WorldWideScience

Sample records for time-resolved powder x-ray

  1. Dehydrogenation kinetics of pure and nickel-doped magnesium hydride investigated by in situ time-resolved powder X-ray diffraction

    DEFF Research Database (Denmark)

    Jensen, T.R.; Andreasen, A.; Vegge, Tejs

    2006-01-01

    The dehydrogenation kinetics of pure and nickel (Ni)-doped (2w/w%) magnesium hydride (MgH2) have been investigated by in situ time-resolved powder X-ray diffraction (PXD). Deactivated samples, i.e. air exposed, are investigated in order to focus on the effect of magnesium oxide (MgO) surface layers......, which might be unavoidable for magnesium (Mg)-based storage media for mobile applications. A curved position-sensitive detector covering 120 degrees in 20 and a rotating anode X-ray source provide a time resolution of 45 s and up to 90 powder pattems collected during an experiment under isothermal...... by the Johnson-Mehi-Avrami formalism in order to derive rate constants at different temperatures. The apparent activation energies for dehydrogenation of pure and Ni-doped magnesium hydride were E-A approximate to 300 and 250 kJ/mol, respectively. Differential scanning calorimetry gave, E-A = 270 k...

  2. An x-ray detector for time-resolved studies

    International Nuclear Information System (INIS)

    Rodricks, B.; Brizard, C.; Clarke, R.; Lowe, W.

    1992-01-01

    The development of ultrahigh-brightness x-ray sources makes time-resolved x-ray studies more and more feasible. Improvements in x-ray optics components are also critical for obtaining the appropriate beam for a particular type of experiment. Moreover, fast parallel detectors will be essential in order to exploit the combination of high intensity x-ray sources and novel optics for time-resolved experiments. A CCD detector with a time resolution of microseconds has been developed at the Advanced Photon Source (APS). This detector is fully programmable using CAMAC electronics and a Micro Vax computer. The techniques of time-resolved x-ray studies, which include scattering, microradiography, microtomography, stroboscopy, etc., can be applied to a range of phenomena (including rapid thermal annealing, surface ordering, crystallization, and the kinetics of phase transition) in order to understand these time-dependent microscopic processes. Some of these applications will be illustrated by recent results performed at synchrotrons. New powerful x-ray sources now under construction offer the opportunity to apply innovative approaches in time-resolved work

  3. Time-resolved suprathermal x-rays

    International Nuclear Information System (INIS)

    Lee, P.H.Y.; Rosen, M.D.

    1978-01-01

    Temporally resolved x-ray spectra in the range of 1 to 20 keV have been obtained from gold disk targets irradiated by 1.06 μm laser pulses from the Argus facility. The x-ray streak camera used for the measurement has been calibrated for streak speed and dynamic range by using an air-gap Fabry-Perot etalon, and the instrument response has been calibrated using a multi-range monoenergetic x-ray source. The experimental results indicate that we are able to observe the ''hot'' x-ray temperature evolve in time and that the experimentally observed values can be qualitatively predicted by LASNEX code computations when the inhibited transport model is used

  4. Time-Resolved Hard X-Ray Spectrometer

    International Nuclear Information System (INIS)

    Kenneth Moya; Ian McKennaa; Thomas Keenana; Michael Cuneob

    2007-01-01

    Wired array studies are being conducted at the SNL Z accelerator to maximize the x-ray generation for inertial confinement fusion targets and high energy density physics experiments. An integral component of these studies is the characterization of the time-resolved spectral content of the x-rays. Due to potential spatial anisotropy in the emitted radiation, it is also critical to diagnose the time-evolved spectral content in a space-resolved manner. To accomplish these two measurement goals, we developed an x-ray spectrometer using a set of high-speed detectors (silicon PIN diodes) with a collimated field-of-view that converged on a 1-cm-diameter spot at the pinch axis. Spectral discrimination is achieved by placing high Z absorbers in front of these detectors. We built two spectrometers to permit simultaneous different angular views of the emitted radiation. Spectral data have been acquired from recent Z shots for the radial and polar views. UNSPEC1 has been adapted to analyze and unfold the measured data to reconstruct the x-ray spectrum. The unfold operator code, UFO2, is being adapted for a more comprehensive spectral unfolding treatment

  5. Time-resolved materials science opportunities using synchrotron x-ray sources

    International Nuclear Information System (INIS)

    Larson, B.C.; Tischler, J.Z.

    1995-06-01

    The high brightness, high intensity, and pulsed time-structure of synchrotron sources provide new opportunities for time-resolved x-ray diffraction investigations. With third generation synchrotron sources coming on line, high brilliance and high brightness are now available in x-ray beams with the highest flux. In addition to the high average flux, the instantaneous flux available in synchrotron beams is greatly enhanced by the pulsed time structure, which consists of short bursts of x-rays that are separated by ∼tens to hundreds of nanoseconds. Time-resolved one- and two-dimensional position sensitive detection techniques that take advantage of synchrotron radiation for materials science x-ray diffraction investigations are presented, and time resolved materials science applications are discussed in terms of recent diffraction and spectroscopy results and materials research opportunities

  6. Time-resolved x-ray diagnostics

    International Nuclear Information System (INIS)

    Lyons, P.B.

    1981-01-01

    Techniques for time-resolved x-ray diagnostics will be reviewed with emphasis on systems utilizing x-ray diodes or scintillators. System design concerns for high-bandwidth (> 1 GHz) diagnostics will be emphasized. The limitations of a coaxial cable system and a technique for equalizing to improve bandwidth of such a system will be reviewed. Characteristics of new multi-GHz amplifiers will be presented. An example of a complete operational system on the Los Alamos Helios laser will be presented which has a bandwidth near 3 GHz over 38 m of coax. The system includes the cable, an amplifier, an oscilloscope, and a digital camera readout

  7. On the theory of time-resolved x-ray diffraction

    DEFF Research Database (Denmark)

    Henriksen, Niels Engholm; Møller, Klaus Braagaard

    2008-01-01

    We derive the basic theoretical formulation for X-ray diffraction with pulsed fields, using a fully quantized description of light and matter. Relevant time scales are discussed for coherent as well as incoherent X-ray pulses, and we provide expressions to be used for calculation...... of the experimental diffraction signal for both types of X-ray sources. We present a simple analysis of time-resolved X-ray scattering for direct bond breaking in diatomic molecules. This essentially analytical approach highlights the relation between the signal and the time-dependent quantum distribution...

  8. Time-resolved x-ray line diagnostics of laser-produced plasmas

    International Nuclear Information System (INIS)

    Kauffman, R.L.; Matthews, D.L.; Kilkenny, J.D.; Lee, R.W.

    1982-11-01

    We have examined the underdense plasma conditions of laser irradiated disks using K x-rays from highly ionized ions. A 900 ps laser pulse of 0.532 μm light is used to irradiate various Z disks which have been doped with low concentrations of tracer materials. The tracers, whose Z's range from 13 to 22, are chosen so that their K x-ray spectrum is sensitive to typical underdense plasma temperatures and densities. Spectra are measured using a time-resolved crystal spectrograph recording the time history of the x-ray spectrum. A spatially-resolved, time-integrated crystal spectrograph also monitors the x-ray lines. Large differences in Al spectra are observed when the host plasms is changed from SiO 2 to PbO or In. Spectra will be presented along with preliminary analysis of the data

  9. Time-resolved x-ray line diagnostics of laser-produced plasmas

    International Nuclear Information System (INIS)

    Kauffman, R.L.; Matthews, D.L.; Kilkenny, J.D.; Lee, R.W.

    1982-01-01

    We have examined the underdense plasma conditions of laser irradiated disks using K x-rays from highly ionized ions. A 900 ps laser pulse of 0.532 μm light is used to irradiate various Z disks which have been doped with low concentrations of tracer materials. The tracers whose Z's range from 13 to 22 are chosen so that their K x-ray spectrum is sensitive to typical underdense plasma temperatures and densities. Spectra are measured using a time-resolved crystal spectrograph recording the time history of the x-ray spectrum. A spatially-resolved, time-integrated crystal spectrograph also monitors the x-ray lines. Large differences in Al spectra are observed when the host plasma is changed from SiO 2 to PbO or In. Spectra will be presented along with preliminary analysis of the data

  10. Watching proteins function with time-resolved x-ray crystallography

    Science.gov (United States)

    Šrajer, Vukica; Schmidt, Marius

    2017-09-01

    Macromolecular crystallography was immensely successful in the last two decades. To a large degree this success resulted from use of powerful third generation synchrotron x-ray sources. An expansive database of more than 100 000 protein structures, of which many were determined at resolution better than 2 Å, is available today. With this achievement, the spotlight in structural biology is shifting from determination of static structures to elucidating dynamic aspects of protein function. A powerful tool for addressing these aspects is time-resolved crystallography, where a genuine biological function is triggered in the crystal with a goal of capturing molecules in action and determining protein kinetics and structures of intermediates (Schmidt et al 2005a Methods Mol. Biol. 305 115-54, Schmidt 2008 Ultrashort Laser Pulses in Biology and Medicine (Berlin: Springer) pp 201-41, Neutze and Moffat 2012 Curr. Opin. Struct. Biol. 22 651-9, Šrajer 2014 The Future of Dynamic Structural Science (Berlin: Springer) pp 237-51). In this approach, short and intense x-ray pulses are used to probe intermediates in real time and at room temperature, in an ongoing reaction that is initiated synchronously and rapidly in the crystal. Time-resolved macromolecular crystallography with 100 ps time resolution at synchrotron x-ray sources is in its mature phase today, particularly for studies of reversible, light-initiated reactions. The advent of the new free electron lasers for hard x-rays (XFELs; 5-20 keV), which provide exceptionally intense, femtosecond x-ray pulses, marks a new frontier for time-resolved crystallography. The exploration of ultra-fast events becomes possible in high-resolution structural detail, on sub-picosecond time scales (Tenboer et al 2014 Science 346 1242-6, Barends et al 2015 Science 350 445-50, Pande et al 2016 Science 352 725-9). We review here state-of-the-art time-resolved crystallographic experiments both at synchrotrons and XFELs. We also outline

  11. Time resolved x-ray photography of a dense plasma focus

    International Nuclear Information System (INIS)

    Burnett, J.C.; Meyer, J.; Rankin, G.

    1977-01-01

    The temporal development of the hot plasma in a dense plasma focus is studied by x-ray streak photography of approximately 2 ns resolution time. It is shown that initially a uniform x-ray emitting pinch plasma is formed which subsequently cools down until x-ray emission stops after approximately 50 ns. At a time of around 100 ns after initial x-ray emission coinciding with the break-up time of the pinch a second burst of x-rays is observed coming from small localized regions. The observations are compared with results obtained from time-resolved shadow and schlieren photography of a similar dense focus discharge. (author)

  12. Time-resolved X-ray studies using third generation synchrotron radiation sources

    International Nuclear Information System (INIS)

    Mills, D.M.

    1991-10-01

    The third generation, high-brilliance, hard x-ray, synchrotron radiation (SR) sources currently under construction (ESRF at Grenoble, France; APS at Argonne, Illinois; and SPring-8 at Harima, Japan) will usher in a new era of x-ray experimentation for both physical and biological sciences. One of the most exciting areas of experimentation will be the extension of x-ray scattering and diffraction techniques to the study of transient or time-evolving systems. The high repetition rate, short-pulse duration, high brilliance, and variable spectral bandwidth of these sources make them ideal for x-ray time-resolved studies. The temporal properties (bunch length, interpulse period, etc.) of these new sources will be summarized. Finally, the scientific potential and the technological challenges of time-resolved x-ray scattering from these new sources will be described. 13 refs., 4 figs

  13. Watching proteins function with time-resolved x-ray crystallography

    Energy Technology Data Exchange (ETDEWEB)

    Šrajer, Vukica; Schmidt, Marius

    2017-08-22

    Macromolecular crystallography was immensely successful in the last two decades. To a large degree this success resulted from use of powerful third generation synchrotron x-ray sources. An expansive database of more than 100 000 protein structures, of which many were determined at resolution better than 2 Å, is available today. With this achievement, the spotlight in structural biology is shifting from determination of static structures to elucidating dynamic aspects of protein function. A powerful tool for addressing these aspects is time-resolved crystallography, where a genuine biological function is triggered in the crystal with a goal of capturing molecules in action and determining protein kinetics and structures of intermediates (Schmidt et al 2005a Methods Mol. Biol. 305 115–54, Schmidt 2008 Ultrashort Laser Pulses in Biology and Medicine (Berlin: Springer) pp 201–41, Neutze and Moffat 2012 Curr. Opin. Struct. Biol. 22 651–9, Šrajer 2014 The Future of Dynamic Structural Science (Berlin: Springer) pp 237–51). In this approach, short and intense x-ray pulses are used to probe intermediates in real time and at room temperature, in an ongoing reaction that is initiated synchronously and rapidly in the crystal. Time-resolved macromolecular crystallography with 100 ps time resolution at synchrotron x-ray sources is in its mature phase today, particularly for studies of reversible, light-initiated reactions. The advent of the new free electron lasers for hard x-rays (XFELs; 5–20 keV), which provide exceptionally intense, femtosecond x-ray pulses, marks a new frontier for time-resolved crystallography. The exploration of ultra-fast events becomes possible in high-resolution structural detail, on sub-picosecond time scales (Tenboer et al 2014 Science 346 1242–6, Barends et al 2015 Science 350 445–50, Pande et al 2016 Science 352 725–9). We review here state-of-the-art time-resolved crystallographic experiments both at synchrotrons and XFELs. We

  14. Watching proteins function with time-resolved x-ray crystallography

    International Nuclear Information System (INIS)

    Šrajer, Vukica; Schmidt, Marius

    2017-01-01

    Macromolecular crystallography was immensely successful in the last two decades. To a large degree this success resulted from use of powerful third generation synchrotron x-ray sources. An expansive database of more than 100 000 protein structures, of which many were determined at resolution better than 2 Å, is available today. With this achievement, the spotlight in structural biology is shifting from determination of static structures to elucidating dynamic aspects of protein function. A powerful tool for addressing these aspects is time-resolved crystallography, where a genuine biological function is triggered in the crystal with a goal of capturing molecules in action and determining protein kinetics and structures of intermediates (Schmidt et al 2005a Methods Mol. Biol . 305 115–54, Schmidt 2008 Ultrashort Laser Pulses in Biology and Medicine (Berlin: Springer) pp 201–41, Neutze and Moffat 2012 Curr. Opin. Struct. Biol . 22 651–9, Šrajer 2014 The Future of Dynamic Structural Science (Berlin: Springer) pp 237–51). In this approach, short and intense x-ray pulses are used to probe intermediates in real time and at room temperature, in an ongoing reaction that is initiated synchronously and rapidly in the crystal. Time-resolved macromolecular crystallography with 100 ps time resolution at synchrotron x-ray sources is in its mature phase today, particularly for studies of reversible, light-initiated reactions. The advent of the new free electron lasers for hard x-rays (XFELs; 5–20 keV), which provide exceptionally intense, femtosecond x-ray pulses, marks a new frontier for time-resolved crystallography. The exploration of ultra-fast events becomes possible in high-resolution structural detail, on sub-picosecond time scales (Tenboer et al 2014 Science 346 1242–6, Barends et al 2015 Science 350 445–50, Pande et al 2016 Science 352 725–9). We review here state-of-the-art time-resolved crystallographic experiments both at synchrotrons and XFELs

  15. Theory of time-resolved inelastic x-ray diffraction

    DEFF Research Database (Denmark)

    Lorenz, Ulf; Møller, Klaus Braagaard; Henriksen, Niels Engholm

    2010-01-01

    Starting from a general theory of time-resolved x-ray scattering, we derive a convenient expression for the diffraction signal based on a careful analysis of the relevant inelastic scattering processes. We demonstrate that the resulting inelastic limit applies to a wider variety of experimental...... conditions than similar, previously derived formulas, and it directly allows the application of selection rules when interpreting diffraction signals. Furthermore, we present a simple extension to systems simultaneously illuminated by x rays and a laser beam....

  16. Flash X-Ray (FXR) Accelerator Optimization Electronic Time-Resolved Measurement of X-Ray Source Size

    International Nuclear Information System (INIS)

    Jacob, J; Ong, M; Wargo, P

    2005-01-01

    Lawrence Livermore National Laboratory (LLNL) is currently investigating various approaches to minimize the x-ray source size on the Flash X-Ray (FXR) linear induction accelerator in order to improve x-ray flux and increase resolution for hydrodynamic radiography experiments. In order to effectively gauge improvements to final x-ray source size, a fast, robust, and accurate system for measuring the spot size is required. Timely feedback on x-ray source size allows new and improved accelerator tunes to be deployed and optimized within the limited run-time constraints of a production facility with a busy experimental schedule; in addition, time-resolved measurement capability allows the investigation of not only the time-averaged source size, but also the evolution of the source size, centroid position, and x-ray dose throughout the 70 ns beam pulse. Combined with time-resolved measurements of electron beam parameters such as emittance, energy, and current, key limiting factors can be identified, modeled, and optimized for the best possible spot size. Roll-bar techniques are a widely used method for x-ray source size measurement, and have been the method of choice at FXR for many years. A thick bar of tungsten or other dense metal with a sharp edge is inserted into the path of the x-ray beam so as to heavily attenuate the lower half of the beam, resulting in a half-light, half-dark image as seen downstream of the roll-bar; by measuring the width of the transition from light to dark across the edge of the roll-bar, the source size can be deduced. For many years, film has been the imaging medium of choice for roll-bar measurements thanks to its high resolution, linear response, and excellent contrast ratio. Film measurements, however, are fairly cumbersome and require considerable setup and analysis time; moreover, with the continuing trend towards all-electronic measurement systems, film is becoming increasingly difficult and expensive to procure. Here, we shall

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

    Directory of Open Access Journals (Sweden)

    L. Miaja-Avila

    2015-03-01

    Full Text Available 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.

  18. Time-resolved X-ray transmission microscopy on magnetic microstructures

    International Nuclear Information System (INIS)

    Puzic, Aleksandar

    2007-01-01

    Three excitation schemes were designed for stroboscopic imaging of magnetization dynamics with time-resolved magnetic transmission X-ray microscopy (TR-MTXM). These techniques were implemented into two types of X-ray microscopes, namely the imaging transmission X-ray microscope (ITXM) and the scanning transmission X-ray microscope (STXM), both installed at the electron storage ring of the Advanced Light Source in Berkeley, USA. Circular diffraction gratings (Fresnel zone plates) used in both microscopes as focusing and imaging elements presently allow for lateral resolution down to 30 nm. Magnetic imaging is performed by using the X-ray magnetic circular dichroism (XMCD) as element specific contrast mechanism. The developed methods have been successfully applied to the experimental investigation of magnetization dynamics in ferromagnetic microstructures. A temporal resolution well below 100 ps was achieved. A conventional pump-probe technique was implemented first. The dynamic response of the magnetization excited by a broadband pulsed magnetic field was imaged spatially resolved using focused X-ray flashes. As a complementary method, the spatially resolved ferromagnetic resonance (SR-FMR) technique was developed for experimental study of magnetization dynamics in the frequency domain. As a third excitation mode, the burst excitation was implemented. The performance and efficiency of the developed methods have been demonstrated by imaging the local magnetization dynamics in laterally patterned ferromagnetic thin-film elements and three-layer stacks. The existence of multiple eigenmodes in the excitation spectra of ferromagnetic microstructures has been verified by using the pump-probe technique. Magnetostatic spin waves were selectively excited and detected with a time resolution of 50 ps using the SR-FMR technique. Thorough analysis of 20 in most cases independently prepared samples has verified that vortices which exhibit a low-amplitude switching of their core

  19. Direct observation of ultrafast atomic motion using time-resolved X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Shymanovich, U.

    2007-11-13

    This thesis is dedicated to the study of the atomic motion in laser irradiated solids on a picosecond to subpicosecond time-scale using the time-resolved X-ray diffraction technique. In the second chapter, the laser system, the laser-plasma based X-ray source and the experimental setup for optical pump / X-ray probe measurements were presented. Chapter 3 is devoted to the characterization and comparison of different types of X-ray optics. Chapter 4 presented the time-resolved X-ray diffraction experiments performed for this thesis. The first two sections of this chapter discuss the measurements of initially unexpected strain-induced transient changes of the integrated reflectivity of the X-ray probe beam. The elimination of the strain-induced transient changes of the integrated reflectivity represented an important prerequisite to perform the study of lattice heating in Germanium after femtosecond optical excitation by measuring the transient Debye-Waller effect. The third section describes the investigations of acoustic waves upon ultrafast optical excitation and discusses the two different pressure contributions driving them: the thermal and the electronic ones. (orig.)

  20. Direct observation of ultrafast atomic motion using time-resolved X-ray diffraction

    International Nuclear Information System (INIS)

    Shymanovich, U.

    2007-01-01

    This thesis is dedicated to the study of the atomic motion in laser irradiated solids on a picosecond to subpicosecond time-scale using the time-resolved X-ray diffraction technique. In the second chapter, the laser system, the laser-plasma based X-ray source and the experimental setup for optical pump / X-ray probe measurements were presented. Chapter 3 is devoted to the characterization and comparison of different types of X-ray optics. Chapter 4 presented the time-resolved X-ray diffraction experiments performed for this thesis. The first two sections of this chapter discuss the measurements of initially unexpected strain-induced transient changes of the integrated reflectivity of the X-ray probe beam. The elimination of the strain-induced transient changes of the integrated reflectivity represented an important prerequisite to perform the study of lattice heating in Germanium after femtosecond optical excitation by measuring the transient Debye-Waller effect. The third section describes the investigations of acoustic waves upon ultrafast optical excitation and discusses the two different pressure contributions driving them: the thermal and the electronic ones. (orig.)

  1. Thin film growth studies using time-resolved x-ray scattering

    Science.gov (United States)

    Kowarik, Stefan

    2017-02-01

    Thin-film growth is important for novel functional materials and new generations of devices. The non-equilibrium growth physics involved is very challenging, because the energy landscape for atomic scale processes is determined by many parameters, such as the diffusion and Ehrlich-Schwoebel barriers. We review the in situ real-time techniques of x-ray diffraction (XRD), x-ray growth oscillations and diffuse x-ray scattering (GISAXS) for the determination of structure and morphology on length scales from Å to µm. We give examples of time resolved growth experiments mainly from molecular thin film growth, but also highlight growth of inorganic materials using molecular beam epitaxy (MBE) and electrochemical deposition from liquids. We discuss how scaling parameters of rate equation models and fundamental energy barriers in kinetic Monte Carlo methods can be determined from fits of the real-time x-ray data.

  2. Time-resolved X-ray PIV technique for diagnosing opaque biofluid flow with insufficient X-ray fluxes.

    Science.gov (United States)

    Jung, Sung Yong; Park, Han Wook; Kim, Bo Heum; Lee, Sang Joon

    2013-05-01

    X-ray imaging is used to visualize the biofluid flow phenomena in a nondestructive manner. A technique currently used for quantitative visualization is X-ray particle image velocimetry (PIV). Although this technique provides a high spatial resolution (less than 10 µm), significant hemodynamic parameters are difficult to obtain under actual physiological conditions because of the limited temporal resolution of the technique, which in turn is due to the relatively long exposure time (~10 ms) involved in X-ray imaging. This study combines an image intensifier with a high-speed camera to reduce exposure time, thereby improving temporal resolution. The image intensifier amplifies light flux by emitting secondary electrons in the micro-channel plate. The increased incident light flux greatly reduces the exposure time (below 200 µs). The proposed X-ray PIV system was applied to high-speed blood flows in a tube, and the velocity field information was successfully obtained. The time-resolved X-ray PIV system can be employed to investigate blood flows at beamlines with insufficient X-ray fluxes under specific physiological conditions. This method facilitates understanding of the basic hemodynamic characteristics and pathological mechanism of cardiovascular diseases.

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

    Directory of Open Access Journals (Sweden)

    Majed Chergui

    2016-05-01

    Full Text Available 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.

  4. Time-resolved hard x-ray studies using third-generation synchrotron radiation sources (abstract)

    International Nuclear Information System (INIS)

    Mills, D.M.

    1992-01-01

    The third-generation, high-brilliance, synchrotron radiation sources currently under construction will usher in a new era of x-ray research in the physical, chemical, and biological sciences. One of the most exciting areas of experimentation will be the extension of static x-ray scattering and diffraction techniques to the study of transient or time-evolving systems. The high repetition rate, short-pulse duration, high-brilliance, variable spectral bandwidth, and large particle beam energies of these sources make them ideal for hard x-ray, time-resolved studies. The primary focus of this presentation will be on the novel instrumentation required for time-resolved studies such as optics which can increase the flux on the sample or disperse the x-ray beam, detectors and electronics for parallel data collection, and methods for altering the natural time structure of the radiation. This work is supported by the U.S. Department of Energy, BES-Materials Science, under Contract No. W-31-109-ENG-38

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

    Science.gov (United States)

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

    2009-11-01

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

  6. Time-resolved protein nano-crystallography using an X-ray free-electron laser

    International Nuclear Information System (INIS)

    Aquila, Andrew; Hunter, Mark S.; Fromme, Petra; Fromme, Raimund; Grotjohann, Ingo; Doak, R. Bruce; Kirian, Richard A.; Schmidt, Kevin E.; Wang, Xiaoyu; Weierstall, Uwe; Spence, John C.H.; White, Thomas A.; Caleman, Carl; DePonte, Daniel P.; Fleckenstein, Holger; Gumprecht, Lars; Liang, Mengning; Martin, Andrew V.; Schulz, Joachim; Stellato, Francesco; Stern, Stephan; Barty, Anton; Andreasson, Jakob; Davidsson, Jan; Hajdu, Janos; Maia, Filipe R.N.C.; Seibert, M. Marvin; Timneanu, Nicusor; Arnlund, David; Johansson, Linda; Malmerberg, Erik; Neutze, Richard; Bajt, Sasa; Barthelmess, Miriam; Graafsma, Heinz; Hirsemann, Helmut; Wunderer, Cornelia; Barends, Thomas R.M.; Foucar, Lutz; Krasniqi, Faton; Lomb, Lukas; Rolles, Daniel; Schlichting, Ilme; Schmidt, Carlo; Bogan, Michael J.; Hampton, Christina Y.; Sierra, Raymond; Starodub, Dmitri; Bostedt, Christoph; Bozek, John D.; Messerschmidt, Marc; Williams, Garth J.; Bottin, Herve

    2012-01-01

    We demonstrate the use of an X-ray free electron laser synchronized with an optical pump laser to obtain X-ray diffraction snapshots from the photo-activated states of large membrane protein complexes in the form of nano-crystals flowing in a liquid jet. Light-induced changes of Photosystem I-Ferredoxin co-crystals were observed at time delays of 5 to 10 μs after excitation. The result correlates with the microsecond kinetics of electron transfer from Photosystem I to ferredoxin. The undocking process that follows the electron transfer leads to large rearrangements in the crystals that will terminally lead to the disintegration of the crystals. We describe the experimental setup and obtain the first time resolved femtosecond serial X-ray crystallography results from an irreversible photo-chemical reaction at the Linac Coherent Light Source. This technique opens the door to time-resolved structural studies of reaction dynamics in biological systems. (authors)

  7. Time-resolved pump-probe X-ray absorption fine structure spectroscopy of Gaq3

    International Nuclear Information System (INIS)

    Dicke, Benjamin

    2013-01-01

    of Gaq 3 was analyzed and presents one of the first time-resolved measurements at PETRA III. In addition to pump-probe XAFS spectroscopy, different phases of Gaq 3 and Alq 3 in form of powder, crystal, film and solution were analyzed by means of UV-VIS and fluorescence spectroscopy. Electronic and optical differences of the molecules related to the particular form could be revealed. Gaq 3 in benzyl alcohol solution and Gaq 3 in crystalline form exhibit very similar optical features, indicating similar structural properties. The various preparation techniques used to obtain the sample forms are presented in this thesis. Analyzing the differences among the diverse sample forms helps to answer the question on how the conclusions extracted from sample systems in liquid form can be transferred to the ones in crystal form or film form, the latter appearing in organic light emitting diodes. The future goal of this research project is the direct measurement of the excited state structure of Alq 3 as well as Gaq 3 , and similar sample systems by time-resolved X-ray crystallography. The sample crystals have to fulfill specific requirements especially for the laser induced photoexcitation process. In this thesis a newly developed preparation method for low roughness singe crystal slices is presented. These crystal slices can be used for future perspective time-resolved X-ray crystallography experiments.

  8. Time-resolved x-ray laser induced photoelectron spectroscopy of isochoric heated copper

    International Nuclear Information System (INIS)

    Nelson, A.J.; Dunn, J.; Hunter, J.; Widmann, K.

    2005-01-01

    Time-resolved x-ray photoelectron spectroscopy is used to probe the nonsteady-state evolution of the valence band electronic structure of laser heated ultrathin (50 nm) copper. A metastable phase is studied using a 527 nm wavelength 400 fs laser pulse containing 0.1-2.5 mJ laser energy focused in a large 500x700 μm 2 spot to create heated conditions of 0.07-1.8x10 12 W cm -2 intensity. Valence band photoemission spectra are presented showing the changing occupancy of the Cu 3d level with heating are presented. These picosecond x-ray laser induced time-resolved photoemission spectra of laser-heated ultrathin Cu foil show dynamic changes in the electronic structure. The ultrafast nature of this technique lends itself to true single-state measurements of shocked and heated materials

  9. High resolution time- and 2-dimensional space-resolved x-ray imaging of plasmas at NOVA

    International Nuclear Information System (INIS)

    Landen, O.L.

    1992-01-01

    A streaked multiple pinhole camera technique, first used by P. Choi et al. to record time- and 2-D space-resolved soft X-ray images of plasma pinches, has been implemented on laser plasmas at NOVA. The instrument is particularly useful for time-resolved imaging of small sources ( 2.5 key imaging, complementing the existing 1--3 key streaked X-ray microscope capabilities at NOVA

  10. Application of combined multivariate techniques for the description of time-resolved powder X-ray diffraction data

    Czech Academy of Sciences Publication Activity Database

    Taris, A.; Grosso, M.; Brundu, M.; Guida, V.; Viani, Alberto

    2017-01-01

    Roč. 50, č. 2 (2017), s. 451-461 ISSN 1600-5767 R&D Projects: GA MŠk(CZ) LO1219 Keywords : in situ X-ray powder diffraction * amorphous content * chemically bonded ceramic s * statistical total correlation spectroscopy * multivariate curve resolution Subject RIV: JJ - Other Materials OBOR OECD: Materials engineering Impact factor: 2.495, year: 2016 http://journals.iucr.org/j/issues/2017/02/00/ap5006/index.html

  11. Evaluating scintillator performance in time-resolved hard X-ray studies at synchrotron light sources

    International Nuclear Information System (INIS)

    Rutherford, Michael E.; Chapman, David J.; White, Thomas G.; Drakopoulos, Michael; Rack, Alexander; Eakins, Daniel E.

    2016-01-01

    Scintillator performance in time-resolved, hard, indirect detection X-ray studies on the sub-microsecond timescale at synchrotron light sources is reviewed, modelled and examined experimentally. LYSO:Ce is found to be the only commercially available crystal suitable for these experiments. The short pulse duration, small effective source size and high flux of synchrotron radiation is ideally suited for probing a wide range of transient deformation processes in materials under extreme conditions. In this paper, the challenges of high-resolution time-resolved indirect X-ray detection are reviewed in the context of dynamic synchrotron experiments. In particular, the discussion is targeted at two-dimensional integrating detector methods, such as those focused on dynamic radiography and diffraction experiments. The response of a scintillator to periodic synchrotron X-ray excitation is modelled and validated against experimental data collected at the Diamond Light Source (DLS) and European Synchrotron Radiation Facility (ESRF). An upper bound on the dynamic range accessible in a time-resolved experiment for a given bunch separation is calculated for a range of scintillators. New bunch structures are suggested for DLS and ESRF using the highest-performing commercially available crystal LYSO:Ce, allowing time-resolved experiments with an interframe time of 189 ns and a maximum dynamic range of 98 (6.6 bits)

  12. Evaluating scintillator performance in time-resolved hard X-ray studies at synchrotron light sources

    Energy Technology Data Exchange (ETDEWEB)

    Rutherford, Michael E.; Chapman, David J.; White, Thomas G. [Imperial College London, London (United Kingdom); Drakopoulos, Michael [Diamond Light Source, I12 Joint Engineering, Environmental, Processing (JEEP) Beamline, Didcot, Oxfordshire (United Kingdom); Rack, Alexander [European Synchrotron Radiation Facility, Grenoble (France); Eakins, Daniel E., E-mail: d.eakins@imperial.ac.uk [Imperial College London, London (United Kingdom)

    2016-03-24

    Scintillator performance in time-resolved, hard, indirect detection X-ray studies on the sub-microsecond timescale at synchrotron light sources is reviewed, modelled and examined experimentally. LYSO:Ce is found to be the only commercially available crystal suitable for these experiments. The short pulse duration, small effective source size and high flux of synchrotron radiation is ideally suited for probing a wide range of transient deformation processes in materials under extreme conditions. In this paper, the challenges of high-resolution time-resolved indirect X-ray detection are reviewed in the context of dynamic synchrotron experiments. In particular, the discussion is targeted at two-dimensional integrating detector methods, such as those focused on dynamic radiography and diffraction experiments. The response of a scintillator to periodic synchrotron X-ray excitation is modelled and validated against experimental data collected at the Diamond Light Source (DLS) and European Synchrotron Radiation Facility (ESRF). An upper bound on the dynamic range accessible in a time-resolved experiment for a given bunch separation is calculated for a range of scintillators. New bunch structures are suggested for DLS and ESRF using the highest-performing commercially available crystal LYSO:Ce, allowing time-resolved experiments with an interframe time of 189 ns and a maximum dynamic range of 98 (6.6 bits)

  13. Ultrafast Structural Dynamics in InSb Probed by Time-Resolved X-Ray Diffraction

    International Nuclear Information System (INIS)

    Chin, A.H.; Shank, C.V.; Chin, A.H.; Schoenlein, R.W.; Shank, C.V.; Glover, T.E.; Leemans, W.P.; Balling, P.

    1999-01-01

    Ultrafast structural dynamics in laser-perturbed InSb are studied using time-resolved x-ray diffraction with a novel femtosecond x-ray source. We report the first observation of a delay in the onset of lattice expansion, which we attribute to energy relaxation processes and lattice strain propagation. In addition, we observe direct indications of ultrafast disordering on a subpicosecond time scale. copyright 1999 The American Physical Society

  14. Time-resolved soft x-ray absorption setup using multi-bunch operation modes at synchrotrons

    International Nuclear Information System (INIS)

    Stebel, L.; Sigalotti, P.; Ressel, B.; Cautero, G.; Malvestuto, M.; Capogrosso, V.; Bondino, F.; Magnano, E.; Parmigiani, F.

    2011-01-01

    Here, we report on a novel experimental apparatus for performing time-resolved soft x-ray absorption spectroscopy in the sub-ns time scale using non-hybrid multi-bunch mode synchrotron radiation. The present setup is based on a variable repetition rate Ti:sapphire laser (pump pulse) synchronized with the ∼500 MHz x-ray synchrotron radiation bunches and on a detection system that discriminates and singles out the significant x-ray photon pulses by means of a custom made photon counting unit. The whole setup has been validated by measuring the time evolution of the L 3 absorption edge during the melting and the solidification of a Ge single crystal irradiated by an intense ultrafast laser pulse. These results pave the way for performing synchrotron time-resolved experiments in the sub-ns time domain with variable repetition rate exploiting the full flux of the synchrotron radiation.

  15. Developments in time-resolved x-ray research at APS beamline 7ID

    Energy Technology Data Exchange (ETDEWEB)

    Walko, D. A., E-mail: d-walko@anl.gov; Adams, B. W.; Doumy, G.; Dufresne, E. M.; Li, Yuelin; March, A. M.; Sandy, A. R.; Wang, Jin; Wen, Haidan; Zhu, Yi [Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439 (United States)

    2016-07-27

    The 7ID beamline of the Advanced Photon Source (APS) is dedicated to time-resolved research using x-ray imaging, scattering, and spectroscopy techniques. Time resolution is achieved via gated detectors and/or mechanical choppers in conjunction with the time structure of the x-ray beam. Three experimental hutches allow for a wide variety of experimental setups. Major areas of research include atomic, molecular, and optical physics; chemistry; condensed matter physics in the bulk, thin film, and surface regimes; and fluid-spray dynamics. Recent developments in facilities at 7ID include a high-power, high-repetition-rate picosecond laser to complement the 1 kHz ultrafast laser. For the ultrafast laser, a newly commissioned optical parametric amplifier provides pump wavelength from 0.2 to 15 µm with energy per pulse up to 200 µJ. A nanodiffraction station has also been commissioned, using Fresnel zone-plate optics to achieve a focused x-ray spot of 300 nm. This nanoprobe is not only used to spatially resolve the evolution of small features in samples after optical excitation, but also has been combined with an intense THz source to study material response under ultrafast electric fields.

  16. Difference structures from time-resolved small-angle and wide-angle x-ray scattering

    Science.gov (United States)

    Nepal, Prakash; Saldin, D. K.

    2018-05-01

    Time-resolved small-angle x-ray scattering/wide-angle x-ray scattering (SAXS/WAXS) is capable of recovering difference structures directly from difference SAXS/WAXS curves. It does so by means of the theory described here because the structural changes in pump-probe detection in a typical time-resolved experiment are generally small enough to be confined to a single residue or group in close proximity which is identified by a method akin to the difference Fourier method of time-resolved crystallography. If it is assumed, as is usual with time-resolved structures, that the moved atoms lie within the residue, the 100-fold reduction in the search space (assuming a typical protein has about 100 residues) allows the exaction of the structure by a simulated annealing algorithm with a huge reduction in computing time and leads to a greater resolution by varying the positions of atoms only within that residue. This reduction in the number of potential moved atoms allows us to identify the actual motions of the individual atoms. In the case of a crystal, time-resolved calculations are normally performed using the difference Fourier method, which is, of course, not directly applicable to SAXS/WAXS. The method developed in this paper may be thought of as a substitute for that method which allows SAXS/WAXS (and hence disordered molecules) to also be used for time-resolved structural work.

  17. A synchrotron radiation camera and data acquisition system for time resolved x-ray scattering studies

    International Nuclear Information System (INIS)

    Bordas, J.; Koch, M.H.J.; Clout, P.N.; Dorrington, E.; Boulin, C.; Gabriel, A.

    1980-01-01

    Until recently, time resolved measurements of x-ray scattering patterns have not been feasible because laboratory x-ray sources were too weak and detectors unavailable. Recent developments in both these fields have changed the situation, and it is now possible to follow changes in x-ray scattering patterns with a time resolution of a few ms. The apparatus used to achieve this is described and some examples from recent biological experiments are given. (author)

  18. Visualizing a protein quake with time-resolved X-ray scattering at a free-electron laser

    DEFF Research Database (Denmark)

    Arnlund, David; Johansson, Linda C.; Wickstrand, Cecilia

    2014-01-01

    We describe a method to measure ultrafast protein structural changes using time-resolved wide-angle X-ray scattering at an X-ray free-electron laser. We demonstrated this approach using multiphoton excitation of the Blastochloris viridis photosynthetic reaction center, observing an ultrafast glob...

  19. Time-resolved x-ray spectra of laser irradiated high-Z targets

    International Nuclear Information System (INIS)

    Lee, P.H.Y.; Attwood, D.T.; Boyle, M.J.; Campbell, E.M.; Coleman, L.C.; Kornblum, H.N.

    1977-01-01

    Recent results obtained by using the Livermore 15 psec x-ray streak camera to record x-ray emission from laser-irradiated high-z targets in the 1-20 keV range are reported. Nine to eleven K-edge filter channels were used for the measurements. In the lower energy channels, a dynamic range of x-ray emission intensity of better than three orders of magnitude have been recorded. Data will be presented which describe temporally and spectrally resolved x-ray spectra of gold disk targets irradiated by laser pulses from the Argus facility, including the temporal evolution of the superthermal x-ray tail

  20. Introducing a standard method for experimental determination of the solvent response in laser pump, x-ray probe time-resolved wide-angle x-ray scattering experiments on systems in solution

    DEFF Research Database (Denmark)

    Kjær, Kasper Skov; Brandt van Driel, Tim; Kehres, Jan

    2013-01-01

    In time-resolved laser pump, X-ray probe wide-angle X-ray scattering experiments on systems in solution the structural response of the system is accompanied by a solvent response. The solvent response is caused by reorganization of the bulk solvent following the laser pump event, and in order...... response-the solvent term-experimentally when applying laser pump, X-ray probe time-resolved wide-angle X-ray scattering. The solvent term describes difference scattering arising from the structural response of the solvent to changes in the hydrodynamic parameters: pressure, temperature and density. We...... is demonstrated to exhibit first order behaviour with respect to the amount of energy deposited in the solution. We introduce a standardized method for recording solvent responses in laser pump, X-ray probe time-resolved X-ray wide-angle scattering experiments by using dye mediated solvent heating. Furthermore...

  1. Time-resolved soft x-ray spectra from laser-produced Cu plasma

    International Nuclear Information System (INIS)

    Cone, K.V.; Dunn, J.; Baldis, H.A.; May, M.J.; Purvis, M.A.; Scott, H.A.; Schneider, M.B.

    2012-01-01

    The volumetric heating of a thin copper target has been studied with time resolved x-ray spectroscopy. The copper target was heated from a plasma produced using the Lawrence Livermore National Laboratory's Compact Multipulse Terrawatt (COMET) laser. A variable spaced grating spectrometer coupled to an x-ray streak camera measured soft x-ray emission (800-1550 eV) from the back of the copper target to characterize the bulk heating of the target. Radiation hydrodynamic simulations were modeled in 2-dimensions using the HYDRA code. The target conditions calculated by HYDRA were post-processed with the atomic kinetics code CRETIN to generate synthetic emission spectra. A comparison between the experimental and simulated spectra indicates the presence of specific ionization states of copper and the corresponding electron temperatures and ion densities throughout the laser-heated copper target.

  2. Time-resolved measurements of supersonic fuel sprays using synchrotron X-rays.

    Science.gov (United States)

    Powell, C F; Yue, Y; Poola, R; Wang, J

    2000-11-01

    A time-resolved radiographic technique has been developed for probing the fuel distribution close to the nozzle of a high-pressure single-hole diesel injector. The measurement was made using X-ray absorption of monochromatic synchrotron-generated radiation, allowing quantitative determination of the fuel distribution in this optically impenetrable region with a time resolution of better than 1 micros. These quantitative measurements constitute the most detailed near-nozzle study of a fuel spray to date.

  3. A system for time-resolved x-ray diffraction and its application to muscle contraction

    International Nuclear Information System (INIS)

    Amemiya, Yoshiyuki; Hashizume, Hiroo.

    1979-01-01

    A data-collection system has been built which permits time-resolved studies of X-ray diffraction diagrams obtained from contracting muscle on millisecond time scale. The system consists of a linear delay-line position sensitive proportional counter (PSPC), a special data transfer unit and an on-line computer. The PSPC used with a mirror-monochromator camera can detect equatorial reflections from stimulated muscle in a total exposure time of a few seconds. Time-resolved data-collection is achieved by stimulating muscle at a regular time interval, dividing a complete cycle of muscle contraction into many successive time slices and accumulating in computer memory X-ray data for each time slice from many repeated cycles of stimulation. The performances of the system have been demonstrated by recording equatorial reflections from frog skeletal muscle during isometric and isotonic twitch with a time resolution of 25 ms. (author)

  4. Modern trends in x-ray powder diffraction

    International Nuclear Information System (INIS)

    Goebel, H.E.; Snyder, R.L.

    1985-01-01

    The revival of interest in X-ray powder diffraction, being quoted as a metamorphosis from the 'ugly duckling' to a 'beautiful swan', can be attributed to a number of modern developments in instrumentation and evaluation software. They result in faster data collection, improved accuracy and resolution, and better detectability of minor phases. The ease of data evaluation on small computers coupled direct to the instrument allows convenient execution of previously tedious and time-consuming off-line tasks like qualitative and quantitative analysis, characterization of microcrystalline properties, indexing, and lattice-constant refinements, as well as structure refinements or even exploration of new crystal structures. Powder diffraction has also progressed from an isolated analytical laboratory method to an in situ technique for analysing solid-state reactions or for the on-stream control of industrial processes. The paper surveys these developments and their real and potential applications, and tries to emphasize new trends that are regarded as important steps for the further progress of X-ray powder diffraction

  5. Time Resolved X-Ray Scattering of molecules in Solution

    DEFF Research Database (Denmark)

    Brandt van Driel, Tim

    The dissertation describes the use of Time-Resolved X-ray Diffuse Scattering (TR-XDS) to study photo-induced structural changes in molecules in solution. The application of the technique is exemplified with experiments on two bimetallic molecules. The main focus is on the data-flow and process......)42+ obtained at European Synchrotron Radiation Facility (ESRF) are presented to exemplify TR-XDS at synchrotrons. Similarly, measurements on Ir2(dimen)42+ are used to show the XFEL data-flow and how it deviates from the prior. A method to identify and account for systematic fluctuations...

  6. Time-resolved X-ray photoelectron spectroscopy techniques for the study of interfacial charge dynamics

    Energy Technology Data Exchange (ETDEWEB)

    Neppl, Stefan, E-mail: sneppl@lbl.gov; Gessner, Oliver

    2015-04-15

    Highlights: • Ultrafast interfacial charge transfer is probed with atomic site specificity. • Femtosecond X-ray photoelectron spectroscopy using a free electron laser. • Efficient and flexible picosecond X-ray photoelectron pump–probe scheme using synchrotron radiation. - Abstract: X-ray photoelectron spectroscopy (XPS) is one of the most powerful techniques to quantitatively analyze the chemical composition and electronic structure of surfaces and interfaces in a non-destructive fashion. Extending this technique into the time domain has the exciting potential to shed new light on electronic and chemical dynamics at surfaces by revealing transient charge configurations with element- and site-specificity. Here, we describe prospects and challenges that are associated with the implementation of picosecond and femtosecond time-resolved X-ray photoelectron spectroscopy at third-generation synchrotrons and X-ray free-electron lasers, respectively. In particular, we discuss a series of laser-pump/X-ray-probe photoemission experiments performed on semiconductor surfaces, molecule-semiconductor interfaces, and films of semiconductor nanoparticles that demonstrate the high sensitivity of time-resolved XPS to light-induced charge carrier generation, diffusion and recombination within the space charge layers of these materials. Employing the showcase example of photo-induced electronic dynamics in a dye-sensitized semiconductor system, we highlight the unique possibility to probe heterogeneous charge transfer dynamics from both sides of an interface, i.e., from the perspective of the molecular electron donor and the semiconductor acceptor, simultaneously. Such capabilities will be crucial to improve our microscopic understanding of interfacial charge redistribution and associated chemical dynamics, which are at the heart of emerging energy conversion, solar fuel generation, and energy storage technologies.

  7. Time-resolved measurements of supersonic fuel sprays using synchrotron x-rays

    International Nuclear Information System (INIS)

    Powell, C.F.; Yue, Y.; Poola, R.; Wang, J.

    2000-11-01

    A time-resolved radiographic technique has been developed for probing the fuel distribution close to the nozzle of a high-pressure single-hole diesel injector. The measurement was made using X-ray absorption of monochromatic synchrotron-generated radiation, allowing quantitative determination of the fuel distribution in this optically impenetrable region with a time resolution of better than 1 μs. These quantitative measurements constitute the most detailed near-nozzle study of a fuel spray to date

  8. Evaluating scintillator performance in time-resolved hard X-ray studies at synchrotron light sources.

    Science.gov (United States)

    Rutherford, Michael E; Chapman, David J; White, Thomas G; Drakopoulos, Michael; Rack, Alexander; Eakins, Daniel E

    2016-05-01

    The short pulse duration, small effective source size and high flux of synchrotron radiation is ideally suited for probing a wide range of transient deformation processes in materials under extreme conditions. In this paper, the challenges of high-resolution time-resolved indirect X-ray detection are reviewed in the context of dynamic synchrotron experiments. In particular, the discussion is targeted at two-dimensional integrating detector methods, such as those focused on dynamic radiography and diffraction experiments. The response of a scintillator to periodic synchrotron X-ray excitation is modelled and validated against experimental data collected at the Diamond Light Source (DLS) and European Synchrotron Radiation Facility (ESRF). An upper bound on the dynamic range accessible in a time-resolved experiment for a given bunch separation is calculated for a range of scintillators. New bunch structures are suggested for DLS and ESRF using the highest-performing commercially available crystal LYSO:Ce, allowing time-resolved experiments with an interframe time of 189 ns and a maximum dynamic range of 98 (6.6 bits).

  9. Versatile, reprogrammable area pixel array detector for time-resolved synchrotron x-ray applications

    Energy Technology Data Exchange (ETDEWEB)

    Gruner, Sol [Cornell Univ., Ithaca, NY (United States)

    2010-05-01

    The final technical report for DOE grant DE-SC0004079 is presented. The goal of the grant was to perform research, development and application of novel imaging x-ray detectors so as to effectively utilize the high intensity and brightness of the national synchrotron radiation facilities to enable previously unfeasible time-resolved x-ray research. The report summarizes the development of the resultant imaging x-ray detectors. Two types of detector platforms were developed: The first is a detector platform (called a Mixed-Mode Pixel Array Detector, or MM-PAD) that can image continuously at over a thousand images per second while maintaining high efficiency for wide dynamic range signals ranging from 1 to hundreds of millions of x-rays per pixel per image. Research on an even higher dynamic range variant is also described. The second detector platform (called the Keck Pixel Array Detector) is capable of acquiring a burst of x-ray images at a rate of millions of images per second.

  10. Static and time-resolved 10-1000 keV x-ray imaging detector options for NIF

    International Nuclear Information System (INIS)

    Landen, O.L.; Bell, P.M.; McDonald, J.W.; Park, H.-S.; Weber, F.; Moody, J.D.; Lowry, M.E.; Stewart, R.E.

    2004-01-01

    High energy (>10 keV) x-ray self-emission imaging and radiography will be essential components of many NIF high energy density physics experiments. In preparation for such experiments, we have evaluated the pros and cons of various static [x-ray film, bare charge-coupled device (CCD), and scintillator + CCD] and time-resolved (streaked and gated) 10-1000 keV detectors

  11. Probing Photoinduced Structural Phase Transitions by Fast or Ultra-Fast Time-Resolved X-Ray Diffraction

    Science.gov (United States)

    Cailleau, Hervé Collet, Eric; Buron-Le Cointe, Marylise; Lemée-Cailleau, Marie-Hélène Koshihara, Shin-Ya

    A new frontier in the field of structural science is the emergence of the fast and ultra-fast X-ray science. Recent developments in time-resolved X-ray diffraction promise direct access to the dynamics of electronic, atomic and molecular motions in condensed matter triggered by a pulsed laser irradiation, i.e. to record "molecular movies" during the transformation of matter initiated by light pulse. These laser pump and X-ray probe techniques now provide an outstanding opportunity for the direct observation of a photoinduced structural phase transition as it takes place. The use of X-ray short-pulse of about 100ps around third-generation synchrotron sources allows structural investigations of fast photoinduced processes. Other new X-ray sources, such as laser-produced plasma ones, generate ultra-short pulses down to 100 fs. This opens the way to femtosecond X-ray crystallography, but with rather low X-ray intensities and more limited experimental possibilities at present. However this new ultra-fast science rapidly progresses around these sources and new large-scale projects exist. It is the aim of this contribution to overview the state of art and the perspectives of fast and ultra-fast X-ray scattering techniques to study photoinduced phase transitions (here, the word ultra-fast is used for sub-picosecond time resolution). In particular we would like to largely present the contribution of crystallographic methods in comparison with optical methods, such as pump-probe reflectivity measurements, the reader being not necessary familiar with X-ray scattering. Thus we want to present which type of physical information can be obtained from the positions of the Bragg peaks, their intensity and their shape, as well as from the diffuse scattering beyond Bragg peaks. An important physical feature is to take into consideration the difference in nature between a photoinduced phase transition and conventional homogeneous photoinduced chemical or biochemical processes where

  12. Time-resolved X-ray transmission microscopy on magnetic microstructures; Zeitaufloesende Roentgentransmissionsmikroskopie an magnetischen Mikrostrukturen

    Energy Technology Data Exchange (ETDEWEB)

    Puzic, Aleksandar

    2007-10-23

    Three excitation schemes were designed for stroboscopic imaging of magnetization dynamics with time-resolved magnetic transmission X-ray microscopy (TR-MTXM). These techniques were implemented into two types of X-ray microscopes, namely the imaging transmission X-ray microscope (ITXM) and the scanning transmission X-ray microscope (STXM), both installed at the electron storage ring of the Advanced Light Source in Berkeley, USA. Circular diffraction gratings (Fresnel zone plates) used in both microscopes as focusing and imaging elements presently allow for lateral resolution down to 30 nm. Magnetic imaging is performed by using the X-ray magnetic circular dichroism (XMCD) as element specific contrast mechanism. The developed methods have been successfully applied to the experimental investigation of magnetization dynamics in ferromagnetic microstructures. A temporal resolution well below 100 ps was achieved. A conventional pump-probe technique was implemented first. The dynamic response of the magnetization excited by a broadband pulsed magnetic field was imaged spatially resolved using focused X-ray flashes. As a complementary method, the spatially resolved ferromagnetic resonance (SR-FMR) technique was developed for experimental study of magnetization dynamics in the frequency domain. As a third excitation mode, the burst excitation was implemented. The performance and efficiency of the developed methods have been demonstrated by imaging the local magnetization dynamics in laterally patterned ferromagnetic thin-film elements and three-layer stacks. The existence of multiple eigenmodes in the excitation spectra of ferromagnetic microstructures has been verified by using the pump-probe technique. Magnetostatic spin waves were selectively excited and detected with a time resolution of 50 ps using the SR-FMR technique. Thorough analysis of 20 in most cases independently prepared samples has verified that vortices which exhibit a low-amplitude switching of their core

  13. Guest–Host Interactions Investigated by Time-Resolved X-ray Spectroscopies and Scattering at MHz Rates

    DEFF Research Database (Denmark)

    Haldrup, Martin Kristoffer; Vanko, G.; Gawelda, W.

    2012-01-01

    We have studied the photoinduced low spin (LS) to high spin (HS) conversion of [Fe(bipy)3]2+ in aqueous solution. In a laser pump/X-ray probe synchrotron setup permitting simultaneous, time-resolved X-ray diffuse scattering (XDS) and X-ray spectroscopic measurements at a 3.26 MHz repetition rate...... lifetime, allowing the detection of an ultrafast change in bulk solvent density. An analysis approach directly utilizing the spectroscopic data in the XDS analysis effectively reduces the number of free parameters, and both combined permit extraction of information about the ultrafast structural dynamics...

  14. An iterative method for unfolding time-resolved soft x-ray spectra of laser plasmas

    International Nuclear Information System (INIS)

    Tang Yongjian; Shen Kexi; Xu Hepin

    1991-01-01

    Dante-recorded temporal waveforms have been unfolded by using Fast Fourier transformation (FFT) and the inverted convolution theorem of Fourier analysis. The conversion of the signals to time-dependent soft x-ray spectra is accomplished on the IBM-PC/XT-286 microcomputer system with the code DTSP including SAND II reported by W.N.Mcelory et al.. An amplitude-limited iterative and periodic smoothing technique has been developed in the code DTSP. Time-resolved soft x-ray spectra with sixteen time-cell, and time-dependent radiation, [T R (t)], have been obtained for hohlraum targets irradiated with laser beams (λ = 1.06 μm) on LF-12 in 1989

  15. Particle tracking during Ostwald ripening using time-resolved laboratory X-ray microtomography

    Energy Technology Data Exchange (ETDEWEB)

    Werz, T., E-mail: thomas.werz@uni-ulm.de [Ulm University, Institute of Micro and Nanomaterials, Albert-Einstein-Allee 47, 89081 (Germany); Baumann, M. [Ulm University, Institute of Micro and Nanomaterials, Albert-Einstein-Allee 47, 89081 (Germany); Wolfram, U. [Ulm University, Institute of Orthopaedic Research and Biomechanics, Helmholtzstrasse 14, 89081 (Germany); Krill, C.E. [Ulm University, Institute of Micro and Nanomaterials, Albert-Einstein-Allee 47, 89081 (Germany)

    2014-04-01

    Laboratory X-ray microtomography is investigated as a method for obtaining time-resolved images of microstructural coarsening of the semisolid state of Al–5 wt.% Cu samples during Ostwald ripening. Owing to the 3D imaging capability of tomography, this technique uniquely provides access to the growth rates of individual particles, thereby not only allowing a statistical characterization of coarsening—as has long been possible by conventional metallography—but also enabling quantification of the influence of local environment on particle boundary migration. The latter information is crucial to understanding growth kinetics during Ostwald ripening at high volume fractions of the coarsening phase. Automated image processing and segmentation routines were developed to close gaps in the network of particle boundaries and to track individual particles from one annealing step to the next. The particle tracking success rate places an upper bound of only a few percent on the likelihood of segmentation errors for any given particle. The accuracy of particle size trajectories extracted from the time-resolved tomographic reconstructions is correspondingly high. Statistically averaged coarsening data and individual particle growth rates are in excellent agreement with the results of prior experimental studies and with computer simulations of Ostwald ripening. - Highlights: • Ostwald ripening in Al–5 wt.% Cu measured by laboratory X-ray microtomography • Time-resolved measurement of individual particle growth • Automated segmentation routines developed to close gaps in particle boundary network • Particle growth/shrinkage rates deviate from LSW model prediction.

  16. Picosecond time-resolved laser pump/X-ray probe experiments using a gated single-photon-counting area detector

    DEFF Research Database (Denmark)

    Ejdrup, T.; Lemke, H.T.; Haldrup, Martin Kristoffer

    2009-01-01

    The recent developments in X-ray detectors have opened new possibilities in the area of time-resolved pump/probe X-ray experiments; this article presents the novel use of a PILATUS detector to achieve X-ray pulse duration limited time-resolution at the Advanced Photon Source (APS), USA...... limited time-resolution of 60 ps using the gated PILATUS detector. This is the first demonstration of X-ray pulse duration limited data recorded using an area detector without the use of a mechanical chopper array at the beamline........ The capability of the gated PILATUS detector to selectively detect the signal from a given X-ray pulse in 24 bunch mode at the APS storage ring is demonstrated. A test experiment performed on polycrystalline organic thin films of [alpha]-perylene illustrates the possibility of reaching an X-ray pulse duration...

  17. Time-resolved x-ray diffraction techniques for bulk polycrystalline materials under dynamic loading

    Energy Technology Data Exchange (ETDEWEB)

    Lambert, P. K.; Hustedt, C. J.; Zhao, M.; Ananiadis, A. G.; Hufnagel, T. C. [Department of Materials Science and Engineering, Johns Hopkins University, Baltimore, Maryland 21218 (United States); Vecchio, K. S. [Department of NanoEngineering, University of California San Diego, La Jolla, California 92093 (United States); Huskins, E. L. [Oak Ridge Institute for Science and Education, Oak Ridge, Tennessee 37830 (United States); US Army Research Laboratory, Aberdeen Proving Ground, Aberdeen, Maryland 21005 (United States); Casem, D. T. [US Army Research Laboratory, Aberdeen Proving Ground, Aberdeen, Maryland 21005 (United States); Gruner, S. M. [Department of Physics, Cornell University, Ithaca, New York 14853 (United States); Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, New York 14853 (United States); Kavli Institute at Cornell for Nanoscale Science, Cornell University, Ithaca, New York 14853 (United States); Tate, M. W.; Philipp, H. T.; Purohit, P.; Weiss, J. T. [Department of Physics, Cornell University, Ithaca, New York 14853 (United States); Woll, A. R. [Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, New York 14853 (United States); Kannan, V.; Ramesh, K. T. [Department of Mechanical Engineering, Johns Hopkins University, Baltimore, Maryland 21218 (United States); Kenesei, P.; Okasinski, J. S.; Almer, J. [X-ray Science Division, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

    2014-09-15

    We have developed two techniques for time-resolved x-ray diffraction from bulk polycrystalline materials during dynamic loading. In the first technique, we synchronize a fast detector with loading of samples at strain rates of ∼10{sup 3}–10{sup 4} s{sup −1} in a compression Kolsky bar (split Hopkinson pressure bar) apparatus to obtain in situ diffraction patterns with exposures as short as 70 ns. This approach employs moderate x-ray energies (10–20 keV) and is well suited to weakly absorbing materials such as magnesium alloys. The second technique is useful for more strongly absorbing materials, and uses high-energy x-rays (86 keV) and a fast shutter synchronized with the Kolsky bar to produce short (∼40 μs) pulses timed with the arrival of the strain pulse at the specimen, recording the diffraction pattern on a large-format amorphous silicon detector. For both techniques we present sample data demonstrating the ability of these techniques to characterize elastic strains and polycrystalline texture as a function of time during high-rate deformation.

  18. Time- and wavelength-resolved luminescence evaluation of several types of scintillators using streak camera system equipped with pulsed X-ray source

    Energy Technology Data Exchange (ETDEWEB)

    Furuya, Yuki, E-mail: f.yuki@mail.tagen.tohoku.ac.j [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577 (Japan); Yanagida, Takayuki; Fujimoto, Yutaka; Yokota, Yuui; Kamada, Kei [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577 (Japan); Kawaguchi, Noriaki [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577 (Japan); Research and Development Division, Tokuyama., Co. Ltd., ICR-Building, Minamiyoshinari, Aoba-ku, Sendai (Japan); Ishizu, Sumito [Research and Development Division, Tokuyama., Co. Ltd., ICR-Building, Minamiyoshinari, Aoba-ku, Sendai (Japan); Uchiyama, Koro; Mori, Kuniyoshi [Hamamatsu Photonics K.K., 325-6, Sunayama-cho, Naka-ku, Hamamatsu, Shizuoka 430-8587 (Japan); Kitano, Ken [Vacuum and Optical Instruments, 2-18-18 Shimomaruko, Ota, Tokyo 146-0092 (Japan); Nikl, Martin [Institute of Physics ASCR, Cukrovarnicka 10, Prague 6, 162-53 (Czech Republic); Yoshikawa, Akira [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577 (Japan); NICHe, Tohoku University, 6-6-10 Aoba, Aramaki, Aoba-ku, Sendai 980-8579 (Japan)

    2011-04-01

    To design new scintillating materials, it is very important to understand detailed information about the events, which occurred during the excitation and emission processes under the ionizing radiation excitation. We developed a streak camera system equipped with picosecond pulsed X-ray source to observe time- and wavelength-resolved scintillation events. In this report, we test the performance of this new system using several types of scintillators including bulk oxide/halide crystals, transparent ceramics, plastics and powders. For all samples, the results were consistent with those reported previously. The results demonstrated that the developed system is suitable for evaluation of the scintillation properties.

  19. Time resolved resonant inelastic X-ray scattering: A supreme tool to understand dynamics in solids and molecules

    International Nuclear Information System (INIS)

    Beye, M.; Wernet, Ph.; Schüßler-Langeheine, C.; Föhlisch, A.

    2013-01-01

    Highlights: •The high specificity of RIXS ideally suits time-resolved measurements. •Methods relating to the core hole lifetime cover the low femtosecond regime. •Pump-probe methods are used starting at sub-ps time scales. •FELs and synchrotrons are useful for pump-probe studies. •Examples from solid state dynamics and molecules are discussed. -- Abstract: Dynamics in materials typically involve different degrees of freedom, like charge, lattice, orbital and spin in a complex interplay. Time-resolved resonant inelastic X-ray scattering (RIXS) as a highly selective tool can provide unique insight and follow the details of dynamical processes while resolving symmetries, chemical and charge states, momenta, spin configurations, etc. In this paper, we review examples where the intrinsic scattering duration time is used to study femtosecond phenomena. Free-electron lasers access timescales starting in the sub-ps range through pump-probe methods and synchrotrons study the time scales longer than tens of ps. In these examples, time-resolved resonant inelastic X-ray scattering is applied to solids as well as molecular systems

  20. Diagnostics of underwater electrical wire explosion through a time- and space-resolved hard x-ray source.

    Science.gov (United States)

    Sheftman, D; Shafer, D; Efimov, S; Gruzinsky, K; Gleizer, S; Krasik, Ya E

    2012-10-01

    A time- and space-resolved hard x-ray source was developed as a diagnostic tool for imaging underwater exploding wires. A ~4 ns width pulse of hard x-rays with energies of up to 100 keV was obtained from the discharge in a vacuum diode consisting of point-shaped tungsten electrodes. To improve contrast and image quality, an external pulsed magnetic field produced by Helmholtz coils was used. High resolution x-ray images of an underwater exploding wire were obtained using a sensitive x-ray CCD detector, and were compared to optical fast framing images. Future developments and application of this diagnostic technique are discussed.

  1. Time-resolved soft-x-ray studies of energy transport in layered and planar laser-driven targets

    International Nuclear Information System (INIS)

    Stradling, G.L.

    1982-01-01

    New low-energy x-ray diagnostic techniques are used to explore energy-transport processes in laser heated plasmas. Streak cameras are used to provide 15-psec time-resolution measurements of subkeV x-ray emission. A very thin (50 μg/cm 2 ) carbon substrate provides a low-energy x-ray transparent window to the transmission photocathode of this soft x-ray streak camera. Active differential vacuum pumping of the instrument is required. The use of high-sensitivity, low secondary-electron energy-spread CsI photocathodes in x-ray streak cameras is also described. Significant increases in sensitivity with only a small and intermittant decrease in dynamic range were observed. These coherent, complementary advances in subkeV, time-resolved x-ray diagnostic capability are applied to energy-transport investigations of 1.06-μm laser plasmas. Both solid disk targets of a variety of Z's as well as Be-on-Al layered-disk targets were irradiated with 700-psec laser pulses of selected intensity between 3 x 10 14 W/cm 2 and 1 x 10 15 W/cm 2

  2. Time resolved, 2-D hard X-ray imaging of relativistic electron-beam target interactions on ETA-II

    International Nuclear Information System (INIS)

    Crist, C.E.; Sampayan, S.; Westenskow, G.; Caporaso, G.; Houck, T.; Weir, J.; Trimble, D.; Krogh, M.

    1998-01-01

    Advanced radiographic applications require a constant source size less than 1 mm. To study the time history of a relativistic electron beam as it interacts with a bremsstrahlung converter, one of the diagnostics they use is a multi-frame time-resolved hard x-ray camera. They are performing experiments on the ETA-II accelerator at Lawrence Livermore National Laboratory to investigate details of the electron beam/converter interactions. The camera they are using contains 6 time-resolved images, each image is a 5 ns frame. By starting each successive frame 10 ns after the previous frame, they create a 6-frame movie from the hard x-rays produced from the interaction of the 50-ns electron beam pulse

  3. Studies of nanostructures using time-resolved x-ray excited optical luminescence*

    International Nuclear Information System (INIS)

    Rosenberg, R.A.; Shenoy, G.K.; Smita, S.; Burda, C.; Sham, T.K.

    2004-01-01

    Full text:The scientific community is currently investing a great deal of effort into understanding the physics and chemistry of nanoscale structures. Synchrotron radiation techniques are being used to study the physical, electronic, and magnetic structure of nanosystems, albeit at a relatively large size (greater than 30 nm). A major challenge facing researchers is finding methods that can probe structures of the smallest scale (less than 10 nm). Optical luminescence has been shown to be directly sensitive to structures in this size range due to quantum confinement phenomena. X-ray-excited optical luminescence (XEOL) provides the capability to chemically map the sites responsible for producing low-energy (1-6 eV) fluorescence. By taking advantage of the time structure of the x-ray pulses at the Advanced Photon Source (70 ps wide, 153 ns separation), it also possible to determine the dynamic behavior of the states involved in the luminescence. In this paper we will present results of time-resolved XEOL experiments on various nanostructures including porous silicon, silicon nanowires, and CdSe nanodots

  4. In Situ High Resolution Synchrotron X-Ray Powder Diffraction Studies of Lithium Batteries

    DEFF Research Database (Denmark)

    Amri, Mahrez; Fitch, Andy; Norby, Poul

    2015-01-01

    allowing diffraction information to be obtained from only the active material during battery operation [2]. High resolution synchrotron x-ray powder diffraction technique has been undertaken to obtain detailed structural and compositional information during lithiation/delithiation of commercial LiFePO4...... materials [3]. We report results from the first in situ time resolved high resolution powder diffraction experiments at beamline ID22/31 at the European Synchrotron Radiation Facility, ESRF. We follow the structural changes during charge of commercial LiFePO4 based battery materials using the Rietveld...... method. Conscientious Rietveld analysis shows slight but continuous deviation of lattice parameters from those of the fully stoichiometric end members LiFePO4 and FePO4 indicating a subsequent variation of stoichiometry during cathode delithiation. The application of an intermittent current pulses during...

