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Sample records for situ x-ray reflectivity

  1. In Situ Study of Silicon Electrode Lithiation with X-ray Reflectivity.

    Science.gov (United States)

    Cao, Chuntian; Steinrück, Hans-Georg; Shyam, Badri; Stone, Kevin H; Toney, Michael F

    2016-12-14

    Surface sensitive X-ray reflectivity (XRR) measurements were performed to investigate the electrochemical lithiation of a native oxide terminated single crystalline silicon (100) electrode in real time during the first galvanostatic discharge cycle. This allows us to gain nanoscale, mechanistic insight into the lithiation of Si and the formation of the solid electrolyte interphase (SEI). We describe an electrochemistry cell specifically designed for in situ XRR studies and have determined the evolution of the electron density profile of the lithiated Si layer (LixSi) and the SEI layer with subnanometer resolution. We propose a three-stage lithiation mechanism with a reaction limited, layer-by-layer lithiation of the Si at the LixSi/Si interface.

  2. In situ X-Ray reflectivity measurements during DC sputtering of vanadium carbide thin films

    Energy Technology Data Exchange (ETDEWEB)

    Kaufholz, Marthe; Krause, Baerbel; Kotapati, Sunil; Baumbach, Tilo [ISS, Karlsruher Institute for Technology (Germany); Ulrich, Sven; Stueber, Michael [IAM-AWP, Karlsruher Institute for Technology (Germany)

    2012-07-01

    Vanadium Carbide (VC) is a promising candidate for new hard coatings used e.g. in medical applications. For optimising the coating properties, the relation between the microstructure formation, deposition conditions and mechanical properties has to be understood. In situ X-Ray Reflectivity (XRR) is a powerful tool to investigate the changes in thickness, electron density and roughness during deposition. In situ XRR measurements during sputtering were performed at ANKA (MPI-Beamline). Several VC films were deposited on Si with different growth conditions. Before and after deposition a full specular XRR curve was taken. During sputtering, the intensity changes e.g. due to the thickness increase were measured at fixed angular position of the detector. For the analysis of the angle - and time-dependent XRR a simulation tool is used based on the Parratt Algorithm. This tool can be adapted to other materials and deposition techniques. First measurements show that the electron density of the thin films depends strongly on the plasma properties during the deposition. This might give the possibility of a controlled growth of layers with different electron density by tuning the plasma conditions.

  3. In situ x-ray reflectivity and grazing incidence x-ray diffraction study of L 1(0) ordering in (57)Fe/Pt multilayers.

    Science.gov (United States)

    Raghavendra Reddy, V; Gupta, Ajay; Gome, Anil; Leitenberger, Wolfram; Pietsch, U

    2009-05-06

    In situ high temperature x-ray reflectivity and grazing incidence x-ray diffraction measurements in the energy dispersive mode are used to study the ordered face-centered tetragonal (fct) L 1(0) phase formation in [Fe(19 Å)/Pt(25 Å)]( × 10) multilayers prepared by ion beam sputtering. With the in situ x-ray measurements it is observed that (i) the multilayer structure first transforms to a disordered FePt and subsequently to an ordered fct L 1(0) phase, (ii) the ordered fct L 1(0) FePt peaks start to appear at 320 °C annealing, (iii) the activation energy of the interdiffusion is 0.8 eV and (iv) ordered fct FePt grains have preferential out-of-plane texture. The magneto-optical Kerr effect and conversion electron Mössbauer spectroscopies are used to study the magnetic properties of the as-deposited and 400 °C annealed multilayers. The magnetic data for the 400 °C annealed sample indicate that the magnetization is at an angle of ∼50° from the plane of the film.

  4. Using in situ X-ray reflectivity to study protein adsorption on hydrophilic and hydrophobic surfaces: benefits and limitations.

    Science.gov (United States)

    Richter, Andrew G; Kuzmenko, Ivan

    2013-04-30

    We have employed in situ X-ray reflectivity (IXRR) to study the adsorption of a variety of proteins (lysozyme, cytochrome c, myoglobin, hemoglobin, serum albumin, and immunoglobulin G) on model hydrophilic (silicon oxide) and hydrophobic surfaces (octadecyltrichlorosilane self-assembled monolayers), evaluating this recently developed technique for its applicability in the area of biomolecular studies. We report herein the highest resolution depiction of adsorbed protein films, greatly improving on the precision of previous neutron reflectivity (NR) results and previous IXRR studies. We were able to perform complete scans in 5 min or less with the maximum momentum transfer of at least 0.52 Å(-1), allowing for some time-resolved information about the evolution of the protein film structure. The three smallest proteins (lysozyme, cytochrome c, and myoglobin) were seen to deposit as fully hydrated, nondenatured molecules onto hydrophilic surfaces, with indications of particular preferential orientations. Time evolution was observed for both lysozyme and myoglobin films. The larger proteins were not observed to deposit on the hydrophilic substrates, perhaps because of contrast limitations. On hydrophobic surfaces, all proteins were seen to denature extensively in a qualitatively similar way but with a rough trend that the larger proteins resulted in lower coverage. We have generated high-resolution electron density profiles of these denatured films, including capturing the growth of a lysozyme film. Because the solution interface of these denatured films is diffuse, IXRR cannot unambiguously determine the film extent and coverage, a drawback compared to NR. X-ray radiation damage was systematically evaluated, including the controlled exposure of protein films to high-intensity X-rays and exposure of the hydrophobic surface to X-rays before adsorption. Our analysis showed that standard measuring procedures used for XRR studies may lead to altered protein films

  5. α-Synuclein insertion into supported lipid bilayers as seen by in situ X-ray reflectivity.

    Science.gov (United States)

    Hähl, Hendrik; Möller, Isabelle; Kiesel, Irena; Campioni, Silvia; Riek, Roland; Verdes, Dorinel; Seeger, Stefan

    2015-03-18

    Large aggregates of misfolded α-synuclein inside neuronal cells are the hallmarks of Parkinson's disease. The protein's natural function and its supposed toxicity, however, are believed to be closely related to its interaction with cell and vesicle membranes. Upon this interaction, the protein folds into an α-helical structure and intercalates into the membrane. In this study, we focus on the changes in the lipid bilayer caused by this intrusion. In situ X-ray reflectivity was applied to determine the vertical density structure of the bilayer before and after exposure to α-synuclein. It was found that the α-synuclein insertion, wild type and E57K variant, caused a reduction in bilayer thickness. This effect may be one factor in the membrane pore formation ability of α-synuclein.

  6. In situ x-ray reflectivity studies of dynamics and morphology during heteroepitaxial complex oxide thin film growth.

    Science.gov (United States)

    Dale, Darren; Suzuki, Y; Brock, J D

    2008-07-02

    We present a method, based on refraction effects in continuous, stratified media, for quantitative analysis of specular x-ray reflectivity from interfaces with atomic-scale roughness. Roughness at interfaces has previously been incorporated into this framework via Fourier transform of a continuous height distribution, but this approach breaks down when roughness approaches the atomic scale and manifests discrete character. By modeling the overall roughness at interfaces as a convolution of discrete and continuous height distributions, we have extended the applicability of this reflectivity model to atomic-scale roughness. The parameterization of thickness and roughness enables quantitative analysis of time-resolved in situ reflectivity studies of thin film growth, modeling step-flow, layer-by-layer and three-dimensional growth within a single framework. We present the application of this model to the analysis of anti-Bragg growth oscillations measured in situ during heteroepitaxial growth of La(0.7)Sr(0.3)MnO(3) on [Formula: see text] SrTiO(3) at different temperatures and pressures, and discuss the evolution of surface morphology.

  7. Exploring the interfacial structure of protein adsorbates and the kinetics of protein adsorption: an in situ high-energy X-ray reflectivity study.

    Science.gov (United States)

    Evers, Florian; Shokuie, Kaveh; Paulus, Michael; Sternemann, Christian; Czeslik, Claus; Tolan, Metin

    2008-09-16

    The high energy X-ray reflectivity technique has been applied to study the interfacial structure of protein adsorbates and protein adsorption kinetics in situ. For this purpose, the adsorption of lysozyme at the hydrophilic silica-water interface has been chosen as a model system. The structure of adsorbed lysozyme layers was probed for various aqueous solution conditions. The effect of solution pH and lysozyme concentration on the interfacial structure was measured. Monolayer formation was observed for all cases except for the highest concentration. The adsorbed protein layers consist of adsorbed lysozyme molecules with side-on or end-on orientation. By means of time-dependent X-ray reflectivity scans, the time-evolution of adsorbed proteins was monitored as well. The results of this study demonstrate the capabilities of in situ X-ray reflectivity experiments on protein adsorbates. The great advantages of this method are the broad wave vector range available and the high time resolution.

  8. X-ray induced optical reflectivity

    Directory of Open Access Journals (Sweden)

    Stephen M. Durbin

    2012-12-01

    Full Text Available The change in optical reflectivity induced by intense x-ray pulses can now be used to study ultrafast many body responses in solids in the femtosecond time domain. X-ray absorption creates photoelectrons and core level holes subsequently filled by Auger or fluorescence processes, and these excitations ultimately add conduction and valence band carriers that perturb optical reflectivity. Optical absorption associated with band filling and band gap narrowing is shown to explain the basic features found in recent measurements on an insulator (silicon nitride, Si3N4, a semiconductor (gallium arsenide, GaAs, and a metal (gold, Au, obtained with ∼100 fs x-ray pulses at 500-2000 eV and probed with 800 nm laser pulses. In particular GaAs exhibits an abrupt drop in reflectivity, persisting only for a time comparable to the x-ray excitation pulse duration, consistent with prompt band gap narrowing.

  9. Distribution of barium and fulvic acid at the mica solution interface using in-situ X-ray reflectivity

    Science.gov (United States)

    Lee, Sang Soo; Nagy, Kathryn L.; Fenter, Paul

    2007-12-01

    The interfacial structures of the basal surface of muscovite mica in solutions containing (1) 5 × 10 -3 m BaCl 2, (2) 500 ppm Elliott Soil Fulvic Acid I (ESFA I), (3) 100 ppm Elliott Soil Fulvic Acid II (ESFA II), (4) 100 ppm Pahokee Peat Fulvic Acid I (PPFA), and (5) 5 × 10 -3 m BaCl 2 and 100 ppm ESFA II were obtained with high resolution in-situ X-ray reflectivity. The derived electron-density profile in BaCl 2 shows two sharp peaks near the mica surface at 1.98(2) and 3.02(4) Å corresponding to the heights of a mixture of Ba 2+ ions and water molecules adsorbed in ditrigonal cavities and water molecules coordinated to the Ba 2+ ions, respectively. This pattern indicates that most Ba 2+ ions are adsorbed on the mica surface as inner-sphere complexes in a partially hydrated form. The amount of Ba 2+ ions in the ditrigonal cavities compensates more than 90% of the layer charge of the mica surface. The electron-density profiles of the fulvic acids (FAs) adsorbed on the mica surface, in the absence of Ba 2+, had overall thicknesses of 4.9-10.8 Å and consisted of one broad taller peak near the surface (likely hydrophobic and positively-charged groups) followed by a broad humped pattern (possibly containing negatively-charged functional groups). The total interfacial electron density and thickness of the FA layer increased as the solution FA concentration increased. The sorbed peat FA which has higher ash content showed a higher average electron density than the sorbed soil FA. When the muscovite reacted with a pre-mixed BaCl 2-ESFA II solution, the positions of the two peaks nearest the surface matched those in the BaCl 2 solution. However, the occupancy of the second peak decreased by about 30% implying that the hydration shell of surface-adsorbed Ba 2+ was partially substituted by FA. The two surface peaks were followed by a broad less electron-dense layer suggesting a sorption mechanism in which Ba 2+ acts dominantly as a bridging cation between the mica

  10. Chain-length dependent growth dynamics of n-alkanes on silica investigated by energy-dispersive x-ray reflectivity in situ and in real-time.

    Science.gov (United States)

    Weber, C; Frank, C; Bommel, S; Rukat, T; Leitenberger, W; Schäfer, P; Schreiber, F; Kowarik, S

    2012-05-28

    We compare the growth dynamics of the three n-alkanes C(36)H(74), C(40)H(82), and C(44)H(90) on SiO(2) using real-time and in situ energy-dispersive x-ray reflectivity. All molecules investigated align in an upright-standing orientation on the substrate and exhibit a transition from layer-by-layer growth to island growth after about 4 monolayers under the conditions employed. Simultaneous fits of the reflected intensity at five distinct points in reciprocal space show that films formed by longer n-alkanes roughen faster during growth. This behavior can be explained by a chain-length dependent height of the Ehrlich-Schwoebel barrier. Further x-ray diffraction measurements after growth indicate that films consisting of longer n-alkanes also incorporate more lying-down molecules in the top region. While the results reveal behavior typical for chain-like molecules, the findings can also be useful for the optimization of organic field effect transistors where smooth interlayers of n-alkanes without coexistence of two or more molecular orientations are required.

  11. Simultaneous in-situ real-time measurements of X-ray reflectivity and optical spectra of organic semiconductor thin film during growth

    Energy Technology Data Exchange (ETDEWEB)

    Hosokai, Takuya; Gerlach, Alexander; Hinderhofer, Alexander; Frank, Christian; Heinemeyer, Ute; Schreiber, Frank [Institut fuer Angewandte Physik, Universitaet Tuebingen (Germany)

    2010-07-01

    The relation between optical and structural properties of organic semiconductors in thin films is crucial for their fundamental understanding as well as their application in electronic devices. Here we present first results of simultaneous in-situ real-time measurements of X-ray reflectivity (XRR) and differential reflectance spectroscopy (DRS) of perfluorinated copper phthalocyanine (F{sub 16}CuPc) thin films grown on SiO{sub 2}/Si wafers. Using DRS we determine the optical absorption spectra of the thin films starting from monolayer coverage whereas real-time XRR provides structural information about the film growth. After a rapid decrease of the reflectivity in the monolayer regime we observe intensity oscillations in time at constant q{sub z} with a strong damping. By calibrating film thickness d(t), we found oscillation period of 1.45 nm at 1/2q Bragg, which correspond to the lattice spacing of standing F{sub 16}CuPc molecules. This behaviour is characteristic for layer-growth with a finite roughness. In the monolayer regime the DRS signal shows a broad absorption peak at {proportional_to}2.0 eV, while for coverages of more than one monolayer an additional and relatively sharp peak appears at {proportional_to}1.6 eV. These results indicate that the film structure in the monolayer regime is different from the layer-growth regime.

