceramic production. Numerous white clay ceramic tiles with highly varied decoration, produced for wall decoration of city's churches and palaces, were found during the archaeological excavations in the old capital. The examination of fourteen ceramic tiles discovered in one of the city's monasteries is aimed at characterization of the chemical profile of the white-clay decorative ceramics produced in Veliki Preslav. Combining different methods and comparing the obtained results provides complementary information regarding the white-clay ceramic production in Veliki Preslav and complete chemical characterization of the examined artefacts.

  19. 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

  20. Electronic Properties of Hydrogen Storage Materials with Photon-in/Photon-out Soft-X-Ray Spectroscopy

    SciTech Connect

    Guo, Jinghua

    2008-09-22

    The applications of resonant soft X-ray emission spectroscopy on a variety of carbon systems have yielded characteristic fingerprints. With high-resolution monochromatized synchrotron radiation excitation, resonant inelastic X-ray scattering has emerged as a new source of information about electronic structure and excitation dynamics. Photon-in/photon-out soft-X-ray spectroscopy is used to study the electronic properties of fundamental materials, nanostructure, and complex hydrides and will offer potential in-depth understanding of chemisorption and/or physisorption mechanisms of hydrogen adsorption/desorption capacity and kinetics.

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

    SciTech Connect

    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, and institutions in France and in the UK, while providing training to undergraduate and graduate students during the experiment. Following this LDRD project, the PI was awarded a 5-year DOE early career research grant to further develop applications of laser-driven x-ray sources for high energy density science experiments and warm dense matter states.

  2. Observation of iron spin-states using tabletop x-ray emission spectroscopy and microcalorimeter sensors

    NASA Astrophysics Data System (ADS)

    Joe, Y. I.; O'Neil, G. C.; Miaja-Avila, L.; Fowler, J. W.; Jimenez, R.; Silverman, K. L.; Swetz, D. S.; Ullom, J. N.

    2016-01-01

    X-ray emission spectroscopy (XES) is a powerful probe of the electronic and chemical state of elemental species embedded within complex compounds. X-ray sensors that combine high resolving power and high collecting efficiency are desirable for photon-starved XES experiments such as measurements of dilute, gaseous, and radiation-sensitive samples, time-resolved measurements, and in-laboratory XES. To assess whether arrays of cryogenic microcalorimeters will be useful in photon-starved XES scenarios, we demonstrate that these emerging energy-dispersive sensors can detect the spin-state of 3d electrons of iron in two different compounds, Fe2O3 and FeS2. The measurements were conducted with a picosecond pulsed laser-driven plasma as the exciting x-ray source. The use of this tabletop source suggests that time-resolved in-laboratory XES will be possible in the future. We also present simulations of {{K}}α and {{K}}β spectra that reveal the spin-state sensitivity of different combinations of sensor resolution and accumulated counts. These simulations predict that our current experimental apparatus can perform time-resolved XES measurements on some samples with a measurement time of a few 10 s of hours per time delay.

  3. 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

  4. 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.

  5. Investigating the speciation of copper in secondary fly ash by X-ray absorption spectroscopy.

    PubMed

    Tian, Shulei; Yu, Meijuan; Wang, Wei; Wang, Qi; Wu, Ziyu

    2009-12-15

    Although some researchers have reported that chlorides may play an important part in the evaporation of copper during heat treatment of municipal solid waste incinerators (MSWI) fly ash (1, 2) , details on the copper speciation in volatile matters (secondary fly ash, SFA) are still lacking. In this work, we used in situ X-ray absorption spectroscopy (XAS) experiments involving three types of SFA, which was collected from a high-temperature tubular electric furnace by thermal treatment of municipal solid waste incinerator (MSWI) fly ash at 1000, 1150, and 1250 degrees C. The results obtained by a linear combination fit (LCF) of X-ray absorption near edge structure (XANES) spectra revealed that in MSWI fly ash copper mainly exists as CuO and CuSO(4).5H(2)O while chloride almost dominated all the content of the SFA conformation, which was more than 80%. Extended X-ray absorption fine structure (EXAFS) data analysis indicated the presence of both Cu-O and Cu-Cl bonds in the first coordination shell of Cu ions in all SFA, while only Cu-O bonds occur in the MSWI fly ash. Consequently, in the MSWI fly ash during heat treatment copper evaporated as chloride, and the latter plays an important role in the formation of copper chloride.

  6. Determining crystal phase purity in c-BP through X-ray absorption spectroscopy.

    PubMed

    Huber, S P; Medvedev, V V; Gullikson, E; Padavala, B; Edgar, J H; van de Kruijs, R W E; Bijkerk, F; Prendergast, D

    2017-02-02

    We employ X-ray absorption near-edge spectroscopy at the boron K-edge and the phosphorus L2,3-edge to study the structural properties of cubic boron phosphide (c-BP) samples. The X-ray absorption spectra are modeled from first-principles within the density functional theory framework using the excited electron core-hole (XCH) approach. A simple structural model of a perfect c-BP crystal accurately reproduces the P L2,3-edge, however it fails to describe the broad and gradual onset of the B K-edge. Simulations of the spectroscopic signatures in boron 1s excitations of intrinsic point defects and the hexagonal BP crystal phase show that these additions to the structural model cannot reproduce the broad pre-edge of the experimental spectrum. Calculated formation enthalpies show that, during the growth of c-BP, it is possible that amorphous boron phases can be grown in conjunction with the desired boron phosphide crystalline phase. In combination with experimental and theoretically obtained X-ray absorption spectra of an amorphous boron structure, which have a similar broad absorption onset in the B K-edge spectrum as the cubic boron phosphide samples, we provide evidence for the presence of amorphous boron clusters in the synthesized c-BP samples.

  7. The Constellation-X Spectroscopy X-ray Telescope: Recent Technology Development

    NASA Technical Reports Server (NTRS)

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

    2006-01-01

    We describe recent progress in the technology development program for the mirror system for the Constellation-X Spectroscopy X-ray Telescope (SXT). Development of this mirror represents a significant technology challenge, as it must provide a combination of large effective area (3 sq. m) and modest angular resolution (15 arc second half power diameter requirement; 5 arc second goal) with a limited mass allocation. The baseline design incorporates over 200 nested Wolter 1 mirrors. Each of these in turn is segmented in order to simplify handling of the mirrors and facilitate mass production. The X-ray reflecting surfaces are fabricated from thin, thermally formed glass sheets. Production improvements have yielded mirror segments that approach the performance requirement without the need for epoxy replication. A mounting and alignment approach incorporating piezoelectric actuators has been shown to manipulate mirror segments with the required precision without introducing significant distortion. Substantial improvements in metrology methodology have provided insights into the mirror segment forming and alignment processes. An X-ray demonstration of a mirror segment pair is planned for early 2006.

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

    PubMed

    Frenkel, Anatoly I; van Bokhoven, Jeroen A

    2014-09-01

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

  9. X-ray Spectroscopy for Chemical and Energy Sciences. the Case of Heterogeneous Catalysis

    SciTech Connect

    Frenkel, A. I.; van Bokhoven, J. A.

    2014-09-01

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

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

    NASA Astrophysics Data System (ADS)

    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.

  11. ODS steel raw material local structure analysis using X-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Cintins, A.; Anspoks, A.; Purans, J.; Kuzmin, A.; Timoshenko, J.; Vladimirov, P.; Gräning, T.; Hoffmann, J.

    2015-03-01

    Oxide dispersion strengthened (ODS) steels are promising materials for fusion power reactors, concentrated solar power plants, jet engines, chemical reactors as well as for hydrogen production from thermolysis of water. In this study we used X-ray absorption spectroscopy at the Fe and Cr K-edges as a tool to get insight into the local structure of ferritic and austenitic ODS steels around Fe and Cr atoms and its transformation during mechanical alloying process. Using the analysis of X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) we found that for austenitic samples a transformation of ferritic steel to austenitic steel is detectable after 10 hours of milling and proceeds till 40 hours of milling; only small amount of a-phase remains after 80 hours of milling. We found that the Cr K-edge EXAFS can be used to observe distortions inside the material and to get an impression on the formation of chromium clusters. In-situ EXAFS experiments offer a reliable method to investigate the ferritic to austenitic transformation.

  12. In Situ Soft X-ray Spectroscopy Characterization of Interfacial Phenomena in Energy Materials and Devices

    NASA Astrophysics Data System (ADS)

    Guo, Jinghua; Liu, Yi-Sheng; Kapilashrami, Mukes; Glans, Per-Anders; Bora, Debajeet; Braun, Artur; Velasco Vélez, Juan Jesús; Salmeron, Miquel; ALS/LBNL Team; EMPA, MSD/LBNL Collaboration

    2015-03-01

    Advanced energy technology arises from the understanding in basic science, thus rest in large on in-situ/operando characterization tools for observing the physical and chemical interfacial processes, which has been largely limited in a framework of thermodynamic and kinetic concepts or atomic and nanoscale. In many important energy systems such as energy conversion, energy storage and catalysis, advanced materials and functionality in devices are based on the complexity of material architecture, chemistry and interactions among constituents within. To understand and thus ultimately control the energy conversion and energy storage applications calls for in-situ/operando characterization tools. Soft X-ray spectroscopy offers a number of very unique features. We will present our development of the in-situ/operando soft X-ray spectroscopic tools of catalytic and electrochemical reactions in recent years, and reveal how to overcome the challenge that soft X-rays cannot easily peek into the high-pressure catalytic cells or liquid electrochemical cells. In this presentation a number of examples are given, including the nanocatalysts and the recent experiment performed for studying the hole generation in a specifically designed photoelectrochemical cell under operando conditions. The ALS is supported by the the U.S. Department of Energy.

  13. Study of a chemically amplified resist for X-ray lithography by Fourier transform infrared spectroscopy.

    PubMed

    Tan, T L; Wong, D; Lee, P; Rawat, R S; Patran, A

    2004-11-01

    Future applications of microelectromechanical systems (MEMS) require lithographic performance of very high aspect ratio. Chemically amplified resists (CARs) such as the negative tone commercial SU-8 provide critical advantages in sensitivity, resolution, and process efficiency in deep ultraviolet, electron-beam, and X-ray lithographies (XRLs), which result in a very high aspect ratio. In this investigation, an SU-8 resist was characterized and optimized for X-ray lithographic applications by studying the cross-linking process of the resist under different conditions of resist thickness and X-ray exposure dose. The exposure dose of soft X-ray (SXR) irradiation at the average weighted wavelength of 1.20 nm from a plasma focus device ranges from 100 to 1600 mJ/cm(2) on the resist surface. Resist thickness varies from 3.5 to 15 mum. The cross-linking process of the resist during post-exposure bake (PEB) was accurately monitored using Fourier transform infrared (FT-IR) spectroscopy. The infrared absorption peaks at 862, 914, 972, and 1128 cm(-1) in the spectrum of the SU-8 resist were found to be useful indicators for the completion of cross-linking in the resist. Results of the experiments showed that the cross-linking of SU-8 was optimized at the exposure dose of 800 mJ/cm(2) for resist thicknesses of 3.5, 9.5, and 15 microm. PEB temperature was set at 95 degrees C and time at 3 min. The resist thickness was measured using interference patterns in the FT-IR spectra of the resist. Test structures with an aspect ratio 3:1 on 10 microm thick SU-8 resist film were obtained using scanning electron microscopy (SEM).

  14. X-ray Spectroscopy of Astrophysical and Laboratory Z-pinch Plasmas

    NASA Astrophysics Data System (ADS)

    Dasgupta, A.; Clark, R. W.; Davis, J.; Giuliani, J. G.

    In recent years, there have been significant advances in instrumental capabilities for making X-ray spectroscopic measurements of astrophysical plasmas. There have been corresponding improvements in X-ray diagnostics for advanced multi-mega-ampere pulse power machines which produce increasingly large radiative yields from gas-puff and wire array Z pinch plasmas. Analysis used for Z pinches can be used to study ICF and also astrophysical plasmas where laboratory measurements and simulations are the only means to interpret observed data. The astrophysical data for Fe, the most cosmically abundant high Z element, can provide a wealth of information about cosmic plasmas. Fe is also the key element in stainless steel (SS) wire arrays that are investigated as an intensive X-ray radiation source at the Z machine in the US Sandia National Laboratories. The implosion dynamics of an array of SS wires on the Z and/or refurbished Z (ZR) accelerator produces an abundance of radiation from the K- and L-shell ionization stages. These dynamic plasmas are inherently non-LTE, with opacity and other factors influencing the X-ray output. As the plasma assembles on axis, a number of time resolved snapshots provide temperature and density profiles and map the emitting region. We will analyze the ionization dynamics and generate K- and L-shell spectra using the conditions generated in the Z and/or ZR, described by a 1-D non-LTE radiation hydrodynamics model. Diagnostics based on spectral shape of L-shell emissions are inherently more difficult than those based on K-shell emissions because of more complex multiplet structures and line overlaps. The non-LTE populations are obtained using detailed atomic models that include all important excitation, ionization, and recombination processes. We will highlight the connection between laboratory Z-pinch plasma simulations and astrophysical plasmas.

  15. Black hole accretion rings revealed by future X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Sochora, V.; Karas, V.; Svoboda, J.; Dovčiak, M.

    2011-11-01

    Spectral features can arise by reflection of coronal X-rays on a black hole accretion disc. The resulting profile bears various imprints of a strong gravitational field acting on the light-emitting gas. The observed shape of the reflection line is formed by integrating contributions over a range of radii across the accretion disc plane, where the individual photons experience a different level of energy shifts, boosting and amplification by relativistic effects. These have to be convolved with the intrinsic emissivity of the line, which is a function of radius and the emission angle in the local frame. We study if the currently discussed instruments on-board X-ray satellites will be able to reveal the departure of the line radial emissivity from a simple smooth power-law function, which is often assumed in data fitting and its interpretation. Such a departure can be a result of excess emission occurring at a certain distance. This could be used to study variations with a radius of the line production or to constrain the position of the inner edge of the accretion disc. By simulating artificial data from a bright active galactic nucleus of a type 1 Seyfert galaxy (inclination ≃30°, X-ray flux ≃1-2 mCrab in a keV energy band) we show that the required sensitivity and energy resolution could be reached with a large area detector of the proposed Large Observatory for X-ray Timing mission. Galactic black holes will provide another category of potentially suitable targets if the relativistic spectral features are indeed produced by reflection from their accretion discs.

  16. Quantitative Determination of Absolute Organohalogen Concentrations in Environmental Samples by X-ray Absorption Spectroscopy

    SciTech Connect

    Leri,A.; Hay, M.; Lanzirotti, A.; Rao, W.; Myneni, S.

    2006-01-01

    An in situ procedure for quantifying total organic and inorganic Cl concentrations in environmental samples based on X-ray absorption near-edge structure (XANES) spectroscopy has been developed. Cl 1s XANES spectra reflect contributions from all Cl species present in a sample, providing a definitive measure of total Cl concentration in chemically heterogeneous samples. Spectral features near the Cl K-absorption edge provide detailed information about the bonding state of Cl, whereas the absolute fluorescence intensity of the spectra is directly proportional to total Cl concentration, allowing for simultaneous determination of Cl speciation and concentration in plant, soil, and natural water samples. Absolute Cl concentrations are obtained from Cl 1s XANES spectra using a series of Cl standards in a matrix of uniform bulk density. With the high sensitivity of synchrotron-based X-ray absorption spectroscopy, Cl concentration can be reliably measured down to the 5-10 ppm range in solid and liquid samples. Referencing the characteristic near-edge features of Cl in various model compounds, we can distinguish between inorganic chloride (Cl{sub inorg}) and organochlorine (Cl{sub org}), as well as between aliphatic Cl{sub org} and aromatic Cl{sub org}, with uncertainties in the range of {approx}6%. In addition, total organic and inorganic Br concentrations in sediment samples are quantified using a combination of Br 1s XANES and X-ray fluorescence (XRF) spectroscopy. Br concentration is detected down to {approx}1 ppm by XRF, and Br 1s XANES spectra allow quantification of the Br{sub inorg} and Br{sub org} fractions. These procedures provide nondestructive, element-specific techniques for quantification of Cl and Br concentrations that preclude extensive sample preparation.