  5. Time Resolved X-Ray Spot Size Diagnostic

    CERN Document Server

    Richardson, Roger; Falabella, Steven; Guethlein, Gary; Raymond, Brett; Weir, John

    2005-01-01

    A diagnostic was developed for the determination of temporal history of an X-ray spot. A pair of thin (0.5 mm) slits image the x-ray spot to a fast scintillator which is coupled to a fast detector, thus sampling a slice of the X-Ray spot. Two other scintillator/detectors are used to determine the position of the spot and total forward dose. The slit signal is normalized to the dose and the resulting signal is analyzed to get the spot size. The position information is used to compensate for small changes due to spot motion and misalignment. The time resolution of the diagnostic is about 1 ns and measures spots from 0.5 mm to over 3 mm. The theory and equations used to calculate spot size and position are presented, as well as data. The calculations assume a symmetric, Gaussian spot. The spot data is generated by the ETA II accelerator, a 2kA, 5.5 MeV, 60ns electron beam focused on a Tantalum target. The spot generated is typically about 1 mm FWHM. Comparisons are made to an X-ray pinhole camera which images th...

  6. Computational time-resolved and resonant x-ray scattering of strongly correlated materials

    Energy Technology Data Exchange (ETDEWEB)

    Bansil, Arun [Northeastern Univ., Boston, MA (United States)

    2016-11-09

    predominantly decays via Auger processes, thereby providing an internal time-scale, which limits intermediate-state processes to timescales of a few femtoseconds. Accordingly, a number of activities directed at modeling K-, L- and M-edge RIXS in correlated materials were also pursused by our CRT. Our research effort supported by this CMCSN grant substantially advanced the understanding of x-ray scattering processes in the time-domain as well as in the more conventional scattering channels, including time-resolved photoemission, and how such processes can be modeled realistically in complex correlated materials more generally. The modeling of relaxation processes involved in time-domain spectroscopies is important also for understanding photoinduced effects such as energy conversion in photosynthesis and solar cell applications, and thus impacts the basic science for energy needs.

  7. Time resolved fluorescence of cow and goat milk powder

    Science.gov (United States)

    Brandao, Mariana P.; de Carvalho dos Anjos, Virgílio; Bell., Maria José V.

    2017-01-01

    Milk powder is an international dairy commodity. Goat and cow milk powders are significant sources of nutrients and the investigation of the authenticity and classification of milk powder is particularly important. The use of time-resolved fluorescence techniques to distinguish chemical composition and structure modifications could assist develop a portable and non-destructive methodology to perform milk powder classification and determine composition. This study goal is to differentiate milk powder samples from cows and goats using fluorescence lifetimes. The samples were excited at 315 nm and the fluorescence intensity decay registered at 468 nm. We observed fluorescence lifetimes of 1.5 ± 0.3, 6.4 ± 0.4 and 18.7 ± 2.5 ns for goat milk powder; and 1.7 ± 0.3, 6.9 ± 0.2 and 29.9 ± 1.6 ns for cow's milk powder. We discriminate goat and cow powder milk by analysis of variance using Fisher's method. In addition, we employed quadratic discriminant analysis to differentiate the milk samples with accuracy of 100%. Our results suggest that time-resolved fluorescence can provide a new method to the analysis of powder milk and its composition.

  8. An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

    Science.gov (United States)

    Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.; Martin, Aiden A.; Depond, Philip J.; Guss, Gabriel M.; Thampy, Vivek; Fong, Anthony Y.; Weker, Johanna Nelson; Stone, Kevin H.; Tassone, Christopher J.; Kramer, Matthew J.; Toney, Michael F.; Van Buuren, Anthony; Matthews, Manyalibo J.

    2018-05-01

    In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at the Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ˜1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ˜50 × 100 μm area. We also discuss the utility of these measurements for model validation and process improvement.

  9. Time-resolved x-ray diffraction analysis of the experimental dehydration of serpentine at high pressure

    International Nuclear Information System (INIS)

    Inoue, Toru; Yoshimi, Isamu; Yamada, Akihiro; Kikegawa, Takumi

    2009-01-01

    Time-resolved, in situ X-ray diffraction analysis was used to determine the dehydration rate and kinetics of serpentine during experimental dehydration at high pressures. The capsule used comprises a diamond sleeve fitted with Au or Pt lids in order to provide high-quality, time-resolved X-ray diffraction data. Antigorite quickly dehydrated to enstatite + forsterite + fluid within 2 h at 650degC below ∼6 GPa. Avrami modeling of the results and SEM observations of the partially dehydrated sample revealed that the nucleation rate was quite high for enstatite but low for forsterite, showing incubation periods of ∼10 min before appearing. The crystallization of these minerals is controlled largely by the composition of the fluid generated from serpentine dehydration. The dehydration boundary determined below 6 GPa in the present study is consistent with the results of previous phase equilibrium studies. This study indicates that serpentine in a subducting slab dehydrates rapidly below 6 GPa when the slab intersects the dehydration boundary conditions. (author)

  10. Resolve Instrument on X-ray Astronomy Recovery Mission (XARM)

    Science.gov (United States)

    Ishisaki, Y.; Ezoe, Y.; Yamada, S.; Ichinohe, Y.; Fujimoto, R.; Takei, Y.; Yasuda, S.; Ishida, M.; Yamasaki, N. Y.; Maeda, Y.; Tsujimoto, M.; Iizuka, R.; Koyama, S.; Noda, H.; Tamagawa, T.; Sawada, M.; Sato, K.; Kitamoto, S.; Hoshino, A.; Brown, G. V.; Eckart, M. E.; Hayashi, T.; Kelley, R. L.; Kilbourne, C. A.; Leutenegger, M. A.; Mori, H.; Okajima, T.; Porter, F. S.; Soong, Y.; McCammon, D.; Szymkowiak, A. E.

    2018-04-01

    The X-ray Astronomy Recovery Mission (XARM) is a recovery mission of ASTRO-H/Hitomi, which is expected to be launched in Japanese Fiscal Year of 2020 at the earliest. The Resolve instrument on XARM consists of an array of 6 × 6 silicon-thermistor microcalorimeters cooled down to 50 mK and a high-throughput X-ray mirror assembly with the focal length of 5.6 m. Hitomi was launched into orbit in February 2016 and observed several celestial objects, although the operation of Hitomi was terminated in April 2016. The soft X-ray spectrometer (SXS) on Hitomi demonstrated high-resolution X-ray spectroscopy of 5 eV FWHM in orbit for most of the pixels. The Resolve instrument is planned to mostly be a copy of the Hitomi SXS and soft X-ray telescope designs, though several changes are planned based on the lessons learned from Hitomi. We report a brief summary of the SXS performance and the status of the Resolve instrument.

  11. Study Of Soot Growth And Nucleation By A Time-Resolved Synchrotron Radiation Based X-Ray Absorption Method

    National Research Council Canada - National Science Library

    Mitchell, Judith I

    2001-01-01

    This report results from a contract tasking University of Rennes I as follows: The contractor will perform a study of soot growth and nucleation by a time-resolved synchrotron radiation based x-ray absorption method...

  12. Probing the influence of X-rays on aqueous copper solutions using time-resolved in situ combined video/X-ray absorption near-edge/ultraviolet-visible spectroscopy

    NARCIS (Netherlands)

    Mesu, J. Gerbrand; Beale, Andrew M.; de Groot, Frank M. F.; Weckhuysen, Bert M.

    2006-01-01

    Time-resolved in situ video monitoring and ultraviolet-visible spectroscopy in combination with X-ray absorption near-edge spectroscopy (XANES) have been used for the first time in a combined manner to study the effect of synchrotron radiation on a series of homogeneous aqueous copper solutions in a

  13. Time-resolved and position-resolved X-ray spectrometry with a pixelated detector

    Energy Technology Data Exchange (ETDEWEB)

    Sievers, Peter

    2012-12-07

    stability of the applied Bayesian deconvolution method enabled the possibility of performing time-resolved spectrometric measurements. By measuring in ToA mode and in parallel performing a THL scan, it is possible to gain information on both energy and time. This method was then tested for a conventional X-ray tube for measuring the time dependence of the spectrum emitted during the switching-on process of the radiation. As expected, the results showed a relatively long time-dependent change of the spectrum. This method was then applied for proving that a newly developed X-ray source shows a spectral change of the spectrum emitted on a very low time scale only. As this time dependence is much shorter compared to the total pulse duration of the radiation, it is negligible. This result guarantees that both pulse duration and energy can be adjusted independently. This enables further investigations with this new X-ray tube in the field of pulsed radiation and its use for e.g. type tests.

  14. Time-resolved and position-resolved X-ray spectrometry with a pixelated detector

    International Nuclear Information System (INIS)

    Sievers, Peter

    2012-01-01

    stability of the applied Bayesian deconvolution method enabled the possibility of performing time-resolved spectrometric measurements. By measuring in ToA mode and in parallel performing a THL scan, it is possible to gain information on both energy and time. This method was then tested for a conventional X-ray tube for measuring the time dependence of the spectrum emitted during the switching-on process of the radiation. As expected, the results showed a relatively long time-dependent change of the spectrum. This method was then applied for proving that a newly developed X-ray source shows a spectral change of the spectrum emitted on a very low time scale only. As this time dependence is much shorter compared to the total pulse duration of the radiation, it is negligible. This result guarantees that both pulse duration and energy can be adjusted independently. This enables further investigations with this new X-ray tube in the field of pulsed radiation and its use for e.g. type tests.

  15. Computation of X-ray powder diffractograms of cement components ...

    Indian Academy of Sciences (India)

    Computation of X-ray powder diffractograms of cement components and its application to phase analysis and hydration performance of OPC cement. Rohan Jadhav N C Debnath. Volume 34 Issue 5 August 2011 pp 1137- ... Keywords. Portland cement; X-ray diffraction; crystal structure; characterization; Rietveld method.

  16. Time resolved techniques: An overview

    International Nuclear Information System (INIS)

    Larson, B.C.; Tischler, J.Z.

    1990-06-01

    Synchrotron sources provide exceptional opportunities for carrying out time-resolved x-ray diffraction investigations. The high intensity, high angular resolution, and continuously tunable energy spectrum of synchrotron x-ray beams lend themselves directly to carrying out sophisticated time-resolved x-ray scattering measurements on a wide range of materials and phenomena. When these attributes are coupled with the pulsed time-structure of synchrotron sources, entirely new time-resolved scattering possibilities are opened. Synchrotron beams typically consist of sub-nanosecond pulses of x-rays separated in time by a few tens of nanoseconds to a few hundred nanoseconds so that these beams appear as continuous x-ray sources for investigations of phenomena on time scales ranging from hours down to microseconds. Studies requiring time-resolution ranging from microseconds to fractions of a nanosecond can be carried out in a triggering mode by stimulating the phenomena under investigation in coincidence with the x-ray pulses. Time resolution on the picosecond scale can, in principle, be achieved through the use of streak camera techniques in which the time structure of the individual x-ray pulses are viewed as quasi-continuous sources with ∼100--200 picoseconds duration. Techniques for carrying out time-resolved scattering measurements on time scales varying from picoseconds to kiloseconds at present and proposed synchrotron sources are discussed and examples of time-resolved studies are cited. 17 refs., 8 figs

  17. X-ray powder diffraction data on miscellaneous lanthanide compounds

    International Nuclear Information System (INIS)

    Ferguson, I.F.; Hughes, T.E.

    1978-08-01

    Recent work on neutron absorbing materials has produced various new X-ray diffraction powder patterns of compounds of the lanthanides. Various inconsistencies in previously published data have been noted, and accurate measurements have been made of the lattice parameters of the rare earth oxides Sm 2 0 3 , Eu 2 0 3 , Gd 2 0 3 which have the monoclinic rare earth type B- structure, as well as Eu0. These data are recorded for reference. The optimum conditions for obtaining X-ray powder diffraction data from europium compounds are also noted. (author)

  18. Broadband time-resolved elliptical crystal spectrometer for X-ray spectroscopic measurements in laser-produced plasmas

    International Nuclear Information System (INIS)

    Wang Rui-Rong; Jia Guo; Fang Zhi-Heng; Wang Wei; Meng Xiang-Fu; Xie Zhi-Yong; Zhang Fan

    2014-01-01

    The X-ray spectrometer used in high-energy-density plasma experiments generally requires both broad X-ray energy coverage and high temporal, spatial, and spectral resolutions for overcoming the difficulties imposed by the X-ray background, debris, and mechanical shocks. By using an elliptical crystal together with a streak camera, we resolve this issue at the SG-II laser facility. The carefully designed elliptical crystal has a broad spectral coverage with high resolution, strong rejection of the diffuse and/or fluorescent background radiation, and negligible source broadening for extended sources. The spectra that are Bragg reflected (23° < θ < 38°) from the crystal are focused onto a streak camera slit 18 mm long and about 80 μm wide, to obtain a time-resolved spectrum. With experimental measurements, we demonstrate that the quartz(1011) elliptical analyzer at the SG-II laser facility has a single-shot spectral range of (4.64–6.45) keV, a typical spectral resolution of E/ΔE = 560, and an enhanced focusing power in the spectral dimension. For titanium (Ti) data, the lines of interest show a distribution as a function of time and the temporal variations of the He-α and Li-like Ti satellite lines and their spatial profiles show intensity peak red shifts. The spectrometer sensitivity is illustrated with a temporal resolution of better than 25 ps, which satisfies the near-term requirements of high-energy-density physics experiments. (atomic and molecular physics)

  19. Developments in time-resolved high pressure x-ray diffraction using rapid compression and decompression

    International Nuclear Information System (INIS)

    Smith, Jesse S.; Sinogeikin, Stanislav V.; Lin, Chuanlong; Rod, Eric; Bai, Ligang; Shen, Guoyin

    2015-01-01

    Complementary advances in high pressure research apparatus and techniques make it possible to carry out time-resolved high pressure research using what would customarily be considered static high pressure apparatus. This work specifically explores time-resolved high pressure x-ray diffraction with rapid compression and/or decompression of a sample in a diamond anvil cell. Key aspects of the synchrotron beamline and ancillary equipment are presented, including source considerations, rapid (de)compression apparatus, high frequency imaging detectors, and software suitable for processing large volumes of data. A number of examples are presented, including fast equation of state measurements, compression rate dependent synthesis of metastable states in silicon and germanium, and ultrahigh compression rates using a piezoelectric driven diamond anvil cell

  20. X-ray powder diffraction in forensic practice

    Czech Academy of Sciences Publication Activity Database

    Kotrlý, M.; Bezdička, Petr

    2006-01-01

    Roč. 13, č. 3 (2006), s. 153-155 ISSN 1210-8529 R&D Projects: GA MV RN20052005001 Institutional research plan: CEZ:AV0Z40320502 Keywords : X-ray powder microdiffraction * pigments * forensic practice Subject RIV: CA - Inorganic Chemistry

  1. Observation of Structure of Surfaces and Interfaces by Synchrotron X-ray Diffraction: Atomic-Scale Imaging and Time-Resolved Measurements

    Science.gov (United States)

    Wakabayashi, Yusuke; Shirasawa, Tetsuroh; Voegeli, Wolfgang; Takahashi, Toshio

    2018-06-01

    The recent developments in synchrotron optics, X-ray detectors, and data analysis algorithms have enhanced the capability of the surface X-ray diffraction technique. This technique has been used to clarify the atomic arrangement around surfaces in a non-contact and nondestructive manner. An overview of surface X-ray diffraction, from the historical development to recent topics, is presented. In the early stage of this technique, surface reconstructions of simple semiconductors or metals were studied. Currently, the surface or interface structures of complicated functional materials are examined with sub-Å resolution. As examples, the surface structure determination of organic semiconductors and of a one-dimensional structure on silicon are presented. A new frontier is time-resolved interfacial structure analysis. A recent observation of the structure and dynamics of the electric double layer of ionic liquids, and an investigation of the structural evolution in the wettability transition on a TiO2 surface that utilizes a newly designed time-resolved surface diffractometer, are presented.

  2. Atomic motion of resonantly vibrating quartz crystal visualized by time-resolved X-ray diffraction

    International Nuclear Information System (INIS)

    Aoyagi, Shinobu; Osawa, Hitoshi; Sugimoto, Kunihisa; Fujiwara, Akihiko; Takeda, Shoichi; Moriyoshi, Chikako; Kuroiwa, Yoshihiro

    2015-01-01

    Transient atomic displacements during a resonant thickness-shear vibration of AT-cut α-quartz are revealed by time-resolved X-ray diffraction under an alternating electric field. The lattice strain resonantly amplified by the alternating electric field is ∼10 4 times larger than that induced by a static electric field. The resonantly amplified lattice strain is achieved by fast displacements of oxygen anions and collateral resilient deformation of Si−O−Si angles bridging rigid SiO 4 tetrahedra, which efficiently transduce electric energy into elastic energy

  3. Time-resolved X-ray scattering by electronic wave packets: analytic solutions to the hydrogen atom

    DEFF Research Database (Denmark)

    Simmermacher, Mats; Henriksen, Niels Engholm; Møller, Klaus Braagaard

    2017-01-01

    Modern pulsed X-ray sources permit time-dependent measurements of dynamical changes in atoms and molecules via non-resonant scattering. The planning, analysis, and interpretation of such experiments, however, require a firm and elaborated theoretical framework. This paper provides a detailed...... description of time-resolved X-ray scattering by non-stationary electronic wave packets in atomic systems. A consistent application of the Waller-Hartree approximation is discussed and different contributions to the total differential scattering signal are identified and interpreted. Moreover......, it is demonstrated how the scattering signal of wave packets in the hydrogen atom can be expressed analytically. This permits simulations without numerical integration and establishes a benchmark for both efficiency and accuracy. Based on that, scattering patterns of an exemplary wave packet in the hydrogen atom...

  4. Time resolved X-ray micro-diffraction measurements of the dynamic local layer response to electric field in antiferroelectric liquid crystals

    Energy Technology Data Exchange (ETDEWEB)

    Takahashi, Yumiko; Iida, Atuso E-mail: atsuo.iida@kek.jp; Takanishi, Yoichi; Ogasawara, Toyokazu; Takezoe, Hideo

    2001-07-21

    The time-resolved synchrotron X-ray microbeam diffraction experiment has been carried out to reveal the local layer response to the electric field in the antiferroelectric liquid crystal. The X-ray microbeam of a few {mu}m spatial resolution was obtained with Kirkpatrick-Baez optics. The time-resolved small angle diffraction experiment was performed with a time resolution ranging from 10 {mu}s to a few ms. The reversible local layer change between the horizontal chevron and the quasi-bookshelf structure was confirmed by the triangular wave form. The transient layer response for the step form electric field was observed. The layer response closely related with an electric field induced antiferroelectric to ferroelectric phase transition.

  5. Time resolved X-ray micro-diffraction measurements of the dynamic local layer response to electric field in antiferroelectric liquid crystals

    International Nuclear Information System (INIS)

    Takahashi, Yumiko; Iida, Atuso; Takanishi, Yoichi; Ogasawara, Toyokazu; Takezoe, Hideo

    2001-01-01

    The time-resolved synchrotron X-ray microbeam diffraction experiment has been carried out to reveal the local layer response to the electric field in the antiferroelectric liquid crystal. The X-ray microbeam of a few μm spatial resolution was obtained with Kirkpatrick-Baez optics. The time-resolved small angle diffraction experiment was performed with a time resolution ranging from 10 μs to a few ms. The reversible local layer change between the horizontal chevron and the quasi-bookshelf structure was confirmed by the triangular wave form. The transient layer response for the step form electric field was observed. The layer response closely related with an electric field induced antiferroelectric to ferroelectric phase transition

  6. Development of soft x-ray time-resolved photoemission spectroscopy system with a two-dimensional angle-resolved time-of-flight analyzer at SPring-8 BL07LSU

    Energy Technology Data Exchange (ETDEWEB)

    Ogawa, Manami; Yamamoto, Susumu; Nakamura, Fumitaka; Yukawa, Ryu; Fukushima, Akiko; Harasawa, Ayumi; Kakizaki, Akito; Matsuda, Iwao [Institute for Solid State Physics, University of Tokyo, 5-1-5 Kashiwanoha, Chiba 277-8581 (Japan); Kousa, Yuka; Kondoh, Hiroshi [Department of Chemistry, Keio University, Yokohama 223-8522 (Japan); Tanaka, Yoshihito [RIKEN/SPring-8 Center, 1-1-1, Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5148 (Japan)

    2012-02-15

    We have developed a soft x-ray time-resolved photoemission spectroscopy system using synchrotron radiation (SR) at SPring-8 BL07LSU and an ultrashort pulse laser system. Two-dimensional angle-resolved measurements were performed with a time-of-flight-type analyzer. The photoemission spectroscopy system is synchronized to light pulses of SR and laser using a time control unit. The performance of the instrument is demonstrated by mapping the band structure of a Si(111) crystal over the surface Brillouin zones and observing relaxation of the surface photo-voltage effect using the pump (laser) and probe (SR) method.

  7. Direct Observation of Insulin Association Dynamics with Time-Resolved X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Rimmerman, Dolev [Department; Leshchev, Denis [Department; Hsu, Darren J. [Department; Hong, Jiyun [Department; Kosheleva, Irina [Center; Chen, Lin X. [Department; Chemical

    2017-09-05

    Biological functions frequently require protein-protein interactions that involve secondary and tertiary structural perturbation. Here we study protein-protein dissociation and reassociation dynamics in insulin, a model system for protein oligomerization. Insulin dimer dissociation into monomers was induced by a nanosecond temperature-jump (T-jump) of ~8 °C in aqueous solution, and the resulting protein and solvent dynamics were tracked by time-resolved X-ray solution scattering (TRXSS) on time scales of 10 ns to 100 ms. The protein scattering signals revealed the formation of five distinguishable transient species during the association process that deviate from simple two state kinetics. Our results show that the combination of T-jump pump coupled to TRXSS probe allows for direct tracking of structural dynamics in nonphotoactive proteins.

  8. Time-resolved x-ray line emission studies of thermal transport in multiple beam uv-irradiated targets

    International Nuclear Information System (INIS)

    Jaanimagi, P.A.; Henke, B.L.; Delettrez, J.; Richardson, M.C.

    1984-01-01

    Thermal transport in spherical targets irradiated with multiple, nanosecond duration laser beams, has been a topic of much discussion recently. Different inferences on the level of thermal flux inhibition have been drawn from plasma velocity and x-ray spectroscopic diagnostics. We present new measurements of thermal transport on spherical targets made through time-resolved x-ray spectroscopic measurements of the progress of the ablation surface through thin layers of material on the surface of the target. These measurements, made with 6 and 12 uv (351 nm) nanosecond beams from OMEGA, will be compared to previous thermal transport measurements. Transparencies of the conference presentation are given

  9. Time resolved x-ray pinhole photography of compressed laser fusion targets

    International Nuclear Information System (INIS)

    Attwood, D.T.

    1976-01-01

    Use of the Livermore x-ray streak camera to temporally record x-ray pinhole images of laser compressed targets is described. Use is made of specially fabricated composite x-ray pinholes which are near diffraction limited for 6 A x-rays, but easily aligned with a He--Ne laser of 6328 A wavelength. With a 6 μm x-ray pinhole, the overall system can be aligned to 5 μm accuracy and provides implosion characteristics with space--time resolutions of approximately 6 μm and 15 psec. Acceptable criteria for pinhole alignment, requisite x-ray flux, and filter characteristics are discussed. Implosion characteristics are presented from our present experiments with 68 μm diameter glass microshell targets and 0.45 terawatt, 70 psec Nd laser pulses. Final implosion velocities in excess of 3 x 10 7 cm/sec are evident

  10. Nonequilibrium lattice-driven dynamics of stripes in nickelates using time-resolved x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Lee, W.S.; Kung, Y.F.; Moritz, B.; Coslovich, G.; Kaindl, R.A.; Chuang, Y.D.; Moore, R.G.; Lu, D.H.; Kirchmann, P.S.; Robinson, J.S.; Minitti, M.P.; Dakovski, G.; Schlotter, W.F.; Turner, J.J.; Gerber, S.; Sasagawa, T.; Hussain, Z.; Shen, Z.X.; Devereaux, T.P.

    2017-03-13

    We investigate the lattice coupling to the spin and charge orders in the striped nickelate, La 1.75 Sr 0.25 NiO 4 , using time-resolved resonant x-ray scattering. Lattice-driven dynamics of both spin and charge orders are observed when the pump photon energy is tuned to that of an E u bond- stretching phonon. We present a likely scenario for the behavior of the spin and charge order parameters and its implications using a Ginzburg-Landau theory.

  11. A split-beam probe-pump-probe scheme for femtosecond time resolved protein X-ray crystallography

    Directory of Open Access Journals (Sweden)

    Jasper J. van Thor

    2015-01-01

    Full Text Available In order to exploit the femtosecond pulse duration of X-ray Free-Electron Lasers (XFEL operating in the hard X-ray regime for ultrafast time-resolved protein crystallography experiments, critical parameters that determine the crystallographic signal-to-noise (I/σI must be addressed. For single-crystal studies under low absorbed dose conditions, it has been shown that the intrinsic pulse intensity stability as well as mode structure and jitter of this structure, significantly affect the crystallographic signal-to-noise. Here, geometrical parameters are theoretically explored for a three-beam scheme: X-ray probe, optical pump, X-ray probe (or “probe-pump-probe” which will allow experimental determination of the photo-induced structure factor amplitude differences, ΔF, in a ratiometric manner, thereby internally referencing the intensity noise of the XFEL source. In addition to a non-collinear split-beam geometry which separates un-pumped and pumped diffraction patterns on an area detector, applying an additional convergence angle to both beams by focusing leads to integration over mosaic blocks in the case of well-ordered stationary protein crystals. Ray-tracing X-ray diffraction simulations are performed for an example using photoactive yellow protein crystals in order to explore the geometrical design parameters which would be needed. The specifications for an X-ray split and delay instrument that implements both an offset angle and focused beams are discussed, for implementation of a probe-pump-probe scheme at the European XFEL. We discuss possible extension of single crystal studies to serial femtosecond crystallography, particularly in view of the expected X-ray damage and ablation due to the first probe pulse.

  12. Development of a fast pixel array detector for use in microsecond time-resolved x-ray diffraction

    International Nuclear Information System (INIS)

    Barna, S.L.; Gruner, S.M.; Shepherd, J.A.

    1995-01-01

    A large-area pixel x-ray detector is being developed to collect eight successive frames of wide dynamic range two-dimensional images at 200kHz rates. Such a detector, in conjunction with a synchrotron radiation x-ray source, will enable time-resolved x-ray studies of proteins and other materials on time scales which have previously been inaccessible. The detector will consist of an array of fully-depleted 150 micron square diodes connected to a CMOS integrated electronics layer with solder bump-bonding. During each framing period, the current resulting from the x-rays stopped in the diodes is integrated in the electronics layer, and then stored in one of eight storage capacitors underneath the pixel. After the last frame, the capacitors are read out at standard data transmission rates. The detector has been designed for a well-depth of at least 10,000 x-rays (at 20keV), and a noise level of one x-ray. Ultimately, the authors intend to construct a detector with over one million pixels (1024 by 1024). They present the results of their development effort and various features of the design. The electronics design is discussed, with special attention to the performance requirements. The choice and design of the detective diodes, as they relate to x-ray stopping power and charge collection, are presented. An analysis of various methods of bump bonding is also presented. Finally, the authors discuss the possible need for a radiation-blocking layer, to be placed between the electronics and the detective layer, and various methods they have pursued in the construction of such a layer

  13. Applications of a table-top time-resolved luminescence spectrometer with nanosecond soft X-ray pulse excitation

    Czech Academy of Sciences Publication Activity Database

    Brůža, P.; Pánek, D.; Fidler, V.; Benedikt, P.; Čuba, V.; Gbur, T.; Boháček, Pavel; Nikl, Martin

    2014-01-01

    Roč. 61, č. 1 (2014), s. 448-451 ISSN 0018-9499 R&D Projects: GA ČR GA13-09876S Institutional support: RVO:68378271 Keywords : LiCaAlF 6 * luminescence * scintillators * soft x-ray * SrHfO 3 * time-resolved spectroscopy * ZnO :Ga Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.283, year: 2014

  14. Contribution to time resolved X-ray fluence and differential spectra measurement method improvement in 5-200 KeV range. Application to pulsed emission sources

    International Nuclear Information System (INIS)

    Vie, M.

    1983-09-01

    Two types of sensors have been developed to measure locally the time-resolved fluence and differential energetic spectrum of pulsed X-ray in the energy range 5 to 200 keV. Rise time of these sensors is very short (10 ns) in order to permit time-resolved measurements. Fluence sensors have been developed by putting filters in front of detector in order to make sensor response independent of X-ray energy and proportional to X-ray fluence. The energetic differential spectrum was calculated by way of a method similar to the ROSS method but using filters separated within a pair defining adjacent spectral width. A detailed analysis of uncertainties affecting calculated fluence and spectrum has been done [fr

  15. Sub-millisecond time-resolved SAXS using a continuous-flow mixer and X-ray microbeam.

    Science.gov (United States)

    Graceffa, Rita; Nobrega, R Paul; Barrea, Raul A; Kathuria, Sagar V; Chakravarthy, Srinivas; Bilsel, Osman; Irving, Thomas C

    2013-11-01

    Small-angle X-ray scattering (SAXS) is a well established technique to probe the nanoscale structure and interactions in soft matter. It allows one to study the structure of native particles in near physiological environments and to analyze structural changes in response to variations in external conditions. The combination of microfluidics and SAXS provides a powerful tool to investigate dynamic processes on a molecular level with sub-millisecond time resolution. Reaction kinetics in the sub-millisecond time range has been achieved using continuous-flow mixers manufactured using micromachining techniques. The time resolution of these devices has previously been limited, in part, by the X-ray beam sizes delivered by typical SAXS beamlines. These limitations can be overcome using optics to focus X-rays to the micrometer size range providing that beam divergence and photon flux suitable for performing SAXS experiments can be maintained. Such micro-SAXS in combination with microfluidic devices would be an attractive probe for time-resolved studies. Here, the development of a high-duty-cycle scanning microsecond-time-resolution SAXS capability, built around the Kirkpatrick-Baez mirror-based microbeam system at the Biophysics Collaborative Access Team (BioCAT) beamline 18ID at the Advanced Photon Source, Argonne National Laboratory, is reported. A detailed description of the microbeam small-angle-scattering instrument, the turbulent flow mixer, as well as the data acquisition and control and analysis software is provided. Results are presented where this apparatus was used to study the folding of cytochrome c. Future prospects for this technique are discussed.

  16. Soft x-ray resonant magnetic powder diffraction on PrNiO{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Staub, U [Swiss Light Source, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); GarcIa-Fernandez, M [Swiss Light Source, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); Mulders, A M [Department of Applied Physics, Curtin University of Technology, GPO Box U1987, Perth WA 6845 (Australia); Bodenthin, Y [Swiss Light Source, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); MartInez-Lope, M J [Instituto de Ciencia de Materiales de Madrid, CSIC, Cantoblanco, E-28049 Madrid (Spain); Alonso, J A [Instituto de Ciencia de Materiales de Madrid, CSIC, Cantoblanco, E-28049 Madrid (Spain)

    2007-03-07

    We report on the first soft x-ray resonant powder diffraction experiments performed at the Ni L{sub 2,3} edges of PrNiO{sub 3}. The temperature, polarization and energy dependence of the (1/2 0 1/2) reflection indicates a magnetic origin for the signal. This experiment demonstrates that x-ray resonant magnetic powder diffraction can be relatively easily performed in the soft x-ray regime due to the very large enhancement factors at the absorption edges. Such experiments allow us to extract important information on the electronic states of the d shell. Similar results can be anticipated from orbital reflections measured in a powder. (fast track communication)

  17. PLEIADES: A picosecond Compton scattering x-ray source for advanced backlighting and time-resolved material studies

    International Nuclear Information System (INIS)

    Gibson, David J.; Anderson, Scott G.; Barty, Christopher P.J.; Betts, Shawn M.; Booth, Rex; Brown, Winthrop J.; Crane, John K.; Cross, Robert R.; Fittinghoff, David N.; Hartemann, Fred V.; Kuba, Jaroslav; Le Sage, Gregory P.; Slaughter, Dennis R.; Tremaine, Aaron M.; Wootton, Alan J.; Hartouni, Edward P.; Springer, Paul T.; Rosenzweig, James B.

    2004-01-01

    The PLEIADES (Picosecond Laser-Electron Inter-Action for the Dynamical Evaluation of Structures) facility has produced first light at 70 keV. This milestone offers a new opportunity to develop laser-driven, compact, tunable x-ray sources for critical applications such as diagnostics for the National Ignition Facility and time-resolved material studies. The electron beam was focused to 50 μm rms, at 57 MeV, with 260 pC of charge, a relative energy spread of 0.2%, and a normalized emittance of 5 mm mrad horizontally and 13 mm mrad vertically. The scattered 820 nm laser pulse had an energy of 180 mJ and a duration of 54 fs. Initial x rays were captured with a cooled charge-coupled device using a cesium iodide scintillator; the peak photon energy was approximately 78 keV, with a total x-ray flux of 1.3x10 6 photons/shot, and the observed angular distribution found to agree very well with three-dimensional codes. Simple K-edge radiography of a tantalum foil showed good agreement with the theoretical divergence-angle dependence of the x-ray energy. Optimization of the x-ray dose is currently under way, with the goal of reaching 10 8 photons/shot and a peak brightness approaching 10 20 photons/mm 2 /mrad 2 /s/0.1% bandwidth

  18. Structure-activity relationships of heterogeneous catalysts from time-resolved X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Ressler, T.; Jentoft, R.E.; Wienold, J.; Girgsdies, F.; Neisius, T.; Timpe, O.

    2003-01-01

    Knowing the composition and the evolution of the bulk structure of a heterogeneous catalyst under working conditions (in situ) is a pre-requisite for understanding structure-activity relationships. X-ray absorption spectroscopy can be employed to study a catalytically active material in situ. In addition to steady-state investigations, the technique permits experiments with a time-resolution in the sub-second range to elucidate the solid-state kinetics of the reactions involved. Combined with mass spectrometry, the evolution of the short-range order structure of a heterogeneous catalyst, the average valence of the constituent metals, and the phase composition can be obtained. Here we present results obtained from time-resolved studies on the reduction of MoO 3 in propene and in propene and oxygen

  19. Time-Resolved X-Ray Diffraction: The Dynamics of the Chemical Bond

    DEFF Research Database (Denmark)

    Møller, Klaus Braagaard; Henriksen, Niels Engholm

    2012-01-01

    We review the basic theoretical formulation for pulsed X-ray scattering on nonstationary molecular states. Relevant time scales are discussed for coherent as well as incpherent X-ray pulses. The general formalism is applied to a nonstationary diatomic molecule in order to highlight the relation b...

  20. Fourier transform infrared spectrophotometry and X-ray powder ...

    African Journals Online (AJOL)

    This study aimed at demonstrating complementary roles offered by both Fourier transform infrared (FTIR) spectrophotometry and x-ray powder diffraction (XRPD) techniques in characterizing clay size fraction of kaolins. The clay size fraction of kaolin samples obtained from Kgwakgwe, Makoro, Lobatse and Serule kaolin ...

  1. Sub-millisecond time-resolved SAXS using a continuous-flow mixer and X-ray microbeam

    International Nuclear Information System (INIS)

    Graceffa, Rita; Nobrega, R. Paul; Barrea, Raul A.; Kathuria, Sagar V.; Chakravarthy, Srinivas; Bilsel, Osman; Irving, Thomas C.

    2013-01-01

    The development of a high-duty-cycle microsecond time-resolution SAXS capability at the Biophysics Collaborative Access Team beamline (BioCAT) 18ID at the Advanced Photon Source, Argonne National Laboratory, USA, is reported. Small-angle X-ray scattering (SAXS) is a well established technique to probe the nanoscale structure and interactions in soft matter. It allows one to study the structure of native particles in near physiological environments and to analyze structural changes in response to variations in external conditions. The combination of microfluidics and SAXS provides a powerful tool to investigate dynamic processes on a molecular level with sub-millisecond time resolution. Reaction kinetics in the sub-millisecond time range has been achieved using continuous-flow mixers manufactured using micromachining techniques. The time resolution of these devices has previously been limited, in part, by the X-ray beam sizes delivered by typical SAXS beamlines. These limitations can be overcome using optics to focus X-rays to the micrometer size range providing that beam divergence and photon flux suitable for performing SAXS experiments can be maintained. Such micro-SAXS in combination with microfluidic devices would be an attractive probe for time-resolved studies. Here, the development of a high-duty-cycle scanning microsecond-time-resolution SAXS capability, built around the Kirkpatrick–Baez mirror-based microbeam system at the Biophysics Collaborative Access Team (BioCAT) beamline 18ID at the Advanced Photon Source, Argonne National Laboratory, is reported. A detailed description of the microbeam small-angle-scattering instrument, the turbulent flow mixer, as well as the data acquisition and control and analysis software is provided. Results are presented where this apparatus was used to study the folding of cytochrome c. Future prospects for this technique are discussed

  2. Sub-millisecond time-resolved SAXS using a continuous-flow mixer and X-ray microbeam

    Energy Technology Data Exchange (ETDEWEB)

    Graceffa, Rita, E-mail: rita.graceffa@gmail.com [Illinois Institute of Technology, 3101 South Dearborn, Chicago, IL 60616 (United States); Nobrega, R. Paul [University of Massachusetts Medical School, 364 Plantation Street, LRB 919, Worcester, MA 01605 (United States); Barrea, Raul A. [Illinois Institute of Technology, 3101 South Dearborn, Chicago, IL 60616 (United States); Kathuria, Sagar V. [University of Massachusetts Medical School, 364 Plantation Street, LRB 919, Worcester, MA 01605 (United States); Chakravarthy, Srinivas [Illinois Institute of Technology, 3101 South Dearborn, Chicago, IL 60616 (United States); Bilsel, Osman [University of Massachusetts Medical School, 364 Plantation Street, LRB 919, Worcester, MA 01605 (United States); Irving, Thomas C. [Illinois Institute of Technology, 3101 South Dearborn, Chicago, IL 60616 (United States)

    2013-11-01

    The development of a high-duty-cycle microsecond time-resolution SAXS capability at the Biophysics Collaborative Access Team beamline (BioCAT) 18ID at the Advanced Photon Source, Argonne National Laboratory, USA, is reported. Small-angle X-ray scattering (SAXS) is a well established technique to probe the nanoscale structure and interactions in soft matter. It allows one to study the structure of native particles in near physiological environments and to analyze structural changes in response to variations in external conditions. The combination of microfluidics and SAXS provides a powerful tool to investigate dynamic processes on a molecular level with sub-millisecond time resolution. Reaction kinetics in the sub-millisecond time range has been achieved using continuous-flow mixers manufactured using micromachining techniques. The time resolution of these devices has previously been limited, in part, by the X-ray beam sizes delivered by typical SAXS beamlines. These limitations can be overcome using optics to focus X-rays to the micrometer size range providing that beam divergence and photon flux suitable for performing SAXS experiments can be maintained. Such micro-SAXS in combination with microfluidic devices would be an attractive probe for time-resolved studies. Here, the development of a high-duty-cycle scanning microsecond-time-resolution SAXS capability, built around the Kirkpatrick–Baez mirror-based microbeam system at the Biophysics Collaborative Access Team (BioCAT) beamline 18ID at the Advanced Photon Source, Argonne National Laboratory, is reported. A detailed description of the microbeam small-angle-scattering instrument, the turbulent flow mixer, as well as the data acquisition and control and analysis software is provided. Results are presented where this apparatus was used to study the folding of cytochrome c. Future prospects for this technique are discussed.

  3. Time-resolved X-ray diffraction with accelerator- and laser-plasma-based X-ray sources

    International Nuclear Information System (INIS)

    Nicoul, Matthieu

    2010-01-01

    Femtosecond X-ray pulses are a powerful tool to investigate atomic motions triggered by femtosecond pump pulses. This thesis is dedicated to the production of such pulses and their use in optical pump - X-ray probe measurement. This thesis describes the laser-plasma-based sources available at the University of Duisburg-Essen. Part of it consists of the description of the design, built-up and characterization of a new ''modular'' X-ray source dedicated to optimize the X-ray flux onto the sample under investigation. The acoustic wave generation in femtosecond optically excited semiconductor (gallium arsenide) and metal (gold) was performed using the sources of the University of Duisburg-Essen. The physical answer of the material was modeled by a simple strain model for the semiconductor, pressure model for the metal, in order to gain information on the interplay of the electronic and thermal pressures rising after excitation. Whereas no reliable information could be obtain in gallium arsenide (principally due to the use of a bulk), the model for gold achieved very good agreement, providing useful information. The relaxation time of the electron to lattice energy was found to be (5.0±0.3) ps, and the ratio of the Grueneisen parameters was found to be γ e / γ i = (0.5±0.1). This thesis also describes the Sub-Picosecond Pulse Source (SPPS) which existed at the (formally) Stanford Linear Accelerator Center, an accelerator-based X-ray source, and two measurements performed with it. The first one is the detailed investigation of the phonon softening of the A 1g mode launch in bismuth upon fluence excitation. Detailed information concerning the new equilibrium position and phonon frequency were obtained over extended laser pump fluences. The second measurement concerned the study of the liquid phase dynamics in a newly formed liquid phase following ultrafast melting in indium antimonide. The formation of the liquid phase and its development for excitations close to the

  4. Time-resolved X-ray diffraction with accelerator- and laser-plasma-based X-ray sources

    Energy Technology Data Exchange (ETDEWEB)

    Nicoul, Matthieu

    2010-09-01

    Femtosecond X-ray pulses are a powerful tool to investigate atomic motions triggered by femtosecond pump pulses. This thesis is dedicated to the production of such pulses and their use in optical pump - X-ray probe measurement. This thesis describes the laser-plasma-based sources available at the University of Duisburg-Essen. Part of it consists of the description of the design, built-up and characterization of a new ''modular'' X-ray source dedicated to optimize the X-ray flux onto the sample under investigation. The acoustic wave generation in femtosecond optically excited semiconductor (gallium arsenide) and metal (gold) was performed using the sources of the University of Duisburg-Essen. The physical answer of the material was modeled by a simple strain model for the semiconductor, pressure model for the metal, in order to gain information on the interplay of the electronic and thermal pressures rising after excitation. Whereas no reliable information could be obtain in gallium arsenide (principally due to the use of a bulk), the model for gold achieved very good agreement, providing useful information. The relaxation time of the electron to lattice energy was found to be (5.0{+-}0.3) ps, and the ratio of the Grueneisen parameters was found to be {gamma}{sub e} / {gamma}{sub i} = (0.5{+-}0.1). This thesis also describes the Sub-Picosecond Pulse Source (SPPS) which existed at the (formally) Stanford Linear Accelerator Center, an accelerator-based X-ray source, and two measurements performed with it. The first one is the detailed investigation of the phonon softening of the A{sub 1g} mode launch in bismuth upon fluence excitation. Detailed information concerning the new equilibrium position and phonon frequency were obtained over extended laser pump fluences. The second measurement concerned the study of the liquid phase dynamics in a newly formed liquid phase following ultrafast melting in indium antimonide. The formation of the liquid phase

  5. Note: An X-ray powder diffractometer with a wide scattering-angle range of 72° using asymmetrically positioned one-dimensional detectors

    Energy Technology Data Exchange (ETDEWEB)

    Katsuya, Yoshio; Tanaka, Masahiko [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science (NIMS), 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan); Song, Chulho [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science (NIMS), 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan); Global Research Center for Environment and Energy based Nanomaterials Science (GREEN), Lithium Air Battery Specially Promoted Research Team, NIMS, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Ito, Kimihiko; Kubo, Yoshimi [Global Research Center for Environment and Energy based Nanomaterials Science (GREEN), Lithium Air Battery Specially Promoted Research Team, NIMS, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science (NIMS), 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan); Global Research Center for Environment and Energy based Nanomaterials Science (GREEN), Lithium Air Battery Specially Promoted Research Team, NIMS, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Synchrotron X-ray Group, Quantum Beam Unit, NIMS, 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan)

    2016-01-15

    An X-ray powder diffractometer has been developed for a time-resolved measurement without the requirement of a scattering angle (2θ) scan. Six one-dimensional detector modules are asymmetrically arranged in a vertical line at a designed distance of 286.5 mm. A detector module actually covers a diffraction angle of about 12° with an angular resolution of 0.01°. A diffracted intensity pattern is simultaneously recorded in a 2θ angular range from 1.63° to 74.37° in a “one shot” measurement. We tested the performance of the diffractometer with reference CeO{sub 2} powders and demonstrated diffraction measurements from an operating lithium-air battery.

  6. Time-resolved x-ray diffraction measurement of C60 under high pressure and temperature using synchrotron radiation

    International Nuclear Information System (INIS)

    Horikawa, T; Suito, K; Kobayashi, M; Onodera, A

    2002-01-01

    C 60 has been studied by means of time-resolved x-ray diffraction measurements using synchrotron radiation. Diffraction patterns were recorded at intervals of 1-10 min for samples under high pressure (12.5 and 14.3 GPa) and high temperature (up to 800 deg. C) for, at the longest, 3 h. Time, pressure, and temperature dependences of the C 60 structure are presented and the relevance to the hardness of materials derived from C 60 is discussed

  7. Modelling the X-ray powder diffraction of nitrogen-expanded austenite using the Debye formula

    DEFF Research Database (Denmark)

    Oddershede, Jette; Christiansen, Thomas; Ståhl, Kenny

    2008-01-01

    Stress-free and homogeneous samples of nitrogen-expanded austenite, a defect-rich f.c.c. structure with a high interstitial nitrogen occupancy (between 0.36 and 0.61), have been studied using X-ray powder diffraction and Debye simulations. The simulations confirm the presence of deformation...... to be indistinguishable to X-ray powder diffraction....

  8. X-ray filter for x-ray powder diffraction

    Science.gov (United States)

    Sinsheimer, John Jay; Conley, Raymond P.; Bouet, Nathalie C. D.; Dooryhee, Eric; Ghose, Sanjit

    2018-01-23

    Technologies are described for apparatus, methods and systems effective for filtering. The filters may comprise a first plate. The first plate may include an x-ray absorbing material and walls defining first slits. The first slits may include arc shaped openings through the first plate. The walls of the first plate may be configured to absorb at least some of first x-rays when the first x-rays are incident on the x-ray absorbing material, and to output second x-rays. The filters may comprise a second plate spaced from the first plate. The second plate may include the x-ray absorbing material and walls defining second slits. The second slits may include arc shaped openings through the second plate. The walls of the second plate may be configured to absorb at least some of second x-rays and to output third x-rays.

  9. Time-Resolved Soft X-ray Diffraction Reveals Transient Structural Distortions of Ternary Liquid Crystals

    Directory of Open Access Journals (Sweden)

    Klaus Mann

    2009-11-01

    Full Text Available Home-based soft X-ray time-resolved scattering experiments with nanosecond time resolution (10 ns and nanometer spatial resolution were carried out at a table top soft X-ray plasma source (2.2–5.2 nm. The investigated system was the lyotropic liquid crystal C16E7/paraffin/glycerol/formamide/IR 5. Usually, major changes in physical, chemical, and/or optical properties of the sample occur as a result of structural changes and shrinking morphology. Here, these effects occur as a consequence of the energy absorption in the sample upon optical laser excitation in the IR regime. The liquid crystal shows changes in the structural response within few hundred nanoseconds showing a time decay of 182 ns. A decrease of the Bragg peak diffracted intensity of 30% and a coherent macroscopic movement of the Bragg reflection are found as a response to the optical pump. The Bragg reflection movement is established to be isotropic and diffusion controlled (1 μs. Structural processes are analyzed in the Patterson analysis framework of the time-varying diffraction peaks revealing that the inter-lamellar distance increases by 2.7 Å resulting in an elongation of the coherently expanding lamella crystallite. The present studies emphasize the possibility of applying TR-SXRD techniques for studying the mechanical dynamics of nanosystems.

  10. IL 12: Femtosecond x-ray powder diffraction

    International Nuclear Information System (INIS)

    Woerner, M.; Zamponi, F.; Rothhardt, P.; Ansari, Z.; Dreyer, J.; Freyer, B.; Premont-Schwarz, M.; Elsaesser, T.

    2010-01-01

    A chemical reaction generates new compounds out of one or more initial species. On a molecular level, the spatial arrangement of electrons and nuclei changes. While the structure of the initial and the product molecules can be measured routinely, the transient structures and molecular motions during a reaction have remained unknown in most cases. This knowledge, however, is a key element for the exact understanding of the reaction. The ultimate dream is a 'reaction microscope' which allows for an in situ imaging of the molecules during a reaction. We report on the first femtosecond x-ray powder diffraction experiment in which we directly map the transient electronic charge density in the unit cell of a crystalline solid with 30 pico-meter spatial and 100 femtosecond temporal resolution. X-ray diffraction from polycrystalline powder samples, the Debye Scherrer diffraction technique, is a standard method for determining equilibrium structures. The intensity of the Debye Scherrer rings is determined by the respective x-ray structure factor which represents the Fourier transform of the spatial electron density. In our experiments, the transient intensity and angular positions of up to 20 Debye Scherrer reactions from a polycrystalline powder are measured and unravel for the first time a concerted electron and proton transfer in hydrogen-bonded ionic (NH 4 ) 2 SO 4 crystals. Photoexcitation of ammonium sulfate induces a sub-100 fs electron transfer from the sulfate groups into a highly conned electron channel along the z-axis of the unit cell. The latter geometry is stabilized by transferring protons from the adjacent ammonium groups into the channel. Time-dependent charge density maps derived from the diffraction data display a periodic modulation of the channels charge density by low-frequency lattice motions with a concerted electron and proton motion between the channel and the initial proton binding site. A deeper insight into the underlying microscopic

  11. CCD-based X-ray detectors for X-ray diffraction studies

    International Nuclear Information System (INIS)

    Ito, K.; Amemiya, Y.

    1999-01-01

    CCD-based X-ray detectors are getting to be used for X-ray diffraction studies especially in the studies where real time (automated) measurements and time-resolved measurements are required. Principles and designs of two typical types of CCD-based detectors are described; one is ths system in which x-ray image intensifiers are coupled to maximize the detective quantum efficiency for time-resolved measurements, and the other is the system in which tapered optical fibers are coupled for the reduction of the image into the CCD, which is optimized for automated measurements for protein crystallography. These CCD-based X-ray detectors have an image distortion and non-uniformity of response to be corrected by software. Correction schemes which we have developed are also described. (author)

  12. Time-resolved pump and probe x-ray absorption fine structure spectroscopy at beamline P11 at PETRA III

    Energy Technology Data Exchange (ETDEWEB)

    Göries, D., E-mail: dennis.goeries@desy.de; Roedig, P.; Stübe, N.; Meyer, J.; Warmer, M.; Weckert, E.; Meents, A., E-mail: alke.meents@desy.de [DESY Photon Science, Deutsches Elektronen-Synchrotron (DESY), Notkestraße 85, 22607 Hamburg (Germany); Dicke, B.; Naumova, M.; Rübhausen, M. [Center for Free-Electron Laser Science (CFEL), Luruper Chaussee 149, 22761 Hamburg (Germany); Galler, A.; Gawelda, W.; Geßler, P.; Sotoudi Namin, H.; Beckmann, A. [European XFEL, Albert-Einstein Ring 19, 22761 Hamburg (Germany); Britz, A.; Bressler, C. [European XFEL, Albert-Einstein Ring 19, 22761 Hamburg (Germany); The Hamburg Centre for Ultrafast Imaging, Luruper Chaussee 149, 22761 Hamburg (Germany); Schlie, M. [Institut für Experimentalphysik, University of Hamburg, Luruper Chaussee 149, 22761 Hamburg (Germany)

    2016-05-15

    We report about the development and implementation of a new setup for time-resolved X-ray absorption fine structure spectroscopy at beamline P11 utilizing the outstanding source properties of the low-emittance PETRA III synchrotron storage ring in Hamburg. Using a high intensity micrometer-sized X-ray beam in combination with two positional feedback systems, measurements were performed on the transition metal complex fac-Tris[2-phenylpyridinato-C2,N]iridium(III) also referred to as fac-Ir(ppy){sub 3}. This compound is a representative of the phosphorescent iridium(III) complexes, which play an important role in organic light emitting diode (OLED) technology. The experiment could directly prove the anticipated photoinduced charge transfer reaction. Our results further reveal that the temporal resolution of the experiment is limited by the PETRA III X-ray bunch length of ∼103 ps full width at half maximum (FWHM).

  13. A sample holder for in-house X-ray powder diffraction studies of protein powders

    DEFF Research Database (Denmark)

    Frankær, Christian Grundahl; Harris, Pernille; Ståhl, Kenny

    2011-01-01

    A sample holder for handling samples of protein for in-house X-ray powder diffraction (XRPD) analysis has been made and tested on lysozyme. The use of an integrated pinhole reduced the background, and good signal-to-noise ratios were obtained from only 7 l of sample, corresponding to approximatel...... 2-3 mg of dry protein. The sample holder is further adaptable to X-ray absorption spectroscopy (XAS) measurements. Both XRPD and XAS at the Zn K-edge were tested with hexameric Zn insulin....

  14. Diagnosis of laser ablated carbon particles measured by time-resolved X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Miyashita, Atsumi; Yoda, Osamu; Ohyanagi, T.; Murakami, K.

    1995-01-01

    The time and space resolved properties of laser ablated carbon particles were measured by X-ray absorption spectroscopy using LPX as an X-ray source. The energy density of the irradiation laser on the sample was in the range of 0.5-20J/cm 2 and the time delay was varied between 0 and 120ns. The absorption spectra exhibited several peaks originated from level to level transitions and an intense broad absorption in the energy range of C-K edge. At a delay time of 120ns, the absorption peak from 1s→2p transition of neutral carbon atom (C 0 ), C - , C + and C 2+ ions were observed. The absorption peak from C 0 was stronger as the probing position was closer to the sample surface and decreased rapidly with distance from the sample surface. The absorption peak C 2+ ion was observed only at comparatively distant positions from surface. The maximum speeds of highly charged ions were faster than that of neutral atoms and negative charged ions. The neutral atom and lower charged ions were emitted from the sample even after laser irradiation. The spatial distributions of the laser ablated carbon particles in the localized helium gas environment were measured. In the helium gas environment, the ablation plume was depressed by the helium cloud generated on the top of ablation plume. (author)

  15. One-dimensional curved wire chamber for powder x-ray crystallography

    International Nuclear Information System (INIS)

    Ortendahl, D.; Perez-Mendez, V.; Stoker, J.; Beyermann, W.

    1978-01-01

    A xenon filled single anode wire chamber with delay line readout has been constructed for use in powder x-ray crystallography using 8 to 20 keV x-rays. The entire chamber including the anode wire and the delay line which forms part of the cathode plane is a section of a circular arc whose center is the powder specimen. The anode wire--38 μm gold-plated tungsten--is suspended in a circular arc by the interaction of a current flowing through it and magnetic field provided by two permanent magnets, above and below the wire, extending along the active length of the chamber. When filled with xenon to 3 atmospheres the chamber has uniform sensitivity in excess of 80% at 8 keV and a spatial resolution better than 0.3 mm

  16. X-ray diffraction microstructural analysis of bimodal size distribution MgO nano powder

    International Nuclear Information System (INIS)

    Suminar Pratapa; Budi Hartono

    2009-01-01

    Investigation on the characteristics of x-ray diffraction data for MgO powdered mixture of nano and sub-nano particles has been carried out to reveal the crystallite-size-related microstructural information. The MgO powders were prepared by co-precipitation method followed by heat treatment at 500 degree Celsius and 1200 degree Celsius for 1 hour, being the difference in the temperature was to obtain two powders with distinct crystallite size and size-distribution. The powders were then blended in air to give the presumably bimodal-size- distribution MgO nano powder. High-quality laboratory X-ray diffraction data for the powders were collected and then analysed using Rietveld-based MAUD software using the lognormal size distribution. Results show that the single-mode powders exhibit spherical crystallite size (R) of 20(1) nm and 160(1) nm for the 500 degree Celsius and 1200 degree Celsius data respectively with the nano metric powder displays narrower crystallite size distribution character, indicated by lognormal dispersion parameter of 0.21 as compared to 0.01 for the sub-nano metric powder. The mixture exhibits relatively more asymmetric peak broadening. Analysing the x-ray diffraction data for the latter specimen using single phase approach give unrealistic results. Introducing two phase models for the double-phase mixture to accommodate the bimodal-size-distribution characteristics give R = 100(6) and σ = 0.62 for the nano metric phase and R = 170(5) and σ= 0.12 for the σ sub-nano metric phase. (author)

  17. Spatially resolved single crystal x-ray spectropolarimetry of wire array z-pinch plasmas.

    Science.gov (United States)

    Wallace, M S; Haque, S; Neill, P; Pereira, N R; Presura, R

    2018-01-01

    A recently developed single-crystal x-ray spectropolarimeter has been used to record paired sets of polarization-dependent and axially resolved x-ray spectra emitted by wire array z-pinches. In this measurement, two internal planes inside a suitable crystal diffract the x-rays into two perpendicular directions that are normal to each other, thereby separating incident x-rays into their linearly polarized components. This paper gives considerations for fielding the instrument on extended sources. Results from extended sources are difficult to interpret because generally the incident x-rays are not separated properly by the crystal. This difficulty is mitigated by using a series of collimating slits to select incident x-rays that propagate in a plane of symmetry between the polarization-splitting planes. The resulting instrument and some of the spatially resolved polarized x-ray spectra recorded for a 1-MA aluminum wire array z-pinch at the Nevada Terawatt Facility at the University of Nevada, Reno will be presented.

  18. RESOLVED COMPANIONS OF CEPHEIDS: TESTING THE CANDIDATES WITH X-RAY OBSERVATIONS

    Energy Technology Data Exchange (ETDEWEB)

    Evans, Nancy Remage; Pillitteri, Ignazio; Wolk, Scott; Karovska, Margarita; Tingle, Evan [Smithsonian Astrophysical Observatory, MS 4, 60 Garden St., Cambridge, MA 02138 (United States); Guinan, Edward; Engle, Scott [Department of Astronomy and Astrophysics, Villanova University, 800 Lancaster Ave., Villanova, PA 19085 (United States); Bond, Howard E. [Department of Astronomy and Astrophysics, Pennsylvania State University, University Park, PA 16802 (United States); Schaefer, Gail H. [The CHARA Array of Georgia State University, Mount Wilson, California 91023 (United States); Mason, Brian D., E-mail: nevans@cfa.harvard.edu, E-mail: heb11@psu.edu, E-mail: schaefer@chara-array.org [US Naval Observatory, 3450 Massachusetts Ave., NW, Washington, DC 20392-5420 (United States)

    2016-04-15

    We have made XMM-Newton observations of 14 Galactic Cepheids that have candidate resolved (≥5″) companion stars based on our earlier HST Wide Field Camera 3 (WFC3) imaging survey. Main-sequence stars that are young enough to be physical companions of Cepheids are expected to be strong X-ray producers in contrast to field stars. XMM-Newton exposures were set to detect essentially all companions hotter than spectral type M0 (corresponding to 0.5 M{sub ⊙}). The large majority of our candidate companions were not detected in X-rays, and hence are not confirmed as young companions. One resolved candidate (S Nor #4) was unambiguously detected, but the Cepheid is a member of a populous cluster. For this reason, it is likely that S Nor #4 is a cluster member rather than a gravitationally bound companion. Two further Cepheids (S Mus and R Cru) have X-ray emission that might be produced by either the Cepheid or the candidate resolved companion. A subsequent Chandra observation of S Mus shows that the X-rays are at the location of the Cepheid/spectroscopic binary. R Cru and also V659 Cen (also X-ray bright) have possible companions closer than 5″ (the limit for this study) which are the likely sources of X-rays. One final X-ray detection (V473 Lyr) has no known optical companion, so the prime suspect is the Cepheid itself. It is a unique Cepheid with a variable amplitude. The 14 stars that we observed with XMM constitute 36% of the 39 Cepheids found to have candidate companions in our HST/WFC3 optical survey. No young probable binary companions were found with separations of ≥5″ or 4000 au.

  19. RESOLVED COMPANIONS OF CEPHEIDS: TESTING THE CANDIDATES WITH X-RAY OBSERVATIONS

    International Nuclear Information System (INIS)

    Evans, Nancy Remage; Pillitteri, Ignazio; Wolk, Scott; Karovska, Margarita; Tingle, Evan; Guinan, Edward; Engle, Scott; Bond, Howard E.; Schaefer, Gail H.; Mason, Brian D.

    2016-01-01

    We have made XMM-Newton observations of 14 Galactic Cepheids that have candidate resolved (≥5″) companion stars based on our earlier HST Wide Field Camera 3 (WFC3) imaging survey. Main-sequence stars that are young enough to be physical companions of Cepheids are expected to be strong X-ray producers in contrast to field stars. XMM-Newton exposures were set to detect essentially all companions hotter than spectral type M0 (corresponding to 0.5 M ⊙ ). The large majority of our candidate companions were not detected in X-rays, and hence are not confirmed as young companions. One resolved candidate (S Nor #4) was unambiguously detected, but the Cepheid is a member of a populous cluster. For this reason, it is likely that S Nor #4 is a cluster member rather than a gravitationally bound companion. Two further Cepheids (S Mus and R Cru) have X-ray emission that might be produced by either the Cepheid or the candidate resolved companion. A subsequent Chandra observation of S Mus shows that the X-rays are at the location of the Cepheid/spectroscopic binary. R Cru and also V659 Cen (also X-ray bright) have possible companions closer than 5″ (the limit for this study) which are the likely sources of X-rays. One final X-ray detection (V473 Lyr) has no known optical companion, so the prime suspect is the Cepheid itself. It is a unique Cepheid with a variable amplitude. The 14 stars that we observed with XMM constitute 36% of the 39 Cepheids found to have candidate companions in our HST/WFC3 optical survey. No young probable binary companions were found with separations of ≥5″ or 4000 au

  20. Butterfly Deformation Modes in a Photoexcited Pyrazolate-Bridged Pt Complex Measured by Time-Resolved X-Ray Scattering in Solution

    DEFF Research Database (Denmark)

    Haldrup, Kristoffer; Dohn, Asmus Ougaard; Shelby, Megan L.

    2016-01-01

    the monochromatic X-ray pulses at Beamline 11IDD of the Advanced Photon Source. The excited-state structural analysis of 1 was performed based on the results from both transient WAXS measurements and density functional theory calculations to shed light on the primary structural changes in its triplet metal-metal...... excited state has remained scarce. Using time-resolved wide-angle X-ray scattering (WAXS), the excited triplet state molecular structure of [Pt(ppy)(μ-t-Bu2pz)]2 (ppy = 2-phenylpyridine; t-Bu2pz = 3,5-di-tert-butylpyrazolate), complex 1, was obtained in a dilute (0.5 mM) toluene solution utilizing...

  1. Chandra Resolves Cosmic X-ray Glow and Finds Mysterious New Sources

    Science.gov (United States)

    2000-01-01

    While taking a giant leap towards solving one of the greatest mysteries of X-ray astronomy, NASA's Chandra X-ray Observatory also may have revealed the most distant objects ever seen in the universe and discovered two puzzling new types of cosmic objects. Not bad for being on the job only five months. Chandra has resolved most of the X-ray background, a pervasive glow of X-rays throughout the universe, first discovered in the early days of space exploration. Before now, scientists have not been able to discern the background's origin, because no X-ray telescope until Chandra has had both the angular resolution and sensitivity to resolve it. "This is a major discovery," said Dr. Alan Bunner, Director of NASA's Structure andEvolution of the universe science theme. "Since it was first observed thirty-seven years ago, understanding the source of the X-ray background has been aHoly Grail of X-ray astronomy. Now, it is within reach." The results of the observation will be discussed today at the 195th national meeting of the American Astronomical Society in Atlanta, Georgia. An article describing this work has been submitted to the journal Nature by Dr. Richard Mushotzky, of NASA Goddard Space Flight Center, Greenbelt, Md., Drs. Lennox Cowie and Amy Barger at the University of Hawaii, Honolulu, and Dr. Keith Arnaud of the University of Maryland, College Park. "We are all very excited by this finding," said Mushotzky. "The resolution of most of the hard X-ray background during the first few months of the Chandra mission is a tribute to the power of this observatory and bodes extremely well for its scientific future," Scientists have known about the X-ray glow, called the X-ray background, since the dawn of X-ray astronomy in the early 1960s. They have been unable to discern its origin, however, for no X-ray telescope until Chandra has had both the angular resolution and sensitivity to resolve it. The German-led ROSAT mission, now completed, resolved much of the lower

  2. X-ray powder microdiffraction in the analysis of art works

    Czech Academy of Sciences Publication Activity Database

    Šímová, Veronika; Bezdička, Petr; Hradilová, J.; Bayerová, T.; Hradil, David

    2004-01-01

    Roč. 11, 1a (2004), s. 43 ISSN 1211-5894. [European Powder Diffraction Conference /9./. Prague, 02.09.2004-05.09.2004] R&D Projects: GA MŠk LN00A028; GA ČR GA203/04/2091; GA AV ČR KJB1032401 Institutional research plan: CEZ:AV0Z4032918 Keywords : X-ray powder microdiffraction * pigments * colour layers of artworks Subject RIV: CA - Inorganic Chemistry

  3. Investigations of time resolved x-ray wide-angle scattering and x-ray small-angle scattering at DESY

    International Nuclear Information System (INIS)

    Zachmann, H.G.; Gehrke, R.; Prieske, W.; Riekel, C.

    1985-01-01

    Instrumentation is described for the simultaneous wide-angle and small-angle x-ray scattering. The method was applied to the study of the isothermal crystallization of polyethylene terephthalates. In agreement with the classical theories of crystallization, the data showed that the density difference between the crystals and the non-crystalline regions does not change with time. The mechanisms of melting, recrystallization, and crystal thickening were investigated by small-angle x-ray scattering with stepwise changes and continuous changes of temperature using polyethylene terephthalate

  4. The Oxford-Diamond In Situ Cell for studying chemical reactions using time-resolved X-ray diffraction

    Science.gov (United States)

    Moorhouse, Saul J.; Vranješ, Nenad; Jupe, Andrew; Drakopoulos, Michael; O'Hare, Dermot

    2012-08-01

    A versatile, infrared-heated, chemical reaction cell has been assembled and commissioned for the in situ study of a range of chemical syntheses using time-resolved energy-dispersive X-ray diffraction (EDXRD) on Beamline I12 at the Diamond Light Source. Specialized reactor configurations have been constructed to enable in situ EDXRD investigation of samples under non-ambient conditions. Chemical reactions can be studied using a range of sample vessels such as alumina crucibles, steel hydrothermal autoclaves, and glassy carbon tubes, at temperatures up to 1200 °C.

  5. Solving Crystal Structures from Powder Diffraction Data

    DEFF Research Database (Denmark)

    Christensen, A. Nørlund; Lehmann, M. S.; Nielsen, Mogens

    1985-01-01

    High resolution powder data from both neutron and X-ray (synchrotron) sources have been used to estimate the possibility of direct structure determination from powder data. Two known structures were resolved by direct methods with neutron and X-ray data. With synchrotron X-ray data, the measured ...

  6. A radially accessible tubular in situ X-ray cell for spatially resolved operando scattering and spectroscopic studies of electrochemical energy storage devices

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Hao; Allan, Phoebe K.; Borkiewicz, Olaf J.; Kurtz, Charles; Grey, Clare P.; Chapman, Karena W.; Chupas, Peter J.

    2016-09-16

    A tubularoperandoelectrochemical cell has been developed to allow spatially resolved X-ray scattering and spectroscopic measurements of individual cell components, or regions thereof, during device operation. These measurements are enabled by the tubular cell geometry, wherein the X-ray-transparent tube walls allow radial access for the incident and scattered/transmitted X-ray beam; by probing different depths within the electrode stack, the transformation of different components or regions can be resolved. The cell is compatible with a variety of synchrotron-based scattering, absorption and imaging methodologies. The reliability of the electrochemical cell and the quality of the resulting X-ray scattering and spectroscopic data are demonstrated for two types of energy storage: the evolution of the distribution of the state of charge of an Li-ion battery electrode during cycling is documented using X-ray powder diffraction, and the redistribution of ions between two porous carbon electrodes in an electrochemical double-layer capacitor is documented using X-ray absorption near-edge spectroscopy.