  12. X-ray reflectivity imager with 15 W power X-ray source.

    Science.gov (United States)

    Jiang, Jinxing; Sakurai, Kenji

    2016-09-01

    X-ray reflectivity is usually used for the routine analysis of layered structures of uniform thin films. So far, the technique has some limitations in the application to more practical inhomogeneous/patterned samples. X-ray reflectivity imaging is recently developed technique and can give the reconstructed image from many X-ray reflection projections. The present article gives the instrumental details of the compact X-ray reflectivity imager. Though the power of X-ray source is only 15 W, it works well. The calibration of the system has been discussed, because it is particularly important for the present grazing incidence geometry. We also give a visualization example of the buried interface, physical meaning of the reconstructed image, and discussions about possibilities for improvement.

  13. Application of kinoform lens for X-ray reflectivity analysis.

    Science.gov (United States)

    Tiwari, M K; Alianelli, L; Dolbnya, I P; Sawhney, K J S

    2010-03-01

    In this paper the first practical application of kinoform lenses for the X-ray reflectivity characterization of thin layered materials is demonstrated. The focused X-ray beam generated from a kinoform lens, a line of nominal size approximately 50 microm x 2 microm, provides a unique possibility to measure the X-ray reflectivities of thin layered materials in sample scanning mode. Moreover, the small footprint of the X-ray beam, generated on the sample surface at grazing incidence angles, enables one to measure the absolute X-ray reflectivities. This approach has been tested by analyzing a few thin multilayer structures. The advantages achieved over the conventional X-ray reflectivity technique are discussed and demonstrated by measurements.

  14. Principles of femtosecond X-ray/optical cross-correlation with X-ray induced transient optical reflectivity in solids

    Energy Technology Data Exchange (ETDEWEB)

    Eckert, S., E-mail: sebastian.eckert@helmholtz-berlin.de, E-mail: martin.beye@helmholtz-berlin.de; Beye, M., E-mail: sebastian.eckert@helmholtz-berlin.de, E-mail: martin.beye@helmholtz-berlin.de; Pietzsch, A.; Quevedo, W.; Hantschmann, M. [Institute for Methods and Instrumentation in Synchrotron Radiation Research, Helmholtz-Zentrum Berlin für Materialien und Energie GmbH, Albert-Einstein-Str. 15, 12489 Berlin (Germany); Ochmann, M.; Huse, N. [Institute for Nanostructure and Solid State Physics, University of Hamburg, Jungiusstr. 11, 20355 Hamburg, Germany and Max Planck Institute for the Structure and Dynamics of Matter, Center for Free-Electron Laser Science, Luruper Chaussee 149, 22761 Hamburg (Germany); Ross, M.; Khalil, M. [Department of Chemistry, University of Washington, Box 351700, Seattle, Washington 98195 (United States); Minitti, M. P.; Turner, J. J.; Moeller, S. P.; Schlotter, W. F.; Dakovski, G. L. [LCLS, SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, California 94025 (United States); Föhlisch, A. [Institute for Methods and Instrumentation in Synchrotron Radiation Research, Helmholtz-Zentrum Berlin für Materialien und Energie GmbH, Albert-Einstein-Str. 15, 12489 Berlin (Germany); Institut für Physik und Astronomie, Universität Potsdam, Karl-Liebknecht-Str. 24/25, 14476 Potsdam (Germany)

    2015-02-09

    The discovery of ultrafast X-ray induced optical reflectivity changes enabled the development of X-ray/optical cross correlation techniques at X-ray free electron lasers worldwide. We have now linked through experiment and theory the fundamental excitation and relaxation steps with the transient optical properties in finite solid samples. Therefore, we gain a thorough interpretation and an optimized detection scheme of X-ray induced changes to the refractive index and the X-ray/optical cross correlation response.

  15. Application of total reflection X-ray fluorescence spectrometry for ...

    Indian Academy of Sciences (India)

    in rainwater are, inductively coupled plasma-mass spectrometry (ICPMS), inductively coupled plasma-atomic emission spectrometry (ICP-AES), atomic absorption spectrom- etry (AAS), X-ray fluorescence (XRF), total reflection X-ray fluorescence (TXRF), neu- tron activation analysis (NAA), electroanalytical techniques, etc.

  16. X-ray reflection in oxygen-rich accretion discs of ultracompact X-ray binaries

    DEFF Research Database (Denmark)

    Madej, O. K.; Garcia, Jeronimo; Jonker, P. G.

    2014-01-01

    . The donor star in these sources is a carbon-oxygen or oxygen-neon-magnesium white dwarf. Hence, the accretion disc is enriched with oxygen which makes the O viii Ly alpha line particularly strong. Modelling the X-ray reflection off a carbon- and oxygen-enriched, hydrogen- and helium-poor disc with models...

  17. X-ray reflectivity measurements of liquid/solid interfaces under high hydrostatic pressure conditions.

    Science.gov (United States)

    Wirkert, Florian J; Paulus, Michael; Nase, Julia; Möller, Johannes; Kujawski, Simon; Sternemann, Christian; Tolan, Metin

    2014-01-01

    A high-pressure cell for in situ X-ray reflectivity measurements of liquid/solid interfaces at hydrostatic pressures up to 500 MPa (5 kbar), a pressure regime that is particularly important for the study of protein unfolding, is presented. The original set-up of this hydrostatic high-pressure cell is discussed and its unique properties are demonstrated by the investigation of pressure-induced adsorption of the protein lysozyme onto hydrophobic silicon wafers. The presented results emphasize the enormous potential of X-ray reflectivity studies under high hydrostatic pressure conditions for the in situ investigation of adsorption phenomena in biological systems.

  18. Structural analysis of Ni/NiO-water interface using X-ray reflectivity

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Jong Jin; Kim, Seung Hyun; Kim, Ji Hyun [Ulsan National Institute of Science and technology, Ulsan (Korea, Republic of); Bahn, Chi Bum [Argonne National Laboratory, Illinois (United States)

    2013-10-15

    These test revealed the epitaxial relationship between Ni substrate and the oxide layer as well as those structures. However, still the resolution of the initial structural data of interface between water and pre oxidized Ni(110) surface is not clear. Therefore, the objective in this study was to obtain detailed structural data between pre-oxidized Ni(110) and water interfaces to investigate the mechanism of growth the passive film formed on Ni(110) by In-situ high energy X-ray reflectivity study and simulated atomistic model. The surface treatment procedure to increase the surface crystallinity was developed to surface x-ray reflectivity measurement. The CTR data shows the surface pre-treatment procedure developed for Ni(110) was suitable for the surface X-ray study. Synchrotron X-ray experiments and analyses will be continued to identify the surface interface between Ni(110), water, and solution contained lead.

  19. Understanding X-ray reflection emissivity profiles in AGN: locating the X-ray source

    Science.gov (United States)

    Wilkins, D. R.; Fabian, A. C.

    2012-08-01

    The illumination pattern (or emissivity profile) of the accretion disc due to the reflection of X-rays in active galactic nucleus can be understood in terms of relativistic effects on the rays propagating from a source in a corona surrounding the central black hole, both on their trajectories and on the accretion disc itself. Theoretical emissivity profiles due to isotropic point sources as well as simple extended geometries are computed in general relativistic ray-tracing simulations performed on graphics processing units (GPUs). Such simulations assuming only general relativity naturally explain the accretion disc emissivity profiles determined from relativistically broadened emission lines which fall off steeply (with power-law indices of between 6 and 8) over the inner regions of the disc, then flattening off to almost a constant before tending to a constant power law of index 3 over the outer disc. Simulations for a variety of source locations, extents and geometries show how the emissivity profiles depend on these properties, and when combined with reverberation time lags allow the location and extent of the primary X-ray source to be constrained. Comparing the emissivity profile determined from the broadened iron K emission line in spectra of 1H 0707-495 obtained in 2008 January to theoretical emissivity profiles and applying constraints from reverberation lags suggest that there exists an extended region of primary X-ray emission located as low as 2rg above the accretion disc, extending outwards to a radius of around 30rg.

  20. Lensless x-ray imaging in reflection geometry

    Energy Technology Data Exchange (ETDEWEB)

    Roy, S.; Parks, D.H.; Seu, K.A.; Turner, J.J.; Chao, W.; Anderson, E.H.; Cabrini, S.; Kevan, S.D.; Su, R.

    2011-02-03

    Lensless X-ray imaging techniques such as coherent diffraction imaging and ptychography, and Fourier transform holography can provide time-resolved, diffraction-limited images. Nearly all examples of these techniques have focused on transmission geometry, restricting the samples and reciprocal spaces that can be investigated. We report a lensless X-ray technique developed for imaging in Bragg and small-angle scattering geometries, which may also find application in transmission geometries. We demonstrate this by imaging a nanofabricated pseudorandom binary structure in small-angle reflection geometry. The technique can be used with extended objects, places no restriction on sample size, and requires no additional sample masking. The realization of X-ray lensless imaging in reflection geometry opens up the possibility of single-shot imaging of surfaces in thin films, buried interfaces in magnetic multilayers, organic photovoltaic and field-effect transistor devices, or Bragg planes in a single crystal.

  1. Crystallization via tubing microfluidics permits both in situ and ex situ X-ray diffraction.

    Science.gov (United States)

    Gerard, Charline J J; Ferry, Gilles; Vuillard, Laurent M; Boutin, Jean A; Chavas, Leonard M G; Huet, Tiphaine; Ferte, Nathalie; Grossier, Romain; Candoni, Nadine; Veesler, Stéphane

    2017-10-01

    A microfluidic platform was used to address the problems of obtaining diffraction-quality crystals and crystal handling during transfer to the X-ray diffractometer. Crystallization conditions of a protein of pharmaceutical interest were optimized and X-ray data were collected both in situ and ex situ.

  2. Application of total reflection x-ray fluorescence (TXRF) technique ...

    African Journals Online (AJOL)

    Nigerian crude oils from eight oil wells have been analysed for the following trace elements: Ni, Cr, Mn, V, Fe, Zn. Pb, Cu, Co and S using total Reflection X-ray Fluorescence (TXRF) analytical method. Concentrations of these elements were found to range from 0.002 – 1.420 ppm. Results showed that Fe was the most ...

  3. Relativistic Effects on Reflection X-ray Spectra of AGN

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Khee-Gan; /University Coll. London; Fuerst, Steven V.; /KIPAC, Menlo Park; Brandwardi-Raymond, Graziella; Wu, Kinwah; Crowley, Oliver; /University Coll. London

    2007-01-05

    We have calculated the reflection component of the X-ray spectra of active galactic nuclei (AGN) and shown that they can be significantly modified by the relativistic motion of the accretion flow and various gravitational effects of the central black hole. The absorption edges in the reflection spectra suffer severe energy shifts and smearing. The degree of distortion depends on the system parameters, and the dependence is stronger for some parameters such as the inner radius of the accretion disk and the disk viewing inclination angles. The relativistic effects are significant and are observable. Improper treatment of the reflection component of the X-ray continuum in spectral fittings will give rise to spurious line-like features, which will mimic the fluorescent emission lines and mask the relativistic signatures of the lines.

  4. Progress in reflection grating spectrometers for X-ray astrophysics

    Science.gov (United States)

    McEntaffer, Randall L.

    2017-08-01

    Soft X-ray spectroscopy can address future science goals pertaining to understanding the cycle of hot baryons in the universe. Detailing feedback processes in galaxies, mapping the distribution of baryons in the circum- and intergalactic medium, and unraveling unknowns in stellar life cycles places demanding requirements upon spectrometers. Here, we detail advancements in reflection grating technologies that can be used to help provide answers to these important questions. We also discuss possible applications including a configuration for the Lynx concept strategic mission.

  5. Backscatter of hard X-rays in the solar atmosphere. [Calculating the reflectance of solar x ray emission

    Science.gov (United States)

    Bai, T.; Ramaty, R.

    1977-01-01

    The solar photosphere backscatters a substantial fraction of the hard X rays from solar flares incident upon it. This reflection was studied using a Monte Carlo simulation which takes into account Compton scattering and photo-electric absorption. Both isotropic and anisotropic X ray sources are considered. The bremsstrahlung from an anisotropic distribution of electrons are evaluated. By taking the reflection into account, the inconsistency is removed between recent observational data regarding the center-to-limb variation of solar X ray emission and the predictions of models in which accelerated electrons are moving down toward the photosphere.

  6. Two-axis Neutron and X-ray Reflectivity

    DEFF Research Database (Denmark)

    Bouwman, W.G.; Vigild, M.E.; Findeisen, E.

    1997-01-01

    Sample alignment for neutron (and in some cases x-ray) reflectometry can be complicated due to a coupling between angle and position which occurs when slits are used to define the path of the beam. Misalignments in sample position or sample rotation angle give rise to systematic errors in the exp......Sample alignment for neutron (and in some cases x-ray) reflectometry can be complicated due to a coupling between angle and position which occurs when slits are used to define the path of the beam. Misalignments in sample position or sample rotation angle give rise to systematic errors...... in the experiments. By measuring the reflectivity both from the back and from the front faces of the sample (twin reflectometry) these alignment errors can be detected and corrected for....