  17. Determination of Yttrium in High Density Silicon Nitride by Emission and X-Ray Fluorescence Spectroscopy.

    DTIC Science & Technology

    1981-08-01

    AD-AI07 596 ARMY MATERIALS AND MECHANICS RESEARCH CENTER WATERTOWN MA F/S 7/4 DETERMINATION OF YTTRIUM IN HIGH DENSITY SILICON NITRIDE BY EMI-ETCIU...AUG Al B H STRAUSS. UNCLASSIFIED AMMRC-TR-Al-39 N AMMRC TR 81-39 A ~LEVEL ’ t’- .- DETERMINATION OF YTTRIUM IN 1 HIGH DENSITY SILICON NITRIDE BY...DETERMINATION OF YTTRIUM IN HIGH DENSITY SILICON NITRIDE BY EMISSION AND X-RAY Final Report FLUORESCENCE SPECTROSCOPY 6 PERFORMING ORG. REPORT NUMBER 7. AUTHOR

  18. The hydration structure of dissolved carbon dioxide from X-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Lam, Royce K.; England, Alice H.; Smith, Jacob W.; Rizzuto, Anthony M.; Shih, Orion; Prendergast, David; Saykally, Richard J.

    2015-07-01

    The dissolution of carbon dioxide in water and its subsequent hydrolysis reactions comprise one of the most central processes in all of science, yet it remains incompletely understood despite enormous effort. We report the detailed characterization of dissolved CO2 gas through the combination of X-ray spectroscopy and first principles theory. The molecule acts as a hydrophobe in water with an average hydrogen bond number of 0.56. The carbon atom interacts weakly with a single water at a distance of >2.67 Å and the carbonyl oxygens serve as weak hydrogen bond acceptors, thus locally enhancing the tetrahedral water hydrogen bonding structure.

  19. Metal release in metallothioneins induced by nitric oxide: X-ray absorption spectroscopy study.

    PubMed

    Casero, Elena; Martín-Gago, José A; Pariente, Félix; Lorenzo, Encarnación

    2004-12-01

    Metallothioneins (MTs) are low molecular weight proteins that include metal ions in thiolate clusters. The capability of metallothioneins to bind different metals has suggested their use as biosensors for different elements. We study here the interaction of nitric oxide with rat liver MTs by using in situ X-ray absorption spectroscopy techniques. We univocally show that the presence of NO induces the release of Zn atoms from the MT structure to the solution. Zn ions transform in the presence of NO from a tetrahedral four-fold coordinated environment in the MT into a regular octahedral six-fold coordinated state, with interatomic distances compatible with those of Zn solvated in water.

  20. Grazing incidence telescopes - A new class for soft X-ray and EUV spectroscopy

    NASA Technical Reports Server (NTRS)

    Hettrick, M. C.; Bowyer, S.

    1984-01-01

    A new class of grazing incidence telescopes is identified, and its advantages for stellar spectroscopy are discussed. In particular, three types of telescope geometry consisting of a primary and a secondary, both at grazing incidence, are proposed. Type I delivers a converging beam having a real focus; type II delivers a diverging beam from a virtual focus, and type III delivers a collimated beam concentrated relative to the primary aperture. The three telescope types are shown to possess unique properties which improve the efficiency and shorten the length of soft X-ray/EUV spectrographs.

  1. Determination of the melting temperature of palladium nanoparticles by X-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Vlasenko, V. G.; Podsukhina, S. S.; Kozinkin, A. V.; Zubavichus, Ya. V.

    2016-02-01

    The anharmonicity parameters of the interatomic potential in ~4-nm palladium nanoparticles deposited on poly(tetra)fluoroethylene microgranules 0.2-0.5 μm in average size were studied by X-ray absorption spectroscopy from an analysis of temperature-dependent EXAFS Pd K edges. The parameters of the interatomic potential obtained were used to calculate melting temperature T melt = 1591 K and Debye temperature ΘD = 257 K of palladium nanoparticles; these temperatures are significantly lower than those in metallic palladium: 277 K and 1825 K, respectively.

  2. FPGA-based compression of streaming x-ray photon correlation spectroscopy data

    SciTech Connect

    Madden, Timothy; Jemian, Peter; Narayanan, Surcsh; Sandy, Alec; Sikorski, Marcin; Sprung, Michael; Weizeorick, John

    2011-08-09

    A data acquisition system to perform real-time background subtraction and lower-level-discrimination-based compression of streaming x-ray photon correlation spectroscopy (XPCS) data from a fast charge-coupled device (CCD) area detector has been built and put into service at the Advanced Photon source (APS) at Argonne National Laboratory. A commercial frame grabber with on-board field-programmable gate array (FPGA) was used in the design, and continuously processes 60 frames per second each consisting of 1,024 x 1,024 pixels with up to 64512 photon hits per frame.

  3. X-Ray Absorption Spectroscopy of Cuprous-Thiolate Clusters in Saccharomyces Cerevisiae Metallothionein

    SciTech Connect

    Zhang, L.; Pickering, I.J.; Winge, D.R.; George, G.N.

    2009-05-28

    Copper (Cu) metallothioneins are cuprous-thiolate proteins that contain multimetallic clusters, and are thought to have dual functions of Cu storage and Cu detoxification. We have used a combination of X-ray absorption spectroscopy (XAS) and density-functional theory (DFT) to investigate the nature of Cu binding to Saccharomyces cerevisiae metallothionein. We found that the XAS of metallothionein prepared, containing a full complement of Cu, was quantitatively consistent with the crystal structure, and that reconstitution of the apo-metallothionein with stoichiometric Cu results in the formation of a tetracopper cluster, indicating cooperative binding of the Cu ions by the metallothionein.

  4. 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.

  5. X-ray photoelectron spectroscopy investigation on electrochemical degradation of proton exchange membrane fuel cell electrodes

    NASA Astrophysics Data System (ADS)

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

    2015-05-01

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

  6. X-ray photoelectron spectroscopy study of the effects of ultrapure water on GaAs

    NASA Astrophysics Data System (ADS)

    Massies, J.; Contour, J. P.

    1985-06-01

    X-ray photoelectron spectroscopy has been used to investigate the effects of de-ionized water on chemical etched GaAs surfaces. When the treatment with water is performed in static conditions (stagnant water) a Ga-rich oxide layer is formed on GaAs at the rate of 10-20 Å h-1. In contrast, when the GaAs surface is treated in dynamic conditions (running water), no oxide buildup is observed. Moreover, running water can remove the oxide film formed in static conditions, as well as oxidized layers due to air exposure. These results are discussed in the framework of cleaning prior to molecular beam epitaxy.

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

    ScienceCinema

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

    2016-07-12

    The capabilities of the Chandra X-ray Observatory and XMM-Newton for high-resolution spectroscopy have brought tradition plasma diagnostic techniques to the study of cosmic plasma. Observations have probed nearly every class of astronomical object, from young proto-starts through massive O starts and black hole binaries, supernova remnants, active galactic nuclei, and the intergalactic medium. Many of these sources show remarkable rich spectra that reveal new physical information, such as emission measure distributions, elemental abundances, accretion disk and wind signatures, and time variability. This talk will present an overview of the Chandra instrumentaton and selected examples of spectral observations of astrophysical and cosmological importance.

  8. X-ray-line polarization spectroscopy in laser-produced plasmas

    SciTech Connect

    Kieffer, J.C.; Matte, J.P.; Chaker, M.; Beaudoin, Y. ); Chien, C.Y.; Coe, S.; Mourou, G. ); Dubau, J. ); Inal, M.K. )

    1993-12-01

    In this work, we show that x-ray-line polarization spectroscopy can be a powerful diagnostic to study laser-produced plasmas. Kinetic calculations are compared to experiments designed to probe the low-density plasma region (with a 1-ps laser pulse) and the overdense plasma (with a 400-fs laser pulse). We observe the transition from a pancakelike'' electron distribution function at low density to a beamlike'' electron distribution function in the overdense plasma. The results are in agreement with the calculations which indicate non-Maxwellian behavior and strong anisotropy due to nonlocal electron heat flow.

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

    SciTech Connect

    Hernández, Rebeca E-mail: aurora.nogales@csic.es; Mijangos, Carmen; Nogales, Aurora E-mail: aurora.nogales@csic.es; Ezquerra, Tiberio A.; Sprung, Michael

    2014-01-14

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

  10. An x-ray absorption spectroscopy study of Cd binding onto a halophilic archaeon

    NASA Astrophysics Data System (ADS)

    Showalter, Allison R.; Szymanowski, Jennifer E. S.; Fein, Jeremy B.; Bunker, Bruce A.

    2016-05-01

    X-ray absorption spectroscopy (XAS) and cadmium (Cd) isotherm experiments determine how Cd adsorbs to the surface of halophilic archaeon Halobacterium noricense. This archaeon, isolated from the Waste Isolation Pilot Plant (WIPP) near Carlsbad, New Mexico could be involved with the transport of toxic metals stored in the transuranic waste in the salt mine. The isotherm experiments show that adsorption is relatively constant across the tolerable pH range for H. noricense. The XAS results indicate that Cd adsorption occurs predominately via a sulfur site, most likely sulfhydryl, with the same site dominating all measured pH values.

  11. Excited-state molecular structures captured by X-ray transient absorption spectroscopy: a decade and beyond.

    PubMed

    Chen, Lin X; Zhang, Xiaoyi; Lockard, Jenny V; Stickrath, Andrew B; Attenkofer, Klaus; Jennings, Guy; Liu, Di-Jia

    2010-03-01

    Transient molecular structures along chemical reaction pathways are important for predicting molecular reactivity, understanding reaction mechanisms, as well as controlling reaction pathways. During the past decade, X-ray transient absorption spectroscopy (XTA, or LITR-XAS, laser-initiated X-ray absorption spectroscopy), analogous to the commonly used optical transient absorption spectroscopy, has been developed. XTA uses a laser pulse to trigger a fundamental chemical process, and an X-ray pulse(s) to probe transient structures as a function of the time delay between the pump and probe pulses. Using X-ray pulses with high photon flux from synchrotron sources, transient electronic and molecular structures of metal complexes have been studied in disordered media from homogeneous solutions to heterogeneous solution-solid interfaces. Several examples from the studies at the Advanced Photon Source in Argonne National Laboratory are summarized, including excited-state metalloporphyrins, metal-to-ligand charge transfer (MLCT) states of transition metal complexes, and charge transfer states of metal complexes at the interface with semiconductor nanoparticles. Recent developments of the method are briefly described followed by a future prospective of XTA. It is envisioned that concurrent developments in X-ray free-electron lasers and synchrotron X-ray facilities as well as other table-top laser-driven femtosecond X-ray sources will make many breakthroughs and realise dreams of visualizing molecular movies and snapshots, which ultimately enable chemical reaction pathways to be controlled.

  12. Excited-state molecular structures captured by x-ray transient absorption spectroscopy : a decade and beyond.

    SciTech Connect

    Chen, L. X.; Zhang, X.; Lockard, J. V.; Stickrath, A. B.; Attenkofer, K.; Jennings, G.; Liu, D.-J.; Northwestern Univ.

    2010-03-02

    Transient molecular structures along chemical reaction pathways are important for predicting molecular reactivity, understanding reaction mechanisms, as well as controlling reaction pathways. During the past decade, X-ray transient absorption spectroscopy (XTA, or LITR-XAS, laser-initiated X-ray absorption spectroscopy), analogous to the commonly used optical transient absorption spectroscopy, has been developed. XTA uses a laser pulse to trigger a fundamental chemical process, and an X-ray pulse(s) to probe transient structures as a function of the time delay between the pump and probe pulses. Using X-ray pulses with high photon flux from synchrotron sources, transient electronic and molecular structures of metal complexes have been studied in disordered media from homogeneous solutions to heterogeneous solution-solid interfaces. Several examples from the studies at the Advanced Photon Source in Argonne National Laboratory are summarized, including excited-state metalloporphyrins, metal-to-ligand charge transfer (MLCT) states of transition metal complexes, and charge transfer states of metal complexes at the interface with semiconductor nanoparticles. Recent developments of the method are briefly described followed by a future prospective of XTA. It is envisioned that concurrent developments in X-ray free-electron lasers and synchrotron X-ray facilities as well as other table-top laser-driven femtosecond X-ray sources will make many breakthroughs and realise dreams of visualizing molecular movies and snapshots, which ultimately enable chemical reaction pathways to be controlled.

  13. Deep spectroscopy of stellar counterparts of ultraluminous X-ray sources

    NASA Astrophysics Data System (ADS)

    Ueda, Yoshihiro

    2011-01-01

    We propose to carry out a deep spectral study of faint stars in X-ray boxes of four ultraluminous X-ray sources (ULXs) in nearby galaxies. They are the most luminous bone-fide ULXs, whose stellar counterparts have unambiguous identification. They were well-studied in the HST and ground-based imaging. Our analysis of archival Subaru spectra (2 out of the 4 targets) has shown that the spectra were taken with inadmissible short exposures resulting in too low S/N, and the spectral range did not include main diagnostical spectral features. All previous studies of the ULXs did not answer the question on their nature. It is astonishing that there was no spectroscopy of their optical counterparts, though it is possible to take good spectra of them in a long-exposure spectroscopy with 8-m class of telescopes. The predictions for the ULX optical counterpart spectrum are clear enough to distinguish between two the most popular models (supercritical accretion disks like that in SS 433 and intermediate-mass black holes with a "normal disk"). The main goal is to distinguish an accretion regime in ULXs, because in both cases the ULXs must be close binaries with a massive donor. This spectroscopy is the necessary first step for subsequent phase-resolved spectroscopic studies to determine the black hole mass.

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

    NASA Astrophysics Data System (ADS)

    Neppl, Stefan

    2015-05-01

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

  15. Development of time resolved x-ray spectroscopy in high intensity laser-plasma interactions

    SciTech Connect

    Notley, M. M.; Weber, R. L.; Fell, B.; Jeffries, J.; Freeman, R. R.; Mackinnon, A. J.; Dickson, R.; Hey, D.; Khattak, F.; Saiz, E. Garcia; Gregori, G.

    2006-10-15

    This article discusses the design of a novel time resolved von Hamos Bragg spectrometer to provide spectra in the region around the titanium K-{alpha} and He-{alpha} lines. The instrument consists of a highly oriented pyrolitic graphite mosaic crystal coupled to a picosecond x-ray streak camera. Measurements of the time dependent behavior from Ti foils illuminated with intense laser pulses can be used to improve the understanding of recombination dynamics, electron transport, and phase transitions in strongly coupled dense plasma. This is important for the modeling of the compression phase in inertial confinement fusion research and the study of astrophysical environments.

  16. X-ray spectroscopy of high temperature plasma in solar flares

    NASA Astrophysics Data System (ADS)

    Culhane, J. L.

    X-ray spectroscopic observations with high wavelength resolution provide information on plasma density, temperature, and emission, together with bulk and turbulent velocity data for the hot plasma. Observations carried out during the 1980 solar maximum with spectrometers on the SMM, P78-1, and Hinotori spacecraft are examined with emphasis on the advances made possible by these missions. During the next solar maximum, flare studies with particular emphasis on the impulsive phase will be undertaken by the Japanese Solar-A mission. Those instruments is designed to study the hot plasma are described, and their proposed role in clarifying the nature of the impulsive phase is discussed.

  17. Electronic structure of individual hybrid colloid particles studied by near-edge X-ray absorption fine structure (NEXAFS) spectroscopy in the X-ray microscope.

    PubMed

    Henzler, Katja; Guttmann, Peter; Lu, Yan; Polzer, Frank; Schneider, Gerd; Ballauff, Matthias

    2013-02-13

    The electronic structure of individual hybrid particles was studied by nanoscale near-edge X-ray absorption spectromicroscopy. The colloidal particles consist of a solid polystyrene core and a cross-linked poly-N-(isopropylacrylamide) shell with embedded crystalline titanium dioxide (TiO(2)) nanoparticles (d = 6 ± 3 nm). The TiO(2) particles are generated in the carrier network by a sol-gel process at room temperature. The hybrid particles were imaged with photon energy steps of 0.1 eV in their hydrated environment with a cryo transmission X-ray microscope (TXM) at the Ti L(2,3)-edge. By analyzing the image stacks, the obtained near-edge X-ray absorption fine structure (NEXAFS) spectra of our individual hybrid particles show clearly that our synthesis generates TiO(2) in the anastase phase. Additionally, our spectromicroscopy method permits the determination of the density distribution of TiO(2) in single carrier particles. Therefore, NEXAFS spectroscopy combined with TXM presents a unique method to get in-depth insight into the electronic structure of hybrid materials.