  7. Time-resolved x-ray diffraction measurement of C{sub 60} under high pressure and temperature using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Horikawa, T [Graduate School of Engineering Science, Osaka University, Toyonaka, Osaka 560-8531 (Japan); Suito, K [Graduate School of Engineering Science, Osaka University, Toyonaka, Osaka 560-8531 (Japan); Kobayashi, M [Graduate School of Engineering Science, Osaka University, Toyonaka, Osaka 560-8531 (Japan); Onodera, A [Graduate School of Engineering Science, Osaka University, Toyonaka, Osaka 560-8531 (Japan)

    2002-11-11

    C{sub 60} has been studied by means of time-resolved x-ray diffraction measurements using synchrotron radiation. Diffraction patterns were recorded at intervals of 1-10 min for samples under high pressure (12.5 and 14.3 GPa) and high temperature (up to 800 deg. C) for, at the longest, 3 h. Time, pressure, and temperature dependences of the C{sub 60} structure are presented and the relevance to the hardness of materials derived from C{sub 60} is discussed.

  8. Penetration route of functional molecules in stratum corneum studied by time-resolved small- and wide-angle x-ray diffraction

    International Nuclear Information System (INIS)

    Hatta, Ichiro; Ohta, Noboru; Yagi, Naoto; Nakazawa, Hiromitsu; Obata, Yasuko; Inoue, Katsuaki

    2011-01-01

    We studied effects of functional molecules on corneocytes in stratum corneum using time-resolved small- and wide-angle x-ray diffraction after applying a functional molecule. From these results it was revealed that in the stratum corneum a typical hydrophilic molecule, ethanol, penetrates via the transcellular route and on the other hand a typical hydrophobic molecule, d-limonene, penetrates via the intercellular route.

  9. Time-resolved studies. Ch. 9

    International Nuclear Information System (INIS)

    Mills, Dennis M.; Argonne National Lab., IL

    1991-01-01

    Synchrotron radiation, with its unique properties, offers a tool to extend X-ray measurements from the static to the time-resolved regime. The most straight-forward application of synchrotron radiation to the study of transient phenomena is directly through the possibility of decreased data-collection times via the enormous increase in flux over that of a laboratory X-ray system. Even further increases in intensity can be obtained through the use of novel X-ray optical devices. Wide-bandpass monochromators, e.g., that utilize the continuous spectral distribution of synchrotron radiation, can increase flux on the sample several orders of magnitude over conventional X-ray optical systems thereby allowing a further shortening of the data-collection time. Another approach that uses the continuous spectral nature of synchrotron radiation to decrease data-collection times is the 'parallel data collection' method. Using this technique, intensities as a function of X-ray energy are recorded simultaneously for all energies rather than sequentially recording data at each energy, allowing for a dramatic decrease in data-collection time. Perhaps the most exciting advances in time-resolved X-ray studies will be made by those methods that exploit the pulsed nature of the radiation emitted from storage rings. Pulsed techniques have had an enormous impact in the study of the temporal evolution of transient phenomena. The extension from continuous to modulated sources for use in time-resolved work has been carried over in a host of fields that use both pulsed particle and pulsed electro-magnetic beams. In this chapter the new experimental techniques are reviewed and illustrated with some experiments. (author). 98 refs.; 20 figs.; 5 tabs

  10. Resolved Companions of Cepheids: Testing the Candidates with X-Ray Observations

    Science.gov (United States)

    Evans, Nancy Remage; Pillitteri, Ignazio; Wolk, Scott; Karovska, Margarita; Tingle, Evan; Guinan, Edward; Engle, Scott; Bond, Howard E.; Schaefer, Gail H.; Mason, Brian D.

    2016-04-01

    We have made XMM-Newton observations of 14 Galactic Cepheids that have candidate resolved (≥5″) companion stars based on our earlier HST Wide Field Camera 3 (WFC3) imaging survey. Main-sequence stars that are young enough to be physical companions of Cepheids are expected to be strong X-ray producers in contrast to field stars. XMM-Newton exposures were set to detect essentially all companions hotter than spectral type M0 (corresponding to 0.5 M⊙). The large majority of our candidate companions were not detected in X-rays, and hence are not confirmed as young companions. One resolved candidate (S Nor #4) was unambiguously detected, but the Cepheid is a member of a populous cluster. For this reason, it is likely that S Nor #4 is a cluster member rather than a gravitationally bound companion. Two further Cepheids (S Mus and R Cru) have X-ray emission that might be produced by either the Cepheid or the candidate resolved companion. A subsequent Chandra observation of S Mus shows that the X-rays are at the location of the Cepheid/spectroscopic binary. R Cru and also V659 Cen (also X-ray bright) have possible companions closer than 5″ (the limit for this study) which are the likely sources of X-rays. One final X-ray detection (V473 Lyr) has no known optical companion, so the prime suspect is the Cepheid itself. It is a unique Cepheid with a variable amplitude. The 14 stars that we observed with XMM constitute 36% of the 39 Cepheids found to have candidate companions in our HST/WFC3 optical survey. No young probable binary companions were found with separations of ≥5″ or 4000 au. Based on observations obtained with XMM-Newton, an ESA science mission with instruments and contributions directly funded by ESA Member States and the USA (NASA).

  11. Vibrational spectra, powder X-ray diffractions and physical properties of cyanide complexes with 1-ethylimidazole

    Science.gov (United States)

    Kürkçüoğlu, Güneş Süheyla; Kiraz, Fulya Çetinkaya; Sayın, Elvan

    2015-10-01

    The heteronuclear tetracyanonickelate(II) complexes of the type [M(etim)Ni(CN)4]n (hereafter, abbreviated as M-Ni-etim, M = Mn(II), Fe(II) or Co(II); etim = 1-ethylimidazole, C5H8N2) were prepared in powder form and characterized by FT-IR and Raman spectroscopy, powder X-ray diffraction (PXRD), thermal (TG; DTG and DTA), and elemental analysis techniques. The structures of these complexes were elucidated using vibrational spectra and powder X-ray diffraction patterns with the peak assignment to provide a better understanding of the structures. It is shown that the spectra are consistent with a proposed crystal structure for these compounds derived from powder X-ray diffraction measurements. Vibrational spectra of the complexes were presented and discussed with respect to the internal modes of both the etim and the cyanide ligands. The C, H and N analyses were carried out for all the complexes. Thermal behaviors of these complexes were followed using TG, DTG and DTA curves in the temperature range 30-700 °C in the static air atmosphere. The FT-IR, Raman spectra, thermal and powder X-ray analyses revealed no significant differences between the single crystal and powder forms. Additionally, electrical and magnetic properties of the complexes were investigated. The FT-IR and Raman spectroscopy, PXRD, thermal and elemental analyses results propose that these complexes are similar in structure to the Hofmann-type complexes.

  12. Time resolved measurement of laser-ablated particles by LAPXAS (Laser Plasma Soft X-ray Absorption Spectroscopy)

    International Nuclear Information System (INIS)

    Miyashita, Atsumi; Yoda, Osamu; Murakami, Kouichi

    1999-01-01

    The time- and spatially-resolved properties of laser ablated carbon, boron and silicon particles were measured by LAPXAS (Laser Plasma Soft X-ray Absorption Spectroscopy). The maximum speed of positively charged ions is higher than those of neutral atoms and negatively charged ions. The spatial distributions of the laser-ablated particles in the localized rare gas environment were measured. In helium gas environment, by the helium cloud generated on the top of ablation plume depressed the ablation plume. There is no formation of silicon clusters till 15 μs after laser ablation in the argon gas environment. (author)

  13. Investigation of Co nanoparticle formation using time-dependent and spatially-resolved X-ray absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Zinoveva, S

    2008-04-15

    A crucial step towards controlled synthesis of nanoparticles is the detailed understanding of the various chemical processes that take place during the synthesis. X-ray Absorption Spectroscopy (XAS) is especially suitable for elucidating the type and structure of the intermediate metal species. It is applicable to materials that have no long range order and provides information on both electronic and geometric structures. Here a comparative study is reported of the formation of cobalt nanoparticles via thermolysis of two organometallic precursors dicobalt octacarbonyl (DCO) and alkyne-bridged dicobalt hexacarbonyl (ADH) in the presence of aluminum organics. Using time-dependent XAS a reaction pathway different from both the atom based La Mer model and the Watzky and Finsky autocatalytic surface growth model is observed. Where prior to the nucleation several intermediates are formed and the initial nucleus is composed of Co atoms coordinated with ligands Co{sub n}(CO){sub m} with n=2-3, m=3-5. The formation of Co nanoparticles was also investigated using a reaction different from thermolysis of cobalt carbonyls, namely reduction of Co (II) acetate by sodium borohydrate. Here the combination of microreactor system and spatially resolved XAS allowed ''in situ'' monitoring of the wet chemical synthesis. Several steps of the reaction were spatially resolved in the microreactor. The vertical size of the X-ray beam (50 {mu}m) focused with Kirkpatrick-Baez mirror system, determines the time resolution (better than 2 ms). The results provide direct insight into rapid process of nanoparticles formation and demonstrate the potential of this new technique for the fundamental studies of such type of processes where miniaturization and timeresolution are important. Like in the carbonyls thermolysis no evidence for the reduction of the starting complex to isolated Co{sup 0} atoms followed by nucleation of Co{sup 0} atoms was observed. (orig.)

  14. Investigation of Co nanoparticle formation using time-dependent and spatially-resolved X-ray absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Zinoveva, S.

    2008-04-15

    A crucial step towards controlled synthesis of nanoparticles is the detailed understanding of the various chemical processes that take place during the synthesis. X-ray Absorption Spectroscopy (XAS) is especially suitable for elucidating the type and structure of the intermediate metal species. It is applicable to materials that have no long range order and provides information on both electronic and geometric structures. Here a comparative study is reported of the formation of cobalt nanoparticles via thermolysis of two organometallic precursors dicobalt octacarbonyl (DCO) and alkyne-bridged dicobalt hexacarbonyl (ADH) in the presence of aluminum organics. Using time-dependent XAS a reaction pathway different from both the atom based La Mer model and the Watzky and Finsky autocatalytic surface growth model is observed. Where prior to the nucleation several intermediates are formed and the initial nucleus is composed of Co atoms coordinated with ligands Co{sub n}(CO){sub m} with n=2-3, m=3-5. The formation of Co nanoparticles was also investigated using a reaction different from thermolysis of cobalt carbonyls, namely reduction of Co (II) acetate by sodium borohydrate. Here the combination of microreactor system and spatially resolved XAS allowed ''in situ'' monitoring of the wet chemical synthesis. Several steps of the reaction were spatially resolved in the microreactor. The vertical size of the X-ray beam (50 {mu}m) focused with Kirkpatrick-Baez mirror system, determines the time resolution (better than 2 ms). The results provide direct insight into rapid process of nanoparticles formation and demonstrate the potential of this new technique for the fundamental studies of such type of processes where miniaturization and timeresolution are important. Like in the carbonyls thermolysis no evidence for the reduction of the starting complex to isolated Co{sup 0} atoms followed by nucleation of Co{sup 0} atoms was observed. (orig.)

  15. Direct measurements of multi-photon induced nonlinear lattice dynamics in semiconductors via time-resolved x-ray scattering.

    Science.gov (United States)

    Williams, G Jackson; Lee, Sooheyong; Walko, Donald A; Watson, Michael A; Jo, Wonhuyk; Lee, Dong Ryeol; Landahl, Eric C

    2016-12-22

    Nonlinear optical phenomena in semiconductors present several fundamental problems in modern optics that are of great importance for the development of optoelectronic devices. In particular, the details of photo-induced lattice dynamics at early time-scales prior to carrier recombination remain poorly understood. We demonstrate the first integrated measurements of both optical and structural, material-dependent quantities while also inferring the bulk impulsive strain profile by using high spatial-resolution time-resolved x-ray scattering (TRXS) on bulk crystalline gallium arsenide. Our findings reveal distinctive laser-fluence dependent crystal lattice responses, which are not described by previous TRXS experiments or models. The initial linear expansion of the crystal upon laser excitation stagnates at a laser fluence corresponding to the saturation of the free carrier density before resuming expansion in a third regime at higher fluences where two-photon absorption becomes dominant. Our interpretations of the lattice dynamics as nonlinear optical effects are confirmed by numerical simulations and by additional measurements in an n-type semiconductor that allows higher-order nonlinear optical processes to be directly observed as modulations of x-ray diffraction lineshapes.

  16. Fundamentals of powder x-ray diffraction practice

    International Nuclear Information System (INIS)

    Raftery, T.

    2002-01-01

    Full text: The goal of powder Xray diffraction is to gain information about a specimen or sample. Key aspects of this goal are 1. the sample selection, preparation and presentation; 2. the data collection process and conditions; 3. the interaction between these and the interpretation of the data. The 'ideal' powder (or polycrystalline) xray diffraction sample is fine grained, randomly orientated, homogenous and representative. There exists standard sample selection and preparation techniques for powders - sometimes however, the required information must be gained by alternate sample selection and preparation techniques. While there are few variables in the data collection process, there are some significant ones such as matching diffractometer resolution and intensity to the data collection goal whether that is phase identity, quantitative analysis or structure refinement, etc. There are also options of optical arrangement (Bragg-Brintano versus parallel beam versus Debye-Scherrer). One important aspect of the collection process is the assessment of the data quality. Powder xray diffraction has many applications from the straight-forward confirmation of phase identity and purity to structural analysis. Some of these applications will be considered and the interaction between the goal of the application and aspects of sample selection. Copyright (2002) Australian X-ray Analytical Association Inc

  17. X-ray powder microdiffraction for routine analysis of paintings

    Czech Academy of Sciences Publication Activity Database

    Šímová, Veronika; Bezdička, Petr; Hradilová, J.; Hradil, David; Grygar, Tomáš

    2005-01-01

    Roč. 20, č. 3 (2005), s. 224-229 ISSN 0885-7156 R&D Projects: GA MŠk(CZ) LN00A028; GA ČR GA203/04/2091; GA AV ČR KJB1032401 Institutional research plan: CEZ:AV0Z40320502 Keywords : powder X-ray microdiffraction * artwork analysis Subject RIV: CA - Inorganic Chemistry Impact factor: 0.483, year: 2005

  18. X-ray streak crystal spectography

    International Nuclear Information System (INIS)

    Kauffman, R.L.; Brown, T.; Medecki, H.

    1983-01-01

    We have built an x-ray streaked crystal spectrograph for making time-resolved x-ray spectral measurements. This instrument can access Bragg angles from 11 0 to 38 0 and x-ray spectra from 200 eV to greater than 10 keV. We have demonstrated resolving powers, E/δE > 200 at 1 keV and time resolution less than 20 psec. A description of the instrument and an example of the data is given

  19. Photolysis of Br2 in CCl4 studied by time-resolved X-ray scattering.

    Science.gov (United States)

    Kong, Qingyu; Lee, Jae Hyuk; Lo Russo, Manuela; Kim, Tae Kyu; Lorenc, Maciej; Cammarata, Marco; Bratos, Savo; Buslaps, Thomas; Honkimaki, Veijo; Ihee, Hyotcherl; Wulff, Michael

    2010-03-01

    A time-resolved X-ray solution scattering study of bromine molecules in CCl(4) is presented as an example of how to track atomic motions in a simple chemical reaction. The structures of the photoproducts are tracked during the recombination process, geminate and non-geminate, from 100 ps to 10 micros after dissociation. The relaxation of hot Br(2)(*) molecules heats the solvent. At early times, from 0.1 to 10 ns, an adiabatic temperature rise is observed, which leads to a pressure gradient that forces the sample to expand. The expansion starts after about 10 ns with the laser beam sizes used here. When thermal artefacts are removed by suitable scaling of the transient solvent response, the excited-state solute structures can be obtained with high fidelity. The analysis shows that 30% of Br(2)(*) molecules recombine directly along the X potential, 60% are trapped in the A/A' state with a lifetime of 5.5 ns, and 10% recombine non-geminately via diffusive motion in about 25 ns. The Br-Br distance distribution in the A/A' state peaks at 3.0 A.

  20. Time-Resolved Small-Angle X-Ray Scattering

    NARCIS (Netherlands)

    ten Elshof, Johan E.; Besselink, R.; Stawski, Tomasz; Castricum, H.L.; Levy, D.; Zayat, M.

    2015-01-01

    This chapter focuses on time-resolved studies of nanostructure development in sol-gel liquids, that is, diluted sols, wet gels, and drying thin fffilms. The most commonly investigated classes of sol-gel materials are silica, organically modified silica, template-directed mesostructured silica,

  1. Resolving hot spot microstructure using x-ray penumbral imaging (invited)

    Science.gov (United States)

    Bachmann, B.; Hilsabeck, T.; Field, J.; Masters, N.; Reed, C.; Pardini, T.; Rygg, J. R.; Alexander, N.; Benedetti, L. R.; Döppner, T.; Forsman, A.; Izumi, N.; LePape, S.; Ma, T.; MacPhee, A. G.; Nagel, S.; Patel, P.; Spears, B.; Landen, O. L.

    2016-11-01

    We have developed and fielded x-ray penumbral imaging on the National Ignition Facility in order to enable sub-10 μm resolution imaging of stagnated plasma cores (hot spots) of spherically shock compressed spheres and shell implosion targets. By utilizing circular tungsten and tantalum apertures with diameters ranging from 20 μm to 2 mm, in combination with image plate and gated x-ray detectors as well as imaging magnifications ranging from 4 to 64, we have demonstrated high-resolution imaging of hot spot plasmas at x-ray energies above 5 keV. Here we give an overview of the experimental design criteria involved and demonstrate the most relevant influences on the reconstruction of x-ray penumbral images, as well as mitigation strategies of image degrading effects like over-exposed pixels, artifacts, and photon limited source emission. We describe experimental results showing the advantages of x-ray penumbral imaging over conventional Fraunhofer and photon limited pinhole imaging and showcase how internal hot spot microstructures can be resolved.

  2. Resolving hot spot microstructure using x-ray penumbral imaging (invited)

    Energy Technology Data Exchange (ETDEWEB)

    Bachmann, B., E-mail: bachmann2@llnl.gov; Field, J.; Masters, N.; Pardini, T.; Rygg, J. R.; Benedetti, L. R.; Döppner, T.; Izumi, N.; LePape, S.; Ma, T.; MacPhee, A. G.; Nagel, S.; Patel, P.; Spears, B.; Landen, O. L. [Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Hilsabeck, T.; Reed, C.; Alexander, N.; Forsman, A. [General Atomics, San Diego, California 92186 (United States)

    2016-11-15

    We have developed and fielded x-ray penumbral imaging on the National Ignition Facility in order to enable sub-10 μm resolution imaging of stagnated plasma cores (hot spots) of spherically shock compressed spheres and shell implosion targets. By utilizing circular tungsten and tantalum apertures with diameters ranging from 20 μm to 2 mm, in combination with image plate and gated x-ray detectors as well as imaging magnifications ranging from 4 to 64, we have demonstrated high-resolution imaging of hot spot plasmas at x-ray energies above 5 keV. Here we give an overview of the experimental design criteria involved and demonstrate the most relevant influences on the reconstruction of x-ray penumbral images, as well as mitigation strategies of image degrading effects like over-exposed pixels, artifacts, and photon limited source emission. We describe experimental results showing the advantages of x-ray penumbral imaging over conventional Fraunhofer and photon limited pinhole imaging and showcase how internal hot spot microstructures can be resolved.

  3. Resolving hot spot microstructure using x-ray penumbral imaging (invited).

    Science.gov (United States)

    Bachmann, B; Hilsabeck, T; Field, J; Masters, N; Reed, C; Pardini, T; Rygg, J R; Alexander, N; Benedetti, L R; Döppner, T; Forsman, A; Izumi, N; LePape, S; Ma, T; MacPhee, A G; Nagel, S; Patel, P; Spears, B; Landen, O L

    2016-11-01

    We have developed and fielded x-ray penumbral imaging on the National Ignition Facility in order to enable sub-10 μm resolution imaging of stagnated plasma cores (hot spots) of spherically shock compressed spheres and shell implosion targets. By utilizing circular tungsten and tantalum apertures with diameters ranging from 20 μm to 2 mm, in combination with image plate and gated x-ray detectors as well as imaging magnifications ranging from 4 to 64, we have demonstrated high-resolution imaging of hot spot plasmas at x-ray energies above 5 keV. Here we give an overview of the experimental design criteria involved and demonstrate the most relevant influences on the reconstruction of x-ray penumbral images, as well as mitigation strategies of image degrading effects like over-exposed pixels, artifacts, and photon limited source emission. We describe experimental results showing the advantages of x-ray penumbral imaging over conventional Fraunhofer and photon limited pinhole imaging and showcase how internal hot spot microstructures can be resolved.

  4. Resolving hot spot microstructure using x-ray penumbral imaging (invited)

    International Nuclear Information System (INIS)

    Bachmann, B.; Field, J.; Masters, N.; Pardini, T.; Rygg, J. R.; Benedetti, L. R.; Döppner, T.; Izumi, N.; LePape, S.; Ma, T.; MacPhee, A. G.; Nagel, S.; Patel, P.; Spears, B.; Landen, O. L.; Hilsabeck, T.; Reed, C.; Alexander, N.; Forsman, A.

    2016-01-01

    We have developed and fielded x-ray penumbral imaging on the National Ignition Facility in order to enable sub-10 μm resolution imaging of stagnated plasma cores (hot spots) of spherically shock compressed spheres and shell implosion targets. By utilizing circular tungsten and tantalum apertures with diameters ranging from 20 μm to 2 mm, in combination with image plate and gated x-ray detectors as well as imaging magnifications ranging from 4 to 64, we have demonstrated high-resolution imaging of hot spot plasmas at x-ray energies above 5 keV. Here we give an overview of the experimental design criteria involved and demonstrate the most relevant influences on the reconstruction of x-ray penumbral images, as well as mitigation strategies of image degrading effects like over-exposed pixels, artifacts, and photon limited source emission. We describe experimental results showing the advantages of x-ray penumbral imaging over conventional Fraunhofer and photon limited pinhole imaging and showcase how internal hot spot microstructures can be resolved.

  5. Synchrotron hard X-ray imaging of shock-compressed metal powders

    Science.gov (United States)

    Rutherford, Michael E.; Chapman, David J.; Collinson, Mark A.; Jones, David R.; Music, Jasmina; Stafford, Samuel J. P.; Tear, Gareth R.; White, Thomas G.; Winters, John B. R.; Drakopoulos, Michael; Eakins, Daniel E.

    2015-06-01

    This poster will present the application of a new, high-energy (50 to 250 keV) synchrotron X-ray radiography technique to the study of shock-compressed granular materials. Following plate-impact loading, transmission radiography was used to quantitatively observe the compaction and release processes in a range of high-Z metal powders (e.g. Fe, Ni, Cu). By comparing the predictions of 3D numerical models initialized from X-ray tomograms-captured prior to loading-with experimental results, this research represents a new approach to refining mesoscopic compaction models. The authors gratefully acknowledge the ongoing support of Imperial College London, EPSRC, STFC and the Diamond Light Source, and AWE Plc.

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

    DEFF Research Database (Denmark)

    Frankær, Christian Grundahl

    This thesis presents thework on combining complementary X-rays techniques for studying the structures of proteins and other biomaterials, and consists of three different projects: (i) Characterization of protein powders with X-ray powder diffraction (XRPD). (ii) The combination of X-ray...... crystallography and X-ray absorption spectroscopy (XAS) applied to studying different hexameric insulin conformations. (iii) The structures of polymorphs of strontium ranelate and the distribution of strontium in bone tissue. A procedure for fast identification and verification of protein powders using XRPD...... was correction for disordered bulk-solvent, but also correction for background and optimization of unit cell parameters have to be taken into account. A sample holder was designed for collecting powder diffraction data on a standard laboratory X-ray powder diffractometer. The background was reduced by use...

  7. Novel energy resolving x-ray pinhole camera on Alcator C-Moda)

    Science.gov (United States)

    Pablant, N. A.; Delgado-Aparicio, L.; Bitter, M.; Brandstetter, S.; Eikenberry, E.; Ellis, R.; Hill, K. W.; Hofer, P.; Schneebeli, M.

    2012-10-01

    A new energy resolving x-ray pinhole camera has been recently installed on Alcator C-Mod. This diagnostic is capable of 1D or 2D imaging with a spatial resolution of ≈1 cm, an energy resolution of ≈1 keV in the range of 3.5-15 keV and a maximum time resolution of 5 ms. A novel use of a Pilatus 2 hybrid-pixel x-ray detector [P. Kraft et al., J. Synchrotron Rad. 16, 368 (2009), 10.1107/S0909049509009911] is employed in which the lower energy threshold of individual pixels is adjusted, allowing regions of a single detector to be sensitive to different x-ray energy ranges. Development of this new detector calibration technique was done as a collaboration between PPPL and Dectris Ltd. The calibration procedure is described, and the energy resolution of the detector is characterized. Initial data from this installation on Alcator C-Mod is presented. This diagnostic provides line-integrated measurements of impurity emission which can be used to determine impurity concentrations as well as the electron energy distribution.

  8. Element-resolved x-ray ferrimagnetic and ferromagnetic resonance spectroscopy

    International Nuclear Information System (INIS)

    Boero, G; Mouaziz, S; Rusponi, S; Bencok, P; Nolting, F; Stepanow, S; Gambardella, P

    2008-01-01

    We report on the measurement of element-specific magnetic resonance spectra at gigahertz frequencies using x-ray magnetic circular dichroism (XMCD). We investigate the ferrimagnetic precession of Gd and Fe ions in Gd-substituted yttrium iron garnet, showing that the resonant field and linewidth of Gd precisely coincide with Fe up to the nonlinear regime of parametric excitations. The opposite sign of the Gd x-ray magnetic resonance signal with respect to Fe is consistent with dynamic antiferromagnetic alignment of the two ionic species. Further, we investigate a bilayer metal film, Ni 80 Fe 20 (5 nm)/Ni(50 nm), where the coupled resonance modes of Ni and Ni 80 Fe 20 are separately resolved, revealing shifts in the resonance fields of individual layers but no mutual driving effects. Energy-dependent dynamic XMCD measurements are introduced, combining x-ray absorption and magnetic resonance spectroscopies

  9. Time-resolved X-ray diffraction study on superconducting YBa{sub 2}Cu{sub 3}O{sub 7} epitaxially grown on SrTiO{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Luebcke, A.

    2007-07-01

    In this PhD thesis time-resolved X-ray diffraction in optical pump - X-ray probe scheme was applied for the first time to a High-Temperature Superconductor in the superconducting state. The aim was to study the possible lattice response to optical Cooper pair breaking. As sample a thin YBa{sub 2}Cu{sub 3}O{sub 7} film with a superconducting transition temperature of T{sub c}=90 K, epitaxially grown on a SrTiO{sub 3} single crystal was used. (orig.)

  10. Two-dimensional time-resolved X-ray diffraction study of directional solidification in steels

    International Nuclear Information System (INIS)

    Yonemura, Mitsuharu

    2009-01-01

    Full text: The high intensity heat source used for fusion welding creates steep thermal gradients of 100 degree C/s from 1800 degree Celsius. Further, the influence of a preferred orientation is serious for observation of a directional solidification that follows the dendrite growth along the direction toward the moving heat source. Therefore, we observed the rapid solidification of weld metal at a time resolution of 0.01∼0.1seconds by the Two-Dimensional Time-Resolved X-ray Diffraction (2DTRXRD) system for real welding. The diffraction ring was dynamically observed by 2DTRXRD during arc-passing over the irradiation area of X-ray with synchrotron energy of 18 KeV. The arc power output was 10 V - 150 A, and a scan speed of the arc was 1.0 mm/s. The temperature rise of instruments was suppressed by the water-cooled copper plate under the sample. Further, the temperature distribution of the weld metal was measured by the thermocouple and related to the diffraction patterns. Consequently, solidification and solid phase transformation of low carbon steels and stainless steels were observed during rapid cooling by 2DTRXRD. In the low-carbon steel, the microstructure is formed in the 2 step process; (i) formation of crystallites and (ii) increase of crystallinity. In the stainless steel, the irregular interface layer of σ/y in the quenched metal after solidification is expected that it is easy for dendrites to move at the lower temperature. In the carbide precipitation stainless steel, it is easy for NbC to grow on σ phase with a little under cooling. Further, a mist-like pattern, which differs from the halo-pattern, in the fusion zone gave some indication of the possibilities to observe the nucleation and the early solidification by 2DTRXRD. (author)

  11. Structure solution from powder neutron and x-ray diffraction data: getting the best of both worlds

    International Nuclear Information System (INIS)

    Hunter, B.A.

    2000-01-01

    Full text: Powder diffraction methods have traditionally been used in three main areas: phase identification and quantification, lattice parameter determination and structure refinement. Until recently structure solution has been the almost exclusive domain of single crystal diffraction methods, predominantly using x-rays. The increasing use of synchrotron and neutron sources, and the unrelenting advances in computing hardware and software means that powder methods are challenging single crystal methods as a practical method for structure solution, especially when single crystal method can not be applied. It is known that structural refinements from a known starting structure using combined X-ray and neutron data sets are capable of providing highly accurate structures. Likewise, using combined x-ray and neutron powder diffraction data in the structure solution process should also be a powerful technique, although to date no one is pursuing this methodology. This paper present examples of solutions to the problem. Namely we are using high resolution powder X-ray and neutron methods to solve the structures of molecular materials and minerals, then refining the structures using both sets of data. In this way we exploit the advantages of both methods while minimising the disadvantages. We present our solution for a small amino acid structure, a metalorganic and a mineral structure

  12. Powder X-ray diffraction study af alkali alanates

    DEFF Research Database (Denmark)

    Cao, Thao; Mosegaard Arnbjerg, Lene; Jensen, Torben René

    Powder X-ray diffraction study of alkali alanates Thao Cao, Lene Arnbjerg, Torben R. Jensen. Center for Materials Crystallography (CMC), Center for Energy Materials (CEM), iNANO and Department of Chemistry, Aarhus University, DK-8000, Denmark. Abstract: To meet the energy demand in the future...... for mobile applications, new materials with high gravimetric and volumetric storage capacity of hydrogen have to be developed. Alkali alanates are promising for hydrogen storage materials. Sodium alanate stores hydrogen reversibly at moderate conditions when catalysed with, e.g. titanium, whereas potassium...

  13. Streaked, x-ray-transmission-grating spectrometer

    International Nuclear Information System (INIS)

    Ceglio, N.M.; Roth, M.; Hawryluk, A.M.

    1981-08-01

    A free standing x-ray transmission grating has been coupled with a soft x-ray streak camera to produce a time resolved x-ray spectrometer. The instrument has a temporal resolution of approx. 20 psec, is capable of covering a broad spectral range, 2 to 120 A, has high sensitivity, and is simple to use requiring no complex alignment procedure. In recent laser fusion experiments the spectrometer successfully recorded time resolved spectra over the range 10 to 120 A with a spectral resolving power, lambda/Δlambda of 4 to 50, limited primarily by source size and collimation effects

  14. Novel spectroscopic techniques with using soft x-ray

    International Nuclear Information System (INIS)

    Gejo, Tatsuo

    2010-01-01

    Recent progress of experimental techniques related to synchrotron radiation makes possible of detail investigation of molecular dynamics after irradiation of soft X-ray. We introduce several novel spectroscopic techniques with using soft X-ray: Symmetry-resolved zero kinetic energy electron spectroscopy, symmetry-resolved metastable photofragment spectroscopy, soft X-ray emission spectroscopy, time-resolved fluorescence spectroscopy, and time-resolved-fluorescence mass-selected-ion coincidence spectroscopy. We also show new techniques performed by other groups at BL27SU in SPring-8. (author)

  15. Mechanical design of a high-resolution x-ray powder diffractometer at the Advanced Photon Source.

    Energy Technology Data Exchange (ETDEWEB)

    Shu, D.; Lee, P.; Preissner, C.; Ramanathan, M.; Beno, M.; VonDreele, R.; Ranay, R.; Ribaud, L.; Kurtz, C.; Jiao, X.; Kline, D.; Jemian, P.; Toby, B.

    2007-01-01

    A novel high-resolution x-ray powder diffractometer has been designed and commissioned at the bending magnet beamline 11-BM at the Advanced Photon Source (APS), Argonne National Laboratory (ANL). This state-of-the-art instrument is designed to meet challenging mechanical and optical specifications for producing high-quality powder diffraction data with high throughput. The 2600 mm (H) X 2100 mm (L) X 1700 mm (W) diffractometer consists of five subassemblies: a customized two-circle goniometer with a 3-D adjustable supporting base; a twelve-channel high-resolution crystal analyzer system with an array of precision x-ray slits; a manipulator system for a twelve scintillator x-ray detectors; a 4-D sample manipulator with cryo-cooling capability; and a robot-based sample exchange automation system. The mechanical design of the diffractometer as well as the test results of its positioning performance are presented in this paper.

  16. Mechanical design of a high-resolution x-ray powder diffractometer at the Advanced Photon Source

    International Nuclear Information System (INIS)

    Shu, D.; Lee, P.; Preissner, C.; Ramanathan, M.; Beno, M.; VonDreele, R.; Ranay, R.; Ribaud, L.; Kurtz, C.; Jiao, X.; Kline, D.; Jemian, P.; Toby, B.

    2007-01-01

    A novel high-resolution x-ray powder diffractometer has been designed and commissioned at the bending magnet beamline 11-BM at the Advanced Photon Source (APS), Argonne National Laboratory (ANL). This state-of-the-art instrument is designed to meet challenging mechanical and optical specifications for producing high-quality powder diffraction data with high throughput. The 2600 mm (H) X 2100 mm (L) X 1700 mm (W) diffractometer consists of five subassemblies: a customized two-circle goniometer with a 3-D adjustable supporting base; a twelve-channel high-resolution crystal analyzer system with an array of precision x-ray slits; a manipulator system for a twelve scintillator x-ray detectors; a 4-D sample manipulator with cryo-cooling capability; and a robot-based sample exchange automation system. The mechanical design of the diffractometer as well as the test results of its positioning performance are presented in this paper.

  17. Acemetacin cocrystal structures by powder X-ray diffraction

    Science.gov (United States)

    Bolla, Geetha

    2017-01-01

    Cocrystals of acemetacin drug (ACM) with nicotinamide (NAM), p-aminobenzoic acid (PABA), valerolactam (VLM) and 2-pyridone (2HP) were prepared by melt crystallization and their X-ray crystal structures determined by high-resolution powder X-ray diffraction. The powerful technique of structure determination from powder data (SDPD) provided details of molecular packing and hydrogen bonding in pharmaceutical cocrystals of acemetacin. ACM–NAM occurs in anhydrate and hydrate forms, whereas the other structures crystallized in a single crystalline form. The carboxylic acid group of ACM forms theacid–amide dimer three-point synthon R 3 2(9)R 2 2(8)R 3 2(9) with three different syn amides (VLM, 2HP and caprolactam). The conformations of the ACM molecule observed in the crystal structures differ mainly in the mutual orientation of chlorobenzene fragment and the neighboring methyl group, being anti (type I) or syn (type II). ACM hydrate, ACM—NAM, ACM–NAM-hydrate and the piperazine salt of ACM exhibit the type I conformation, whereas ACM polymorphs and other cocrystals adopt the ACM type II conformation. Hydrogen-bond interactions in all the crystal structures were quantified by calculating their molecular electrostatic potential (MEP) surfaces. Hirshfeld surface analysis of the cocrystal surfaces shows that about 50% of the contribution is due to a combination of strong and weak O⋯H, N⋯H, Cl⋯H and C⋯H interactions. The physicochemical properties of these cocrystals are under study. PMID:28512568

  18. Acemetacin cocrystal structures by powder X-ray diffraction

    Directory of Open Access Journals (Sweden)

    Geetha Bolla

    2017-05-01

    Full Text Available Cocrystals of acemetacin drug (ACM with nicotinamide (NAM, p-aminobenzoic acid (PABA, valerolactam (VLM and 2-pyridone (2HP were prepared by melt crystallization and their X-ray crystal structures determined by high-resolution powder X-ray diffraction. The powerful technique of structure determination from powder data (SDPD provided details of molecular packing and hydrogen bonding in pharmaceutical cocrystals of acemetacin. ACM–NAM occurs in anhydrate and hydrate forms, whereas the other structures crystallized in a single crystalline form. The carboxylic acid group of ACM forms theacid–amide dimer three-point synthon R32(9R22(8R32(9 with three different syn amides (VLM, 2HP and caprolactam. The conformations of the ACM molecule observed in the crystal structures differ mainly in the mutual orientation of chlorobenzene fragment and the neighboring methyl group, being anti (type I or syn (type II. ACM hydrate, ACM—NAM, ACM–NAM-hydrate and the piperazine salt of ACM exhibit the type I conformation, whereas ACM polymorphs and other cocrystals adopt the ACM type II conformation. Hydrogen-bond interactions in all the crystal structures were quantified by calculating their molecular electrostatic potential (MEP surfaces. Hirshfeld surface analysis of the cocrystal surfaces shows that about 50% of the contribution is due to a combination of strong and weak O...H, N...H, Cl...H and C...H interactions. The physicochemical properties of these cocrystals are under study.

  19. Study of properties of chemically modified samples of halloysite mineral with X-ray fluorescence and X-ray powder diffraction methods

    International Nuclear Information System (INIS)

    Banaś, D.; Kubala-Kukuś, A.; Braziewicz, J.; Majewska, U.; Pajek, M.; Wudarczyk-Moćko, J.; Czech, K.; Garnuszek, M.; Słomkiewicz, P.; Szczepanik, B.

    2013-01-01

    Elemental and chemical composition of raw and activated samples of halloysite mineral using wavelength dispersive X-ray fluorescence (WDXRF), total reflection X-ray fluorescence (TXRF) and X-ray powder diffraction (XRPD) methods were determined. As the result, it has been shown that application of the complementary X-ray spectrometry techniques allows very precise observation of changes in composition of halloysite mineral samples caused by its chemical modifications. Sample preparation procedure and usability of the research methods applied are described in details. Procedure of activation of raw halloysite mineral samples by etching them in sulfuric acid of various concentrations has been described and discussed. The ability of the samples to adsorb lead from intentionally contaminated water was tested and confirmed. - Author-Highlights: • We measured elemental and chemical composition of raw and activated halloysite mineral samples. • We showed that X-ray techniques allow precise study of changes in the sample composition. • We describe procedure of activation of the samples by etching them in sulfuric acid. • We tested ability of halloysite mineral to absorb lead from contaminated water

  20. X-Ray Powder Diffraction with Guinier - Haegg Focusing Cameras

    Energy Technology Data Exchange (ETDEWEB)

    Brown, Allan

    1970-12-15

    The Guinier - Haegg focusing camera is discussed with reference to its use as an instrument for rapid phase analysis. An actual camera and the alignment procedure employed in its setting up are described. The results obtained with the instrument are compared with those obtained with Debye - Scherrer cameras and powder diffractometers. Exposure times of 15 - 30 minutes with compounds of simple structure are roughly one-sixth of those required for Debye - Scherrer patterns. Coupled with the lower background resulting from the use of a monochromatic X-ray beam, the shorter exposure time gives a ten-fold increase in sensitivity for the detection of minor phases as compared with the Debye - Scherrer camera. Attention is paid to the precautions taken to obtain reliable Bragg angles from Guinier - Haegg film measurements, with particular reference to calibration procedures. The evaluation of unit cell parameters from Guinier - Haegg data is discussed together with the application of tests for the presence of angle-dependent systematic errors. It is concluded that with proper calibration procedures and least squares treatment of the data, accuracies of the order of 0.005% are attainable. A compilation of diffraction data for a number of compounds examined in the Active Central Laboratory at Studsvik is presented to exemplify the scope of this type of powder camera.

  1. X-Ray Powder Diffraction with Guinier - Haegg Focusing Cameras

    International Nuclear Information System (INIS)

    Brown, Allan

    1970-12-01

    The Guinier - Haegg focusing camera is discussed with reference to its use as an instrument for rapid phase analysis. An actual camera and the alignment procedure employed in its setting up are described. The results obtained with the instrument are compared with those obtained with Debye - Scherrer cameras and powder diffractometers. Exposure times of 15 - 30 minutes with compounds of simple structure are roughly one-sixth of those required for Debye - Scherrer patterns. Coupled with the lower background resulting from the use of a monochromatic X-ray beam, the shorter exposure time gives a ten-fold increase in sensitivity for the detection of minor phases as compared with the Debye - Scherrer camera. Attention is paid to the precautions taken to obtain reliable Bragg angles from Guinier - Haegg film measurements, with particular reference to calibration procedures. The evaluation of unit cell parameters from Guinier - Haegg data is discussed together with the application of tests for the presence of angle-dependent systematic errors. It is concluded that with proper calibration procedures and least squares treatment of the data, accuracies of the order of 0.005% are attainable. A compilation of diffraction data for a number of compounds examined in the Active Central Laboratory at Studsvik is presented to exemplify the scope of this type of powder camera

  2. Time-resolved Neutron Powder Diffraction

    International Nuclear Information System (INIS)

    Pannetier, J.

    1986-01-01

    The use of a high-flux neutron source together with a large position sensitive detector (PSD) allows a powder diffraction pattern to be recorded at a time-scale of a few minutes so that crystalline systems under non-equilibrium conditions may now conveniently be investigated. This introduces a new dimension into powder diffraction (the time and transient phenomena like heterogeneous chemical reactions can now be easily studied. The instrumental parameters relevant for the design of such time-dependent experiments are briefly surveyed and the current limits of the method are discussed. The applications are illustrated by two kinds of experiment in the field of inorganic solid state chemistry: true kinetic studies of heterogeneous chemical reactions and thermodiffractometry experiments

  3. Time-resolved pump-probe experiments at the LCLS

    Energy Technology Data Exchange (ETDEWEB)

    Glownia, James; /SLAC /Stanford U., Appl. Phys. Dept.; Cryan, J.; /SLAC /Stanford U., Phys. Dept.; Andreasson, J.; /Uppsala U.; Belkacem, A.; /LBNL, Berkeley; Berrah, N.; /Western Michigan U.; Blaga, C.L.; /Ohio State U.; Bostedt, C.; Bozek, J.; /SLAC; DiMauro, L.F.; /Ohio State U.; Fang, L.; /Western Michigan U.; Frisch, J.; /SLAC; Gessner, O.; /LBNL; Guhr, M.; /SLAC; Hajdu, J.; /Uppsala U.; Hertlein, M.P.; /LBNL; Hoener, M.; /Western Michigan U. /LBNL; Huang, G.; Kornilov, O.; /LBNL; Marangos, J.P.; /Imperial Coll., London; March, A.M.; /Argonne; McFarland, B.K.; /SLAC /Stanford U., Phys. Dept. /SLAC /IRAMIS, Saclay /Stanford U., Phys. Dept. /Georgia Tech /Argonne /Kansas State U. /SLAC /Stanford U., Phys. Dept. /SLAC /Stanford U., Appl. Phys. Dept. /Stanford U., Appl. Phys. Dept. /SLAC /LBNL /Argonne /SLAC /SLAC /Stanford U., Appl. Phys. Dept. /Stanford U., Phys. Dept.

    2011-08-12

    The first time-resolved x-ray/optical pump-probe experiments at the SLAC Linac Coherent Light Source (LCLS) used a combination of feedback methods and post-analysis binning techniques to synchronize an ultrafast optical laser to the linac-based x-ray laser. Transient molecular nitrogen alignment revival features were resolved in time-dependent x-ray-induced fragmentation spectra. These alignment features were used to find the temporal overlap of the pump and probe pulses. The strong-field dissociation of x-ray generated quasi-bound molecular dications was used to establish the residual timing jitter. This analysis shows that the relative arrival time of the Ti:Sapphire laser and the x-ray pulses had a distribution with a standard deviation of approximately 120 fs. The largest contribution to the jitter noise spectrum was the locking of the laser oscillator to the reference RF of the accelerator, which suggests that simple technical improvements could reduce the jitter to better than 50 fs.

  4. Time-resolved X-ray diffraction studies of laser-induced acoustic wave propagation in bilayer metallic thin crystals

    Energy Technology Data Exchange (ETDEWEB)

    Er, Ali Oguz [Department of Physics and Astronomy, Western Kentucky University, Bowling Green, Kentucky 42101 (United States); Tang, Jau, E-mail: jautang@gate.sinica.edu.tw, E-mail: prentzepis@ece.tamu.edu [Research Center for Applied Sciences Academia Sinica, Taipei, Taiwan (China); Chen, Jie [Key Laboratory for Laser Plasmas (Ministry of Education) and Department of Physics and Astronomy, Shanghai Jiao Tong University, Shanghai 200240 (China); Rentzepis, Peter M., E-mail: jautang@gate.sinica.edu.tw, E-mail: prentzepis@ece.tamu.edu [Department of Electrical and Computer Engineering, Texas A and M University, College Station, Texas 77843 (United States)

    2014-09-07

    Phonon propagation across the interface of a Cu/Ag(111) bilayer and transient lattice disorder, induced by a femtosecond 267 nm pulse, in Ag(111) crystal have been measured by means of time resolved X-ray diffraction. A “blast” force due to thermal stress induced by suddenly heated electrons is formed within two picoseconds after excitation and its “blast wave” propagation through the interface and Ag (111) crystal was monitored by the shift and broadening of the rocking curve, I vs. ω, as a function of time after excitation. Lattice disorder, contraction and expansion as well as thermal strain formation and wave propagation have also been measured. The experimental data and mechanism proposed are supported by theoretical simulations.

  5. Experimental set-up for time resolved small angle X-ray scattering studies of nanoparticles formation using a free-jet micromixer

    Energy Technology Data Exchange (ETDEWEB)

    Marmiroli, Benedetta [Institute for Biophysics and Nanosystem Research, Austrian Academy of Science, Schmiedlstrasse 6, Graz (Austria); Grenci, Gianluca [TASC INFM/CNR, SS 14 km 163.5, Basovizza, TS (Italy); Cacho-Nerin, Fernando; Sartori, Barbara; Laggner, Peter [Institute for Biophysics and Nanosystem Research, Austrian Academy of Science, Schmiedlstrasse 6, Graz (Austria); Businaro, Luca [TASC INFM/CNR, SS 14 km 163.5, Basovizza, TS (Italy); Amenitsch, Heinz, E-mail: heinz.amenitsch@elettra.trieste.i [Institute for Biophysics and Nanosystem Research, Austrian Academy of Science, Schmiedlstrasse 6, Graz (Austria)

    2010-02-15

    Recently, we have designed, fabricated and tested a free-jet micromixer for time resolved small angle X-ray scattering (SAXS) studies of nanoparticles formation in the <100 mus time range. The microjet has a diameter of 25 mum and a time of first accessible measurement of 75 mus has been obtained. This result can still be improved. In this communication, we present a method to estimate whether a given chemical or biological reaction can be investigated with the micromixer, and to optimize the beam size for the measurement at the chosen SAXS beamline. Moreover, we describe a system based on stereoscopic imaging which allows the alignment of the jet with the X-ray beam with a precision of 20 mum. The proposed experimental procedures have been successfully employed to observe the formation of calcium carbonate (CaCO{sub 3}) nanoparticles from the reaction of sodium carbonate (Na{sub 2}CO{sub 3}) and calcium chloride (CaCl{sub 2}). The induction time has been estimated in the order of 200 mus and the determined radius of the particles is about 14 nm.

  6. X-Ray Scattering Applications Using Pulsed X-Ray Sources

    Energy Technology Data Exchange (ETDEWEB)

    Larson, B.C.

    1999-05-23

    Pulsed x-ray sources have been used in transient structural phenomena investigations for over fifty years; however, until the advent of synchrotrons sources and the development of table-top picosecond lasers, general access to ligh temporal resolution x-ray diffraction was relatively limited. Advances in diffraction techniques, sample excitation schemes, and detector systems, in addition to IncEased access to pulsed sources, have ld tO what is now a diverse and growing array of pulsed-source measurement applications. A survey of time-resolved investigations using pulsed x-ray sources is presented and research opportunities using both present and planned pulsed x-ray sources are discussed.

  7. Determination of Ni(II) crystal structure by powder x-ray diffraction ...

    African Journals Online (AJOL)

    X-ray powder diffraction pattern was used to determine the length of the unit cell, “a”, the lattice structure type, and the number of atoms per unit cell of Ni(II) crystal. The “a” value was determined to be 23.66 ± 0.005 Å, particle size of 34.87 nm, volume 13.24 Å and Strain value ε = 9.8 x 10-3. The cell search on PXRD patterns ...

  8. In situ time-resolved X-ray near-edge absorption spectroscopy of selenite reduction by siderite

    International Nuclear Information System (INIS)

    Badaut, V.; Schlegel, M.L.; Descostes, M.; Moutiers, G.

    2012-01-01

    The reduction oxidation-reaction between aqueous selenite (SeO 3 2- ) and siderite (FeCO 3 (s)) was monitored by in situ, time-resolved X-ray absorption near-edge structure (XANES) spectroscopy at the selenium K edge in a controlled electrochemical environment. Spectral evolutions showed that more than 60% of selenite was reduced at the siderite surface after 20 h of experiment, at which time the reaction was still incomplete. Fitting of XANES spectra by linear combination of reference spectra showed that selenite reaction with siderite is essentially a two-step process, selenite ions being immobilized on siderite surface prior to their reduction. A kinetic model of the reduction step is proposed, allowing to identify the specific contribution of surface reduction. These results have strong implications for the retention of selenite by corrosion products in nuclear waste repositories and in a larger extent for the fate of selenium in the environment. (authors)

  9. Computer x-ray powder diffraction patterns and densities for corundum, aluminium, zirconium, delta-UZr2 and the zirconium hydrides

    International Nuclear Information System (INIS)

    Ferguson, I.F.

    1976-11-01

    The computer-calculated X-ray powder diffraction patterns and theoretical densities of α-Al 2 O 3 ; Al; α-Zr; β-Zr; delta-UZr 2 ; γ, delta - and epsilon-zirconium hydrides are presented. Brief comments are given on some of the published X-ray powder diffraction data on these phases. (author)

  10. Powder X-ray diffraction laboratory, Reston, Virginia

    Science.gov (United States)

    Piatak, Nadine M.; Dulong, Frank T.; Jackson, John C.; Folger, Helen W.

    2014-01-01

    The powder x-ray diffraction (XRD) laboratory is managed jointly by the Eastern Mineral and Environmental Resources and Eastern Energy Resources Science Centers. Laboratory scientists collaborate on a wide variety of research problems involving other U.S. Geological Survey (USGS) science centers and government agencies, universities, and industry. Capabilities include identification and quantification of crystalline and amorphous phases, and crystallographic and atomic structure analysis for a wide variety of sample media. Customized laboratory procedures and analyses commonly are used to characterize non-routine samples including, but not limited to, organic and inorganic components in petroleum source rocks, ore and mine waste, clay minerals, and glassy phases. Procedures can be adapted to meet a variety of research objectives.

  11. Mesoscopic structural phase progression in photo-excited VO2 revealed by time-resolved x-ray diffraction microscopy

    Science.gov (United States)

    Zhu, Yi; Cai, Zhonghou; Chen, Pice; Zhang, Qingteng; Highland, Matthew J.; Jung, Il Woong; Walko, Donald A.; Dufresne, Eric M.; Jeong, Jaewoo; Samant, Mahesh G.; Parkin, Stuart S. P.; Freeland, John W.; Evans, Paul G.; Wen, Haidan

    2016-02-01

    Dynamical phase separation during a solid-solid phase transition poses a challenge for understanding the fundamental processes in correlated materials. Critical information underlying a phase transition, such as localized phase competition, is difficult to reveal by measurements that are spatially averaged over many phase separated regions. The ability to simultaneously track the spatial and temporal evolution of such systems is essential to understanding mesoscopic processes during a phase transition. Using state-of-the-art time-resolved hard x-ray diffraction microscopy, we directly visualize the structural phase progression in a VO2 film upon photoexcitation. Following a homogenous in-plane optical excitation, the phase transformation is initiated at discrete sites and completed by the growth of one lattice structure into the other, instead of a simultaneous isotropic lattice symmetry change. The time-dependent x-ray diffraction spatial maps show that the in-plane phase progression in laser-superheated VO2 is via a displacive lattice transformation as a result of relaxation from an excited monoclinic phase into a rutile phase. The speed of the phase front progression is quantitatively measured, and is faster than the process driven by in-plane thermal diffusion but slower than the sound speed in VO2. The direct visualization of localized structural changes in the time domain opens a new avenue to study mesoscopic processes in driven systems.

  12. Fast X-ray powder diffraction on I11 at Diamond.

    Science.gov (United States)

    Thompson, Stephen P; Parker, Julia E; Marchal, Julien; Potter, Jonathan; Birt, Adrian; Yuan, Fajin; Fearn, Richard D; Lennie, Alistair R; Street, Steven R; Tang, Chiu C

    2011-07-01

    The commissioning and performance characterization of a position-sensitive detector designed for fast X-ray powder diffraction experiments on beamline I11 at Diamond Light Source are described. The detecting elements comprise 18 detector-readout modules of MYTHEN-II silicon strip technology tiled to provide 90° coverage in 2θ. The modules are located in a rigid housing custom designed at Diamond with control of the device fully integrated into the beamline data acquisition environment. The detector is mounted on the I11 three-circle powder diffractometer to provide an intrinsic resolution of Δ2θ approximately equal to 0.004°. The results of commissioning and performance measurements using reference samples (Si and AgI) are presented, along with new results from scientific experiments selected to demonstrate the suitability of this facility for powder diffraction experiments where conventional angle scanning is too slow to capture rapid structural changes. The real-time dehydrogenation of MgH(2), a potential hydrogen storage compound, is investigated along with ultrafast high-throughput measurements to determine the crystallite quality of different samples of the metastable carbonate phase vaterite (CaCO(3)) precipitated and stabilized in the presence of amino acid molecules in a biomimetic synthesis process.

  13. Two-dimensional time-resolved X-ray diffraction study of liquid/solid fraction and solid particle size in Fe-C binary system with an electrostatic levitator furnace

    International Nuclear Information System (INIS)

    Yonemura, M; Okada, J; Ishikawa, T; Nanao, S; Watanabe, Y; Shobu, T; Toyokawa, H

    2013-01-01

    Liquid state provides functions such as matter transport or a reaction field and plays an important role in manufacturing processes such as refining, forging or welding. However, experimental procedures are significantly difficult for an observation of solidification process of iron and iron-based alloys in order to identify rapid transformations subjected to fast temperature evolution. Therefore, in order to study the solidification in iron and iron-based alloys, we considered a combination of high energy X-ray diffraction measurements and an electrostatic levitation method (ESL). In order to analyze the liquid/solid fraction, the solidification of melted spherical specimens was measured at a time resolution of 0.1 seconds during rapid cooling using the two-dimensional time-resolved X-ray diffraction. Furthermore, the observation of particle sizes and phase identification was performed on a trial basis using X-ray small angle scattering with X-ray diffraction.

  14. A standardless method of quantitative ceramic analysis using X-ray powder diffraction

    International Nuclear Information System (INIS)

    Mazumdar, S.

    1999-01-01

    A new procedure using X-ray powder diffraction data for quantitative estimation of the crystalline as well as the amorphous phase in ceramics is described. Classification of the crystalline and amorphous X-ray scattering was achieved by comparison of the slopes at two successive points of the powder pattern at scattering angles at which the crystalline and amorphous phases superimpose. If the second slope exceeds the first by a stipulated value, the intensity is taken as crystalline; otherwise the scattering is considered as amorphous. Crystalline phase analysis is obtained by linear programming techniques using the concept that each observed X-ray diffraction peak has contributions from n component phases, the proportionate analysis of which is required. The method does not require the measurement of calibration data for use as an internal standard, but knowledge of the approximate crystal structure of each phase of interest in the mixture is necessary. The technique is also helpful in qualitative analysis because each suspected phase is characterized by the probability that it will be present when a reflection zone is considered in which the suspected crystalline phase could contribute. The amorphous phases are determined prior to the crystalline ones. The method is applied to ceramic materials and some results are presented. (orig.)

  15. Laser wakefield generated X-ray probe for femtosecond time-resolved measurements of ionization states of warm dense aluminum

    Energy Technology Data Exchange (ETDEWEB)

    Mo, M. Z.; Chen, Z.; Tsui, Y. Y.; Fedosejevs, R. [Department of Electrical and Computer Engineering, University of Alberta, Edmonton, Alberta T6G 2V4 (Canada); Fourmaux, S.; Saraf, A.; Otani, K.; Kieffer, J. C. [INRS-EMT, Université du Québec, 1650 Lionel Boulet, Varennes, Québec J3X 1S2 (Canada); Ng, A. [Department of Physics and Astronomy, University of British Columbia, British Columbia V6T 1Z1 (Canada)

    2013-12-15

    We have developed a laser wakefield generated X-ray probe to directly measure the temporal evolution of the ionization states in warm dense aluminum by means of absorption spectroscopy. As a promising alternative to the free electron excited X-ray sources, Betatron X-ray radiation, with femtosecond pulse duration, provides a new technique to diagnose femtosecond to picosecond transitions in the atomic structure. The X-ray probe system consists of an adjustable Kirkpatrick-Baez (KB) microscope for focusing the Betatron emission to a small probe spot on the sample being measured, and a flat Potassium Acid Phthalate Bragg crystal spectrometer to measure the transmitted X-ray spectrum in the region of the aluminum K-edge absorption lines. An X-ray focal spot size of around 50 μm was achieved after reflection from the platinum-coated 10-cm-long KB microscope mirrors. Shot to shot positioning stability of the Betatron radiation was measured resulting in an rms shot to shot variation in spatial pointing on the sample of 16 μm. The entire probe setup had a spectral resolution of ∼1.5 eV, a detection bandwidth of ∼24 eV, and an overall photon throughput efficiency of the order of 10{sup −5}. Approximately 10 photons were detected by the X-ray CCD per laser shot within the spectrally resolved detection band. Thus, it is expected that hundreds of shots will be required per absorption spectrum to clearly observe the K-shell absorption features expected from the ionization states of the warm dense aluminum.

  16. Evaluation of high packing density powder X-ray screens by Monte Carlo methods

    International Nuclear Information System (INIS)

    Liaparinos, P.; Kandarakis, I.; Cavouras, D.; Kalivas, N.; Delis, H.; Panayiotakis, G.

    2007-01-01

    Phosphor materials are employed in intensifying screens of both digital and conventional X-ray imaging detectors. High packing density powder screens have been developed (e.g. screens in ceramic form) exhibiting high-resolution and light emission properties, and thus contributing to improved image transfer characteristics and higher radiation to light conversion efficiency. For the present study, a custom Monte Carlo simulation program was used in order to examine the performance of ceramic powder screens, under various radiographic conditions. The model was developed using Mie scattering theory for the description of light interactions, based on the physical characteristics (e.g. complex refractive index, light wavelength) of the phosphor material. Monte Carlo simulations were carried out assuming: (a) X-ray photon energy ranging from 18 up to 49 keV, (b) Gd 2 O 2 S:Tb phosphor material with packing density of 70% and grain size of 7 μm and (c) phosphor thickness ranging between 30 and 70 mg/cm 2 . The variation of the Modulation Transfer Function (MTF) and the Luminescence Efficiency (LE) with respect to the X-ray energy and the phosphor thickness was evaluated. Both aforementioned imaging characteristics were shown to take high values at 49 keV X-ray energy and 70 mg/cm 2 phosphor thickness. It was found that high packing density screens may be appropriate for use in medical radiographic systems

  17. Measuring the x-ray resolving power of bent potassium acid phthalate diffraction crystals

    International Nuclear Information System (INIS)

    Haugh, M. J.; Jacoby, K. D.; Wu, M.; Loisel, G. P.

    2014-01-01

    This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals that we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories in Albuquerque, New Mexico. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a double crystal diffractometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed

  18. Measuring the x-ray resolving power of bent potassium acid phthalate diffraction crystals

    Energy Technology Data Exchange (ETDEWEB)

    Haugh, M. J., E-mail: haughmj@nv.doe.gov; Jacoby, K. D. [National Security Technologies, LLC, Livermore, California 94550 (United States); Wu, M.; Loisel, G. P. [Sandia National Laboratories, Albuquerque, New Mexico 87123 (United States)

    2014-11-15

    This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals that we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories in Albuquerque, New Mexico. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a double crystal diffractometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.

  19. Atom-resolving x-ray holography

    International Nuclear Information System (INIS)

    Adams, B.; Hiort, T.; Materlik, G.; Nishino, Y.; Novikov, D. V.

    2000-01-01

    The current state of atomic resolution x-ray holography is discussed on the basis of theory and experimental results. X-ray holography is theoretically described in quantum theory. Presently-used experimental implementations are shown together with the data analysis used. Reconstructions of experimental and simulated holograms are compared for a Cu 3 Au crystal structure. Rigorous experimental realizations of pure direct and reciprocal x-ray holography methods are demonstrated, and future developments and applications of the method are suggested

  20. Time-resolved studies

    International Nuclear Information System (INIS)

    Mills, D.M.

    1992-01-01

    When new or more powerful probes become available that offer both shorter data-collection times and the opportunity to apply innovative approaches to established techniques, it is natural that investigators consider the feasibility of exploring the kinetics of time-evolving systems. This stimulating area of research not only can lead to insights into the metastable or excited states that a system may populate on its way to a ground state, but can also lead to a better understanding of that final state. Synchrotron radiation, with its unique properties, offers just such a tool to extend X-ray measurements from the static to the time-resolved regime. The most straight-forward application of synchrotron radiation to the study of transient phenomena is directly through the possibility of decreased data-collection times via the enormous increase in flux over that of a laboratory X-ray system. Even further increases in intensity can be obtained through the use of novel X-ray optical devices. Widebandpass monochromators, e.g., that utilize the continuous spectral distribution of synchrotron radiation, can increase flux on the sample several orders of magnitude over conventional X-ray optical systems thereby allowing a further shortening of the data-collection time. Another approach that uses the continuous spectral nature of synchrotron radiation to decrease data-collection times is the open-quote parallel data collectionclose quotes method. Using this technique, intensities as a function of X-ray energy are recorded simultaneously for all energies rather than sequentially recording data at each energy, allowing for a dramatic decrease in the data-collection time

  1. Soft X-ray images of krypton gas-puff Z-pinches

    International Nuclear Information System (INIS)

    Qiu Mengtong; Kuai Bin; Zeng Zhengzhong; Lu Min; Wang Kuilu; Qiu Aici; Zhang Mei; Luo Jianhui

    2002-01-01

    A series of experiments has been carried out on Qiang-guang I generator to study the dynamics of krypton gas-puff Z-pinches. The generator was operated at a peak current of 1.5 MA with a rise-time of 80 ns. The specific linear mass of gas liner was about 20 μg/cm in these experiments. In the diagnostic system, a four-frame x-ray framing camera and a pinhole camera were employed. A novel feature of this camera is that it can give time-resolved x-ray images with four frames and energy-resolved x-ray images with two different filters and an array of 8 pinholes integrated into one compact assemble. As a typical experimental result, an averaged radial imploding velocity of 157 km/s over 14 ns near the late phase of implosion was measured from the time-resolved x-ray images. From the time-integrated x-ray image an averaged radial convergence of 0.072 times of the original size was measured. An averaged radial expansion velocity was 130 km/s and the maximum radial convergence of 0.04 times of the original size were measured from the time-resolved x-ray images. The dominant axial wavelengths of instabilities in the plasma were between 1 and 2 mm. The change in average photons energy was observed from energy spectrum- and time-resolved x-ray images

  2. Soft X-ray Images of Krypton Gas-Puff Z-Pinches

    Institute of Scientific and Technical Information of China (English)

    邱孟通; 蒯斌; 曾正中; 吕敏; 王奎禄; 邱爱慈; 张美; 罗建辉

    2002-01-01

    A series of experiments has been carried out on Qiang-guang Ⅰ generator to study the dynamics of krypton gas-puff Z-pinches. The generator was operated at a peak current of 1.5 MA with a rise-time of 80 ns. The specific linear mass of gas liner was about 20 μg/cm in these experiments. In the diagnostic system, a four-frame x-ray framing camera and a pinhole camera were employed. A novel feature of this camera is that it can give time-resolved x-ray images with four frames and energy-resolved x-ray images with two different filters and an array of 8 pinholes integrated into one compact assemble. As a typical experimental result, an averaged radial imploding velocity of 157 km/s over 14 ns near the late phase of implosion was measured from the time-resolved x-ray images. From the time-integrated x-ray image an averaged radial convergence of 0.072 times of the original size was measured. An averaged radial expansion velocity was 130 km/s and the maximum radial convergence of 0.04 times of the original size were measured from the time-resolved x-ray images. The dominant axial wavelengths of instabilities in the plasma were between 1 and 2 mm. The change in average photons energy was observed from energy spectrum- and time-resolved x-ray images.

  3. X-ray powder crystallography with vertex instrumentation

    International Nuclear Information System (INIS)

    Chatzisotiriou, V.; Christofis, I.; Dimitriou, N.; Karvelas, S.; Karydas, A.G.; Loukas, D.; Pavlidis, A.; Spirou, S.; Dre, C.; Haralabidis, N.; Misiakos, K.; Tsoi, E.; Perdikatsis, V.; Psycharis, V.; Terzis, A.; Turchetta, R.

    1998-01-01

    An X-ray Diffractometer for Powder Crystallography is described along with experimental results and future plans. This is an intermediate instrument toward a long linear array system. Three channels of a silicon microstrip detector, are the detecting elements in the present instrument. Each detector channel is followed by a VLSI readout chain, which consists of a charge preamplifier with pulse shaping circuitry, a discriminator, and a 16-bit counter. Control and data acquisition is performed with a custom made PC readout card. A motorized goniometer scans the angle range of interest. Calibration of the system is done with reference samples and data which are captured with a one-channel conventional NaI detector. (Copyright (c) 1998 Elsevier Science B.V., Amsterdam. All rights reserved.)

  4. Space- and time-resolved diagnostics of soft x-ray emission from laser plasmas

    International Nuclear Information System (INIS)

    Richardson, M.C.; Jaanimagi, P.A.; Chen, H.

    1988-01-01

    The analysis of soft x-ray emission from plasmas created by intense short-wavelength laser radiation can provide much useful information on the density, temperature and ionization distribution of the plasma. Until recently, limitations of sensitivity and the availability of suitable x-ray optical elements have restricted studies of soft x-ray emission from laser plasmas. In this paper, the authors describe novel instrumentation which provides high sensitivity in the soft x-ray spectrum with spatial and temporal resolution in the micron and picosecond ranges respectively. These systems exploit advances made in soft x-ray optic and electro-optic technology. Their application in current studies of laser fusion, x-ray lasers, and high density atomic physics are discussed

  5. Elemental investigation of talcum baby powder by X-Ray florescence and fast neutron activation Techniques

    International Nuclear Information System (INIS)

    Hassan, M. F.; Abd El Wahab, M.; Nada, A.

    2008-01-01

    Different samples of Egyptian and Hungarian talcum powders were studied, using X-ray florescence (XRF) and Fast Neutron Activation Analysis (FNAA) techniques to ensure the safety of its use. The K (X-rays) and the gamma-rays were measured, using Si(Li) and high-purity germanium (HPGe) spectrometers to detect and determine qualitatively and quantitatively the constituents of the studied samples. The concentrations of the elements (Mg, Si, Al, Fe, Zn, and Ba) were measured and their presence was confirmed by X-ray, lifetime and/or XRF measurements. One of these samples was also studied, using the Environmental Scanning Electron Microscope (ESEM)

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

    DEFF Research Database (Denmark)

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

    2013-01-01

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

  7. An electrochemical cell for in operando studies of lithium/sodium batteries using a conventional x-ray powder diffractometer

    DEFF Research Database (Denmark)

    Shen, Yanbin; Pedersen, Erik Ejler; Christensen, Mogens

    2014-01-01

    An electrochemical cell has been designed for powder X-ray diffraction (PXRD) studies of lithium ion batteries (LIB) and sodium ion batteries (SIB) in operando with high time resolution using conventional powder X-ray diffractometer. The cell allows for studies of both anode and cathode electrode...... to operate and maintain. Test examples on lithium insertion/extraction in two spinel-type LIB electrode materials (Li4Ti5O12 anode and LiMn2O4 cathode) are presented as well as first results on sodium extraction from a layered SIB cathode material (Na0.84Fe0.56Mn0.44O2)....

  8. Combined PIXE and X-ray SEM studies on time-resolved deposits of welding shop aerosols

    International Nuclear Information System (INIS)

    Barfoot, K.M.; Mitchell, I.V.; Verheyen, F.; Babeliowsky, T.

    1981-01-01

    Time-resolved deposits of welding shop air particulates have been obtained using a streak sampling system. PIXE analysis of these deposits, using 2 MeV protons, typically revealed the presence of a large number of elements, with many in the range Z = 11-30. Strong variations, up to three orders of magnitude, in the concentrations of several elements such as Al, Si and Fe as well as Zn, Na, K and Ca were found. The 2 h sampling resolution normally used was found to be insufficient to follow the short pollution episodes that regularly occur in a welding shop environment and so sampling with a 20 min resolution was used. The variation of elemental concentrations for different sampling times together with information on the physical nature of these air particulates, determined with a scanning electron microscope (SEM) and Si(Li) X-ray detector attachment, are presented. This type of information together with that obtained from the PIXE analysis is of importance industrial hygiene studies. The need to make corrections for partial filter clogging, based on air-flow rate monitoring, is discussed. (orig.)