  7. Reflective Coating for Lightweight X-Ray Optics

    Science.gov (United States)

    Chan, Kai-Wing; Zhang, William W.; Windt, David; Hong, Mao-Ling; Saha, Timo; McClelland, Ryan; Sharpe, Marton; Dwivedi, Vivek H.

    2012-01-01

    X-ray reflective coating for next generation's lightweight, high resolution, optics for astronomy requires thin-film deposition that is precisely fine-tuned so that it will not distort the thin sub-mm substrates. Film of very low stress is required. Alternatively, mirror distortion can be cancelled by precisely balancing the deformation from multiple films. We will present results on metallic film deposition for the lightweight optics under development. These efforts include: low-stress deposition by magnetron sputtering and atomic layer deposition of the metals, balancing of gross deformation with two-layer depositions of opposite stresses and with depositions on both sides of the thin mirrors.

  8. Custom AFM for X-ray beamlines: in situ biological investigations under physiological conditions

    Energy Technology Data Exchange (ETDEWEB)

    Gumí-Audenis, B. [ESRF, The European Synchrotron, Grenoble (France); Institute for Bioengineering of Catalonia (IBEC), Barcelona (Spain); Physical Chemistry Department, Universitat de Barcelona, Barcelona (Spain); Networking Biomedical Research Center on Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN), Madrid (Spain); Carlà, F. [ESRF, The European Synchrotron, Grenoble (France); Vitorino, M. V. [University of Lisboa, Falculty of Science, Biosystems and Integrative Sciences Institute - BIOISI, Lisbon (Portugal); Panzarella, A. [ESRF, The European Synchrotron, Grenoble (France); Porcar, L. [Institut Laue-Langevin, Grenoble (France); Boilot, M. [ORTEC, Marseille (France); Guerber, S. [CEA, LETI Grenoble (France); Bernard, P. [ESRF, The European Synchrotron, Grenoble (France); Rodrigues, M. S. [University of Lisboa, Falculty of Science, Biosystems and Integrative Sciences Institute - BIOISI, Lisbon (Portugal); Sanz, F.; Giannotti, M. I. [Institute for Bioengineering of Catalonia (IBEC), Barcelona (Spain); Physical Chemistry Department, Universitat de Barcelona, Barcelona (Spain); Networking Biomedical Research Center on Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN), Madrid (Spain); Costa, L., E-mail: luca.costa@esrf.fr [ESRF, The European Synchrotron, Grenoble (France)

    2015-09-30

    The performance of a custom atomic force microscope for grazing-incidence X-ray experiments on hydrated soft and biological samples is presented. A fast atomic force microscope (AFM) has been developed that can be installed as a sample holder for grazing-incidence X-ray experiments at solid/gas or solid/liquid interfaces. It allows a wide range of possible investigations, including soft and biological samples under physiological conditions (hydrated specimens). The structural information obtained using the X-rays is combined with the data gathered with the AFM (morphology and mechanical properties), providing a unique characterization of the specimen and its dynamics in situ during an experiment. In this work, lipid monolayers and bilayers in air or liquid environment have been investigated by means of AFM, both with imaging and force spectroscopy, and X-ray reflectivity. In addition, this combination allows the radiation damage induced by the beam on the sample to be studied, as has been observed on DOPC and DPPC supported lipid bilayers under physiological conditions.

  9. In situ Synchrotron X-ray Thermodiffraction of Boranes

    Directory of Open Access Journals (Sweden)

    Pascal G. Yot

    2016-01-01

    Full Text Available Boranes of low molecular weight are crystalline materials that have been much investigated over the past decade in the field of chemical hydrogen storage. In the present work, six of them have been selected to be studied by in situ synchrotron X-ray thermodiffraction. The selected boranes are ammonia borane NH3BH3 (AB, hydrazine borane N2H4BH3 (HB, hydrazine bisborane N2H4(BH32 (HBB, lithium LiN2H3BH3 (LiHB and sodium NaN2H3BH3 (NaHB hydrazinidoboranes, and sodium triborane NaB3H8 (STB. They are first investigated separately over a wide range of temperature (80–300 K, and subsequently compared. Differences in crystal structures, the existence of phase transition, evolutions of unit cell parameters and volumes, and variation of coefficients of thermal expansion can be observed. With respect to AB, HB and HBB, the differences are mainly explained in terms of molecule size, conformation and motion (degree of freedom of the chemical groups (NH3, N2H4, BH3. With respect to LiHB, NaHB and STB, the differences are explained by a stabilization effect favored by the alkali cations via M···H interactions with four to five borane anions. The main results are presented and discussed herein.

  10. Surface layering and melting in an ionic liquid studied by resonant soft X-ray reflectivity

    OpenAIRE

    Mezger, Markus; Ocko, Benjamin M.; Reichert, Harald; Deutsch, Moshe

    2013-01-01

    The molecular-scale structure of the ionic liquid [C18mim]+[FAP]− near its free surface was studied by complementary methods. X-ray absorption spectroscopy and resonant soft X-ray reflectivity revealed a depth-decaying near-surface layering. Element-specific interfacial profiles were extracted with submolecular resolution from energy-dependent soft X-ray reflectivity data. Temperature-dependent hard X-ray reflectivity, small- and wide-angle X-ray scattering, and infrared spectroscopy uncovere...

  11. Surface layering and melting in an ionic liquid studied by resonant soft X-ray reflectivity.

    Science.gov (United States)

    Mezger, Markus; Ocko, Benjamin M; Reichert, Harald; Deutsch, Moshe

    2013-03-05

    The molecular-scale structure of the ionic liquid [C18mim](+)[FAP](-) near its free surface was studied by complementary methods. X-ray absorption spectroscopy and resonant soft X-ray reflectivity revealed a depth-decaying near-surface layering. Element-specific interfacial profiles were extracted with submolecular resolution from energy-dependent soft X-ray reflectivity data. Temperature-dependent hard X-ray reflectivity, small- and wide-angle X-ray scattering, and infrared spectroscopy uncovered an intriguing melting mechanism for the layered region, where alkyl chain melting drove a negative thermal expansion of the surface layer spacing.

  12. An update on X-ray reflection gratings developed for future missions

    Science.gov (United States)

    Miles, Drew

    2018-01-01

    X-ray reflection gratings are a key technology being studied for future X-ray spectroscopy missions, including the Lynx X-ray mission under consideration for the 2020 Decadal Survey. We present an update on the status of X-ray reflection gratings being developed at Penn State University, including current fabrication techniques and mass-replication processes and the latest diffraction efficiency results and resolving power measurements. Individual off-plane X-ray reflection gratings have exceeded the current Lynx requirements for both effective area and resolving power. Finally, we discuss internal projects that will advance the technology readiness level of these gratings.

  13. In situ ultrasound-assisted preparation of Fe3O4@MnO2 core-shell nanoparticles integrated with ion co-precipitation for multielemental analysis by total reflection X-ray fluorescence

    Science.gov (United States)

    Nourbala-Tafti, Elaheh; Romero, Vanesa; Lavilla, Isela; Dadfarnia, Shayesteh; Bendicho, Carlos

    2017-05-01

    In this work, a new analytical approach based on in situ ultrasound-assisted preparation of manganese dioxide coated magnetite nanoparticles (Fe3O4@MnO2 NPs) was applied for extraction and preconcentration of Ni, Cu, Zn, Tl, Pb, Bi and Se. The Fe3O4@MnO2 core-shell nanocomposite was synthesized by application of high-intensity sonication to an aqueous reaction medium in the presence of the target analytes, which are trapped during NPs formation. In this way, synthesis of the nanosorbent and extraction can be simultaneously accomplished within only 30 s. After the extraction step, the resulting Fe3O4@MnO2 NPs enriched with the target analytes were separated by an external magnetic field, so that filtration or centrifugation steps were unnecessary. A 10 μL aliquot of the solid phase was deposited onto a sample carrier (quartz reflector) and directly analyzed by total-reflection X-ray fluorescence (TXRF) without the need for an elution step. A comprehensive characterization of the Fe3O4@MnO2 NPs was carried out by transmission electron microscopy and TXRF. Detection limits ranged from 0.19 to 0.98 μg L- 1 depending on the analyte. Enrichment factors in the range of 402-540 were obtained. The repeatability expressed as relative standard deviation was around 1.7% (N = 5). The accuracy of the proposed method was assessed by analyzing the certified reference material BCR®-610 (groundwater). An effective, simple, rapid and sensitive procedure for multielemental analysis of water samples was accomplished.

  14. Interface-sensitive imaging by an image reconstruction aided X-ray reflectivity technique1

    OpenAIRE

    Jiang, Jinxing; Hirano, Keiichi; Sakurai, Kenji

    2017-01-01

    Recently, the authors have succeeded in realizing X-ray reflectivity imaging of heterogeneous ultrathin films at specific wavevector transfers by applying a wide parallel beam and an area detector. By combining in-plane angle and grazing-incidence angle scans, it is possible to reconstruct a series of interface-sensitive X-ray reflectivity images at different grazing-incidence angles (proportional to wavevector transfers). The physical meaning of a reconstructed X-ray reflectivity image at a ...

  15. Characterization of Gas-Solid Reactions using In Situ Powder X-ray Diffraction

    DEFF Research Database (Denmark)

    Møller, Kasper Trans; Hansen, Bjarne Rosenlund Søndertoft; Dippel, Ann-Christin

    2014-01-01

    X-ray diffraction is a superior technique for structural characterization of crystalline matter. Here we review the use of in situ powder X-ray diffraction (PXD) mainly for real-time studies of solid/gas reactions, data analysis and the extraction of valuable knowledge of structural, chemical...

  16. In-situ Scanning Transmission X-Ray Microscopy of Catalytic Solids and Related Nanomaterials

    NARCIS (Netherlands)

    de Groot, F.M.F.; de Smit, E.; van Schooneveld, M.M.; Aramburo, L.R.; Weckhuysen, B.M.

    2013-01-01

    The present status of in-situ scanning transmission X-ray microscopy (STXM) is reviewed, with an emphasis on the abilities of the STXM technique in comparison with electron microscopy. The experimental aspects and interpretation of X-ray absorption spectroscopy (XAS) are briefly introduced and the

  17. Combined EUV reflectance and X-ray reflectivity data analysis of periodic multilayer structures

    NARCIS (Netherlands)

    Yakunin, S. N.; Makhotkin, I. A.; K. V. Nikolaev,; van de Kruijs, R. W. E.; Chuev, M. A.; F. Bijkerk,

    2014-01-01

    We present a way to analyze the chemical composition of periodical multilayer structures using the simultaneous analysis of grazing incidence hard X-Ray reflectivity (GIXR) and normal incidence extreme ultraviolet reflectance (EUVR). This allows to combine the high sensitivity of GIXR data to layer

  18. X-ray reflectivity investgation of structure and kinetics of photoswitchable lipid monolayers

    DEFF Research Database (Denmark)

    Chatterjee, Kuntal; Haushahn, Björn; Shen, Chen

    The mechanical and dynamic properties of phospholipid membranes are of importance for important biological functions, such as switching of embedded proteins. In order to investigate these properties we study model systems in which amphiphilic photoswitchable molecules are integrated into Langmuir...... transand cis-conformation by illumination with UV and blue light. We have followed the structural changes in this model membrane and the switching kinetics of the system with Langmuir isotherms and in situ X-ray reflectivity at the LISA diffractometer P08, PETRA III....

  19. X-ray reflectivity investgation of structure and kinetics of photoswitchable lipid monolayers

    DEFF Research Database (Denmark)

    Chatterjee, Kuntal; Haushahn, Björn; Shen, Chen

    The mechanical and dynamic properties of phospholipid membranes are of importance for important biological functions, such as switching of embedded proteins. In order to investigate these properties we study model systems in which amphiphilic photoswitchable molecules are integrated into Langmuir......- and cis-conformation by illumination with UV and blue light. We have followed the structural changes in this model membrane and the switching kinetics of the system with Langmuir isotherms and in situ X-ray reflectivity at the LISA diffractometer P08, PETRA III....

  20. A new setup for high resolution fast X-ray reflectivity data acquisition.

    Science.gov (United States)

    Lippmann, Milena; Buffet, Adeline; Pflaum, Kathrin; Ehnes, Anita; Ciobanu, Anca; Seeck, Oliver H

    2016-11-01

    A new method for fast x-ray reflectivity data acquisition is presented. The method is based on a fast rotating, slightly tilted sample reflecting to a stationary mounted position sensitive detector and it allows for measurements of reflectivity curves in a quarter of a second. The resolution in q-space mainly depends on the beam properties and the pixel size of the detector. Maximum qz-value of 1 Å-1 can be achieved. The time-temperature depending structure changes of poly(N-isopropylacrylamide) thin films were investigated in situ by applying the fast-reflectivity setup. The results are presented in this paper as illustration of the method and proof of principle.