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

    PubMed

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

    2015-06-07

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

  19. X-ray magnetic circular dichroism and x-ray absorption spectroscopy of novel magnetic thin films

    SciTech Connect

    Brewer, M.A.; Ju, H.L.; Krishnan, K.M.

    1997-04-01

    The optimization of the magnetic properties of materials for a wide range of applications requires a dynamic iteration between synthesis, property measurements and characterization at appropriate length scales. The authors interest arises both from the increased appreciation of the degree to which magnetic properties can be influenced by tailored microstructures and the ability to characterize them by x-ray scattering/dichroism techniques. Preliminary results of this work at the ALS on `giant` moment in {alpha}{double_prime}-Fe{sub 16}N{sub 2} and `colossal` magnetoresistance in manganite perovskites is presented here. It has recently been claimed that {alpha}{double_prime}-Fe{sub 16}N{sub 2} possesses a giant magnetization of 2.9 T ({approximately}2300 emu/cc) when grown on lattice-matched In{sub 0.2}Ga{sub 0.8}As(001) and Fe/GaAs(001). However, attempts at growth on simpler substrates have resulted in only a modest enhancement in moment and often in multiphase mixtures. Theoretical calculations based on the band structure of Fe{sub 16}N{sub 2} predict values for the magnetization around 2.3 T ({approximately}1780 emu/cc), well below Sugita`s claims, but consistent with the magnetization reported by several other workers. Using appropriate sum rules applied to the integrated MCD spectrum, they hope to determine the magnetic moment of the iron species in the {alpha}{double_prime}-Fe{sub 16}N{sub 2} films and other phases and resolve the orbital and spin contributions to the moment. There is also rapidly growing interest in the `colossal magnetoresistance` effect observed in manganese oxides for both fundamental and commercial applications. To address some of these issues the authors have measured the electron energy loss spectra (EELS) of manganese perovskites at room temperature.

  20. A new nondestructive instrument for bulk residual stress measurement using tungsten kα1 X-ray

    NASA Astrophysics Data System (ADS)

    Ma, Ce; Dou, Zuo-yong; Chen, Li; Li, Yun; Tan, Xiao; Dong, Ping; Zhang, Jin; Zheng, Lin; Zhang, Peng-cheng

    2016-11-01

    We describe an experimental instrument used for measuring nondestructively the residual stress using short wavelength X-ray, tungsten kα1. By introducing a photon energy screening technology, the monochromatic X-ray diffraction of tungsten kα1 was realized using a CdTe detector. A high precision Huber goniometer is utilized in order to reduce the error in residual stress measurement. This paper summarizes the main performance of this instrument, measurement depth, stress error, as opposed to the neutron diffraction measurements of residual stress. Here, we demonstrate an application on the determination of residual stress in an aluminum alloy welded by the friction stir welding.

  1. A new nondestructive instrument for bulk residual stress measurement using tungsten kα1 X-ray.

    PubMed

    Ma, Ce; Dou, Zuo-Yong; Chen, Li; Li, Yun; Tan, Xiao; Dong, Ping; Zhang, Jin; Zheng, Lin; Zhang, Peng-Cheng

    2016-11-01

    We describe an experimental instrument used for measuring nondestructively the residual stress using short wavelength X-ray, tungsten kα1. By introducing a photon energy screening technology, the monochromatic X-ray diffraction of tungsten kα1 was realized using a CdTe detector. A high precision Huber goniometer is utilized in order to reduce the error in residual stress measurement. This paper summarizes the main performance of this instrument, measurement depth, stress error, as opposed to the neutron diffraction measurements of residual stress. Here, we demonstrate an application on the determination of residual stress in an aluminum alloy welded by the friction stir welding.

  2. AN X-RAY STUDY OF THE ETHYLENE GLYCOLMONTMORILLONITE COMPLEX.

    DTIC Science & Technology

    SOILS, * MONTMORILLONITE , *GLYCOLS, *X RAY SPECTROSCOPY, X RAY SPECTRA, X RAY SPECTRA, X RAY SPECTRA, CLAY MINERALS, COMPLEX COMPOUNDS, FOURIER ANALYSIS, CRYSTAL STRUCTURE, THERMAL PROPERTIES, MATHEMATICAL MODELS.

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

    NASA Astrophysics Data System (ADS)

    Kawaguchi, Tomoya; Fukuda, Katsutoshi; Matsubara, Eiichiro

    2017-03-01

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

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

    PubMed

    Kawaguchi, Tomoya; Fukuda, Katsutoshi; Matsubara, Eiichiro

    2017-03-22

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

  5. A liquid flatjet system for solution phase soft-x-ray spectroscopy

    PubMed Central

    Ekimova, Maria; Quevedo, Wilson; Faubel, Manfred; Wernet, Philippe; Nibbering, Erik T. J.

    2015-01-01

    We present a liquid flatjet system for solution phase soft-x-ray spectroscopy. The flatjet set-up utilises the phenomenon of formation of stable liquid sheets upon collision of two identical laminar jets. Colliding the two single water jets, coming out of the nozzles with 50 μm orifices, under an impact angle of 48° leads to double sheet formation, of which the first sheet is 4.6 mm long and 1.0 mm wide. The liquid flatjet operates fully functional under vacuum conditions (<10−3 mbar), allowing soft-x-ray spectroscopy of aqueous solutions in transmission mode. We analyse the liquid water flatjet thickness under atmospheric pressure using interferomeric or mid-infrared transmission measurements and under vacuum conditions by measuring the absorbance of the O K-edge of water in transmission, and comparing our results with previously published data obtained with standing cells with Si3N4 membrane windows. The thickness of the first liquid sheet is found to vary between 1.4–3 μm, depending on the transverse and longitudinal position in the liquid sheet. We observe that the derived thickness is of similar magnitude under 1 bar and under vacuum conditions. A catcher unit facilitates the recycling of the solutions, allowing measurements on small sample volumes (∼10 ml). We demonstrate the applicability of this approach by presenting measurements on the N K-edge of aqueous NH4+. Our results suggest the high potential of using liquid flatjets in steady-state and time-resolved studies in the soft-x-ray regime. PMID:26798824

  6. Ultraprecision motion control technique for high-resolution x-ray instrumentation

    SciTech Connect

    Shu, D.; Toellner, T. S.; Alp, E. E.

    2000-07-17

    With the availability of third-generation hard x-ray synchrotron radiation sources, such as the Advanced Photon Source (APS) at Argonne National Laboratory, x-ray inelastic scattering and x-ray nuclear resonant scattering provide powerful means for investigating the vibrational dynamics of a variety of materials and condensed matter systems. Novel high-resolution hard x-ray optics with meV energy resolution requires a compact positioning mechanism with 20--50-nrad angular resolution and stability. In this paper, the authors technical approach to this design challenge is presented. Sensitivity and stability test results are also discussed.

  7. Near-Edge X-ray Absorption Fine Structure Spectroscopy of Diamondoid Thiol Monolayers on Gold

    SciTech Connect

    Willey, T M; Fabbri, J; Lee, J I; Schreiner, P; Fokin, A A; Tkachenko, B A; Fokina, N A; Dahl, J; Carlson, B; Vance, A L; Yang, W; Terminello, L J; van Buuren, T; Melosh, N

    2007-11-27

    Diamondoids, hydrocarbon molecules with cubic-diamond-cage structures, have unique properties with potential value for nanotechnology. The availability and ability to selectively functionalize this special class of nanodiamond materials opens new possibilities for surface-modification, for high-efficiency field emitters in molecular electronics, as seed crystals for diamond growth, or as robust mechanical coatings. The properties of self-assembled monolayers (SAMs) of diamondoids are thus of fundamental interest for a variety of emerging applications. This paper presents the effects of thiol substitution position and polymantane order on diamondoid SAMs on gold using near-edge X-ray absorption fine structure spectroscopy (NEXAFS) and X-ray photoelectron spectroscopy (XPS). A framework to determine both molecular tilt and twist through NEXAFS is presented and reveals highly ordered diamondoid SAMs, with the molecular orientation controlled by the thiol location. C 1s and S 2p binding energies are lower in adamantane thiol than alkane thiols on gold by 0.67 {+-} 0.05 eV and 0.16 {+-} 0.04 eV respectively. These binding energies vary with diamondoid monolayer structure and thiol substitution position, consistent with different amounts of steric strain and electronic interaction with the substrate. This work demonstrates control over the assembly, in particular the orientational and electronic structure, providing a flexible design of surface properties with this exciting new class of diamond clusters.

  8. Evolution of silver nanoparticles in the rat lung investigated by X-ray absorption spectroscopy

    SciTech Connect

    Davidson, R. Andrew; Anderson, Donald S.; Van Winkle, Laura S.; Pinkerton, Kent E.; Guo, T.

    2014-12-16

    Following a 6-h inhalation exposure to aerosolized 20 and 110 nm diameter silver nanoparticles, lung tissues from rats were investigated with X-ray absorption spectroscopy, which can identify the chemical state of silver species. Lung tissues were processed immediately after sacrifice of the animals at 0, 1, 3, and 7 days post exposure and the samples were stored in an inert and low-temperature environment until measured. We found that it is critical to follow a proper processing, storage and measurement protocol; otherwise only silver oxides are detected after inhalation even for the larger nanoparticles. The results of X-ray absorption spectroscopy measurements taken in air at 85 K suggest that the dominating silver species in all the postexposure lung tissues were metallic silver, not silver oxide, or solvated silver cations. The results further indicate that the silver nanoparticles in the tissues were transformed from the original nanoparticles to other forms of metallic silver nanomaterials and the rate of this transformation depended on the size of the original nanoparticles. Furthermore, we found that 20 nm diameter silver nanoparticles were significantly modified after aerosolization and 6-h inhalation/deposition, whereas larger, 110 nm diameter nanoparticles were largely unchanged. Over the seven-day postexposure period the smaller 20 nm silver nanoparticles underwent less change in the lung tissue than the larger 110 nm silver nanoparticles. In contrast, silica-coated gold nanoparticles did not undergo any modification processes and remained as the initial nanoparticles throughout the 7-day study period.

  9. X-ray absorption spectroscopy (XAS) of toxic metal mineral transformations by fungi.

    PubMed

    Fomina, Marina; Charnock, John; Bowen, Andrew D; Gadd, Geoffrey M

    2007-02-01

    Fungi can be highly efficient biogeochemical agents and accumulators of soluble and particulate forms of metals. This work aims to understand some of the physico-chemical mechanisms involved in toxic metal transformations focusing on the speciation of metals accumulated by fungi and mycorrhizal associations. The amorphous state or poor crystallinity of metal complexes within biomass and relatively low metal concentrations make the determination of metal speciation in biological systems a challenging problem but this can be overcome by using synchrotron-based element-specific X-ray absorption spectroscopy (XAS) techniques. In this research, we have exposed fungi and ectomycorrhizas to a variety of copper-, zinc- and lead-containing minerals. X-ray absorption spectroscopy studies revealed that oxygen ligands (phosphate, carboxylate) played a major role in toxic metal coordination within the fungal and ectomycorrhizal biomass during the accumulation of mobilized toxic metals. Coordination of toxic metals within biomass depended on the fungal species, initial mineral composition, the nitrogen source, and the physiological state/age of the fungal mycelium.

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

    PubMed

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

    2016-11-05

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

  11. Soft X-Ray Spectroscopy of Glycyl-Glycine Adsorbed on Cu(110) Surface

    NASA Astrophysics Data System (ADS)

    Feyer, V.; Plekan, O.; Lyamayev, V.; Skala, T.; Prince, K. C.; Chab, V.; Tsud, N.; Matolin, V.; Carravetta, V.

    2010-06-01

    Studies of the interaction between organic compounds and surfaces are motivated by their application as bio sensors, and their relevance to biocompatibility of implants and the origin of life. In the present work interaction of the simplest peptide, glycyl-glycine, with the Cu surface has been studied. Multilayer, monolayer and sub-monolayer films of this dipeptide on the clean and oxygen modified Cu(110) surface were prepared by thermal evaporation in high vacuum. The techniques used were soft X-ray photoelectron spectroscopy, near edge X-ray absorption fine structure spectroscopy and density functional theory calculations. By comparing the experimental and theoretical spectra, detailed models of the electronic structure and adsorption geometry for each coverage have been proposed, which are in good agreement with the theoretical calculations. The carboxylic acid group of glycyl-glycine loses hydrogen and the molecule is coordinated via the carboxylate oxygen atoms to the surface. At low coverage the amino group bonds to the surface via a hydrogen atom, while at higher coverage the bonding is via the nitrogen lone pair. The peptide group is not involved in the bonding to the surface.

  12. Adsorption of mercury on lignin: combined surface complexation modeling and X-ray absorption spectroscopy studies.

    PubMed

    Lv, Jitao; Luo, Lei; Zhang, Jing; Christie, Peter; Zhang, Shuzhen

    2012-03-01

    Adsorption of mercury (Hg) on lignin was studied at a range of pH values using a combination of batch adsorption experiments, a surface complexation model (SCM) and synchrotron X-ray absorption spectroscopy (XAS). Surface complexation modeling indicates that three types of acid sites on lignin surfaces, namely aliphatic carboxylic-, aromatic carboxylic- and phenolic-type surface groups, contributed to Hg(II) adsorption. The bond distance and coordination number of Hg(II) adsorption samples at pH 3.0, 4.0 and 5.5 were obtained from extended X-ray absorption fine structure (EXAFS) spectroscopy analysis. The results of SCM and XAS combined reveal that the predominant adsorption species of Hg(II) on lignin changes from HgCl(2)(0) to monodentate complex -C-O-HgCl and then bidentate complex -C-O-Hg-O-C- with increasing pH value from 2.0 to 6.0. The good agreement between SCM and XAS results provides new insight into understanding the mechanisms of Hg(II) adsorption on lignin.

  13. Evolution of Silver Nanoparticles in the Rat Lung Investigated by X-ray Absorption Spectroscopy

    PubMed Central

    2015-01-01

    Following a 6-h inhalation exposure to aerosolized 20 and 110 nm diameter silver nanoparticles, lung tissues from rats were investigated with X-ray absorption spectroscopy, which can identify the chemical state of silver species. Lung tissues were processed immediately after sacrifice of the animals at 0, 1, 3, and 7 days post exposure and the samples were stored in an inert and low-temperature environment until measured. We found that it is critical to follow a proper processing, storage and measurement protocol; otherwise only silver oxides are detected after inhalation even for the larger nanoparticles. The results of X-ray absorption spectroscopy measurements taken in air at 85 K suggest that the dominating silver species in all the postexposure lung tissues were metallic silver, not silver oxide, or solvated silver cations. The results further indicate that the silver nanoparticles in the tissues were transformed from the original nanoparticles to other forms of metallic silver nanomaterials and the rate of this transformation depended on the size of the original nanoparticles. We found that 20 nm diameter silver nanoparticles were significantly modified after aerosolization and 6-h inhalation/deposition, whereas larger, 110 nm diameter nanoparticles were largely unchanged. Over the seven-day postexposure period the smaller 20 nm silver nanoparticles underwent less change in the lung tissue than the larger 110 nm silver nanoparticles. In contrast, silica-coated gold nanoparticles did not undergo any modification processes and remained as the initial nanoparticles throughout the 7-day study period. PMID:25517690

  14. 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.