  9. Establishment of X-ray Measurement System for On-line Monitoring of Water Content in Powder

    Energy Technology Data Exchange (ETDEWEB)

    Hwang, J. S. [Korea Institute of Industrial Technology, Cheonan (Korea, Republic of); Choi, Y. S. [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of); Choi, B. J. [Idealsystem Co., Daegu (Korea, Republic of)

    2012-05-15

    On-line process monitoring is of critical importance in many industries, and therefore a variety of the state-of-the-art physical and chemical measurement techniques have been proposed. But, these techniques have their own pros and cons under the field process environments. Because the field process environments are very different from the well-organized chemical laboratories, many factors should be considered in order to optimize the process monitoring system. However, there have been few studies on the on-line measurement of water content in powder materials. For that reason, the X-ray measurement system based on the X-ray scattering technique, which was first proposed in 2011 as a new method for the determination of water content in powder, has been improved. in the present study, our original X-ray measurement system has been modified for more rapid, simple, and adequate for maximizing the field applicability of the on-line monitoring system

  10. Phase transitions of Cu.sub.3+x./sub.Si observed by temperature-dependent x-ray powder diffraction

    Czech Academy of Sciences Publication Activity Database

    Correa, Cinthia Antunes; Poupon, Morgane; Kopeček, Jaromír; Král, Robert; Zemenová, Petra; Lecourt, J.; Barrier, N.; Brázda, Petr; Klementová, Mariana; Palatinus, Lukáš

    2017-01-01

    Roč. 91, Dec (2017), s. 129-139 ISSN 0966-9795 R&D Projects: GA ČR GC15-08842J Institutional support: RVO:68378271 Keywords : X-ray powder diffraction * differential scanning calorimetry * phase transitions * Cu3+xSi Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 3.140, year: 2016

  11. Space- and time-resolved X-ray diffraction from pinned and sliding charge-density-waves in NbSe3

    International Nuclear Information System (INIS)

    Requardt, H.; Nad, F.Ya.; Monceau, P.; Lorenzo, J.E.; Smilgies, D.; Gruebel, G.

    1999-01-01

    We have determined the spatial distribution of the local charge-density-wave (CDW) strain in the sliding state of NbSe 3 . The strain is measured by monitoring the spatially-varying shift q(x) of the CDW satellite wave vector between current contacts. Experiments were carried out at T=90 K in the upper CDW state using high spatial resolution (30-50 μm) X-ray diffraction. Applying direct currents about twice the threshold value, we observe a steep exponential decrease of the shift within a few hundred microns from the contact followed by a linear variation of q in the central section of the sample. This latter regime is attributed to transverse pinning of the CDW dislocation loops (DL), while the exponential regime is controlled by the finite DL nucleation rate. Additional to these data in the stationary state of the sliding CDW, we investigated the relaxation of the CDW strain q(t) upon switching off the current (T=75 K). Using time-resolved high-spatial resolution X-ray diffraction, we observe at 800 μm from the electrode a decay law of the stretched exponential type: q(t)=q 0 exp(-(t/τ) u ), with τ=283 ms and μ=0.37. (orig.)

  12. X-Pinch And Its Applications In X-ray Radiograph

    International Nuclear Information System (INIS)

    Zou Xiaobing; Wang Xinxin; Liu Rui; Zhao Tong; Zeng Naigong; Zhao Yongchao; Du Yanqiang

    2009-01-01

    An X-pinch device and the related diagnostics of x-ray emission from X-pinch were briefly described. The time-resolved x-ray measurements with photoconducting diodes show that the x-ray pulse usually consists of two subnanosecond peaks with a time interval of about 0.5 ns. Being consistent with these two peaks of the x-ray pulse, two point x-ray sources of size ranging from 100 μm to 5 μm and depending on cut-off x-ray photon energy were usually observed on the pinhole pictures. The x-pinch was used as x-ray source for backlighting of the electrical explosion of single wire and the evolution of X-pinch, and for phase-contrast imaging of soft biological objects such as a small shrimp and a mosquito.

  13. Calculated powder x-ray diffraction data for three tantalum tungstates

    International Nuclear Information System (INIS)

    Holcombe, C.E. Jr.

    1976-11-01

    A study was made of computer-simulated powder x-ray diffraction data for Ta 22 W 4 O 67 , Ta 2 WO 8 , and Ta 16 W 18 O 94 --the three compounds in the Ta 2 O 5 --WO 3 system from 27 to 69 mole percent WO 3 . The crystal structures of Ta 2 WO 8 and one form of Ta 16 W 18 O 94 (Type B) were deduced from reported data. 8 tables

  14. Application of focused-beam flat-sample method to synchrotron powder X-ray diffraction with anomalous scattering effect

    International Nuclear Information System (INIS)

    Tanaka, M; Katsuya, Y; Matsushita, Y

    2013-01-01

    The focused-beam flat-sample method (FFM), which is a method for high-resolution and rapid synchrotron X-ray powder diffraction measurements by combination of beam focusing optics, a flat shape sample and an area detector, was applied for diffraction experiments with anomalous scattering effect. The advantages of FFM for anomalous diffraction were absorption correction without approximation, rapid data collection by an area detector and good signal-to-noise ratio data by focusing optics. In the X-ray diffraction experiments of CoFe 2 O 4 and Fe 3 O 4 (By FFM) using X-rays near the Fe K absorption edge, the anomalous scattering effect between Fe/Co or Fe 2+ /Fe 3+ can be clearly detected, due to the change of diffraction intensity. The change of observed diffraction intensity as the incident X-ray energy was consistent with the calculation. The FFM is expected to be a method for anomalous powder diffraction.

  15. Batch crystallization of rhodopsin for structural dynamics using an X-ray free-electron laser

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Wenting; Nogly, Przemyslaw; Rheinberger, Jan; Kick, Leonhard M.; Gati, Cornelius; Nelson, Garrett; Deupi, Xavier; Standfuss, Jörg; Schertler, Gebhard; Panneels, Valérie, E-mail: valerie.panneels@psi.ch [Paul Scherrer Institute, OFLC/103, 5232 Villigen-PSI (Switzerland)

    2015-06-27

    A new batch preparation method is presented for high-density micrometre-sized crystals of the G protein-coupled receptor rhodopsin for use in time-resolved serial femtosecond crystallography at an X-ray free-electron laser using a liquid jet. Rhodopsin is a membrane protein from the G protein-coupled receptor family. Together with its ligand retinal, it forms the visual pigment responsible for night vision. In order to perform ultrafast dynamics studies, a time-resolved serial femtosecond crystallography method is required owing to the nonreversible activation of rhodopsin. In such an approach, microcrystals in suspension are delivered into the X-ray pulses of an X-ray free-electron laser (XFEL) after a precise photoactivation delay. Here, a millilitre batch production of high-density microcrystals was developed by four methodical conversion steps starting from known vapour-diffusion crystallization protocols: (i) screening the low-salt crystallization conditions preferred for serial crystallography by vapour diffusion, (ii) optimization of batch crystallization, (iii) testing the crystal size and quality using second-harmonic generation (SHG) imaging and X-ray powder diffraction and (iv) production of millilitres of rhodopsin crystal suspension in batches for serial crystallography tests; these crystals diffracted at an XFEL at the Linac Coherent Light Source using a liquid-jet setup.

  16. Spatially and temporally resolved x-ray emission from imploding laser fusion targets

    International Nuclear Information System (INIS)

    Attwood, D.T.; Coleman, L.W.; Boyle, M.J.; Phillion, D.W.; Swain, J.E.; Manes, K.R.; Larsen, J.T.

    1976-09-01

    The Livermore 15 psec x-ray streak camera has been used in conjunction with 6 μm diameter pinholes to record well resolved implosion histories of DT filled laser fusion targets. The space-time compression data provide clearly identified implosion velocities, typically 3 x 10 7 cm/sec for two-sided clamshell irradiation of a 70 μm/sup D/, .5 μm wall DT filled glass microshell. Single-sided irradiation results show hydrodynamic convergence at the target center, followed by an asymmetric but two-sided target disassembly. These experiments were performed at the two arm Janus Laser facility, which typically delivered a total of 0.4 TW in a 70 psec pulse for these experiments

  17. Efficiency of Lu2SiO5:Ce (LSO) powder phosphor as X-ray to light converter under mammographic imaging conditions

    International Nuclear Information System (INIS)

    David, S.; Michail, C.; Valais, I.; Nikolopoulos, D.; Liaparinos, P.; Kalivas, N.; Kalatzis, I.; Toutountzis, A.; Efthimiou, N.; Loudos, G.; Sianoudis, I.; Cavouras, D.; Dimitropoulos, N.; Nomicos, C.D.; Kandarakis, I.; Panayiotakis, G.S.

    2007-01-01

    The aim of the present study was to examine the light emission efficiency of Lu 2 SiO 5 :Ce (LSO) powder scintillator under X-ray mammographic imaging conditions. Powder LSO scintillator has never been used in X-ray imaging. For the purposes of the present study, a 25 mg/cm 2 thick scintillating screen was prepared in our laboratory, by sedimentation of Lu 2 SiO 5 :Ce powder. Absolute luminescence efficiency measurements were performed within the range of X-ray tube voltages (22-49 kVp) used in mammographic applications. Parameters related to X-ray detection, i.e. the energy absorption efficiency (EAE) and the quantum detection efficiency (QDE) were calculated. A theoretical model, describing radiation and light transfer, was employed to fit experimental data and to estimate values of the intrinsic conversion efficiency and the light attenuation coefficients of the screen. The spectral compatibility of the LSO powder scintillator to mammographic X-ray films and to various electronic optical detectors was determined by performing light emission spectrum measurements and by taking into account the spectral sensitivity of the optical detectors. Results in the voltage range used in mammography showed that Lu 2 SiO 5 :Ce powder scintillator has approximately 10% higher values of QDE and 4.5% higher values of EAE than Gd 2 O 2 S:Tb

  18. Two-dimensional time-resolved x-ray diffraction study of dual phase rapid solidification in steels

    Science.gov (United States)

    Yonemura, Mitsuharu; Osuki, Takahiro; Terasaki, Hidenori; Komizo, Yuichi; Sato, Masugu; Toyokawa, Hidenori; Nozaki, Akiko

    2010-01-01

    The high intensity heat source used for fusion welding creates steep thermal gradients of 100 °C/s from 1800 °C. Further, the influence of preferred orientation is important for the observation of a directional solidification that follows the dendrite growth along the ⟨100⟩ direction toward the moving heat source. In the present study, we observed the rapid solidification of weld metal at a time resolution of 0.01-0.1 s by a two-dimensional time-resolved x-ray diffraction (2DTRXRD) system for real welding. The diffraction rings were dynamically observed by 2DTRXRD with synchrotron energy of 18 keV while the arc passes over the irradiation area of the x-rays. The arc power output was 10 V-150 A, and the scan speed of the arc was 1.0 mm/s. The temperature rise in instruments was suppressed by a water-cooled copper plate under the specimen. Further, the temperature distribution of the weld metal was measured by a thermocouple and correlated with the diffraction patterns. Consequently, solidification and solid phase transformation of low carbon steels and stainless steels were observed during rapid cooling by 2DTRXRD. In the low carbon steel, the microstructure is formed in a two step process, (i) formation of crystallites and (ii) increase of crystallinity. In stainless steel, the irregular interface layer of δ/γ in the quenched metal after solidification is expected to show the easy movement of dendrites at a lower temperature. In carbide precipitation stainless steel, it is easy for NbC to grow on δ phase with a little undercooling. Further, a mistlike pattern, which differs from the halo pattern, in the fusion zone gave some indication of the possibilities to observe the nucleation and the early solidification by 2DTRXRD.

  19. Ultrashort X-ray pulse science

    Energy Technology Data Exchange (ETDEWEB)

    Chin, Alan Hap [Univ. of California, Berkeley, CA (US). Dept. of Physics; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

    1998-05-01

    A variety of phenomena involves atomic motion on the femtosecond time-scale. These phenomena have been studied using ultrashort optical pulses, which indirectly probe atomic positions through changes in optical properties. Because x-rays can more directly probe atomic positions, ultrashort x-ray pulses are better suited for the study of ultrafast structural dynamics. One approach towards generating ultrashort x-ray pulses is by 90° Thomson scattering between terawatt laser pulses and relativistic electrons. Using this technique, the author generated ~ 300 fs, 30 keV (0.4 Å) x-ray pulses. These x-ray pulses are absolutely synchronized with ultrashort laser pulses, allowing femtosecond optical pump/x-ray probe experiments to be performed. Using the right-angle Thomson scattering x-ray source, the author performed time-resolved x-ray diffraction studies of laser-perturbated InSb. These experiments revealed a delayed onset of lattice expansion. This delay is due to the energy relaxation from a dense electron-hole plasma to the lattice. The dense electron-hole plasma first undergoes Auger recombination, which reduces the carrier concentration while maintaining energy content. Longitudinal-optic (LO) phonon emission then couples energy to the lattice. LO phonon decay into acoustic phonons, and acoustic phonon propagation then causes the growth of a thermally expanded layer. Source characterization is instrumental in utilizing ultrashort x-ray pulses in time-resolved x-ray spectroscopies. By measurement of the electron beam diameter at the generation point, the pulse duration of the Thomson scattered x-rays is determined. Analysis of the Thomson scattered x-ray beam properties also provides a novel means of electron bunch characterization. Although the pulse duration is inferred for the Thomson scattering x-ray source, direct measurement is required for other x-ray pulse sources. A method based on the laser-assisted photoelectric effect (LAPE) has been demonstrated as a

  20. Ultrashort X-ray pulse science

    International Nuclear Information System (INIS)

    Chin, A.H.; Lawrence Berkeley National Lab., CA

    1998-01-01

    A variety of phenomena involves atomic motion on the femtosecond time-scale. These phenomena have been studied using ultrashort optical pulses, which indirectly probe atomic positions through changes in optical properties. Because x-rays can more directly probe atomic positions, ultrashort x-ray pulses are better suited for the study of ultrafast structural dynamics. One approach towards generating ultrashort x-ray pulses is by 90 o Thomson scattering between terawatt laser pulses and relativistic electrons. Using this technique, the author generated ∼ 300 fs, 30 keV (0.4 (angstrom)) x-ray pulses. These x-ray pulses are absolutely synchronized with ultrashort laser pulses, allowing femtosecond optical pump/x-ray probe experiments to be performed. Using the right-angle Thomson scattering x-ray source, the author performed time-resolved x-ray diffraction studies of laser-perturbated InSb. These experiments revealed a delayed onset of lattice expansion. This delay is due to the energy relaxation from a dense electron-hole plasma to the lattice. The dense electron-hole plasma first undergoes Auger recombination, which reduces the carrier concentration while maintaining energy content. Longitudinal-optic (LO) phonon emission then couples energy to the lattice. LO phonon decay into acoustic phonons, and acoustic phonon propagation then causes the growth of a thermally expanded layer. Source characterization is instrumental in utilizing ultrashort x-ray pulses in time-resolved x-ray spectroscopies. By measurement of the electron beam diameter at the generation point, the pulse duration of the Thomson scattered x-rays is determined. Analysis of the Thomson scattered x-ray beam properties also provides a novel means of electron bunch characterization. Although the pulse duration is inferred for the Thomson scattering x-ray source, direct measurement is required for other x-ray pulse sources. A method based on the laser-assisted photoelectric effect (LAPE) has been

  1. Photoinduced charge transfer in a transition metal complex investigated by time-resolved X-ray absorption fine structure spectroscopy. Setup and experiment

    International Nuclear Information System (INIS)

    Goeries, Dennis

    2015-02-01

    In the framework of this thesis the development of a time-resolved X-ray absorption spectroscopy experiment and its application to fac-Ir(ppy) 3 is described. Such experiments require a very stable setup in terms of spatial and temporal accuracy. Therefore, the stability properties of the present installation were investigated in detail and continuously improved, in particular the synchronization of the ultrashort pulse laser system to the storage ring as well as the spatial stability of both X-ray and laser beam. Experiments utilizing the laser pump and X-ray probe configuration were applied on the green phosphorescence emitter complex fac-Ir(ppy) 3 dissolved in dimethyl sulfoxide. Structural and electronic changes were triggered by photoexcitation of the metal-to-ligand charge transfer band with ultrashort laser pulses at a wavelength of 343 nm. The excited triplet state spectrum was extracted from the measured pump-probe X-ray absorption spectrum using an ionic approximation. The results con rm the anticipated metal-to-ligand charge transfer as shown by an ionization potential shift of the iridium atom. The symmetry of the complex was found to be pseudo-octahedral. This allowed the first experimental determination of the bond length of fac-Ir(ppy) 3 in an octahedral approximation and revealed a decrease of bond length of the first coordination shell in the triplet state. The first and second-order decay kinetics of the triplet state were investigated in a combination of X-ray and laser based experiments and revealed self-quenching as well as triplet-triplet annihilation rate constants.

  2. Anisotropy enhanced X-ray scattering from solvated transition metal complexes

    DEFF Research Database (Denmark)

    Biasin, Elisa; van Driel, Tim B.; Levi, Gianluca

    2018-01-01

    Time-resolved X-ray scattering patterns from photoexcited molecules in solution are in many cases anisotropic at the ultrafast time scales accessible at X-ray free-electron lasers (XFELs). This anisotropy arises from the interaction of a linearly polarized UV-Vis pump laser pulse with the sample......, which induces anisotropic structural changes that can be captured by femtosecond X-ray pulses. In this work, a method for quantitative analysis of the anisotropic scattering signal arising from an ensemble of molecules is described, and it is demonstrated how its use can enhance the structural...... sensitivity of the time-resolved X-ray scattering experiment. This method is applied on time-resolved X-ray scattering patterns measured upon photoexcitation of a solvated di-platinum complex at an XFEL, and the key parameters involved are explored. It is shown that a combined analysis of the anisotropic...

  3. Deactivation of Zeolite Catalyst H-ZSM-5 during Conversion of Methanol to Gasoline: Operando Time- and Space-Resolved X-ray Diffraction.

    Science.gov (United States)

    Rojo-Gama, Daniel; Mentel, Lukasz; Kalantzopoulos, Georgios N; Pappas, Dimitrios K; Dovgaliuk, Iurii; Olsbye, Unni; Lillerud, Karl Petter; Beato, Pablo; Lundegaard, Lars F; Wragg, David S; Svelle, Stian

    2018-03-15

    The deactivation of zeolite catalyst H-ZSM-5 by coking during the conversion of methanol to hydrocarbons was monitored by high-energy space- and time-resolved operando X-ray diffraction (XRD) . Space resolution was achieved by continuous scanning along the axial length of a capillary fixed bed reactor with a time resolution of 10 s per scan. Using real structural parameters obtained from XRD, we can track the development of coke at different points in the reactor and link this to a kinetic model to correlate catalyst deactivation with structural changes occurring in the material. The "burning cigar" model of catalyst bed deactivation is directly observed in real time.

  4. Timepix3 as X-ray detector for time resolved synchrotron experiments

    Energy Technology Data Exchange (ETDEWEB)

    Yousef, Hazem, E-mail: hazem.yousef@diamond.ac.uk; Crevatin, Giulio; Gimenez, Eva N.; Horswell, Ian; Omar, David; Tartoni, Nicola

    2017-02-11

    The Timepix3 ASIC can be used very effectively for time resolved experiments at synchrotron facilities. We have carried out characterizations with the synchrotron beam in order to determine the time resolution and other characteristics such as the energy resolution, charge sharing and signals overlapping. The best time resolution achieved is 19 ns FWHM for 12 keV photons and 350 V bias voltage. The time resolution shows dependency on the photon energy as well as on the chip and acquisition parameters. - Highlights: • An estimate time resolution of the Timepix3 is produced based on the arrival time. • At high resolution, the time structure of the DLS synchrotron beam is resolved. • The arrival time information improves combining the charge split events. • The results enable performing a wide range of time resolved experiments.

  5. Timepix3 as X-ray detector for time resolved synchrotron experiments

    International Nuclear Information System (INIS)

    Yousef, Hazem; Crevatin, Giulio; Gimenez, Eva N.; Horswell, Ian; Omar, David; Tartoni, Nicola

    2017-01-01

    The Timepix3 ASIC can be used very effectively for time resolved experiments at synchrotron facilities. We have carried out characterizations with the synchrotron beam in order to determine the time resolution and other characteristics such as the energy resolution, charge sharing and signals overlapping. The best time resolution achieved is 19 ns FWHM for 12 keV photons and 350 V bias voltage. The time resolution shows dependency on the photon energy as well as on the chip and acquisition parameters. - Highlights: • An estimate time resolution of the Timepix3 is produced based on the arrival time. • At high resolution, the time structure of the DLS synchrotron beam is resolved. • The arrival time information improves combining the charge split events. • The results enable performing a wide range of time resolved experiments.

  6. Capillary based Li-air batteries for in situ synchrotron X-ray powder diffraction studies

    DEFF Research Database (Denmark)

    Storm, Mie Møller; Johnsen, Rune E.; Younesi, Reza

    2015-01-01

    For Li-air batteries to reach their full potential as energy storage system, a complete understanding of the conditions and reactions in the battery during operation is needed. To follow the reactions in situ a capillary-based Li-O2 battery has been developed for synchrotron-based in situ X......-ray powder diffraction (XRPD). In this article, we present the results for the analysis of 1st and 2nd deep discharge and charge for a cathode being cycled between 2 and 4.6 V. The crystalline precipitation of Li2O2 only is observed in the capillary battery. However, there are indications of side reactions...... of constant exposure of X-ray radiation to the electrolyte and cathode during charge of the battery was also investigated. X-ray exposure during charge leads to changes in the development of the intensity and the FWHM of the Li2O2 diffraction peaks. The X-ray diffraction results are supported by ex situ X...

  7. Combined experimental powder X-ray diffraction and DFT data to obtain the lowest energy molecular conformation of friedelin

    International Nuclear Information System (INIS)

    Oliveira, Djalma Menezes de; Mussel, Wagner da Nova; Duarte, Lucienir Pains; Silva, Gracia Divina de Fatima; Duarte, Helio Anderson; Gomes, Elionai Cassiana de Lima; Guimaraes, Luciana; Vieira Filho, Sidney A.

    2012-01-01

    Friedelin molecular conformers were obtained by Density Functional Theory (DFT) and by ab initio structure determination from powder X-ray diffraction. Their conformers with the five rings in chair-chair-chair-boat-boat, and with all rings in chair, are energy degenerated in gas-phase according to DFT results. The powder diffraction data reveals that rings A, B and C of friedelin are in chair, and rings D and E in boat-boat, conformation. The high correlation values among powder diffraction data, DFT and reported single crystal data indicate that the use of conventional X-ray diffractometer can be applied in routine laboratory analysis in the absence of a single-crystal diffractometer. (author)

  8. Combined experimental powder X-ray diffraction and DFT data to obtain the lowest energy molecular conformation of friedelin

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Djalma Menezes de; Mussel, Wagner da Nova; Duarte, Lucienir Pains; Silva, Gracia Divina de Fatima; Duarte, Helio Anderson; Gomes, Elionai Cassiana de Lima [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil). Dept. de Quimica; Guimaraes, Luciana [Universidade Federal de Sao Joao Del-Rei (UFSJ), MG (Brazil). Dept. de Ciencias Naturais; Vieira Filho, Sidney A., E-mail: bibo@ef.ufop.br [Universidade Federal de Ouro Preto (UFOP), MG (Brazil). Dept. de Farmacia

    2012-07-01

    Friedelin molecular conformers were obtained by Density Functional Theory (DFT) and by ab initio structure determination from powder X-ray diffraction. Their conformers with the five rings in chair-chair-chair-boat-boat, and with all rings in chair, are energy degenerated in gas-phase according to DFT results. The powder diffraction data reveals that rings A, B and C of friedelin are in chair, and rings D and E in boat-boat, conformation. The high correlation values among powder diffraction data, DFT and reported single crystal data indicate that the use of conventional X-ray diffractometer can be applied in routine laboratory analysis in the absence of a single-crystal diffractometer. (author)

  9. Bond Shortening (1.4 Å) in the Singlet and Triplet Excited States of [Ir2(dimen)4]2+ in Solution Determined by Time-Resolved X-ray Scattering

    DEFF Research Database (Denmark)

    Haldrup, Martin Kristoffer; Harlang, Tobias; Christensen, Morten

    2011-01-01

    Ground- and excited-state structures of the bimetallic, ligand-bridged compound Ir2(dimen)42+ are investigated in acetonitrile by means of time-resolved X-ray scattering. Following excitation by 2 ps laser pulses at 390 nm, analysis of difference scattering patterns obtained at eight different ti...

  10. Time-resolved spectral measurements above 80 A

    International Nuclear Information System (INIS)

    Kauffman, R.L.; Ceglio, N.; Medecki, H.

    1983-01-01

    We have made time-resolved spectral measurements above 80 A from laser-produced plasmas. These are made using a transmission grating spectrograph whose primary components are a cylindrically-curved x-ray mirror for light collection, a transmission grating for spectral dispersions, and an x-ray streak camera for temporal resolution. A description of the instrument and an example of the data are given

  11. X-ray powder diffraction analysis of liquid-phase-sintered silicon carbide ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Ortiz, A.L.; Sanchez-Bajo, F. [Universidad de Extremadura, Badajoz (Spain). Dept. de Electronica e Ingenieria Electromecanica; Cumbrera, F.L. [Universidad de Extremadura, Badajoz (Spain). Dept. de Fisica

    2002-07-01

    In an attempt to gain a comprehensive understanding of the microstructural evolution in liquid-phase-sintered silicon carbide ceramics, the effect of the starting {beta}-SiC powder has been studied. Pellets of two different {beta}-SiC starting powders were sintered with simultaneous additions of Al{sub 2}O{sub 3} and Y{sub 2}O{sub 3} at 1950 C for 1 hour in flowing argon atmosphere. Here we have used X-ray diffraction to obtain the relative abundance of the resulting SiC polytypes after sintering. The significant influence of the defects concentration on the {beta} to {alpha} transformation rate has been determined using the Rietveld method. (orig.)

  12. Excitation-resolved cone-beam x-ray luminescence tomography.

    Science.gov (United States)

    Liu, Xin; Liao, Qimei; Wang, Hongkai; Yan, Zhuangzhi

    2015-07-01

    Cone-beam x-ray luminescence computed tomography (CB-XLCT), as an emerging imaging technique, plays an important role in in vivo small animal imaging studies. However, CB-XLCT suffers from low-spatial resolution due to the ill-posed nature of reconstruction. We improve the imaging performance of CB-XLCT by using a multiband excitation-resolved imaging scheme combined with principal component analysis. To evaluate the performance of the proposed method, the physical phantom experiment is performed with a custom-made XLCT/XCT imaging system. The experimental results validate the feasibility of the method, where two adjacent nanophosphors (with an edge-to-edge distance of 2.4 mm) can be located.

  13. X-ray spectrometer having 12 000 resolving power at 8 keV energy

    Science.gov (United States)

    Seely, John F.; Hudson, Lawrence T.; Henins, Albert; Feldman, Uri

    2017-10-01

    An x-ray spectrometer employing a thin (50 μm) silicon transmission crystal was used to record high-resolution Cu Kα spectra from a laboratory x-ray source. The diffraction was from the (331) planes that were at an angle of 13.26° to the crystal surface. The components of the spectral lines resulting from single-vacancy (1s) and double-vacancy (1s and 3d) transitions were observed. After accounting for the natural lifetime widths from reference double-crystal spectra and the spatial resolution of the image plate detector, the intrinsic broadening of the transmission crystal was measured to be as small as 0.67 eV and the resolving power 12 000, the highest resolving power achieved by a compact (0.5 m long) spectrometer employing a single transmission crystal operating in the hard x-ray region. By recording spectra with variable source-to-crystal distances and comparing to the calculated widths from various geometrical broadening mechanisms, the primary contributions to the intrinsic crystal broadening were found to be the source height at small distances and the crystal apertured height at large distances. By reducing these two effects, using a smaller source size and vignetting the crystal height, the intrinsic crystal broadening is then limited by the crystal thickness and the rocking curve width and would be 0.4 eV at 8 keV energy (20 000 resolving power).

  14. Time-dependent, x-ray spectral unfolds and brightness temperatures for intense Li+ ion beam-driven hohlraums

    International Nuclear Information System (INIS)

    Fehl, D.L.; Chandler, G.A.; Biggs, F.; Dukart, R.J.; Moats, A.R.; Leeper, R.J.

    1996-01-01

    X-ray-producing hohlraums are being studied as indirect drives for Inertial Confinement Fusion targets. In a 1994 target series on the PBFAII accelerator, cylindrical hohlraum targets were heated by an intense Li + ion beam and viewed by an array of 13 time-resolved, filtered x-ray detectors (XRDs). The UFO unfold code and its suite of auxiliary functions were used extensively in obtaining time- resolved x-ray spectra and radiation temperatures from this diagnostic. UFO was also used to obtain fitted response functions from calibration data, to simulate data from blackbody x-ray spectra of interest, to determine the suitability of various unfolding parameters (e.g., energy domain, energy partition, smoothing conditions, and basis functions), to interpolate the XRD signal traces, and to unfold experimental data. The simulation capabilities of the code were useful in understanding an anomalous feature in the unfolded spectra at low photon energies (≤ 100 eV). Uncertainties in the differential and energy-integrated unfolded spectra were estimated from uncertainties in the data. The time-history of the radiation temperature agreed well with independent calculations of the wall temperature in the hohlraum

  15. Time-dependent, x-ray spectral unfolds and brightness temperatures for intense Li+ ion beam-driven hohlraums

    International Nuclear Information System (INIS)

    Fehl, D.L.; Chandler, G.A.; Biggs, F.; Dukart, R.J.; Moats, A.R.; Leeper, R.J.

    1997-01-01

    X-ray-producing hohlraums are being studied as indirect drives for inertial confinement fusion targets. In a 1994 target series on the PBFAII accelerator, cylindrical hohlraum targets were heated by an intense Li + ion beam and viewed by an array of 13 time-resolved, filtered x-ray detectors (XRDs). The unfold operator (UFO) code and its suite of auxiliary functions were used extensively in obtaining time-resolved x-ray spectra and radiation temperatures from this diagnostic. The UFO was also used to obtain fitted response functions from calibration data, to simulate data from blackbody x-ray spectra of interest, to determine the suitability of various unfolding parameters (e.g., energy domain, energy partition, smoothing conditions, and basis functions), to interpolate the XRD signal traces, and to unfold experimental data. The simulation capabilities of the code were useful in understanding an anomalous feature in the unfolded spectra at low photon energies (≤100 eV). Uncertainties in the differential and energy-integrated unfolded spectra were estimated from uncertainties in the data. The time endash history of the radiation temperature agreed well with independent calculations of the wall temperature in the hohlraum. copyright 1997 American Institute of Physics

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

    Science.gov (United States)

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

    2018-01-01

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

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

    Science.gov (United States)

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

    2018-01-01

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

  18. Novel technique for spatially resolved imaging of molecular bond orientations using x-ray birefringence

    Energy Technology Data Exchange (ETDEWEB)

    Sutter, John P., E-mail: john.sutter@diamond.ac.uk; Dolbnya, Igor P.; Collins, Stephen P. [Diamond Light Source Ltd, Harwell Science and Innovation Campus, Chilton, Didcot, Oxfordshire OX11 0DE (United Kingdom); Harris, Kenneth D. M., E-mail: HarrisKDM@cardiff.ac.uk; Edwards-Gau, Gregory R.; Kariuki, Benson M. [School of Chemistry, Cardiff University, Park Place, Cardiff CF10 3AT (United Kingdom); Palmer, Benjamin A. [Department of Structural Biology, Weizmann Institute of Science, 234 Herzl St., Rehovot 7610001 (Israel)

    2016-07-27

    Birefringence has been observed in anisotropic materials transmitting linearly polarized X-ray beams tuned close to an absorption edge of a specific element in the material. Synchrotron bending magnets provide X-ray beams of sufficiently high brightness and cross section for spatially resolved measurements of birefringence. The recently developed X-ray Birefringence Imaging (XBI) technique has been successfully applied for the first time using the versatile test beamline B16 at Diamond Light Source. Orientational distributions of the C–Br bonds of brominated “guest” molecules within crystalline “host” tunnel structures (in thiourea or urea inclusion compounds) have been studied using linearly polarized incident X-rays near the Br K-edge. Imaging of domain structures, changes in C–Br bond orientations associated with order-disorder phase transitions, and the effects of dynamic averaging of C–Br bond orientations have been demonstrated. The XBI setup uses a vertically deflecting high-resolution double-crystal monochromator upstream from the sample and a horizontally deflecting single-crystal polarization analyzer downstream, with a Bragg angle as close as possible to 45°. In this way, the ellipticity and rotation angle of the polarization of the beam transmitted through the sample is measured as in polarizing optical microscopy. The theoretical instrumental background calculated from the elliptical polarization of the bending-magnet X-rays, the imperfect polarization discrimination of the analyzer, and the correlation between vertical position and photon energy introduced by the monochromator agrees well with experimental observations. The background is calculated analytically because the region of X-ray phase space selected by this setup is sampled inefficiently by standard methods.

  19. A full-field transmission x-ray microscope for time-resolved imaging of magnetic nanostructures

    Energy Technology Data Exchange (ETDEWEB)

    Ewald, J.; Nisius, T.; Abbati, G.; Baumbach, S.; Overbuschmann, J.; Wilhein, T. [Institute for X-Optics (IXO), Hochschule Koblenz, Joseph-Rovan-Allee 2, 53424 Remagen (Germany); Wessels, P.; Wieland, M.; Drescher, M. [The Hamburg Centre for Ultrafast Imaging (CUI), University of Hamburg, Luruper Chaussee 149, 22761 Hamburg (Germany); Institut für Experimentalphysik, University of Hamburg, Luruper Chaussee 149, 22761 Hamburg (Germany); Vogel, A. [Institut für Angewandte Physik, University of Hamburg, Jungiusstraße 11, 20355 Hamburg (Germany); Viefhaus, J. [Deutsches Elektronen-Synchrotron (DESY), Notkestraße 85, 22607 Hamburg (Germany); Meier, G. [The Hamburg Centre for Ultrafast Imaging (CUI), University of Hamburg, Luruper Chaussee 149, 22761 Hamburg (Germany); Max Planck Institute for the Structure and Dynamics of Matter, Luruper Chaussee 149, 22761 Hamburg (Germany)

    2016-01-28

    Sub-nanosecond magnetization dynamics of small permalloy (Ni{sub 80}Fe{sub 20}) elements has been investigated with a new full-field transmission microscope at the soft X-ray beamline P04 of the high brilliance synchrotron radiation source PETRA III. The soft X-ray microscope generates a flat-top illumination field of 20 μm diameter using a grating condenser. A tilted nanostructured magnetic sample can be excited by a picosecond electric current pulse via a coplanar waveguide. The transmitted light of the sample plane is directly imaged by a micro zone plate with < 65 nm resolution onto a 2D gateable X-ray detector to select one particular bunch in the storage ring that probes the time evolution of the dynamic information successively via XMCD spectromicroscopy in a pump-probe scheme. In the experiments it was possible to generate a homogeneously magnetized state in patterned magnetic layers by a strong magnetic Oersted field pulse of 200 ps duration and directly observe the recovery to the initial flux-closure vortex patterns.

  20. High-pressure powder x-ray diffraction experiments on Zn at low temperature

    CERN Document Server

    Takemura, K; Fujihisa, H; Kikegawa, T

    2002-01-01

    High-pressure powder x-ray diffraction experiments have been performed on Zn with a He-pressure medium at low temperature. When the sample was compressed in the He medium at low temperature, large nonhydrostaticity developed, yielding erroneous lattice parameters. On the other hand, when the pressure was changed at high temperatures, good hydrostaticity was maintained. No anomaly in the volume dependence of the c/a axial ratio has been found.

  1. Challenges for energy dispersive X-ray absorption spectroscopy at the ESRF: microsecond time resolution and Mega-bar pressures

    International Nuclear Information System (INIS)

    Aquilanti, G.

    2002-01-01

    This Thesis concerns the development of two different applications of energy-dispersive X-ray absorption spectroscopy at the ESRF: time-resolved studies pushed to the microsecond time resolution and high-pressure studies at the limit of the Mega-bar pressures. The work has been developed in two distinct parts, and the underlying theme has been the exploitation of the capabilities of an X-ray absorption spectrometer in dispersive geometry on a third generation synchrotron source. For time-resolved studies, the study of the triplet excited state following a laser excitation of Pt 2 (P 2 O 5 H 2 ) 4 4- has been chosen to push the technique to the microsecond time resolution. In the high-pressure part, the suitability of the energy dispersive X-ray absorption spectrometer for high-pressure studies using diamond anvils cell is stressed. Some technical developments carried out on beamline ID24 are discussed. Finally, the most extensive scientific part concerns a combined X-ray absorption and diffraction study of InAs under pressure. (author)

  2. Multichord time-resolved electron temperature measurements by the x-ray absorber-foil method on TFTR

    International Nuclear Information System (INIS)

    Kiraly, J.; Bitter, M.; Efthimion, P.

    1985-09-01

    Absorber foils have been installed in the TFTR X-Ray Imaging System to permit measurement of the electron temperature along 10 to 30 chords spaced at 5-12.5 cm with a time resolution of less than 100 μs. The technique uses the ratio of x-ray fluxes transmitted through two different foils. The ratio depends mainly on electron temperature. Simulations show that strong impurity line radiation can distort this ratio. To correct for these effects, special beryllium-scandium filters are employed to select the line-free region between 2 and 4.5 keV. Other filter pairs allow corrections for Fe L and Ni L line radiation as well as Ti K and Ni K emission. Good accuracy is also obtained with simple beryllium filters, provided that impurity corrections are incorporated in the analysis, taking line intensities from the x-ray pulse-height analysis diagnostic. A description of modeling calculations and a comparison of temperature values from this diagnostic with data from the x-ray pulse height analysis, the electron cyclotron emission, and the Thomson scattering diagnostics are presented. Several applications of the absorber foil electron temperature diagnostic on TFTR are discussed

  3. Multichord time-resolved electron temperature measurements by the x-ray absorber-foil method on TFTR

    Energy Technology Data Exchange (ETDEWEB)

    Kiraly, J.; Bitter, M.; Efthimion, P.; von Goeler, S.; Grek, B.; Hill, K.W.; Johnson, D.; McGuire, K.; Sauthoff, N.; Sesnic, S.

    1985-09-01

    Absorber foils have been installed in the TFTR X-Ray Imaging System to permit measurement of the electron temperature along 10 to 30 chords spaced at 5-12.5 cm with a time resolution of less than 100 ..mu..s. The technique uses the ratio of x-ray fluxes transmitted through two different foils. The ratio depends mainly on electron temperature. Simulations show that strong impurity line radiation can distort this ratio. To correct for these effects, special beryllium-scandium filters are employed to select the line-free region between 2 and 4.5 keV. Other filter pairs allow corrections for Fe L and Ni L line radiation as well as Ti K and Ni K emission. Good accuracy is also obtained with simple beryllium filters, provided that impurity corrections are incorporated in the analysis, taking line intensities from the x-ray pulse-height analysis diagnostic. A description of modeling calculations and a comparison of temperature values from this diagnostic with data from the x-ray pulse height analysis, the electron cyclotron emission, and the Thomson scattering diagnostics are presented. Several applications of the absorber foil electron temperature diagnostic on TFTR are discussed.

  4. Ultra fast x-ray streak camera

    International Nuclear Information System (INIS)

    Coleman, L.W.; McConaghy, C.F.

    1975-01-01

    A unique ultrafast x-ray sensitive streak camera, with a time resolution of 50psec, has been built and operated. A 100A thick gold photocathode on a beryllium vacuum window is used in a modified commerical image converter tube. The X-ray streak camera has been used in experiments to observe time resolved emission from laser-produced plasmas. (author)

  5. Picosecond x-ray streak camera studies

    International Nuclear Information System (INIS)

    Kasyanov, Yu.S.; Malyutin, A.A.; Richardson, M.C.; Chevokin, V.K.

    1975-01-01

    Some initial results of direct measurement of picosecond x-ray emission from laser-produced plasmas are presented. A PIM-UMI 93 image converter tube, incorporating an x-ray sensitive photocathode, linear deflection, and three stages of image amplification was used to analyse the x-ray radiation emanating from plasmas produced from solid Ti targets by single high-intensity picosecond laser pulses. From such plasmas, the x-ray emission typically persisted for times of 60psec. However, it is shown that this detection system should be capable of resolving x-ray phenomena of much shorter duration. (author)

  6. Multi-scale mechanics of granular solids from grain-resolved X-ray measurements

    Science.gov (United States)

    Hurley, R. C.; Hall, S. A.; Wright, J. P.

    2017-11-01

    This work discusses an experimental technique for studying the mechanics of three-dimensional (3D) granular solids. The approach combines 3D X-ray diffraction and X-ray computed tomography to measure grain-resolved strains, kinematics and contact fabric in the bulk of a granular solid, from which continuum strains, grain stresses, interparticle forces and coarse-grained elasto-plastic moduli can be determined. We demonstrate the experimental approach and analysis of selected results on a sample of 1099 stiff, frictional grains undergoing multiple uniaxial compression cycles. We investigate the inter-particle force network, elasto-plastic moduli and associated length scales, reversibility of mechanical responses during cyclic loading, the statistics of microscopic responses and microstructure-property relationships. This work serves to highlight both the fundamental insight into granular mechanics that is furnished by combined X-ray measurements and describes future directions in the field of granular materials that can be pursued with such approaches.

  7. Spatially resolved density and ionization measurements of shocked foams using x-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    MacDonald, M. J.; Keiter, P. A.; Montgomery, D. S.; Scott, H. A.; Biener, M. M.; Fein, J. R.; Fournier, K. B.; Gamboa, E. J.; Kemp, G. E.; Klein, S. R.; Kuranz, C. C.; LeFevre, H. J.; Manuel, M. J. -E.; Wan, W. C.; Drake, R. P.

    2016-09-28

    We present experiments at the Trident laser facility demonstrating the use of x-ray fluorescence (XRF) to simultaneously measure density, ionization state populations, and electron temperature in shocked foams. An imaging x-ray spectrometer obtained spatially resolved measurements of Ti K-α emission. Density profiles were measured from K-α intensity. Ti ionization state distributions and electron temperatures were inferred by fitting K-α spectra to spectra from CRETIN simulations. This work shows that XRF provides a powerful tool to complement other diagnostics to make equation of state measurements of shocked materials containing a suitable tracer element.

  8. Reflection-mode x-ray powder diffraction cell for in situ studies of electrochemical reactions

    International Nuclear Information System (INIS)

    Roberts, G.A.; Stewart, K.D.

    2004-01-01

    The design and operation of an electrochemical cell for reflection-mode powder x-ray diffraction experiments are discussed. The cell is designed for the study of electrodes that are used in rechargeable lithium batteries. It is designed for assembly in a glove box so that air-sensitive materials, such as lithium foil electrodes and carbonate-based electrolytes with lithium salts, can be used. The cell uses a beryllium window for x-ray transmission and electrical contact. A simple mechanism for compressing the electrodes is included in the design. Sample results for the cell are shown with a Cu Kα source and a position-sensitive detector

  9. Determining grain resolved stresses in polycrystalline materials using three-dimensional X-ray diffraction

    DEFF Research Database (Denmark)

    Oddershede, Jette; Schmidt, Søren; Poulsen, Henning Friis

    2010-01-01

    An algorithm is presented for characterization of the grain resolved (type II) stress states in a polycrystalline sample based on monochromatic X-ray diffraction data. The algorithm is a robust 12-parameter-per-grain fit of the centre-of-mass grain positions, orientations and stress tensors...

  10. Characterisation of microfocused beam for synchrotron powder diffraction using a new X-ray camera

    International Nuclear Information System (INIS)

    Thomas, C; Potter, J; Tang, C C; Lennie, A R

    2012-01-01

    The powder diffraction beamline I11, Diamond Light Source, is being continually upgraded as requirements of the user community evolve. Intensities of X-rays from the I11 in-vacuum electron undulator in the 3 GeV synchrotron fall off at higher energies. By focusing higher energy X-rays, we can overcome flux limitations, and open up new diffraction experiments. Here, we describe characterisation of microfocusing using compound refractive lenses (CRL). For a relatively modest outlay, we have developed an experimental setup and a novel X-ray camera with good sensitivity and a resolution specification suitable for characterising these focusing optics. We show that vertical oscillations in the focused beam compromise resolution of the source imaged by the CRL. Nevertheless, we have measured CRL focusing properties, and demonstrate the use of energy scanning to determine lens alignment. Real benefits of the intensity gain are illustrated.

  11. On the response of Y 3Al 5O 12: Ce (YAG: Ce) powder scintillating screens to medical imaging X-rays

    Science.gov (United States)

    Kandarakis, I.; Cavouras, D.; Sianoudis, I.; Nikolopoulos, D.; Episkopakis, A.; Linardatos, D.; Margetis, D.; Nirgianaki, E.; Roussou, M.; Melissaropoulos, P.; Kalivas, N.; Kalatzis, I.; Kourkoutas, K.; Dimitropoulos, N.; Louizi, A.; Nomicos, C.; Panayiotakis, G.

    2005-02-01

    The aim of this study was to examine Y 3Al 5O 12:Ce (also known as YAG:Ce) powder scintillator under X-ray imaging conditions. This material shows a very fast scintillation decay time and it has never been used in X-ray medical imaging. In the present study various scintillator layers (screens) with coating thickness ranging from 13 to 166 mg/cm 2 were prepared in our laboratory by sedimentation of Y 3Al 5O 12: Ce powder. Optical emission spectra and light emission efficiency (spectrum area over X-ray exposure) of the layers were measured under X-ray excitation using X-ray tube voltages (80-120 kVp) often employed in general medical radiography and fluoroscopy. Spectral compatibility with various optical photon detectors (photodiodes, photocathodes, charge coupled devices, films) and intrinsic conversion efficiency values were determined using emission spectrum data. In addition, parameters related to X-ray detection, energy absorption efficiency and K-fluorescence characteristic emission were calculated. A theoretical model describing radiation and light transfer through scattering media was used to fit experimental data. Intrinsic conversion efficiency (η≈0.03-0.05) and light attenuation coefficients (σ≈26.5 cm/g) were derived through this fitting. Y 3Al 5O 12:Ce showed peak emission in the wavelength range 530-550 nm. The light emission efficiency was found to be maximum for the 107 mg/cm 2 layer. Due to its "green" emission spectrum, Y 3Al 5O 12:Ce showed excellent compatibility (of the order of 0.9) with the sensitivity of many currently used photodetectors. Taking into account its very fast response Y 3Al 5O 12:Ce could be considered for application in X-ray imaging especially in various digital detectors.

  12. On the response of Y3Al5O12: Ce (YAG: Ce) powder scintillating screens to medical imaging X-rays

    International Nuclear Information System (INIS)

    Kandarakis, I.; Cavouras, D.; Sianoudis, I.; Nikolopoulos, D.; Episkopakis, A.; Linardatos, D.; Margetis, D.; Nirgianaki, E.; Roussou, M.; Melissaropoulos, P.; Kalivas, N.; Kalatzis, I.; Kourkoutas, K.; Dimitropoulos, N.; Louizi, A.; Nomicos, C.; Panayiotakis, G.

    2005-01-01

    The aim of this study was to examine Y 3 Al 5 O 12 :Ce (also known as YAG:Ce) powder scintillator under X-ray imaging conditions. This material shows a very fast scintillation decay time and it has never been used in X-ray medical imaging. In the present study various scintillator layers (screens) with coating thickness ranging from 13 to 166mg/cm 2 were prepared in our laboratory by sedimentation of Y 3 Al 5 O 12 : Ce powder. Optical emission spectra and light emission efficiency (spectrum area over X-ray exposure) of the layers were measured under X-ray excitation using X-ray tube voltages (80-120kVp) often employed in general medical radiography and fluoroscopy. Spectral compatibility with various optical photon detectors (photodiodes, photocathodes, charge coupled devices, films) and intrinsic conversion efficiency values were determined using emission spectrum data. In addition, parameters related to X-ray detection, energy absorption efficiency and K-fluorescence characteristic emission were calculated. A theoretical model describing radiation and light transfer through scattering media was used to fit experimental data. Intrinsic conversion efficiency (ηC ∼0.03-0.05) and light attenuation coefficients (σ∼26.5cm 2 /g) were derived through this fitting. Y 3 Al 5 O 12 :Ce showed peak emission in the wavelength range 530-550nm. The light emission efficiency was found to be maximum for the 107mg/cm 2 layer. Due to its 'green' emission spectrum, Y 3 Al 5 O 12 :Ce showed excellent compatibility (of the order of 0.9) with the sensitivity of many currently used photodetectors. Taking into account its very fast response Y 3 Al 5 O 12 :Ce could be considered for application in X-ray imaging especially in various digital detectors

  13. Qualitative analysis of a powdered diamond sample by particle induced X-ray emission (PIXE)

    International Nuclear Information System (INIS)

    Mabida, C.; Annegarn, H.J.; Renan, M.J.; Sellschop, J.P.F.

    The main purpose of this analysis was to determine whether nickel is present in diamond powder as a trace element. Particle induced X-ray emission (PIXE) showed unambiguously that nickel was present. Due to the convenience of PIXE in multielemental analysis, the investigations also include a number of other trace elements in the sample

  14. Thermal analysis, X-ray powder diffraction and electron microscopy data related with the production of 1:1 Caffeine:Glutaric Acid cocrystals

    Directory of Open Access Journals (Sweden)

    Íris Duarte

    2016-09-01

    Full Text Available The data presented in this article are related to the production of 1:1 Caffeine:Glutaric Acid cocrystals as part of the research article entitled “Green production of cocrystals using a new solvent-free approach by spray congealing” (Duarte et al., 2016 [1]. More specifically, here we present the thermal analysis and the X-ray powder diffraction data for pure Glutaric Acid, used as a raw material in [1]. We also include the X-ray powder diffraction and electron microscopy data obtained for the 1:1 Caffeine:Glutaric Acid cocrystal (form II produced using the cooling crystallization method reported in “Operating Regions in Cooling Cocrystallization of Caffeine and Glutaric Acid in Acetonitrile” (Yu et al., 2010 [2]. Lastly, we show the X-ray powder diffraction data obtained for assessing the purity of the 1:1 Caffeine:Glutaric cocrystals produced in [1].

  15. Analysis and implementation of a space resolving spherical crystal spectrometer for x-ray Thomson scattering experiments.

    Science.gov (United States)

    Harding, E C; Ao, T; Bailey, J E; Loisel, G; Sinars, D B; Geissel, M; Rochau, G A; Smith, I C

    2015-04-01

    The application of a space-resolving spectrometer to X-ray Thomson Scattering (XRTS) experiments has the potential to advance the study of warm dense matter. This has motivated the design of a spherical crystal spectrometer, which is a doubly focusing geometry with an overall high sensitivity and the capability of providing high-resolution, space-resolved spectra. A detailed analysis of the image fluence and crystal throughput in this geometry is carried out and analytical estimates of these quantities are presented. This analysis informed the design of a new spectrometer intended for future XRTS experiments on the Z-machine. The new spectrometer collects 6 keV x-rays with a spherically bent Ge (422) crystal and focuses the collected x-rays onto the Rowland circle. The spectrometer was built and then tested with a foam target. The resulting high-quality spectra prove that a spherical spectrometer is a viable diagnostic for XRTS experiments.

  16. Determination of crystal structures with large known fragments directly from measured X-ray powder diffraction intensities

    International Nuclear Information System (INIS)

    Rius, J.; Miravitlles, C.

    1988-01-01

    A strategy for the determination of crystal structures with large known fragments directly from measured X-ray powder diffraction intensities is presented. It is based on the automated full-symmetry Patterson search method described by Rius and Miravitlles where the Fourier coefficients of the observed Patterson function are modified to allow the use of powder diffraction intensity data. Its application to two structures, one with simulated and one with experimental data, is shown. (orig.)

  17. X-ray excited optical luminescence of polynuclear aromatic hydrocarbons

    Energy Technology Data Exchange (ETDEWEB)

    Oestreich, G.J.

    1979-05-01

    X-ray excited optical luminescence (XEOL) coupled with time resolved spectroscopy was employed to analyze polynuclear aromatic hydrocarbons (PAH) in n-alkane solvents at 10 K. A pulsed XEOL system which was designed around minicomputer control of a medical x-ray unit was developed. Computer software which generated variable width x-ray pulses, monitored timing reference pulses, controlled data acquisition, and analyzed data was written. Phosphorescence decay constants of several PAHs were determined. Synthetic mixtures of zone refined PAHs were prepared and time resolved with the pulsed XEOL technique. Analytical results obtained from the five component mixtures of PAHs at the part per million level were tabulated. Systematic improvements and further development of the pulsed XEOL method were considered.

  18. Development of x-ray laminography under an x-ray microscopic condition

    International Nuclear Information System (INIS)

    Hoshino, Masato; Uesugi, Kentaro; Takeuchi, Akihisa; Suzuki, Yoshio; Yagi, Naoto

    2011-01-01

    An x-ray laminography system under an x-ray microscopic condition was developed to obtain a three-dimensional structure of laterally-extended planar objects which were difficult to observe by x-ray tomography. An x-ray laminography technique was introduced to an x-ray transmission microscope with zone plate optics. Three prototype sample holders were evaluated for x-ray imaging laminography. Layered copper grid sheets were imaged as a laminated sample. Diatomite powder on a silicon nitride membrane was measured to confirm the applicability of this method to non-planar micro-specimens placed on the membrane. The three-dimensional information of diatom shells on the membrane was obtained at a spatial resolution of sub-micron. Images of biological cells on the membrane were also obtained by using a Zernike phase contrast technique.

  19. Direct Structural and Chemical Characterization of the Photolytic Intermediates of Methylcobalamin Using Time-Resolved X-ray Absorption Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Subramanian, Ganesh; Zhang, Xiaoyi; Kodis, Gerdenis; Kong, Qingyu; Liu, Cunming; Chizmeshya, Andrew; Weierstall, Uwe; Spence, John

    2018-04-05

    Cobalt−carbon bond cleavage is crucial to most natural and synthetic applications of the cobalamin class of compounds, and here we present the first direct electronic and geometric structural characteristics of intermediates formed following photoexcitation of methylcobalamin (MeCbl) using time-resolved X-ray absorption spectroscopy (XAS). We catch transients corresponding to two intermediates, in the hundreds of picoseconds and a few microseconds. Highlights of the picosecond intermediate, which is reduced in comparison to the ground state, are elongation of the upper axial Co−C bond and relaxation of the corrin ring. This is not so with the recombining photocleaved products captured at a few microseconds, where the Co−C bond almost (yet not entirely) reverts to its ground state configuration and a substantially elongated lower axial Co−NIm bond is observed. The reduced cobalt site here confirms formation of methyl radical as the photoproduct.

  20. Photo-Induced Spin-State Conversion in Solvated Transition Metal Complexes Probed via Time-Resolved Soft X-ray Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Huse, Nils; Kim, Tae Kyu; Jamula, Lindsey; McCusker, James K.; de Groot, Frank M. F.; Schoenlein, Robert W.

    2010-04-30

    Solution-phase photoinduced low-spin to high-spin conversion in the FeII polypyridyl complex [Fe(tren(py)3)]2+ (where tren(py)3 is tris(2-pyridylmethyliminoethyl)amine) has been studied via picosecond soft X-ray spectroscopy. Following 1A1 --> 1MLCT (metal-to-ligand charge transfer) excitation at 560 nm, changes in the iron L2- and L3-edges were observed concomitant with formation of the transient high-spin 5T2 state. Charge-transfer multiplet calculations coupled with data acquired on low-spin and high-spin model complexes revealed a reduction in ligand field splitting of 1 eV in the high-spin state relative to the singlet ground state. A significant reduction in orbital overlap between the central Fe-3d and the ligand N-2p orbitals was directly observed, consistent with the expected ca. 0.2 Angstrom increase in Fe-N bond length upon formation of the high-spin state. The overall occupancy of the Fe-3d orbitals remains constant upon spin crossover, suggesting that the reduction in sigma-donation is compensated by significant attenuation of pi-back-bonding in the metal-ligand interactions. These results demonstrate the feasibility and unique potential of time-resolved soft X-ray absorption spectroscopy to study ultrafast reactions in the liquid phase by directly probing the valence orbitals of first-row metals as well as lighter elements during the course of photochemical transformations.

  1. Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

    Science.gov (United States)

    Zhang, Hongjia; Sui, Tan; Daisenberger, Dominik; Fong, Kai Soon

    2018-01-01

    High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation. PMID:29543728

  2. Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

    Directory of Open Access Journals (Sweden)

    Hongjia Zhang

    2018-03-01

    Full Text Available High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short. As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation.

  3. Carbon Condensation during High Explosive Detonation with Time Resolved Small Angle X-ray Scattering

    Science.gov (United States)

    Hammons, Joshua; Bagge-Hansen, Michael; Nielsen, Michael; Lauderbach, Lisa; Hodgin, Ralph; Bastea, Sorin; Fried, Larry; May, Chadd; Sinclair, Nicholas; Jensen, Brian; Gustavsen, Rick; Dattelbaum, Dana; Watkins, Erik; Firestone, Millicent; Ilavsky, Jan; van Buuren, Tony; Willey, Trevor; Lawrence Livermore National Lab Collaboration; Los Alamos National Laboratory Collaboration; Washington State University/Advanced Photon Source Team

    Carbon condensation during high-energy detonations occurs under extreme conditions and on very short time scales. Understanding and manipulating soot formation, particularly detonation nanodiamond, has attracted the attention of military, academic and industrial research. An in-situ characterization of these nanoscale phases, during detonation, is highly sought after and presents a formidable challenge even with today's instruments. Using the high flux available with synchrotron X-rays, pink beam small angle X-ray scattering is able to observe the carbon phases during detonation. This experimental approach, though powerful, requires careful consideration and support from other techniques, such as post-mortem TEM, EELS and USAXS. We present a comparative survey of carbon condensation from different CHNO high explosives. This work was performed under the auspices of the US DOE by LLNL under Contract DE-AC52-07NA27344.

  4. Time-resolved absorption measurements on OMEGA

    International Nuclear Information System (INIS)

    Jaanimagi, P.A.; DaSilva, L.; Delettrez, J.; Gregory, G.G.; Richardson, M.C.

    1986-01-01

    Time-resolved measurements of the incident laser light that is scattered and/or refracted from targets irradiated by the 24 uv-beam OMEGA laser at LLE, have provided some interesting features related to time-resolved absorption. The decrease in laser absorption characteristic of irradiating a target that implodes during the laser pulse has been observed. The increase in absorption expected as the critical density surface moves from a low to a high Z material in the target has also been noted. The detailed interpretation of these results is made through comparisons with simulation using the code LILAC, as well as with streak data from time-resolved x-ray imaging and spectroscopy. In addition, time and space-resolved imaging of the scattered light yields information on laser irradiation uniformity conditions on the target. The report consists of viewgraphs

  5. Mechanically activated SHS reaction in the Fe-Al system: in-situ time resolved diffraction using synchrotron radiation

    International Nuclear Information System (INIS)

    Gaffet, E.; Charlot, F.; Klein, D.; Bernard, F.; Niepce, J.C.

    1998-01-01

    The mechanical activation self propagating high temperature synthesis (M.A.S.H.S.) processing is a new way to produce nanocrystalline iron aluminide intermetallic compounds. This process is maily the combination of two steps; in the one hand, a mechanical activation where the Fe - Al powder mixture was milled during a short time at given energy and frequency of shocks and in the other hand, a self propagating high temperature synthesis (S.H.S.) reaction, for which the exothermicity of the Fe + Al reaction is used. This fast propagated MASHS reaction has been in-situ investigated using the time resolved X-ray diffraction (TRXRD) using a X-ray synchrotron beam and an infrared thermography camera, allowing the coupling of the materials structure and the temperature field. The effects of the initial mean compositions, of the milling conditions as well as of the compaction parameters on the MASHS reaction are reported. (orig.)

  6. Time-resolving electron temperature diagnostic for ALCATOR C

    International Nuclear Information System (INIS)

    Fairfax, S.A.

    1984-05-01

    A diagnostic that provides time-resolved central electron temperatures has been designed, built, and tested on the ALCATOR C Tokamak. The diagnostic uses an array of fixed-wavelength x-ray crystal monochromators to sample the x-ray continuum and determine the absolute electron temperature. The resolution and central energy of each channel were chosen to exclude any contributions from impurity line radiation. This document describes the need for such a diagnostic, the design methodology, and the results with typical ALCATOR C plasmas. Sawtooth (m = 1) temperature oscillations were observed after pellet fueling of the plasma. This is the first time that such oscillations have been observed with an x-ray temperature diagnostic

  7. Characterization for solidification and phase transformations of pure-titanium steel weld metal with time-resolved X-ray diffraction system

    International Nuclear Information System (INIS)

    Terasaki, Hidenori; Komizo, Yu-ichi; Nishino, Fumihiro; Ikeda, Masahiko

    2007-01-01

    Understanding and controlling solidification and phase transformation process of weld metal is essential for forming the microstructure with superior mechanical property. Recent evolution of analysis technique makes for solidification and phase transformation process to be in-situ analyzed, in direct and reciprocal lattice space. In the present work, unidirectional-solidification and phase transformation in the weld metal of commercial pure-titanium in Gas Tungsten Arc welding was in-situ observed by using Time-Resolved X-Ray Diffraction system with two-dimensional pixel detector. An undulator beam was used as a probe. Larger diffraction area could be detected in the time-resolution of 0.05 seconds, in unidirectional solidification and subsequent phase transformation process of pure-titanium weld metal. Furthermore, the microstructure formation during β-α phase transformation was in situ observed with High temperature Laser Scanning Confocal Microscopy. The crystal configurations in unidirectional solidification of weld metal and rapid change of phase ratio in reconstructive phase transformation were clearly analyzed. (author)

  8. The X-ray powder diffraction pattern and lattice parameters of perovskite

    International Nuclear Information System (INIS)

    Ball, C.J.; Napier, J.G.

    1988-02-01

    The interplanar spacings and intensities of all lines appearing in the X-ray powder diffraction pattern of perovskite have been calculated. Many of the lines occur in groups with a large amount of overlap. As an aid to identifying the lines which are observed, the intensity profiles of the major groups have been plotted. Those lines which are relatively free of overlap and can be identified unambiguously have been used to calculate the lattice parameters, with the results a=5.4424 ± 0.0001 A, b=7.6417 ± 0.0002 A, c=5.3807 ± 0.0001 A

  9. Development of real-time x-ray microtomography system

    International Nuclear Information System (INIS)

    Takano, H; Morikawa, M; Konishi, S; Azuma, H; Shimomura, S; Tsusaka, Y; Kagoshima, Y; Nakano, S; Kosaka, N; Yamamoto, K

    2013-01-01

    We have developed a four-dimensional (4D) x-ray microcomputed tomography (CT) system that can obtain time-lapse CT volumes in real time. The system consists of a high-speed sample rotation system and a high-frame-rate x-ray imager, which are installed at a synchrotron radiation x-ray beamline. As a result of system optimization and introduction of a 'zoom resolution' procedure, a real-time 4D CT movie with a frame rate of 30 was obtained with a voxel size of 2.5 μm using 10 keV x-rays

  10. Measurement and analysis of thermal conductivity of isotopically controlled silicon layers by time-resolved X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Eon, S.; Frieling, R.; Bracht, H. [Institute for Materials Physics, University of Muenster, 48149 Muenster (Germany); Plech, A. [Institute for Photon Science and Synchrotron Radiation (IPS), 76344 Eggenstein-Leopoldshafen (Germany)

    2016-11-15

    Nanostructuring is considered to be an efficient way to tailor phonon scattering and to reduce the thermal conductivity while keeping good electronic properties. This can be ideally realized by mass modulation of chemical identical elements. In this work, we report measurements of the crossplane thermal conductivity of isotopically modulated {sup 28}Si/{sup 30}Si multilayer structures and of isotopically pure {sup 28}Si layers by means of time-resolved X-ray scattering. Compared to earlier investigations, an improved measurement technique has been applied to determine the cooling behavior of a top gold metal layer after laser excitation with picosecond time resolution until thermal equilibration is established. Detailed analysis of the cooling behavior not only confirms a reduced thermal conductivity of {sup 28}Si/{sup 30}Si multilayer structures compared to natural and isotopically enriched {sup 28}Si layers but also provides evidence of direct laser heating of the Si layer. This and extrinsic effects affecting the cooling behavior of the gold layer are taken into account to determine the thermal conductivity by means of the pump-and-probe measurement technique. (copyright 2016 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  11. A MEMS-based high frequency x-ray chopper

    Energy Technology Data Exchange (ETDEWEB)

    Siria, A; Schwartz, W; Chevrier, J [Institut Neel, CNRS-Universite Joseph Fourier Grenoble, BP 166, F-38042 Grenoble Cedex 9 (France); Dhez, O; Comin, F [ESRF, 6 rue Jules Horowitz, F-38043 Grenoble Cedex 9 (France); Torricelli, G [Department of Physics and Astronomy, University of Leicester, University Road, Leicester LE1 7RH (United Kingdom)

    2009-04-29

    Time-resolved x-ray experiments require intensity modulation at high frequencies (advanced rotating choppers have nowadays reached the kHz range). We here demonstrate that a silicon microlever oscillating at 13 kHz with nanometric amplitude can be used as a high frequency x-ray chopper. We claim that using micro-and nanoelectromechanical systems (MEMS and NEMS), it will be possible to achieve higher frequencies in excess of hundreds of megahertz. Working at such a frequency can open a wealth of possibilities in chemistry, biology and physics time-resolved experiments.

  12. X-ray Outburst in Mira A

    OpenAIRE

    Karovska, M.; Schlegel, E.; Hack, W.; Wood, B.

    2005-01-01

    We report here the Chandra ACIS-S detection of a bright soft X-ray transient in the Mira AB interacting symbiotic-like binary. We resolved the system for the first time in the X-rays. Using Chandra and HST images we determined that the unprecedented outburst is likely associated with the cool AGB star (Mira A), the prototype of Mira-type variables. X-rays have never before been detected from an AGB star, and the recent activity signals that the system is undergoing dramatic changes. The total...

  13. Characterization by X-ray tomography of granulated alumina powder during in situ die compaction

    Energy Technology Data Exchange (ETDEWEB)

    Cottrino, Sandrine; Jorand, Yves, E-mail: yves.jorand@insa-lyon.fr; Maire, Eric; Adrien, Jérôme

    2013-07-15

    Compaction process, the aim of which being to obtain green bodies with low porosity and small size, is often used before sintering treatment. Prior to die filling, the ceramic powder is generally granulated to improve flowability. However during compaction, density heterogeneity and critical size defects may appear due to intergranule and granule-die wall frictions. In this work, the influence of granule formulation on the compact morphology has been studied. To do so, a compaction setup was installed inside an X-ray tomography equipment so that the evolution of the compact morphology could be analysed during the whole compaction process. We have demonstrated that high humidity rate and the addition of binder in the granule formulation increase density heterogeneity and generate larger defects. - Highlights: • An original compaction set up was installed inside an X-Ray tomography equipment. • The compaction process of granulated ceramic powder is imaged. • The compact green microstructure is quantified and related to the compaction stages. • The most detrimental defects of dry-pressed parts are caused by hollow granules. • Formulations without binder allow a reduction of the number of large defects.

  14. Time-resolved X-ray scattering program at the Advanced Photon Source

    International Nuclear Information System (INIS)

    Rodricks, B.

    1994-01-01

    The Time-Resolved Scattering Program's goal is the development of instruments and techniques for time-resolved studies. This entails the development of wide bandpass and focusing optics, high-speed detectors, mechanical choppers, and components for the measurement and creation of changes in samples. Techniques being developed are pump-probe experiments, single-bunch scattering experiments, high-speed white and pink beam Laue scattering, and nanosecond to microsecond synchronization of instruments. This program will be carried out primarily from a white-beam, bend-magnet source, experimental station, 1-BM-B, that immediately follows the first optics enclosure (1-BM-A). This paper will describe the experimental station and instruments under development to carry out the program

  15. Driving force behind adsorption-induced protein unfolding: a time-resolved X-ray reflectivity study on lysozyme adsorbed at an air/water interface.