  1. Reflection surface x-ray diffraction patterns: k-space images

    Energy Technology Data Exchange (ETDEWEB)

    Hong, Hawoong [Fredrick Seitz Materials Research Laboratory, University of Illinois at Urbana-Champaign, 438D, 9700 South Cass Avenue, Argonne, Illinois 60439 (United States); Wu, Z. [Fredrick Seitz Materials Research Laboratory, University of Illinois at Urbana-Champaign, 104 South Goodwin Avenue, Urbana, Illinois 61801-2902 (United States); Department of Materials Science and Engineering, University of Illinois at Urbana-Champaign, 1304 West Green Street, Urbana, Illinois 61801-2980 (United States); Chiang, T.-C. [Fredrick Seitz Materials Research Laboratory, University of Illinois at Urbana-Champaign, 104 South Goodwin Avenue, Urbana, Illinois 61801-2902 (United States); Department of Physics, University of Illinois at Urbana-Champaign, 1110 West Green Street, Urbana, Illinois 61801-3080 (United States); Zschack, P. [Fredrick Seitz Materials Research Laboratory, University of Illinois at Urbana-Champaign, 438D, 9700 South Cass Avenue, Argonne, Illinois 60439 (United States); Jemian, P. [Fredrick Seitz Materials Research Laboratory, University of Illinois at Urbana-Champaign, 438D, 9700 South Cass Avenue, Argonne, Illinois 60439 (United States); Chen, Haydn [Fredrick Seitz Materials Research Laboratory, University of Illinois at Urbana-Champaign, 104 South Goodwin Avenue, Urbana, Illinois 61801-2902 (United States); Aburano, R. D. [Cypress Semiconductor, 3901 North First Street, San Jose, California 95134 (United States)

    2000-08-01

    For the past two decades, x-ray diffraction has been utilized for surface structural determination. Unlike reflection high-energy electron diffraction (RHEED) which is a complicated dynamical scattering process, x-ray surface analysis is simple and straightforward due to the kinematic nature of x rays. Using high brilliance x rays from an undulator beamline and a highly sensitive charge coupled device detector, we successfully observed RHEED-like x-ray diffraction patterns. The patterns were recorded during the preparation of Si(111)-(7x7), transformation to Ge/Si(111)-(5x5) and Ge growth. Also, simultaneous measurements of x-ray reflectivity and crystal truncation rods are shown feasible with this technique. (c) 2000 American Institute of Physics.

  2. X-ray grating interferometer for in situ and at-wavelength wavefront metrology.

    Science.gov (United States)

    Kayser, Yves; David, Christian; Flechsig, Uwe; Krempasky, Juraj; Schlott, Volker; Abela, Rafael

    2017-01-01

    A wavefront metrology setup based on the X-ray grating interferometry technique for spatially resolved, quantitative, in situ and at-wavelength measurements of the wavefront at synchrotron radiation and hard X-ray free-electron laser beamlines is reported. Indeed, the ever-increasing demands on the optical components to preserve the wavefront shape and the coherence of the delivered X-ray beam call for more and more sensitive diagnostic instruments. Thanks to its angular sensitivity, X-ray grating interferometry has been established in recent years as an adequate wavefront-sensing technique for quantitatively assessing the quality of the X-ray wavefront under working conditions and hence for the in situ investigation of X-ray optical elements. In order to characterize the optical elements at any given beamline by measuring the aberrations introduced in the wavefront, a transportable X-ray grating interferometry setup was realised at the Swiss Light Source (SLS). The instrument, which is expected to be a valuable tool for investigating the quality of the X-ray beam delivered at an endstation, will be described hereafter in terms of the hardware setup and the related data analysis procedure. Several exemplary experiments performed at the X05DA Optics beamline of the SLS will be presented.

  3. X-ray Reflected Spectra from Accretion Disk Models: A Complete Grid of Ionized Reflection Calculations

    Science.gov (United States)

    Garcia, Javier; Dauser, T.; Reynolds, C. S.; Kallman, T. R.; McClintock, J. E.; Narayan, R.; Wilms, J.; Eikmann, W.

    2013-04-01

    We present a new and complete library of synthetic spectra to model the reprocessed and reflected X-ray radiation from illuminated accretion disks, using an updated version of our code XILLVER. Several improvements have been implemented to both the routines and the atomic data, allowing the production a large grid of reflection models covering a wide range of parameters. Each model is characterized by the photon index Γ of the illuminating radiation (assumed to be a power-law), the ionization parameter ξ at the surface of the disk (i.e., the ratio of the X-ray flux over the gas density), and the iron abundance AFe with respect to the solar value. The ranges of the parameters covered are: 1.2 ≤ Γ ≤ 3.4, 1 ≤ ξ ≤ 104, and 0.5 ≤ AFe ≤ 10. This choice is motivated to represent the physical conditions typically observed in most active galactic nuclei, as well as in some galactic black holes. This library is particularly intended to model reflection from accreting sources where the thermal disk emission is small compared to the incident power-law spectrum. A total of 720 reflection spectra are provided in a single FITS file suitable for the analysis of X-ray observations via the atable model in XSPEC. A detailed comparison with previous models highlights the improvements achieved in the present calculations, and their implications on the analysis of X-ray spectra is discussed.

  4. Direct analysis of biological samples by total reflection X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Lue M, Marco P. [Unidad de Analisis Instrumental, Departamento de Quimica y Suelos, Decanato de Agronomia, Universidad Centro-occidental Lisandro Alvarado, Apartado Postal 4076, Cabudare 3023 (Venezuela)]. E-mail: luemerumarco@yahoo.es; Hernandez-Caraballo, Edwin A. [Instituto Venezolano-Andino para la Investigacion Quimica (IVAIQUIM), Facultad de Ciencias, Universidad de los Andes, Merida 5101 (Venezuela)

    2004-08-31

    The technique of total reflection X-ray fluorescence (TXRF) is well suited for the direct analysis of biological samples due to the low matrix interferences and simultaneous multi-element nature. Nevertheless, biological organic samples are frequently analysed after digestion procedures. The direct determination of analytes requires shorter analysis time, low reactive consumption and simplifies the whole analysis process. On the other hand, the biological/clinical samples are often available in minimal amounts and routine studies require the analysis of large number of samples. To overcome the difficulties associated with the analysis of organic samples, particularly of solid ones, different procedures of sample preparation and calibration to approach the direct analysis have been evaluated: (1) slurry sampling, (2) Compton peak standardization, (3) in situ microwave digestion, (4) in situ chemical modification and (5) direct analysis with internal standardization. Examples of analytical methods developed by our research group are discussed. Some of them have not been previously published, illustrating alternative strategies for coping with various problems that may be encountered in the direct analysis by total reflection X-ray fluorescence spectrometry.

  5. Application of total reflection X-ray fluorescence spectrometry for ...

    Indian Academy of Sciences (India)

    Applicability of total reflection X-ray fluorescence (TXRF) spectrometry for trace elemental analysis of rainwater samples was studied. The study was used to develop these samples as rainwater standards by the National University of Singapore (NUS). Our laboratory was one of the participants to use TXRF for this study.

  6. IN SITU SURFACE X-RAY SCATTERING STUDIES OF ELECTROSORPTION

    Energy Technology Data Exchange (ETDEWEB)

    WANG,J.X.; ADZIC,R.R.; OCKO,B.M.

    1998-07-01

    A short review of the application of surface x-ray scattering techniques to the electrode/electrolyte interfaces is presented. Recent results on metal, halide, and metal-halide adlayers with three specific systems: Bi on Au(100) and Au(110); Br on Au(100) and Ag(100); and the coadsorption of Tl with Br or I on Au(111), are given as an illustration. Factors affecting ordering of pure metal and halide adlayers and the metal-halide surface compounds are discussed in some detail.

  7. X-ray total reflection mirrors for coherent illumination

    CERN Document Server

    Ishikawa, T; Yabashi, M; Souvorov, A; Yamauchi, K; Yamamura, K; Mimura, H; Saito, A; Mori, Y

    2002-01-01

    X-ray mirrors for coherent illumination demand much higher surface quality than is achievable with the conventional polishing techniques. Plasma chemical vaporization machining (CVM) and elastic emission machining (EEM) have been applied for x-ray mirror manufacturing. Figure error of a flat silicon single crystal mirrors made with CVM+EEM process was reduced to 2.0 nm peak-to-valley and 0.2 nm RMS. The machining process was also applied to make elliptical mirrors. One-dimensional focusing with a single elliptical mirror showed diffraction-limited properties with the focal width of 200 nm. Two-dimensional focusing with Kirkpatric-Baez configuration gave a focal spot size of 200 nm x 200 nm. (author)

  8. High energy x-ray reflectivity and scattering study from spectrum-x-gamma flight mirrors

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; Budtz-Jørgensen, Carl; Frederiksen, P. Kk

    1993-01-01

    Line radiation from Fe K-alpha(1), Cu K-alpha(1), and Ag K-alpha(1) is used to study the high energy X-ray reflectivity and scattering behavior of flight-quality X-ray mirrors having various Al substrates. When both the specular and the scattered radiation are integrated, near theoretical...

  9. Reflectivity studies on a synchrotron radiation mirror in the hard X-ray regime

    CERN Document Server

    Keil, P; Novikov, D V; Hahn, U; Frahm, R

    2001-01-01

    The optical performance and roughness parameters of an X-ray mirror that was used for several years in a synchrotron radiation beamline are determined by studying its X-ray reflectivity and diffuse scattering behavior. These values are compared to the data derived from topographic measurements with an atomic force microscope (AFM).

  10. Interaction between lipid monolayers and poloxamer 188: An X-ray reflectivity and diffraction study

    DEFF Research Database (Denmark)

    Wu, G.H.; Majewski, J.; Ege, C.

    2005-01-01

    The mechanism by which poloxamer 188 (P188) seals a damaged cell membrane is examined using the lipid monolayer as a model system. X-ray reflectivity and grazing-incidence x-ray diffraction results show that at low nominal lipid density, P188, by physically occupying the available area and phase...

  11. Modelling of a total reflection X-ray fluorescence (TXRF) system ...

    African Journals Online (AJOL)

    A robust computer program to simulate X-ray fluorescence (XRF) system and particularly applied to the total reflection mode is presented in this paper. The simulation of the different stages involved in x-ray fluorescence emissions was carried out by writing a suite of computer programs using FORTRAN programming ...

  12. Temporal cross-correlation of x-ray free electron and optical lasers using soft x-ray pulse induced transient reflectivity.

    Science.gov (United States)

    Krupin, O; Trigo, M; Schlotter, W F; Beye, M; Sorgenfrei, F; Turner, J J; Reis, D A; Gerken, N; Lee, S; Lee, W S; Hays, G; Acremann, Y; Abbey, B; Coffee, R; Messerschmidt, M; Hau-Riege, S P; Lapertot, G; Lüning, J; Heimann, P; Soufli, R; Fernández-Perea, M; Rowen, M; Holmes, M; Molodtsov, S L; Föhlisch, A; Wurth, W

    2012-05-07

    The recent development of x-ray free electron lasers providing coherent, femtosecond-long pulses of high brilliance and variable energy opens new areas of scientific research in a variety of disciplines such as physics, chemistry, and biology. Pump-probe experimental techniques which observe the temporal evolution of systems after optical or x-ray pulse excitation are one of the main experimental schemes currently in use for ultrafast studies. The key challenge in these experiments is to reliably achieve temporal and spatial overlap of the x-ray and optical pulses. Here we present measurements of the x-ray pulse induced transient change of optical reflectivity from a variety of materials covering the soft x-ray photon energy range from 500eV to 2000eV and outline the use of this technique to establish and characterize temporal synchronization of the optical-laser and FEL x-ray pulses.

  13. Interface-sensitive imaging by an image reconstruction aided X-ray reflectivity technique1

    Science.gov (United States)

    Hirano, Keiichi

    2017-01-01

    Recently, the authors have succeeded in realizing X-ray reflectivity imaging of heterogeneous ultrathin films at specific wavevector transfers by applying a wide parallel beam and an area detector. By combining in-plane angle and grazing-incidence angle scans, it is possible to reconstruct a series of interface-sensitive X-ray reflectivity images at different grazing-incidence angles (proportional to wavevector transfers). The physical meaning of a reconstructed X-ray reflectivity image at a specific wavevector transfer is the two-dimensional reflectivity distribution of the sample. In this manner, it is possible to retrieve the micro-X-ray reflectivity (where the pixel size is on the microscale) profiles at different local positions on the sample. PMID:28656036

  14. Interface-sensitive imaging by an image reconstruction aided X-ray reflectivity technique.

    Science.gov (United States)

    Jiang, Jinxing; Hirano, Keiichi; Sakurai, Kenji

    2017-06-01

    Recently, the authors have succeeded in realizing X-ray reflectivity imaging of heterogeneous ultrathin films at specific wavevector transfers by applying a wide parallel beam and an area detector. By combining in-plane angle and grazing-incidence angle scans, it is possible to reconstruct a series of interface-sensitive X-ray reflectivity images at different grazing-incidence angles (proportional to wavevector transfers). The physical meaning of a reconstructed X-ray reflectivity image at a specific wavevector transfer is the two-dimensional reflectivity distribution of the sample. In this manner, it is possible to retrieve the micro-X-ray reflectivity (where the pixel size is on the microscale) profiles at different local positions on the sample.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-04-15

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

  16. Molecular orientation in soft matter thin films studied by resonant soft X-ray reflectivity

    Energy Technology Data Exchange (ETDEWEB)

    Mezger, Markus; Jerome, Blandine; Kortright, Jeffrey B.; Valvidares, Manuel; Gullikson, Eric; Giglia, Angelo; Mahne, Nicola; Nannarone, Stefano

    2011-01-12

    We present a technique to study depth profiles of molecular orientation in soft matter thin films with nanometer resolution. The method is based on dichroism in resonant soft X-ray reflectivity using linear s- and p-polarization. It combines the chemical sensitivity of Near-Edge X-ray Absorption Fine Structure spectroscopy to specific molecular bonds and their orientation relative to the polarization of the incident beam with the precise depth profiling capability of X-ray reflectivity. We demonstrate these capabilities on side chain liquid crystalline polymer thin films with soft X-ray reflectivity data at the carbon K edge. Optical constants of the anisotropic refractive index ellipsoid were obtained from a quantitative analysis using the Berreman formalism. For films up to 50 nm thickness we find that the degree of orientation of the long axis exhibits no depth variation and isindependent of the film thickness.