  15. X-ray photoelectron spectroscopy characterization of the {omega} phase in water quenched Ti-5553 alloy

    SciTech Connect

    Qin, Dongyang; Lu, Yafeng; Zhang, Kong; Liu, Qian; Zhou, Lian

    2012-11-15

    X-ray photoelectron spectroscopy was used to investigate the {omega} phase in water quenched Ti-5553 alloy with a nominal composition of Ti-5Al-5V-5Mo-3Cr (wt.%), and the {omega} and the {beta} phase were distinguished by deconvoluting the XPS spectra of Al2p, V2p and Cr2p core level regions. In addition, it is found that the binding energy of core level electron of alloying elements shifts comparing with that of pure metals, and the fact was interpreted by charge redistribution model. X-ray photoelectron spectroscopy technique could be used to characterize the nano-scale {omega} phase in {beta} alloys. - Highlights: Black-Right-Pointing-Pointer We characterize the {omega} phase in Ti-5553 alloy by XPS. Black-Right-Pointing-Pointer Binding energy of Al2p, V2p and Cr2p electron are different in the {omega} and {beta} phase. Black-Right-Pointing-Pointer Structural difference leads to the binding energy gap.

  16. 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.

  17. Time Resolved Spectroscopy, High Sensitivity Power Spectrum & a Search for the X-Ray QPO in NGC 5548

    NASA Astrophysics Data System (ADS)

    Yaqoob, Tahir

    1999-09-01

    Controversy surrounds the EXOSAT discovery of a QPO (period ~500 s) in NGC 5548 due to the data being plagued by high background and instrumental systematics. If the NGC 5548 QPO is real, the implications for the physics of the X-ray emission mechanism and inner-most disk/black-hole system are enormous. AXAF provides the first opportunity to settle the issue, capable of yielding power spectra with unprecedented sensitivity, pushing the limit on finding new features. Using HETG/ACIS we will also perform time-resolved spectroscopy of the ionized absorption features and Fe-K emission line, search for energy-dependent time lags in the continuum, between the continuum and spectral features, and between the spectral features. These data will provide powerful constraints on models of AGN.

  18. Measurement of c-axis angular orientation in calcite (CaCO3) nanocrystals using X-ray absorption spectroscopy

    PubMed Central

    Gilbert, P. U. P. A.; Young, Anthony; Coppersmith, Susan N.

    2011-01-01

    We demonstrate that the ability to manipulate the polarization of synchrotron radiation can be exploited to enhance the capabilities of X-ray absorption near-edge structure (XANES) spectroscopy, to include linear dichroism effects. By acquiring spectra at the same photon energies but different polarizations, and using a photoelectron emission spectromicroscope (PEEM), one can quantitatively determine the angular orientation of micro- and nanocrystals with a spatial resolution down to 10 nm. XANES-PEEM instruments are already present at most synchrotrons, hence these methods are readily available. The methods are demonstrated here on geologic calcite (CaCO3) and used to investigate the prismatic layer of a mollusk shell, Pinctada fucata. These XANES-PEEM data reveal multiply oriented nanocrystals within calcite prisms, previously thought to be monocrystalline. The subdivision into multiply oriented nanocrystals, spread by more than 50°, may explain the excellent mechanical properties of the prismatic layer, known for decades but never explained. PMID:21693647

  19. First results from the high-brightness x-ray spectroscopy beamline 9. 3.1 at ALS

    SciTech Connect

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

    1995-10-01

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

  20. Core and valence excitations in resonant X-ray spectroscopy using restricted excitation window time-dependent density functional theory

    PubMed Central

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

    2012-01-01

    We report simulations of X-ray absorption near edge structure (XANES), resonant inelastic X-ray scattering (RIXS) and 1D stimulated X-ray Raman spectroscopy (SXRS) signals of cysteine at the oxygen, nitrogen, and sulfur K and \\documentclass[12pt]{minimal}\\begin{document}$\\textrm {L}_{2,3}$\\end{document}L2,3 edges. Comparison of the simulated XANES signals with experiment shows that the restricted window time-dependent density functional theory is more accurate and computationally less expensive than the static exchange method. Simulated RIXS and 1D SXRS signals give some insights into the correlation of different excitations in the molecule. PMID:23181305

  1. Development of intelligent control system for X-ray streak camera in diagnostic instrument manipulator

    NASA Astrophysics Data System (ADS)

    Pei, Chengquan; Wu, Shengli; Tian, Jinshou; Liu, Zhen; Fang, Yuman; Gao, Guilong; Liang, Lingliang; Wen, Wenlong

    2015-11-01

    An intelligent control system for an X ray streak camera in a diagnostic instrument manipulator (DIM) is proposed and implemented, which can control time delay, electric focusing, image gain adjustment, switch of sweep voltage, acquiring environment parameters etc. The system consists of 16 A/D converters and 16 D/A converters, a 32-channel general purpose input/output (GPIO) and two sensors. An isolated DC/DC converter with multi-outputs and a single mode fiber were adopted to reduce the interference generated by the common ground among the A/D, D/A and I/O. The software was designed using graphical programming language and can remotely access the corresponding instrument from a website. The entire intelligent control system can acquire the desirable data at a speed of 30 Mb/s and store it for later analysis. The intelligent system was implemented on a streak camera in a DIM and it shows a temporal resolution of 11.25 ps, spatial distortion of less than 10% and dynamic range of 279:1. The intelligent control system has been successfully used in a streak camera to verify the synchronization of multi-channel laser on the Inertial Confinement Fusion Facility.

  2. Atmospheric Electron-induced X-Ray Spectrometer (AEXS) Instrument Development

    NASA Technical Reports Server (NTRS)

    Urgiles, E.; Wilcox, J. Z.; Toda, R.; Crisp, J.; George, T.

    2005-01-01

    Introduction: This paper describes the progress in data acquisition and establishing the observational capability of the AEXS instrument. The AEXS is a miniature instrument[1-4] based on the excitation of characteristic X-Ray Fluorescence (XRF) and luminescence spectra using a focused electron beam which enables nondestructive evaluation of sample surfaces in planetary ambient atmospheres. In situ operation is obtained through the use of a thin electron transmissive membrane to isolate the vacuum of the AEXS source from the outside ambient atmosphere. Thus eliminating the need for a vacuum pumped sample chamber as is common in all laboratory SEM s. The transmitted electrons impinge on the sample exciting XRF spectra from the irradiated spot on in-situ or collected samples with sub-mm to cm-scale spatial resolution at Mars atmospheric pressure. The AEXS system (Fig 1) consists of a high-energy (>10keV) electron gun encapsulated by the isolation membrane, an XRF detection and analyzer system, and a high voltage power supply. The XRF data are analyzed to determine the elemental abundance for the irradiated spots. The approach to demonstrating a proof of concept of the AEXS has been through 1) demonstrating the viability of microfabricated membranes, 2) assembling AEXS setups with increasingly integrated functional components, and 3) simulating the AEXS observational capabilities. The development of the instrument is described in detail in the poster paper[4] at this conference. This paper focuses on describing the progress of the AEXS instrument to acquire XRF data and using commercially available software to analyze the data streams and determine the accuracy, precision and resolution of the analysis compared to the certified elemental abundance.

  3. 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. Uses of Auger and x ray photoelectron spectroscopy in the study of adhesion and friction

    NASA Technical Reports Server (NTRS)

    Miyoshi, Kazuhisa

    1990-01-01

    Three studies are described characterizing the possible contributions of surface science to tribology. These include surface contamination formed by the interaction of a surface with the environment, contaminants obtained with diffusion of compounds, and surface chemical changes resulting from selective thermal evaporation. Surface analytical tools such as Auger electron spectroscopy (AES) and x ray photoelectron spectroscopy (XPS) incorporated directly into adhesion and friction systems are primarily used to define the nature of tribological surfaces before and after tribological experimentation and to characterize the mechanism of solid-to-solid interaction. Emphasis is on fundamental studies involving the role of surfaces in controlling the adhesion and friction properties of materials emerging as a result of the surface analyses. The materials which were studied include metals and ceramics such as elemental metals, amorphous alloys (metallic glasses), and silicon-based ceramics.

  5. In situ Raman and X-ray spectroscopies to monitor microbial activities under high hydrostatic pressure.

    PubMed

    Oger, Phil M; Daniel, Isabelle; Picard, Aude

    2010-02-01

    Until recently, monitoring of cells and cellular activities at high hydrostatic pressure (HHP) was mainly limited to ex situ observations. Samples were analyzed prior to and following the depressurization step to evaluate the effect of the pressure treatment. Such ex situ measurements have several drawbacks: (i) it does not allow for kinetic measurements and (ii) the depressurization step often leads to artifactual measurements. Here, we describe recent advances in diamond anvil cell (DAC) technology to adapt it to the monitoring of microbial processes in situ. The modified DAC is asymmetrical, with a single anvil and a diamond window to improve imaging quality and signal collection. Using this novel DAC combined to Raman and X-ray spectroscopy, we monitored the metabolism of glucose by baker's yeast and the reduction of selenite by Agrobacterium tumefaciens in situ under HHP. In situ spectroscopy is also a promising tool to study piezophilic microorganisms.

  6. An XPS (X-Ray Photoelectron Spectroscopy) Study of the Composition of Thin Polyimide Films Formed by Vapor Deposition.

    DTIC Science & Technology

    1987-07-15

    1985) 2857. 13. B. D. Silverman, J. W. Bartha, J. G. Clabes, P. S Ho and A. R. Rossi, J. Polym . Sci. Part A 24 (1986) 3325. 14. E. Cartier , P. Pfluger...Benzenetetracarboxylic anhydride (PMDA), imidization, polymer , in situ, X-ray Photoelectron Spectroscopy (XPS),Cu(111) 20. ABSTRACT (Continue an...ODA) and 1,2,4,5 Benzenetetracarboxylic anhydride (PMDA). The imidization reaction leading to polymer formation was followed in situ with X-ray

  7. 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

  8. Probing local structure of pyrochlore lead zinc niobate with synchrotron x-ray absorption spectroscopy technique

    NASA Astrophysics Data System (ADS)

    Kanchiang, Kanokwan; Pramchu, Sittichain; Yimnirun, Rattikorn; Pakawanit, Phakkhananan; Ananta, Supon; Laosiritaworn, Yongyut

    2013-08-01

    Local structure of lead zinc niobate (PZN) ceramic, synthesized via B-site oxide precursor route in atmospheric pressure, was investigated using synchrotron x-ray absorption spectroscopy (XAS) technique. The x-ray absorption near-edge structure (XANES) simulation was first carried out. The XANES simulation results indicate that the PZN ceramic is in pyrochlore phase having Zn2+ substituted on Nb5+ site. Afterwards, the extended x-ray absorption fine structure (EXAFS) analysis was performed to extract the bond length information between Zn2+ and its neighboring atoms. From the EXAFS fitting, the bond length between Zn2+ and Pb2+ in the pyrochlore phase was found to be longer than the previously reported bond length in the perovskite phase. Further, with the radial distribution information of Zn2+'s neighboring atoms, the formation energies along the precursor-to-pyrochlore and precursor-to-perovskite reaction paths were calculated using the density functional theory (DFT). The calculated results show that the formation energy of the perovskite phase is noticeably higher than that of the pyrochlore phase, which is influenced by the presence of energetic Pb2+ lone pair, as the perovskite phase has shorter Zn2+ to Pb2+ bonding. This therefore suggests the steric hindrance of Pb2+ lone pair and the mutual interactions between Pb2+ lone pair and Zn2+ are main causes of the instability of lead zinc niobate in the perovskite structure and confirm the efficacy of XAS and DFT analysis in revealing local structural details of complex pyrochlore materials.

  9. Characterization of Metalloproteins by High-throughput X-ray Absorption Spectroscopy

    SciTech Connect

    W Shi; M Punta; J Bohon; J Sauder; R DMello; M Sullivan; J Toomey; D Abel; M Lippi; et al.

    2011-12-31

    High-throughput X-ray absorption spectroscopy was used to measure transition metal content based on quantitative detection of X-ray fluorescence signals for 3879 purified proteins from several hundred different protein families generated by the New York SGX Research Center for Structural Genomics. Approximately 9% of the proteins analyzed showed the presence of transition metal atoms (Zn, Cu, Ni, Co, Fe, or Mn) in stoichiometric amounts. The method is highly automated and highly reliable based on comparison of the results to crystal structure data derived from the same protein set. To leverage the experimental metalloprotein annotations, we used a sequence-based de novo prediction method, MetalDetector, to identify Cys and His residues that bind to transition metals for the redundancy reduced subset of 2411 sequences sharing <70% sequence identity and having at least one His or Cys. As the HT-XAS identifies metal type and protein binding, while the bioinformatics analysis identifies metal-binding residues, the results were combined to identify putative metal-binding sites in the proteins and their associated families. We explored the combination of this data with homology models to generate detailed structure models of metal-binding sites for representative proteins. Finally, we used extended X-ray absorption fine structure data from two of the purified Zn metalloproteins to validate predicted metalloprotein binding site structures. This combination of experimental and bioinformatics approaches provides comprehensive active site analysis on the genome scale for metalloproteins as a class, revealing new insights into metalloprotein structure and function.

  10. X-ray And EUV Spectroscopy Of Highly Charged Tungsten Ions

    SciTech Connect

    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 a 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.

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

    SciTech Connect

    Gamboa, E. J.; Fletcher, L. B.; Lee, H. J.; MacDonald, M. J.; Zastrau, U.; Gauthier, M.; Gericke, D. O.; Vorberger, J.; Granados, E.; Hastings, J. B.; Glenzer, S. H.

    2016-01-25

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

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

    SciTech Connect

    Farmand, Maryam

    2013-05-19

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

  13. Fiber-optic based in situ atomic spectroscopy for manufacturing of x-ray optics

    NASA Astrophysics Data System (ADS)

    Atanasoff, George; Metting, Christopher J.; von Bredow, Hasso

    2016-09-01

    The manufacturing of multilayer Laue (MLL) components for X-ray optics by physical vapor deposition (PVD) requires high precision and accuracy that presents a significant process control challenge. Currently, no process control system provides the accuracy, long-term stability and broad capability for adoption in the manufacturing of X-ray optics. In situ atomic absorption spectroscopy is a promising process control solution, capable of monitoring the deposition rate and chemical composition of extremely thin metal silicide films during deposition and overcoming many limitations of the traditional methods. A novel in situ PVD process control system for the manufacturing of high-precision thin films, based on combined atomic absorption/emission spectrometry in the vicinity of the deposited substrate, is described. By monitoring the atomic concentration in the plasma region independently from the film growth on the deposited substrate, the method allows deposition control of extremely thin films, compound thin films and complex multilayer structures. It provides deposition rate and film composition measurements that can be further utilized for dynamic feedback process control. The system comprises a reconfigurable hardware module located outside the deposition chamber with hollow cathode light sources and a fiber-optic-based frame installed inside the deposition chamber. Recent experimental results from in situ monitoring of Al and Si thin films deposited by DC and RF magnetron sputtering at a variety of plasma conditions and monitoring configurations are presented. The results validate the operation of the system in the deposition of compound thin films and provide a path forward for use in manufacturing of X-Ray optics.

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

    SciTech Connect

    Lawniczak-Jablonska, K. |; Jia, J.J.; Underwood, J.H.

    1997-04-01

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

  15. The use of (micro)-X-ray absorption spectroscopy in cement research.

    PubMed

    Scheidegger, A M; Vespa, M; Grolimund, D; Wieland, E; Harfouche, M; Bonhoure, I; Dähn, R

    2006-01-01

    Long-term predictions on the mobility and the fate of radionuclides and contaminants in cementitious waste repositories require a molecular-level understanding of the geochemical immobilization processes involved. In this study, the use of X-ray absorption spectroscopy (XAS) for chemical speciation of trace elements in cementitious materials will be outlined presenting two examples relevant for nuclear waste management. The first example addresses the use of XAS on powdered cementitious materials to determine the local coordination environment of Sn(IV) bound to calcium silicate hydrates (C-S-H). Sn K-edge XAS data of Sn(IV) doped C-S-H can be rationalized by corner sharing binding of Sn octahedra to Si tetrahedra of the C-S-H structure. XAS was further applied to determine the binding mechanism of Sn(IV) in the complex cement matrix. The second example illustrates the potential of emerging synchrotron-based X-ray micro-probe techniques for elucidating the spatial distribution and the speciation of contaminants in highly heterogeneous cementitious materials at the micro-scale. Micro X-ray fluorescence (XRF) and micro-XAS investigations were carried out on Co(II) doped hardened cement paste. These preliminary investigations reveal a highly heterogeneous spatial Co distribution. The presence of a Co(II)-hydroxide-like phase Co(OH)2 and/or Co-Al layered double hydroxide (Co-Al LDH) or Co-phyllosilicate was observed. Surprisingly, some of the initial Co(II) was partially oxidized and incorporated into a Co(III)O(OH)-like phase or a Co-phyllomanganate.