    Science.gov (United States)

    Yano, Yohko F; Uruga, Tomoya; Tanida, Hajime; Toyokawa, Hidenori; Terada, Yasuko; Takagaki, Masafumi; Yamada, Hironari

    2009-01-06

    Time-resolved X-ray reflectivity measurements for lysozyme (LSZ) adsorbed at an air/water interface were performed to study the mechanism of adsorption-induced protein unfolding. The time dependence of the density profile at the air/water interface revealed that the molecular conformation changed significantly during adsorption. Taking into account previous work using Fourier transform infrared (FTIR) spectroscopy, we propose that the LSZ molecules initially adsorbed on the air/water interface have a flat unfolded structure, forming antiparallel beta-sheets as a result of hydrophobic interactions with the gas phase. In contrast, as adsorption continues, a second layer forms in which the molecules have a very loose structure having random coils as a result of hydrophilic interactions with the hydrophilic groups that protrude from the first layer.

  16. X-ray imaging and spectroscopic measurements of implosions

    International Nuclear Information System (INIS)

    Hammel, B.A.; Ress, D.R.; Keane, C.J.; Kilkenny, J.D.; Landen, O.L.; Bell, P.; Pasha, R.; Wallace, R.J.; Bradley, D.K.

    1992-01-01

    Time-resolved x-ray measurements are essential in the investigation of laser-driven inertial confinement fusion, where neutron and x-ray emission are the only observable signatures of the compressed core conditions. High-speed detectors, available for x-ray measurement, provide a means of measuring the rapidly evolving conditions in imploding capsules on picosecond time scales. We address a wide range of issues in our indirectly driven implosion experiments on Nova, with a large variety of x-ray measurement techniques. Critical issues include symmetry of the compressed core, fuel density and temperature and hydrodynamic mix at the pusher/fuel interface

  17. Grain-resolved elastic strains in deformed copper measured by three-dimensional X-ray diffraction

    DEFF Research Database (Denmark)

    Oddershede, Jette; Schmidt, Søren; Poulsen, Henning Friis

    2011-01-01

    This X-ray diffraction study reports the grain-resolved elastic strains in about 1000 randomly oriented grains embedded in a polycrystalline copper sample. Diffraction data were collected in situ in the undeformed state and at a plastic strain of 1.5% while the sample was under tensile load...

  18. A high-temperature furnace and a heating/drawing device designed for time-resolved X-ray diffraction measurements of polymer solids using imaging plates

    International Nuclear Information System (INIS)

    Murakami, Syozo; Tanno, Kiyomitsu; Tsuji, Masaki; Kohjiya, Shinzo

    1995-01-01

    For time-resolved X-ray diffraction measurements using the imaging plate system in the drawing and/or heating process of polymer solids, a high-temperature furnace for heat treatment and a heating/drawing device were newly designed and constructed. Then, to demonstrate their performance, some experimental results obtained in the drawing process of an extruded/blown film of high-density polyethylene at room temperature and in the crystallization process of an oriented amorphous film of poly(ethylene naphthalene-2,6-dicarboxylate) by heating were presented. Other experimental results obtained using them were also briefly cited. (author)

  19. Crystallized solids characterization by X-ray diffraction

    International Nuclear Information System (INIS)

    Broll, N.

    1996-01-01

    This work deals with the crystallized solids characterization by X-ray diffraction. The powders diffraction principle is described. Then are given the different powders diffraction experimental methods. An X-ray diffraction device is essentially constituted of three parts: the X-rays source, the sample and the detector. The source is usually constituted by an X-rays tube whereas the sample can be fixed on a photographic chamber or put on a goniometer. The different photographic chambers which can be used (Debye-Scherrer, Seeman-Bohlin and Guinier) are described. The powders diffractometer the most used is a Bragg-Brentano focusing diffractometer because it allows to obtain very sharp spectral lines and an important diffracted intensity. The detectors which are the mainly used are the scintillation counters. The most important use in powders diffractometry is the identification of the different phases of a sample. The phases identification consists to compare the unknown sample spectrum at those of standard materials indexed until now. Two methods exist at present. They are explained and their limits in the phases search are given. Another use of the X-ray diffraction is the quantitative analysis. It consists to determine the concentrations of each crystal phases of a sample. The principles of these quantitative methods are given. The lattice parameters of a polycrystal material can be determined from its X-ray pattern too with a very high precision. The way to index powders patterns is given. The residual stresses of materials can also be estimated. The principle of this measured method is explained. It is at last possible to study from an X-ray pattern, the material grain orientations during the different steps of preparation and working. (O.M.). 13 refs., 19 figs., 1 tab

  20. JAX: a micro-computer based X-ray diffractometer controller

    International Nuclear Information System (INIS)

    Naval, P.C. Jr.

    1987-05-01

    This paper describes a micro-computer based X-ray diffractometer controller and explores its possibilities in simplifying acquisition and analysis of X-ray powder diffraction data. The interrupt-driven controller can operate in both present time and present count data acquisition modes and allows a data analysis program to execute concurrently with data collection. (Auth.). 16 figs.; 2 tabs

  1. Time-resolved x-ray diffraction from frog skeletal muscle during shortening against an inertial load and a quick release

    International Nuclear Information System (INIS)

    Amemiya, Yoshiyuki; Hashizume, Hiroo; Tameyasu, Tsukasa; Tanaka, Hidehiro; Sugi, Haruo.

    1980-01-01

    A group of Japanese researchers conducted, for the first time in this field, experiments on time-resolved x-ray diffraction of frog (bullfrog, Rana catesbeiana) skeletal muscle in conditions where both the force and the muscle length change with time. During an isotonic twitch under a load of about 0.3 P 0 , the intensity ratio started falling on stimulation and reached a minimum value of 0.5 - 0.6 at the early shortening phase, which was maintained until the beginning of relaxation. Except that the minimum value was not retained until the start of relaxation, the same was observed during a twitch against an inertial load whereby the peak force exerted by the muscle was about 0.4 P 0 . The results may be taken to indicate that the change in the intensity ratio reflects not the time course of shortening but that of force generation. When a quick release (3 - 4% of muscle length) was applied during the rising phase of an isometric twitch, the intensity ratio showed no distinct change. Judging from tentative calculation results, however, the foregoing result is subject to further experiments with a much improved time resolution of the measurements. (Kitajima, A.)

  2. X-ray holography

    International Nuclear Information System (INIS)

    Faigel, G.; Tegze, M.; Belakhovsky, M.; Marchesini, S.; Bortel, G.

    2003-01-01

    In the last decade holographic methods using hard X-rays were developed. They are able to resolve atomic distances, and can give the 3D arrangement of atoms around a selected element. Therefore, hard X-ray holography has potential applications in chemistry, biology and physics. In this article we give a general description of these methods and discuss the developments in the experimental technique. The capabilities of hard X-ray holography are demonstrated by examples

  3. Measuring and understanding ultrafast phenomena using X-rays

    DEFF Research Database (Denmark)

    Haldrup, Kristoffer; Nielsen, Martin Meedom

    2014-01-01

    Within the last decade, significant advances in X-ray sources and instrumentation as well as simultaneous developments in analysis methodology has allowed the field of fast- and ultrafast time-resolved X-ray studies of solution-state systems to truly come of age. We here describe some aspects of ...

  4. An Inquiry-Based Project Focused on the X-Ray Powder Diffraction Analysis of Common Household Solids

    Science.gov (United States)

    Hulien, Molly L.; Lekse, Jonathan W.; Rosmus, Kimberly A.; Devlin, Kasey P.; Glenn, Jennifer R.; Wisneski, Stephen D.; Wildfong, Peter; Lake, Charles H.; MacNeil, Joseph H.; Aitken, Jennifer A.

    2015-01-01

    While X-ray powder diffraction (XRPD) is a fundamental analytical technique used by solid-state laboratories across a breadth of disciplines, it is still underrepresented in most undergraduate curricula. In this work, we incorporate XRPD analysis into an inquiry-based project that requires students to identify the crystalline component(s) of…

  5. Phased-Resolved Strain Measuremetns in Hydrated Ordinary Portland Cement Using Synchrotron x-Rays (Prop. 2003-033)

    International Nuclear Information System (INIS)

    Biernacki, Joseph J.; Watkins, Thomas R.; Parnham, C.J.; Hubbard, Camden R.; Bai, J.

    2006-01-01

    X-ray diffraction methods developed for the determination of residual stress states in crystalline materials have been applied to study residual strains and strains because of mechanical loading of ordinary portland cement paste. Synchrotron X-rays were used to make in situ measurements of interplanar spacings in the calcium hydroxide (CH) phase of hydrated neat portland cement under uniaxial compression. The results indicate that strains on the order of 1/100 000 can be resolved providing an essentially new technique by which to measure the phase-resolved meso-scale mechanical behavior of cement under different loading conditions. Evaluation of these strain data in view of published elastic parameters for CH suggests that the CH carries a large fraction of the applied stress and that plastic interactions with the matrix are notable.

  6. The x-ray laser coherence experiments in neon-like yttrium

    International Nuclear Information System (INIS)

    Shimkaveg, G.M.; Carter, M.R.; Walling, R.S.; Ticehurst, J.M.; Koch, J.A.; Mrowka, S.; Trebes, J.E.; MacGowan, B.J.; Da Silva, L.B.; Matthews, D.L.; London, R.A.; Stewart, R.E.

    1992-01-01

    We present recent results from neon-like x-ray laser experiments conducted at the Nova laser's Two-Beam Facility. This begins a series of experiments aimed at the characterization and control of the degree of spatial coherece in our soft x-ray laser beams, important to planned applications areas susch as microscopy and holography. New instrumentation developed for this effort include a fully time-resolved coherence diagnostic (which records a multiple-slit diffraction pattern) and wide-angle extreme ultraviolet spectrographs and beam divergence cameras. We present new measurements of beam profiles and gain, as well as spatial coherence data such as time-resolved multi-slit diffraction patterns. This new time-resolved coherence data exhibit aperture functions which increase in size during the time of the lasing. Also, some preliminary data is given from the first ''double-foil'' experiments, involving two x-ray amplifiers spatially separated by 29 cm and shot sequentially, in an ''oscillator-amplifier'' configuration

  7. Spatially Resolved Hard X-ray Emission in the Central 5 kpc of the Galaxy Merger NGC 6240

    Science.gov (United States)

    Wang, Junfeng; Nardini, E.; Fabbiano, G.; Karovska, M.; Elvis, M.; Pellegrini, S.; Max, C. E.; Risaliti, G.; U, V.; Zezas, A.

    2013-04-01

    We have obtained a deep, sub-arcsecond resolution X-ray image of the nuclear region of the luminous galaxy merger NGC 6240 with Chandra, which resolves the X-ray emission from the pair of active nuclei and the diffuse hot gas in great detail. We detect extended hard X-ray emission from 70 million K hot gas over a spatial scale of 5 kpc, indicating the presence of fast shocks with velocity of 2200 km/s. For the first time we obtain spatial distribution of this highly ionized gas emitting FeXXV and find that it shows a remarkable correspondence to the large scale morphology of H_2(1-0) S(1) line emission and Hα filaments. Propagation of fast shocks originated in the starburst driven wind into the ambient dense gas can account for this morphological correspondence. Both the energetics and the iron mass in the hot gas are consistent with the expected injection from the supernovae explosion during the starburst that is commensurate with its high star formation rate.

  8. a Time-Resolved X-Ray Scattering Study of the Ordering Kinetics in COPPER(3)-GOLD

    Science.gov (United States)

    Shannon, Robert Francis, Jr.

    Time-resolved x-ray scattering has been used to study ordering kinetics in single crystal bulk Cu _3Au, as well as in sputtered and molecular beam epitaxy grown films. After annealing at high temperatures the sample is rapidly quenched to fixed temperatures below the order-disorder transition temperature. The development of order is monitored in real time using scattering techniques. The bulk sample clearly showed three regimes: nucleation, ordering, and coarsening. The anisotropic superlattice peaks that reflect the domains structure are investigated in connection with the ordering kinetics. The line shape of the scattering function exhibits a crossover from gaussian to lorentzian-squared as the system goes from the ordering regime to the coarsening regime. Coarsening in Cu_3Au is consistent with curvature driven growth. Domain coarsening in stoichiometric sputtered films is also consistent with curvature driven growth. However, coarsening in copper rich films proceeds much more slowly. The results suggest the extra copper affects the ordering kinetics in the same way diffusive impurities would, resulting in a logarithmic like time dependence. The M.B.E. films show a slowing of the growth at late times. The 4500A film starts out with curvature driven growth but then continuously slows down as the domains grow. The 710A film shows an interesting temperature dependence for the growth, in such a way that at temperatures close to the transition, the domain growth almost freezes at late times. The dominate factor is probably strain, all of the trends for slower growth are consistent with greater strain. The dimensionality in the M.B.E. film systems is considered. The scaling in the 4500A and 710A films is clearly three dimensional. However, the dimension of the scaling in the 260A film is unclear.

  9. A multiple CCD X-ray detector and its first operation with synchrotron radiation X-ray beam

    CERN Document Server

    Suzuki, M; Kumasaka, T; Sato, K; Toyokawa, H; Aries, I F; Jerram, P A; Ueki, T

    1999-01-01

    A 4x4 array structure of 16 identical CCD X-ray detector modules, called the multiple CCD X-ray detector system (MCCDX), was submitted to its first synchrotron radiation experiment at the protein crystallography station of the RIKEN beamline (BL45XU) at the SPring-8 facility. An X-ray diffraction pattern of cholesterol powder was specifically taken in order to investigate the overall system performance.

  10. Time-resolved X-ray absorption spectroscopy for laser-ablated silicon particles in xenon gas

    International Nuclear Information System (INIS)

    Makimura, Tetsuya; Sakuramoto, Tamaki; Murakami, Kouichi

    1996-01-01

    We developed a laboratory-scale in situ apparatus for soft X-ray absorption spectroscopy with a time resolution of 10 ns and a space resolution of 100 μm. Utilizing this spectrometer, we have investigated the dynamics of silicon atoms formed by laser ablation in xenon gas. It was found that 4d-electrons in the xenon atoms are excited through collision with electrons in the laser-generated silicon plasma. (author)

  11. Ultrafast, laser-based, x-ray science: the dawn of atomic-scale cinematography

    International Nuclear Information System (INIS)

    Barty, C.P.J.

    2000-01-01

    The characteristics of ultrafast chirped pulse amplification systems are reviewed. Application of ultrafast chirped pulse amplification to the generation of femtosecond, incoherent, 8-keV line radiation is outlined and the use of femtosecond laser-based, x-rays for novel time-resolved diffraction studies of crystalline dynamics with sub-picosecond temporal resolution and sub-picometer spatial resolution is reviewed in detail. Possible extensions of laser-based, x-ray technology and evaluation of alternative x-ray approaches for time-resolved studies of the atomic scale dynamics are given. (author)

  12. Ultrafast, laser-based, x-ray science: the dawn of atomic-scale cinematography

    Energy Technology Data Exchange (ETDEWEB)

    Barty, C.P.J. [University of California, Department of Applied Mechanics and Engineering Science, Urey Hall, Mali Code 0339, San Diego, La Jolla, CA (United States)

    2000-03-01

    The characteristics of ultrafast chirped pulse amplification systems are reviewed. Application of ultrafast chirped pulse amplification to the generation of femtosecond, incoherent, 8-keV line radiation is outlined and the use of femtosecond laser-based, x-rays for novel time-resolved diffraction studies of crystalline dynamics with sub-picosecond temporal resolution and sub-picometer spatial resolution is reviewed in detail. Possible extensions of laser-based, x-ray technology and evaluation of alternative x-ray approaches for time-resolved studies of the atomic scale dynamics are given. (author)

  13. Invited article: The fast readout low noise camera as a versatile x-ray detector for time resolved dispersive extended x-ray absorption fine structure and diffraction studies of dynamic problems in materials science, chemistry, and catalysis

    International Nuclear Information System (INIS)

    Labiche, Jean-Claude; Mathon, Olivier; Pascarelli, Sakura; Newton, Mark A.; Ferre, Gemma Guilera; Curfs, Caroline; Vaughan, Gavin; Homs, Alejandro; Carreiras, David Fernandez

    2007-01-01

    Originally conceived and developed at the European Synchrotron Radiation Facility (ESRF) as an 'area' detector for rapid x-ray imaging studies, the fast readout low noise (FReLoN) detector of the ESRF [J.-C. Labiche, ESRF Newsletter 25, 41 (1996)] has been demonstrated to be a highly versatile and unique detector. Charge coupled device (CCD) cameras at present available on the public market offer either a high dynamic range or a high readout speed. A compromise between signal dynamic range and readout speed is always sought. The parameters of the commercial cameras can sometimes be tuned, in order to better fulfill the needs of specific experiments, but in general these cameras have a poor duty cycle (i.e., the signal integration time is much smaller than the readout time). In order to address scientific problems such as time resolved experiments at the ESRF, a FReLoN camera has been developed by the Instrument Support Group at ESRF. This camera is a low noise CCD camera that combines high dynamic range, high readout speed, accuracy, and improved duty cycle in a single image. In this paper, we show its application in a quasi-one-dimensional sense to dynamic problems in materials science, catalysis, and chemistry that require data acquisition on a time scale of milliseconds or a few tens of milliseconds. It is demonstrated that in this mode the FReLoN can be applied equally to the investigation of rapid changes in long range order (via diffraction) and local order (via energy dispersive extended x-ray absorption fine structure) and in situations of x-ray hardness and flux beyond the capacity of other detectors

  14. Time switch for X-ray diagnosis apparatus

    Energy Technology Data Exchange (ETDEWEB)

    Distler, G; Goetzl, H

    1977-04-07

    A time switch for dental X-rays consists of a knob to select exposure time. Two scales are concentrically mounted, one for time, and one with the various tooth symbols, in such a way that the various teeth are in correspondence with the usually recommended times. However, should the X-ray tube characteristics vary at some stage, by pressing the knob, then turning, the 'tooth scale' can be rotated for setting the exposure times at higher or lower levels.

  15. Radial Growth of Self-Catalyzed GaAs Nanowires and the Evolution of the Liquid Ga-Droplet Studied by Time-Resolved in Situ X-ray Diffraction.

    Science.gov (United States)

    Schroth, Philipp; Jakob, Julian; Feigl, Ludwig; Mostafavi Kashani, Seyed Mohammad; Vogel, Jonas; Strempfer, Jörg; Keller, Thomas F; Pietsch, Ullrich; Baumbach, Tilo

    2018-01-10

    We report on a growth study of self-catalyzed GaAs nanowires based on time-resolved in situ X-ray structure characterization during molecular-beam-epitaxy in combination with ex situ scanning-electron-microscopy. We reveal the evolution of nanowire radius and polytypism and distinguish radial growth processes responsible for tapering and side-wall growth. We interpret our results using a model for diameter self-stabilization processes during growth of self-catalyzed GaAs nanowires including the shape of the liquid Ga-droplet and its evolution during growth.

  16. Elasticity of Tantalum to 105 Gpa using a stress and angle-resolved x-ray diffraction

    International Nuclear Information System (INIS)

    Cynn, H; Yoo, C S

    1999-01-01

    Determining the mechanical properties such as elastic constants of metals at Mbar pressures has been a difficult task in experiment. Following the development of anisotropic elastic theory by Singh et al.[l], Mao et a1.[2] have recently developed a novel experimental technique to determine the elastic constants of Fe by using the stress and energy-dispersive x-ray diffraction (SEX). In this paper, we present an improved complementary technique, stress and angle-resolved x-ray diffraction (SAX), which we have applied to determine the elastic constants of tantalum to 105 GPa. The extrapolation of the tantalum elastic data shows an excellent agreement with the low-pressure ultrasonic data[3]. We also discuss the improvement of this SAX method over the previous SEX.[elastic constant, anisotropic elastic theory, angle-dispersive synchrotron x-ray diffraction, mechanical properties

  17. CONTINUING THE DEVELOPMENT OF A 100 FEMTOSECOND X-RAY DETECTOR

    International Nuclear Information System (INIS)

    Zenghu Chang

    2005-01-01

    The detector is an x-ray streak camera running in accumulation mode for time resolved x-ray studies at the existing third generation synchrotron facilities and will also be used for the development and applications of the fourth generation x-ray sources. We have made significant progress on both the detector development and its applications at Synchrotron facilities

  18. Solid-state structural properties of 2,4,6-trimethoxybenzene derivatives, determined directly from powder X-ray diffraction data in conjunction with other techniques

    International Nuclear Information System (INIS)

    Pan Zhigang; Xu Mingcan; Cheung, Eugene Y.; Platts, James A.; Harris, Kenneth D.M.; Constable, Edwin C.; Housecroft, Catherine E.

    2006-01-01

    Structural properties of 2,4,6-trimethoxybenzaldehyde, 2,4,6-trimethoxybenzyl alcohol and 2,4,6-trimethoxyacetophenone have been determined directly from powder X-ray diffraction data, using the direct-space Genetic Algorithm (GA) technique for structure solution followed by Rietveld refinement. Structural similarities and contrasts within this family of materials are elucidated. The work illustrates the value of utilizing information from other sources, including spectroscopic data and computational techniques, as a means of augmenting the structural knowledge established from the powder X-ray diffraction data

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

    Directory of Open Access Journals (Sweden)

    Tatiana Minkina

    2017-04-01

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

  20. Deflection evaluation using time-resolved radiography

    International Nuclear Information System (INIS)

    Fry, D.A.; Lucero, J.P.

    1990-01-01

    Time-resolved radiography is the creation of an x-ray image for which both the start-exposure and stop-exposure times are known with respect to the event under study. The combination of image and timing are used to derive information about the event. The authors have applied time-resolved radiography to evaluate motions of explosive-driven events. In the particular application discussed in this paper, the author's intent is to measure maximum deflections of the components involved. Exposures are made during the time just before to just after the event of interest occurs. A smear or blur of motion out to its furthest extent is recorded on the image. Comparison of the dynamic images with static images allows deflection measurements to be made

  1. submitter Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

    CERN Document Server

    Zhang, Hongjia; Salvati, Enrico; Daisenberger, Dominik; Lunt, Alexander J G; Fong, Kai Soon; Song, Xu; Korsunsky, Alexander M

    2018-01-01

    High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated...

  2. Short irradiation time characteristics of the inverter type X-ray generator

    International Nuclear Information System (INIS)

    Miyazaki, Shigeru; Hara, Takamitu; Matutani, Kazuo; Saito, Kazuhiko.

    1994-01-01

    The linearity of the X-ray output is an important factor in radiography. It is a composite of the linearities of the X-ray tube voltage, the X-ray tube current, and the exposure time. This paper focuses on the linearity of exposure time. Non-linearity of the X-ray output for short-time exposure became a problem when the three-phase X-ray generator was introduced. This paper describes the inverter-type X-ray generator, which is expected to become predominant in the future. Previously, we investigated X-ray output linearity during short-time exposure using the technique of dynamic study. In this paper, we describe the application of a digital memory and a personal computer to further investigation. The non-linearity of the X-ray output was caused by irregular waveforms of the X-ray tube voltage found at the rise time and the fall time. When the rise time was about 0.6 ms, the non-linearity was about 2%, which is negligibly small. The non-linearity due to the fall time of the X-ray tube varied greatly according to the X-ray tube current. For the minimum irradiation time of 1 ms, 4% to 27% of the non-linearity was attributable to the fall time. The main cause was the stray capacitance of the X-ray high-voltage cables. When the X-ray tube current exceeded 400 mA, the rise time was almost equal to the fall time, and the problem did not occur. Consequently, the ideal generator should have a fall time which is equal to the rise time of the X-ray tube voltage. Strictly speaking, such a generator should have rectangular waveforms. (author)

  3. The X-ray Astronomy Recovery Mission

    Science.gov (United States)

    Tashiro, M.; Kelley, R.

    2017-10-01

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

  4. Time-resolved imaging of purely valence-electron dynamics during a chemical reaction

    DEFF Research Database (Denmark)

    Hockett, Paul; Bisgaard, Christer Z.; Clarkin, Owen J.

    2011-01-01

    Chemical reactions are manifestations of the dynamics of molecular valence electrons and their couplings to atomic motions. Emerging methods in attosecond science can probe purely electronic dynamics in atomic and molecular systems(1-6). By contrast, time-resolved structural-dynamics methods...... such as electron(7-10) or X-ray diffraction(11) and X-ray absorption(12) yield complementary information about the atomic motions. Time-resolved methods that are directly sensitive to both valence-electron dynamics and atomic motions include photoelectron spectroscopy(13-15) and high-harmonic generation(16......,17): in both cases, this sensitivity derives from the ionization-matrix element(18,19). Here we demonstrate a time-resolved molecular-frame photoelectron-angular-distribution (TRMFPAD) method for imaging the purely valence-electron dynamics during a chemical reaction. Specifically, the TRMFPADs measured during...

  5. Challenge for real-time and real-space resolved spectroscopy of surface chemical reactions. Aiming at trace of irreversible and inhomogeneous reactions

    International Nuclear Information System (INIS)

    Amemiya, Kenta

    2015-01-01

    A novel experimental technique, time-resolved wavelength-dispersive soft X-ray imaging spectroscopy, is proposed in order to achieve real-time and real-space resolved spectroscopy for the observation of irreversible and inhomogeneous surface chemical reactions. By combining the wavelength-dispersed soft X rays, in which the X-ray wavelength (photon energy) changes as a function of position on the sample, with the photoelectron emission microscope, the soft X-ray absorption spectra are separately obtained at different positions on the sample without scanning the X-ray monochromator. Therefore, the real-time resolved measurement of site-selective soft X-ray absorption spectroscopy is realized in one event without repeating the chemical reaction. It is expected that the spatial distribution of different chemical species is traced during the surface chemical reaction, which is essential to understand the reaction mechanism. (author)

  6. Spatially resolved x-ray laser spectra and demonstration of gain in nickel-like systems

    Energy Technology Data Exchange (ETDEWEB)

    Whelan, D.A.; Keane, C.J.; MacGowan, B.J.; Matthews, D.L.; Trebes, J.E.; Eckart, M.J.

    1987-09-25

    A recent series of experiments have provided spatially resolved near field images of several candidate x-ray lasing transition in neon-like, nickel-like, and hydrogen-like ions from laser-produced plasmas. From these time-gated, spatially, and spectrally resolved measurements the source size for the J = 0 - 1 and the J = 2 - 1 transitions in Ne-like selenium have been determined. Source regions as small as 50 ..mu..m have been observed on transitions with gain-length products >9. In addition, we have obtained the first experimental evidence for the amplification of spontaneous emission in the nickel-like ions of europium and ytterbium. Gains of order 1 cm/sup -1/ and gain-length products of up to 3.8 are observed on the J = 0 - 1, 4d-4p transitions in Eu + 35 at 65.26 and 71.00 A. Analogous transitions in Yb = +42 have been identified and some evidence for ASE has been observed. 7 refs., 11 figs.

  7. Spatially resolved X-ray laser spectra and demonstration of gain in nickel-like systems

    International Nuclear Information System (INIS)

    Whelan, D.A.; Keane, C.J.; MacGowan, B.J.; Matthews, D.L.; Trebes, J.E.; Eckart, M.J.

    1987-01-01

    A recent series of experiments have provided spatially resolved near field images of several candidate x-ray lasing transition in neon-like, nickel-like, and hydrogen-like ions from laser-produced plasmas. From these time-gated, spatially, and spectrally resolved measurements the source size for the J=0-1 and the J=2-1 transitions in Ne-like selenium have been determined. Source regions as small as 50 μm have been observed on transitions with gain-length products >9. In addition, the authors have obtained the first experimental evidence for the amplification of spontaneous emission in the nickel-like ions of europium and ytterbium. Gains of order 1 cm/sup -1/ and gain-length products of up to 3.8 are observed on the J=0-1,4d-4p transitions in Eu/sup +35/ at 65.83 and 71.00A. Analogous transitions in Yb/sup +42/ have been identified and some evidence for ASE has been observed

  8. Real-time soft x-ray imaging on composite materials

    International Nuclear Information System (INIS)

    Polichar, R.

    1985-01-01

    The increased use of composite materials in aircraft structures has emphasized many of the unique and difficult aspects of the inspection of such components. Ultrasound has been extensively applied to certain configurations since it is relatively sensitive to laminar discontinuities in structure. Conversely, the use of conventional x-ray examination has been severely hampered by the fact that these composite materials are virtually transparent to the x-ray energies commonly encountered in industrial radiography (25 kv and above). To produce images with contrast approaching conventional radiography, one must use x-ray beams with average energies below 10 KEV where the absorption coefficients begin to rise rapidly for these low atomic number materials. This new regime of soft x-rays presents a major challenge to real-time imaging components. Special screen and window technology is required if these lower energy x-rays are to be effectively detected. Moreover, conventional x-ray tubes become very inefficient for generating the required x-ray flux at potentials much below 29 kv and the increased operating currents put significant limitations on conventional power sources. The purpose of this paper is to explore these special problems related to soft x-ray real-time imaging and to define the optimal technologies. Practical results obtained with the latest commerical and developmental instruments for real-time imaging will be shown. These instruments include recently developed imaging systems, new x-ray tubes and various approaches to generator design. The measured results convincingly demonstrate the effectiveness practicality of real-time soft x-ray imaging. They also indicate the major changes in technology and approach that must be taken for practical systems to be truly effective

  9. The advantages of soft X-rays and cryogenic spectrometers for measuring chemical speciation by X-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Drury, Owen B. [Lawrence Livermore National Laboratory, Advanced Detector Group, 7000 East Ave., L-270, Livermore, CA 94550 (United States); UC Davis, Biophysics Graduate Group, 1 Shields Ave, CA 95616 (United States); LBNL, Advanced Biological and Environmental X-ray Facility, 1 Cyclotron Road, MS 6-2100, Berkeley, CA 92720 (United States); Friedrich, Stephan [Lawrence Livermore National Laboratory, Advanced Detector Group, 7000 East Ave., L-270, Livermore, CA 94550 (United States) and LBNL, Advanced Biological and Environmental X-ray Facility, 1 Cyclotron Road, MS 6-2100, Berkeley, CA 92720 (United States)]. E-mail: friedrich1@llnl.gov; George, Simon J. [LBNL, Advanced Biological and Environmental X-ray Facility, 1 Cyclotron Road, MS 6-2100, Berkeley, CA 92720 (United States); Cramer, Stephen P. [UC Davis, Biophysics Graduate Group, 1 Shields Ave, CA 95616 (United States); LBNL, Advanced Biological and Environmental X-ray Facility, 1 Cyclotron Road, MS 6-2100, Berkeley, CA 92720 (United States)

    2006-04-15

    We have built a 36-pixel high-resolution superconducting tunnel junction (STJ) soft X-ray spectrometer for chemical analysis of dilute metals by fluorescence-detected X-ray absorption spectroscopy (XAS) at the Advanced Light Source synchrotron. Soft X-ray absorption edges are preferred over traditional hard X-ray spectroscopy at the K-edges, since they have narrower natural linewidths and exhibit stronger chemical shifts. STJ detectors are preferred in the soft X-ray band over traditional Ge or grating spectrometers, since they have sufficient energy resolution to resolve transition metal L and M lines from light element K emission, and sufficient detection efficiency to measure the weak lines of dilute specimens within an acceptable time. We demonstrate the capabilities of our STJ spectrometer for chemical analysis with soft XAS measurements of molybdenum speciation on the Mo M{sub 4,5}-edges.

  10. Angle-resolved X-ray fluorescence spectrometry using synchrotron radiation at ELSA

    International Nuclear Information System (INIS)

    Schmitt, W.; Rothe, J.; Hormes, J.; Gries, W.H.

    1994-01-01

    Measurements on the centroid depth of ion-implanted phosphorus-in-silicon specimen by the method of angle-resolved, self-ratio X-ray fluorescence spectrometry (AR/SR/XFS) have been carried out using 'white' synchrotron radiation (SR). The measurements were performed using a modified wavelength-dispersive fluorescence spectrometer. Problems due to the use of SR, like carbonaceous specimen contamination and sample heating were overcome by flooding the specimen chamber with helium and by pre-absorbing the non-exciting parts of the incident SR with suitable filters, respectively. The decaying primary intensity was monitored by measuring the compensation current of the photoelectrons emitted from a tungsten wire stretched across the primary beam. Results have been obtained for specimen with dose density levels of 10 16 cm -2 and 3x10 15 cm -2 . (orig.)

  11. Experimental time resolved measurement of fluence and energy spectra of photons emitted by a pulsed X-ray generator in the range 5-300 keV

    International Nuclear Information System (INIS)

    Vie, M.; Baboulet, J.P.

    1989-01-01

    We have developed: - A sensor to measure locally X ray fluence rate amplitude and variation versus time during X ray pulses, - A spectrometer based on ROSS method to measure absolute X ray spectrum versus time during X ray pulses. This metrology is used to characterise single shot X ray pulsed sources emitting photons in the range of 5 to 300 keV. Fluence domain is between 10 -9 and 5 10 -4 J. cm -2 with a few nanoseconds time resolution [fr

  12. XRMON-GF: A novel facility for solidification of metallic alloys with in situ and time-resolved X-ray radiographic characterization in microgravity conditions

    Science.gov (United States)

    Nguyen-Thi, H.; Reinhart, G.; Salloum Abou Jaoude, G.; Mathiesen, R. H.; Zimmermann, G.; Houltz, Y.; Voss, D.; Verga, A.; Browne, D. J.; Murphy, A. G.

    2013-07-01

    As most of the phenomena involved during the growth of metallic alloys from the melt are dynamic, in situ and time-resolved X-ray imaging should be retained as the method of choice for investigating the solidification front evolution. On Earth, the gravity force is the major source of various disturbing effects (natural convection, buoyancy/sedimentation, and hydrostatic pressure) which can significantly modify or mask certain physical mechanisms. Therefore solidification under microgravity is an efficient way to eliminate such perturbations to provide unique benchmark data for the validation of models and numerical simulations. Up to now, in situ observation during microgravity solidification experiments were limited to the investigations on transparent organic alloys, using optical methods. On the other hand, in situ observation on metallic alloys generally required synchrotron facilities. This paper reports on a novel facility we have designed and developed to investigate directional solidification on metallic alloys in microgravity conditions with in situ X-ray radiography observation. The facility consists of a Bridgman furnace and an X-ray radiography device specifically devoted to the study of Al-based alloys. An unprecedented experiment was recently performed on board a sounding rocket, with a 6 min period of microgravity. Radiographs were successfully recorded during the entire experiment including the melting and solidification phases of the sample, with a Field-of-View of about 5 mm×5 mm, a spatial resolution of about 4 µm and a frequency of 2 frames per second. Some preliminary results are presented on the solidification of the Al-20 wt% Cu sample, which validate the apparatus and confirm the potential of in situ X-ray characterization for the investigation of dynamical phenomena in materials processing, and particularly for the studying of metallic alloys solidification.

  13. 1-(2-furoyl)-3,3-(diphenyl)thiourea: spectroscopic characterization and structural study from X-ray powder diffraction using simulated annealing

    Energy Technology Data Exchange (ETDEWEB)

    Estevez H, O.; Duque, J. [Universidad de La Habana, Instituto de Ciencia y Tecnologia de Materiales, 10400 La Habana (Cuba); Rodriguez H, J. [UNAM, Instituto de Investigaciones en Materiales, 04510 Mexico D. F. (Mexico); Yee M, H., E-mail: oestevezh@yahoo.com [Instituto Politecnico Nacional, Escuela Superior de Fisica y Matematicas, 07738 Mexico D. F. (Mexico)

    2015-07-01

    1-Furoyl-3,3-diphenylthiourea (FDFT) was synthesized, and characterized by Ftir, {sup 1}H and {sup 13}C NMR and ab initio X-ray powder structure analysis. FDFT crystallizes in the monoclinic space group P2{sub 1} with a = 12.691(1), b = 6.026(2), c = 11.861(1) A, β = 117.95(2) and V = 801.5(3) A{sup 3}. The crystal structure has been determined from laboratory X-ray powder diffraction data using direct space global optimization strategy (simulated annealing) followed by the Rietveld refinement. The thiourea group makes a dihedral angle of 73.8(6) with the furoyl group. In the crystal structure, molecules are linked by van der Waals interactions, forming one-dimensional chains along the a axis. (Author)

  14. Optoelectronic Picosecond Detection of Synchrotron X-rays

    Energy Technology Data Exchange (ETDEWEB)

    Durbin, Stephen M. [Purdue Univ., West Lafayette, IN (United States)

    2017-08-04

    The goal of this research program was to develop a detector that would measure x-ray time profiles with picosecond resolution. This was specifically aimed for use at x-ray synchrotrons, where x-ray pulse profiles have Gaussian time spreads of 50-100 ps (FWHM), so the successful development of such a detector with picosecond resolution would permit x-ray synchrotron studies to break through the pulse width barrier. That is, synchrotron time-resolved studies are currently limited to pump-probe studies that cannot reveal dynamics faster than ~50 ps, whereas the proposed detector would push this into the physically important 1 ps domain. The results of this research effort, described in detail below, are twofold: 1) the original plan to rely on converting electronic signals from a semiconductor sensor into an optical signal proved to be insufficient for generating signals with the necessary time resolution and sensitivity to be widely applicable; and 2) an all-optical method was discovered whereby the x-rays are directly absorbed in an optoelectronic material, lithium tantalate, which can then be probed by laser pulses with the desired picosecond sensitivity for detection of synchrotron x-rays. This research program has also produced new fundamental understanding of the interaction of x-rays and optical lasers in materials that has now created a viable path for true picosecond detection of synchrotron x-rays.

  15. The equation of state of PbTiO sub 3 up to 37 GPa: a synchrotron x-ray powder diffraction study

    CERN Document Server

    Sani, A; Levy, D

    2002-01-01

    High-pressure synchrotron x-ray powder diffraction patterns were collected using ID09 of ESRF (Grenoble, France) for a powder sample of PbTiO sub 3 , placed in a diamond anvil cell. The patterns were collected at room temperature using nitrogen (up to 37 GPa) and methanol-ethanol solution (up to 7 GPa) as pressure-transmitting media. The bulk moduli were calculated for the first time using the Vinet equation of state and they were compared to those of isostructural compounds. The trend of the spontaneous polarization as a function of pressure confirms that the ferroelectric-paraelectric phase transition at 11.2 GPa possesses a second-order character.

  16. Long time scale hard X-ray variability in Seyfert 1 galaxies

    Science.gov (United States)

    Markowitz, Alex Gary

    This dissertation examines the relationship between long-term X-ray variability characteristics, black hole mass, and luminosity of Seyfert 1 Active Galactic Nuclei. High dynamic range power spectral density functions (PSDs) have been constructed for six Seyfert 1 galaxies. These PSDs show "breaks" or characteristic time scales, typically on the order of a few days. There is resemblance to PSDs of lower-mass Galactic X-ray binaries (XRBs), with the ratios of putative black hole masses and variability time scales approximately the same (106--7) between the two classes of objects. The data are consistent with a linear correlation between Seyfert PSD break time scale and black hole mass estimate; the relation extrapolates reasonably well over 6--7 orders of magnitude to XRBs. All of this strengthens the case for a physical similarity between Seyfert galaxies and XRBs. The first six years of RXTE monitoring of Seyfert 1s have been systematically analyzed to probe hard X-ray variability on multiple time scales in a total of 19 Seyfert is in an expansion of the survey of Markowitz & Edelson (2001). Correlations between variability amplitude, luminosity, and black hole mass are explored, the data support the model of PSD movement with black hole mass suggested by the PSD survey. All of the continuum variability results are consistent with relatively more massive black holes hosting larger X-ray emission regions, resulting in 'slower' observed variability. Nearly all sources in the sample exhibit stronger variability towards softer energies, consistent with softening as they brighten. Direct time-resolved spectral fitting has been performed on continuous RXTE monitoring of seven Seyfert is to study long-term spectral variability and Fe Kalpha variability characteristics. The Fe Kalpha line displays a wide range of behavior but varies less strongly than the broadband continuum. Overall, however, there is no strong evidence for correlated variability between the line and

  17. High Brightness, Laser-Driven X-ray Source for Nanoscale Metrology and Femtosecond Dynamics

    Energy Technology Data Exchange (ETDEWEB)

    Siders, C W; Crane, J K; Semenov, V; Betts, S; Kozioziemski, B; Wharton, K; Wilks, S; Barbee, T; Stuart, B; Kim, D E; An, J; Barty, C

    2007-02-26

    This project developed and demonstrated a new, bright, ultrafast x-ray source based upon laser-driven K-alpha generation, which can produce an x-ray flux 10 to 100 times greater than current microfocus x-ray tubes. The short-pulse (sub-picosecond) duration of this x-ray source also makes it ideal for observing time-resolved dynamics of atomic motion in solids and thin films.

  18. Strain analysis of trabecular bone using time-resolved X-ray microtomography

    Czech Academy of Sciences Publication Activity Database

    Jiroušek, Ondřej; Zlámal, Petr; Kytýř, Daniel; Kroupa, M.

    2011-01-01

    Roč. 633, Suppl. 1 (2011), s. 148-151 ISSN 0168-9002. [International Workshop on Radiation Imaging Detectors /11./. Praha, 28.06.2009-02.07.2009] R&D Projects: GA ČR(CZ) GP103/07/P483 Institutional research plan: CEZ:AV0Z20710524 Keywords : trabecular bone * X-ray microtomography * strain analysis * intrinsic material properties Subject RIV: JB - Sensors, Measurment, Regulation Impact factor: 1.207, year: 2011

  19. Resolving the origin of the diffuse soft X-ray background

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Randall K.; Foster, Adam R.; Edgar, Richard J.; Brickhouse, Nancy S. [Harvard-Smithsonian Center for Astrophysics, 60 Garden Street, Cambridge MA 02138 (United States)

    2014-05-20

    The ubiquitous diffuse soft (1/4 keV) X-ray background was one of the earliest discoveries of X-ray astronomy. At least some of the emission may arise from charge exchange between solar wind ions and neutral atoms in the heliosphere, but no detailed models have been fit to the available data. Here, we report on a new model for charge exchange in the solar wind, which, when combined with a diffuse hot plasma component, filling the Local Cavity provides a good fit to the only available high-resolution soft X-ray and extreme ultraviolet spectra using plausible parameters for the solar wind. The implied hot plasma component is in pressure equilibrium with the local cloud that surrounds the solar system, creating for the first time a self-consistent picture of the local interstellar medium.

  20. X-ray vision of fuel sprays

    International Nuclear Information System (INIS)

    Wang, J.

    2005-01-01

    With brilliant synchrotron X-ray sources, microsecond time-resolved synchrotron X-ray radiography and tomography have been used to elucidate the detailed three-dimensional structure and dynamics of high-pressure high-speed fuel sprays in the near-nozzle region. The measurement allows quantitative determination of the fuel distribution in the optically impenetrable region owing to the multiple scattering of visible light by small atomized fuel droplets surrounding the jet. X-radiographs of the jet-induced shock waves prove that the fuel jets become supersonic under appropriate injection conditions and that the quantitative analysis of the thermodynamic properties of the shock waves can also be derived from the most direct measurement. In other situations where extremely axial-asymmetric sprays are encountered, mass deconvolution and cross-sectional fuel distribution models can be computed based on the monochromatic and time-resolved X-radiographic images collected from various rotational orientations of the sprays. Such quantitative analysis reveals the never-before-reported characteristics and most detailed near-nozzle mass distribution of highly transient fuel sprays

  1. Thermal expansion and phase transformation studies on some materials by high temperature x-ray powder diffractometry

    International Nuclear Information System (INIS)

    Rajagopalan, S.; Kutty, K.V.G.; Jajoo, H.K.; Ananthakrishnan, S.K.; Asurvatharaman, R.

    1988-01-01

    A high temperature chamber based on electrical resistance heating has been integrated to an existing x-ray powder diffractometer. The system is capable of going upto 2500degC at programmed rates of heating. Temperature measurement is carried out by means by Pt/Rh or W/Re thermocouples or by optical pyrometry depending upon the temperature range. Provision exists for performing high temperature x-ray diffractometry in vacuum or in a gaseous atmosphere of low x-ray absorption. The x-ray optical alignment has been ensured by accurately measuring the unit cell lengths of x-ray diffraction standards like silicon and tungsten. The thermocouples have been calibrated within the system by monitoring the melting points of gold and silver. The well characterized transformation of zirconia from the monoclinic to tetragonal structure occuring around 1100degC has been satisfactorily reproduced . The high temperature phase transitions in some rare earth oxides have been studi ed. lattice parameter measurements on a variety of materials as a function of temperature upto 1500degC have been carried out and the data found to be in agreement with the literature values. From the measured lattice parameter values, percentage thermal expansion and coefficients of thermal expansion have been calculated for many substances from room temperature to 15000degC. (author). 20 refs., 9 figs

  2. Time-resolved PHERMEX image restorations constrained with an additional multiply-exposed image

    International Nuclear Information System (INIS)

    Kruger, R.P.; Breedlove, J.R. Jr.; Trussell, H.J.

    1978-06-01

    There are a number of possible industrial and scientific applications of nanosecond cineradiographs. Although the technology exists to produce closely spaced pulses of x rays for this application, the quality of the time-resolved radiographs is severely limited. The limitations arise from the necessity of using a fluorescent screen to convert the transmitted x rays to light and then using electro-optical imaging systems to gate and to record the images with conventional high-speed cameras. It has been proposed that, in addition to the time-resolved images, a conventional multiply exposed radiograph be obtained. This report uses both PHERMEX and conventional photographic simulations to demonstrate that the additional information supplied by the multiply exposed radiograph can be used to improve the quality of digital image restorations of the time-resolved pictures over what could be achieved with the degraded images alone

  3. In situ X-ray powder diffraction, synthesis, and magnetic properties of InVO 3

    Science.gov (United States)

    Lundgren, Rylan J.; Cranswick, Lachlan M. D.; Bieringer, Mario

    2006-12-01

    We report the first synthesis and high-temperature in situ X-ray diffraction study of InVO 3. Polycrystalline InVO 3 has been prepared via reduction of InVO 4 using a carbon monoxide/carbon dioxide buffer gas. InVO 3 crystallizes in the bixbyite structure in space group Ia-3 (206) with a=9.80636(31) Å with In 3+/V 3+ disorder on the (8 b) and (24 d) cation sites. In situ powder X-ray diffraction experiments and thermal gravimetric analysis in a CO/CO 2 buffer gas revealed the existence of the metastable phase InVO 3. Bulk samples with 98.5(2)% purity were prepared using low-temperature reduction methods. The preparative methods limited the crystallinity of this new phase to approximately 225(50) Å. Magnetic susceptibility and neutron diffraction experiments suggest a spin-glass ground state for InVO 3.

  4. Characterization of Beryllium Windows for Coherent X-ray Optics

    International Nuclear Information System (INIS)

    Goto, Shunji; Yabashi, Makina; Tamasaku, Kenji; Ishikawa, Tetsuya

    2007-01-01

    Beryllium foils fabricated by several processes were characterized using spatially coherent x rays at 1-km beamline of SPring-8. By thickness dependence of bright x-ray spot density due to Fresnel diffraction from several-micron deficiencies, we found that speckles (bright x-ray spots) were due to voids with densities 103-104 mm-3 in powder foils and ingot foils. Compared with powder and ingot foils, a polished physical-vapor-deposited (PVD) beryllium foil gave highly uniform beams with no speckles. The PVD process eliminates the internal voids in principle and the PVD foil is the best for coherent x-ray applications

  5. Real-time digital x-ray subtraction imaging

    International Nuclear Information System (INIS)

    Mistretta, C.A.; Kruger, R.A.; Houk, T.L.

    1982-01-01

    A method of producing visible difference images derived from an x-ray image of an anatomical subject is described. X-rays are directed through the subject, and the image is converted into television fields comprising trains of analog video signals. The analog signals are converted into digital signals, which are then integrated over a predetermined time corresponding to several television fields. Difference video signals are produced by performing a subtraction between the ongoing video signals and the corresponding integrated signals, and are converted into visible television difference images representing changes in the x-ray image

  6. Scientific Challenges for a New X-ray Timing Mission

    International Nuclear Information System (INIS)

    Lamb, Frederick K.

    2004-01-01

    The Rossi X-ray Timing Explorer (RXTE) is an immensely successful mission of exploration and discovery. It has discovered a wealth of rapid X-ray variability phenomena that can be used to address fundamental questions concerning the properties of dense matter and strong gravitational fields as well as important astrophysical questions. It has answered many questions and is likely to answer many more, but to follow up fully on the major discoveries RXTE has made will require a new X-ray timing mission with greater capabilities. This introduction to the present volume describes briefly the advantages of X-ray timing measurements for determining the properties of dense matter and strong gravitational fields, indicates some of the key scientific questions that can be addressed using X-ray timing, and summarizes selected achievements of the RXTE mission. It concludes by citing some of the scientific capabilities a proposed follow-on mission will need in order to be successful

  7. The complex ion structure of warm dense carbon measured by spectrally resolved x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Kraus, D.; Barbrel, B.; Falcone, R. W. [Department of Physics, University of California, Berkeley, California 94720 (United States); Vorberger, J. [Max-Planck-Institut für Physik komplexer Systeme, Nöthnitzer Straße 38, 01187 Dresden (Germany); Helfrich, J.; Frydrych, S.; Ortner, A.; Otten, A.; Roth, F.; Schaumann, G.; Schumacher, D.; Siegenthaler, K.; Wagner, F.; Roth, M. [Institut für Kernphysik, Technische Universität Darmstadt, Schlossgartenstraße 9, 64289 Darmstadt (Germany); Gericke, D. O.; Wünsch, K. [Centre for Fusion, Space and Astrophysics, Department of Physics, University of Warwick, Coventry CV4 7AL (United Kingdom); Bachmann, B.; Döppner, T. [Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Bagnoud, V.; Blažević, A. [GSI Helmholtzzentrum für Schwerionenforschung GmbH, Planckstraße 1, 64291 Darmstadt (Germany); and others

    2015-05-15

    We present measurements of the complex ion structure of warm dense carbon close to the melting line at pressures around 100 GPa. High-pressure samples were created by laser-driven shock compression of graphite and probed by intense laser-generated x-ray sources with photon energies of 4.75 keV and 4.95 keV. High-efficiency crystal spectrometers allow for spectrally resolving the scattered radiation. Comparing the ratio of elastically and inelastically scattered radiation, we find evidence for a complex bonded liquid that is predicted by ab-initio quantum simulations showing the influence of chemical bonds under these conditions. Using graphite samples of different initial densities we demonstrate the capability of spectrally resolved x-ray scattering to monitor the carbon solid-liquid transition at relatively constant pressure of 150 GPa. Showing first single-pulse scattering spectra from cold graphite of unprecedented quality recorded at the Linac Coherent Light Source, we demonstrate the outstanding possibilities for future high-precision measurements at 4th Generation Light Sources.

  8. Sixa-silicon x-ray array

    International Nuclear Information System (INIS)

    Taylor, I.

    1995-01-01

    Full text: The Spectrum-X-Gamma (SRG) satellite is scheduled for launch in 1995-96. Mission objectives include broad and narrow band imaging spectroscopy over a wide range of energies from the EUV through hard X-rays with an emphasis on studying galactic and extragalactic X-ray sources. Timing and moderate resolution spectroscopy can be performed with the solid state spectrometer SIXA (Silicon X-Ray Array), placed on the focal plane of the SODART telescope with total effective area of 1150 cm 2 at 6 keV (for f = 8 in telescope). The detector consists of 19 circular Si(Li) pixels, each with an active diameter of 9.2 min and thickness of 3 min. A radiative cooler will be used to bring the detector to the proper operating temperature (120-130 K). The energy range 0.5-20 keV is divided into 1024 channels of 20 eV size. Photons can be recorded with 30 μs time resolution and 160-200 eV (1-7 keV) energy resolution. Potential observing programmes (for e.g. time-resolved Iron Kα line spectroscopy) include stellar coronae, cataclysmic variables and X-ray binaries; accretion discs and coronae of neutron stars and black hole candidates; supernova remnants, active galactic nuclei and clusters of galaxies. (author)

  9. Development of x-ray computed tomographic scanner for iron and steel

    International Nuclear Information System (INIS)

    Taguchi, Isamu; Nakamura, Shigeo.

    1985-01-01

    X-ray computed tomography is extensively used in medicine, but has rarely been applied to non-medical purposes. Steel specimens pose particularly difficult problems-very poor transmission of X-rays and the need for high resolving capability. There has thus been no effective tomographic method of examining steel specimens. Due to the growing need for non-destructive, non-contact methods for observing and analyzing the internal conditions of steel microscopically, however, we have developed an X-ray Computed Tomographic Scanner for Steel (CTS) system, specifically for examination of steel specimens. Its major specifications and functions are as follows. Type: the second-generation CT, 8-channels, Scanning method: 6 0 revolution, 30-times traversing, Slice width: 0.5 mm, Resolving capability: 0.25 x 0.25 mm, X-ray source: 420 kV, 3 mA, X-ray detector: BGO scintillator, Standard specimen shape: 50 mm dia., 100 mm high, Measuring time: 10.5 min. Porosity of a stainless steel (SUS 304) bloom was examined three-dimensionally by the CTS system. Corrosion procedure of a steel slab was also examined. (author)

  10. The Mapping X-ray Fluorescence Spectrometer (MapX)

    Science.gov (United States)

    Sarrazin, P.; Blake, D. F.; Marchis, F.; Bristow, T.; Thompson, K.

    2017-12-01

    Many planetary surface processes leave traces of their actions as features in the size range 10s to 100s of microns. The Mapping X-ray Fluorescence Spectrometer (MapX) will provide elemental imaging at 100 micron spatial resolution, yielding elemental chemistry at a scale where many relict physical, chemical, or biological features can be imaged and interpreted in ancient rocks on planetary bodies and planetesimals. MapX is an arm-based instrument positioned on a rock or regolith with touch sensors. During an analysis, an X-ray source (tube or radioisotope) bombards the sample with X-rays or alpha-particles / gamma-rays, resulting in sample X-ray Fluorescence (XRF). X-rays emitted in the direction of an X-ray sensitive CCD imager pass through a 1:1 focusing lens (X-ray micro-pore Optic (MPO)) that projects a spatially resolved image of the X-rays onto the CCD. The CCD is operated in single photon counting mode so that the energies and positions of individual X-ray photons are recorded. In a single analysis, several thousand frames are both stored and processed in real-time. Higher level data products include single-element maps with a lateral spatial resolution of 100 microns and quantitative XRF spectra from ground- or instrument- selected Regions of Interest (ROI). XRF spectra from ROI are compared with known rock and mineral compositions to extrapolate the data to rock types and putative mineralogies. When applied to airless bodies and implemented with an appropriate radioisotope source for alpha-particle excitation, MapX will be able to analyze biogenic elements C, N, O, P, S, in addition to the cations of the rock-forming elements >Na, accessible with either X-ray or gamma-ray excitation. The MapX concept has been demonstrated with a series of lab-based prototypes and is currently under refinement and TRL maturation.

  11. Real-time digital x-ray subtraction imaging

    International Nuclear Information System (INIS)

    Mistretta, C.A.

    1982-01-01

    The invention provides a method of producing visible difference images derived from an X-ray image of an anatomical subject, comprising the steps of directing X-rays through the anatomical subject for producing an image, converting the image into television fields comprising trains of on-going video signals, digitally storing and integrating the on-going video signals over a time interval corresponding to several successive television fields and thereby producing stored and integrated video signals, recovering the video signals from storage and producing integrated video signals, producing video difference signals by performing a subtraction between the integrated video signals and the on-going video signals outside the time interval, and converting the difference signals into visible television difference images representing on-going changes in the X-ray image

  12. Time-Resolved WAXD and SAXS Investigations on Butyl Branched Alkane at Elevated Pressures

    NARCIS (Netherlands)

    Rastogi, A.; Hobbs, J.K.; Rastogi, S.

    2002-01-01

    The crystallization behavior and the morphological aspect of the butyl branched alkane C96H193CH(C4H9)C94H189 have been investigated using time-resolved wide-angle X-ray diffraction (WAXD) and small-angle X-ray scattering (SAXS) at atmospheric and elevated pressures. The solution crystallized sample

  13. Introducing the ARL X'Tra x-ray diffraction system

    International Nuclear Information System (INIS)

    Harris, L.

    2002-01-01

    Full text: The ARL X'Tra is a state-of-the-art solution for powder X-ray diffraction in a large range of applications such as pharmaceuticals and biosciences, chemicals, earth sciences, semi-conductors, metallurgy and ceramics. The X'Tra offers the latest technology in key diffraction components to produce a high performance instrument at an affordable price. This presentation examines some of the hardware and performance features of this instrument. Copyright (2002) Australian X-ray Analytical Association Inc

  14. Absolute determination by X-ray diffraction of a binary or ternary mixture: nickel oxide and fluoride in a nickel powder (1960)

    International Nuclear Information System (INIS)

    Charpin, P.; Hauptman, A.

    1960-01-01

    The method employed is based upon the comparison between computed and measured intensities for conveniently selected X-Ray diffraction lines of each component of the powder. Care must be taken to allow for absorption, both inside each grain and in overall sample. This method has been applied to the determination of nickel oxide and fluoride in a nickel powder. (author) [fr

  15. XIPE, the X-ray imaging polarimetry explorer: Opening a new window in the X-ray sky

    Science.gov (United States)

    Soffitta, Paolo; XIPE Collaboration

    2017-11-01

    XIPE, the X-ray Imaging Polarimetry Explorer, is a candidate ESA fourth medium size mission, now in competitive phase A, aimed at time-spectrally-spatially-resolved X-ray polarimetry of a large number of celestial sources as a breakthrough in high energy astrophysics and fundamental physics. Its payload consists of three X-ray optics with a total effective area larger than one XMM mirror but with a low mass and of three Gas Pixel Detectors at their focus. The focal length is 4 m and the whole satellite fits within the fairing of the Vega launcher without the need of an extendable bench. XIPE will be an observatory with 75% of the time devoted to a competitive guest observer program. Its consortium across Europe comprises Italy, Germany, Spain, United Kingdom, Switzerland, Poland, Sweden Until today, thanks to a dedicated experiment that dates back to the '70, only the Crab Nebula showed a non-zero polarization with large significance [1] in X-rays. XIPE, with its innovative detector, promises to make significative measurements on hundreds of celestial sources.

  16. Settling time of dental x-ray tube head after positioning

    International Nuclear Information System (INIS)

    Yun, Suk Ja; Kang, Byung Cheol; Wang, Se Myung; Koh, Chang Sung

    2002-01-01

    The aim of this study was to introduce a method of obtaining the oscillation graphs of the dental x-ray tube heads relative to time using an accelerometer. An Accelerometer, Piezotron type 8704B25 (Kistler Instrument Co., Amherst, NY, USA) was utilized to measure the horizontal oscillation of the x-ray tube head immediately after positioning the tube head for an intraoral radiograph. The signal from the sensor was transferred to a dynamic signal analyzer, which displayed the magnitude of the acceleration on the Y-axis and time lapse on the X-axis. The horizontal oscillation of the tube head was measured relative to time, and the settling time was also determined on the basis of the acceleration graphs for 6 wall type, 5 floor-fixed type, and 4 mobile type dental x-ray machines. The oscillation graphs showed that tube head movement decreased rapidly over time. The settling time varied with x-ray machine types. Wall-type x-ray machines had a settling time of up to 6 seconds, 5 seconds for fixed floor-types, and 11 seconds for the mobile-types. Using an accelerometer, we obtained the oscillation graphs of the dental x-ray tube head relative to time. The oscillation graph with time can guide the operator to decide upon the optimum exposure moment after xray tube head positioning for better radiographic resolution.

  17. Settling time of dental x-ray tube head after positioning

    Energy Technology Data Exchange (ETDEWEB)

    Yun, Suk Ja; Kang, Byung Cheol [Department of Oral and Maxillofacial Radiology, Chonnam National University, Gwangju (Korea, Republic of); Wang, Se Myung; Koh, Chang Sung [Department of Mechatronics, Kwangju Institute of Science and Technology, Gwangju (Korea, Republic of)

    2002-09-15

    The aim of this study was to introduce a method of obtaining the oscillation graphs of the dental x-ray tube heads relative to time using an accelerometer. An Accelerometer, Piezotron type 8704B25 (Kistler Instrument Co., Amherst, NY, USA) was utilized to measure the horizontal oscillation of the x-ray tube head immediately after positioning the tube head for an intraoral radiograph. The signal from the sensor was transferred to a dynamic signal analyzer, which displayed the magnitude of the acceleration on the Y-axis and time lapse on the X-axis. The horizontal oscillation of the tube head was measured relative to time, and the settling time was also determined on the basis of the acceleration graphs for 6 wall type, 5 floor-fixed type, and 4 mobile type dental x-ray machines. The oscillation graphs showed that tube head movement decreased rapidly over time. The settling time varied with x-ray machine types. Wall-type x-ray machines had a settling time of up to 6 seconds, 5 seconds for fixed floor-types, and 11 seconds for the mobile-types. Using an accelerometer, we obtained the oscillation graphs of the dental x-ray tube head relative to time. The oscillation graph with time can guide the operator to decide upon the optimum exposure moment after xray tube head positioning for better radiographic resolution.

  18. Hard alpha-keratin degradation inside a tissue under high flux X-ray synchrotron micro-beam: a multi-scale time-resolved study.

    Science.gov (United States)

    Leccia, Emilie; Gourrier, Aurélien; Doucet, Jean; Briki, Fatma

    2010-04-01

    X-rays interact strongly with biological organisms. Synchrotron radiation sources deliver very intense X-ray photon fluxes within micro- or submicro cross-section beams, resulting in doses larger than the MGy. The relevance of synchrotron radiation analyses of biological materials is therefore questionable since such doses, million times higher than the ones used in radiotherapy, can cause huge damages in tissues, with regard to not only DNA, but also proteic and lipid organizations. Very few data concerning the effect of very high X-ray doses in tissues are available in the literature. We present here an analysis of the structural phenomena which occur when the model tissue of human hair is irradiated by a synchrotron X-ray micro-beam. The choice of hair is supported by its hierarchical and partially ordered keratin structure which can be analysed inside the tissue by X-ray diffraction. To assess the damages caused by hard X-ray micro-beams (1 microm(2) cross-section), short exposure time scattering SAXS/WAXS patterns have been recorded at beamline ID13 (ESRF) after various irradiation times. Various modifications of the scattering patterns are observed, they provide fine insight of the radiation damages at various hierarchical levels and also unexpectedly provide information about the stability of the various hierarchical structural levels. It appears that the molecular level, i.e. the alpha helices which are stabilized by hydrogen bonds and the alpha-helical coiled coils which are stabilized by hydrophobic interactions, is more sensitive to radiation than the supramolecular architecture of the keratin filament and the filament packing within the keratin associated proteins matrix, which is stabilized by disulphide bonds. (c) 2009 Elsevier Inc. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2014-01-01

    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 Pr 0.67 Sr 0.33 MnO 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

  20. Time-resolved crystallography using the Hadamard Transform

    Science.gov (United States)

    Yorke, Briony A.; Beddard, Godfrey S.; Owen, Robin L.; Pearson, Arwen R.

    2014-01-01

    A new method for performing time-resolved X-ray crystallographic experiments based on the Hadamard Transform is proposed and demonstrated. The time-resolution is defined by the underlying periodicity of the probe pulse sequence and the signal to noise is greatly improved compared to the fastest experiments depending on a single pulse. This approach is general and equally applicable to any spectroscopic or imaging measurement where the probe can be encoded. PMID:25282611

  1. Application of powder X-ray diffraction in studying the compaction behavior of bulk pharmaceutical powders.

    Science.gov (United States)

    Bandyopadhyay, Rebanta; Selbo, Jon; Amidon, Gregory E; Hawley, Michael

    2005-11-01

    This study investigates the effects of crystal lattice deformation on the powder X-ray diffraction (PXRD) patterns of compressed polycrystalline specimen (compacts/tablets) made from molecular, crystalline powders. The displacement of molecules and the corresponding adjustment of interplanar distances (d-spacings) between diffracting planes of PNU-288034 and PNU-177553, which have crystal habits with a high aspect ratio favoring preferred orientation during tableting, are demonstrated by shifts in the diffracted peak positions. The direction of shift in diffracted peak positions suggests a reduction of interplanar d-spacing in the crystals of PNU-288034 and PNU-177553 following compaction. There is also a general reduction of peak intensities following compression at the different compressive loads. The lattice strain representing the reduction in d-spacing is proportional to the original d-spacing of the uncompressed sample suggesting that, as with systems that obey a simple Hooke's law relationship, the further apart the planes of atoms/molecules within the lattice are, the easier it is for them to approach each other under compressive stresses. For a third model compound comprising more equant-shaped crystals of PNU-141659, the shift in diffracted peak positions are consistent with an expansion of lattice spacing after compression. This apparent anomaly is supported by the PXRD studies of the bulk powder consisting of fractured crystals where also, the shift in peak position suggests expansion of the lattice planes. Thus the crystals of PNU-141659 may be fracturing under the compressive loads used to produce the compacts. Additional studies are underway to relate the PXRD observations with the bulk tableting properties of these model compounds.

  2. X-Ray Timing Analysis of Cyg X-3 Using AstroSat/LAXPC: Detection of Milli-hertz Quasi-periodic Oscillations during the Flaring Hard X-Ray State

    Energy Technology Data Exchange (ETDEWEB)

    Pahari, Mayukh; Misra, Ranjeev [Inter-University Center for Astronomy and Astrophysics, Ganeshkhind, Pune 411007 (India); Antia, H M; Yadav, J S; Chauhan, Jai Verdhan; Chitnis, V R; Dedhia, Dhiraj; Katoch, Tilak; Madhwani, P; Shah, Parag [Tata Institute of Fundamental Research, Homi Bhabha Road, Mumbai 400005 (India); Agrawal, P C [UM-DAE Center of Excellence for Basic Sciences, University of Mumbai, Kalina, Mumbai 400098 (India); Manchanda, R K [University of Mumbai, Kalina, Mumbai 400098 (India); Paul, B, E-mail: mayukh@iucaa.in [Department of Astronomy and Astrophysics, Raman Research Institute, Bengaluru 560080 (India)

    2017-11-01

    We present here results from the X-ray timing and spectral analysis of the X-ray binary Cyg X-3 using observations from the Large Area X-ray proportional Counter on board AstroSat . Consecutive light curves observed over a period of one year show the binary orbital period of 17253.56 ± 0.19 s. Another low-amplitude, slow periodicity of the order of 35.8 ± 1.4 days is observed, which may be due to the orbital precession as suggested earlier by Molteni et al. During the rising binary phase, power density spectra from different observations during the flaring hard X-ray state show quasi-periodic oscillations (QPOs) at ∼5–8 mHz, ∼12–14 mHz, and ∼18–24 mHz frequencies at the minimum confidence of 99%. However, during the consecutive binary decay phase, no QPO is detected up to 2 σ significance. Energy-dependent time-lag spectra show soft lag (soft photons lag hard photons) at the mHz QPO frequency and the fractional rms of the QPO increases with the photon energy. During the binary motion, the observation of mHz QPOs during the rising phase of the flaring hard state may be linked to the increase in the supply of the accreting material in the disk and corona via stellar wind from the companion star. During the decay phase, the compact source moves in the outer wind region causing the decrease in supply of material for accretion. This may cause weakening of the mHz QPOs below the detection limit. This is also consistent with the preliminary analysis of the orbital phase-resolved energy spectra presented in this paper.

  3. Mix and Inject: Reaction Initiation by Diffusion for Time-Resolved Macromolecular Crystallography

    Directory of Open Access Journals (Sweden)

    Marius Schmidt

    2013-01-01

    Full Text Available Time-resolved macromolecular crystallography unifies structure determination with chemical kinetics, since the structures of transient states and chemical and kinetic mechanisms can be determined simultaneously from the same data. To start a reaction in an enzyme, typically, an initially inactive substrate present in the crystal is activated. This has particular disadvantages that are circumvented when active substrate is directly provided by diffusion. However, then it is prohibitive to use macroscopic crystals because diffusion times become too long. With small micro- and nanocrystals diffusion times are adequately short for most enzymes and the reaction can be swiftly initiated. We demonstrate here that a time-resolved crystallographic experiment becomes feasible by mixing substrate with enzyme nanocrystals which are subsequently injected into the X-ray beam of a pulsed X-ray source.

  4. X-ray diffraction identification of clay minerals by microcomputer

    International Nuclear Information System (INIS)

    Rodrigues, S.; Imasava, F.J.

    1988-01-01

    The identification of clay minerals by X-ray powder diffraction are done by searching an unknown pattern with a file of standard X-ray diffraction patterns. For this searching done by hand is necessary a long time. This paper shows a program in ''Basic'' language to be utilized in microcomputers for the math of the unknown pattern, using the high velocity of comparison of the microcomputer. A few minutes are used for the match. (author) [pt

  5. Long term variability of Cygnus X-1. VI. Energy-resolved X-ray variability 1999-2011

    NARCIS (Netherlands)

    Grinberg, V.; Pottschmidt, K.; Böck, M.; Schmid, C.; Nowak, M.A.; Uttley, P.; Tomsick, J.A.; Rodriguez, J.; Hell, N.; Markowitz, A.; Bodaghee, A.; Cadolle Bel, M.; Rothschild, R.E.; Wilms, J.