  17. Monte Carlo simulation applied in total reflection x-ray fluorescence: Preliminary results

    Energy Technology Data Exchange (ETDEWEB)

    Meira, Luiza L. C.; Inocente, Guilherme F.; Vieira, Leticia D.; Mesa, Joel [Departamento de Fisica e Biofisica - Instituto de Biociencias de Botucatu, Universidade Estadual Paulista Julio de Mesquita Filho (Brazil)

    2013-05-06

    The X-ray Fluorescence (XRF) analysis is a technique for the qualitative and quantitative determination of chemical constituents in a sample. This method is based on detection of the characteristic radiation intensities emitted by the elements of the sample, when properly excited. A variant of this technique is the Total Reflection X-ray Fluorescence (TXRF) that utilizes electromagnetic radiation as excitation source. In total reflection of X-ray, the angle of refraction of the incident beam tends to zero and the refracted beam is tangent to the sample support interface. Thus, there is a minimum angle of incidence at which no refracted beam exists and all incident radiation undergoes total reflection. In this study, we evaluated the influence of the energy variation of the beam of incident x-rays, using the MCNPX code (Monte Carlo NParticle) based on Monte Carlo method.

  18. Simultaneous parameter optimization of x-ray and neutron reflectivity data using genetic algorithms

    Science.gov (United States)

    Singh, Surendra; Basu, Saibal

    2016-05-01

    X-ray and neutron reflectivity are two non destructive techniques which provide a wealth of information on thickness, structure and interracial properties in nanometer length scale. Combination of X-ray and neutron reflectivity is well suited for obtaining physical parameters of nanostructured thin films and superlattices. Neutrons provide a different contrast between the elements than X-rays and are also sensitive to the magnetization depth profile in thin films and superlattices. The real space information is extracted by fitting a model for the structure of the thin film sample in reflectometry experiments. We have applied a Genetic Algorithms technique to extract depth dependent structure and magnetic in thin film and multilayer systems by simultaneously fitting X-ray and neutron reflectivity data.

  19. Simultaneous parameter optimization of x-ray and neutron reflectivity data using genetic algorithms

    Energy Technology Data Exchange (ETDEWEB)

    Singh, Surendra, E-mail: surendra@barc.gov.in; Basu, Saibal [Solid State Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 India (India)

    2016-05-23

    X-ray and neutron reflectivity are two non destructive techniques which provide a wealth of information on thickness, structure and interracial properties in nanometer length scale. Combination of X-ray and neutron reflectivity is well suited for obtaining physical parameters of nanostructured thin films and superlattices. Neutrons provide a different contrast between the elements than X-rays and are also sensitive to the magnetization depth profile in thin films and superlattices. The real space information is extracted by fitting a model for the structure of the thin film sample in reflectometry experiments. We have applied a Genetic Algorithms technique to extract depth dependent structure and magnetic in thin film and multilayer systems by simultaneously fitting X-ray and neutron reflectivity data.

  20. A modular reactor design for in situ synchrotron x-ray investigation of atomic layer deposition processes

    Science.gov (United States)

    Klug, Jeffrey A.; Weimer, Matthew S.; Emery, Jonathan D.; Yanguas-Gil, Angel; Seifert, Sönke; Schlepütz, Christian M.; Martinson, Alex B. F.; Elam, Jeffrey W.; Hock, Adam S.; Proslier, Thomas

    2015-11-01

    Synchrotron characterization techniques provide some of the most powerful tools for the study of film structure and chemistry. The brilliance and tunability of the Advanced Photon Source allow access to scattering and spectroscopic techniques unavailable with in-house laboratory setups and provide the opportunity to probe various atomic layer deposition (ALD) processes in situ starting at the very first deposition cycle. Here, we present the design and implementation of a portable ALD instrument which possesses a modular reactor scheme that enables simple experimental switchover between various beamlines and characterization techniques. As first examples, we present in situ results for (1) X-ray surface scattering and reflectivity measurements of epitaxial ZnO ALD on sapphire, (2) grazing-incidence small angle scattering of MnO nucleation on silicon, and (3) grazing-incidence X-ray absorption spectroscopy of nucleation-regime Er2O3 ALD on amorphous ALD alumina and single crystalline sapphire.

  1. Two-dimensional in situ metrology of X-ray mirrors using the speckle scanning technique

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Hongchang, E-mail: hongchang.wang@diamond.ac.uk; Kashyap, Yogesh; Laundy, David; Sawhney, Kawal [Diamond Light Source Ltd, Harwell Science and Innovation Campus, Didcot OX11 0DE (United Kingdom)

    2015-06-06

    The two-dimensional slope error of an X-ray mirror has been retrieved by employing the speckle scanning technique, which will be valuable at synchrotron radiation facilities and in astronomical telescopes. In situ metrology overcomes many of the limitations of existing metrology techniques and is capable of exceeding the performance of present-day optics. A novel technique for precisely characterizing an X-ray bimorph mirror and deducing its two-dimensional (2D) slope error map is presented. This technique has also been used to perform fast optimization of a bimorph mirror using the derived 2D piezo response functions. The measured focused beam size was significantly reduced after the optimization, and the slope error map was then verified by using geometrical optics to simulate the focused beam profile. This proposed technique is expected to be valuable for in situ metrology of X-ray mirrors at synchrotron radiation facilities and in astronomical telescopes.

  2. Ptychographic characterization of the wavefield in the focus of reflective hard X-ray optics.

    Science.gov (United States)

    Kewish, Cameron M; Thibault, Pierre; Dierolf, Martin; Bunk, Oliver; Menzel, Andreas; Vila-Comamala, Joan; Jefimovs, Konstantins; Pfeiffer, Franz

    2010-03-01

    A technique for quantitatively characterizing the complex-valued focal wavefield of arbitrary optics is described and applied to reconstructing the coherent focused beam produced by a reflective/diffractive hard X-ray mirror. This phase-retrieval method, based on ptychography, represents an important advance in X-ray optics characterization because the information obtained and potential resolution far exceeds that accessible to methods of directly probing the focus. Ptychography will therefore be well-suited for characterizing and aligning future nanofocusing X-ray optics. (c) 2010 Elsevier B.V. All rights reserved.

  3. Protegrin interaction with lipid monolayers: Grazing incidence X-ray diffraction and X-ray reflectivity study

    Science.gov (United States)

    Neville, Frances; Ishitsuka, Yuji; Hodges, Chris S.; Konovalov, Oleg; Waring, Alan J.; Lehrer, Robert; Lee, Ka Yee C.; Gidalevitz, David

    2009-01-01

    Interactions of the antimicrobial peptide protegrin-1 (PG-1) with phospholipid monolayers have been investigated by using grazing incidence X-ray diffraction (GIXD) and specular X-ray reflectivity (XR). The structure of a PG-1 film at the air-aqueous interface was also investigated by XR for the first time. Lipid A, dipalmitoyl-phosphatidylglycerol (DPPG) and dipalmitoyl-phosphatidylcholine (DPPC) monolayers were formed at the air-aqueous interface to mimic the surface of the bacterial cell wall and the outer leaflet of the erythrocyte cell membrane, respectively. Experiments were carried out under constant area conditions where the pressure changes upon insertion of peptide into the monolayer. GIXD data suggest that the greatest monolayer disruption produced by PG-1 is seen with the DPPG system at 20 mN/m since the Bragg peaks completely disappear after introduction of PG-1 to the system. PG-1 shows greater insertion into the lipid A system compared to the DPPC system when both films are held at the same initial surface pressure of 20 mN/m. The degree of insertion lessens at 30 mN/m with both DPPC and DPPG monolayer systems. XR data further reveal that PG-1 inserts primarily in the head group region of lipid monolayers. However, only the XR data of the anionic lipids suggest the existence of an additional adsorbed peptide layer below the head group of the monolayer. Overall the data show that the extent of peptide/lipid interaction and lipid monolayer disruption depends not only on the lipid composition of the monolayer, but the packing density of the lipids in the monolayer prior to the introduction of peptide to the subphase. PMID:19672319

  4. Fast X-ray reflectivity measurements using an X-ray pixel area detector at the DiffAbs beamline, Synchrotron SOLEIL.

    Science.gov (United States)

    Mocuta, Cristian; Stanescu, Stefan; Gallard, Manon; Barbier, Antoine; Dawiec, Arkadiusz; Kedjar, Bouzid; Leclercq, Nicolas; Thiaudiere, Dominique

    2018-01-01

    This paper describes a method for rapid measurements of the specular X-ray reflectivity signal using an area detector and a monochromatic, well collimated X-ray beam (divergence below 0.01°), combined with a continuous data acquisition mode during the angular movements of the sample and detector. In addition to the total integrated (and background-corrected) reflectivity signal, this approach yields a three-dimensional mapping of the reciprocal space in the vicinity of its origin. Grazing-incidence small-angle scattering signals are recorded simultaneously. Measurements up to high momentum transfer values (close to 0.1 nm-1, also depending on the X-ray beam energy) can be performed in total time ranges as short as 10 s. The measurement time can be reduced by up to 100 times as compared with the classical method using monochromatic X-ray beams, a point detector and rocking scans (integrated reflectivity signal).

  5. Simultaneous analysis of Grazing Incidence X-Ray reflectivity and X-ray standing waves from periodic multilayer systems

    NARCIS (Netherlands)

    Yakunin, S.N.; Makhotkin, Igor Alexandrovich; Chuyev, M.A.; Seregin, A.Y.; Pashayev, E.M.; Louis, Eric; van de Kruijs, Robbert Wilhelmus Elisabeth; Bijkerk, Frederik; Kovalchuk, M.V.

    2012-01-01

    Structural analysis of periodic multilayers with small period thickness (~4 nm) is a challenging task, especially when thicknesses of intermixed interfaces become comparable to individual layer thicknesses. In general, angular dependent X-ray fluorescence measurements, excited by the X-ray standing

  6. Determination of x-ray elastic constants using an in situ pressing device

    NARCIS (Netherlands)

    Teeuw, D.H.J.; Hosson, J.Th.M. De

    1998-01-01

    The experimental determination of x-ray elastic constants are performed by in situ measurements of the dependence of the strain state in selected crystallites for different applied external compressive stresses. The use of compressive applied stresses instead of tensile applied stresses is of

  7. In-situ soft X-ray absorption of over-exchanged Fe/ZSM5

    NARCIS (Netherlands)

    Heijboer, WM; Battiston, AA; Knop-Gericke, A; Havecker, M; Mayer, R; Bluhm, H; Schlogl, R; Weckhuysen, BM|info:eu-repo/dai/nl/285484397; Koningsberger, DC; de Groot, FMF|info:eu-repo/dai/nl/08747610X

    2003-01-01

    In-situ soft X-ray absorption spectroscopy (XAS) has been applied to study the iron redox behavior in over-exchanged Fe/ZSM5. The Fe L-2,L-3 XAS and O K spectral shapes of the Fe/ZSM5 surface have been measured during heat treatments and reduction/oxidation cycles. Charge-transfer multiplet

  8. PLD fabrication of a soft X-ray multilayer mirror and LPP reflectance test

    Science.gov (United States)

    Weaver, I.; Lewis, C. L. S.; MacPhee, A. G.; Warwick, P. J.; Jordan, R.; Lunney, J. G.

    1998-05-01

    A soft X-ray mirror based on a molybdenum-silicon (Mo/Si) multilayer structure has been fabricated by the pulsed laser deposition (PLD) technique. The multilayer was designed to reflect at 196 Å for normal incidence operation. An iterative graphical procedure was used to calculate the optimum periodic multilayer structure. The normal incidence reflectance of the multilayer was determined using a continuum source of soft X-rays from a laser-produced plasma (LPP). The multilayer peak reflectance was 7.3% at 190 Å, with the magnitude of reflectance consistent with an effective interfacial roughness within the structure equal to ˜15 Å.

  9. Functional materials analysis using in situ and in operando X-ray and neutron scattering.

    Science.gov (United States)

    Peterson, Vanessa K; Papadakis, Christine M

    2015-03-01

    In situ and in operando studies are commonplace and necessary in functional materials research. This review highlights recent developments in the analysis of functional materials using state-of-the-art in situ and in operando X-ray and neutron scattering and analysis. Examples are given covering a number of important materials areas, alongside a description of the types of information that can be obtained and the experimental setups used to acquire them.

  10. Functional materials analysis using in situ and in operando X-ray and neutron scattering

    Directory of Open Access Journals (Sweden)

    Vanessa K. Peterson

    2015-03-01

    Full Text Available In situ and in operando studies are commonplace and necessary in functional materials research. This review highlights recent developments in the analysis of functional materials using state-of-the-art in situ and in operando X-ray and neutron scattering and analysis. Examples are given covering a number of important materials areas, alongside a description of the types of information that can be obtained and the experimental setups used to acquire them.

  11. Functional materials analysis using in situ and in operando X-ray and neutron scattering

    Science.gov (United States)

    Peterson, Vanessa K.; Papadakis, Christine M.

    2015-01-01

    In situ and in operando studies are commonplace and necessary in functional materials research. This review highlights recent developments in the analysis of functional materials using state-of-the-art in situ and in operando X-ray and neutron scattering and analysis. Examples are given covering a number of important materials areas, alongside a description of the types of information that can be obtained and the experimental setups used to acquire them. PMID:25866665

  12. Controllable reflection of X-rays on crystals of saccharose

    CERN Document Server

    Navasardyan, M A; Hayrapetyan, K T; Gabrielyan, R T

    2003-01-01

    Multiple (ten times and more) increase in intensities of separate reflections and of lauegram reflections from organic single crystals of saccharose (C sub 1 2H sub 2 2O sub 1 1) was observed under influence of certain temperature gradient. On the base of the present experiment and the data of our previous woks we show that the controllable reflection process has a common nature and the intensity of the diffracted beam under external influences does not depend on the total number of electrons per unit volume of the unit cell of the single crystal.