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

    PubMed

    Uhlig, J; Doriese, W B; Fowler, J W; Swetz, D S; Jaye, C; Fischer, D A; Reintsema, C D; Bennett, D A; Vale, L R; Mandal, U; O'Neil, G C; Miaja-Avila, L; Joe, Y I; El Nahhas, A; Fullagar, W; Gustafsson, F Parnefjord; Sundström, V; Kurunthu, D; Hilton, G C; Schmidt, D R; Ullom, J N

    2015-05-01

    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-edge 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.

  17. Beyond structure: ultrafast X-ray absorption spectroscopy as a probe of non-adiabatic wavepacket dynamics.

    PubMed

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

    2016-12-16

    The excited state non-adiabatic dynamics of polyatomic molecules, leading to the coupling of structural and electronic dynamics, is a fundamentally important yet challenging problem for both experiment and theory. Ongoing developments in ultrafast extreme vacuum ultraviolet (XUV) and soft X-ray sources present new probes of coupled electronic-structural dynamics because of their novel and desirable characteristics. As one example, inner-shell spectroscopy offers localized, atom-specific probes of evolving electronic structure and bonding (via chemical shifts). In this work, we present the first on-the-fly ultrafast X-ray time-resolved absorption spectrum simulations of excited state wavepacket dynamics: photo-excited ethylene. This was achieved by coupling the ab initio multiple spawning (AIMS) method, employing on-the-fly dynamics simulations, with high-level algebraic diagrammatic construction (ADC) X-ray absorption cross-section calculations. Using the excited state dynamics of ethylene as a test case, we assessed the ability of X-ray absorption spectroscopy to project out the electronic character of complex wavepacket dynamics, and evaluated the sensitivity of the calculated spectra to large amplitude nuclear motion. In particular, we demonstrate the pronounced sensitivity of the pre-edge region of the X-ray absorption spectrum to the electronic and structural evolution of the excited-state wavepacket. We conclude that ultrafast time-resolved X-ray absorption spectroscopy may become a powerful tool in the interrogation of excited state non-adiabatic molecular dynamics.

  18. Chemical composition and sulfur speciation in bulk tissue by x-ray spectroscopy and x-ray microscopy: corneal development during embryogenesis.

    PubMed

    Koudouna, Elena; Veronesi, Giulia; Patel, Imran I; Cotte, Marine; Knupp, Carlo; Martin, Francis L; Quantock, Andrew J

    2012-07-18

    The chemical composition and sulfur (S) speciation of developing chick corneas at embryonic days 12, 14, and 16 were investigated using synchrotron scanning x-ray fluorescence microscopy and x-ray absorption near-edge structure spectroscopy. The aim was to develop techniques for the analysis of bulk tissue and identify critical physicochemical variations that correlate with changes in corneal structure-function relationships. Derived data were subjected to principal component analysis and linear discriminant analysis, which highlighted differences in the elemental and S species composition at different stages of embryonic growth. Notably, distinct elemental compositions of chlorine, potassium, calcium, phosphorus, and S altered with development during the transition of the immature opaque cornea to a mature transparent tissue. S structure spectroscopy revealed developmentally regulated alterations in thiols, organic monosulfides, ester sulfate, and inorganic sulfate species. The transient molecular structures and compositional changes reported here provide a deeper understanding of the underlying basis of corneal development during the acquisition of transparency. The experimental and analytical approach is new, to our knowledge, and has wide potential applicability in the life sciences.

  19. Testing the theory of colliding winds: the periastron passage of 9 Sagittarii. I. X-ray and optical spectroscopy

    NASA Astrophysics Data System (ADS)

    Rauw, G.; Blomme, R.; Nazé, Y.; Spano, M.; Mahy, L.; Gosset, E.; Volpi, D.; van Winckel, H.; Raskin, G.; Waelkens, C.

    2016-05-01

    Context. The long-period, highly eccentric O-star binary 9 Sgr, known for its non-thermal radio emission and its relatively bright X-ray emission, went through its periastron in 2013. Aims: Such an event can be used to observationally test the predictions of the theory of colliding stellar winds over a broad range of wavelengths. Methods: We conducted a multi-wavelength monitoring campaign of 9 Sgr around the 2013 periastron. In this paper, we focus on X-ray observations and optical spectroscopy. Results: The optical spectra allow us to revisit the orbital solution of 9 Sgr and to refine its orbital period to 9.1 years. The X-ray flux is maximum at periastron over all energy bands, but with clear differences as a function of energy. The largest variations are observed at energies above 2 keV, whilst the spectrum in the soft band (0.5-1.0 keV) remains mostly unchanged, indicating that it arises far from the collision region, in the inner winds of the individual components. The level of the hard emission at periastron clearly deviates from the 1 /r relation expected for an adiabatic wind-interaction zone, whilst this relation seems to hold at the other phases that are covered by our observations. The spectra taken at phase 0.946 reveal a clear Fe xxv line at 6.7 keV, but no such line is detected at periastron (φ = 0.000), although a simple model predicts a strong line that should be easily visible in the data. Conclusions: The peculiarities of the X-ray spectrum of 9 Sgr could reflect the effect of radiative inhibition as well as a phase-dependent efficiency of particle acceleration on the shock properties. Based on observations with XMM-Newton, an ESA Science Mission with instruments and contributions directly funded by ESA Member states and the USA (NASA). Also based on observations collected at the European Southern Observatory (La Silla, Chile) and with the Mercator Telescope operated on the island of La Palma by the Flemish Community, at the Spanish

  20. Probing hot-electron effects in wide area plasmonic surfaces using X-ray photoelectron spectroscopy

    SciTech Connect

    Ayas, Sencer; Cupallari, Andi; Dana, Aykutlu

    2014-12-01

    Plasmon enhanced hot carrier formation in metallic nanostructures increasingly attracts attention due to potential applications in photodetection, photocatalysis, and solar energy conversion. Here, hot-electron effects in nanoscale metal-insulator-metal (MIM) structures are investigated using a non-contact X-ray photoelectron spectroscopy based technique using continuous wave X-ray and laser excitations. The effects are observed through shifts of the binding energy of the top metal layer upon excitation with lasers of 445, 532, and 650 nm wavelength. The shifts are polarization dependent for plasmonic MIM grating structures fabricated by electron beam lithography. Wide area plasmonic MIM surfaces fabricated using a lithography free route by the dewetting of evaporated Ag on HfO{sub 2} exhibit polarization independent optical absorption and surface photovoltage. Using a simple model and making several assumptions about the magnitude of the photoemission current, the responsivity and external quantum efficiency of wide area plasmonic MIM surfaces are estimated as 500 nA/W and 11 × 10{sup −6} for 445 nm illumination.

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

    USGS Publications Warehouse

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

    2006-01-01

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

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

    SciTech Connect

    Andrews, J.C. |

    1995-08-01

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

  3. Molybdenum speciation in uranium mine tailings using X-ray absorption spectroscopy.

    PubMed

    Essilfie-Dughan, Joseph; Pickering, Ingrid J; Hendry, M Jim; George, Graham N; Kotzer, Tom

    2011-01-15

    Uranium (U) mill tailings in northern Saskatchewan, Canada, contain elevated concentrations of molybdenum (Mo). The potential for long-term (>10,000 years) mobilization of Mo from the tailings management facilities to regional groundwater systems is an environmental concern. To assist in characterizing long-term stability, X-ray absorption spectroscopy was used to define the chemical (redox and molecular) speciation of Mo in tailings samples from the Deilmann Tailings Management Facility (DTMF) at the Key Lake operations of Cameco Corporation. Comparison of Mo K near-edge X-ray absorption spectra of tailings samples and reference compounds of known oxidation states indicates Mo exists mainly as molybdate (+6 oxidation state). Principal component analysis of tailings samples spectra followed by linear combination fitting using spectra of reference compounds indicates that various proportions of NiMoO(4) and CaMoO(4) complexes, as well as molybdate adsorbed onto ferrihydrite, are the Mo species present in the U mine tailings. Tailings samples with low Fe/Mo (<708) and high Ni/Mo (>113) molar ratios are dominated by NiMoO(4), whereas those with high Fe/Mo (>708) and low Ni/Mo (<113) molar ratios are dominated by molybdate adsorbed onto ferrihydrite. This suggests that the speciation of Mo in the tailings is dependent in part on the chemistry of the original ore.

  4. Biomedical and agricultural applications of energy dispersive X-ray spectroscopy in electron microscopy.

    PubMed

    Wyroba, Elżbieta; Suski, Szymon; Miller, Karolina; Bartosiewicz, Rafał

    2015-09-01

    Energy dispersive X-ray spectroscopy (EDS) in electron microscopy has been widely used in many research areas since it provides precise information on the chemical composition of subcellular structures that may be correlated with their high resolution images. In EDS the characteristic X-rays typical of each element are analyzed and the new detectors - an example of which we describe - allow for setting precisely the area of measurements and acquiring signals as a point analysis, as a linescan or in the image format of the desired area. Mapping of the elements requires stringent methods of sample preparation to prevent redistribution/loss of the elements as well as elimination of the risk of overlapping spectra. Both qualitative and quantitative analyses may be performed at a low probe current suitable for thin biological samples. Descriptions of preparation techniques, drawbacks and precautions necessary to obtain reliable results are provided, including data on standards, effects of specimen roughness and quantification. Data on EPMA application in different fields of biomedical and agricultural studies are reviewed. In this review we refer to recent EDS/EPMA applications in medical diagnostics, studies on air pollution and agrochemicals as well as on plant models used to monitor the environment.

  5. Can we detect Li K X-ray in lithium compounds using energy dispersive spectroscopy?

    PubMed

    Hovington, Pierre; Timoshevskii, Vladimir; Burgess, Simon; Demers, Hendrix; Statham, Peter; Gauvin, Raynald; Zaghib, Karim

    2016-11-01

    Lithium is the key element for the development of battery and new technology and the development of an analytical technique to spatially and quantitatively resolve this element is of key importance. Detection of Li K in pure metallic lithium is now possible in the Scanning Electron Microscope (SEM) with newly designed Energy Dispersive Spectroscopy (EDS). However, this work is clearly showing, for the first time using EDS, the detection of Li K in several binary lithium compounds (LiH, Li3 N, Li2 S, LiF and LiCl). Experimental Li K X-rays intensity is compared with a specially modified Monte Carlo simulation program showing discrepancies between theoretical and experimental Li K measurements. The effect of chemical bounding on the X-rays emission using density functional theory with the all-electron linearized augmented plane wave is showing that the emission of Li K from the binary compounds studied should be, at least, 12 times lower than in metallic Li. SCANNING 38:571-578, 2016. © 2016 Wiley Periodicals, Inc.

  6. X-ray absorption spectroscopy of iron at multimegabar pressures in laser shock experiments

    NASA Astrophysics Data System (ADS)

    Harmand, M.; Ravasio, A.; Mazevet, S.; Bouchet, J.; Denoeud, A.; Dorchies, F.; Feng, Y.; Fourment, C.; Galtier, E.; Gaudin, J.; Guyot, F.; Kodama, R.; Koenig, M.; Lee, H. J.; Miyanishi, K.; Morard, G.; Musella, R.; Nagler, B.; Nakatsutsumi, M.; Ozaki, N.; Recoules, V.; Toleikis, S.; Vinci, T.; Zastrau, U.; Zhu, D.; Benuzzi-Mounaix, A.

    2015-07-01

    Taking advantage of the new opportunities provided by x-ray free electron laser (FEL) sources when coupled to a long laser pulse as available at the Linear Coherent Light Source (LCLS), we have performed x-ray absorption near-edge spectroscopy (XANES) of laser shock compressed iron up to 420 GPa (±50 ) and 10 800 K (±1390 ). Visible diagnostics coupled with hydrodynamic simulations were used to infer the thermodynamical conditions along the Hugoniot and the release adiabat. A modification of the pre-edge feature at 7.12 keV in the XANES spectra is observed above pressures of 260 GPa along the Hugoniot. Comparing with ab initio calculations and with previous laser-heated diamond cell data, we propose that such changes in the XANES pre-edge could be a signature of molten iron. This interpretation then suggests that iron is molten at pressures and temperatures higher than 260 GPa (±29 ) and 5680 K (±700 ) along the principal Fe Hugoniot.

  7. High Spatial Resolution X-Ray Spectroscopy of Cas A with Chandra

    NASA Astrophysics Data System (ADS)

    Yang, Xue-Juan; Lu, Fang-Jun; Chen, Li

    2008-08-01

    We present high spatial resolution X-ray spectroscopy of the supernova remnant Cassiopeia A with the Chandra observations. The X-ray emitting region of this remnant was divided into 38 × 34 pixels of 10″× 10″ each. Spectra of 960 pixels were created and fitted with an absorbed two component non-equilibrium ionization model. From the results of the spectral analysis we obtained maps of absorbing column density, temperatures, ionization ages, and the abundances of Ne, Mg, Si, S, Ca and Fe. The Si, S and possibly Ca abundance maps show obvious jet structures, while Fe does not follow the jet but seems to be distributed perpendicular to it. The abundances of Si, S and Ca show tight correlations between one another over a range of about two dex. This suggests that they are ejecta from explosive O-burning and incomplete Si-burning. Meanwhile, the Ne abundance is well correlated with that of Mg, indicating them to be the ashes of explosive C/Ne burning. The Fe abundance is positively correlated with that of Si when the latter is lower than 3 times the solar value, and is negatively correlated when higher. We suggest that such a two phase correlation is due to the different ways in which Fe was synthesized.

  8. 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.

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

    SciTech Connect

    Himpsel, Franz J.

    2015-06-12

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

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

    SciTech Connect

    Ward, Jesse D.; Bowden, Mark E.; Resch, Charles T.; Smith, Steven C.; McNamara, Bruce K.; Buck, Edgar C.; Eiden, Gregory C.; Duffin, Andrew M.

    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 to 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.

  11. X-ray absorption spectroscopy study of a copper-containing material after thermal treatment.

    PubMed

    Wei, Y-L; Huang, M-Y; Wang, H-C; Huang, H-C; Lee, J-F

    2006-04-17

    Thermal immobilization of copper contaminant in a copper-containing solid material collected from local copper smelting and foundry area is investigated in the present work. X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) are employed for copper speciation. XAS results indicate that cupric hydroxide is the major copper species in the solid material dried at 105 degrees C. After being subjected to a 500 degrees C thermal process, cupric hydroxide still remains as the main copper species, but some Cu(II) is chemically reduced to Cu(I). More cupric hydroxide is progressively converted to Cu(I) as the sample was heated at 1100 degrees C than that heated at 500 degrees C. The sample heated at 500 degrees C is in its original powder form. However, thermal treatment at 1100 degrees C transforms the powder into a hardened granule-like form that is much bigger in size and difficult to be ground into powders. The sample is sintered with the sparingly soluble cuprous oxide and elemental copper being encapsulated inside. Toxicity characteristic leaching procedure (TCLP) results depict that amount of copper leached from the sample (containing 133,000 mg copper kg-1) heated at 1100 degrees C for 2 h is considerably minor, being 367 mg copper kg-1.