    2014-01-01

    We present the most extensive analysis of Fourier-based X-ray timing properties of the black hole binary Cygnus X-1 to date, based on 12 years of bi-weekly monitoring with RXTE from 1999 to 2011. Our aim is a comprehensive study of timing behavior across all spectral states, including the elusive

  6. Time-dependent nonequilibrium soft x-ray response during a spin crossover

    Energy Technology Data Exchange (ETDEWEB)

    van Veenendaal, Michel

    2018-03-01

    The rapid development of high-brilliance pulsed X-ray sources with femtosecond time resolution has created a need for a better theoretical understanding of the time-dependent soft-X-ray response of dissipative many-body quantum systems. It is demonstrated how soft-X-ray spectroscopies, such as X-ray absorption and resonant inelastic X-ray scattering at transition-metal L-edges, can provide insight into intersystem crossings, such as a spin crossover. The photoinduced doublet-to-quartet spin crossover on cobalt in Fe-Co Prussian blue analogues is used as an example to demonstrate how the X-ray response is affected by the dissipative nonequilibrium dynamics. The time-dependent soft-X-ray spectra provide a wealth of information that reflect the changes in the nonequilibrium initial state via continuously changing spectral lineshapes that cannot be decomposed into initial photoexcited and final metastable spectra, strong broadenings, a collapse of clear selection rules during the intersystem crossing, strong fluctuations in the isotropic branching ratio in X-ray absorption, and crystal-field collapse/oscillations and strongly time-dependent anti-Stokes processes in RIXS.

  7. CMOS-sensors for energy-resolved X-ray imaging

    International Nuclear Information System (INIS)

    Doering, D.; Amar-Youcef, S.; Deveaux, M.; Linnik, B.; Müntz, C.; Stroth, Joachim; Baudot, J.; Dulinski, W.; Kachel, M.

    2016-01-01

    Due to their low noise, CMOS Monolithic Active Pixel Sensors are suited to sense X-rays with a few keV quantum energy, which is of interest for high resolution X-ray imaging. Moreover, the good energy resolution of the silicon sensors might be used to measure this quantum energy. Combining both features with the good spatial resolution of CMOS sensors opens the potential to build ''color sensitive' X-ray cameras. Taking such colored images is hampered by the need to operate the CMOS sensors in a single photon counting mode, which restricts the photon flux capability of the sensors. More importantly, the charge sharing between the pixels smears the potentially good energy resolution of the sensors. Based on our experience with CMOS sensors for charged particle tracking, we studied techniques to overcome the latter by means of an offline processing of the data obtained from a CMOS sensor prototype. We found that the energy resolution of the pixels can be recovered at the expense of reduced quantum efficiency. We will introduce the results of our study and discuss the feasibility of taking colored X-ray pictures with CMOS sensors

  8. Real-time digital X-ray subtraction imaging

    International Nuclear Information System (INIS)

    Mistretta, C.A.; Kruger, R.A.; Houk, T.L.

    1979-01-01

    A diagnostic anatomical X-ray apparatus comprising a converter and a television camera for converting an X-ray image of a subject into a series of television fields of video signals is described in detail. A digital memory system stores and integrates the video signals over a time interval corresponding to a plurality of successive television fields. The integrated video signals are recovered from storage and fed to a digital or analogue subtractor, the resulting output being displayed on a television monitor. Thus the display represents on-going changes in the anatomical X-ray image. In a modification, successive groups of fields are stored and integrated in three memories, cyclically, and subtractions are performed between successive pieces of integrated signals to provide a display of successive alterations in the X-ray image. For investigations of the heart, the integrating interval should be of the order of one cardiac cycle. (author)

  9. Quantum effets in nonresonant X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Slowik, Jan Malte

    2015-11-15

    Due to their versatile properties, X rays are a unique tool to investigate the structure and dynamics of matter. X-ray scattering is the fundamental principle of many imaging techniques. Examples are X-ray crystallography, which recently celebrated one hundred years and is currently the leading method in structure determination of proteins, as well as X-ray phase contrast imaging (PCI), which is an imaging technique with countless applications in biology, medicine, etc. The technological development of X-ray free electron lasers (XFEL) has brought X-ray imaging at the edge of a new scientific revolution. XFELs offer ultrashort X-ray pulses with unprecedented high X-ray fluence and excellent spatial coherence properties. These properties make them an outstanding radiation source for X-ray scattering experiments, providing ultrafast temporal resolution as well as atomic spatial resolution. However, the radiation-matter interaction in XFEL experiments also advances into a novel regime. This demands a sound theoretical fundament to describe and explore the new experimental possibilities. This dissertation is dedicated to the theoretical study of nonresonant X-ray scattering. As the first topic, I consider the near-field imaging by propagation based X-ray phase contrast imaging (PCI). I devise a novel theory of PCI, in which radiation and matter are quantized. Remarkably, the crucial interference term automatically excludes contributions from inelastic scattering. This explains the success of the classical description thus far. The second topic of the thesis is the X-ray imaging of coherent electronic motion, where quantum effects become particularly apparent. The electron density of coherent electronic wave packets - important in charge transfer and bond breaking - varies in time, typically on femto- or attosecond time scales. In the near future, XFELs are envisaged to provide attosecond X-ray pulses, opening the possibility for time-resolved ultrafast X-ray scattering

  10. Quantum effets in nonresonant X-ray scattering

    International Nuclear Information System (INIS)

    Slowik, Jan Malte

    2015-11-01

    Due to their versatile properties, X rays are a unique tool to investigate the structure and dynamics of matter. X-ray scattering is the fundamental principle of many imaging techniques. Examples are X-ray crystallography, which recently celebrated one hundred years and is currently the leading method in structure determination of proteins, as well as X-ray phase contrast imaging (PCI), which is an imaging technique with countless applications in biology, medicine, etc. The technological development of X-ray free electron lasers (XFEL) has brought X-ray imaging at the edge of a new scientific revolution. XFELs offer ultrashort X-ray pulses with unprecedented high X-ray fluence and excellent spatial coherence properties. These properties make them an outstanding radiation source for X-ray scattering experiments, providing ultrafast temporal resolution as well as atomic spatial resolution. However, the radiation-matter interaction in XFEL experiments also advances into a novel regime. This demands a sound theoretical fundament to describe and explore the new experimental possibilities. This dissertation is dedicated to the theoretical study of nonresonant X-ray scattering. As the first topic, I consider the near-field imaging by propagation based X-ray phase contrast imaging (PCI). I devise a novel theory of PCI, in which radiation and matter are quantized. Remarkably, the crucial interference term automatically excludes contributions from inelastic scattering. This explains the success of the classical description thus far. The second topic of the thesis is the X-ray imaging of coherent electronic motion, where quantum effects become particularly apparent. The electron density of coherent electronic wave packets - important in charge transfer and bond breaking - varies in time, typically on femto- or attosecond time scales. In the near future, XFELs are envisaged to provide attosecond X-ray pulses, opening the possibility for time-resolved ultrafast X-ray scattering

  11. High-speed x-ray imaging with the Keck pixel array detector (Keck PAD) for time-resolved experiments at synchrotron sources

    Energy Technology Data Exchange (ETDEWEB)

    Philipp, Hugh T., E-mail: htp2@cornell.edu; Tate, Mark W.; Purohit, Prafull; Shanks, Katherine S.; Weiss, Joel T. [Laboratory of Atomic and Solid State Physics, Cornell University, Ithaca, NY (United States); Chamberlain, Darol; Gruner, Sol M. [Laboratory of Atomic and Solid State Physics, Cornell University, Ithaca, NY (United States); Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, NY (United States)

    2016-07-27

    Modern storage rings are readily capable of providing intense x-ray pulses, tens of picoseconds in duration, millions of times per second. Exploiting the temporal structure of these x-ray sources opens avenues for studying rapid structural changes in materials. Many processes (e.g. crack propagation, deformation on impact, turbulence, etc.) differ in detail from one sample trial to the next and would benefit from the ability to record successive x-ray images with single x-ray sensitivity while framing at 5 to 10 MHz rates. To this end, we have pursued the development of fast x-ray imaging detectors capable of collecting bursts of images that enable the isolation of single synchrotron bunches and/or bunch trains. The detector technology used is the hybrid pixel array detector (PAD) with a charge integrating front-end, and high-speed, in-pixel signal storage elements. A 384×256 pixel version, the Keck-PAD, with 150 µm × 150 µm pixels and 8 dedicated in-pixel storage elements is operational, has been tested at CHESS, and has collected data for compression wave studies. An updated version with 27 dedicated storage capacitors and identical pixel size has been fabricated.

  12. A study of x-ray microbeam stress measurement for local area

    International Nuclear Information System (INIS)

    Natsume, Yoshitaka; Miyakawa, Susumu

    1987-01-01

    A new type X-ray microbeam equipment which is capable of three-dimensional oscillation at an X-ray radiation position was used to measure the residual stress of pure iron powder and bending plate specimens as well as that in the vicinity of fatigue crack tip of 1/2 CT specimen. The results obtained are summerized as follows. (1) Diffraction profiles of pure iron powder with diameter 0.02 ∼ 0.03 μm particle size obtained by the present microbeam technique in the beam area of 80 μm in diamether and measuring time more than 800 sec showed Kα 1 and Kα 2 peaks clearly, so that these profiles are good enough for stress measurement. (2) The measured stress of pure iron powder with diameter 10 ∼ 25 μm particle size in the beam area of 80 μm in diameter was not equal to 0 MPa. The measured stress varied greatly and was independent of measuring time. (3) The measured stress of pure iron powder with diameter 0.02 ∼ 0.03 μm particle size in the beam area of 80 μm in diameter was almost 1 MPa, which shows the good accuracy of this X-ray micro-beam equipment. (4) The relation between the X-ray measured stress and the mechanically applied stress showed good agreement. (5) The distribution of residual stress at the vicinity of fatigue crack tip showed that the residual stress at the fatigue crack tip was compression and the residual stress in front of crack tip was tension. This tensile residual stress in front of crack tip existed in the area from 0.02 mm to 2 mm. (6) The above results show that the present equipment is advantageous in the investigation of local stress, shortening the measuring time without sacrificing the accuracy. (author)

  13. Serial femtosecond X-ray diffraction of enveloped virus microcrystals

    Directory of Open Access Journals (Sweden)

    Robert M. Lawrence

    2015-07-01

    Full Text Available Serial femtosecond crystallography (SFX using X-ray free-electron lasers has produced high-resolution, room temperature, time-resolved protein structures. We report preliminary SFX of Sindbis virus, an enveloped icosahedral RNA virus with ∼700 Å diameter. Microcrystals delivered in viscous agarose medium diffracted to ∼40 Å resolution. Small-angle diffuse X-ray scattering overlaid Bragg peaks and analysis suggests this results from molecular transforms of individual particles. Viral proteins undergo structural changes during entry and infection, which could, in principle, be studied with SFX. This is an important step toward determining room temperature structures from virus microcrystals that may enable time-resolved studies of enveloped viruses.

  14. Time response characteristics of X-ray detector system on Silex-Ⅰ laser facility

    International Nuclear Information System (INIS)

    Yi Rongqing; He Xiao'an; Li Hang; Du Huabing; Zhang Haiying; Cao Zhurong

    2013-01-01

    On the Silex-Ⅰ laser facility, the time response characteristics of XRD detector were studied. A laser with a pulse of 32 fs and a wavelength of 800 nm was used to irradiate a plane Au target. X-ray calibrated method of time of exposure X-ray framing camera and time resolution of X-ray streak camera was explored. The time response characteristics of XRD detector and time process of X-ray emission were obtained from experiment. We obtained X-ray calibration method of time of exposure X-ray framing camera and time resolution of X-ray streak camera. (authors)

  15. The Athena X-ray Integral Field Unit (X-IFU)

    NARCIS (Netherlands)

    Barret, Didier; Lam Trong, Thien; den Herder, Jan-Willem; Piro, Luigi; Barcons, Xavier; Huovelin, Juhani; Kelley, Richard; Mas-Hesse, J. Miguel; Mitsuda, Kazuhisa; Paltani, Stéphane; Rauw, Gregor; RoŻanska, Agata; Wilms, Joern; Barbera, Marco; Bozzo, Enrico; Ceballos, Maria Teresa; Charles, Ivan; Decourchelle, Anne; den Hartog, Roland; Duval, Jean-Marc; Fiore, Fabrizio; Gatti, Flavio; Goldwurm, Andrea; Jackson, Brian; Jonker, Peter; Kilbourne, Caroline; Macculi, Claudio; Mendez, Mariano; Molendi, Silvano; Orleanski, Piotr; Pajot, François; Pointecouteau, Etienne; Porter, Frederick; Pratt, Gabriel W.; Prêle, Damien; Ravera, Laurent; Renotte, Etienne; Schaye, Joop; Shinozaki, Keisuke; Valenziano, Luca; Vink, Jacco; Webb, Natalie; Yamasaki, Noriko; Delcelier-Douchin, Françoise; Le Du, Michel; Mesnager, Jean-Michel; Pradines, Alice; Branduardi-Raymont, Graziella; Dadina, Mauro; Finoguenov, Alexis; Fukazawa, Yasushi; Janiuk, Agnieszka; Miller, Jon; Nazé, Yaël; Nicastro, Fabrizio; Sciortino, Salvatore; Torrejon, Jose Miguel; Geoffray, Hervé; Hernandez, Isabelle; Luno, Laure; Peille, Philippe; André, Jérôme; Daniel, Christophe; Etcheverry, Christophe; Gloaguen, Emilie; Hassin, Jérémie; Hervet, Gilles; Maussang, Irwin; Moueza, Jérôme; Paillet, Alexis; Vella, Bruno; Campos Garrido, Gonzalo; Damery, Jean-Charles; Panem, Chantal; Panh, Johan; Bandler, Simon; Biffi, Jean-Marc; Boyce, Kevin; Clénet, Antoine; DiPirro, Michael; Jamotton, Pierre; Lotti, Simone; Schwander, Denis; Smith, Stephen; van Leeuwen, Bert-Joost; van Weers, Henk; Brand, Thorsten; Cobo, Beatriz; Dauser, Thomas; de Plaa, Jelle; Cucchetti, Edoardo

    2016-01-01

    The X-ray Integral Field Unit (X-IFU) on board the Advanced Telescope for High-ENergy Astrophysics (Athena) will provide spatially resolved high-resolution X-ray spectroscopy from 0.2 to 12 keV, with 5" pixels over a field of view of 5 arc minute equivalent diameter and a spectral resolution of 2.5

  16. Aqueous Nucleation and Growth of Titanium Oxides Using Time-Resolved Synchrotron X- ray Diffraction

    Science.gov (United States)

    Hummer, D. R.; Heaney, P. J.; Post, J. E.

    2006-05-01

    The inorganic precipitation of oxide minerals in soil environments has profound effects on a variety of geochemical processes. These include the removal of metals from the aqueous phase, the production of coatings that reduce the reactive surface area of pre-existing mineral grains, and the generation of feedstocks for microbial metabolic reactions. Recent observations of transient, metastable phases during the growth of oxide crystallites has raised questions about their role in crystallization mechanisms, and created a need for more detailed structural measurements. To better understand the process of nucleation and growth, we investigated the crystallization of Ti oxides from aqueous 0.5 M TiCl4 solutions using synchrotron X-ray diffraction at temperatures of 100 and 150 °C. Solutions were heated in a 1.0 mm internal diameter quartz glass capillary sealed with epoxy. Powder diffraction patterns of the growing crystallites were collected using image plate technology with a time step of ~ 4 minutes, providing high resolution in situ measurements of structural changes during the crystallization process. The data indicate a co-precipitation of the two crystalline phases anatase and rutile within the first 30 minutes of heating, followed by a gradual phase transition from anatase to rutile during particle coarsening throughout the 10 hour duration of an experiment. The co-existence of anatase and rutile at the onset of crystallization lends additional support to the assertion of nearly identical free energies for anatase and rutile at the nanoscale, believed to be due to the prominence of surface energy effects (Ranade et al., 2001). Whole pattern analyses using the Rietveld refinement method also documented previously unobserved changes in lattice parameters of both phases during growth, on the order of 0.2-0.3 % expansion for each axis. The trends in lattice parameters are observed to be temperature dependent, generally having lower values at higher

  17. Imaging properties of cerium doped Yttrium Aluminum Oxide (YAP:Ce) powder scintillating screens under X-ray excitation

    Energy Technology Data Exchange (ETDEWEB)

    Kalivas, N. [Greek Atomic Energy Commission, 15310 Ag. Paraskevi, P.O. Box 60092 (Greece); Valais, I. [Department of Medical Physics, Medical School, University of Patras, 26500 Patras (Greece)]|[Department of Medical Instruments Technology, Technological Educational Institution of Athens, Ag. Spyridonos Street, Aigaleo, 12210 Athens (Greece); Salemis, G.; Karagiannis, C.; Konstantinidis, A.; Nikolopoulos, D. [Department of Medical Instruments Technology, Technological Educational Institution of Athens, Ag. Spyridonos Street, Aigaleo, 12210 Athens (Greece); Loudos, G.; Sakelios, N.; Karakatsanis, N.; Nikita, K. [Department of Electrical and Computer Engineering, National Technical University of Athens, 9 Iroon Polytechniou, 15780 Zografos (Greece); Gayshan, V.L.; Gektin, A.V. [Institute of Scintillation Materials, Lenin Avenue 60, 310072 Kharkov (Ukraine); Sianoudis, I. [Department of Physics, Chemistry and Materials Technology, Technological Educational Institution of Athens, Aigaleo, 12210 Athens (Greece); Giokaris, N. [Physics Department National Capodistrian University of Athens, Panepistimioupolis Ilisia, 15771 Athens (Greece)]|[Institute of Accelerating Systems and Applications, P.O. Box 17214, 10024 Athens (Greece); Nomicos, C.D. [Department of Electronics, Technological Educational Institution of Athens, Aigaleo, 12210 Athens (Greece); Dimitropoulos, N. [Department of Medical Imaging, ' Euromedica' Medical Center, Mesogeion 2-4, 11527 Athens (Greece); Cavouras, D. [Department of Medical Instruments Technology, Technological Educational Institution of Athens, Ag. Spyridonos Street, Aigaleo, 12210 Athens (Greece); Panayiotakis, G. [Department of Medical Physics, Medical School, University of Patras, 26500 Patras (Greece); Kandarakis, I. [Department of Medical Instruments Technology, Technological Educational Institution of Athens, Ag. Spyridonos Street, Aigaleo, 12210 Athens (Greece)]. E-mail: kandarakis@teiath.gr

    2006-12-20

    The aim of the present study was to evaluate the imaging performance of YAP:Ce powder scintillating screens under exposure conditions employed in diagnostic radiology (50-140 kV). Various screens were prepared in our laboratory from YAP: Ce powder (Phosphor Technology, Ltd.), with coating thickness ranging from 53 to 110 mg/cm{sup 2}. The imaging performance of the screens was assessed by experimental determination of the modulation transfer function (MTF) and the noise transfer function (NTF). MTF was determined by the edge spread function (ESF) method while NTF was estimated by noise power spectrum (NPS) measurements after uniform screen irradiation. In addition, parameters related to overall image quality, such as the signal-to-noise ratio transfer (MTF/NTF), were estimated. MTF curves were affected by the beam hardening effects caused by the patient simulating 20 mm thick aluminum phantom. Under these conditions MTF values were found to increase with the mean X-ray photon energy. A similar effect was observed for NTF curves. Results were compared with data obtained on CsI:Tl scintillator. Taking into consideration the very fast response of YAP:Ce, these data may be of interest in designing X-ray imaging detectors.

  18. Time-resolved x-ray spectra from laser-generated high-density plasmas

    Science.gov (United States)

    Andiel, U.; Eidmann, Klaus; Witte, Klaus-Juergen

    2001-04-01

    We focused frequency doubled ultra short laser pulses on solid C, F, Na and Al targets, K-shell emission was systematically investigated by time resolved spectroscopy using a sub-ps streak camera. A large number of laser shots can be accumulated when triggering the camera with an Auston switch system at very high temporal precision. The system provides an outstanding time resolution of 1.7ps accumulating thousands of laser shots. The time duration of the He-(alpha) K-shell resonance lines was observed in the range of (2-4)ps and shows a decrease with the atomic number. The experimental results are well reproduced by hydro code simulations post processed with an atomic kinetics code.

  19. First spin-resolved electron distributions in crystals from combined polarized neutron and X-ray diffraction experiments

    Directory of Open Access Journals (Sweden)

    Maxime Deutsch

    2014-05-01

    Full Text Available Since the 1980s it has been possible to probe crystallized matter, thanks to X-ray or neutron scattering techniques, to obtain an accurate charge density or spin distribution at the atomic scale. Despite the description of the same physical quantity (electron density and tremendous development of sources, detectors, data treatment software etc., these different techniques evolved separately with one model per experiment. However, a breakthrough was recently made by the development of a common model in order to combine information coming from all these different experiments. Here we report the first experimental determination of spin-resolved electron density obtained by a combined treatment of X-ray, neutron and polarized neutron diffraction data. These experimental spin up and spin down densities compare very well with density functional theory (DFT calculations and also confirm a theoretical prediction made in 1985 which claims that majority spin electrons should have a more contracted distribution around the nucleus than minority spin electrons. Topological analysis of the resulting experimental spin-resolved electron density is also briefly discussed.

  20. First spin-resolved electron distributions in crystals from combined polarized neutron and X-ray diffraction experiments.

    Science.gov (United States)

    Deutsch, Maxime; Gillon, Béatrice; Claiser, Nicolas; Gillet, Jean-Michel; Lecomte, Claude; Souhassou, Mohamed

    2014-05-01

    Since the 1980s it has been possible to probe crystallized matter, thanks to X-ray or neutron scattering techniques, to obtain an accurate charge density or spin distribution at the atomic scale. Despite the description of the same physical quantity (electron density) and tremendous development of sources, detectors, data treatment software etc., these different techniques evolved separately with one model per experiment. However, a breakthrough was recently made by the development of a common model in order to combine information coming from all these different experiments. Here we report the first experimental determination of spin-resolved electron density obtained by a combined treatment of X-ray, neutron and polarized neutron diffraction data. These experimental spin up and spin down densities compare very well with density functional theory (DFT) calculations and also confirm a theoretical prediction made in 1985 which claims that majority spin electrons should have a more contracted distribution around the nucleus than minority spin electrons. Topological analysis of the resulting experimental spin-resolved electron density is also briefly discussed.

  1. 100ps UV/x-ray framing camera

    International Nuclear Information System (INIS)

    Eagles, R.T.; Freeman, N.J.; Allison, J.M.; Sibbett, W.; Sleat, W.E.; Walker, D.R.

    1988-01-01

    The requirement for a sensitive two-dimensional imaging diagnostic with picosecond time resolution, particularly in the study of laser-produced plasmas, has previously been discussed. A temporal sequence of framed images would provide useful supplementary information to that provided by time resolved streak images across a spectral region of interest from visible to x-ray. To fulfill this requirement the Picoframe camera system has been developed. Results pertaining to the operation of a camera having S20 photocathode sensitivity are reviewed and the characteristics of an UV/x-ray sensitive version of the Picoframe system are presented

  2. An x-ray technique for precision laser beam synchronization

    International Nuclear Information System (INIS)

    Landen, O.L.; Lerche, R.A.; Hay, R.G.; Hammel, B.A.; Kalantar, D.; Cable, M.D.

    1994-01-01

    A new x-ray technique for recording the relative arrival times of multiple laser beams at a common target with better than ± 10 ps accuracy has been implemented at the Nova laser facility. 100 ps, 3ω Nova beam are focused to separate locations on a gold ribbon target viewed from the side. The measurement consists of using well characterized re-entrant x-ray streak cameras for 1-dimensional streaked imaging of the > 3 keV x-rays emanating from these isolated laser plasmas. After making the necessary correction for the differential laser, x-ray and electron transit times involved, timing offsets as low as ± 7 ps are resolved, and on subsequent shots, corrected for, verified and independently checked. This level of synchronization proved critical in meeting the power balance requirements for indirectly-driven pulse-shaped Nova implosions

  3. A comparison between the Structural Results obtained by X-ray Single Crystal Data and by Neutron Powder Data for BaVs/sb3/

    International Nuclear Information System (INIS)

    Marezio, M.

    1986-01-01

    The structure of BaVs/sb3/, as refined from X-ray single-crystal data to an R factor of 0.011, is compared to the structure of the same compound obtained from neutron powder data (Rsb(ro) = 6.82, Rsb(psilon) = 4.09). As expected, the X-ray standard deviations of the positional and thermal parameters are smaller than the corresponding neutron standard deviations. However, the dynamical disorder deduced from the anomalously large thermal vibrations of the vanadium atoms obtained from the X-ray data is also evidenced by the neutron refinement. On the other hand, the neutron standard deviations of the lattice parameters are smaller than the X-ray counterparts

  4. X-ray photoelectron spectroscopy (XPS) investigation of the surface film on magnesium powders.

    Science.gov (United States)

    Burke, Paul J; Bayindir, Zeynel; Kipouros, Georges J

    2012-05-01

    Magnesium (Mg) and its alloys are attractive for use in automotive and aerospace applications because of their low density and good mechanical properties. However, difficulty in forming magnesium and the limited number of available commercial alloys limit their use. Powder metallurgy may be a suitable solution for forming near-net-shape parts. However, sintering pure magnesium presents difficulties due to surface film that forms on the magnesium powder particles. The present work investigates the composition of the surface film that forms on the surface of pure magnesium powders exposed to atmospheric conditions and on pure magnesium powders after compaction under uniaxial pressing at a pressure of 500 MPa and sintering under argon at 600 °C for 40 minutes. Initially, focused ion beam microscopy was utilized to determine the thickness of the surface layer of the magnesium powder and found it to be ~10 nm. The X-ray photoelectron analysis of the green magnesium sample prior to sintering confirmed the presence of MgO, MgCO(3)·3H(2)O, and Mg(OH)(2) in the surface layer of the powder with a core of pure magnesium. The outer portion of the surface layer was found to contain MgCO(3)·3H(2)O and Mg(OH)(2), while the inner portion of the layer is primarily MgO. After sintering, the MgCO(3)·3H(2)O was found to be almost completely absent, and the amount of Mg(OH)(2) was also decreased significantly. This is postulated to occur by decomposition of the compounds to MgO and gases during the high temperature of sintering. An increase in the MgO content after sintering supports this theory.

  5. A readout system for X-ray powder crystallography

    CERN Document Server

    Loukas, D; Pavlidis, A; Karvelas, E; Psycharis, K; Misiakos, V; Mousa, J; Dre, C

    2000-01-01

    A system for capturing and processing data, from radiation detectors, in the field of X-ray crystallography has been developed. The system includes a custom-made mixed analog-digital 16-channel VLSI circuit in 50 mu m pitch. Each channel comprises a charge amplifier, a shaper, a comparator and a 21-bit counter. The circuit can be scaled in a daisy chain configuration. Data acquisition is performed with a custom made PCI card while the control software is developed with Visual C++ under the MS Windows NT environment. Performance of a fully operational system, in terms of electronic noise, statistical variations and data capture speed is presented. The noise level permits counting of X-rays down to 8 keV while the counting capability is in excess of 200 kHz. The system is intended for X-ray crystallography with silicon detectors.

  6. Time-of-flight position-sensitive x-ray detection

    International Nuclear Information System (INIS)

    Mowat, J.W.

    1981-01-01

    A new method for recording beam-foil time-of-flight data is described. A stationary, side-window, position-senstive proportional counter, oriented with anode wire parallel to the ion beam, views the decay in flight of excited ions through a Soller slit x-ray collimator. In contrast to the standard method, the exciter foil, placed within or upstream from the field of view, is not moved during the acquisition of a decay curve. Each point on the anode acts like an independent detector seeing a unique segment of the ion beam. The correspondence between the downstream distance at which an ion decays and the position along the anode at which the x-ray is detected makes a pulse-height spectrum of position pulses equivalent to a time-of-flight decay curve. Thus an entire decay curve can now be acquired without moving the foil. Increased efficiency is the most significant improvement over the standard method in which the radiation detector views only a small segment of the flight path at any one time. Experiments using translating foils are subject to a spurious dependence of x-ray intensity on foil position if the foil is non-uniform (or non-uniformly aged) and wobbles as it moves. This effect is eliminated here. Foil aging effects which influence excitation rates and introduce a slowly varying time dependence of the x-ray intensity are automatically normalized by this multichannel technique. The application of this method to metastable x-ray emitting states of low-Z ions are discussed

  7. X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Ray, N.B.

    1977-01-01

    The principle, instrument and procedure of X-ray fluorescence spectrometry are described. It is a rapid, simple and sensitive method for the trace analysis of elements from sodium to uranium in powder, liquid or metal samples. (M.G.B.)

  8. Aggregation of bovine serum albumin upon cleavage of its disulfide bonds, studied by the time-resolved small-angle X-ray scattering technique with synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Ueki, Tatzuo; Inoko, Yoji; Hiragi, Yuzuru; Kataoka, Mikio; Amemiya, Yoshiyuki; Izumi, Yoshinobu; Tagawa, Hiroyuki; Muroga, Yoshio

    1985-11-01

    A rapid mixing system of the stopped-flow type, used with small-angle X-ray scattering equipment using synchrotron radiation, is described. The process of aggregation of bovine serum albumin was traced with a time interval of 50s, initiated upon cleavage of its disulfide bonds by reduction with dithiothreitol. The results indicate that a 218-fold molar excess of dithiothreitol over the number of moles of disulfide bonds in bovine serum albumin is sufficient to initiate the reaction immediately after mixing, which reaches equilibrium in about 15 min. On the other hand, half this amount is not sufficient to initiate the reaction, so that the reaction is delayed by about 150s. Such a single-shot time-resolved experiment showed that experiments with a time interval of 100 ms are possible with repeated multi-shot runs. 26 refs.; 8 figs.

  9. Aggregation of bovine serum albumin upon cleavage of its disulfide bonds, studied by the time-resolved small-angle X-ray scattering technique with synchrotron radiation

    International Nuclear Information System (INIS)

    Ueki, Tatzuo; Inoko, Yoji; Izumi, Yoshinobu; Tagawa, Hiroyuki; Muroga, Yoshio

    1985-01-01

    A rapid mixing system of the stopped-flow type, used with small-angle X-ray scattering equipment using synchrotron radiation, is described. The process of aggregation of bovine serum albumin was traced with a time interval of 50 s, initiated upon cleavage of its disulfide bonds by reduction with dithiothreitol. The results indicate that a 218-fold molar excess of dithiothreitol over the number of moles of disulfide bonds in bovine serum albumin is sufficient to initiate the reaction immediately after mixing, which reaches equilibrium in about 15 min. On the other hand, half this amount is not sufficient to initiate the reaction, so that the reaction is delayed by about 150 s. Such a single-shot time-resolved experiment showed that experiments with a time interval of 100 ms are possible with repeated multi-shot runs. (Auth.)

  10. Evaluation of laboratory powder X-ray micro-diffraction for applications in the fields of cultural heritage and forensic science

    Czech Academy of Sciences Publication Activity Database

    Švarcová, Silvie; Kočí, Eva; Bezdička, Petr; Hradil, David; Hradilová, J.

    2010-01-01

    Roč. 398, č. 2 (2010), s. 1061-1076 ISSN 1618-2642 R&D Projects: GA AV ČR KJB200320901 Institutional research plan: CEZ:AV0Z40320502 Keywords : powder X-ray micro-diffraction * quantitative phase analysis * forensic Subject RIV: CA - Inorganic Chemistry Impact factor: 3.841, year: 2010

  11. Femtosecond x-ray photoelectron diffraction on gas-phase dibromobenzene molecules

    International Nuclear Information System (INIS)

    Rolles, D; Boll, R; Epp, S W; Erk, B; Foucar, L; Hömke, A; Adolph, M; Gorkhover, T; Aquila, A; Chapman, H N; Coppola, N; Delmas, T; Gumprecht, L; Holmegaard, L; Bostedt, C; Bozek, J D; Coffee, R; Decleva, P; Filsinger, F; Johnsson, P

    2014-01-01

    We present time-resolved femtosecond photoelectron momentum images and angular distributions of dissociating, laser-aligned 1,4-dibromobenzene (C 6 H 4 Br 2 ) molecules measured in a near-infrared pump, soft-x-ray probe experiment performed at an x-ray free-electron laser. The observed alignment dependence of the bromine 2p photoelectron angular distributions is compared to density functional theory calculations and interpreted in terms of photoelectron diffraction. While no clear time-dependent effects are observed in the angular distribution of the Br(2p) photoelectrons, other, low-energy electrons show a pronounced dependence on the time delay between the near-infrared laser and the x-ray pulse. (paper)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-05-10

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

  13. Study of the ultrafast polarization dynamics in lithium borohydride by means of femtosecond X-ray diffraction

    International Nuclear Information System (INIS)

    Stingl, Johannes

    2013-01-01

    In this thesis the ultrafast electronic polarisation in the crystalline material lithium borohydride (LiBH 4 ) is examined. The material is excited by a femtosecond long optical pulse and scanned by a likewise short X-ray pulse. Using X-ray scattering the optically induced spatial rearrangement of electronic charge can be directly mapped with atomic spatial resolution. Copper K-alpha X-rays for the experiment are produced in a laboratory table-top laserplasma source with 1 kHz repetition rate. This radiation is then focused on a powdered sample. Debye-Scherrer rings produced from powder diffraction are collected on a large area detector and processed to yield intensity profiles. Using pump-probe technique the change in diffracted intensity, triggered by excitation with a femtosecond optical pulse is examined. The temporal resolution is given by the delay between pump and probe pulse. This way insight is gained into the dynamic electronic evolution of the system. Intensity changes can be correlated to changes in charge density in the relevant material to elucidate structural dynamics on the femtosecond time scale. Lithium borohydride was chosen since it displays necessary characteristics for the exploration of ultrafast electronic polarisation. Up to date there has been no spatially resolved research in the femtosecond regime elucidating this electronic phenomenon. This work presents the ultrafast resonse in Lithiumborhydrid (LiBH 4 ) to strong electronic fields with optical frequencies, which leads to charge relocation accompanied by electronic polarisation.

  14. Determination of the structure factors of a LiF powder sample by the energy dispersive x-ray diffraction

    International Nuclear Information System (INIS)

    Uno, R.; Ahtee, A.; Paakkari, T.

    1977-01-01

    The structure factors of a LiF powder sample were determined by energy dispersive x-ray diffraction in the range 9 to 25 keV, with the use of a Si(Li) solid state detector, following the method applied on GaP. Since the absorption coefficient of LiF is small at high energy, a fraction of the incident x-rays penetrates through the sample and does not contribute to the diffraction. This effect was taken into account in the determination of the structure factors. Then the structure factors generally agree, within the limit of 5 % error, with those obtained by the usual angle dispersive method, if the penetrated part of the incident beam is less than 40 %. (author)

  15. Femtosecond profiling of shaped x-ray pulses

    Science.gov (United States)

    Hoffmann, M. C.; Grguraš, I.; Behrens, C.; Bostedt, C.; Bozek, J.; Bromberger, H.; Coffee, R.; Costello, J. T.; DiMauro, L. F.; Ding, Y.; Doumy, G.; Helml, W.; Ilchen, M.; Kienberger, R.; Lee, S.; Maier, A. R.; Mazza, T.; Meyer, M.; Messerschmidt, M.; Schorb, S.; Schweinberger, W.; Zhang, K.; Cavalieri, A. L.

    2018-03-01

    Arbitrary manipulation of the temporal and spectral properties of x-ray pulses at free-electron lasers would revolutionize many experimental applications. At the Linac Coherent Light Source at Stanford National Accelerator Laboratory, the momentum phase-space of the free-electron laser driving electron bunch can be tuned to emit a pair of x-ray pulses with independently variable photon energy and femtosecond delay. However, while accelerator parameters can easily be adjusted to tune the electron bunch phase-space, the final impact of these actuators on the x-ray pulse cannot be predicted with sufficient precision. Furthermore, shot-to-shot instabilities that distort the pulse shape unpredictably cannot be fully suppressed. Therefore, the ability to directly characterize the x-rays is essential to ensure precise and consistent control. In this work, we have generated x-ray pulse pairs via electron bunch shaping and characterized them on a single-shot basis with femtosecond resolution through time-resolved photoelectron streaking spectroscopy. This achievement completes an important step toward future x-ray pulse shaping techniques.

  16. Deep Chandra Survey of the Small Magellanic Cloud. II. Timing Analysis of X-Ray Pulsars

    Energy Technology Data Exchange (ETDEWEB)

    Hong, JaeSub; Antoniou, Vallia; Zezas, Andreas; Drake, Jeremy J.; Plucinsky, Paul P. [Harvard-Smithsonian Center for Astrophysics, 60 Garden St., Cambridge, MA 02138 (United States); Haberl, Frank [Max-Planck-Institut für extraterrestrische Physik, Giessenbach straße, D-85748 Garching (Germany); Sasaki, Manami [Friedrich-Alexander-Universität Erlangen-Nürnberg, Sternwartstrasse 7, 96049 Bamberg (Germany); Laycock, Silas, E-mail: jaesub@head.cfa.harvard.edu [Department of Physics, University of Massachusetts Lowell, MA 01854 (United States)

    2017-09-20

    We report the timing analysis results of X-ray pulsars from a recent deep Chandra survey of the Small Magellanic Cloud (SMC). We analyzed a total exposure of 1.4 Ms from 31 observations over a 1.2 deg{sup 2} region in the SMC under a Chandra X-ray Visionary Program. Using the Lomb–Scargle and epoch-folding techniques, we detected periodic modulations from 20 pulsars and a new candidate pulsar. The survey also covered 11 other pulsars with no clear sign of periodic modulation. The 0.5–8 keV X-ray luminosity ( L {sub X} ) of the pulsars ranges from 10{sup 34} to 10{sup 37} erg s{sup −1} at 60 kpc. All of the Chandra sources with L {sub X} ≳ 4 × 10{sup 35} erg s{sup −1} exhibit X-ray pulsations. The X-ray spectra of the SMC pulsars (and high-mass X-ray binaries) are in general harder than those of the SMC field population. All but SXP 8.02 can be fitted by an absorbed power-law model with a photon index of Γ ≲ 1.5. The X-ray spectrum of the known magnetar SXP 8.02 is better fitted with a two-temperature blackbody model. Newly measured pulsation periods of SXP 51.0, SXP 214, and SXP 701, are significantly different from the previous XMM-Newton and RXTE measurements. This survey provides a rich data set for energy-dependent pulse profile modeling. Six pulsars show an almost eclipse-like dip in the pulse profile. Phase-resolved spectral analysis reveals diverse spectral variations during pulsation cycles: e.g., for an absorbed power-law model, some exhibit an (anti)-correlation between absorption and X-ray flux, while others show more intrinsic spectral variation (i.e., changes in photon indices).

  17. Techniques for materials research with synchrotron radiation x-rays

    International Nuclear Information System (INIS)

    Bowen, D.K.

    1983-01-01

    A brief introductory survey is presented of the properties and generation of synchrotron radiation and the main techniques developed so far for its application to materials problems. Headings are:synchrotron radiation; X-ray techniques in synchrotron radiation (powder diffraction; X-ray scattering; EXAFS (Extended X-ray Absorption Fine Structure); X-ray fluorescent analysis; microradiography; white radiation topography; double crystal topography); future developments. (U.K.)

  18. Small Angle X-Ray Scattering Detector

    Energy Technology Data Exchange (ETDEWEB)

    Hessler, Jan P.

    2004-06-15

    A detector for time-resolved small-angle x-ray scattering includes a nearly constant diameter, evacuated linear tube having an end plate detector with a first fluorescent screen and concentric rings of first fiber optic bundles for low angle scattering detection and an annular detector having a second fluorescent screen and second fiber optic bundles concentrically disposed about the tube for higher angle scattering detection. With the scattering source, i.e., the specimen under investigation, located outside of the evacuated tube on the tube's longitudinal axis, scattered x-rays are detected by the fiber optic bundles, to each of which is coupled a respective photodetector, to provide a measurement resolution, i.e., dq/q, where q is the momentum transferred from an incident x-ray to an x-ray scattering specimen, of 2% over two (2) orders of magnitude in reciprocal space, i.e., qmax/qmin approx=lO0.

  19. Simultaneously time- and space-resolved spectroscopic characterization of laser-produced plasmas

    International Nuclear Information System (INIS)

    Charatis, G.; Young, B.K.F.; Busch, G.E.

    1988-01-01

    The CHROMA laser facility at KMS Fusion has been used to irradiate a variety of microdot targets. These include aluminum dots and mixed bromine dots doped with K-shell (magnesium) emitters. Simultaneously time- and space-resolved K-shell and L-shell spectra have been measured and compared to dynamic model predictions. The electron density profiles are measured using holographic interferometry. Temperatures, densities, and ionization distributions are determined using K-shell and L-shell spectral techniques. Time and spatial gradients are resolved simultaneously using three diagnostics: a framing crystal x-ray spectrometer, an x-ray streaked crystal spectrometer with a spatial imaging slit, and a 4-frame holographic interferometer. Significant differences have been found between the interferometric and the model-dependent spectral measurements of plasma density. Predictions by new non-stationary L-shell models currently being developed are also presented. 14 refs., 10 figs

  20. Operation manual for EDXRDDA - a software package for Bragg peak analysis of energy dispersive powder X-ray diffraction data

    International Nuclear Information System (INIS)

    Jayaswal, Balhans; Vijaykumar, V.; Momin, S.N.; Sikka, S.K.

    1992-01-01

    EDXRDDA is a software package for analysis of raw data for energy dispersive x-ray diffraction from powder samples. It resolves the spectra into individual peaks by a constrained non-linear least squares method (Hughes and Sexton, 1988). The profile function adopted is the Gaussian/Lorentzian product with the mixing ratio refinable in the program. The program is implemented on an IBM PC and is highly interactive with extensive plotting facilities. This report is a user's guide for running the program. In the first step after inputting the spectra, the full spectra is plotted on the screen. The user then chooses a portion of this for peak resolution. The initial guess for the peak intensity, peak position are input with the help of a cursor or a mouse. Upto twenty peaks can be fitted at a time in an interval of 500 channels. For overlapping peaks, various constraints can be applied. Bragg peaks and fluorescence peaks with different half widths can be handled simultaneously. The program on execution produces a look up table which contains the refined values of the peak position, half width, peak intensity, integrated intensity, and their error estimates of each peak. The program is very general and can also be used for curve fitting of data from many other experiments. (author). 2 refs., 7 figs., 2 appendices

  1. ENDIX. A computer program to simulate energy dispersive X-ray and synchrotron powder diffraction diagrams

    International Nuclear Information System (INIS)

    Hovestreydt, E.; Karlsruhe Univ.; Parthe, E.; Benedict, U.

    1987-01-01

    A Fortran 77 computer program is described which allows the simulation of energy dispersive X-ray and synchrotron powder diffraction diagrams. The input consists of structural data (space group, unit cell dimensions, atomic positional and displacement parameters) and information on the experimental conditions (chosen Bragg angle, type of X-ray tube and applied voltage or operating power of synchrotron radiation source). The output consists of the normalized intensities of the diffraction lines, listed by increasing energy (in keV), and of an optional intensity-energy plot. The intensities are calculated with due consideration of the wave-length dependence of both the anomalous dispersion and the absorption coefficients. For a better agreement between observed and calculated spectra provision is made to optionally superimpose, on the calculated diffraction line spectrum, all additional lines such as fluorescence and emission lines and escape peaks. The different effects which have been considered in the simulation are discussed in some detail. A sample calculation of the energy dispersive powder diffraction pattern of UPt 3 (Ni 3 Sn structure type) is given. Warning: the user of ENDIX should be aware that for a successful application it is necessary to adapt the program to correspond to the actual experimental conditions. Even then, due to the only approximately known values of certain functions, the agreement between observed and calculated intensities will not be as good as for angle dispersive diffraction methods

  2. Characterization of cubic ceria?zirconia powders by X-ray diffraction and vibrational and electronic spectroscopy

    Science.gov (United States)

    Sánchez Escribano, Vicente; Fernández López, Enrique; Panizza, Marta; Resini, Carlo; Gallardo Amores, José Manuel; Busca, Guido

    2003-10-01

    The X-ray diffraction (XRD) patterns and the Infrared, Raman and UV-visible spectra of CeO 2ZrO 2 powders prepared by co-precipitation are presented. Raman spectra provide evidence for the largely predominant cubic structure of the powders with CeO 2 molar composition higher than 25%. Also skeletal IR spectra allow to distinguish cubic from tetragonal phases which are instead not easily distinguished on the basis of the XRD patterns. All mixed oxides including pure ceria are strong UV absorbers although also absorb in the violet visible region. By carefully selecting their composition and treatment temperature, the onset of the radiation that they cut off can be chosen in the 425-475 nm interval. Although they are likely metastable, the cubic phases are still pure even after heating at 1173 K for 4 h.

  3. Compact x-ray microradiograph for in situ imaging of solidification processes: Bringing in situ x-ray micro-imaging from the synchrotron to the laboratory

    Energy Technology Data Exchange (ETDEWEB)

    Rakete, C.; Baumbach, C.; Goldschmidt, A.; Samberg, D.; Schroer, C. G. [Institut fuer Strukturphysik, Technische Universitaet Dresden, D-01062 Dresden (Germany); Breede, F.; Stenzel, C. [Astrium-Space Transportation, Department: TO 611, Claude-Dornier-Strasse, D-88039 Friedrichshafen (Germany); Zimmermann, G.; Pickmann, C. [ACCESS e.V., Intzestrasse 5, D-52072 Aachen (Germany); Houltz, Y.; Lockowandt, C. [Science Services Division, SSC, Box 4207, SE-17104 Solna (Sweden); Svenonius, O.; Wiklund, P. [Scint-X AB, Torshamnsgatan 35, SE-164 40 Kista (Sweden); Mathiesen, R. H. [Inst. for Fysikk, NTNU, N-7491 Trondheim (Norway)

    2011-10-15

    A laboratory based high resolution x-ray radiograph was developed for the investigation of solidification dynamics in alloys. It is based on a low-power microfocus x-ray tube and is potentially appropriate for x-ray diagnostics in space. The x-ray microscope offers a high spatial resolution down to approximately 5 {mu}m. Dynamic processes can be resolved with a frequency of up to 6 Hz. In reference experiments, the setup was optimized to yield a high contrast for AlCu-alloys. With samples of about 150 {mu}m thickness, high quality image sequences of the solidification process were obtained with high resolution in time and space.

  4. Simulation tools for scattering corrections in spectrally resolved x-ray computed tomography using McXtrace

    Science.gov (United States)

    Busi, Matteo; Olsen, Ulrik L.; Knudsen, Erik B.; Frisvad, Jeppe R.; Kehres, Jan; Dreier, Erik S.; Khalil, Mohamad; Haldrup, Kristoffer

    2018-03-01

    Spectral computed tomography is an emerging imaging method that involves using recently developed energy discriminating photon-counting detectors (PCDs). This technique enables measurements at isolated high-energy ranges, in which the dominating undergoing interaction between the x-ray and the sample is the incoherent scattering. The scattered radiation causes a loss of contrast in the results, and its correction has proven to be a complex problem, due to its dependence on energy, material composition, and geometry. Monte Carlo simulations can utilize a physical model to estimate the scattering contribution to the signal, at the cost of high computational time. We present a fast Monte Carlo simulation tool, based on McXtrace, to predict the energy resolved radiation being scattered and absorbed by objects of complex shapes. We validate the tool through measurements using a CdTe single PCD (Multix ME-100) and use it for scattering correction in a simulation of a spectral CT. We found the correction to account for up to 7% relative amplification in the reconstructed linear attenuation. It is a useful tool for x-ray CT to obtain a more accurate material discrimination, especially in the high-energy range, where the incoherent scattering interactions become prevailing (>50 keV).

  5. Handbook of X-Ray Astronomy

    Science.gov (United States)

    Arnaud, Keith A. (Editor); Smith, Randall K.; Siemiginowska, Aneta

    2011-01-01

    X-ray astronomy was born in the aftermath of World War II as military rockets were repurposed to lift radiation detectors above the atmosphere for a few minutes at a time. These early flights detected and studied X-ray emission from the Solar corona. The first sources beyond the Solar System were detected during a rocket flight in 1962 by a team headed by Riccardo Giaccom at American Science and Engineering, a company founded by physicists from MIT. The rocket used Geiger counters with a system designed to reduce non-X-ray backgrounds and collimators limiting the region of sky seen by the counters. As the rocket spun, the field of view (FOV) happened to pass over what was later found to be the brightest non-Solar X-ray source; later designated See X-1. It also detected a uniform background glow which could not be resolved into individual sources. A follow-up campaign using X-ray detectors with better spatial resolution and optical telescopes identified See X-1 as an interacting binary with a compact (neutron star) primary. This success led to further suborbital rocket flights by a number of groups. More X-ray binaries were discovered, as well as X-ray emission from supernova remnants, the radio galaxies M87 and Cygnus-A, and the Coma cluster. Detectors were improved and Geiger counters were replaced by proportional counters, which provided information about energy spectra of the sources. A constant challenge was determining precise positions of sources as only collimators were available.

  6. Extra-oral dental radiography for disaster victims using a flat panel X-ray detector and a hand-held X-ray generator.

    Science.gov (United States)

    Ohtani, M; Oshima, T; Mimasaka, S

    2017-12-01

    Forensic odontologists commonly incise the skin for post-mortem dental examinations when it is difficult to open the victim's mouth. However, it is prohibited by law to incise dead bodies without permission in Japan. Therefore, we attempted using extra-oral dental radiography, using a digital X-ray equipment with rechargeable batteries, to overcome this restriction. A phantom was placed in the prone position on a table, and three plain dental radiographs were used per case: "lateral oblique radiographs" for left and right posterior teeth and a "contact radiograph" for anterior teeth were taken using a flat panel X-ray detector and a hand-held X-ray generator. The resolving power of the images was measured by a resolution test chart, and the scattered X-ray dose was measured using an ionization chamber-type survey meter. The resolving power of the flat panel X-ray detector was 3.0 lp/mm, which was less than that of intra-oral dental methods, but the three extra-oral plain dental radiographs provided the overall dental information from outside of the mouth, and this approach was less time-consuming. In addition, the higher dose of scattered X-rays was laterally distributed, but the dose per case was much less than that of intra-oral dental radiographs. Extra-oral plain dental radiography can be used for disaster victim identification by dental methods even when it is difficult to open the mouth. Portable and rechargeable devices, such as a flat panel X-ray detector and a hand-held X-ray generator, are convenient to bring and use anywhere, even at a disaster scene lacking electricity and water.

  7. X-ray lasers for structural and dynamic biology

    International Nuclear Information System (INIS)

    Spence, J C H; Weierstall, U; Chapman, H N

    2012-01-01

    Research opportunities and techniques are reviewed for the application of hard x-ray pulsed free-electron lasers (XFEL) to structural biology. These include the imaging of protein nanocrystals, single particles such as viruses, pump–probe experiments for time-resolved nanocrystallography, and snapshot wide-angle x-ray scattering (WAXS) from molecules in solution. The use of femtosecond exposure times, rather than freezing of samples, as a means of minimizing radiation damage is shown to open up new opportunities for the molecular imaging of biochemical reactions at room temperature in solution. This is possible using a ‘diffract-and-destroy’ mode in which the incident pulse terminates before radiation damage begins. Methods for delivering hundreds of hydrated bioparticles per second (in random orientations) to a pulsed x-ray beam are described. New data analysis approaches are outlined for the correlated fluctuations in fast WAXS, for protein nanocrystals just a few molecules on a side, and for the continuous x-ray scattering from a single virus. Methods for determining the orientation of a molecule from its diffraction pattern are reviewed. Methods for the preparation of protein nanocrystals are also reviewed. New opportunities for solving the phase problem for XFEL data are outlined. A summary of the latest results is given, which now extend to atomic resolution for nanocrystals. Possibilities for time-resolved chemistry using fast WAXS (solution scattering) from mixtures is reviewed, toward the general goal of making molecular movies of biochemical processes. (key issues reviews)

  8. The Crystal Structure of the Malaria Pigment Hemozoin as Elucidated by X-ray Powder Diffraction

    DEFF Research Database (Denmark)

    Straasø, Tine

    survival. Successful inhibition of hemozoin crystallization will lead to parasitic death and thus break the cycle. The aim of this thesis is to elucidate the structure of hemozoin by means of X-ray diffraction techniques. Knowledge of the structure will help facilitate intelligent drug design in the future....... As part of the project an all-in-vacuum powder diffractometer was developed, which provides data with a minimum background level and an improved signal-to-noise ratio. Moreover, the diffractometer is designed with the particular purpose of decreasing the number of parameters to be fitted. Installation...

  9. Crystallization behavior of polyethylene on silicon wafers in solution casting processes traced by time-resolved measurements of synchrotron grazing-incidence small-angle and wide-angle X-ray scattering

    International Nuclear Information System (INIS)

    Sasaki, S; Masunaga, H; Takata, M; Itou, K; Tashiro, K; Okuda, H; Takahara, A

    2009-01-01

    Crystallization behavior of polyethylene (PE) on silicon wafers in solution casting processes has been successfully traced by time-resolved grazing-incidence small-angle and wide-angle X-ray scattering (GISWAXS) measurements utilizing synchrotron radiation. A p-xylene solution of PE kept at ca. 343 K was dropped on a silicon wafer at ca. 298 K. While the p-xylene evaporated naturally from the dropped solution sample, PE chains crystallized to be a thin film. Raman spectral measurements were performed simultaneously with the GISWAXS measurements to evaluate quantitatively the p-xylene the dropped solution contained. Grazing-incidence wide-angle X-ray scattering (GIWAXS) patterns indicated nucleation and crystal growth in the dropped solution and the following as-cast film. GIWAXS and Raman spectral data revealed that crystallization of PE was enhanced after complete evaporation of the p-xylene from the dropped solution. The [110] and [200] directions of the orthorhombic PE crystal became relatively parallel to the wafer surface with time, which implied that the flat-on lamellae with respect to the wafer surface were mainly formed in the as-cast film. On the other hand, grazing-incidence small-angle X-ray scattering (GISAXS) patterns implied formation of isolated lamellae in the dropped solution. The lamellae and amorphous might alternatively be stacked in the preferred direction perpendicular to the wafer surface. The synchrotron GISWAXS experimental method could be applied for kinetic study on hierarchical structure of polymer thin films.

  10. X-ray spectroscopy for high energy-density X pinch density and temperature measurements (invited)

    International Nuclear Information System (INIS)

    Pikuz, S.A.; Shelkovenko, T.A.; Chandler, K.M.; Mitchell, M.D.; Hammer, D.A.; Skobelev, I.Y.; Shlyaptseva, A.S.; Hansen, S.B.

    2004-01-01

    X pinch plasmas produced from fine metal wires can reach near solid densities and temperatures of 1 keV or even more. Plasma conditions change on time scales as short as 5-10 ps as determined using an x-ray streak camera viewing a focusing crystal spectrograph or directly viewing the plasma through multiple filters on a single test. As a result, it is possible to determine plasma conditions from spectra with ∼10 ps time resolution. Experiments and theory are now coming together to give a consistent picture of the dynamics and kinetics of these high energy density plasmas with very high temporal and spatial precision. A set of diagnostic techniques used in experiments for spectrally, temporally, and spatially resolved measurements of X pinch plasmas is described. Results of plasma parameter determination from these measurements are presented. X ray backlighting of one x-pinch by another with ∼30 ps x-ray pulses enables the dynamics and kinetics to be correlated in time

  11. High-temperature dehydration of talc: a kinetics study using in situ X-ray powder diffraction

    Science.gov (United States)

    Wang, Duojun; Yi, Li; Huang, Bojin; Liu, Chuanjiang

    2015-06-01

    High-temperature in situ X-ray powder diffraction patterns were used to study the dehydration kinetics of natural talc with a size of 10-15 µm. The talc was annealed from 1073 to 1223 K, and the variations in the characteristic peaks corresponding to talc with the time were recorded to determine the reaction progress. The decomposition of talc occurred, and peaks corresponding to talc and peaks corresponding to enstatite and quartz were observed. The enstatite and talc exhibited a topotactic relationship. The dehydration kinetics of talc was studied as a function of temperature between 1073 and 1223 K. The kinetics data could be modeled using an Avrami equation that considers nucleation and growth processes ? where n varies from 0.4 to 0.8. The rate constant (k) equation for the natural talc is ? The reaction mechanism for the dehydration of talc is a heterogeneous nucleation and growth mechanism.

  12. X-ray methods for the chemical characterization of atmospheric aerosols

    International Nuclear Information System (INIS)

    Jaklevic, J.M.; Thompson, A.C.

    1981-05-01

    The development and use of several x-ray methods for the chemical characterization of atmospherical aerosol particulate samples are described. These methods are based on the emission, absorption, and scattering of x-ray photons with emphasis on the optimization for the non-destructive analysis of dilute specimens. Techniques discussed include photon induced energy dispersive x-ray fluorescence, extended x-ray absorption fine structure spectroscopy using synchrotron radiation and high-rate x-ray powder diffractometry using a position-sensitive gas proportional counter. These x-ray analysis methods were applied to the measurement of the chemical compositions of size-segregated aerosol particulate samples obtained with dichotomous samplers. The advantages of the various methods for use in such measurements are described and results are presented. In many cases, the complementary nature of the analytical information obtained from the various measurements is an important factor in the characterization of the sample. For example, the multiple elemental analyses obtained from x-ray fluorescence can be used as a cross check on the major compounds observed by powder diffraction

  13. Time-resolved X-ray diffraction studies of frog skeletal muscle isometrically twitched by two successive stimuli using synchrotron radiation

    International Nuclear Information System (INIS)

    Tanaka, Hidehiro; Kobayashi, Takakazu; Wakabayashi, Katsuzo

    1986-01-01

    In order to clarify the delay between muscular structural changes and mechanical responses, the intensity changes of the equatorial and myosin layer-line reflections were studied by a time-resolved X-ray diffraction technique using synchrotron radiation. The muscle was stimulated at 12-13 0 C by two successive stimuli at an interval during which the second twitch started while tension was still being exerted by the muscle. At the first twitch, the intensity changes of the 1,0 and 1,1 equatorial reflections reached 65 and 200% of the resting values, and further changes to 55 and 220% were seen at the second twitch, respectively. Although the second twitch decreased not only the time to peak tension but also that to the maximum intensity changes of the equatorial reflections, the delay between the intensity changes and the development of tension at the first twitch were still observed at the second twitch. On the other hand, the intensities of the 42.9 nm off-meridional and the 21.5 nm meridional myosin reflections decreased at the first twitch to the levels found when a muscle was isometrically tetanized, and no further decrease in their intensities was observed at the second twitch. These results indicate that a certain period of time is necessary for myosin heads to contr0116e to tension development after their arrival in the vicinity of the thin filaments during contraction. (Auth.)

  14. Comparison of x-ray output of inverter-type x-ray equipment

    International Nuclear Information System (INIS)

    Asano, Hiroshi; Miyake, Hiroyuki; Yamamoto, Keiichi

    2000-01-01

    The x-ray output of 54 inverter-type x-ray apparatuses used at 18 institutions was investigated. The reproducibility and linearity of x-ray output and variations among the x-ray equipment were evaluated using the same fluorescence meter. In addition, the x-ray apparatuses were re-measured using the same non-invasive instrument to check for variations in tube voltage, tube current, and irradiation time. The non-invasive instrument was calibrated by simultaneously obtaining measurements with an invasive instrument, employing the tube voltage and current used for the invasive instrument, and the difference was calculated. Reproducibility of x-ray output was satisfactory for all x-ray apparatuses. The coefficient of variation was 0.04 or less for irradiation times of 5 ms or longer. In 84.3% of all x-ray equipment, variation in the linearity of x-ray output was 15% or less for an irradiation time of 5 ms. However, for all the apparatuses, the figure was 50% when irradiation time was the shortest (1 to 3 ms). Variation in x-ray output increased as irradiation time decreased. Variation in x-ray output ranged between 1.8 and 2.5 compared with the maximum and minimum values, excluding those obtained at the shortest irradiation time. The relative standard deviation ranged from ±15.5% to ±21.0%. The largest variation in x-ray output was confirmed in regions irradiated for the shortest time, with smaller variations observed for longer irradiation times. The major factor responsible for variation in x-ray output in regions irradiated for 10 ms or longer, which is a relatively long irradiation time, was variation in tube current. Variation in tube current was slightly greater than 30% at maximum, with an average value of 7% compared with the preset tube current. Variations in x-ray output in regions irradiated for the shortest time were due to photographic effects related to the rise and fall times of the tube voltage waveform. Accordingly, in order to obtain constant x-ray

  15. X-ray coherent scattering tomography of textured material (Conference Presentation)

    Science.gov (United States)

    Zhu, Zheyuan; Pang, Shuo

    2017-05-01

    Small-angle X-ray scattering (SAXS) measures the signature of angular-dependent coherently scattered X-rays, which contains richer information in material composition and structure compared to conventional absorption-based computed tomography. SAXS image reconstruction method of a 2 or 3 dimensional object based on computed tomography, termed as coherent scattering computed tomography (CSCT), enables the detection of spatially-resolved, material-specific isotropic scattering signature inside an extended object, and provides improved contrast for medical diagnosis, security screening, and material characterization applications. However, traditional CSCT methods assumes materials are fine powders or amorphous, and possess isotropic scattering profiles, which is not generally true for all materials. Anisotropic scatters cannot be captured using conventional CSCT method and result in reconstruction errors. To obtain correct information from the sample, we designed new imaging strategy which incorporates extra degree of detector motion into X-ray scattering tomography for the detection of anisotropic scattered photons from a series of two-dimensional intensity measurements. Using a table-top, narrow-band X-ray source and a panel detector, we demonstrate the anisotropic scattering profile captured from an extended object and the reconstruction of a three-dimensional object. For materials possessing a well-organized crystalline structure with certain symmetry, the scatter texture is more predictable. We will also discuss the compressive schemes and implementation of data acquisition to improve the collection efficiency and accelerate the imaging process.

  16. Phase-Resolved Spectroscopy of the Low-Mass X-ray Binary V801 Ara

    Science.gov (United States)

    Brauer, Kaley; Vrtilek, Saeqa Dil; Peris, Charith; McCollough, Michael

    2018-06-01

    We present phase-resolved optical spectra of the low mass X-ray binary system V801 Ara. The spectra, obtained in 2014 with IMACS on the Magellan/Baade telescope at Las Campanas Observatory, cover the full binary orbit of 3.8 hours. They contain strong emission features allowing us to map the emission of Hα, Hβ, He II λ4686, and the Bowen blend at λ4640. The radial velocity curves of the Bowen blend shows significantly stronger modulation at the orbital period than Hα as expected for the former originating on the secondary with the latter consistent with emission dominated by the disk. Our tomograms of Hα and Hβ are the most detailed studies of these lines for V801 to date and they clearly detect the accretion disk. The Hβ emission extends to higher velocities than Hα, suggesting emission from closer to the neutron star and differentiating temperature variance in the accretion disk for the first time. The center of the accretion disk appears offset from the center-of-mass of the neutron star as has been seen in several other X-ray binaries. This is often interpreted to imply disk eccentricity. Our tomograms do not show strong evidence for a hot spot at the point where the accretion stream hits the disk. This could imply a reduced accretion rate or could be due to the spot being drowned out by bright accretion flow around it. There is enhanced emission further along the disk, however, which implies gas stream interaction downstream of the hot spot.

  17. Time-resolved x-ray diffraction from frog skeletal muscle during an isotonic twitch under a small load

    International Nuclear Information System (INIS)

    Sugi, Haruo; Amemiya, Yoshiyuki; Hashizume, Hiroo.

    1978-01-01

    A time-resolved x-ray diffraction technique was used to study the time course of change in the intensity ratio Isub(1,0)/Isub(1,1) during isotonic twitch (initial sarcomere, 2.4 μm) under a small load and to determine the kinetic properties of the crossbridges responsible for muscle contraction. Isotonic twitches in four other preparations with an initial sarcomere of 2.4 μm and in two with an initial sarcomere of 2.3 μm and 2.2 μm, respectively, were examined. In each case, the intensity ratio started to decrease at stimulation, reached a minimum value of 0.8 - 1.0 within the first 20 - 30% of the shortening phase, and maintained this value until the beginning of the relaxation phase. Gradual recovery of the intensity ratio to the resting value was seen during the relaxation phase. During the recovery phase, the intensity ratio appeared to exhibit oscillatory changes. Though the extent of shortening was reduced by about 30% at the end of each experiment, the duration of the shortening phase remained almost unchanged in all the preparations examined. The time course of change in the intensity ratio was also examined during an isometric twitch in four preparations (sarcomere, 2.4 μm) with the tibial end connected to a strain gauge. The extent of internal shortening of muscle fibres against the tendons and the recording system during an isometric twitch or a tetanus at low temperatures was estimated. The intensity ratio decreased to a minimum value of 0.5 - 0.6 during the rising phase of isometric tension and started to return to the resting value after the beginning of relaxation. In both isotonic and isometric twitches, a decrease in the intensity ratio resulted from both a decrease in the 1,0 intensity and an increase in the 1,1 intensity. (J.P.N.)

  18. Space resolved x-ray diffraction measurements of the supercooled state of polymers

    International Nuclear Information System (INIS)

    Asano, Tsutomu; Yoshida, Shinya; Nishida, Akira; Mina, M.F.

    2002-01-01

    In order to measure an ordering process of polymers, the supercooled state near the crystallizing surface was observed by a space resolved X-ray diffraction method at Photon Factory (PF). Using temperature slope crystallization, low density polyethylene and even-number paraffins were examined during crystallization from the melt state. The results indicate that polyethylene shows a sharp b-axis orientation where the lamellar normal and crystalline c-axis are perpendicular to the temperature slope. The crystalline lamellae are well-developed with lamellar thickness of 180 A. The supercooled melt state just above the crystallizing plane shows some diffraction in the small angle region without any crystalline reflection in the wide angle. This fact suggests that a long-range ordering (lamellar structure) appears prior to the short-range one (crystalline structure). The in-situ crystallizing surface was observed by an optical microscope connected to a TV system. The crystallizing surface of even-number paraffins moves to upwards in the temperature slope. In-situ X-ray measurements at PF revealed that the crystalline c-axis and lamellar normal of the even number paraffins are parallel to the temperature slope. From these results, the crystalline ordering and the surface movement of even number paraffins are explained using special nucleation mechanism including a screw dislocation. (author)

  19. X-ray beam size measurements on the Advanced Test Accelerator

    International Nuclear Information System (INIS)

    Struve, K.W.; Chambers, F.W.; Lauer, E.J.; Slaughter, D.R.

    1986-01-01

    The electron beam size has been determined on the Advanced Test Accelerator (ATA) by intercepting the beam with a target and measuring the resulting x-ray intensity as a function of time as the target is moved through the beam. Several types of targets have been used. One is a tantalum rod which extends completely across the drift chamber. Another is a tungsten powder filled carbon crucible. Both of these probes are moved from shot to shot so that the x-ray signal intensity varies with probe position. A third is a larger tantalum disk which is inserted on beam axis to allow determining beam size on a one shot basis. The x-ray signals are detected with an MCP photomultiplier tube located at 90 0 to the beamline. It is sufficiently shielded to reject background x-rays and neutrons. The signals were digitized, recorded and later unfolded to produce plots of x-ray intensity versus probe position for several times during the pulse. The presumption that the x-ray intensity is proportional to beam current density is checked computationally. Details of the probe construction and PMT shielding, as well as sample measurements are given

  20. Structure and dynamics in liquid water from x-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Wernet, Philippe

    2009-01-01

    Oxygen K-edge x-ray absorption spectra of water are discussed. The spectra of gas-phase water, liquid water and ice illustrate the sensitivity of oxygen K-edge x-ray absorption spectroscopy to hydrogen bonding in water. Transmission mode spectra of amorphous and crystalline ice are compared to x-ray Raman spectra of ice. The good agreement consolidates the experimental spectrum of crystalline ice and represents an incentive for theoretical calculations of the oxygen K-edge absorption spectrum of crystalline ice. Time-resolved infrared-pump and x-ray absorption probe results are finally discussed in the light of this structural interpretation.

  1. Surface characterization of selected polymer thin films by total-reflection x-ray fluorescence spectroscopy and x-ray reflectivity

    International Nuclear Information System (INIS)

    Innis, Vallerie Ann A.