  13. In Situ X-Ray Probing Reveals Fingerprints of Surface Platinum Oxide

    Energy Technology Data Exchange (ETDEWEB)

    Friebel, Daniel

    2011-08-24

    In situ x-ray absorption spectroscopy (XAS) at the Pt L{sub 3} edge is a useful probe for Pt-O interactions at polymer electrolyte membrane fuel cell (PEMFC) cathodes. We show that XAS using the high energy resolution fluorescence detection (HERFD) mode, applied to a well-defined monolayer Pt/Rh(111) sample where the bulk penetrating hard x-rays probe only surface Pt atoms, provides a unique sensitivity to structure and chemical bonding at the Pt-electrolyte interface. Ab initio multiple-scattering calculations using the FEFF8 code and complementary extended x-ray absorption fine structure (EXAFS) results indicate that the commonly observed large increase of the white-line at high electrochemical potentials on PEMFC cathodes originates from platinum oxide formation, whereas previously proposed chemisorbed oxygen-containing species merely give rise to subtle spectral changes.

  14. Hydrothermal formation of tobermorite studied by in situ X-ray diffraction under autoclave condition.

    Science.gov (United States)

    Kikuma, Jun; Tsunashima, Masamichi; Ishikawa, Tetsuji; Matsuno, Shin-ya; Ogawa, Akihiro; Matsui, Kunio; Sato, Masugu

    2009-09-01

    Hydrothermal formation of tobermorite from a pre-cured cake has been investigated by transmission X-ray diffraction (XRD) using high-energy X-rays from a synchrotron radiation source in combination with a newly designed autoclave cell. The autoclave cell has a large and thin beryllium window for wide-angle X-ray diffraction; nevertheless, it withstands a steam pressure of more than 1.2 MPa, which enables in situ XRD measurements in a temperature range of 373 to 463 K under a saturated steam pressure. Formation and/or decomposition of several components has been successfully observed during 7.5 h of reaction time. From the intensity changes of the intermediate materials, namely non-crystalline C-S-H and hydroxylellestadite, two pathways for tobermorite formation have been confirmed. Thus, the newly developed autoclave cell can be used for the analyses of reaction mechanisms under specific atmospheres and temperatures.

  15. In situ laser heating and radial synchrotron X-ray diffraction ina diamond anvil cell

    Energy Technology Data Exchange (ETDEWEB)

    Kunz, Martin; Caldwell, Wendel A.; Miyagi, Lowell; Wenk,Hans-Rudolf

    2007-06-29

    We report a first combination of diamond anvil cell radialx-ray diffraction with in situ laser heating. The laser-heating setup ofALS beamline 12.2.2 was modified to allow one-sided heating of a samplein a diamond anvil cell with an 80 W yttrium lithium fluoride laser whileprobing the sample with radial x-ray diffraction. The diamond anvil cellis placed with its compressional axis vertical, and perpendicular to thebeam. The laser beam is focused onto the sample from the top while thesample is probed with hard x-rays through an x-ray transparentboron-epoxy gasket. The temperature response of preferred orientation of(Fe,Mg)O is probed as a test experiment. Recrystallization was observedabove 1500 K, accompanied by a decrease in stress.

  16. Influence of a carbon over-coat on the X-ray reflectance of XEUS mirrors

    DEFF Research Database (Denmark)

    Lumb, D.H.; Christensen, Finn Erland; Cooper-Jensen, Carsten P.

    2007-01-01

    We describe measurements of the X-ray reflectance in the range 2-10 keV of samples representative of coated silicon wafers that are proposed for the fabrication of the X-ray evolving universe spectrometer (XEUS) mission. We compare the reflectance of silicon samples coated with bare Pt......, with that for samples with an additional 10 nm thick carbon over-coating. We demonstrate a significant improvement in reflectance in the energy range similar to 1-4 keV, and at a grazing incidence angle of 10 mrad (0.57 degrees). We consider the resulting effective area that could be attained with an optimized design...

  17. Reactor for nano-focused x-ray diffraction and imaging under catalytic in situ conditions

    Science.gov (United States)

    Richard, M.-I.; Fernández, S.; Hofmann, J. P.; Gao, L.; Chahine, G. A.; Leake, S. J.; Djazouli, H.; De Bortoli, Y.; Petit, L.; Boesecke, P.; Labat, S.; Hensen, E. J. M.; Thomas, O.; Schülli, T.

    2017-09-01

    A reactor cell for in situ studies of individual catalyst nanoparticles or surfaces by nano-focused (coherent) x-ray diffraction has been developed. Catalytic reactions can be studied in flow mode in a pressure range of 10-2-103 mbar and temperatures up to 900 °C. This instrument bridges the pressure and materials gap at the same time within one experimental setup. It allows us to probe in situ the structure (e.g., shape, size, strain, faceting, composition, and defects) of individual nanoparticles using a nano-focused x-ray beam. Here, the setup was used to observe strain and facet evolution of individual model Pt catalysts during in situ experiments. It can be used for heating other (non-catalytically active) nanoparticles (e.g., nanowires) in inert or reactive gas atmospheres or vacuum as well.

  18. Electrochemical cell for in situ x-ray diffraction under ultrapure conditions

    DEFF Research Database (Denmark)

    Koop, T.; Schindler, W.; Kazimirov, A.

    1998-01-01

    of the crystal using a Luggin capillary and a standard reference electrode. We demonstrate the performance of our cell by in situ synchrotron x-ray diffraction measurements on ultrathin Co layers electrodeposited on Cu(001) in an aqueous H(2)SO(4)/CoSO(4) solution. (C) 1998 American Institute of Physics.......An electrochemical cell has been developed for in situ x-ray diffraction from a working electrode under clean conditions equivalent to ultrahigh vacuum conditions of 5 x 10(-10) mbar. The substrate crystals can be prepared ex situ and transferred into the cell under protection of ultrapure water...... within a few seconds. The oxygen level in the electrolyte is reduced by continuous N(2) flow to less than 0.2% compared to that of a fresh electrolyte. This can be done while rotating the cell by 360 degrees about the surface normal. The electrode potential is accurately measured at the position...

  19. X-ray reflectivity investigation of interlayer at interfaces of multilayer ...

    Indian Academy of Sciences (India)

    We report the effect of interlayer on multilayer X-ray reflectivity (XRR) profile using simulations at 8.047 keV (CuK) energy. We distinguished the effect of interfacial roughness and in-depth interlayer on reflectivity profile. The interfacial roughness reduces the intensity of individual peak while the in-depth interlayer ...

  20. X-ray measurements of total reflectivity and scattering from Au-coated foils

    DEFF Research Database (Denmark)

    Hornstrup, Allan; Christensen, Finn Erland; Jespersen, Ellen

    1990-01-01

    We present x-ray measurements of total reflectivity and scattering from gold-coated foils. The foils are two sorts of 0.3 mm thick dip-lacquered aluminum, 0.125 mm thick plastic (Upilex) and 0.5 mm thick dip-lacquered nickel. The analysis of the data shows a high reflectivity for all...

  1. X-Ray Measurements Of Total Reflectivity And Scattering From Au-Coated Foils

    DEFF Research Database (Denmark)

    Hornstrup, Allan; Christensen, Finn Erland; Schnopper, H. W.

    1989-01-01

    We present X-ray measurements of total reflectivity and scattering from gold coated foils. The foils are two sorts of 0.3 mm thick dip-lacquered aluminum, 0.125 mm thick plastic (Upilex) and 0.5 mm thick dip-lacquered nickel. The analysis of the data show a high reflectivity for all but the plastic...

  2. Characterization of multilayers by Fourier analysis of x-ray reflectivity

    NARCIS (Netherlands)

    Voorma, H. J.; E. Louis,; Koster, N. B.; F. Bijkerk,; Spiller, E.

    1997-01-01

    We discuss a new method to characterize multilayer structures with grazing-incidence reflectivity measurements using hard x-ray radiation, such as Cu-K-alpha or Mo-K-alpha radiation. The method is based on the analysis of the reverse Fourier transforms of the reflectivity at the Bragg peaks in

  3. X-ray reflectivity investigation of interlayer at interfaces of multilayer ...

    Indian Academy of Sciences (India)

    Argon ion etching gun was used for depth profiling of the. MLs. 3. Results. 3.1 Hard X-ray reflectivity. The typical angle dependent reflectivity spectra of Mo/Si .... defined multilayer structure with good control over depo- sited thicknesses. The decrease in intensity of the higher order peaks, compared to a two-layer model, ...

  4. Analysis of archaeological ceramics by total-reflection X-ray fluorescence: Quantitative approaches

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez-Ruiz, R. [Servicio Interdepartamental de Investigacion, Facultad de Ciencias, Universidad Autonoma de Madrid, Modulo C-9, Laboratorio de TXRF, Crta. Colmenar, Km 15, Cantoblanco, E-28049, Madrid (Spain)], E-mail: ramon.fernandez@uam.es; Garcia-Heras, M. [Grupo de Arqueometria de Vidrios y Materiales Ceramicos, Instituto de Historia, Centro de Ciencias Humanas y Sociales, CSIC, C/ Albasanz, 26-28, 28037 Madrid (Spain)

    2008-09-15

    This paper reports the quantitative methodologies developed for the compositional characterization of archaeological ceramics by total-reflection X-ray fluorescence at two levels. A first quantitative level which comprises an acid leaching procedure, and a second selective level, which seeks to increase the number of detectable elements by eliminating the iron present in the acid leaching procedure. Total-reflection X-ray fluorescence spectrometry has been compared, at a quantitative level, with Instrumental Neutron Activation Analysis in order to test its applicability to the study of this kind of materials. The combination of a solid chemical homogenization procedure previously reported with the quantitative methodologies here presented allows the total-reflection X-ray fluorescence to analyze 29 elements with acceptable analytical recoveries and accuracies.

  5. NASA's Chandra Finds That Saturn Reflects X-rays From Sun

    Science.gov (United States)

    2005-05-01

    When it comes to mysterious X-rays from Saturn, the ringed planet may act as a mirror, reflecting explosive activity from the sun, according to scientists using NASA's Chandra X-ray Observatory. The findings stem from the first observation of an X-ray flare reflected from Saturn's low-latitudes - the region that correlates to Earth's equator and tropics. Led by Dr. Anil Bhardwaj, a planetary scientist at NASA's Marshall Space Flight Center (MSFC) in Huntsville, Ala., the study revealed that Saturn acts as a diffuse mirror for solar X-rays. Counting photons - particles that carry electromagnetic energy including X-rays - was critical to this discovery. For every few thousand X-ray photons Saturn receives from the sun, it reflects a single X-ray photon back. Previous studies revealed that Jupiter, with a diameter 11 times that of Earth, behaves in a similar fashion. Saturn is about 9.5 times as big as Earth, but is twice as far from Earth as Jupiter. "The bigger the planet and nearer to the Sun, the more solar photons it will intercept - resulting in more reflected X-rays," said Bhardwaj. "These results imply we could use giant planets like Jupiter and Saturn as remote-sensing tools. By reflecting solar activity back to us, they could help us monitor X-ray flaring on portions of the sun facing away from Earth's space satellites." Massive solar explosions called flares often accompany coronal mass ejections, which emit solar material and magnetic field. When directed toward the Earth, these ejections can wreak havoc on communication systems from cell phones to satellites. Even as the research appears to have solved one mystery - the source of Saturn's X-rays, it fueled longstanding questions about magnetic fields. Earth's magnetic field is the reason compasses work, since the field acts like a huge bar magnet, causing the magnetic north pole of a compass to point to the magnetic south pole of the Earth. In addition, migratory birds seem to sense the magnetic field

  6. In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Lee, J. H.; Freeland, J. W.; Hong, Hawoong, E-mail: hhong@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Tung, I. C. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Department of Materials Science and Engineering, Northwestern University, Evanston, Illinois 60208 (United States); Chang, S.-H.; Bhattacharya, A.; Fong, D. D. [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

    2016-01-15

    In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques.

  7. In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Lee, J. H. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439, USA; Tung, I. C. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439, USA; Department of Materials Science and Engineering, Northwestern University, Evanston, Illinois 60208, USA; Chang, S. -H. [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439, USA; Bhattacharya, A. [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439, USA; Fong, D. D. [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439, USA; Freeland, J. W. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439, USA; Hong, Hawoong [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439, USA

    2016-01-01

    In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques.

  8. Cyclic olefin homopolymer-based microfluidics for protein crystallization and in situ X-ray diffraction

    Science.gov (United States)

    Emamzadah, Soheila; Petty, Tom J.; De Almeida, Victor; Nishimura, Taisuke; Joly, Jacques; Ferrer, Jean-Luc; Halazonetis, Thanos D.