  12. Double-core-hole spectroscopy for chemical analysis with an intense X-ray femtosecond laser

    PubMed Central

    Berrah, Nora; Fang, Li; Murphy, Brendan; Osipov, Timur; Ueda, Kiyoshi; Kukk, Edwin; Feifel, Raimund; van der Meulen, Peter; Salen, Peter; Schmidt, Henning T.; Thomas, Richard D.; Larsson, Mats; Richter, Robert; Prince, Kevin C.; Bozek, John D.; Bostedt, Christoph; Wada, Shin-ichi; Piancastelli, Maria N.; Tashiro, Motomichi; Ehara, Masahiro

    2011-01-01

    Theory predicts that double-core-hole (DCH) spectroscopy can provide a new powerful means of differentiating between similar chemical systems with a sensitivity not hitherto possible. Although DCH ionization on a single site in molecules was recently measured with double- and single-photon absorption, double-core holes with single vacancies on two different sites, allowing unambiguous chemical analysis, have remained elusive. Here we report that direct observation of double-core holes with single vacancies on two different sites produced via sequential two-photon absorption, using short, intense X-ray pulses from the Linac Coherent Light Source free-electron laser and compare it with theoretical modeling. The observation of DCH states, which exhibit a unique signature, and agreement with theory proves the feasibility of the method. Our findings exploit the ultrashort pulse duration of the free-electron laser to eject two core electrons on a time scale comparable to that of Auger decay and demonstrate possible future X-ray control of physical inner-shell processes. PMID:21969540

  13. X-ray absorption spectroscopy of lithium sulfur battery reaction intermediates

    NASA Astrophysics Data System (ADS)

    Wujcik, Kevin; Pascal, Tod; Prendergast, David; Balsara, Nitash

    2015-03-01

    Lithium sulfur batteries have a theoretical energy density nearly five times greater than current lithium ion battery standards, but questions still remain regarding the reaction pathways through which soluble lithium polysulfide (Li2Sx, ``x'' ranging from 2 to 8) reaction intermediates are formed. Complicating spectroelectrochemical approaches to elucidate redox pathways is the challenge of obtaining spectral standards for individual Li2Sx species. Lithium polysulfides cannot be isolated as individual component and exist only in solution as a distribution of different Li2Sx molecules formed via disproportionation reactions (e.g. 2Li2S4 goes to Li2S3 + Li2S5). X-ray absorption spectroscopy (XAS) at the sulfur K-edge has recently been employed as a technique to study Li-S chemistry. We have recently obtained XAS standards for individual Li2Sx species via first principles DFT simulations and the excited electron and core hole approach. Here, experimental sulfur K-edge XAS of Li2Sx species dissolved in poly(ethylene oxide) are compared to spectra obtained from analogous theoretical calculations. The impact that polysulfide solution concentration and the presence of other lithium salts (e.g. LiNO3) have on X-ray spectra of Li2Sx species is explored via experiment and theory.

  14. X-ray absorption spectroscopy as a probe of dissolved polysulfides in lithium sulfur batteries

    NASA Astrophysics Data System (ADS)

    Pascal, Tod; Prendergast, David

    2015-03-01

    There has been enormous interest lately in lithium sulfur batteries, since they have 5 times the theoretical capacity of lithium ion batteries. Large-scale adoption of this technology has been hampered by numerous shortcomings, chiefly the poor utilization of the active cathode material and rapid capacity fading during cycling. Overcoming these limitations requires methods capable of identifying and quantifying the products of the poorly understood electrochemical reactions. One recent advance has been the use of X-ray absorption spectroscopy (XAS), an element-specific probe of the unoccupied energy levels around an excited atom upon absorption of an X-ray photon, to identify the reaction products and intermediates. In this talk, we'll present first principles molecular dynamics and spectral simulations of dissolved lithium polysulfide species, showing how finite temperature dynamics, molecular geometry, molecular charge state and solvent environment conspire to determine the peak positions and intensity of the XAS. We'll present a spectral analysis of the radical (-1e charge) species, and reveal a unique low energy feature that can be used to identify these species from their more common dianion (-2e charge) counterparts.

  15. 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.

  16. High-resolution x-ray absorption spectroscopy studies of metal compounds in neurodegenerative brain tissue

    NASA Astrophysics Data System (ADS)

    Collingwood, J. F.; Mikhaylova, A.; Davidson, M. R.; Batich, C.; Streit, W. J.; Eskin, T.; Terry, J.; Barrea, R.; Underhill, R. S.; Dobson, J.

    2005-01-01

    Fluorescence mapping and microfocus X-ray absorption spectroscopy are used to detect, locate and identify iron biominerals and other inorganic metal accumulations in neurodegenerative brain tissue at sub-cellular resolution (<5 microns). Recent progress in developing the technique is reviewed. Synchrotron X-rays are used to map tissue sections for metals of interest, and XANES and XAFS are used to characterise anomalous concentrations of the metals in-situ so that they can be correlated with tissue structures and disease pathology. Iron anomalies associated with biogenic magnetite, ferritin and haemoglobin are located and identified in an avian tissue model with a pixel resolution ~5 microns. Subsequent studies include brain tissue sections from transgenic Huntington's mice, and the first high-resolution mapping and identification of iron biominerals in human Alzheimer's and control autopsy brain tissue. Technical developments include use of microfocus diffraction to obtain structural information about biominerals in-situ, and depositing sample location grids by lithography for the location of anomalies by conventional microscopy. The combined techniques provide a breakthrough in the study of both intra- and extra-cellular iron compounds and related metals in tissue. The information to be gained from this approach has implications for future diagnosis and treatment of neurodegeneration, and for our understanding of the mechanisms involved.

  17. High-resolution x-ray absorption spectroscopy studies of metal compounds in neurodegenerative brain tissue

    SciTech Connect

    Collingwood, J.F.; Mikhaylova, A.; Davidson, M.R.; Batich, C.; Streit, W.J.; Eskin, T.; Terry, J.; Barrea, R.; Underhill, R.S.; Dobson, J.

    2008-06-16

    Fluorescence mapping and microfocus X-ray absorption spectroscopy are used to detect, locate and identify iron biominerals and other inorganic metal accumulations in neurodegenerative brain tissue at sub-cellular resolution (< 5 microns). Recent progress in developing the technique is reviewed. Synchrotron X-rays are used to map tissue sections for metals of interest, and XANES and XAFS are used to characterize anomalous concentrations of the metals in-situ so that they can be correlated with tissue structures and disease pathology. Iron anomalies associated with biogenic magnetite, ferritin and haemoglobin are located and identified in an avian tissue model with a pixel resolution {approx} 5 microns. Subsequent studies include brain tissue sections from transgenic Huntington's mice, and the first high-resolution mapping and identification of iron biominerals in human Alzheimer's and control autopsy brain tissue. Technical developments include use of microfocus diffraction to obtain structural information about biominerals in-situ, and depositing sample location grids by lithography for the location of anomalies by conventional microscopy. The combined techniques provide a breakthrough in the study of both intra- and extra-cellular iron compounds and related metals in tissue. The information to be gained from this approach has implications for future diagnosis and treatment of neurodegeneration, and for our understanding of the mechanisms involved.

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

    PubMed

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

    2014-02-01

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

  19. Mossbauer spectroscopy and X-ray diffraction of samples from the Santa Catharina iron meteorite

    NASA Technical Reports Server (NTRS)

    Roy-Poulsen, H.; Clarke, R. S., Jr.; Jensen, G. B.; Knudsen, J. M.; Larsen, L.; Roy-Poulsen, N. O.; Vistisen, L.

    1984-01-01

    Conversion electron Mossbauer spectroscopy (CEMS) of samples from the Santa Catharina iron meteorite shows the presence of the ordered iron-nickel phase with 50% Ni, tetrataenite, and of the paramagnetic iron-nickel phase with 25% Ni. The FeNi phase with 50% Ni amounts to 70% of the iron-nickel alloys. Futhermore, the CEM spectra show the presence of small peaks from one or more spinel compounds. These small peaks are more pronounced when regions near the rim of the samples are analyzed. The X-ray diffraction of different areas of the samples, both optically dark and optically light areas, shows the presence of a diffraction pattern from a single f.c.c. lattice with a lattice parameter of a=3.58A This means that the two different Fe-Ni phases seen in the CEMS analysis occupy the same lattice. The X-ray photographs also show the presence of super-structure reflections from the ordered FeNi phase, and that the orientation of the f.c.c. lattice is the same within the whole sample.

  20. Millisecond Kinetics of Nanocrystal Cation Exchange UsingMicrofluidic X-ray Absorption Spectroscopy

    SciTech Connect

    Chan, Emory M.; Marcus, Matthew A.; Fakra, Sirine; Elnaggar,Mariam S.; Mathies, Richard A.; Alivisatos, A. Paul

    2007-05-07

    We describe the use of a flow-focusing microfluidic reactorto measure the kinetics of theCdSe-to-Ag2Se nanocrystal cation exchangereaction using micro-X-ray absorption spectroscopy (mu XAS). The smallmicroreactor dimensions facilitate the millisecond mixing of CdSenanocrystal and Ag+ reactant solutions, and the transposition of thereaction time onto spatial coordinates enables the in situ observation ofthe millisecond reaction with mu XAS. XAS spectra show the progression ofCdSe nanocrystals to Ag2Se over the course of 100 ms without the presenceof long-lived intermediates. These results, along with supporting stoppedflow absorption experiments, suggest that this nanocrystal cationexchange reaction is highly efficient and provide insight into how thereaction progresses in individual particles. This experiment illustratesthe value and potential of in situ microfluidic X-ray synchrotrontechniques for detailed studies of the millisecond structuraltransformations of nanoparticles and other solution-phase reactions inwhich diffusive mixing initiates changes in local bond structures oroxidation states.

  1. 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).

  2. Americium characterization by X-ray fluorescence and absorption spectroscopy in plutonium uranium mixed oxide

    NASA Astrophysics Data System (ADS)

    Degueldre, Claude; Cozzo, Cedric; Martin, Matthias; Grolimund, Daniel; Mieszczynski, Cyprian

    2013-06-01

    Plutonium uranium mixed oxide (MOX) fuels are currently used in nuclear reactors. The actinides in these fuels need to be analyzed after irradiation for assessing their behaviour with regard to their environment and the coolant. In this work the study of the atomic structure and next-neighbour environment of Am in the (Pu,U)O2 lattice in an irradiated (60 MW d kg-1) MOX sample was performed employing micro-X-ray fluorescence (µ-XRF) and micro-X-ray absorption fine structure (µ-XAFS) spectroscopy. The chemical bonds, valences and stoichiometry of Am (˜0.66 wt%) are determined from the experimental data gained for the irradiated fuel material examined in its peripheral zone (rim) of the fuel. In the irradiated sample Am builds up as Am3+ species within an [AmO8]13- coordination environment (e.g. >90%) and no (<10%) Am(IV) or (V) can be detected in the rim zone. The occurrence of americium dioxide is avoided by the redox buffering activity of the uranium dioxide matrix.

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

    PubMed

    Susi, Toma; Pichler, Thomas; Ayala, Paola

    2015-01-01

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

  4. A Suborbital Payload for Soft X-ray Spectroscopy of Extended Sources

    NASA Astrophysics Data System (ADS)

    Oakley, Phillip Henry Howard

    This thesis details the intent, design and results of an X-ray suborbital rocket payload whose scientific target was the Cygnus Loop Supernova Remnant. The payload consists of wire grid collimators, off-plane gratings arrays and gaseous electron multiplier (GEM) detectors. The system was designed for measurements in the 17-107 Å bandpass with a resolution up to ∼ 60 (λ=Δλ). This instrument was christened the Extended X-ray Off-plane Spectrometer (EXOS) and was launched on a Terrier-Black Brant rocket on November 13th, 2009 from White Sands Missile Range and obtained 340 seconds of useable scientific data. The emission is dominated by O VII and O VIII, including the He-like O VII triplet at ∼22 Å. Another feature at ∼45 Å is composed primarily of Si XI and Si XII. The best-fit model to this spectrum is an equilibrium plasma model at a temperature of log(T) = 6.4 (0.23 keV).

  5. A miniature metal-ceramic x-ray source for spacecraft instrumentation.

    PubMed

    Koppel, L N; Marshall, J R

    1998-04-01

    Definitive mineralogical identification of materials with x-ray diffraction and fluorescence on remote planetary probes requires the development of a rugged miniature x-ray source that complies with the mass, power, thermal, and electrical management constraints imposed by space missions. Conventional x-ray tubes are generally fragile, glass-envelope designs with heat-sensitive seals. They are too brittle and bulky for planetary missions, and usually require cumbersome and power-consuming cooling systems. Here we describe the development of a novel, rugged miniature x-ray source employing a ceramic BeO substrate upon which a metal target material is deposited. Conventional thermionic emission and high-voltage acceleration of electrons to strike the metal target material produce an x-ray yield comparable to conventional x-ray tubes. Thermal management of the x-ray source is achieved with the excellent heat transport properties of the BeO target substrate coupled with a passive heatpipe.

  6. Towards laboratory x-ray nanotomography: instrumental improvements on a SEM-based system

    NASA Astrophysics Data System (ADS)

    Gomes Perini, L. A.; Bleuet, P.; Buijsse, B.; Kwakman, L. F. Tz.; Parker, W.

    2016-10-01

    We aim at resolving deca-nanometer features in microelectronic samples using a laboratory SEM-based X-ray tomography microscope. Such a system produces X-rays through the interaction between a focused SEM electron beam and a metallic target. The effective source size of the X-ray beam can be adjusted by varying the target material and geometry. For instance, the use of tungsten nanowires (few hundred nanometers of length) combined with a high electron beam current leads to an increased X-ray flux generated in a reduced volume, necessary for detecting interface details of the analyzed object. It improves resolution and signal-to-noise ratio (SNR), but is also sensitive to electron beam-target instabilities during the scan. To improve robustness, a FFT-based image correlation is integrated in the process through a closed-loop control scheme. It allows stabilizing the electron beam on the target and to preserve the X-ray flux intensity and alignment. Also, a state of the art high-resolution scientific-CMOS (sCMOS) X-ray detector was installed, allowing to reduce noise and to increase quantum efficiency. Results show that such numerical and equipment improvements lead to significant gains in spatial resolution, SNR and scanning time of the SEM-based tomography. It paves the way to routine, high resolution, 3D X-ray imaging in the laboratory.

  7. Electronic Structures of Uranium Compounds Studied by Soft X-ray Photoelectron Spectroscopy

    NASA Astrophysics Data System (ADS)

    Fujimori, Shin-ichi; Takeda, Yukiharu; Okane, Tetsuo; Saitoh, Yuji; Fujimori, Atsushi; Yamagami, Hiroshi; Haga, Yoshinori; Yamamoto, Etsuji; Ōnuki, Yoshichika

    2016-06-01

    The electronic structures of uranium-based compounds have been studied by photoelectron spectroscopy with soft X-ray synchrotron radiation. Angle-resolved photoelectron spectroscopy with soft X-rays has made it possible to directly observe their bulk band structures and Fermi surfaces. It has been shown that the band structures and Fermi surfaces of itinerant compounds such as UB2, UN, and UFeGa5 are quantitatively described by a band-structure calculation treating all U 5f electrons as itinerant. Furthermore, the overall electronic structures of heavy-fermion compounds such as UPd2Al3, UNi2Al3, and URu2Si2 are also explained by a band-structure calculation, although some disagreements exist, which might originate from the electron correlation effect. This suggests that the itinerant description of U 5f states is an appropriate starting point for the description of their electronic structures. The situation is similar for ferromagnetic superconductors such as UGe2, URhGe, UCoGe, and UIr, although the complications from their low-symmetry crystal structures make it more difficult to describe their detailed electronic structures. The local electronic structures of the uranium site have been probed by core-level photoelectron spectroscopy with soft X-rays. The comparisons of core-level spectra of heavy-fermion compounds with typical itinerant and localized compounds suggest that the local electronic structures of most itinerant and heavy-fermion compounds are close to the U 5f3 configuration except for UPd2Al3 and UPt3. The core-level spectrum of UPd2Al3 has similarities to those of both itinerant and localized compounds, suggesting that it is located at the boundary between the itinerant and localized states. Moreover, the spectrum of UPt3 is very close to that of the localized compound UPd3, suggesting that it is nearly localized, although there are narrow quasi-particle bands in the vicinity of EF.

  8. Planetary and satellite x ray spectroscopy: A new window on solid-body composition by remote sensing

    NASA Technical Reports Server (NTRS)

    Chenette, D. L.; Wolcott, R. W.; Selesnick, R. S.