    2006-01-01

    Development of available x-ray characterizations tools for grazing incidence techniques was done to be able to probe nano-size thin films. Alignment of a Philips x-ray powder diffractometer was improved to let it perform as an x-ray reflectometer. X-ray reflectometry was coupled with total-reflection x-ray fluorescence spectroscopy. Evaluation of the performance of this grazing incidence techniques was done by preparing polymer thin films of carboxymethylcellulose, carrageenan and polyvinylpyrrolidone (PVP). The thickness of the films were varied by varying the process parameters such as concentration, spin speed and spin time. Angle-dispersive total-reflection x-ray fluorescence spectroscopy profiles of three films showed film formation only in carrageenan and PVP. For both carrageenan and PVP, an increase in concentration yielded a corresponding increase in intensity of the fluorescent or scattered peaks. XRR profiles of carrageenan thin films yielded a mean value for the critical angle close to quartz substrate. Thickness measurements of the prepared carrageenan thin films showed that concentration was the main determinant for final film thickness over the other process parameters. Sulfur fluorescent intensity derived from the TXRF measurement showed a linear relationship with the measured thickness by XRR. For PVP, measured critical angle is lower than quartz. Poor adhesion of the polymer onto the substrate yielded a limited number of thickness measurements made from the XRR profiles. (Author)

  2. Obtaining absolute spatial flux measurements with a time-resolved pinhole camera

    International Nuclear Information System (INIS)

    Baker, K.L.; Porter, J.L.; Ruggles, L.E.; Fehl, D.L.; Chandler, G.A.; Vargas, M.; Mix, L.P.; Simpson, W.W.; Deeney, C.; Chrien, R.E.; Idzorek, G.C.

    1999-01-01

    A technique is described to determine the spatial x-ray flux emitted from a hohlraum wall and subsequently transmitted through a diagnostic hole. This technique uses x-ray diodes, bolometers, and a time-resolved pinhole camera to determine the spatial flux of x rays emitted through a hohlraum close-quote s diagnostic hole. The primary motivation for this analysis was the relatively long duration, nearly 100 ns, of the x-ray drive present in z-pinch driven hohlraums. This radiation causes plasma to ablate from the hohlraum walls surrounding the diagnostic hole and results in a partial obscuration that reduces the effective area over which diagnostics view the radiation. The effective change in area leads to an underestimation of the wall temperature when nonimaging diagnostics such as x-ray diodes and bolometers are used to determine power and later to infer a wall temperature. An analysis similar to the one described below is then necessary to understand the radiation environment present in x-ray driven hohlraums when these diagnostics are used and hole closure is important. copyright 1999 American Institute of Physics

  3. Time- and position-resolved synchrotron x-ray scattering for structure research on biological connective tissue

    International Nuclear Information System (INIS)

    Zizak, I.

    2000-03-01

    ELETTRA in Trieste. The results obtained during this thesis can be summarized in the following way: - If the tendon is stretched fast (0.1 %/second), the collagen fibers are not stretched an equal amount. Interfibrillar connections are responsible for about 50 % of the elongation of the tendon. - If the tendon is slowly stretched, the fibers creep, so they are stretched even less. At stretching speeds of 0.001 %/second the fibers are stretched only 10 % of the total tendon elongation. - There are two different processes in the collagen fiber which occur during the stretching. Stretching of the collagen triple helix is responsible for about 1/4 of the fibril elongation, and the rest can be described with the slippage of the helices, where only the cross-links between the molecules are stretched. There are indications that this process also depends on the velocity, what would include the viscose processes on the molecular level. Scanning small angle x-ray scattering of bone and cartilage Bone and cartilage are composite tissues consisting of an organic matrix (collagen) and small mineral particles (hydroxyapatite). The mineral particles have a typical thickness of about 3 nm and a length of a few hundreds of nanometers. At a higher hierarchical levels (sub-mm), the tissues have a foam like, trabecular structure with the trabeculae oriented along the main tension lines. The mechanical properties of bone depend on the structure at all levels of hierarchical organization. At the nanometer level, they are determined mainly by the size, shape and orientation of the (hard) mineral crystals within the (soft) organic matrix. In the course of this work, the hierarchical structure of the bone and cartilage was investigated using light- and scanning electron microscopy as well as position resolved scattering methods. A great advantage is the use of scanning small angle x-ray scattering (sSAXS) and wide angle scattering (WAXD, also x-ray diffraction, XRD), which provides simultaneous

  4. Preparation of specimens for analysis by: X-ray diffraction and X-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Banos L, L.

    2004-01-01

    Specimen preparation is one of the most important requirements in the analysis of samples by X-ray Diffraction and X-ray Fluorescence. This statement is especially true for samples containing different types of materials. There are many forms of specimen suitable for X-ray analysis and the type of the sample as received will generally determine the method of pretreatment. It is convenient to refer to the material received for analysis as the sample, and that, which is actually analyzed as the specimen. The powder Diffraction method assumes that the particles in the specimen are ideally random orientation and that there are enough crystallites in the specimen to achieve a representative intensity distribution for these crystallites. X ray Fluorescence is essentially a comparative method of analysis, it is vital that all standards and unknowns be presented to the spectrometer in a reproducible and identical manner. (Author) 3 refs., 6 figs

  5. Three-dimensional electron diffraction as a complementary technique to powder X-ray diffraction for phase identification and structure solution of powders

    Directory of Open Access Journals (Sweden)

    Yifeng Yun

    2015-03-01

    Full Text Available Phase identification and structure determination are important and widely used techniques in chemistry, physics and materials science. Recently, two methods for automated three-dimensional electron diffraction (ED data collection, namely automated diffraction tomography (ADT and rotation electron diffraction (RED, have been developed. Compared with X-ray diffraction (XRD and two-dimensional zonal ED, three-dimensional ED methods have many advantages in identifying phases and determining unknown structures. Almost complete three-dimensional ED data can be collected using the ADT and RED methods. Since each ED pattern is usually measured off the zone axes by three-dimensional ED methods, dynamic effects are much reduced compared with zonal ED patterns. Data collection is easy and fast, and can start at any arbitrary orientation of the crystal, which facilitates automation. Three-dimensional ED is a powerful technique for structure identification and structure solution from individual nano- or micron-sized particles, while powder X-ray diffraction (PXRD provides information from all phases present in a sample. ED suffers from dynamic scattering, while PXRD data are kinematic. Three-dimensional ED methods and PXRD are complementary and their combinations are promising for studying multiphase samples and complicated crystal structures. Here, two three-dimensional ED methods, ADT and RED, are described. Examples are given of combinations of three-dimensional ED methods and PXRD for phase identification and structure determination over a large number of different materials, from Ni–Se–O–Cl crystals, zeolites, germanates, metal–organic frameworks and organic compounds to intermetallics with modulated structures. It is shown that three-dimensional ED is now as feasible as X-ray diffraction for phase identification and structure solution, but still needs further development in order to be as accurate as X-ray diffraction. It is expected that three

  6. Three-dimensional electron diffraction as a complementary technique to powder X-ray diffraction for phase identification and structure solution of powders.

    Science.gov (United States)

    Yun, Yifeng; Zou, Xiaodong; Hovmöller, Sven; Wan, Wei

    2015-03-01

    Phase identification and structure determination are important and widely used techniques in chemistry, physics and materials science. Recently, two methods for automated three-dimensional electron diffraction (ED) data collection, namely automated diffraction tomography (ADT) and rotation electron diffraction (RED), have been developed. Compared with X-ray diffraction (XRD) and two-dimensional zonal ED, three-dimensional ED methods have many advantages in identifying phases and determining unknown structures. Almost complete three-dimensional ED data can be collected using the ADT and RED methods. Since each ED pattern is usually measured off the zone axes by three-dimensional ED methods, dynamic effects are much reduced compared with zonal ED patterns. Data collection is easy and fast, and can start at any arbitrary orientation of the crystal, which facilitates automation. Three-dimensional ED is a powerful technique for structure identification and structure solution from individual nano- or micron-sized particles, while powder X-ray diffraction (PXRD) provides information from all phases present in a sample. ED suffers from dynamic scattering, while PXRD data are kinematic. Three-dimensional ED methods and PXRD are complementary and their combinations are promising for studying multiphase samples and complicated crystal structures. Here, two three-dimensional ED methods, ADT and RED, are described. Examples are given of combinations of three-dimensional ED methods and PXRD for phase identification and structure determination over a large number of different materials, from Ni-Se-O-Cl crystals, zeolites, germanates, metal-organic frameworks and organic compounds to intermetallics with modulated structures. It is shown that three-dimensional ED is now as feasible as X-ray diffraction for phase identification and structure solution, but still needs further development in order to be as accurate as X-ray diffraction. It is expected that three-dimensional ED methods

  7. High Resolution, Non-Dispersive X-Ray Calorimeter Spectrometers on EBITs and Orbiting Observatories

    Science.gov (United States)

    Porter, Frederick S.

    2010-01-01

    X-ray spectroscopy is the primary tool for performing atomic physics with Electron beam ion trap (EBITs). X-ray instruments have generally fallen into two general categories, 1) dispersive instruments with very high spectral resolving powers but limited spectral range, limited count rates, and require an entrance slit, generally, for EBITs, defined by the electron beam itself, and 2) non-dispersive solid-state detectors with much lower spectral resolving powers but that have a broad dynamic range, high count rate ability and do not require a slit. Both of these approaches have compromises that limit the type and efficiency of measurements that can be performed. In 1984 NASA initiated a program to produce a non-dispersive instrument with high spectral resolving power for x-ray astrophysics based on the cryogenic x-ray calorimeter. This program produced the XRS non-dispersive spectrometers on the Astro-E, Astro-E2 (Suzaku) orbiting observatories, the SXS instrument on the Astro-H observatory, and the planned XMS instrument on the International X-ray Observatory. Complimenting these spaceflight programs, a permanent high-resolution x-ray calorimeter spectrometer, the XRS/EBIT, was installed on the LLNL EBIT in 2000. This unique instrument was upgraded to a spectral resolving power of 1000 at 6 keV in 2003 and replaced by a nearly autonomous production-class spectrometer, the EBIT Calorimeter Spectrometer (ECS), in 2007. The ECS spectrometer has a simultaneous bandpass from 0.07 to over 100 keV with a spectral resolving power of 1300 at 6 keV with unit quantum efficiency, and 1900 at 60 keV with a quantum efficiency of 30%. X-ray calorimeters are event based, single photon spectrometers with event time tagging to better than 10 us. We are currently developing a follow-on instrument based on a newer generation of x-ray calorimeters with a spectral resolving power of 3000 at 6 keV, and improved timing and measurement cadence. The unique capabilities of the x-ray

  8. Thermoluminescent dosemeter in a X-ray diffractometer

    International Nuclear Information System (INIS)

    Mendoza A, D.; Gonzalez M, P.; Falcon B, T.; Castano, V.M.

    1999-01-01

    In this work it was presented the results obtained of the dosimetry which was realized in a X-ray diffractometer for powders, trademark Siemens D5000, using the thermoluminescent signal generated by the X-rays in the commercial dosemeter TLD-100 of Harshaw, US. In according to the results obtained, the radiation quantity received by an analysed material in the diffractometer, will be proportional to exposure time and it can vary from unities until tenths of grays. These results are very outstanding when are analysed crystalline materials in a diffractometer, for knowing the present crystalline phases, mainly if these are highly sensitive to the ionizing radiation, as it is the case of the thermoluminescent materials. (Author)

  9. Validation of powder X-ray diffraction following EN ISO/IEC 17025.

    Science.gov (United States)

    Eckardt, Regina; Krupicka, Erik; Hofmeister, Wolfgang

    2012-05-01

    Powder X-ray diffraction (PXRD) is used widely in forensic science laboratories with the main focus of qualitative phase identification. Little is found in literature referring to the topic of validation of PXRD in the field of forensic sciences. According to EN ISO/IEC 17025, the method has to be tested for several parameters. Trueness, specificity, and selectivity of PXRD were tested using certified reference materials or a combination thereof. All three tested parameters showed the secure performance of the method. Sample preparation errors were simulated to evaluate the robustness of the method. These errors were either easily detected by the operator or nonsignificant for phase identification. In case of the detection limit, a statistical evaluation of the signal-to-noise ratio showed that a peak criterion of three sigma is inadequate and recommendations for a more realistic peak criterion are given. Finally, the results of an international proficiency test showed the secure performance of PXRD. © 2012 American Academy of Forensic Sciences.

  10. X-ray Powder Diffraction for Characterization of Raw Materials in Banknotes.

    Science.gov (United States)

    Marabello, Domenica; Benzi, Paola; Lombardozzi, Antonietta; Strano, Morela

    2017-07-01

    We report about the X-ray powder diffraction characterization of crystalline materials used to produce genuine and counterfeit banknotes, performed with a single-crystal diffractometer that permits fast and nondestructive measurements in different 0.5-mm sized areas; 20-euro denomination genuine banknotes were analyzed, and results were compared with counterfeit banknotes. The analysis shows that the papers used to print real banknotes are composed, as expected, of cotton-based cellulose and titanium dioxide as crystalline additive, but different polymorphs of TiO 2 for different emission countries are evidenced. The counterfeit banknotes are composed of cellulose based on wood pulp; moreover, an unexpected significant quantity of TiO 2 was found to be mixed with calcite, indicating that the paper employed by forgers is not simply a common low-cost type. The crystalline index and intensity ratios between the peaks attributable to cellulose and fillers can provide additional information to trace back paper suppliers for forensic purposes. © 2017 American Academy of Forensic Sciences.

  11. Simulation and evaluation of the absorption edge subtraction technique in energy-resolved X-ray radiography applied to the cultural heritage studies

    International Nuclear Information System (INIS)

    Leyva Pernia, Diana; Cabal Rodriguez, Ana E.; Pinnera Hernandez, Ibrahin; Leyva Fabelo, Antonio; Abreu Alfonso, Yamiel; Espen, Piet Van

    2011-01-01

    In this work the mathematical simulation of photon transport in the matter was used to evaluate the potentials of a new energy-resolved X-ray radiography system. The system is intended for investigations of cultural heritage object, mainly painting. The radiographic system uses polychromatic radiation from an X-ray tube and measures the spectrum transmitted through the object with an energy-dispersive X-ray detector on a pixel-by-pixel basis. Manipulation of the data-set obtained allows constructing images with enhanced contrast for certain elements. Here the use of the absorption edge subtraction technique was emphasized. The simulated results were in good agreement with the experimental data.(author)

  12. X-ray polarimetry with a conventional gas proportional counter through rise-time analysis

    CERN Document Server

    Hayashida, K; Tsunemi, H; Torii, K; Murakami, H; Ohno, Y; Tamura, K

    1999-01-01

    We have performed an experiment on the signal rise time of a Xe gas proportional counter using a polarized X-ray beam of synchrotron orbital radiation with energies from 10 to 40 keV. When the counter anode is perpendicular to the electric vector of the incident X-ray photons, the average rise time becomes significantly longer than that for the parallel case. This indicates that the conventional gas proportional counters are useful for X-ray polarimetry. The moderate modulation contrast of this rise-time polarimeter (M=0.1 for 10 keV X-rays and M=0.35 for 40 keV X-rays), with capability of the simultaneous measuring X-ray energies and the timing, would be useful for applications in X-ray astronomy and in other fields.

  13. A Chandra High-Resolution X-ray Image of Centaurus A.

    Science.gov (United States)

    Kraft; Forman; Jones; Kenter; Murray; Aldcroft; Elvis; Evans; Fabbiano; Isobe; Jerius; Karovska; Kim; Prestwich; Primini; Schwartz; Schreier; Vikhlinin

    2000-03-01

    We present first results from a Chandra X-Ray Observatory observation of the radio galaxy Centaurus A with the High-Resolution Camera. All previously reported major sources of X-ray emission including the bright nucleus, the jet, individual point sources, and diffuse emission are resolved or detected. The spatial resolution of this observation is better than 1&arcsec; in the center of the field of view and allows us to resolve X-ray features of this galaxy not previously seen. In particular, we resolve individual knots of emission in the inner jet and diffuse emission between the knots. All of the knots are diffuse at the 1&arcsec; level, and several exhibit complex spatial structure. We find the nucleus to be extended by a few tenths of an arcsecond. Our image also suggests the presence of an X-ray counterjet. Weak X-ray emission from the southwest radio lobe is also seen, and we detect 63 pointlike galactic sources (probably X-ray binaries and supernova remnants) above a luminosity limit of approximately 1.7x1037 ergs s-1.

  14. A program for the derivation of crystal unit cell parameters from X-ray powder diffraction measurements

    International Nuclear Information System (INIS)

    Ferguson, I.F.; Rogerson, A.H.

    1984-01-01

    The program, FIRESTAR, determines the dimensions of a crystallographic unit cell from a set of X-ray powder diffraction measurements corresponding to a set of Bragg reflections, provided that the crystal system applicable is known and the Bragg reflections have been indexed. The program includes a range of possible extrapolation functions, and the data may be weighted. Provision is made for detecting and rejecting a single 'bad' measurement, and then rejecting measurements which lie outside an error limit set in the input data. (orig.)

  15. Fourier techniques in X-ray timing

    NARCIS (Netherlands)

    van der Klis, M.

    1988-01-01

    Basic principles of Fourier techniques often used in X-ray time series analysis are reviewed. The relation between the discrete Fourier transform and the continuous Fourier transform is discussed to introduce the concepts of windowing and aliasing. The relation is derived between the power spectrum

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

    Directory of Open Access Journals (Sweden)

    Trache D.

    2013-07-01

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

  17. A time resolved microfocus XEOL facility at the Diamond Light Source

    International Nuclear Information System (INIS)

    Mosselmans, J F W; Taylor, R P; Quinn, P D; Cibin, G; Gianolio, D; Finch, A A; Sapelkin, A V

    2013-01-01

    We have constructed a Time-Resolved X-ray Excited Optical Luminescence (TR-XEOL) detection system at the Microfocus Spectroscopy beamline I18 at the Diamond Light Source. Using the synchrotron in h ybrid bunch mode , the data collection is triggered by the RF clock, and we are able to record XEOL photons with a time resolution of 6.1 ps during the 230 ns gap between the hybrid bunch and the main train of electron bunches. We can detect photons over the range 180-850 nm using a bespoke optical fibre, with X-ray excitation energies between 2 and 20 keV. We have used the system to study a range of feldspars. The detector is portable and has also been used on beamline B18 to collect Optically Determined X-ray Absorption Spectroscopy (OD-XAS) in QEXAFS mode.

  18. A time resolved microfocus XEOL facility at the Diamond Light Source

    Science.gov (United States)

    Mosselmans, J. F. W.; Taylor, R. P.; Quinn, P. D.; Finch, A. A.; Cibin, G.; Gianolio, D.; Sapelkin, A. V.

    2013-03-01

    We have constructed a Time-Resolved X-ray Excited Optical Luminescence (TR-XEOL) detection system at the Microfocus Spectroscopy beamline I18 at the Diamond Light Source. Using the synchrotron in "hybrid bunch mode", the data collection is triggered by the RF clock, and we are able to record XEOL photons with a time resolution of 6.1 ps during the 230 ns gap between the hybrid bunch and the main train of electron bunches. We can detect photons over the range 180-850 nm using a bespoke optical fibre, with X-ray excitation energies between 2 and 20 keV. We have used the system to study a range of feldspars. The detector is portable and has also been used on beamline B18 to collect Optically Determined X-ray Absorption Spectroscopy (OD-XAS) in QEXAFS mode.

  19. Noise reduction in real time x-ray images

    International Nuclear Information System (INIS)

    Tsuda, Motohisa; Kimura, Yutaro

    1986-01-01

    The signal-to-noise ratio of real-time digital X-ray imaging systems consisting of an X-ray image intensifer-television chain was investigated while concentrating on the effect of the X-ray quantum nature. Along with conventional signal accumulation, logarithmic conversion and subtraction, a new technique called the peak hold method is introduced. Theoretical and simulational studies were made with practical parameters. Theory and simulation showed good agreement. An accumulation of signal is most effective for improving the signal-to-noise ratio; the peak-hold method comes next. The peak hold method, however, offers a new image-display mode. Moreover, this method is superior to signal accumulation for specific conditions. (author)

  20. Comparing neutron and X-ray images from NIF implosions

    Directory of Open Access Journals (Sweden)

    Wilson D.C.

    2013-11-01

    Full Text Available Directly laser driven and X-radiation driven DT filled capsules differ in the relationship between neutron and X-ray images. Shot N110217, a directly driven DT-filled glass micro-balloon provided the first neutron images at the National Ignition Facility. As seen in implosions on the Omega laser, the neutron image can be enclosed inside time integrated X-ray images. HYDRA simulations show the X-ray image is dominated by emission from the hot glass shell while the neutron image arises from the DT fuel it encloses. In the absence of mix or jetting, X-ray images of a cryogenically layered THD fuel capsule should be dominated by emission from the hydrogen rather than the cooler plastic shell that is separated from the hot core by cold DT fuel. This cool, dense DT, invisible in X-ray emission, shows itself by scattering hot core neutrons. Germanium X-ray emission spectra and Ross pair filtered X-ray energy resolved images suggest that germanium doped plastic emits in the torus shaped hot spot, probably reducing the neutron yield.

  1. Time-dependent nonequilibrium soft x-ray response during a spin crossover

    Science.gov (United States)

    van Veenendaal, Michel

    2018-03-01

    A theoretical framework is developed for better understanding the time-dependent soft-x-ray response of dissipative quantum many-body systems. It is shown how x-ray absorption and resonant inelastic x-ray scattering (RIXS) at transition-metal L edges can provide insight into ultrafast intersystem crossings of importance for energy conversion, ultrafast magnetism, and catalysis. The photoinduced doublet-to-quartet spin crossover on cobalt in Fe-Co Prussian blue analogs is used as a model system to demonstrate how the x-ray response is affected by the nonequilibrium dynamics on a femtosecond time scale. Changes in local spin and symmetry and the underlying mechanism are reflected in strong broadenings, a collapse of clear selection rules during the intersystem crossing, fluctuations in the isotropic branching ratio in x-ray absorption, crystal-field collapse and/or oscillations, and time-dependent anti-Stokes processes in RIXS.

  2. Resolving the Origin of the Diffuse Soft X-ray Background

    Science.gov (United States)

    Smith, Randall K.; Foster, Adam R.; Edgar, Ricard J.; Brickhouse, Nancy S.; Sanders, Wilton T.

    2012-01-01

    In January 1993, the Diffuse X-ray Spectrometer (DXS) measured the first high-resolution spectrum of the diffuse soft X-ray background between 44-80A. A line-dominated spectrum characteristic of a 10(exp 6)K collisionally ionized plasma' was expected but while the observed spectrum was clearly line-dominated, no model would fit. Then in 2003 the Cosmic Hot Interstellar Plasma Spectrometer (CHIPS) launched and observed the diffuse extreme-ultraviolet (EUV) spectrum between 90- 265A. Although many emission lines were again expected; only Fe IX at 171.1A was detected. The discovery of X-rays from comets led to the realization that heavy ions (Z=6-28) in the solar wind will emit soft X-rays as the ions interact via charge exchange with neutral atoms in the heliosphere and geocorona. Using a new model for solar wind charge exchange (SWCX) emission, we show that the diffuse soft X-ray background can be understood as a combination of emission from charge exchange onto the slow and fast solar wind together with a more distant and diffuse hot (10(exp 6)K) plasma.

  3. Functional coordination polymers and MOFs from reactions of the lanthanides and barium with azole ligands. Synthesis and characterization with a focus on structure determination from X-ray powder diffraction data

    International Nuclear Information System (INIS)

    Rybak, Jens-Christoph

    2012-01-01

    This thesis deals with the synthesis and characterization of coordination polymers and MOFs of the lanthanides and barium with different azolic N-heterocycles. A total of 18 new organic-inorganic hybrid materials, as well as a series of co-doped compounds is presented. Besides the structural characterization of these materials from X-ray diffraction powder data, the focus of the investigations is on the thermal and photoluminescence spectroscopic properties. The lanthanides La - Lu, except Eu and Pm, can be reacted with 1H-1,2,3-triazole to give the series of the isotypic dense 3D-MOFs 3 ∞ [Ln(Tz * ) 3 ]. Investigation of the photoluminescence properties of these compounds reveals a broad range of different luminescence phenomena, including the first observation of an intrinsic inner-filter effect of the Ln 3+ -ions. The structure of this isotypic series of compounds was solved and refined from X-ray powder diffraction data. A 2D-polymorph of these compounds 2 ∞ [Ln(Tz * ) 3 ], is observed for Ln = Sm, Tb and was characterized by single crystal data. The reaction of Eu with 1H-benzotriazole yields the 1D-coordination polymer 1 ∞ [Eu(Btz) 2 (BtzH) 2 ], which is the first example of a divalent rare earth benzotriazolate. Analysis of the thermal properties reveals the transformation to the 3D-MOF 3 ∞ [Eu(Btz) 2 ] at higher temperatures. The structure of this material was also solved from X-ray powder diffraction data. Investigation of the photoluminescence properties of the co-doped compounds 3 ∞ [Ba 1-x Eu x (Im) 2 ], which were obtained from reaction of the salt-like hydrides BaH 2 and EuH 2 with imidazole, show that the synthesis of luminescent MOF materials by co-doping of non-luminescent networks with luminescence centers is possible. The structure of these materials was solved from X-ray powder diffraction data of the undoped compound 3 ∞ [BaEu(Im) 2 ]. Structural characterization of materials from X-ray powder diffraction data is an important aspect

  4. Ultrafast X-Ray Spectroscopy of Conical Intersections

    Science.gov (United States)

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

    2018-06-01

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

  5. Magnetic x-ray microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Evans, Paul G [Computer-Aided Engineering Center, University of Wisconsin, Madison, WI 53706 (United States); Isaacs, Eric D [Center for Nanoscale Materials, Argonne National Laboratory, Argonne, IL 60439 (United States)

    2006-08-07

    Magnetic x-ray microdiffraction uses the structural specificity of x-ray diffraction to probe complex magnetic structures at the length scales relevant to physical phenomena including domain dynamics and phase transitions. Conventional magnetic crystallography techniques such as neutron or x-ray diffraction lack this spatial resolution. The combination of both reciprocal space and real space resolution with a rich magnetic cross section allows new microscopy techniques to be developed and applied to magnetism at the scale of single domains. Potential applications include a wide range of magnetic problems in nanomagnetism, the interaction of strain, polarization and magnetization in complex oxides and spatially resolved studies of magnetic phase transitions. We present the physical basis for x-ray microdiffraction and magnetic scattering processes, review microdiffraction domain imaging techniques in antiferromagnetic and ferromagnetic materials and discuss potential directions for studies. (topical review)

  6. X-ray chemical analyzer for field applications

    International Nuclear Information System (INIS)

    Gamba, O.O.M.

    1977-01-01

    A self-supporting portable field multichannel x-ray chemical analyzer system is claimed. It comprises a lightweight, flexibly connected, remotely locatable, radioisotope-excited sensing probe utilizing a cryogenically-cooled solid state semi-conductor crystal detector for fast in situ non-destructive, qualitative and quantitative analysis of elements in solid, powder, liquid or slurried form, utilizing an x-ray energy dispersive spectrometry technique

  7. Development of X-ray and ion diagnostic methods for plasma focus research

    International Nuclear Information System (INIS)

    Sadowski, M.

    1986-12-01

    A review of experimental methods used for investigation of X-rays and ion-beams emmited from plasma focus facilities is presented. The research program has been realized at the Institute for Nuclear Studies in Swierk and at the Institut fuer Plasmaforschung in Stuttgart, within the frames of an international co-operation. The studies on ion emission from different PF facilities are reviewed. The application of CN-films with Al-filters and of different ion-pinhole cameras is described. The use of a Thomson mass-spectrometer adopted for plasma studies is presented. The time-resolved measurements combined with a simultaneous mass- and energy-analysis of the ion beams are also described. The most important results of these studies are summarized. Particular attention is also paid to the studies of the X-ray emission. The use of stereoscopic sets of vacuum pinhole cameras with thin Be-filters is described. The application of X-ray pinhole cameras equipped with miniature scintillators for time-resolved measurements is also presented. The most important results of the X-ray emission studies are summarized. 35 refs., 12 figs. (author)

  8. Time-resolved magnetic field effects in exciplex systems under X-irradiation

    International Nuclear Information System (INIS)

    Anishchik, S.V.; Lavrik, N.L.

    1988-01-01

    The presence of exciplex systems after X-irradiation of pyrene and N,N-diethylaniline in methanol as well as the influence of the applied magnetic field on exciplex fluorescence was registered using a time-resolving method. The experimental results confirmed the hypothesis on exciplex emergence in the system under study. (author)

  9. Syntheses and crystal structure determination by X-ray powder diffraction of new compounds of Benzovesamicol

    International Nuclear Information System (INIS)

    Rukiah, M.; Assaad, Th.

    2012-06-01

    The compound 2,2,2-Trifluoro-N-(1a,2,7,7 a-tetra-hydronaphtho[2,3-b]oxiren-3-yl)- acetamide, C 1 2H 1 0F 3 NO 2 , an important precursor in the preparation of benzovesamicol analogues for the diagnosis of Alzheimers disease, was prepared by the epoxidation of 5,8-dihydronaphthalene-1-amine using 3-chloroperoxybenzoic acid. The structure was determined by X-ray powder diffraction, multinuclear NMR spectroscopy and FT-IR spectroscopy. A pair of molecules form intermolecular N- H...O hydrogen bonds, involving the amino and oxirene groups, to produce a dimer.The two racemic compounds (2RS,3RS)-5-amino-3-(4-phenylpiperazin-1-yl)-1,2,3,4 tetrahydronaphthalene-2-ol, C 2 0H 2 5N 3 O, (I) and (2RS,3RS)-5-amino-3-[4-(3- methoxyphenyl)piperazin-1-yl]-1,2,3,4-tetrahydronaphthalene-2-ol, C 2 1H 2 7N 3 O 2 , (II) important benzovesamicol analogues for the diagnosis of Alzheimer's disease, have been synthesized and characterized by FT-IR, and 1 H and 13 C NMR spectroscopic analyses. The crystal structures were analyses using powder diffraction as no suitable single crystal were obtained. The two compounds are racemic mixtures of enantiomers which crystallize in the monoclinic system in a centrosymmetric space group (P21/c). Crystallography, in particular powder X-ray diffraction, was pivotal in revealing that the enantio-resolution did not succeed. In two compounds, the piperazine ring has a chair conformation, while the cyclohexene ring assumes a half-chair conformation. In (I) the crystal packing is mediated by weak contacts, principally by complementary intermolecular N--H...O hydrogen bonds that connect successive molecules into a chain. Further stabilization is provided by weak C--H...N contacts and by a weak intermolecular C--H...π interaction. While in (II), the crystal packing is dominated by intermolecular O--H...N hydrogen bonding which links molecules along the c direction. (authors)

  10. Quantitative determination of mineral composition by powder X-ray diffraction

    International Nuclear Information System (INIS)

    Pawloski, G.A.

    1986-01-01

    A method is described of quantitatively determining the mineral composition in a test sample containing a number (m) of minerals from a group (n) of known minerals, wherein n=13, where mless than or equal ton, by x-ray diffraction, comprising: determining from standard samples of the known minerals a set of (n) standard coefficients K/sub j/=(X/sub j//X/sub l/)(I/sub l//I/sub j/) for each mineral (j=2...n) in the group of known minerals (j=2...n) relative to one mineral (l) in the group selected as a reference mineral, where X is the weight fraction of the mineral in a standard sample, and I is the x-ray integrated intensity peak of each mineral obtained from the standard sample; obtaining an x-ray diffraction pattern of the test sample; identifying each of the (m) minerals in the test sample for the x-ray diffraction pattern; calculating the relative weight fractions X/sub j//X/sub l/ for each mineral (j=2...m) compared to the reference mineral (l) from the ratio of the measured highest integrated intensity peak I/sub j/ of each mineral in the test sample to the measured highest integrated intensity peak I/sub l/ of the reference mineral in the test sample, and from the previously determined standard coefficients, X/sub j//X/sub l/=K/sub j/(I/sub j//I/sub l/

  11. An experimental measurement of metal multilayer x-ray reflectivity degradation due to intense x-ray flux

    International Nuclear Information System (INIS)

    Hockaday, M.Y.P.

    1987-06-01

    The degradation of the x-ray reflection characteristics of metal multilayer Bragg diffractors due to intense x-ray flux was investigated. The Z-pinch plasma produced by PROTO II of Sandia National Laboratories, Albuquerque, New Mexico, was used as the source. The plasma generated total x-ray yields of as much as 40 kJ with up to 15 kJ in the neon hydrogen- and helium-like resonance lines in nominal 20-ns pulses. Molybdenum-carbon, palladium-carbon, and tungsten-carbon metal multilayers were placed at 15 and 150 cm from the plasma center. The multilayers were at nominal angles of 5 0 and 10 0 to diffract the neon resonance lines. The time-integrated x-ray reflection of the metal multilayers was monitored by x-ray film. A fluorescer-fiber optic-visible streak camera detector system was then used to monitor the time-resolved x-ray reflection characteristics of 135 A- 2d tungsten-carbon multilayers. A large specular component in the reflectivity prevented determination of the rocking curve of the multilayer. For a neon implosion onto a vanadium-doped polyacrylic acid foam target shot, detailed modeling was attempted. The spectral flux was determined with data from 5 XRD channels and deconvolved using the code SHAZAM. The observed decay in reflectivity was assumed to correspond to the melting of the first tungsten layer. A ''conduction factor'' of 82 was required to manipulate the heat loading of the first tungsten layer such that the time of melting corresponded to the observed decay. The power at destruction was 141 MW/cm 2 and the integrated energy at destruction was 2.0 J/cm 2 . 82 refs., 66 figs., 10 tabs

  12. Kinetics and mechanism of the pressure-induced lamellar order/disorder transition in phosphatidylethanolamine: a time-resolved X-ray diffraction study.

    Science.gov (United States)

    Mencke, A P; Caffrey, M

    1991-03-05

    By using synchrotron radiation, a movie was made of the X-ray scattering pattern from a biological liquid crystal undergoing a phase transition induced by a pressure jump. The system studied includes the fully hydrated phospholipid dihexadecylphosphatidylethanolamine in the lamellar gel (L beta') phase at a temperature of 68 degrees C and a pressure of 9.7 MPa (1400 psig). Following the rapid release of pressure to atmospheric the L beta' phase transforms slowly into the lamellar liquid crystal (L alpha) phase. The pressure perturbation is applied with the intention of producing a sudden phase disequilibrium followed by monitoring the system as it relaxes to its new equilibrium condition. Remarkably, the proportion of sample in the L alpha phase grows linearly with time, taking 37 s to totally consume the L beta' phase. The time dependencies of radius, peak intensity, and width of the powder diffraction ring of the low-angle (001) lamellar reflections were obtained from the movie by image processing. The concept of an "effective pressure" is introduced to account for the temperature variations that accompany the phase transition and to establish that the observed large transit time is indeed intrinsic to the sample and not due to heat exchange with the environment. The reverse transformation, L alpha to L beta', induced by a sudden jump from atmospheric pressure to 9.7 MPa, is complete in less than 13 s. These measurements represent a new approach for studying the kinetics of lipid phase transitions and for gaining insights into the mechanism of the lamellar order/disorder transition.

  13. Structure and function of proteins investigated by crystallographic and spectroscopic time-resolved methods

    Science.gov (United States)

    Purwar, Namrta

    Biomolecules play an essential role in performing the necessary functions for life. The goal of this thesis is to contribute to an understanding of how biological systems work on the molecular level. We used two biological systems, beef liver catalase (BLC) and photoactive yellow protein (PYP). BLC is a metalloprotein that protects living cells from the harmful effects of reactive oxygen species by converting H2O2 into water and oxygen. By binding nitric oxide (NO) to the catalase, a complex was generated that mimics the Cat-H2O2 adduct, a crucial intermediate in the reaction promoted by the catalase. The Cat-NO complex is obtained by using a convenient NO generator (1-(N,N-diethylamino)diazen-1-ium-1,2-diolate). Concentrations up to 100˜200 mM are reached by using a specially designed glass cavity. With this glass apparatus and DEANO, sufficient NO occupation is achieved and structure determination of the catalase with NO bound to the heme iron becomes possible. Structural changes upon NO binding are minute. NO has a slightly bent geometry with respect to the heme normal, which results in a substantial overlap of the NO orbitals with the iron-porphyrin molecular orbitals. From the structure of the iron-NO complex, conclusions on the electronic properties of the heme iron can be drawn that ultimately lead to an insight into the catalytic properties of this enzyme. Enzyme kinetics is affected by additional parameters such as temperature and pH. Additionally, in crystallography, the absorbed X-ray dose may impair protein function. To address the effect of these parameters, we performed time-resolved crystallographic experiments on a model system, PYP. By collecting multiple time-series on PYP at increasing X-ray dose levels, we determined a kinetic dose limit up to which kinetically meaningful X-ray data sets can be collected. From this, we conclude that comprehensive time-series spanning up to 12 orders of magnitude in time can be collected from a single PYP

  14. The LOFT perspective on neutron star thermonuclear bursts: White paper in support of the mission concept of the large observatory for X-ray timing

    Energy Technology Data Exchange (ETDEWEB)

    in' t Zand, J. J.M. [SRON Netherlands Institute for Space Research, Utrecht (The Netherlands); Malone, Christopher M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Altamirano, D. [Univ. of Southampton, Southampton (United Kingdom); Ballantyne, D. R. [Georgia Inst. of Technology, Atlanta, GA (United States); Bhattacharyya, S. [Tata Institute of Fundamental Research, Mumbai (India); Brown, E. F. [Michigan State Univ., East Lansing, MI (United States); Cavecchi, Y. [Univ. of Amsterdam, Amsterdam (The Netherlands); Chakrabarty, D. [Massachusetts Inst. of Technology (MIT), Cambridge, MA (United States); Chenevez, J. [Technical Univ. of Denmark, Lyngby (Denmark); Cumming, A. [McGill Univ., Montreal, QC (Canada); Degenaar, N. [Univ. of Cambridge, Cambridge (United Kingdom); Falanga, M. [International Space Science Institute, Bern (Switzerland); Galloway, D. K. [Monash Univ., VIC (Australia); Heger, A. [Monash Univ., VIC (Australia); Jose, J. [Univ. Politecnica de Catalunya, Barcelona (Spain); Institut d' Estudis Espacials de Catalunya, Barcelona (Spain); Keek, L. [Georgia Institute of Technology, Atlanta, GA (United States); Linares, M. [Univ. de La Laguna, Tenerife (Spain); Mahmoodifar, S. [Univ. of Maryland, College Park, MD (United States); Mendez, M. [Univ. of Groningen, Groningen (The Netherlands); Miller, M. C. [Univ. of Maryland, College Park, MD (United States); Paerels, F. B. S. [Columbia Astrophysics Lab., New York, NY (United States); Poutanen, J. [Univ. of Turku, Piikkio (Finland); Rozanska, A. [N. Copernicus Astronomical Center PAS, Warsaw (Poland); Schatz, H. [National Superconducting Cyclotron Laboratory at Michigan State University; Serino, M. [Institute of Physical and Chemical Research (RIKEN); Strohmayer, T. E. [NASA' s Goddard Space Flight Center, Greenbelt, MD (United States); Suleimanov, V. F. [Univ. Tubingen, Tubingen (Germany); Thielemann, F. -K. [Univ. Basel, Basel (Switzerland); Watts, A. L. [Univ. of Amsterdam, Amsterdam (The Netherlands); Weinberg, N. N. [Massachusetts Institute of Technology, Cambridge, MA (United States); Woosley, S. E. [Univ. of California, Santa Cruz, CA (United States); Yu, W. [Chinese Academy of Sciences (CAS), Shanghai (China); Zhang, S. [Institute of High-Energy Physics, Beijing (China); Zingale, M. [Stony Brook Univ., Stony Brook, NY (United States)

    2015-01-14

    The Large Area Detector (LAD) on the Large Observatory For X-ray Timing ( LOFT ), with a 8.5 m 2 photon- collecting area in the 2–30 keV bandpass at CCD-class spectral resolving power (λ/Δλ = 10 – 100), is designed for optimum performance on bright X-ray sources. Thus, it is well-suited to study thermonuclear X-ray bursts from Galactic neutron stars. These bursts will typically yield 2 x 105 photon detections per second in the LAD, which is at least 15 times more than with any other instrument past, current or anticipated. The Wide Field Monitor (WFM) foreseen for LOFT uniquely combines 2–50 keV imaging with large (30%) prompt sky coverage. This will enable the detection of tens of thousands of thermonuclear X-ray bursts during a 3-yr mission, including tens of superbursts. Both numbers are similar or more than the current database gathered in 50 years of X-ray astronomy.

  15. Solar and Stellar X-ray Cycles

    Science.gov (United States)

    Martens, P. C. H.; SADE Team

    2004-05-01

    Stern et al. have shown that Yohkoh-SXT full disk X-ray irradiance shows an 11 year cycle with an max/min amplitude ratio of a factor 30. Similar cyclic X-ray variation in Sun-like stars observed by ROSAT and its predecessors is observed in only a few cases and limited to a factor two or three. We will show, by means of detailed bandpass comparisons, that this discrepancy cannot be ascribed to the differences in energy response between SXT and the stellar soft X-ray detectors. Is the Sun exceptional? After centuries of geocentric and heliocentric worldviews we find this a difficult proposition to entertain. But perhaps the Sun is a member of a small class of late-type stars with large amplitudes in their X-ray cycles. The stellar X-ray observations listed in the HEASARC catalog are too sparse to verify this hypothesis. To resolve these and related questions we have proposed a small low-cost stellar X-ray spectroscopic imager originally called SADE to obtain regular time series from late and early-type stars and accretion disks. This instrument is complimentary to the much more advanced Chandra and XMM-Newton observatories, and allows them to focus on those sources that require their full spatial and spectral resolution. We will describe the basic design and spectroscopic capability of SADE and show it meets the mission requirements.

  16. Homogeneity characterisation of (U,Gd)O2 sintered pellets by X-ray diffraction powder analysis applying Rietveld method

    International Nuclear Information System (INIS)

    Leyva, Ana G.; Vega, Daniel R.; Trimarco, Veronica G.; Marchi, Daniel E.

    1999-01-01

    The (U,Gd)O 2 sintered pellets are fabricated by different methods. The homogeneity characterisation of Gd content seems to be necessary as a production control to qualify the process and the final product. The micrographic technique is the most common method used to analyse the homogeneity of these samples, this method requires time and expertise to obtain good results. In this paper, we propose an analysis of the X-ray diffraction powder patterns through the Rietveld method, in which the differences between the experimental data and the calculated from a crystalline structure model proposed are evaluated. This result allows to determine the cell parameters, that can be correlated with the Gd concentration, and the existence of other phases with different Gd ratio. (author)

  17. Investigation on diagnostic techniques of X-ray radiation characteristic from slit target

    International Nuclear Information System (INIS)

    Cheng Jinxiu; Miao Wenyong; Sun Kexu; Wang Hongbin; Cao Leifeng; Yang Jiamin; Chen Zhenglin

    2001-01-01

    On the Xingguang-II facility, X-ray transport process in a cavity target was simulated in a long cylindrical cavity with slits. High temporally and spatially resolved Microchannel Plate (MCP) gated X-ray picosecond frame camera and soft X-ray steak camera were used to investigate the temporal and spatial distribution of the soft X-ray emitted from the cavity wall through the slit. X-ray transport velocity, X-ray emission time and amount of intensity decay was obtained. X-ray CCD pinhole transmission grating spectrometer was used to investigate the spectrum change of the emitted X-ray versus its location. The change characteristic of the spectrum of X-ray absorbed and emitted again and again in transport was obtained. X-ray diodes and Dante spectrometer were used to measure X-ray flux and radiation temperature in the slit, the source and the transport end, respectively. The typical results in the experiment were given. A brief and essential analysis and discussion were made

  18. X-RAY PULSATIONS FROM THE RADIO-QUIET GAMMA-RAY PULSAR IN CTA 1

    International Nuclear Information System (INIS)

    Caraveo, P. A.; De Luca, A.; Marelli, M.; Bignami, G. F.; Ray, P. S.; Saz Parkinson, P. M.; Kanbach, G.

    2010-01-01

    Prompted by the Fermi-LAT discovery of a radio-quiet gamma-ray pulsar inside the CTA 1 supernova remnant, we obtained a 130 ks XMM-Newton observation to assess the timing behavior of this pulsar. Exploiting both the unprecedented photon harvest and the contemporary Fermi-LAT timing measurements, a 4.7σ single-peak pulsation is detected, making PSR J0007+7303 the second example, after Geminga, of a radio-quiet gamma-ray pulsar also seen to pulsate in X-rays. Phase-resolved spectroscopy shows that the off-pulse portion of the light curve is dominated by a power-law, non-thermal spectrum, while the X-ray peak emission appears to be mainly of thermal origin, probably from a polar cap heated by magnetospheric return currents, pointing to a hot spot varying throughout the pulsar rotation.

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

    NARCIS (Netherlands)

    Groot, F.M.F. de

    2000-01-01

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

  20. Time dependence of X-ray polarizability of a crystal induced by an intense femtosecond X-ray pulse

    Directory of Open Access Journals (Sweden)

    A. Leonov

    2014-11-01

    Full Text Available The time evolution of the electron density and the resulting time dependence of Fourier components of the X-ray polarizability of a crystal irradiated by highly intense femtosecond pulses of an X-ray free-electron laser (XFEL is investigated theoretically on the basis of rate equations for bound electrons and the Boltzmann equation for the kinetics of the unbound electron gas. The photoionization, Auger process, electron-impact ionization, electron–electron scattering and three-body recombination have been implemented in the system of rate equations. An algorithm for the numerical solution of the rate equations was simplified by incorporating analytical expressions for the cross sections of all the electron configurations in ions within the framework of the effective charge model. Using this approach, the time dependence of the inner shell populations during the time of XFEL pulse propagation through the crystal was evaluated for photon energies between 4 and 12 keV and a pulse width of 40 fs considering a flux of 1012 photons pulse−1 (focusing on a spot size of ∼1 µm. This flux corresponds to a fluence ranging between 0.8 and 2.4 mJ µm−2. The time evolution of the X-ray polarizability caused by the change of the atomic scattering factor during the pulse propagation is numerically analyzed for the case of a silicon crystal. The time-integrated polarizability drops dramatically if the fluence of the X-ray pulse exceeds 1.6 mJ µm−2.

  1. Applications of pixellated GaAs X-ray detectors in a synchrotron radiation beam

    CERN Document Server

    Watt, J; Campbell, M; Mathieson, K; Mikulec, B; O'Shea, V; Passmore, M S; Schwarz, C; Smith, K M; Whitehill, C

    2001-01-01

    Hybrid semiconductor pixel detectors are being investigated as imaging devices for radiography and synchrotron radiation beam applications. Based on previous work in the CERN RD19 and the UK IMPACT collaborations, a photon counting GaAs pixel detector (PCD) has been used in an X-ray powder diffraction experiment. The device consists of a 200 mu m thick SI-LEC GaAs detector patterned in a 64*64 array of 170 mu m pitch square pixels, bump-bonded to readout electronics operating in single photon counting mode. Intensity peaks in the powder diffraction pattern of KNbO/sub 3/ have been resolved and compared with results using the standard scintillator, and a PCD predecessor (the Omega 3). The PCD shows improved speed, dynamic range, 2-D information and comparable spatial resolution to the standard scintillator based systems. It also overcomes the severe dead time limitations of the Omega 3 by using a shutter based acquisition mode. A brief demonstration of the possibilities of the system for dental radiography and...

  2. Powder X-ray diffraction studies of structural and kinetic aspects of polymorphism

    International Nuclear Information System (INIS)

    Chan, F.C.

    1999-01-01

    Polymorphism is a poorly understood phenomenon that is of considerable technological interest to the pharmaceutical industry. The polymorph selected can influence the bioavailability, processing and stability of the pharmaceutical dosage form. In this study structural, kinetic and thermodynamics aspects of polymorphism and polymorphic phase transformations have been examined using powder X-ray diffraction (PXRD). The compound sulphathiazole is a well-studied model in the investigation of polymorphism and crystal growth. There are five known polymorphic forms and the structure of form V was unknown until this study. The difficulty has been that it has not been possibly to prepare crystals of appropriate size and quality for single crystal diffraction. Furthermore, structure solution from powder data for organic molecules is almost impossible. Despite the challenge the structure of sulphathiazole form V have been solved ab initio from powder data using direct methods. With 16 non-hydrogen atoms in the molecule and two molecules in the asymmetric unit, this structure represents a significant advance in terms of the complexity of an organic structure solved from PXRD data. The structural data should be invaluable for rationalizing experimental observations and the development of theoretical ideas regarding polymorphism and crystal growth. The second part of the study, has examined kinetics of polymorphic phase transformations as a function of pressure combined with temperature using real-time synchrotron PXRD. The significance of pressure arises from the fact that phase transitions can be induced in pharmaceuticals during tabletting. The phase transformation behaviour of rubidium iodide (chosen as a simple test model) has been investigated as a function of isobaric pressure at ambient and elevated temperatures. The kinetics have been characterized by using the Johnson-Melil-Avrami equation. The effect of successive cycling across the transition pressure was also

  3. X-ray analysis and mapping by wavelength dispersive X-ray spectroscopy in an electron microscope

    International Nuclear Information System (INIS)

    Tanaka, Miyoko; Takeguchi, Masaki; Furuya, Kazuo

    2008-01-01

    A compact and easy-to-use wavelength dispersive X-ray spectrometer using a multi-capillary X-ray lens attached to a scanning (transmission) electron microscope has been tested for thin-film analysis. B-K spectra from thin-film boron compounds (B 4 C, h-BN, and B 2 O 3 ) samples showed prominent peak shifts and detailed structural differences. Mapping images of a thin W/Si double-layer sample resolved each element clearly. Additionally, a thin SiO 2 film grown on a Si substrate was imaged with O-K X-rays. Energy and spatial resolution of the system is also discussed

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

    Energy Technology Data Exchange (ETDEWEB)

    Seidler, G. T., E-mail: seidler@uw.edu; Mortensen, D. R.; Remesnik, A. J.; Pacold, J. I.; Ball, N. A.; Barry, N.; Styczinski, M.; Hoidn, O. R. [Physics Department, University of Washington, Seattle, Washington 98195-1560 (United States)

    2014-11-15

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

  5. Conformational analysis of an acyclic tetrapeptide: ab-initio structure determination from X-ray powder diffraction, Hirshfeld surface analysis and electronic structure.

    Science.gov (United States)

    Das, Uday; Naskar, Jishu; Mukherjee, Alok Kumar

    2015-12-01

    A terminally protected acyclic tetrapeptide has been synthesized, and the crystal structure of its hydrated form, Boc-Tyr-Aib-Tyr-Ile-OMe·2H2O (1), has been determined directly from powder X-ray diffraction data. The backbone conformation of tetrapeptide (1) exhibiting two consecutive β-turns is stabilized by two 4 → 1 intramolecular N-H · · · O hydrogen bonds. In the crystalline state, the tetrapeptide molecules are assembled through water-mediated O-H · · · O hydrogen bonds to form two-dimensional molecular sheets, which are further linked by intermolecular C-H · · · O hydrogen bonds into a three-dimensional supramolecular framework. The molecular electrostatic potential (MEP) surface of (1) has been used to supplement the crystallographic observations. The nature of intermolecular interactions in (1) has been analyzed quantitatively through the Hirshfeld surface and two-dimensional fingerprint plot. The DFT optimized molecular geometry of (1) agrees closely with that obtained from the X-ray structure analysis. The present structure analysis of Boc-Tyr-Aib-Tyr-Ile-OMe·2H2 O (1) represents a case where ab-initio crystal structure of an acyclic tetrapeptide with considerable molecular flexibility has been accomplished from laboratory X-ray powder diffraction data. Copyright © 2015 European Peptide Society and John Wiley & Sons, Ltd.

  6. Theory and Modelling of Ultrafast X-ray Imaging of Dynamical Non-equilibrium Systems

    DEFF Research Database (Denmark)

    Lorenz, Ulf

    Over the next few years, a new generation of x-ray sources is going online. These freeelectron lasers will provide extremely bright subpicosecond x-ray pulses. Traditionally, x-ray diraction has the advantage of directly determining the atomic positions within a sample. With these new machines......, it becomes feasible to exploit this concept for ultrafast processes; in eect, we can study chemical reactions as they occur. This thesis deals with theoretical aspect of ultrafast time-resolved x-ray diraction (TRXD).We derive general formulas for calculating the diraction signal that are closely related...

  7. Understanding the spectral and timing behaviour of a newly discovered transient X-ray pulsar Swift J0243.6+6124

    Science.gov (United States)

    Jaisawal, Gaurava K.; Naik, Sachindra; Chenevez, Jérôme

    2018-03-01

    We present the results obtained from timing and spectral studies of the newly discovered accreting X-ray binary pulsar Swift J0243.6+6124 using Nuclear Spectroscopy Telescope Array observation in 2017 October at a flux level of ˜280 mCrab. Pulsations at 9.854 23(5) s were detected in the X-ray light curves of the pulsar. Pulse profiles of the pulsar were found to be strongly energy dependent. A broad profile at lower energies was found to evolve into a double-peaked profile in ≥ 30 keV. The 3-79 keV continuum spectrum of the pulsar was well described with a negative and positive exponential cutoff or high-energy cutoff power-law models modified with a hot blackbody at ˜3 keV. An iron emission line was also detected at 6.4 keV in the source spectrum. We did not find any signature of cyclotron absorption line in our study. Results obtained from phase-resolved and time-resolved spectroscopy are discussed in the paper.

  8. Energy weighted x-ray dark-field imaging.

    Science.gov (United States)

    Pelzer, Georg; Zang, Andrea; Anton, Gisela; Bayer, Florian; Horn, Florian; Kraus, Manuel; Rieger, Jens; Ritter, Andre; Wandner, Johannes; Weber, Thomas; Fauler, Alex; Fiederle, Michael; Wong, Winnie S; Campbell, Michael; Meiser, Jan; Meyer, Pascal; Mohr, Jürgen; Michel, Thilo

    2014-10-06

    The dark-field image obtained in grating-based x-ray phase-contrast imaging can provide information about the objects' microstructures on a scale smaller than the pixel size even with low geometric magnification. In this publication we demonstrate that the dark-field image quality can be enhanced with an energy-resolving pixel detector. Energy-resolved x-ray dark-field images were acquired with a 16-energy-channel photon-counting pixel detector with a 1 mm thick CdTe sensor in a Talbot-Lau x-ray interferometer. A method for contrast-noise-ratio (CNR) enhancement is proposed and validated experimentally. In measurements, a CNR improvement by a factor of 1.14 was obtained. This is equivalent to a possible radiation dose reduction of 23%.

  9. Characterization of polymorphic solid-state changes using variable temperature X-ray powder diffraction

    DEFF Research Database (Denmark)

    Karjalainen, Milja; Airaksinen, Sari; Rantanen, Jukka

    2005-01-01

    The aim of this study was to use variable temperature X-ray powder diffraction (VT-XRPD) to understand the solid-state changes in the pharmaceutical materials during heating. The model compounds studied were sulfathiazole, theophylline and nitrofurantoin. This study showed that the polymorph form...... of sulfathiazole SUTHAZ01 was very stable and SUTHAZ02 changed as a function of temperature to SUTHAZ01. Theophylline monohydrate changed via its metastable form to its anhydrous form during heating and nitrofurantoin monohydrate changed via amorphous form to its anhydrous form during heating. The crystallinity...... to the anhydrous form. The average crystallite size of sulfathiazole samples varied only a little during heating. The average crystallite size of both theophylline and nitrofurantoin monohydrate decreased during heating. However, the average crystallite size of nitrofurantoin monohydrate returned back to starting...

  10. Structural changes during contraction in vertebrate skeletal muscle as studied by time-resolved X-ray diffraction technique

    International Nuclear Information System (INIS)

    Sugi, H.; Tanaka, H.; Kobayashi, T.; Iwamoto, H.; Wakabayashi, K.; Hamanaka, T.; Mitsui, T.; Amemiya, Y.

    1986-01-01

    To obtain information about the structural changes in vertebrate skeletal muscle during contraction, time-resolved X-ray diffraction studies were performed on the intensity changes of the 59 A and 51 A actin layer lines from bullfrog sartorius muscle during the isometric force development, and the intensity changes of the 143 A and 215 A myosin meridional reflections and of the 1,0 and 1,1 equatorial reflections when isometrically contracting muscle was subjected to sinusoidal length changes (1%, 5-10Hz) with the following results. The integrated intensities of the 59 A and 51 A actin layer lines increased during the force development by 30-50% for the 59 A reflection, and by about 70% for the 51 A reflection compard to their respective resting values. These intensity changes were greater than those taking place during the transition from rest to rigor state, and observed to precede the intensity changes of the 429 A myosin off-meridional reflection and of equatorial reflections. When sinusoidal length changes were applied to the muscle generating steady isometric force, the resulting periodic intensity changes in the 1,0 and 1,1 equatorial reflections were in phase and in antiphase with the length changes, respectively. On the other hand, the 143 A myosin reflection exhibited a characteristic periodic change; its intensity reached a maximum at each boundary between the stretch and release phases of the length changes. These results are discussed in connection with the behavior of the cross-bridges during contraction. (author)

  11. U-shape rotating anti-cathode compact X-ray generator: 20 times stronger than the commercially available X-ray source

    Energy Technology Data Exchange (ETDEWEB)

    Sakabe, N., E-mail: sakabe-dsb@sbsp.jp; Sakabe, K. [High Energy Accelerator Research Organization (KEK), 1-1 Oho, Tsukuba 305-0801 (Japan); Foundation for Advancement of International Science (FAIS), Kasuga 3-chome, Tsukuba, Ibaraki 305-0821 (Japan); Ohsawa, S.; Sakai, T.; Kobayakawa, H.; Sugimura, T.; Ikeda, M.; Tawada, M. [High Energy Accelerator Research Organization (KEK), 1-1 Oho, Tsukuba, Ibaraki 305-0801 (Japan); Watanabe, N.; Sasaki, K. [Nagoya University, Chikusa, Nagoya, Aichi 464-8603 (Japan); Wakatsuki, M. [National Institute of Advanced Industrial Science and Technology (AIST), 1-1-1 Higashi, Tsukuba, Ibaraki 305-8568 (Japan)

    2013-11-01

    A new type of U-shape anti-cathode X-ray generator in which the inner surface of a cylindrical target is irradiated by an electron beam has been made by modifying a conventional rotating anti-cathode X-ray generator whose brightness in the catalog is 12 kW mm{sup −2}. A brightness of 129 kW mm{sup −2} was thereby obtained with this new U-shape-type X-ray generator. This new X-ray generator is expected to be of keen interest for applications in academia, industry and in hospitals. A new type of U-shape anti-cathode X-ray generator in which the inner surface of a cylindrical target is irradiated by an electron beam has been made by modifying a conventional rotating anti-cathode X-ray generator whose brightness in the catalog is 12 kW mm{sup −2}. The target material (Cu), target radius (50 mm) and rotating speed (6000 r.p.m.) were not changed in this modification. A brightness of 52 kW mm{sup −2} was obtained by this U-shape-type X-ray generator. This means that the brightness of the new type is 4.3 times greater than that of the old unmodified one. Furthermore, the new-type X-ray generator yielded a brightness of 129 kW mm{sup −2} by adding a carbon coating on the Cu target. This means an overall increase of brightness of ten times. The original generator has the highest brightness in the generators of the same class (having a radius of 50 mm and rotation speed of 6000 r.p.m.). Observations showed that Cu Kα counts at vertical incidence of the electron beam onto the surface of the new target, which is initially optically smooth, decrease as the surface is roughened by a severe thermal stress caused by strong electron beam exposure. Further observation reveals, however, that oblique incidence of the electron beam onto the roughened surface drastically increased the X-ray output and amounts to twice as much as that from a smooth surface at vertical incidence. Thus, at the present stage, an overall increase of brightness has been realised at a level 20 times

  12. TIME-DEPENDENT ELECTRON ACCELERATION IN BLAZAR TRANSIENTS: X-RAY TIME LAGS AND SPECTRAL FORMATION

    Energy Technology Data Exchange (ETDEWEB)

    Lewis, Tiffany R.; Becker, Peter A. [Department of Physics and Astronomy, George Mason University, Fairfax, VA 22030-4444 (United States); Finke, Justin D., E-mail: pbecker@gmu.edu, E-mail: tlewis13@gmu.edu, E-mail: justin.finke@nrl.navy.mil [U.S. Naval Research Laboratory, Code 7653, 4555 Overlook Avenue SW, Washington, DC 20375-5352 (United States)

    2016-06-20

    Electromagnetic radiation from blazar jets often displays strong variability, extending from radio to γ -ray frequencies. In a few cases, this variability has been characterized using Fourier time lags, such as those detected in the X-rays from Mrk 421 using Beppo SAX. The lack of a theoretical framework to interpret the data has motivated us to develop a new model for the formation of the X-ray spectrum and the time lags in blazar jets based on a transport equation including terms describing stochastic Fermi acceleration, synchrotron losses, shock acceleration, adiabatic expansion, and spatial diffusion. We derive the exact solution for the Fourier transform of the electron distribution and use it to compute the Fourier transform of the synchrotron radiation spectrum and the associated X-ray time lags. The same theoretical framework is also used to compute the peak flare X-ray spectrum, assuming that a steady-state electron distribution is achieved during the peak of the flare. The model parameters are constrained by comparing the theoretical predictions with the observational data for Mrk 421. The resulting integrated model yields, for the first time, a complete first-principles physical explanation for both the formation of the observed time lags and the shape of the peak flare X-ray spectrum. It also yields direct estimates of the strength of the shock and the stochastic magnetohydrodynamical wave acceleration components in the Mrk 421 jet.

  13. Neutron and X-ray emission studies in a low energy plasma focus

    Energy Technology Data Exchange (ETDEWEB)

    Zakaullah, M. [Quaid-i-Azam Univ., Islamabad (Pakistan). Dept. of Physics; Murtaza, G. [Quaid-i-Azam Univ., Islamabad (Pakistan). Dept. of Physics; Qamar, S. [Quaid-i-Azam Univ., Islamabad (Pakistan). Dept. of Physics; Ahmad, I. [Quaid-i-Azam Univ., Islamabad (Pakistan). Dept. of Physics; Beg, M.M. [Quaid-i-Azam Univ., Islamabad (Pakistan). Dept. of Physics

    1996-03-01

    In a low energy Mather-type plasma focus energized by a single 32 {mu}F capacitor, the X-ray and neutron emission is investigated using time-integrated and time-resolved detectors. The X-ray emission profile has a width (FWHM) of 40-50 ns. The neutron emission profile is broader compared to the X-ray emission profile and also delayed by 30-40 ns. To identify different regimes of X-ray emission, an X-ray pin-hole camera along with different absorption filters is employed. While the X-ray emission is high within a narrow pressure range of 2.0-2.5 mbar, the neutron emission is intense for a wider range of 1.0-4.5 mbar. The intense X-ray emission seems to originate from the axially moving shock wave. These results also indicate rather different production mechanisms for X-ray and neutron emission. Also on comparing the X-ray images with Al(2 {mu}m), Al(5 {mu}m), Al(9 {mu}m) filters, we find that the bulk of X-rays from the focus filament have energies less than 2 keV. (orig.).

  14. High-pressure powder X-ray diffraction at the turn of the century

    International Nuclear Information System (INIS)

    Paszkowicz, W.

    2002-01-01

    Studies at extreme pressures and temperatures are helpful for understanding the physical properties of the solid state, including such classes of materials as semiconductors, superconductors or minerals. This is connected with the opportunity of tuning the pressure by many orders of magnitude. Diamond-anvil and large-anvil pressure cells installed at dedicated synchrotron beamlines are efficient tools for examination of crystal structure, equation of state, compressibility and phase transitions. One of basic methods in such studies is powder diffraction. This review is devoted to methods of powder X-ray diffraction at high-pressures generated by devices installed at synchrotron radiation sources, in particular to the principles of operation of high-pressure-high-temperature cells. General information on high-pressure diffraction facilities installed at 11 synchrotron storage rings in the world is provided. Measurement aspects are considered, including (i) pressure generation and calibration, (ii) strain in the sample, the pressure marker and the pressure-transmitting medium and (iii) pressure and temperature distributions within the cells. Sources of interest in high-pressure diffraction studies (design of new materials, observation of new phenomena, confrontation of theory with experiment) are briefly discussed. Recent developments of high-pressure methods make that pressure becomes a variable playing a key role in investigation of condensed matter. The paper ends with some remarks on the possible future developments of the technique

  15. Plasma polarization spectroscopy. Time resolved spectroscopy in soft x-ray region on recombining plasma

    International Nuclear Information System (INIS)

    Iwamae, Atsushi; Hasuo, Masahiro; Atake, Makoto; Hasegawa, Noboru; Kawachi, Tetsuya

    2007-01-01

    We present an experimental study of polarization of emission radiations from recombining plasmas generated by the interaction of 60 fs ultra-short laser pulses with a gas jet. Time-resolved spectroscopy with a temporal resolution of 5 ps with repetitive accumulation is used to follow the recombination time histories. (author)

  16. Observation of material, thickness, and bremsstrahlung x-ray intensity dependent effects in moderate and high Z targets in a gamma and x-ray LIDAR experiment

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Xiaodong, E-mail: xzhang39@utk.edu [Department of Nuclear Engineering, University of Tennessee, TN 37996 (United States); Ayaz-Maierhafer, Birsen; Laubach, Mitchell A. [Department of Nuclear Engineering, University of Tennessee, TN 37996 (United States); Hayward, Jason P. [Department of Nuclear Engineering, University of Tennessee, TN 37996 (United States); Oak Ridge National Lab, Oak Ridge, TN 37831 (United States)

    2015-06-01

    A high energy gamma and x-ray LIDAR system consisting of a fast pulse (~50 ps, FWHM) LINAC and a Cherenkov detection system was used to investigate response differences among materials, their thicknesses, and bremsstrahlung x-ray intensities. The energies and pulse width of electrons used to produce bremsstrahlung x-rays were set at 20 or 40 MeV and 50 ps FWHM duration, respectively. The Cherenkov detector was built with a fused silica glass optically coupled to a 51 mm fast timing photomultiplier tube, which has an intrinsic energy threshold of 340.7 keV for Compton backscattered gammas. Such a fast detection system yields a coincidence resolving time of 93 ps FWHM, which is equivalent to a depth resolving capability of about 3 cm FWHM. The thicknesses of iron and lead targets were varied from 1 in. to 7 in. with a step of 1 in., and the thicknesses of DU were varied from 1/3 in. to 1 in. with a step of 1/3 in. The experimental results show that iron targets tend to produce a factor of five less observed x-rays and gammas, with less energetic photoelectron frequency distributions, compared with DU and lead targets for the same beam intensity and target thicknesses. Additionally, the self-shielding effect causes the lead to yield more gammas than the DU considering the experimental observation point. For the setup used in this study, a charge per pulse in the range of 1–2.5 nC yields the best resolving capability between the DU and lead targets.

  17. The Athena X-ray Integral Field Unit (X-IFU)

    Science.gov (United States)

    Barret, Didier; Trong, Thein Lam; Den Herder, Jan-Willem; Piro, Luigi; Barcons, Xavier; Huovelin, Juhani; Kelley, Richard; Mas-Hesse, J. Miquel; Mitsuda, Kazuhisa; Paltani, Stephane; hide

    2016-01-01

    The X-ray Integral Field Unit (X-IFU) on board the Advanced Telescope for High-ENergy Astrophysics (Athena) will provide spatially resolved high-resolution X-ray spectroscopy from 0.2 to 12 keV, with 5 pixels over a field of view of 5 arc minute equivalent diameter and a spectral resolution of 2.5 eV up to 7 keV. In this paper, we first review the core scientific objectives of Athena, driving the main performance parameters of the X-IFU, namely the spectral resolution, the field of view, the effective area, the count rate capabilities, the instrumental background. We also illustrate the breakthrough potential of the X-IFU for some observatory science goals. Then we brie y describe the X-IFU design as defined at the time of the mission consolidation review concluded in May 2016, and report on its predicted performance. Finally, we discuss some options to improve the instrument performance while not increasing its complexity and resource demands (e.g. count rate capability, spectral resolution). (2016) .

  18. A high count rate one-dimensional position sensitive detector and a data acquisition system for time resolved X-ray scattering studies

    International Nuclear Information System (INIS)

    Pernot, P.

    1982-01-01

    A curved multiwire proportional drift chamber has been built as a general purpose instrument for X-ray scattering and X-ray diffraction experiments with synchrotron radiation. This parallaxe-free one-dimensional linear position sensitive detector has a parallel readout with a double hit logic. The data acquisition system, installed as a part of the D11 camera at LURE-DCI, is designed to perform time slicing and cyclic experiments; it has been used with either the fast multiwire chamber or a standard position sensitive detector with delay line readout [fr

  19. Complex UV/X-ray variability of 1H 0707-495

    Science.gov (United States)

    Pawar, P. K.; Dewangan, G. C.; Papadakis, I. E.; Patil, M. K.; Pal, Main; Kembhavi, A. K.