    2009-01-01

    Microfluidics is a promising technology for the rapid iden­tification of protein crystallization conditions. However, most of the existing systems utilize silicone elastomers as the chip material which, despite its many benefits, is highly permeable to water vapour. This limits the time available for protein crystallization to less than a week. Here, the use of a cyclic olefin homopolymer-based microfluidics system for protein crystallization and in situ X-ray diffraction is described. Liquid handling in this system is performed in 2 mm thin transparent cards which contain 500 chambers, each with a volume of 320 nl. Microbatch, vapour-diffusion and free-interface diffusion protocols for protein crystallization were implemented and crystals were obtained of a number of proteins, including chicken lysozyme, bovine trypsin, a human p53 protein containing both the DNA-binding and oligomerization domains bound to DNA and a functionally important domain of Arabidopsis Morpheus’ molecule 1 (MOM1). The latter two polypeptides have not been crystallized previously. For X-ray diffraction analysis, either the cards were opened to allow mounting of the crystals on loops or the crystals were exposed to X-rays in situ. For lysozyme, an entire X-ray diffraction data set at 1.5 Å resolution was collected without removing the crystal from the card. Thus, cyclic olefin homopolymer-based microfluidics systems have the potential to further automate protein crystallization and structural genomics efforts. PMID:19690369

  9. Cyclic olefin homopolymer-based microfluidics for protein crystallization and in situ X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Emamzadah, Soheila [Department of Molecular Biology, University of Geneva, CH-1205 Geneva (Switzerland); Department of Biochemistry, University of Geneva, CH-1205 Geneva (Switzerland); Petty, Tom J. [Department of Molecular Biology, University of Geneva, CH-1205 Geneva (Switzerland); Biomedical Graduate Studies Genomics and Computational Biology Group, University of Pennsylvania, Philadelphia, PA 19104 (United States); De Almeida, Victor [Department of Molecular Biology, University of Geneva, CH-1205 Geneva (Switzerland); Department of Biochemistry, University of Geneva, CH-1205 Geneva (Switzerland); Nishimura, Taisuke [Department of Plant Biology, University of Geneva, CH-1205 Geneva (Switzerland); Joly, Jacques; Ferrer, Jean-Luc [Institut de Biologie Structurale J.-P. Ebel, CEA-CNRS-University J. Fourier, 38027 Grenoble CEDEX 1 (France); Halazonetis, Thanos D., E-mail: thanos.halazonetis@unige.ch [Department of Molecular Biology, University of Geneva, CH-1205 Geneva (Switzerland); Department of Biochemistry, University of Geneva, CH-1205 Geneva (Switzerland)

    2009-09-01

    A cyclic olefin homopolymer-based microfluidics system has been established for protein crystallization and in situ X-ray diffraction. Microfluidics is a promising technology for the rapid identification of protein crystallization conditions. However, most of the existing systems utilize silicone elastomers as the chip material which, despite its many benefits, is highly permeable to water vapour. This limits the time available for protein crystallization to less than a week. Here, the use of a cyclic olefin homopolymer-based microfluidics system for protein crystallization and in situ X-ray diffraction is described. Liquid handling in this system is performed in 2 mm thin transparent cards which contain 500 chambers, each with a volume of 320 nl. Microbatch, vapour-diffusion and free-interface diffusion protocols for protein crystallization were implemented and crystals were obtained of a number of proteins, including chicken lysozyme, bovine trypsin, a human p53 protein containing both the DNA-binding and oligomerization domains bound to DNA and a functionally important domain of Arabidopsis Morpheus’ molecule 1 (MOM1). The latter two polypeptides have not been crystallized previously. For X-ray diffraction analysis, either the cards were opened to allow mounting of the crystals on loops or the crystals were exposed to X-rays in situ. For lysozyme, an entire X-ray diffraction data set at 1.5 Å resolution was collected without removing the crystal from the card. Thus, cyclic olefin homopolymer-based microfluidics systems have the potential to further automate protein crystallization and structural genomics efforts.

  10. X-ray reflection and scatter measurements on selected optical samples

    Science.gov (United States)

    Fields, S. A.; Reynolds, J. M.; Holland, R. L.

    1975-01-01

    The results from an experimental program to determine the reflection efficiency and scatter parameters of selected optical samples are presented. The measurements were made using 8.34A X-rays at various angles of incidence. Selected samples were contaminated after being measured and then remeasured to determine the effects of contamination. The instrumentation involved in taking the data, including the X-ray reflectometer and data processing equipment, is discussed in detail. The condition of the optical surfaces, the total reflection measurements, the scatter measurements, and the analysis are discussed.

  11. Structure of Magainin and Alamethicin in Model Membranes Studied by X-Ray Reflectivity

    OpenAIRE

    Li, C.; Salditt, T.

    2006-01-01

    We have investigated the structure of lipid bilayers containing varied molar ratios of different lipids and the antimicrobial peptides magainin and alamethicin. For this structural study, we have used x-ray reflectivity on highly aligned solid-supported multilamellar lipid membranes. The reflectivity curves have been analyzed by semi-kinematical reflectivity theory modeling the bilayer density profile ρ(z). Model simulations of the reflectivity curves cover a large range of vertical momentum ...

  12. The adsorption of methanol and water on SAPO-34: in situ and ex situ X-ray diffraction studies

    DEFF Research Database (Denmark)

    Wragg, David S.; Johnsen, Rune; Norby, Poul

    2010-01-01

    The adsorption of methanol on SAPO-34 has been studied using a combination of in situ synchrotron powder X-ray diffraction to follow the process and ex situ high resolution powder diffraction to determine the structure. The unit cell volume of SAPO-34 is found to expand by 0.5% during methanol ad...... for adsorbed water molecules on the same framework, supporting the observation from the in situ data that water is more strongly bound than methanol. The results are consistent with previous results from thermodynamic and tapered element oscillating microbalance measurements.......The adsorption of methanol on SAPO-34 has been studied using a combination of in situ synchrotron powder X-ray diffraction to follow the process and ex situ high resolution powder diffraction to determine the structure. The unit cell volume of SAPO-34 is found to expand by 0.5% during methanol...

  13. On the use of CCD area detectors for high-resolution specular X-ray reflectivity.

    Science.gov (United States)

    Fenter, P; Catalano, J G; Park, C; Zhang, Z

    2006-07-01

    The use and application of charge coupled device (CCD) area detectors for high-resolution specular X-ray reflectivity is discussed. Direct comparison of high-resolution specular X-ray reflectivity data measured with CCD area detectors and traditional X-ray scintillator ('point') detectors demonstrates that the use of CCD detectors leads to a substantial (approximately 30-fold) reduction in data acquisition rates because of the elimination of the need to scan the sample to distinguish signal from background. The angular resolution with a CCD detector is also improved by a factor of approximately 3. The ability to probe the large dynamic range inherent to high-resolution X-ray reflectivity data in the specular reflection geometry was demonstrated with measurements of the orthoclase (001)- and alpha-Al2O3 (012)-water interfaces, with measured reflectivity signals varying by a factor of approximately 10(6) without the use of any beam attenuators. Statistical errors in the reflectivity signal are also derived and directly compared with the repeatability of the measurements.

  14. Increase in the Reflected Intensity of X-Ray Films Using Photonic Crystals

    Science.gov (United States)

    Aly, Arafa H.; Eissa, M. F.

    Photographic film is the familiar image of recording X-ray method. Examinations performed with radiographic intensifying screens reduce the patient’s exposure to radiation of X-rays compared with those without radiographic intensifying screens, where it directs less than half of the light emitted from the X-ray film with a screen interaction. A reflective layer made of magnesium oxide or titanium dioxide is located between the screen and the base of the film; this layer can help regain the control of the header light in other directions and is forwarded to the film. One-dimensional array of photonic crystals (PCs) consists of MgO with Al and TiO2 with Al used as reflectors. This array may increase the reflected intensity by an amount of 10.88% if MgO-Al PCs with periodicity N=1 are used as reflectors.

  15. X-Ray Reflectivity from the Surface of a Liquid Crystal:

    DEFF Research Database (Denmark)

    Pershan, P.S.; Als-Nielsen, Jens Aage

    1984-01-01

    X-ray reflectivity from the surface of a nematic liquid crystal is interpreted as the coherent superposition of Fresnel reflection from the surface and Bragg reflection from smectic order induced by the surface. Angular dependence of the Fresnel effect yields information on surface structure. Mea....... Measurement of the intensity of diffuse critical scattering relative to the Fresnel reflection yields the absolute value of the critical part of the density-density correlation function.......X-ray reflectivity from the surface of a nematic liquid crystal is interpreted as the coherent superposition of Fresnel reflection from the surface and Bragg reflection from smectic order induced by the surface. Angular dependence of the Fresnel effect yields information on surface structure...

  16. In Situ Ptychography of Heterogeneous Catalysts using Hard X-Rays

    DEFF Research Database (Denmark)

    Baier, Sina; Damsgaard, Christian Danvad; Scholz, Maria

    2016-01-01

    A new closed cell is presented for in situ X-ray ptychography which allows studies under gas flow and at elevated temperature. In order to gain complementary information by transmission and scanning electron microscopy, the cell makes use of a Protochips E-chipTM which contains a small, thin...... electron transparent window and allows heating. Two gold-based systems, 50 nm gold particles and nanoporous gold as a relevant catalyst sample, were used for studying the feasibility of the cell. Measurements showing a resolution around 40 nm have been achieved under a flow of synthetic air and during...... heating up to temperatures of 933 K. An elevated temperature exhibited little influence on image quality and resolution. With this study, the potential of in situ hard X-ray ptychography for investigating annealing processes of real catalyst samples is demonstrated. Furthermore, the possibility to use...

  17. Two-dimensional in situ metrology of X-ray mirrors using the speckle scanning technique.

    Science.gov (United States)

    Wang, Hongchang; Kashyap, Yogesh; Laundy, David; Sawhney, Kawal

    2015-07-01

    In situ metrology overcomes many of the limitations of existing metrology techniques and is capable of exceeding the performance of present-day optics. A novel technique for precisely characterizing an X-ray bimorph mirror and deducing its two-dimensional (2D) slope error map is presented. This technique has also been used to perform fast optimization of a bimorph mirror using the derived 2D piezo response functions. The measured focused beam size was significantly reduced after the optimization, and the slope error map was then verified by using geometrical optics to simulate the focused beam profile. This proposed technique is expected to be valuable for in situ metrology of X-ray mirrors at synchrotron radiation facilities and in astronomical telescopes.

  18. Observation of X-ray shadings in synchrotron radiation-total reflection X-ray fluorescence using a color X-ray camera

    Energy Technology Data Exchange (ETDEWEB)

    Fittschen, Ursula Elisabeth Adriane, E-mail: ursula.fittschen@chemie.uni-hamburg.de [Institut für Anorganische und Angewandte Chemie, Universität Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany); Menzel, Magnus [Institut für Anorganische und Angewandte Chemie, Universität Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany); Scharf, Oliver [IfG Institute for Scientific Instruments GmbH, Berlin (Germany); Radtke, Martin; Reinholz, Uwe; Buzanich, Günther [BAM Federal Institute of Materials Research and Testing, Berlin (Germany); Lopez, Velma M.; McIntosh, Kathryn [Los Alamos National Laboratory, Los Alamos, NM (United States); Streli, Christina [Atominstitut, TU Wien, Vienna (Austria); Havrilla, George Joseph [Los Alamos National Laboratory, Los Alamos, NM (United States)

    2014-09-01

    Absorption effects and the impact of specimen shape on TXRF analysis has been discussed intensively. Model calculations indicated that ring shaped specimens should give better results in terms of higher counts per mass signals than filled rectangle or circle shaped specimens. One major reason for the difference in signal is shading effects. Full field micro-XRF with a color X-ray camera (CXC) was used to investigate shading, which occurs when working with small angles of excitation as in TXRF. The device allows monitoring the illuminated parts of the sample and the shaded parts at the same time. It is expected that sample material hit first by the primary beam shade material behind it. Using the CXC shading could be directly visualized for the high concentration specimens. In order to compare the experimental results with calculation of the shading effect the generation of controlled specimens is crucial. This was achieved by “drop on demand” technology. It allows generating uniform, microscopic deposits of elements. The experimentally measured shadings match well with those expected from calculation. - Highlights: • Use of a color X-ray camera and drop on demand printing to diagnose X-ray shading • Specimens were obtained uniform and well-defined in shape and concentration by printing. • Direct visualization and determination of shading in such specimens using the camera.

  19. Nanocalorimeter platform for in situ specific heat measurements and x-ray diffraction at low temperature

    Science.gov (United States)

    Willa, K.; Diao, Z.; Campanini, D.; Welp, U.; Divan, R.; Hudl, M.; Islam, Z.; Kwok, W.-K.; Rydh, A.

    2017-12-01

    Recent advances in electronics and nanofabrication have enabled membrane-based nanocalorimetry for measurements of the specific heat of microgram-sized samples. We have integrated a nanocalorimeter platform into a 4.5 T split-pair vertical-field magnet to allow for the simultaneous measurement of the specific heat and x-ray scattering in magnetic fields and at temperatures as low as 4 K. This multi-modal approach empowers researchers to directly correlate scattering experiments with insights from thermodynamic properties including structural, electronic, orbital, and magnetic phase transitions. The use of a nanocalorimeter sample platform enables numerous technical advantages: precise measurement and control of the sample temperature, quantification of beam heating effects, fast and precise positioning of the sample in the x-ray beam, and fast acquisition of x-ray scans over a wide temperature range without the need for time-consuming re-centering and re-alignment. Furthermore, on an YBa2Cu3O7-δ crystal and a copper foil, we demonstrate a novel approach to x-ray absorption spectroscopy by monitoring the change in sample temperature as a function of incident photon energy. Finally, we illustrate the new insights that can be gained from in situ structural and thermodynamic measurements by investigating the superheated state occurring at the first-order magneto-elastic phase transition of Fe2P, a material that is of interest for magnetocaloric applications.

  20. Biblical Poetry as Ethical Reflection: An X-Ray | Nmah | UJAH ...

    African Journals Online (AJOL)

    UJAH: Unizik Journal of Arts and Humanities. Journal Home · ABOUT · Advanced Search · Current Issue · Archives · Journal Home > Special Edition 2011 >. Log in or Register to get access to full text downloads. Username, Password, Remember me, or Register. Biblical Poetry as Ethical Reflection: An X-Ray. PE Nmah ...

  1. Development of a total reflection X-ray fluorescence spectrometer for ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 25; Issue 5. Development of a total reflection X-ray fluorescence spectrometer for ultra-trace element analysis. M K Tiwari B Gowrishankar V K Raghuvanshi R V Nandedkar K J S Sawhney. Instrumentation Volume 25 Issue 5 October 2002 pp 435-441 ...

  2. Enhanced Reflectivity of Soft-X-Ray Multilayer Mirrors by Reduction of Si Atomic Density

    NARCIS (Netherlands)

    Schlatmann, R.; Keppel, A.; Xue, Y.; Verhoeven, J.; van der Wiel, M. J.

    1993-01-01

    We report a significant increase of the reflectivity of a soft x-ray Mo/Si multilayer mirror after low energy hydrogen ion beam bombardment of each of the Si layers after deposition. Cross section transmission electron microscopy pictures indicate no significant qualitative difference in interface

  3. Neutron and X-ray reflection from surface monolayers of a lipopolyoxazoline

    DEFF Research Database (Denmark)

    Wurlitzer, A.; Politsch, E.; Cevc, G.