    1993-01-01

    The rings and most of the satellites of the outer planets orbit within the radiation belts of their parent bodies. This is an environment with intense fluxes of energetic electrons. As a result, these objects are strong emitters of X-rays. The characteristic X-ray lines from these bodies depend on atomic composition, but they are not sensitive to how the material is arranged in compounds or mixtures. X-ray fluorescence spectral analysis has demonstrated its unique value in the laboratory as a qualitative and quantitative analysis tool. This technique has yet to be fully exploited in a planetary instrument for remote sensing. The characteristic X-ray emissions provide atomic relative abundances. These results are complementary to the molecular composition information obtained from IR, visible, and UV emission spectra. The atomic relative abundances are crucial to understanding the formation and evolution of these bodies. They are also crucial to the proper interpretation of the molecular composition results from the other sensors. The intensities of the characteristic X-ray emissions are sufficiently strong to be measured with an instrument of modest size. Recent developments in X-ray detector technologies and electronic miniaturization have made possible space-flight X-ray imaging and nonimaging spectrometers of high sensitivity and excellent energy resolution that are rugged enough to survive long-duration space missions. Depending on the application, such instruments are capable of resolving elemental abundances of elements from carbon through iron. At the same time, by measuring the bremsstrahlung intensity and energy spectrum, the characteristics of the source electron flux can be determined. We will discuss these concepts, including estimated source strengths, and will describe a small instrument capable of providing this unique channel of information for future planetary missions. We propose to build this instrument using innovative electronics packaging

  9. Distribution and speciation of bromine in mammalian tissue and fluids by X-ray fluorescence imaging and X-ray absorption spectroscopy.

    PubMed

    Ceko, Melanie J; Hummitzsch, Katja; Hatzirodos, Nicholas; Bonner, Wendy; James, Simon A; Kirby, Jason K; Rodgers, Raymond J; Harris, Hugh H

    2015-05-01

    Bromine is one of the most abundant and ubiquitous trace elements in the biosphere and until recently had not been shown to perform any essential biological function in animals. A recent study demonstrated that bromine is required as a cofactor for peroxidasin-catalysed formation of sulfilimine crosslinks in Drosophila. In addition, bromine dietary deficiency is lethal in Drosophila, whereas bromine replenishment restores viability. The aim of this study was to examine the distribution and speciation of bromine in mammalian tissues and fluids to provide further insights into the role and function of this element in biological systems. In this study we used X-ray fluorescence (XRF) imaging and inductively coupled plasma-mass spectrometry (ICP-MS) to examine the distribution of bromine in bovine ovarian tissue samples, follicular fluid and aortic serum, as well as human whole blood and serum and X-ray absorption spectroscopy (XAS) to identify the chemical species of bromine in a range of mammalian tissue (bovine, ovine, porcine and murine), whole blood and serum samples (bovine, ovine, porcine, murine and human), and marine samples (salmon (Salmo salar), kingfish (Seriola lalandi) and Scleractinian coral). Bromine was found to be widely distributed across all tissues and fluids examined. In the bovine ovary in particular it was more concentrated in the sub-endothelial regions of arterioles. Statistical comparison of the near-edge region of the X-ray absorption spectra with a library of bromine standards led to the conclusion that the major form of bromine in all samples analysed was bromide.

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

    SciTech Connect

    Butorin, S.M.; Guo, J.; Magnuson, M.

    1997-04-01

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

  11. 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.

  12. Visualizing interfacial charge transfer in dye sensitized nanoparticles using x-ray transient absorption spectroscopy.

    SciTech Connect

    Zhang, X. Y.; Smolentsev, G.; Guo, J.; Attenkofer, K.; Kurtz, C.; Jennings, G.; Lockard, J. V.; Stickrath, A. B.; Chen, L. X.

    2011-01-01

    A molecular level understanding of the structural reorganization accompanying interfacial electron transfer is important for rational design of solar cells. Here we have applied XTA (X-ray transient absorption) spectroscopy to study transient structures in a heterogeneous interfacial system mimicking the charge separation process in dye-sensitized solar cell (DSSC) with Ru(dcbpy){sub 2}(NCS){sub 2} (RuN3) dye adsorbed to TiO{sub 2} nanoparticle surfaces. The results show that the average Ru-NCS bond length reduces by 0.06 {angstrom}, whereas the average Ru-N(dcbpy) bond length remains nearly unchanged after the electron injection. The differences in bond-order change and steric hindrance between two types of ligands are attributed to their structural response in the charge separation. This study extends the application of XTA into optically opaque hybrid interfacial systems relevant to the solar energy conversion.

  13. Electronic topological transition in zinc under pressure: An x-ray absorption spectroscopy study

    SciTech Connect

    Aquilanti, G.; Trapananti, A.; Pascarelli, S.; Minicucci, M.; Principi, E.; Liscio, F.; Twarog, A.

    2007-10-01

    Zinc metal has been studied at high pressure using x-ray absorption spectroscopy. In order to investigate the role of the different degrees of hydrostaticity on the occurrence of structural anomalies following the electronic topological transition, two pressure transmitting media have been used. Results show that the electronic topological transition, if it exists, does not induce an anomaly in the local environment of compressed Zn as a function of hydrostatic pressure and any anomaly must be related to a loss of hydrostaticity of the pressure transmitting medium. The near-edge structures of the spectra, sensitive to variations in the electronic density of states above the Fermi level, do not show any evidence of electronic transition whatever pressure transmitting medium is used.

  14. Sodium Chloride Diffusion during Muscle Salting Evidenced by Energy-Dispersive X-ray Spectroscopy Imaging.

    PubMed

    Filgueras, Rénata; Peyrin, Frédéric; Vénien, Annie; Hénot, Jean Marc; Astruc, Thierry

    2016-01-27

    To better understand the relationship between the muscle structure and NaCl transfers in meat, we used energy-dispersive X-ray spectroscopy (EDS) coupled with scanning electron microscopy (SEM) to analyze brined and dry-salted rat muscles. The muscles were freeze-dried to avoid the delocalization of soluble ions that happens in regular dehydration through a graded series of ethanol. Na and Cl maps were superimposed on SEM images to combine the muscle structure and NaCl diffusion. Brining causes rapid diffusion of NaCl through the tissue. Most brine diffuses in a linear front from the muscle surface, but a small proportion enters through the perimysium network. The muscle area penetrated by brine shows heterogeneous patterns of NaCl retention, with some connective tissue islets containing more NaCl than other parts of perimysium. NaCl penetration is considerably slower after dry salting than after brining.

  15. X-Ray absorption spectroscopy investigation of 1-alkyl-3-methylimidazolium bromide salts

    SciTech Connect

    D'Angelo, Paola; Zitolo, Andrea; Migliorati, Valentina; Bodo, Enrico; Caminiti, Ruggero; Aquilanti, Giuliana; Hazemann, Jean Louis; Testemale, Denis; Mancini, Giordano

    2011-08-21

    X-ray absorption spectroscopy (XAS) has been used to unveil the bromide ion local coordination structure in 1-alkyl-3-methylimidazolium bromide [C{sub n}mim]Br ionic liquids (ILs) with different alkyl chains. The XAS spectrum of 1-ethyl-3-methylimidazolium bromide has been found to be different from those of the other members of the series, from the butyl to the decyl derivatives, that have all identical XAS spectra. This result indicates that starting from 1-buthyl-3-methylimidazolium bromide the local molecular arrangement around the bromide anion is the same independently from the length of the alkyl chain, and that the imidazolium head groups in the liquid ILs with long alkyl chains assume locally the same orientation as in the [C{sub 4}mim]Br crystal. With this study we show that the XAS technique is an effective direct tool for unveiling the local structural arrangements around selected atoms in ILs.

  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. Studies of Y-Ba-Cu-O single crystals by x-ray absorption spectroscopy

    SciTech Connect

    Krol, A.; Ming, Z.H.; Kao, Y.H.; Nuecker, N.; Roth, G.; Fink, J.; Smith, G.C.; Erband, A.; Mueller-Vogt, G.; Karpinski, J.; Kaldis, E.; Schoenmann, K.

    1992-02-01

    The symmetry and density of unoccupied states of YBa{sub 2}Cu{sub 3}O{sub 7} YBa{sub 2}Cu{sub 4}O{sub 8} have been investigated by orientation dependent x-ray absorption spectroscopy on the O 1s edge using a bulk-sensitive fluorescence-yield-detection method. It has been found that the O 2p holes are distributed equally between the CuO{sub 2} planes and CuO chains and that the partial density of unoccupied O 2p states in the CuO{sub 2} planes are identical in both systems investigated. The upper Hubbard band has been observed in the planes but not in the chains in both systems. 18 refs.

  18. Zinc ligands in the metal hyperaccumulator Thlaspi caerulescens as determined using X-ray absorption spectroscopy

    SciTech Connect

    Salt, D.E.; Prince, R.C.; Baker, A.J.M.; Raskin, I.; Pickering, I.J.

    1999-03-01

    Using the noninvasive technique of X-ray absorption spectroscopy (XAS), the authors have been able to determine the ligand environment of Zn in different tissues of the Zn-hyperaccumulator Thlaspi caerulescens. The majority of intracellular Zn in roots of T. caerulescens was found to be coordinated with histidine. In the xylem sap Zn was found to be transported mainly as the free hydrated Zn{sup 2+} cation with a smaller proportion coordinated with organic acids. In the shoots, Zn coordination occurred mainly via organic acids, with a smaller proportion present as the hydrated cation and coordinated with histidine and the cell wall. Their data suggest that histidine plays an important role in Zn homeostasis in the roots, whereas organic acids are involved in xylem transport and Zn storage in shoots.

  19. The irradiation of ammonia ice studied by near edge x-ray absorption spectroscopy

    SciTech Connect

    Parent, Ph.; Bournel, F.; Lasne, J.; Laffon, C.; Carniato, S.; Lacombe, S.; Strazzulla, G.; Gardonio, S.; Lizzit, S.; Kappler, J.-P.; Joly, L.

    2009-10-21

    A vapor-deposited NH{sub 3} ice film irradiated at 20 K with 150 eV photons has been studied with near-edge x-ray absorption fine structure (NEXAFS) spectroscopy at the nitrogen K-edge. Irradiation leads to the formation of high amounts (12%) of molecular nitrogen N{sub 2}, whose concentration as a function of the absorbed energy has been quantified to 0.13 molecule/eV. The stability of N{sub 2} in solid NH{sub 3} has been also studied, showing that N{sub 2} continuously desorbs between 20 and 95 K from the irradiated ammonia ice film. Weak concentrations (<1%) of other photoproducts are also detected. Our NEXAFS simulations show that these features own to NH{sub 2}, N{sub 2}H{sub 2}, and N{sub 3}{sup -}.

  20. Assessment of the weathering of protective coatings using x-ray photoelectron spectroscopy

    SciTech Connect

    Wilson, G.R.; Skerry, B.S.

    1993-12-31

    Three fully formulated coatings systems: polyurethane, alkyd and latex, were exposed either outdoors to a natural industrial atmospheric environment or to an accelerated corrosion/weathering test incorporating UV-condensation exposures and wet/dry corrosion cycling or to an RF generated {open_quotes}in-glow{close_quotes} oxygen plasma. Changes in coating surface chemistry as a function of time in each environment were followed using X-ray photoelectron spectroscopy (XPS). XPS detected changes in the surface composition of all three systems for all three environmentS. Some of the trends in degradation detected on the exterior exposed samples were reproduced by both accelerated tests. The data obtained from this study also suggested that the corrosion/weathering test would benefit from an increase in the amount of UV exposure over that which is currently used. Oxygen plasma etching also appears to have some potential as a tool for accelerated weathering of paint systems.

  1. X-ray photoelectron spectroscopy study of chemically-etched Nd-Ce-Cu-O surfaces

    NASA Technical Reports Server (NTRS)

    Vasquez, R. P.; Gupta, A.; Kussmaul, A.

    1991-01-01

    Acetic acid, Br2, and HCl solutions are investigated for removing insulating species from Nd(1.85)Ce(0.15)CuO(4-delta) (NCCO) thin film surfaces. X-ray photoelectron spectroscopy (XPS) shows that the HCl etch is most effective, yielding O 1s spectra comparable to those obtained from samples cleaned in vacuum and a clear Fermi edge in the valence band region. Reduction and oxidation reversibly induces and eliminates, respectively, Fermi level states for undoped samples, but has no clearly observable effect on the XPS spectra for doped samples. Reactivity to air is much less for NCCO compared to hole superconductors, which is attributed to the lack of reactive alkaline earth elements in NCCO.

  2. X-Ray Absorption Spectroscopy Of Thin Foils Irradiated By An Ultra-short Laser Pulse

    SciTech Connect

    Renaudin, P.; Blancard, C.; Cosse, P.; Faussurier, G.; Lecherbourg, L.; Audebert, P.; Bastiani-Ceccotti, S.; Geindre, J.-P.; Shepherd, R.

    2007-08-02

    Point-projection K-shell absorption spectroscopy has been used to measure absorption spectra of transient plasma created by an ultra-short laser pulse. The 1s-2p and 1s-3p absorption lines of weakly ionized aluminum and the 2p-3d absorption lines of bromine were measured over an extended range of densities in a low-temperature regime. Independent plasma characterization was obtained using frequency domain interferometry diagnostic (FDI) that allows the interpretation of the absorption spectra in terms of spectral opacities. Assuming local thermodynamic equilibrium, spectral opacity calculations have been performed using the density and temperature inferred from the FDI diagnostic to compare to the measured absorption spectra. A good agreement is obtained when non-equilibrium effects due to non-stationary atomic physics are negligible at the x-ray probe time.

  3. 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.

  4. Determination of band profiles in GaN films using hard X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Saito, Shinji; Yoshiki, Masahiko; Nunoue, Shinya; Sano, Nobuyuki

    2017-02-01

    We investigated band-profile control by introducing interlayers between a semiconductor and metal contact layers to improve the electrical properties of GaN-based semiconductor devices. We evaluated the electronic structure of the semiconductor surface and the metal/semiconductor interface by hard X-ray photoelectron spectroscopy. We also performed Monte Carlo simulations using the Boltzmann transport equation under the potential profile obtained using the Poisson equation. The band profile in the semiconductor substrate was then examined by comparing the energy spectra from the simulations with those from the experiments. We obtained good agreement between the two results. The present experimental and theoretical methods allow one to determine the band profile near the surface of a semiconductor as well as that in a metal interface. This approach may become a useful tool in the design and/or evaluation of processing conditions.

  5. Enzymatic modification and X-ray photoelectron spectroscopy analysis of a functionalized polydiacetylene thin film

    SciTech Connect

    Wilson, T.E.; Spevak, W.; Bednarski, M.D. Lawrence Berkeley Lab., CA ); Charych, D.H. )

    1994-05-01

    The mild conditions and specificity of biological catalysts are attractive incentives for their use in the formation of surfaces with well-defined chemical functionality. Herein, we describe the synthesis, characterization, and enzymatic modification of a functionalized polymeric bilayer assembly. The assembly is composed of a self-assembled monolayer of octadecylsilane and a Langmuir-Blodgett monolayer of polydiacetylene functionalized with the dipeptide phenylalanine-alanine (Phe-Ala). We demonstrate via X-ray photoelectron spectroscopy surface analysis that the surface-bound Phe-Ala dipeptide is a substrate for specific cleavage by the enzyme subtilisin BPN[prime]. In-situ surface transformations via enzymatic synthesis or cleavage offer an alternative to chemical treatments of organic thin films. 28 refs., 4 figs.

  6. 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.

  7. Structural analysis of sulfur in natural rubber using X-ray absorption near-edge spectroscopy.

    PubMed

    Pattanasiriwisawa, Wanwisa; Siritapetawee, Jaruwan; Patarapaiboolchai, Orasa; Klysubun, Wantana

    2008-09-01

    X-ray absorption near-edge spectroscopy (XANES) has been applied to natural rubber in order to study the local environment of sulfur atoms in sulfur crosslinking structures introduced in the vulcanization process. Different types of chemical accelerators in conventional, semi-efficient and efficient vulcanization systems were investigated. The experimental results show the good sensitivity and reproducibility of XANES to characterize the local geometry and electronic environment of the sulfur K-shell under various conditions of vulcanization and non-vulcanization of natural rubber. Several applications of XANES in this study demonstrate an alternative way of identifying sulfur crosslinks in treated natural rubber based on differences in their spectra and oxidation states.