    2017-12-01

    We study the relationship between the UV and X-ray variability of the narrow-line Seyfert 1 galaxy 1H 0707-495. Using a year-long Swift monitoring and four long XMM-Newton observations, we perform cross-correlation analyses of the UV and X-ray light curves, on both long and short time-scales. We also perform time-resolved X-ray spectroscopy on 1-2 ks scale, and study the relationship between the UV emission and the X-ray spectral components - soft X-ray excess and a power law. We find that the UV and X-ray variations anticorrelate on short, and possibly on long time-scales as well. Our results rule out reprocessing as the dominant mechanism for the UV variability, as well as the inward propagating fluctuations in the accretion rate. Absence of a positive correlation between the photon index and the UV flux suggests that the observed UV emission is unlikely to be the seed photons for the thermal Comptonization. We find a strong correlation between the continuum flux and the soft-excess temperature which implies that the soft excess is most likely the reprocessed X-ray emission in the inner accretion disc. Strong X-ray heating of the innermost regions in the disc, due to gravitational light bending, appears to be an important effect in 1H 0707-495, giving rise to a significant fraction of the soft excess as reprocessed thermal emission. We also find indications for a non-static, dynamic X-ray corona, where either the size or height (or both) vary with time.

  20. A method for measuring the time structure of synchrotron x-ray beams

    International Nuclear Information System (INIS)

    Moses, W.W.; Derenzo, S.E.

    1989-08-01

    We describe a method employing a plastic scintillator coupled to a fast photomultiplier tube to generate a timing pulse from the x-ray bursts emitted from a synchrotron radiation source. This technique is useful for performing synchrotron experiments where detailed knowledge of the timing distribution is necessary, such as time resolved spectroscopy or fluorescence lifetime experiments. By digitizing the time difference between the timing signal generated on one beam crossing with the timing signal generated on the next beam crossing, the time structure of a synchrotron beam can be analyzed. Using this technique, we have investigated the single bunch time structure at the National Synchrotron Light Source (NSLS) during pilot runs in January, 1989, and found that the majority of the beam (96%) is contained in one rf bucket, while the remainder of the beam (4%) is contained in satellite rf buckets preceeding and following the main rf bucket by 19 ns. 1 ref., 4 figs

  1. Structural studies of carbon nanotubes by powder x-ray diffraction at SPring-8 and KEK PF

    CERN Document Server

    Maniwa, Y; Fujiwara, A

    2003-01-01

    Powder X-ray diffraction (XRD) studies on carbon nanotubes (CNTs) using synchrotron radiation are reported. In spite of the observed broad XRD peak profiles of two-dimensional triangular (hexagonal) lattice of single-wall carbon nanotubes (SWNTs), it was shown that useful structural information, such as the tube diameter and its distribution, can be deduced from detailed analysis of the characteristic XRD patterns. In particular, powder-XRD measurements were performed to study the phase transition of encapsulated materials inside SWNTs. In the C sub 7 sub 0 -one dimensional (1D) crystals formed inside SWNTs, importance of one-dimensionality in the C sub 7 sub 0 -molecular dynamics was suggested. It was also shown that water inside SWNTs undergoes a phase transition from liquid to an ice-nanotube structure below -38degC. Conversion process from SWNT to double-wall carbon nanotube (DWNT) was also studied by XRD.

  2. Effect of powder sample granularity on fluorescent intensity and on thermal parameters in x-ray diffraction Rietveld analysis

    International Nuclear Information System (INIS)

    Sparks, C.J.; Specht, E.D.; Ice, G.E.; Kumar, R.; Zschack, P.; Shiraishi, T.; Hisatsune, K.

    1991-01-01

    The effect of sample granularity on diffracted x-ray intensity was evaluated by measuring the 2θ dependence of x-ray fluorescence from various samples. Measurements were made in the symmetric geometry on samples ranging from single crystals to highly absorbing coarse powders. A characteristic shape for the absorption correction was observed. A demonstration of the sensitivity of Rietveld refined site occupation parameters is made on CuAu and Cu 50 Au 44 Ni 6 alloys refined with and without granularity corrections. These alloys provide a good example of the effect of granularity due to their large linear x-ray absorption coefficients. Sample granularity and refined thermal parameters obtained from the Rietveld analysis were found to be correlated. Without a granularity correction, the refined thermal parameters are too low and can actually become negative in an attempt to compensate for granularity. A general shape for granularity correction can be included in refinement procedures. If no granularity correction is included, data should be restricted to above 30 degrees 2θ, and thermal parameters should be ignored unless extreme precautions are taken to produce >5 μm particles and high packing densities

  3. High intensity line source for x-ray spectrometer calibration

    International Nuclear Information System (INIS)

    Thoe, R.S.

    1986-06-01

    A high intensity electron-impact x-ray source using a one-dimensional Pierce lens has been built for the purpose of calibrating a bent crystal x-ray spectrometer. This source focuses up to 100 mA of 20-keV electrons to a line on a liquid-cooled anode. The line (which can serve as a virtual slit for the spectrometer) measures approximately 800 μ x 2 cm. The source is portable and therefore adaptable to numerous types of spectrometer applications. One particular application, the calibration of a high resolution (r = 10 4 ) time-resolved cyrstal spectrometer, will be discussed in detail

  4. Characterization of x-ray diffraction and electron spin resonance: Effects of sintering time and temperature on bovine hydroxyapatite

    International Nuclear Information System (INIS)

    Kusrini, Eny; Sontang, Muhammad

    2012-01-01

    The physical and chemical properties of a hydroxyapatite produced by the sintering of bovine bone were investigated by powder x-ray diffraction (PXRD), electron spin resonance (ESR), energy dispersive x-ray spectroscopy (EDX), scanning electron microscopy (SEM), Fourier transform infrared (FTIR), and differential thermal analysis (DTA). A bovine bone powder was sintered at different temperatures ranging from 500 to 1400 °C. The influences of post-irradiation storage on the radiation ESR response of the bovine bone powder before and after sintering were also studied. The results indicate that the sintered bovine bone powder contained hydroxyapatite. Diffraction patterns were sharp and clear based on the (211), (300), and (202) reflections corresponding to bovine hydroxyapatite (BHA), which confirmed the phase purity and high crystalline grade of the BHA produced. The PXRD profile of BHA was dependent on sintering temperatures and times. The molecular formula of BHA was determined by Rietveld analysis showed a similar structure and composition to calcium hydroxyapatite in hexagonal P6 3 /m space group a=b=9.435 Å and c=6.895 Å. ESR data showed that the sintering process can decrease the number of free radicals in BHA; it also revealed that the number of free radicals is constant during long storage periods (75 days). The sintering technique described in this study may be used to extract hydroxyapatite from biowaste bovine bone, leading to its application as a bone filler. - Highlights: ► Natural hydroxyapatite was produced from the bio-wasting bovine bones by sintering method. ► PXRD profile of BHA is dependent on the different temperatures and times in sintering process. ► ESR data is useful to study the typical of free radicals formed in the samples after irradiation. ► Stability and physicochemical properties of BHA is dependent on the different storage times. ► Technique is able to be used to find the natural hydroxyapatite applicable for bone filler.

  5. NuSTAR Hard X-ray Survey of the Galactic Center Region. I. Hard X-ray Morphology and Spectroscopy of the Diffuse Emission

    DEFF Research Database (Denmark)

    Mori, Kaya; Hailey, Charles J.; Krivonos, Roman

    2015-01-01

    We present the first sub-arcminute images of the Galactic Center above 10 keV, obtained with NuSTAR. NuSTAR resolves the hard X-ray source IGR J17456-2901 into non-thermal X-ray filaments, molecular clouds, point sources, and a previously unknown central component of hard X-ray emission (CHXE). Nu...

  6. Bright ultrashort x-rays from intense subpicosecond laser-plasma interactions

    International Nuclear Information System (INIS)

    Umstadter, D.

    1995-01-01

    Short-pulse, high-intensity lasers interacting with solid targets make possible the study of a new class of laser-plasma interactions. They are unique because during the ultrashort laser pulse relatively little expansion occurs, and the density scale length remains much less than the laser wavelength. This makes possible the direct deposition of a significant amount of the laser energy at close to solid density. Steep plasma temperature and density gradients subsequently cause rapid cooling, resulting in highly non-equilibrium conditions and the concurrent emission of extremely bright ultrashort x-ray pulses. In this study, the latter are investigated experimentally with temporally and spectrally resolved soft x-ray diagnostics. The emitted x-ray spectra from solid targets with various atomic numbers are characterized for a laser pulse width τ l ∼ 400 fs. These ultrashort x rays may be used as (1) a diagnostic of solid-density plasma conditions, (2) a tool for the study of radiation hydrodynamics in a parameter regime that is otherwise inaccessible, and (3) a source for time-resolved diffraction, spectroscopy, or microscopy studies of transient chemical, biological or physical phenomena

  7. Combined Approach for the Structural Characterization of Alkali Fluoroscandates: Solid-State NMR, Powder X-ray Diffraction, and Density Functional Theory Calculations.

    Science.gov (United States)

    Rakhmatullin, Aydar; Polovov, Ilya B; Maltsev, Dmitry; Allix, Mathieu; Volkovich, Vladimir; Chukin, Andrey V; Boča, Miroslav; Bessada, Catherine

    2018-02-05

    The structures of several fluoroscandate compounds are presented here using a characterization approach combining powder X-ray diffraction and solid-state NMR. The structure of K 5 Sc 3 F 14 was fully determined from Rietveld refinement performed on powder X-ray diffraction data. Moreover, the local structures of NaScF 4 , Li 3 ScF 6 , KSc 2 F 7 , and Na 3 ScF 6 compounds were studied in detail from solid-state 19 F and 45 Sc NMR experiments. The 45 Sc chemical shift ranges for six- and seven-coordinated scandium environments were defined. The 19 F chemical shift ranges for bridging and terminal fluorine atoms were also determined. First-principles calculations of the 19 F and 45 Sc NMR parameters were carried out using plane-wave basis sets and periodic boundary conditions (CASTEP), and the results were compared with the experimental data. A good agreement between the calculated shielding constants and experimental chemical shifts was obtained. This demonstrates the good potential of computational methods in spectroscopic assignments of solid-state 45 Sc NMR spectroscopy.

  8. Effects of quartz particle size and water-to-solid ratio on hydrothermal synthesis of tobermorite studied by in-situ time-resolved X-ray diffraction

    International Nuclear Information System (INIS)

    Kikuma, J.; Tsunashima, M.; Ishikawa, T.; Matsuno, S.; Ogawa, A.; Matsui, K.; Sato, M.

    2011-01-01

    Hydrothermal synthesis process of tobermorite (5CaO.6SiO 2 .5H 2 O) has been investigated by in-situ X-ray diffraction using high-energy X-rays from a synchrotron radiation source in combination with a purpose-build autoclave cell. Dissolution rates of quartz were largely affected by its particle size distribution in the starting mixtures. However, the composition (Ca/Si) of non-crystalline C-S-H at the start of tobermorite formation was identical regardless of the quartz dissolution rate. An effect of water-to-solid ratio (w/s) was investigated for samples using fine particle quartz. Tobermorite did not occur with w/s of 1.7 but occurred with w/s higher than 3.0. Surprisingly, however, the dissolution curves of quartz were nearly identical for all samples with w/s from 1.7 to 9, indicating that the dissolution rate is predominated by surface area. Possible reaction mechanism for tobermorite formation will be discussed in terms of Ca and/or silicate ion concentration in the liquid phase and distribution of Ca/Si in non-crystalline C-S-H. - Graphical abstract: Time-resolved XRD data set was obtained at up to 190 deg. C under a saturated steam pressure. Tobermorite (5CaO.6SiO 2 .5H 2 O) formation reaction was investigated in detail for several different starting materials. Highlights: → Hydrothermal formation of tobermorite was monitored by in-situ XRD. → Ca/Si of C-S-H at the start time of tobermorite formation was determined. → The Ca/Si value was identical regardless of the quartz particle size in the starting mixture.

  9. Short-time X-ray diffraction with an efficient-optimized, high repetition-rate laser-plasma X-ray-source

    International Nuclear Information System (INIS)

    Kaehle, Stephan

    2009-01-01

    This thesis deals with the production and application of ultrashort X-ray pulses. In the beginning different possibilities for the production of X-ray pulses with pulse durations of below one picosecond are presented, whereby the main topic lies on the so called laser-plasma X-ray sources with high repetition rate. In this case ultrashort laser pulses are focused on a metal, so that in the focus intensities of above 10 16 W/cm 2 dominate. In the ideal case in such way ultrafast electrons are produced, which are responsible for line radiation. In these experiments titanium K α radiation is produced, thes photons possess an energy of 4.51 keV. For the efficient production of line radiation here the Ti:Sa laser is optimized in view of the laser energy and the pulse shape and the influence of the different parameters on the K α production systematically studied. The influences of laser intensity, system-conditioned pre-pulses and of phase modulation are checked. It turns out that beside the increasement of the K α radiation by a suited laser intensity a reduction of the X-ray background radiation is of deciding importance for the obtaining of clear diffraction images. This background radiation is mainly composed of bremsstrahlung. It can be suppressed by the avoidance of intrinsic pre-pulses and by means of 2nd-order phase modulation. By means of optical excitation and X-ray exploration experiments the production of acoustic waves after ultrashort optical excitation in a 150 nm thick Ge(111) film on Si(111) is studied. These acoustic waves are driven by thermal (in this time scale time-independent) and electronic (time dependent) pressure amounts. As essential results it turns out that the relative amount of the electronic pressure increases with decreasing excitation density [de

  10. Sample cell for powder x-ray diffraction at up to 500 bars and 200 deg. C

    International Nuclear Information System (INIS)

    Jupe, Andrew C.; Wilkinson, Angus P.

    2006-01-01

    A low cost sample cell for powder diffraction at high pressure and temperature that employs either sapphire or steel pressure tubes is described. The cell can be assembled rapidly, facilitating the study of chemically reacting systems, and it provides good control of both pressure and temperature in a regimen where diamond anvil cells and multianvil apparatus cannot be used. The design provides a relatively large sample volume making it suitable for the study of quite large grain size materials, such as hydrating cement slurries. However, relatively high energy x rays are needed to penetrate the pressure tube

  11. The stoichiometry of synthetic alunite as a function of hydrothermal aging investigated by solid-state NMR spectroscopy, powder X-ray diffraction and infrared spectroscopy

    DEFF Research Database (Denmark)

    Grube, Elisabeth; Nielsen, Ulla Gro

    2015-01-01

    The stoichiometry of a series of synthetic alunite (nominally KAl3(SO4)2(OH)6) samples prepared by hydrothermal methods as a function of reaction time (1 – 31 days) has been investigated by powder X-ray diffraction, Fourier transform infrared spectroscopy as well as solid-state 1H and 27Al magic...... of potassium defects present, from 17.261(1) to 17.324(5) Å. Solid-state 27Al MAS NMR revealed a decrease in the defect concentration as a function of time and showed the presence of 7-10 % impurities in the samples....

  12. Fast time-resolved aerosol collector: proof of concept

    Science.gov (United States)

    Yu, X.-Y.; Cowin, J. P.; Iedema, M. J.; Ali, H.

    2010-10-01

    Atmospheric particles can be collected in the field on substrates for subsequent laboratory analysis via chemically sensitive single particle methods such as scanning electron microscopy with energy dispersive x-ray analysis. With moving substrates time resolution of seconds to minutes can be achieved. In this paper, we demonstrate how to increase the time resolution when collecting particles on a substrate to a few milliseconds to provide real-time information. Our fast time-resolved aerosol collector ("Fast-TRAC") microscopically observes the particle collection on a substrate and records an on-line video. Particle arrivals are resolved to within a single frame (4-17 ms in this setup), and the spatial locations are matched to the subsequent single particle analysis. This approach also provides in-situ information on particle size and number concentration. Applications are expected in airborne studies of cloud microstructure, pollution plumes, and surface long-term monitoring.

  13. Catalytic Mechanism of Nitrile Hydratase Proposed by Time-resolved X-ray Crystallography Using a Novel Substrate, tert-Butylisonitrile*S⃞

    Science.gov (United States)

    Hashimoto, Koichi; Suzuki, Hiroyuki; Taniguchi, Kayoko; Noguchi, Takumi; Yohda, Masafumi; Odaka, Masafumi

    2008-01-01

    Nitrile hydratases (NHases) have an unusual iron or cobalt catalytic center with two oxidized cysteine ligands, cysteine-sulfinic acid and cysteine-sulfenic acid, catalyzing the hydration of nitriles to amides. Recently, we found that the NHase of Rhodococcus erythropolis N771 exhibited an additional catalytic activity, converting tert-butylisonitrile (tBuNC) to tert-butylamine. Taking advantage of the slow reactivity of tBuNC and the photoreactivity of nitrosylated NHase, we present the first structural evidence for the catalytic mechanism of NHase with time-resolved x-ray crystallography. By monitoring the reaction with attenuated total reflectance-Fourier transform infrared spectroscopy, the product from the isonitrile carbon was identified as a CO molecule. Crystals of nitrosylated inactive NHase were soaked with tBuNC. The catalytic reaction was initiated by photo-induced denitrosylation and stopped by flash cooling. tBuNC was first trapped at the hydrophobic pocket above the iron center and then coordinated to the iron ion at 120 min. At 440 min, the electron density of tBuNC was significantly altered, and a new electron density was observed near the isonitrile carbon as well as the sulfenate oxygen of αCys114. These results demonstrate that the substrate was coordinated to the iron and then attacked by a solvent molecule activated by αCys114-SOH. PMID:18948265

  14. Characterization of a pulsed x-ray source for fluorescent lifetime measurements

    International Nuclear Information System (INIS)

    Blankespoor, S.C.; Derenzo, S.E.; Moses, W.W.; Rossington, C.S.; Ito, M.; Oba, K.

    1994-01-01

    To search for new, fast, inorganic scintillators, the authors have developed a bench-top pulsed x-ray source for determining fluorescent lifetimes and wavelengths of compounds in crystal or powdered form. This source uses a light-excited x-ray tube which produces x-rays when light from a laser diode strikes its photocathode. The x-ray tube has a tungsten anode, a beryllium exit window, a 30 kV maximum tube bias, and a 50 μA maximum average cathode current. The laser produces 3 x 10 7 photons at 650 nm per ∼100 ps pulse, with up to 10 7 pulses/sec. The time spread for the laser diode, x-ray tube, and a microchannel plate photomultiplier tube is less than 120 ps fwhm. The mean x-ray energy at tube biases of 20, 25, and 30 kV is 9.4, 10.3, and 11.1 keV, respectively. The authors measured 140, 230, and 330 x-ray photons per laser diode pulse per steradian, at tube biases of 20, 25, and 30 kV, respectively. Background x-rays due to dark current occur at a rate of 1 x 10 6 and 3 x 10 6 photons/sec/steradian at biases of 25 and 30 kV, respectively. Data characterizing the x-ray output with an aluminum filter in the x-ray beam are also presented

  15. Time-resolved electron beam phase space tomography at a soft x-ray free-electron laser

    Directory of Open Access Journals (Sweden)

    Michael Röhrs

    2009-05-01

    Full Text Available High-gain free-electron lasers (FELs in the ultraviolet and x-ray regime put stringent demands on the peak current, transverse emittance, and energy spread of the driving electron beam. At the soft x-ray FEL FLASH, a transverse deflecting microwave structure (TDS has been installed to determine these parameters for the longitudinally compressed bunches, which are characterized by a narrow leading peak of high charge density and a long tail. The rapidly varying electromagnetic field in the TDS deflects the electrons vertically and transforms the time profile into a streak on an observation screen. The bunch current profile was measured single shot with an unprecedented resolution of 27 fs under FEL operating conditions. A precise single-shot measurement of the energy distribution along a bunch was accomplished by using the TDS in combination with an energy spectrometer. Variation of quadrupole strengths allowed for a determination of the horizontal emittance as a function of the longitudinal position within a bunch, the so-called slice emittance. In the bunch tail, a normalized slice emittance of about 2  μm was found, in agreement with expectations. In the leading spike, however, surprisingly large emittance values were observed, in apparent contradiction with the low emittance deduced from the measured FEL gain. By applying three-dimensional phase space tomography, we were able to show that the bunch head contains a central core of low emittance and high local current density, which is presumably the lasing part of the bunch.

  16. Secondary-source energy-dispersive x-ray spectrometer

    International Nuclear Information System (INIS)

    Larsen, R.P.; Tisue, G.T.

    1975-01-01

    A secondary-source energy-dispersive x-ray spectrometer has been built and tested. In this instrument the primary source of x rays is a tungsten-target tube powered by a high-voltage (75 kV), a high-power (3.7 kW) generator from a wavelength spectrometer (G.E. XRD-6). The primary polychromatic x rays irradiate an elemental foil, the secondary source. Its characteristic essentially monochromatic x rays are used to irradiate the sample. Fluorescent x rays from the sample are detected and resolved by a lithium-drifted silicon detector, multichannel-analyzer system. The design of the instrument provides a convenient means for changing the secondary, and hence, the energy of the excitation radiation

  17. Real time 2 dimensional detector for charged particle and soft X-ray images

    International Nuclear Information System (INIS)

    Ishikawa, M.; Ito, M.; Endo, T.; Oba, K.

    1995-01-01

    The conventional instruments used in experiments for the soft X-ray region such as X-ray diffraction analysis are X-ray films or imaging plates. However, these instruments are not suitable for real time observation. In this paper, newly developed imaging devices will be presented, which have the capability to take X-ray images in real time with a high detection efficiency. Also, another capability, to take elementary particle tracking images, is described. (orig.)

  18. Spatially resolved synchrotron radiation induced X-ray fluorescence analyses of rare Rembrandt silverpoint drawings

    International Nuclear Information System (INIS)

    Reiche, I.; Radtke, M.; Berger, A.; Goerner, W.; Merchel, S.; Riesemeier, H.; Bevers, H.

    2006-01-01

    New analyses of a series of very rare silverpoint drawings that were executed by Rembrandt Harmensz. van Rijn (1606-1669) which are kept today in the Kupferstichkabinett (Museum of Prints and Drawings) of the State Museums of Berlin are reported here. Analysis of these drawings requires particular attention because the study has to be fully non-destructive and extremely sensitive. The metal alloy on the paper does not exceed some hundreds of μg/cm 2 . Therefore, synchrotron radiation induced X-ray fluorescence (SR-XRF) is - together with external micro-proton-induced X-ray emission - the only well-suited method for the analyses of metalpoint drawings. In some primary work, about 25 German and Flemish metalpoint drawings were investigated using spatially resolved SR-XRF analysis at the BAMline at BESSY. This study enlarges the existing French-German database of metalpoint drawings dating from the 15th and 16th centuries, as these Rembrandt drawings originate from the 17th century where this graphical technique was even rarer and already obsolete. It also illustrates how SR-XRF analysis can reinforce art historical assumptions on the dating of drawings and their connection. (orig.)

  19. Systematic investigation of lard polymorphism using combined DSC and time-resolved synchrotron X-ray diffraction

    NARCIS (Netherlands)

    Kalnin, D.J.E.; Lesieur, P.; Artzner, F.; Keller, G.; Ollivon, M.

    2005-01-01

    The polymorphic behavior of lard was systematically investigated by differential scanning calorimetry (DSC) while simultaneously monitoring the formation of the different crystal forms with X-ray diffraction (XRDT). To interpret the complex polymorphic evolution of the sample analyzed by regular

  20. Twenty-seventh annual conference applications of x-ray analysis

    International Nuclear Information System (INIS)

    McCarthy, G.J.; Ruud, C.O.

    1978-01-01

    Abstracts are presented of papers given at the conference. Topics covered include: special techniques in powder diffraction; specimen handling; x-ray fluorescence applications; applications of XRD and x-ray imaging; progress in the reduction of matrix effects in XRF; evaluation of XRD patterns; XRF innovations; XRD stress analysis and mathematical data analysis

  1. Neutron and X-ray Detectors

    Energy Technology Data Exchange (ETDEWEB)

    Carini, Gabriella [SLAC National Accelerator Lab., Menlo Park, CA (United States); Denes, Peter [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Gruener, Sol [Cornell Univ., Ithaca, NY (United States); Lessner, Elianne [Dept. of Energy (DOE), Washington DC (United States). Office of Science Office of Basic Energy Sciences

    2012-08-01

    (and two computing hurdles that result from the corresponding increase in data volume) for the detector community to overcome in order to realize the full potential of BES neutron and X-ray facilities. Resolving these detector impediments will improve scientific productivity both by enabling new types of experiments, which will expand the scientific breadth at the X-ray and neutron facilities, and by potentially reducing the beam time required for a given experiment. These research priorities are summarized in the table below. Note that multiple, simultaneous detector improvements are often required to take full advantage of brighter sources. High-efficiency hard X-ray sensors: The fraction of incident particles that are actually detected defines detector efficiency. Silicon, the most common direct-detection X-ray sensor material, is (for typical sensor thicknesses) 100% efficient at 8 keV, 25%efficient at 20 keV, and only 3% efficient at 50 keV. Other materials are needed for hard X-rays. Replacement for 3He for neutron detectors: 3He has long been the neutron detection medium of choice because of its high cross section over a wide neutron energy range for the reaction 3He + n —> 3H + 1H + 0.764 MeV. 3He stockpiles are rapidly dwindling, and what is available can be had only at prohibitively high prices. Doped scintillators hold promise as ways to capture neutrons and convert them into light, although work is needed on brighter, more efficient scintillator solutions. Neutron detectors also require advances in speed and resolution. Fast-framing X-ray detectors: Today’s brighter X-ray sources make time-resolved studies possible. For example, hybrid X-ray pixel detectors, initially developed for particle physics, are becoming fairly mature X-ray detectors, with considerable development in Europe. To truly enable time-resolved studies, higher frame rates and dynamic range are required, and smaller pixel sizes are desirable. High-speed spectroscopic X-ray detectors

  2. Spatially resolved X-ray spectra of coronal active regions

    International Nuclear Information System (INIS)

    Catura, R.C.; Acton, L.W.; Joki, E.G.; Rapley, C.G.; Culhane, J.L.

    1975-01-01

    X-ray spectra from a number of coronal active regions were obtained during ATM support rocket flights carried out by the Lockheed group on June 11 and December 19, 1973. Multi-grid collimators were used to provide fields of view of 40ins. diameter and 90ins. diameter for a number of scanning crystal spectrometers and a bent crystal spectrometer which employed a position sensitive proportional counter to register the diffracted spectrum. A solar image was produced on film and on a TV camera on board the rocket with the aid of a 1 A Hα filter. A small part of the X-ray collimator was used to generate a multiple spot diffraction pattern which was superimposed on the Hα image and the composite picture was transmitted to the ground. Pre-launch calibrations allowed the spot corresponding to the X-ray collimator axis to be identified and so the collimator pointing direction on the solar disc was controlled from the ground by means of commands sent to the rocket. (Auth.)

  3. Time-resolved small-angle x-ray scattering study of the early stage of amyloid formation of an apomyoglobin mutant

    Science.gov (United States)

    Ortore, Maria Grazia; Spinozzi, Francesco; Vilasi, Silvia; Sirangelo, Ivana; Irace, Gaetano; Shukla, Anuj; Narayanan, Theyencheri; Sinibaldi, Raffaele; Mariani, Paolo

    2011-12-01

    The description of the fibrillogenesis pathway and the identification of “on-pathway” or “off-pathway” intermediates are key issues in amyloid research as they are concerned with the mechanism for onset of certain diseases and with therapeutic treatments. Recent results on the fibril formation process revealed an unexpected complexity both in the number and in the types of species involved, but the early aggregation events are still largely unknown, mainly because of their experimental inaccessibility. To provide information on the early stage events of self-assembly of an amyloidogenic protein, during the so-called lag phase, stopped-flow time-resolved small angle x-ray scattering (SAXS) experiments were performed. Using a global fitting analysis, the structural and aggregation properties of the apomyoglobin W7FW14F mutant, which is monomeric and partly folded at acidic pH but forms amyloid fibrils after neutralization, were derived from the first few milliseconds onward. SAXS data indicated that the first aggregates appear in less than 20 ms after the pH jump to neutrality and further revealed the simultaneous presence of diverse species. In particular, worm-like unstructured monomers, very large assemblies, and elongated particles were detected, and their structural features and relative concentrations were derived as a function of time on the basis of our model. The final results show that, during the lag phase, early assembling occurs due to the presence of transient monomeric species very prone to association and through successive competing aggregation and rearrangement processes leading to coexisting on-pathway and off-pathway transient species.

  4. A high time resolution x-ray diagnostic on the Madison Symmetric Torus

    Science.gov (United States)

    DuBois, Ami M.; Lee, John David; Almagri, Abdulgadar F.

    2015-07-01

    A new high time resolution x-ray detector has been installed on the Madison Symmetric Torus (MST) to make measurements around sawtooth events. The detector system is comprised of a silicon avalanche photodiode, a 20 ns Gaussian shaping amplifier, and a 500 MHz digitizer with 14-bit sampling resolution. The fast shaping time diminishes the need to restrict the amount of x-ray flux reaching the detector, limiting the system dead-time. With a much higher time resolution than systems currently in use in high temperature plasma physics experiments, this new detector has the versatility to be used in a variety of discharges with varying flux and the ability to study dynamics on both slow and fast time scales. This paper discusses the new fast x-ray detector recently installed on MST and the improved time resolution capabilities compared to the existing soft and hard x-ray diagnostics. In addition to the detector hardware, improvements to the detector calibration and x-ray pulse identification software, such as additional fitting parameters and a more sophisticated fitting routine are discussed. Finally, initial data taken in both high confinement and standard reversed-field pinch plasma discharges are compared.

  5. Diagnostics for an XUV/soft x-ray laser

    International Nuclear Information System (INIS)

    Kauffman, R.L.; Matthews, D.L.; Ceglio, N.; Medecki, H.

    1984-01-01

    We have begun investigating the production of an XUV/soft x-ray laser, using our high-powered glass lasers as drivers. A major diagnostic for lasing is the measure of the absolute power produced in the lasing line. I have developed a spectrograph to time-resolved lasing lines in the energy range from 50 eV to greater than 200 eV. the spectrograph combines a transmission grating and x-ray streak camera to produce a flat field instrument. A cylindrical mirror is used in front of the grating to image the source and act as a collecting optic. The efficiency of the components is calibrated so that absolute intensities can be measured. I will compare the performance of this instrument with reflection grating systems. I will also discuss planned improvements to the system which should increase total throughput, image quality, and resolving power

  6. X-ray time and spectral variability as probes of ultraluminous x-ray sources

    Science.gov (United States)

    Pasham, Dheeraj Ranga Reddy

    A long-standing debate in the field of ultraluminous X-ray sources (ULXs: luminosities > 3x1039 ergs s-1) is whether these objects are powered by stellar-mass black holes (mass range of 3-25 solar masses) undergoing hyper-accretion/emission or if they host the long-sought after class of intermediate-mass black holes (mass range of a few 100-1000 solar masses) accreting material at sub-Eddington rates. We present X-ray time and energy spectral variability studies of ULXs in order to understand their physical environments and accurately weigh their compact objects. A sample of ULXs exhibit quasi-periodic oscillations (QPOs) with centroid frequencies in the range of 10-200 mHz. The nature of the power density spectra (PDS) of these sources is qualitatively similar to stellar-mass black holes when they exhibit the so-called type-C low-frequency QPOs (frequency range of 0.2-15 Hz). However, the crucial difference is that the characteristic frequencies within the PDS of ULXs, viz., the break frequencies and the centroid frequencies of the QPOs, are scaled down by a factor of approximately 10-100 compared to stellar-mass black holes. It has thus been argued that the ULX mHz QPOs are the type-C low-frequency QPO analogs of stellar-mass black holes and that the observed difference in the frequencies (a fewx0.01 Hz compared with a few Hz) is due to the presence of intermediate-mass black holes ( MULX = (QPOstellar-mass black hole }/QPOULX)xM stellar-mass black hole, where M and QPO are the mass and the QPO frequency, respectively) within these ULXs. We analyzed all the archival XMM-Newton X-ray data of ULXs NGC 5408 X-1 and M82 X-1 in order to test the hypothesis that the ULX mHz QPOs are the type-C analogs by searching for a correlation between the mHz QPO frequency and the energy spectral power-law index as type-C QPOs show such a dependence. From our multi-epoch timing and spectral analysis of ULXs NGC 5408 X-1 and M82 X-1, we found that the mHz QPOs of these sources vary

  7. Structural, microstructural and Mössbauer studies of nanocrystalline Fe100-x Alx powders elaborated by mechanical alloying

    Directory of Open Access Journals (Sweden)

    Akkouche K.

    2012-06-01

    Full Text Available Nanocrystalline Fe100-xAlx powders (x= 25, 30, 34 and 40 at % were prepared by the mechanical alloying process using a vario-planetary high-energy ball mill for a milling time of 35 h. The formation and physical properties of the alloys were investigated as a function of Al content by means of X-ray diffraction, scanning electron microscopy (SEM, energy dispersive X-ray and Mössbauer spectroscopy. For all Fe100-xAlx samples, the complete formation of bcc phase was observed after 35 h of milling. As Al content increases, the lattice parameter increases, whereas the grain size decreases from 106 to 12 nm. The powder particle morphology for different compositions was observed by SEM. The Mössbauer spectra were adjusted with a singlet line and a sextet containing two components. The singlet was attributed to the formation of paramagnetic A2 disordered structure rich with Al. About the sextet, the first component indicated the formation of Fe clusters/ Fe-rich phases; however, the second component is characteristic of disordered ferromagnetic phase.

  8. Review - X-ray diffraction measurements in high magnetic fields and at high temperatures

    Directory of Open Access Journals (Sweden)

    Yoshifuru Mitsui, Keiichi Koyama and Kazuo Watanabe

    2009-01-01

    Full Text Available A system was developed measuring x-ray powder diffraction in high magnetic fields up to 5 T and at temperatures from 283 to 473 K. The stability of the temperature is within 1 K over 6 h. In order to examine the ability of the system, the high-field x-ray diffraction measurements were carried out for Si and a Ni-based ferromagnetic shape-memory alloy. The results show that the x-ray powder diffraction measurements in high magnetic fields and at high temperatures are useful for materials research.

  9. Deflection gating for time-resolved x-ray magnetic circular dichroism-photoemission electron microscopy using synchrotron radiation

    Science.gov (United States)

    Wiemann, C.; Kaiser, A. M.; Cramm, S.; Schneider, C. M.

    2012-06-01

    In this paper, we present a newly developed gating technique for a time-resolving photoemission microscope. The technique makes use of an electrostatic deflector within the microscope's electron optical system for fast switching between two electron-optical paths, one of which is used for imaging, while the other is blocked by an aperture stop. The system can be operated with a switching time of 20 ns and shows superior dark current rejection. We report on the application of this new gating technique to exploit the time structure in the injection bunch pattern of the synchrotron radiation source BESSY II at Helmholtz-Zentrum Berlin for time-resolved measurements in the picosecond regime.

  10. Molecular Packing of Amphiphilic Nanosheets Resolved by X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Harutyunyan, Boris; Dannenhoffer, Adam; Kewalramani, Sumit; Aytun, Taner; Fairfield, Daniel J.; Stupp, Samuel I.; Bedzyk, Michael J. (NWU)

    2016-12-29

    Molecular packing in light harvesting 2D assemblies of photocatalytic materials is a critical factor for solar-to-fuel conversion efficiency. However, structure–function correlations have yet to be fully established. This is partly due to the difficulties in extracting the molecular arrangements from the complex 3D powder averaged diffraction patterns of 2D lattices, obtained via in situ wide-angle X-ray scattering. Here, we develop a scattering theory formalism and couple it with a simple geometrical model for the molecular shape of chromophore 9-methoxy-N-(sodium hexanoate)perylene-3,4-dicarboximide (MeO-PMI) used in our study. This generally applicable method fully reproduces the measured diffraction pattern including the asymmetric line shapes for the Bragg reflections and yields the molecular packing arrangement within a 2D crystal structure with a remarkable degree of detail. We find an approximate edge-centered herringbone structure for the PMI fused aromatic rings and ordering of the carboxypentyl chains above and below the nanosheets. Such a packing arrangement differs from the more symmetric face-to-face orientation of the unsubstituted PMI rings. This structural difference is correlated to our measurement of the reduced catalytic performance of MeO-PMI nanosheets as compared to the mesoscopically similar unsubstituted PMI assemblies.

  11. X-ray emission from stainless steel foils irradiated by femtosecond petawatt laser pulses

    Science.gov (United States)

    Alkhimova, M. A.; Faenov, A. Ya; Pikuz, T. A.; Skobelev, I. Yu; Pikuz, S. A.; Nishiuchi, M.; Sakaki, H.; Pirozhkov, A. S.; Sagisaka, S.; Dover, N. P.; Kondo, Ko; Ogura, K.; Fukuda, Y.; Kiriyama, H.; Esirkepov, T.; Bulanov, S. V.; Andreev, A.; Kando, M.; Zhidkov, A.; Nishitani, K.; Miyahara, T.; Watanabe, Y.; Kodama, R.; Kondo, K.

    2018-01-01

    We report about nonlinear growth of x-ray emission intensity emitted from plasma generated by femtosecond petawatt laser pulses irradiating stainless steel foils. X-ray emission intensity increases as ˜ I 4.5 with laser intensity I on a target. High spectrally resolved x-ray emission from front and rear surfaces of 5 μm thickness stainless steel targets were obtained at the wavelength range 1.7-2.1 Å, for the first time in experiments at femtosecond petawatt laser facility J-KAREN-P. Total intensity of front x-ray spectra three times dominates to rear side spectra for maximum laser intensity I ≈ 3.2×1021 W/cm2. Growth of x-ray emission is mostly determined by contribution of bremsstrahlung radiation that allowed estimating bulk electron plasma temperature for various magnitude of laser intensity on target.

  12. Influence of experimental conditions on atom column visibility in energy dispersive X-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Dycus, J.H.; Xu, W.; Sang, X. [Department of Materials Science and Engineering, North Carolina State University, 911 Partners Way Engineering Building 1, Raleigh, NC 27606 (United States); D' Alfonso, A.J. [School of Physics, University of Melbourne, Parkville, Victoria 3010 (Australia); Chen, Z. [School of Physics and Astronomy, Monash University, Clayton, Victoria 3800 (Australia); Weyland, M. [Monash Centre for Electron Microscopy, Monash University, Clayton, Victoria 3800 (Australia); Department of Materials Science and Engineering, Monash University, Clayton, Victoria 3800 (Australia); Allen, L.J. [School of Physics, University of Melbourne, Parkville, Victoria 3010 (Australia); Findlay, S.D. [School of Physics and Astronomy, Monash University, Clayton, Victoria 3800 (Australia); LeBeau, J.M., E-mail: jmlebeau@ncsu.edu [Department of Materials Science and Engineering, North Carolina State University, 911 Partners Way Engineering Building 1, Raleigh, NC 27606 (United States)

    2016-12-15

    Here we report the influence of key experimental parameters on atomically resolved energy dispersive X-ray spectroscopy (EDX). In particular, we examine the role of the probe forming convergence semi-angle, sample thickness, lattice spacing, and dwell/collection time. We show that an optimum specimen-dependent probe forming convergence angle exists to maximize the signal-to-noise ratio of the atomically resolved signal in EDX mapping. Furthermore, we highlight that it can be important to select an appropriate dwell time to efficiently process the X-ray signal. These practical considerations provide insight for experimental parameters in atomic resolution energy dispersive X-ray analysis. - Highlights: • Impacts of microscope operating conditions on EDX signal and atom column contrast are demonstrated. • Influence of sample thickness and lattice spacing is shown. • Conditions for obtaining optimal signal and contrast for different sample types are discussed. • Effects of dwell time during EDX acquisition are discussed.

  13. SUPERORBITAL PHASE-RESOLVED ANALYSIS OF SMC X-1

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Chin-Ping; Chou, Yi; Yang, Ting-Chang; Su, Yi-Hao, E-mail: m929011@astro.ncu.edu.tw, E-mail: yichou@astro.ncu.edu.tw [Graduate Institute of Astronomy, National Central University, Jhongli 32001, Taiwan (China)

    2013-08-10

    The high-mass X-ray binary SMC X-1 is an eclipsing binary with an orbital period of 3.89 days. This system exhibits a superorbital modulation with a period varying between {approx}40 days and {approx}65 days. The instantaneous frequency and the corresponding phase of the superorbital modulation can be obtained by a recently developed time-frequency analysis technique, the Hilbert-Huang transform (HHT). We present a phase-resolved analysis of both the spectra and the orbital profiles with the superorbital phase derived from the HHT. The X-ray spectra observed by the Proportional Counter Array on board the Rossi X-ray Timing Explorer are fitted well by a blackbody plus a Comptonized component. The plasma optical depth, which is a good indicator of the distribution of material along the line of sight, is significantly anti-correlated with the flux detected at 2.5-25 keV. However, the relationship between the plasma optical depth and the equivalent width of the iron line is not monotonic. There is no significant correlation for fluxes higher than {approx}35 mCrab but clear positive correlation when the intensity is lower than {approx}20 mCrab. This indicates that the iron line production is dominated by different regions of this binary system in different superorbital phases. To study the dependence of the orbital profile on the superorbital phase, we obtained the eclipse profiles by folding the All Sky Monitor light curve with the orbital period for different superorbital states. A dip feature, similar to the pre-eclipse dip in Her X-1, lying at orbital phase {approx}0.6-0.85, was discovered during the superorbital transition state. This indicates that the accretion disk has a bulge that absorbs considerable X-ray emission in the stream-disk interaction region. The dip width is anti-correlated with the flux, and this relation can be interpreted by the precessing tilted accretion disk scenario.

  14. Growth and Characterization of La1-x Mnx O3 (x=0.01 mol) Powder and Fibre

    International Nuclear Information System (INIS)

    Yin Yin Win; Pwint Yee Thein; Than Than Win; Yin Maung Maung; Ko Ko Kyaw Soe

    2010-12-01

    An improved method is proposed for the preparation of Ianthanum manganite (LaMaO3) powder by the calcinations of a composite carbonate of the respective metallic elements formed by mixing an aqueous solution of a water-soluble ammonium carbonate and an aqueous solution of inorganic salts, e.g, chlorides, of the respective metallic elements. The surface morphology of the LaMnO3 is studied by scanning electron microscopy (SEM), X-rays fluorescent (XRF) technique is used for chemical analysis. Structural properties are characterized by X-rays Diffraction (XRD). Chemical and physical reaction of LaMnO3 powder is investigated by Thermogravimetric Analysis-Differential Thermal Analysis (TGA-DTA). Electrospun LaMnO3 fibre is formed on Al-foil and their characteristic is examined by SEM and XRD.

  15. Soft X-ray radiation power characteristics of tungsten wire arrays on Yang accelerator

    International Nuclear Information System (INIS)

    Zhang Siqun; Ouyang Kai; Huang Xianbin; Dan Jiakun; Zhou Rongguo; Yang Liang

    2013-01-01

    A series of experiments were carried out to research the X-ray radiation characteristics of tungsten wire arrays on Yang accelerator. In those experiments, we charged the Marx generator of 60 kV, and the load current of 0.85-1.00 MA, the rise time of 75-90 ns (10%-90%). A soft X-ray scintillator powermeter which responded flatly to 50-1800 eV X-rays was used to measure the power of soft X-ray emitted from implosion plasma. In this paper, we present the measuring results of time-resolved soft X-ray radiation power, and discuss the radiation characteristics of implosion plasma by analyzing the correlations of soft X-ray radiant power and the diameter, length, wire number of the tungsten wire arrays. The optimizing wire array configuration parameters on Yang are as follows: 8 mm array diameter, 15 mm wire length, and 24 wire number. We also present the radiant power difference in radial and axial directions of the wire arrays. (authors)

  16. X-ray studies, spectral characterization and thermal behaviour of a ...

    African Journals Online (AJOL)

    HP04)3]. H20, I, was synthesized by reacting Zn2+ ions with tris-(2-aminoethyl) amine phosphate [C6H21N4][P04].5H20. The compound was characterized by powder x-ray diffraction analysis, energy dispersive analysis by x-ray and infrared ...

  17. Soft x-ray measurements from the PDX tokamak

    International Nuclear Information System (INIS)

    Silver, E.H.; Bitter, M.; Brau, K.; Eames, D.; Greenberger, A.; Hill, K.W.; Meade, D.M.; Roney, W.; Sauthoff, N.R.; von Goeler, S.

    1982-05-01

    Temporally and spatially-resolved profiles of the PDX soft x-ray spectra have been measured during single tokamak pulses of circular and divertor plasmas with a recently developed pulse height analyzer. This detection system incorporates an array of five vertically displaced sets of lithium-drifted silicon detectors, each consisting of three independent channels optimized for rapid data collection in adjacent energy regions. Simultaneous measurement of x-ray emission integrated along five chords of the plasma cross section can thereby be achieved. Abel inversion of these data yields temporally-resolved radial profiles of the local electron temperature from the slope of the continuum, concentrations of high-Z impurities from the characteristic line intensities, and a measure of Z/sub eff/ from the continuum intensity. The techniques of x-ray pulse height analysis, with illustrations featuring the results from the initial PDX circular plasma experiments are discussed in detail. In addition, comparisons between circular and divertor plasmas on PDX, derived from the x-ray measurements, are also presented

  18. Considerations for a soft x-ray spectromicroscopy beamline

    International Nuclear Information System (INIS)

    Winn, B.; Hao, X.; Jacobsen, C.

    1996-01-01

    The X-1A soft x-ray undulator at the NSLS is the source for the experimental programs in spectromicroscopy. The authors require both spatial and temporal coherence. Due to the relatively large horizontal divergence of the electron beam in the low β straight section of the x-ray storage ring, it has been possible to split the beam using a scraping mirror into two branches: X-1A used by the authors' program and X-1B used for high resolution spectroscopy. They are now rebuilding the X-1A beamline to provide improved resolving power and essentially linear trade-off between photon rate at the zone plate and resolving power for the soft x-ray spectromicroscopy experiments. This new beamline will exploit both additional floorspace due to the NSLS building expansion and increases in the brightness of the x-ray ring. The beam will be further split into two separate beamlines, both of which will use toroidal mirrors to focus the source on the monochromator entrance slits horizontally and to focus on the monochromator exit slits vertically. This separation comes at no loss of coherent flux and permits low thermal loading on the optics, since the authors need little more than the coherent fraction of the beam at the Fresnel zone plate for microfocusing. Because of the small angular acceptance for spatially coherent illumination of the zone plates and the use of an approximately satisfied Rowland condition, the monochromators have sufficient resolving power with fixed exit arms. Experiments can then be placed near the exit slits, with spatial coherence established by the exit slit size. Resolving power will be controlled by adjusting the entrance slit alone with no change of spatial coherence. The zone plates will be overfilled to be less sensitive to beam vibration and drift

  19. Moving the Frontier of Quantum Control into the Soft X-Ray Spectrum

    Directory of Open Access Journals (Sweden)

    A. Aquila

    2011-01-01

    Full Text Available The femtosecond nature of X-ray free electron laser (FEL pulses opens up exciting research possibilities in time-resolved studies including femtosecond photoemission and diffraction. The recent developments of seeding X-ray FELs extend their capabilities by creating stable, temporally coherent, and repeatable pulses. This in turn opens the possibility of spectral engineering soft X-ray pulses to use as a probe for the control of quantum dynamics. We propose a method for extending coherent control pulse-shaping techniques to the soft X-ray spectral range by using a reflective geometry 4f pulse shaper. This method is based on recent developments in asymmetrically cut multilayer optic technology and piezoelectric substrates.

  20. Single shot diffraction of picosecond 8.7-keV x-ray pulses

    Directory of Open Access Journals (Sweden)

    F. H. O’Shea

    2012-02-01

    Full Text Available We demonstrate multiphoton, single shot diffraction images of x rays produced by inverse Compton scattering a high-power CO_{2} laser from a relativistic electron beam, creating a pulse of 8.7 keV x rays. The tightly focused, relatively high peak brightness electron beam and high photon density from the 2 J CO_{2} laser yielded 6×10^{7} x-ray photons over the full opening angle in a single shot. Single shot x-ray diffraction is performed by passing the x rays though a vertical slit and on to a flat silicon (111 crystal. 10^{2} diffracted photons were detected. The spectrum of the detected x rays is compared to simulation. The diffraction and detection of 10^{2} x rays is a key step to a more efficient time resolved diagnostic in which the number of observed x rays might reach 10^{4}; enabling a unique, flexible x-ray source as a sub-ps resolution diagnostic for studying the evolution of chemical reactions, lattice deformation and melting, and magnetism.

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

    International Nuclear Information System (INIS)

    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

  2. X-ray scattering of soft matter

    International Nuclear Information System (INIS)

    Stribeck, N.

    2007-01-01

    This coherently written volume summarizes the analytical power of modern X-ray scattering in the field of soft matter. Applications of X-ray scattering to soft matter have advanced considerably within recent years, both conceptually and technically. There are now mature high-power X-ray sources, synchrotrons and rotating anodes, as well as high-speed detectors, which have become readily available and which make the whole process more viable. High-quality time-resolved experiments on polymer structure can now be performed with ease, a major advancement due to the genuine power of the scattering method. This manual is a detailed description of simple tools that can elucidate the mechanisms of structure evolution in the studied materials. It is also a step-by-step guide to more advanced methods of the latest X-ray scattering techniques, and breaks down these methods. Data analysis based on clear, unequivocal results is rendered simple and straightforward - with a stress on the careful planning of experiments and adequate recording of all required data. This book, then, serves as a useful ready-reference guide. It has been written for the modern scientist who is a generalist and needs a concise reference, and demonstrates typical errors in data evaluation. (orig.)

  3. Ultrafast x-ray scattering on nanoparticle dynamics

    International Nuclear Information System (INIS)

    Plech, A; Ibrahimkutty, S; Issenmann, D; Kotaidis, V; Siems, A

    2013-01-01

    Pulsed X-ray scattering is used for the determination of structural dynamics of laser-irradiated gold particles. By combining several scattering methods such as powder scattering, small angle scattering and diffuse wide angle scattering it is possible to reconstruct the kinetics of structure evolution on several lengths scales and derive complementary information on the particles and their local environment. A generic structural phase diagram for the reaction as function of delay time after laser excitation and laser fluence can be constructed.

  4. A deep X-ray view of the bare AGN Ark 120. III. X-ray timing analysis and multiwavelength variability

    Science.gov (United States)

    Lobban, A. P.; Porquet, D.; Reeves, J. N.; Markowitz, A.; Nardini, E.; Grosso, N.

    2018-03-01

    We present the spectral/timing properties of the bare Seyfert galaxy Ark 120 through a deep ˜420 ks XMM-Newton campaign plus recent NuSTAR observations and a ˜6-month Swift monitoring campaign. We investigate the spectral decomposition through fractional rms, covariance and difference spectra, finding the mid- to long-time-scale (˜day-year) variability to be dominated by a relatively smooth, steep component, peaking in the soft X-ray band. Additionally, we find evidence for variable Fe K emission redward of the Fe Kα core on long time-scales, consistent with previous findings. We detect a clearly defined power spectrum which we model with a power law with a slope of α ˜ 1.9. By extending the power spectrum to lower frequencies through the inclusion of Swift and Rossi X-ray Timing Explorer data, we find tentative evidence of a high-frequency break, consistent with existing scaling relations. We also explore frequency-dependent Fourier time lags, detecting a negative (`soft') lag for the first time in this source with the 0.3-1 keV band lagging behind the 1-4 keV band with a time delay, τ, of ˜900 s. Finally, we analyse the variability in the optical and ultraviolet (UV) bands using the Optical/UV Monitor onboard XMM-Newton and the Ultra-Violet/Optical Telescope onboard Swift and search for time-dependent correlations between the optical/UV/X-ray bands. We find tentative evidence for the U-band emission lagging behind the X-rays with a time delay of τ = 2.4 ± 1.8 d, which we discuss in the context of disc reprocessing.

  5. Structure of La2Cu2O5 by high-resolution synchrotron X-ray powder diffraction

    International Nuclear Information System (INIS)

    La Placa, S.J.; Bringley, J.F.; Scott, B.A.; Cox, D.E.

    1993-01-01

    Dicopper(II) dilanthanum pentaoxide, La 2 Cu 2 O 5 , M r =484.90, orthorhombic, Pbam. At T=300 K: a=5.5490(1), b=10.4774(2), c=3.8796(1) A, V=225.557(8) A 3 , Z=2, D x =7.139 g cm -3 , λ=1.2000 A. Final R I =6.20, R p =14.6 and R wp =20.61%, 124 independent reflections observed. The structure has been refined from high-resolution synchrotron X-ray powder diffraction data using the Rietveld method. It is of the oxygen-defect perovskite type and is composed entirely of corner-shared CuO 5 square pyramids, which share oxygen vacancies forming vacancy tunnels along the c axis. The La atoms reside at a perovskite-like A-site and are tenfold coordinated by oxygen. (orig.)

  6. Soft X-ray excited colour-centre luminescence and XANES studies of calcium oxide

    International Nuclear Information System (INIS)

    Ko, J.Y.P.; Heigl, F.; Yiu, Y.M.; Zhou, X.-T.; Regier, T.; Blyth, R.I.R.; Sham, T.-K.

    2007-01-01

    In this study, we show that colour centres can be produced by irradiating calcium oxide with soft X-rays from a synchrotron radiation source. Using the X-ray excited optical Iuminescence (XEOL) technique, two colour centres, F-centre, and F + -centre can be identified. These colour centres emit photons at characteristic wavelengths. In addition, by performing time-resolved XEOL (TRXEOL), we are able to reveal timing and decay characteristics of the colour centres. We also present X-ray absorption near-edge structure (XANES) spectra collected across oxygen K-edge, calcium L 3,2 -edge, and calcium K-edge. Experimental results are compared with density functional theory (DFT) calculations. (author)

  7. X-Ray Calorimeter Arrays for Astrophysics

    Science.gov (United States)

    Kilbourne, Caroline A.

    2009-01-01

    High-resolution x-ray spectroscopy is a powerful tool for studying the evolving universe. The grating spectrometers on the XMM and Chandra satellites started a new era in x-ray astronomy, but there remains a need for instrumentation that can provide higher spectral resolution with high throughput in the Fe-K band (around 6 keV) and can enable imaging spectroscopy of extended sources, such as supernova remnants and galaxy clusters. The instrumentation needed is a broad-band imaging spectrometer - basically an x-ray camera that can distinguish tens of thousands of x-ray colors. The potential benefits to astrophysics of using a low-temperature calorimeter to determine the energy of an incident x-ray photon via measurement of a small change in temperature was first articulated by S. H. Moseley over two decades ago. In the time since, technological progress has been steady, though full realization in an orbiting x-ray telescope is still awaited. A low-temperature calorimeter can be characterized by the type of thermometer it uses, and three types presently dominate the field. The first two types are temperature-sensitive resistors - semiconductors in the metal-insulator transition and superconductors operated in the superconducting-normal transition. The third type uses a paramagnetic thermometer. These types can be considered the three generations of x-ray calorimeters; by now each has demonstrated a resolving power of 2000 at 6 keV, but only a semiconductor calorimeter system has been developed to spaceflight readiness. The Soft X-ray Spectrometer on Astro-H, expected to launch in 2013, will use an array of silicon thermistors with I-IgTe x-ray absorbers that will operate at 50 mK. Both the semiconductor and superconductor calorimeters have been implemented in small arrays, kilo-pixel arrays of the superconducting calorimeters are just now being produced, and it is anticipated that much larger arrays will require the non-dissipative advantage of magnetic thermometers.

  8. The Large Observatory For x-ray Timing

    DEFF Research Database (Denmark)

    Feroci, M.; Herder, J. W. den; Bozzo, E.

    2014-01-01

    The Large Observatory For x-ray Timing (LOFT) was studied within ESA M3 Cosmic Vision framework and participated in the final down-selection for a launch slot in 2022-2024. Thanks to the unprecedented combination of effective area and spectral resolution of its main instrument, LOFT will study th...

  9. Solid state characterization and crystal structure from X-ray powder diffraction of two polymorphic forms of ranitidine base.

    Science.gov (United States)

    de Armas, Héctor Novoa; Peeters, Oswald M; Blaton, Norbert; Van Gyseghem, Elke; Martens, Johan; Van Haele, Gerrit; Van Den Mooter, Guy

    2009-01-01

    Ranitidine hydrochloride (RAN-HCl), a known anti-ulcer drug, is the product of reaction between HCl and ranitidine base (RAN-B). RAN-HCl has been extensively studied; however this is not the case of the RAN-B. The solid state characterization of RAN-B polymorphs has been carried out using different analytical techniques (microscopy, thermal analysis, Fourier transform infrared spectrometry in the attenuated total reflection mode, (13)C-CPMAS-NMR spectroscopy and X-ray powder diffraction). The crystal structures of RAN-B form I and form II have been determined using conventional X-ray powder diffraction in combination with simulated annealing and whole profile pattern matching, and refined using rigid-body Rietveld refinement. RAN-B form I is a monoclinic polymorph with cell parameters: a = 7.317(2), b = 9.021(2), c = 25.098(6) A, beta = 95.690(1) degrees and space group P2(1)/c. The form II is orthorhombic: a = 31.252(4), b = 13.052(2), c = 8.0892(11) A with space group Pbca. In RAN-B polymorphs, the nitro group is involved in a strong intramolecular hydrogen bond responsible for the existence of a Z configuration in the enamine portion of the molecules. A tail to tail packing motif can be denoted via intermolecular hydrogen bonds. The crystal structures of RAN-B forms are compared to those of RAN-HCl polymorphs. RAN-B polymorphs are monotropic polymorphic pairs. (c) 2008 Wiley-Liss, Inc. and the American Pharmacists Association

  10. Thermal management of next-generation contact-cooled synchrotron x-ray mirrors

    Energy Technology Data Exchange (ETDEWEB)

    Khounsary, A.

    1999-10-29

    In the past decade, several third-generation synchrotrons x-ray sources have been constructed and commissioned around the world. Many of the major problems in the development and design of the optical components capable of handling the extremely high heat loads of the generated x-ray beams have been resolved. It is expected, however, that in the next few years even more powerful x-ray beams will be produced at these facilities, for example, by increasing the particle beam current. In this paper, the design of a next generation of synchrotron x-ray mirrors is discussed. The author shows that the design of contact-cooled mirrors capable of handing x-ray beam heat fluxes in excess of 500 W/mm{sup 2} - or more than three times the present level - is well within reach, and the limiting factor is the thermal stress rather then thermally induced slope error.

  11. Microwave-assisted hydrothermal synthesis of lead zirconate fine powders

    Directory of Open Access Journals (Sweden)

    Apinpus Rujiwatra

    2011-01-01

    Full Text Available A rapid synthesis of lead zirconate fine powders by microwave-assisted hydrothermal technique is reported. The influences of type of lead precursor, concentration of potassium hydroxide mineraliser, applied microwave power and irradiation time are described. The synthesised powders were characterised by powder X-ray diffraction, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopic microanalysis and light scattering technique. The merits of the microwave application in reducing reaction time and improving particle mono-dispersion and size uniformity as well as the drawbacks, viz. low purity of the desired phase and increasing demand of mineraliser, are discussed in relation to conventional heating method.

  12. Attosecond time-energy structure of X-ray free-electron laser pulses

    Science.gov (United States)

    Hartmann, N.; Hartmann, G.; Heider, R.; Wagner, M. S.; Ilchen, M.; Buck, J.; Lindahl, A. O.; Benko, C.; Grünert, J.; Krzywinski, J.; Liu, J.; Lutman, A. A.; Marinelli, A.; Maxwell, T.; Miahnahri, A. A.; Moeller, S. P.; Planas, M.; Robinson, J.; Kazansky, A. K.; Kabachnik, N. M.; Viefhaus, J.; Feurer, T.; Kienberger, R.; Coffee, R. N.; Helml, W.

    2018-04-01

    The time-energy information of ultrashort X-ray free-electron laser pulses generated by the Linac Coherent Light Source is measured with attosecond resolution via angular streaking of neon 1s photoelectrons. The X-ray pulses promote electrons from the neon core level into an ionization continuum, where they are dressed with the electric field of a circularly polarized infrared laser. This induces characteristic modulations of the resulting photoelectron energy and angular distribution. From these modulations we recover the single-shot attosecond intensity structure and chirp of arbitrary X-ray pulses based on self-amplified spontaneous emission, which have eluded direct measurement so far. We characterize individual attosecond pulses, including their instantaneous frequency, and identify double pulses with well-defined delays and spectral properties, thus paving the way for X-ray pump/X-ray probe attosecond free-electron laser science.

  13. Imaging Molecular Motion: Femtosecond X-Ray Scattering of an Electrocyclic Chemical Reaction

    Science.gov (United States)

    Minitti, M. P.; Budarz, J. M.; Kirrander, A.; Robinson, J. S.; Ratner, D.; Lane, T. J.; Zhu, D.; Glownia, J. M.; Kozina, M.; Lemke, H. T.; Sikorski, M.; Feng, Y.; Nelson, S.; Saita, K.; Stankus, B.; Northey, T.; Hastings, J. B.; Weber, P. M.

    2015-06-01

    Structural rearrangements within single molecules occur on ultrafast time scales. Many aspects of molecular dynamics, such as the energy flow through excited states, have been studied using spectroscopic techniques, yet the goal to watch molecules evolve their geometrical structure in real time remains challenging. By mapping nuclear motions using femtosecond x-ray pulses, we have created real-space representations of the evolving dynamics during a well-known chemical reaction and show a series of time-sorted structural snapshots produced by ultrafast time-resolved hard x-ray scattering. A computational analysis optimally matches the series of scattering patterns produced by the x rays to a multitude of potential reaction paths. In so doing, we have made a critical step toward the goal of viewing chemical reactions on femtosecond time scales, opening a new direction in studies of ultrafast chemical reactions in the gas phase.

  14. X-Ray powder diffractometry, crystallographic phase analysis and ...

    African Journals Online (AJOL)

    Computerized X-Ray diffraction system has been used to determine the composition and lattice parameters of raw and activated kaolinite. The universal diffractometry URD 63 was interfaced with computer via an APX 63 software package for rapid capturing of data on reflected intensity and other crystallographic ...

  15. Time variability of X-ray binaries: observations with INTEGRAL. Modeling

    International Nuclear Information System (INIS)

    Cabanac, Clement

    2007-01-01

    The exact origin of the observed X and Gamma ray variability in X-ray binaries is still an open debate in high energy astrophysics. Among others, these objects are showing aperiodic and quasi-periodic luminosity variations on timescales as small as the millisecond. This erratic behavior must put constraints on the proposed emission processes occurring in the vicinity of the neutrons star or the stellar mass black-hole held by these objects. We propose here to study their behavior following 3 different ways: first we examine the evolution of a particular X-ray source discovered by INTEGRAL, IGR J19140+0951. Using timing and spectral data given by different instruments, we show that the source type is plausibly consistent with a High Mass X-ray Binary hosting a neutrons star. Subsequently, we propose a new method dedicated to the study of timing data coming from coded mask aperture instruments. Using it on INTEGRAL/ISGRI real data, we detect the presence of periodic and quasi-periodic features in some pulsars and micro-quasars at energies as high as a hundred keV. Finally, we suggest a model designed to describe the low frequency variability of X-ray binaries in their hardest state. This model is based on thermal comptonization of soft photons by a warm corona in which a pressure wave is propagating in cylindrical geometry. By computing both numerical simulations and analytical solution, we show that this model should be suitable to describe some of the typical features observed in X-ray binaries power spectra in their hard state and their evolution such as aperiodic noise and low frequency quasi-periodic oscillations. (author) [fr

  16. X-ray fluorescence spectroscopic determination of heavy metals and ...

    African Journals Online (AJOL)

    Purpose: To determine the heavy metal and trace element composition of the powdered aerial parts of Origanum sipyleum L. and its water extract. Methods: The heavy metal and trace elements content of the powdered plant material and 2 % aqueous extract were evaluated by x-ray fluorescence spectroscopy with silicon ...

  17. Structural and microstructural changes during anion exchange of CoAl layered double hydroxides: an in situ X-ray powder diffraction study

    DEFF Research Database (Denmark)

    Johnsen, Rune; Krumeich, Frank; Norby, Poul

    2010-01-01

    Anion-exchange processes in cobalt-aluminium layered double hydroxides (LDHs) were studied by in situ synchrotron X-ray powder diffraction (XRPD). The processes investigated were CoAl-CO3 CoAl-Cl CoAl-CO3, CoAl-Cl CoAl-NO3 and CoAl-CO3 CoAl-SO4. The XRPD data show that the CoAl-CO3 CoAl-Cl process...

  18. Thermoluminescent dosemeter in a X-ray diffractometer; Dosimetria termoluminiscente en un difractometro de rayos X

    Energy Technology Data Exchange (ETDEWEB)

    Mendoza A, D.; Gonzalez M, P.; Falcon B, T. [Instituto Nacional de Investigaciones Nucleares, A.P. 18-1027, Mexico D.F. (Mexico); Castano, V.M. [Instituto de Fisica, UNAM, Laboratorio Juriquilla, A.P. 1-1010, C.P. 76001, Queretaro (Mexico)

    1999-07-01

    In this work it was presented the results obtained of the dosimetry which was realized in a X-ray diffractometer for powders, trademark Siemens D5000, using the thermoluminescent signal generated by the X-rays in the commercial dosemeter TLD-100 of Harshaw, US. In according to the results obtained, the radiation quantity received by an analysed material in the diffractometer, will be proportional to exposure time and it can vary from unities until tenths of grays. These results are very outstanding when are analysed crystalline materials in a diffractometer, for knowing the present crystalline phases, mainly if these are highly sensitive to the ionizing radiation, as it is the case of the thermoluminescent materials. (Author)

  19. On the Nature of the mHz X-Ray QPOs from ULX M82 X-1: Evidence for Timing-Spectral (anti) Correlation

    Science.gov (United States)

    Pasham, Dheeraj R.; Strohmayer, Tod E.

    2013-01-01

    Using all the archival XMM-Newton X-ray (3-10 keV) observations of the ultraluminous X-ray source (ULX) M82 X-1 we searched for a correlation between its variable mHz quasi-periodic oscillation (QPO) frequency and its energy spectral power-law index. These quantities are known to correlate in stellar mass black holes (StMBHs) exhibiting Type-C QPOs (approx 0.2-15 Hz). The detection of such a correlation would strengthen the identification of its mHz QPOs as Type-C and enable a more reliable mass estimate by scaling its QPO frequencies to those of Type-C QPOs in StMBHs of known mass. We resolved the count rates of M82 X-1 and a nearby bright ULX (source 5/X42.3+59) through surface brightness modeling and identify observations in which M82 X-1 was at least as bright as source 5. Using only those observations, we detect QPOs in the frequency range of 36-210 mHz during which the energy spectral power-law index varied from 1.7-2.2. Interestingly, we find evidence for an anti-correlation (Pearsons correlation coefficient = -0.95) between the power-law index and the QPO centroid frequency. While such an anti-correlation is observed in StMBHs at high Type-C QPO frequencies (approx 5-15 Hz), the frequency range over which it holds in StMBHs is significantly smaller (factor of approx 1.5-3) than the QPO range reported here from M82 X-1 (factor of 6). However, it remains possible that contamination from source 5 can bias our result. Joint Chandra/XMM-Newton observations in the future can resolve this problem and confirm the timing-spectral anti-correlation reported here.

  20. Spectral encoding method for measuring the relative arrival time between x-ray/optical pulses

    International Nuclear Information System (INIS)

    Bionta, M. R.; Hartmann, N.; Weaver, M.; French, D.; Glownia, J. M.; Bostedt, C.; Chollet, M.; Ding, Y.; Fritz, D. M.; Fry, A. R.; Krzywinski, J.; Lemke, H. T.; Messerschmidt, M.; Schorb, S.; Zhu, D.; White, W. E.; Nicholson, D. J.; Cryan, J. P.; Baker, K.; Kane, D. J.

    2014-01-01

    The advent of few femtosecond x-ray light sources brings promise of x-ray/optical pump-probe experiments that can measure chemical and structural changes in the 10–100 fs time regime. Widely distributed timing systems used at x-ray Free-Electron Laser facilities are typically limited to above 50 fs fwhm jitter in active x-ray/optical synchronization. The approach of single-shot timing measurements is used to sort results in the event processing stage. This has seen wide use to accommodate the insufficient precision of active stabilization schemes. In this article, we review the current technique for “measure-and-sort” at the Linac Coherent Light Source at the SLAC National Accelerator Laboratory. The relative arrival time between an x-ray pulse and an optical pulse is measured near the experimental interaction region as a spectrally encoded cross-correlation signal. The cross-correlation provides a time-stamp for filter-and-sort algorithms used for real-time sorting. Sub-10 fs rms resolution is common in this technique, placing timing precision at the same scale as the duration of the shortest achievable x-ray pulses