  8. X-Ray Absorption Spectroscopy Of Thin Foils Irradiated By An Ultra-short Laser Pulse

    NASA Astrophysics Data System (ADS)

    Renaudin, P.; Lecherbourg, L.; Blancard, C.; Cossé, P.; Faussurier, G.; Audebert, P.; Bastiani-Ceccotti, S.; Geindre, J.-P.; Shepherd, R.

    2007-08-01

    Point-projection K-shell absorption spectroscopy has been used to measure absorption spectra of transient plasma created by an ultra-short laser pulse. The 1s-2p and 1s-3p absorption lines of weakly ionized aluminum and the 2p-3d absorption lines of bromine were measured over an extended range of densities in a low-temperature regime. Independent plasma characterization was obtained using frequency domain interferometry diagnostic (FDI) that allows the interpretation of the absorption spectra in terms of spectral opacities. Assuming local thermodynamic equilibrium, spectral opacity calculations have been performed using the density and temperature inferred from the FDI diagnostic to compare to the measured absorption spectra. A good agreement is obtained when non-equilibrium effects due to non-stationary atomic physics are negligible at the x-ray probe time.

  9. Time-resolved x-ray absorption spectroscopy with a water window high-harmonic source

    NASA Astrophysics Data System (ADS)

    Pertot, Yoann; Schmidt, Cédric; Matthews, Mary; Chauvet, Adrien; Huppert, Martin; Svoboda, Vit; von Conta, Aaron; Tehlar, Andres; Baykusheva, Denitsa; Wolf, Jean-Pierre; Wörner, Hans Jakob

    2017-01-01

    Time-resolved x-ray absorption spectroscopy (TR-XAS) has so far practically been limited to large-scale facilities, to subpicosecond temporal resolution, and to the condensed phase. We report the realization of TR-XAS with a temporal resolution in the low femtosecond range by developing a tabletop high-harmonic source reaching up to 350 electron volts, thus partially covering the spectral region of 280 to 530 electron volts, where water is transmissive. We used this source to follow previously unexamined light-induced chemical reactions in the lowest electronic states of isolated CF4+ and SF6+ molecules in the gas phase. By probing element-specific core-to-valence transitions at the carbon K-edge or the sulfur L-edges, we characterized their reaction paths and observed the effect of symmetry breaking through the splitting of absorption bands and Rydberg-valence mixing induced by the geometry changes.

  10. Melting of iron determined by X-ray absorption spectroscopy to 100 GPa

    PubMed Central

    Aquilanti, Giuliana; Trapananti, Angela; Karandikar, Amol; Kantor, Innokenty; Marini, Carlo; Mathon, Olivier; Pascarelli, Sakura; Boehler, Reinhard

    2015-01-01

    Temperature, thermal history, and dynamics of Earth rely critically on the knowledge of the melting temperature of iron at the pressure conditions of the inner core boundary (ICB) where the geotherm crosses the melting curve. The literature on this subject is overwhelming, and no consensus has been reached, with a very large disagreement of the order of 2,000 K for the ICB temperature. Here we report new data on the melting temperature of iron in a laser-heated diamond anvil cell to 103 GPa obtained by X-ray absorption spectroscopy, a technique rarely used at such conditions. The modifications of the onset of the absorption spectra are used as a reliable melting criterion regardless of the solid phase from which the solid to liquid transition takes place. Our results show a melting temperature of iron in agreement with most previous studies up to 100 GPa, namely of 3,090 K at 103 GPa. PMID:26371317

  11. Uranium and thorium sorption on minerals studied by x-ray absorption spectroscopy

    SciTech Connect

    Hudson, E.A.; Terminello, L.J.; Viani, B.E.

    1995-12-01

    Several actinide-mineral sorption systems were studied by uranium and thorium L{sub 3}-edge x-ray absorption spectroscopy. A series of layer silicate minerals, including micas, were selected for their systematic variations in surface structure, e.g. degree of permanent negative charge on the basal planes. An expansible layer silicate, vermiculite, was treated to provide several different interlayer spacings, allowing variations in the accessibility of interior cation exchange sites. The finely powdered minerals were exposed to aqueous solutions of uranyl chloride or thorium chloride. Analysis of the EXAFS and XANES spectra indicates the influence of the mineral substrate upon the local structure of the bound actinide species. Trends in the data are interpreted based upon the known variations in mineral structure.

  12. 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.

  13. X-ray photoelectron spectroscopy study of radiofrequency-sputtered refractory compound steel interfaces

    NASA Technical Reports Server (NTRS)

    Wheeler, D. R.; Brainard, W. A.

    1978-01-01

    Radiofrequency sputtering was used to deposit Mo2C, Mo2B5, and MoSi2 coatings on 440C steel substrates. Both sputter etched and preoxidized substrates were used, and the films were deposited with and without a substrate bias of -300 V. The composition of the coatings was measured as a function of depth by X-ray photoelectron spectroscopy combined with argon ion etching. In the interfacial region there was evidence that bias produced a graded interface in Mo2B5 but not in Mo2C. Oxides of iron and of all film constituents except carbon were presented in all cases but the iron oxide concentration was higher and the layer thicker on the preoxidized substrates. The film and iron oxides were mixed in the MoSi2 and Mo2C films but layered in the Mo2B5 film. The presence of mixed oxides correlates with enhanced film adhesion.

  14. Resolution enhancement in coherent x-ray diffraction imaging by overcoming instrumental noise.

    PubMed

    Kim, Chan; Kim, Yoonhee; Song, Changyong; Kim, Sang Soo; Kim, Sunam; Kang, Hyon Chol; Hwu, Yeukuang; Tsuei, Ku-Ding; Liang, Keng San; Noh, Do Young

    2014-11-17

    We report that reference objects, strong scatterers neighboring weak phase objects, enhance the phase retrieval and spatial resolution in coherent x-ray diffraction imaging (CDI). A CDI experiment with Au nano-particles exhibited that the reference objects amplified the signal-to-noise ratio in the diffraction intensity at large diffraction angles, which significantly enhanced the image resolution. The interference between the diffracted x-ray from reference objects and a specimen also improved the retrieval of the phase of the diffraction signal. The enhancement was applied to image NiO nano-particles and a mitochondrion and confirmed in a simulation with a bacteria phantom. We expect that the proposed method will be of great help in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.

  15. Development of Kilo-Pixel Arrays of Transition-Edge Sensors for X-Ray Spectroscopy

    NASA Technical Reports Server (NTRS)

    Adams, J. S.; Bandler, S. R.; Busch, S. E.; Chervenak, J. A.; Chiao, M. P.; Eckart, M. E.; Ewin, A. J.; Finkbeiner, F. M.; Kelley, R. L.; Kelly, D. P.; Kilbourne, C. A.; Leutenegger, M. A.; Porst, J.-P.; Porter, F. S.; Ray, C. A.; Sadleir, J. E.; Smith, S. J.; Wassell, E. J.; Doriese, W. B.; Fowler, J. W.; Hilton, G. C.; Irwin, K. D.; Reintsema, C. D.; Smith, D. R.; Swetz, D. S.

    2012-01-01

    We are developing kilo-pixel arrays of transition-edge sensor (TES) microcalorimeters for future X-ray astronomy observatories or for use in laboratory astrophysics applications. For example, Athena/XMS (currently under study by the european space agency) would require a close-packed 32x32 pixel array on a 250-micron pitch with < 3.0 eV full-width-half-maximum energy resolution at 6 keV and at count-rates of up to 50 counts/pixel/second. We present characterization of 32x32 arrays. These detectors will be readout using state of the art SQUID based time-domain multiplexing (TDM). We will also present the latest results in integrating these detectors and the TDM readout technology into a 16 row x N column field-able instrument.

  16. Local electronic states of Fe4N films revealed by x-ray absorption spectroscopy and x-ray magnetic circular dichroism

    NASA Astrophysics Data System (ADS)

    Ito, Keita; Toko, Kaoru; Takeda, Yukiharu; Saitoh, Yuji; Oguchi, Tamio; Suemasu, Takashi; Kimura, Akio

    2015-05-01

    We performed x-ray absorption spectroscopy (XAS) and x-ray magnetic circular dichroism (XMCD) measurements at Fe L2,3 and N K-edges for Fe4N epitaxial films grown by molecular beam epitaxy. In order to clarify the element specific local electronic structure of Fe4N, we compared experimentally obtained XAS and XMCD spectra with those simulated by a combination of a first-principles calculation and Fermi's golden rule. We revealed that the shoulders observed at Fe L2,3-edges in the XAS and XMCD spectra were due to the electric dipole transition from the Fe 2p core-level to the hybridization state generated by σ* anti-bonding between the orbitals of N 2p at the body-centered site and Fe 3d on the face-centered (II) sites. Thus, the observed shoulders were attributed to the local electronic structure of Fe atoms at II sites. As to the N K-edge, the line shape of the obtained spectra was explained by the dipole transition from the N 1s core-level to the hybridization state formed by π* and σ* anti-bondings between the Fe 3d and N 2p orbitals. This hybridization plays an important role in featuring the electronic structures and physical properties of Fe4N.

  17. Local electronic states of Fe{sub 4}N films revealed by x-ray absorption spectroscopy and x-ray magnetic circular dichroism

    SciTech Connect

    Ito, Keita; Toko, Kaoru; Suemasu, Takashi; Takeda, Yukiharu; Saitoh, Yuji; Oguchi, Tamio; Kimura, Akio

    2015-05-21

    We performed x-ray absorption spectroscopy (XAS) and x-ray magnetic circular dichroism (XMCD) measurements at Fe L{sub 2,3} and N K-edges for Fe{sub 4}N epitaxial films grown by molecular beam epitaxy. In order to clarify the element specific local electronic structure of Fe{sub 4}N, we compared experimentally obtained XAS and XMCD spectra with those simulated by a combination of a first-principles calculation and Fermi's golden rule. We revealed that the shoulders observed at Fe L{sub 2,3}-edges in the XAS and XMCD spectra were due to the electric dipole transition from the Fe 2p core-level to the hybridization state generated by σ* anti-bonding between the orbitals of N 2p at the body-centered site and Fe 3d on the face-centered (II) sites. Thus, the observed shoulders were attributed to the local electronic structure of Fe atoms at II sites. As to the N K-edge, the line shape of the obtained spectra was explained by the dipole transition from the N 1s core-level to the hybridization state formed by π* and σ* anti-bondings between the Fe 3d and N 2p orbitals. This hybridization plays an important role in featuring the electronic structures and physical properties of Fe{sub 4}N.

  18. L-Edge X-ray Absorption Spectroscopy of Dilute Systems Relevant to Metalloproteins Using an X-ray Free-Electron Laser

    PubMed Central

    Mitzner, Rolf; Rehanek, Jens; Kern, Jan; Gul, Sheraz; Hattne, Johan; Taguchi, Taketo; Alonso-Mori, Roberto; Tran, Rosalie; Weniger, Christian; Schröder, Henning; Quevedo, Wilson; Laksmono, Hartawan; Sierra, Raymond G.; Han, Guangye; Lassalle-Kaiser, Benedikt; Koroidov, Sergey; Kubicek, Katharina; Schreck, Simon; Kunnus, Kristjan; Brzhezinskaya, Maria; Firsov, Alexander; Minitti, Michael P.; Turner, Joshua J.; Moeller, Stefan; Sauter, Nicholas K.; Bogan, Michael J.; Nordlund, Dennis; Schlotter, William F.; Messinger, Johannes; Borovik, Andrew; Techert, Simone; de Groot, Frank M. F.; Föhlisch, Alexander; Erko, Alexei; Bergmann, Uwe; Yachandra, Vittal K.; Wernet, Philippe; Yano, Junko

    2013-01-01

    L-edge spectroscopy of 3d transition metals provides important electronic structure information and has been used in many fields. However, the use of this method for studying dilute aqueous systems, such as metalloenzymes, has not been prevalent because of severe radiation damage and the lack of suitable detection systems. Here we present spectra from a dilute Mn aqueous solution using a high-transmission zone-plate spectrometer at the Linac Coherent Light Source (LCLS). The spectrometer has been optimized for discriminating the Mn L-edge signal from the overwhelming O K-edge background that arises from water and protein itself, and the ultrashort LCLS X-ray pulses can outrun X-ray induced damage. We show that the deviations of the partial-fluorescence yield-detected spectra from the true absorption can be well modeled using the state-dependence of the fluorescence yield, and discuss implications for the application of our concept to biological samples. PMID:24466387

  19. X-ray photoelectron spectroscopy and luminescent properties of Y2O3:Bi3+ phosphor

    NASA Astrophysics Data System (ADS)

    Jafer, R. M.; Coetsee, E.; Yousif, A.; Kroon, R. E.; Ntwaeaborwa, O. M.; Swart, H. C.

    2015-03-01

    X-ray photoelectron spectroscopy (XPS) results provided proof for the blue and green emission of Bi3+ in the Y2O3:Bi3+ phosphor. The Y2O3:Bi3+ phosphor was successfully prepared by the combustion process during the investigation of down-conversion materials for Si solar cell application. The X-ray diffraction (XRD) patterns indicated that a single-phase cubic crystal structure with the Ia3 space group was formed. X-ray photoelectron spectroscopy (XPS) showed that the Bi3+ ion replaces the Y3+ ion in two different coordination sites in the Y2O3 crystal structure. The O 1s peak shows five peaks, two which correlate with the O2- ion in Y2O3 in the two different sites, two which correlate with O2- in Bi2O3 in the two different sites and the remaining peak relates to hydroxide. The Y 3d spectrum shows two peaks for the Y3+ ion in the Y2O3 structure in two different sites and the Bi 4f spectrum shows the Bi3+ ion in the two different sites in Bi2O3. The photoluminescence (PL) results showed three broad emission bands in the blue and green regions under ultraviolet excitation, which were also present for panchromatic cathodoluminescence (CL) results. These three peaks have maxima at ∼3.4, 3.0 and 2.5 eV. The PL emission ∼3.0 eV (blue emission) showed two excitation bands centered at ∼3.7 and 3.4 eV while the PL emission at ∼2.5 eV (green emission) showed a broad excitation band from ∼4 to 3.4 eV. The panchromatic CL images were obtained for selected wavelengths at (2.99 ± 0.08) eV (for blue emission) and (2.34 ± 0.06) eV (for green emission). These luminescence results correlate with the XPS results that show that there are two different Bi3+ sites in the host lattice.

  20. Americium characterization by X-ray fluorescence and absorption spectroscopy in plutonium uranium mixed oxide

    SciTech Connect

    Degueldre, Claude Cozzo, Cedric; Martin, Matthias; Grolimund, Daniel; Mieszczynski, Cyprian

    2013-06-01

    Plutonium uranium mixed oxide (MOX) fuels are currently used in nuclear reactors. The actinides in these fuels need to be analyzed after irradiation for assessing their behaviour with regard to their environment and the coolant. In this work the study of the atomic structure and next-neighbour environment of Am in the (Pu,U)O₂ lattice in an irradiated (60 MW d kg⁻¹) MOX sample was performed employing micro-X-ray fluorescence (µ-XRF) and micro-X-ray absorption fine structure (µ-XAFS) spectroscopy. The chemical bonds, valences and stoichiometry of Am (~0.66 wt%) are determined from the experimental data gained for the irradiated fuel material examined in its peripheral zone (rim) of the fuel. In the irradiated sample Am builds up as Am³⁺ species within an [AmO₈]¹³⁻ coordination environment (e.g. >90%) and no (<10%) Am(IV) or (V) can be detected in the rim zone. The occurrence of americium dioxide is avoided by the redox buffering activity of the uranium dioxide matrix. - Graphical abstract: Americium LIII XAFS spectra recorded for the irradiated MOX sub-sample in the rim zone for a 300 μm×300 μm beam size area investigated over six scans of 4 h. The records remain constant during multi-scan. The analysis of the XAFS signal shows that Am is found as trivalent in the UO₂ matrix. This analytical work shall open the door of very challenging analysis (speciation of fission product and actinides) in irradiated nuclear fuels. - Highlights: • Americium was characterized by microX-ray absorption spectroscopy in irradiated MOX fuel. • The americium redox state as determined from XAS data of irradiated fuel material was Am(III). • In the sample, the Am³⁺ face an AmO₈¹³⁻coordination environment in the (Pu,U)O₂ matrix. • The americium dioxide is reduced by the uranium dioxide matrix.