    2000-01-01

    A new class of lipopolymers with polyoxazoline headgroups has been synthesized for the design of drug carriers, These amphiphatic molecules form stable monolayers at the air-water interface. Using X-ray and neutron reflectivity, the molecular conformations of the lipopolymer at the liquid surface...

  4. X-ray reflectivity theory for determining the density profile of a liquid under nanometre confinement.

    Science.gov (United States)

    Perret, Edith; Nygård, Kim; Satapathy, Dillip K; Balmer, Tobias E; Bunk, Oliver; Heuberger, Manfred; van der Veen, J Friso

    2010-07-01

    An X-ray reflectivity theory on the determination of the density profile of a molecular liquid under nanometre confinement is presented. The confinement geometry acts like an X-ray interferometer, which consists of two opposing atomically flat single-crystal mica membranes with an intervening thin liquid film of variable thickness. The X-rays reflected from the parallel crystal planes (of known structure) and the layered liquid in between them (of unknown structure) interfere with one another, making X-ray reflectivity highly sensitive to the liquid's density profile along the confinement direction. An expression for the reflected intensity as a function of momentum transfer is given. The total structure factor intensity for the liquid-filled confinement device is derived as a sum of contributions from the inner and outer crystal terminations. The method presented readily distinguishes the confined liquid from the liquid adsorbed on the outer mica surfaces. It is illustrated for the molecular liquid tetrakis(trimethyl)siloxysilane, confined by two mica surfaces at a distance of 8.6 nm.

  5. X-ray-reflectivity study of the growth kinetics of vapor-deposited silver films

    NARCIS (Netherlands)

    Thompson, C.; Palasantzas, G.; Feng, Y.P.; Krim, J.

    1994-01-01

    X-ray-reflectivity measurements have been carried out on silver films which were vapor deposited onto silicon substrates, to investigate the thickness evolution of the film’s surface roughness. The growth exponent was found to be β=0.26±0.05, and the roughness exponenet was found to be H=0.70±0.10.

  6. A facile method for the density determination of ceramic thin films using X-ray reflectivity

    NARCIS (Netherlands)

    Veldhuis, Sjoerd; Brinks, Peter; Stawski, Tomasz; Göbel, Ole; ten Elshof, Johan E.

    2014-01-01

    A fast and non-destructive method based on X-ray reflectivity was developed to determine the density of sol–gel derived ceramic thin films, without prior assumptions on the microstructure of the system. The thin film density is calculated from the critical angle θc, i.e. the maximum angle at which

  7. Interaction between Lipid Monolayers and Poloxamer 188: An X-Ray Reflectivity and Diffraction Study

    Science.gov (United States)

    Wu, Guohui; Majewski, Jaroslaw; Ege, Canay; Kjaer, Kristian; Weygand, Markus Jan; Lee, Ka Yee C.

    2005-01-01

    The mechanism by which poloxamer 188 (P188) seals a damaged cell membrane is examined using the lipid monolayer as a model system. X-ray reflectivity and grazing-incidence x-ray diffraction results show that at low nominal lipid density, P188, by physically occupying the available area and phase separating from the lipids, forces the lipid molecules to pack tightly and restore the barrier function of the membrane. Upon compression to bilayer equivalent pressure, P188 is squeezed out from the lipid monolayer, allowing a graceful exit of P188 when the membrane integrity is restored. PMID:16100276

  8. Reflection of femtosecond pulses from soft X-ray free-electron laser by periodical multilayers

    Energy Technology Data Exchange (ETDEWEB)

    Ksenzov, D.; Grigorian, S.; Pietsch, U. [Faculty of Physics, University of Siegen (Germany); Hendel, S.; Bienert, F.; Sacher, M.D.; Heinzmann, U. [Faculty of Physics, University of Bielefeld (Germany)

    2009-08-15

    Recent experiments on a soft X-ray free-electron laser (FEL) source (FLASH in Hamburg) have shown that multilayers (MLs) can be used as optical elements for highly intense X-ray irradiation. An effort to find most appropriate MLs has to consider the femtosecond time structure and the particular photon energy of the FEL. In this paper we have analysed the time response of 'low absorbing' MLs (e.g. such as La/B{sub 4}C) as a function of the number of periods. Interaction of a pulse train of Gaussian shaped sub-pulses using a realistic ML grown by electron-beam evaporation technique has been analysed in the soft-X-ray range. The structural parameters of the MLs were obtained by reflectivity measurements at BESSY II and subsequent profile fittings. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  9. In situ measurements of X-ray peak profile asymmetry from individual grains

    DEFF Research Database (Denmark)

    Wejdemann, Christian; Lienert, U.; Pantleon, Wolfgang

    2010-01-01

    Two copper samples, pre-deformed in tension to 5% plastic strain, are subjected to an in situ tensile deformation of 1% plastic strain while X-ray peak profiles from individual bulk grains are obtained. One sample is oriented with the in situ tensile axis parallel to the pre-deformation axis......, and peak profiles are obtained with the scattering vector parallel to this direction. The profiles show the expected asymmetry explained by the composite model as caused by intra-grain stresses. The other sample is oriented with the in situ tensile axis perpendicular to the pre-deformation axis, and peak...... profiles are obtained with the scattering vector parallel to the in situ tensile axis. In this case the profiles initially show an opposite asymmetry, but during the in situ deformation the asymmetry reverses sign as the deformation under new loading conditions leads to changes in the intra-grain stresses....

  10. Recent Developments in the X-Ray Reflectivity Analysis for Rough Surfaces and Interfaces of Multilayered Thin Film Materials

    OpenAIRE

    Yoshikazu Fujii

    2013-01-01

    X-ray reflectometry is a powerful tool for investigations on rough surface and interface structures of multilayered thin film materials. The X-ray reflectivity has been calculated based on the Parratt formalism, accounting for the effect of roughness by the theory of Nevot-Croce conventionally. However, in previous studies, the calculations of the X-ray reflectivity often show a strange effect where interference effects would increase at a rough surface. And estimated surface and interface ro...

  11. In situ X-ray diffraction studies on the piezoelectric response of PZT thin films

    Energy Technology Data Exchange (ETDEWEB)

    Davydok, A., E-mail: davydok@mpie.de [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France); Max-Planck-Institut für Eisenforschung, Department Structure and Nano-/Micromechanics of Materials, D-40237 Düsseldorf (Germany); Cornelius, T.W. [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France); Mocuta, C. [SOLEIL Synchrotron, DiffAbs beamline, L' Orme des Merisiers, Saint-Aubin - BP 48, 91192 Gif-sur-Yvette Cedex (France); Lima, E.C. [Universidade Federal do Tocantins, 77500-000 Porto Nacional, TO (Brazil); Araujo, E.B. [Departamento de Fisica e Quimica, Universidade Estadual Paulista, Av. Brasil, 56 Centro, 15385-000 Ilha Solteira, SP (Brazil); Thomas, O. [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France)

    2016-03-31

    Piezoelectric properties of randomly oriented self-polarized PbZr{sub 0.50}Ti{sub 0.50}O{sub 3} (PZT) thin films were investigated using in situ synchrotron X-ray diffraction. Possibilities for investigating the piezoelectric effect using micro-sized hard X-ray beams are demonstrated and perspectives for future dynamical measurements on PZT samples with variety of compositions and thicknesses are given. Studies performed on the crystalline [100, 110] directions evidenced piezoelectric anisotropy. The piezoelectric coefficient d{sub 33} was calculated in terms of the lab reference frame (d{sub perp}) and found to be two times larger along the [100] direction than along the [110] direction. The absolute values for the d{sub perp} amount to 120 and 230 pm/V being in good agreement with experimental and theoretical values found in literature for bulk PZT ceramics. - Highlights: • We performed in situ synchrotron X-ray diffraction studies on (PZT) thin films. • We discuss anisotropy of piezo effect in different crystallographic directions. • Perpendicular component Piezo coefficient of thin PZT layer is defined.

  12. Combined EUV reflectance and X-ray reflectivity data analysis of periodic multilayer structures.

    Science.gov (United States)

    Yakunin, S N; Makhotkin, I A; Nikolaev, K V; van de Kruijs, R W E; Chuev, M A; Bijkerk, F

    2014-08-25

    We present a way to analyze the chemical composition of periodical multilayer structures using the simultaneous analysis of grazing incidence hard X-Ray reflectivity (GIXR) and normal incidence extreme ultraviolet reflectance (EUVR). This allows to combine the high sensitivity of GIXR data to layer and interface thicknesses with the sensitivity of EUVR to the layer densities and atomic compositions. This method was applied to the reconstruction of the layered structure of a LaN/B multilayer mirror with 3.5 nm periodicity. We have compared profiles obtained by simultaneous EUVR and GIXR and GIXR-only data analysis, both reconstructed profiles result in a similar description of the layered structure. However, the simultaneous analysis of both EUVR and GIXR by a single algorithm lead to a ∼ 2x increased accuracy of the reconstructed layered model, or a more narrow range of solutions, as compared to the GIXR analysis only. It also explains the inherent difficulty of accurately predicting EUV reflectivity from a GIXR-only analysis.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-05-02

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

  14. In Situ X-ray Diffraction Studies of (De)lithiation Mechanism in Silicon Nanowire Anodes

    KAUST Repository

    Misra, Sumohan

    2012-06-26

    Figure Persented: Silicon is a promising anode material for Li-ion batteries due to its high theoretical specific capacity. From previous work, silicon nanowires (SiNWs) are known to undergo amorphorization during lithiation, and no crystalline Li-Si product has been observed. In this work, we use an X-ray transparent battery cell to perform in situ synchrotron X-ray diffraction on SiNWs in real time during electrochemical cycling. At deep lithiation voltages the known metastable Li 15Si 4 phase forms, and we show that avoiding the formation of this phase, by modifying the SiNW growth temperature, improves the cycling performance of SiNW anodes. Our results provide insight on the (de)lithiation mechanism and a correlation between phase evolution and electrochemical performance for SiNW anodes. © 2012 American Chemical Society.

  15. In situ X-ray diffraction studies of (de)lithiation mechanism in silicon nanowire anodes.

    Science.gov (United States)

    Misra, Sumohan; Liu, Nian; Nelson, Johanna; Hong, Seung Sae; Cui, Yi; Toney, Michael F

    2012-06-26

    Silicon is a promising anode material for Li-ion batteries due to its high theoretical specific capacity. From previous work, silicon nanowires (SiNWs) are known to undergo amorphorization during lithiation, and no crystalline Li-Si product has been observed. In this work, we use an X-ray transparent battery cell to perform in situ synchrotron X-ray diffraction on SiNWs in real time during electrochemical cycling. At deep lithiation voltages the known metastable Li(15)Si(4) phase forms, and we show that avoiding the formation of this phase, by modifying the SiNW growth temperature, improves the cycling performance of SiNW anodes. Our results provide insight on the (de)lithiation mechanism and a correlation between phase evolution and electrochemical performance for SiNW anodes.

  16. Understanding X-ray Reflection as a Probe of Accreting Black Holes

    Science.gov (United States)

    Wilkins, Dan

    2014-01-01

    Active galactic nuclei (AGN) are some of the most luminous objects we see in the Universe, powered by the accretion of matter onto a supermassive black hole in the centre of a galaxy, yet many of the physical processes by which the energy is released and injected into the surroundings remain a mystery. X-rays are emitted from a ‘corona’ of energetic particles surrounding the black hole and as well as being observed directly, they are seen to be reflected from the accreting disc, producing a number of spectral features including emission lines that are broadened by relativistic effects in the proximity of the black hole. In my thesis, I develop methods through which detailed measurement of the reflected X-rays from the accretion disc can be used to probe the innermost regions of accretion flow and corona, right down to the innermost stable orbit and the event horizon. Novel spectral analysis techniques allow us to reconstruct, from the observed relativistic X-ray reflection spectrum the spatially resolved illumination pattern of the accretion disc and will discuss how comparing this to the results of systematic general relativistic ray tracing simulations I have developed, we are able to constrain the location and geometry of the X-ray emitting corona and understand the dramatic change of the narrow line Seyfert 1 galaxy 1H 0707-495 into an extremely low flux state in terms of a collapse in the corona. I will discuss how measurements of the X-ray variability, specifically the reverberation time lags that are observed between variability in the directly observed X-rays from the corona and those reflected from the accretion disc add a further dimension to the study of accreting black holes, letting us not only build up a three dimensional image of the immediate vicinity of the black hole but also to probe mechanisms by which the energy is released from the accretion flow; techniques that will let us exploit not just current instrumentation but future proposed X-ray

  17. Three-dimensional coherent X-ray surface scattering imaging near total external reflection

    Science.gov (United States)

    Sun, Tao; Jiang, Zhang; Strzalka, Joseph; Ocola, Leonidas; Wang, Jin

    2012-09-01

    Lensless X-ray coherent diffraction imaging (CDI) has emerged as a thriving field promising applications in materials and biological sciences with a theoretical imaging resolution only limited by the X-ray wavelength. Most CDI methods use transmission geometry, which is not suitable for nanostructures grown on opaque substrates or for objects of interest comprising only surfaces or interfaces. Attempts have been made to perform CDI experiments in reflection geometry, both optically and with X-rays, but the reconstruction resulted in mostly planar images, with less success in the third dimension. Here, we discuss the development of coherent surface scattering imaging in grazing-incidence geometry that takes advantage of enhanced X-ray surface scattering and interference near total external reflection. We demonstrate the successful reconstruction of substrate-supported non-periodic surface patterns in three dimensions with nanometre resolution in the direction normal to the substrate, promising wide applications in elucidating structures in substrate-supported and buried nanoelectronics and photonics.

  18. ZnO thin film characterization by X-ray reflectivity optimization using genetic algorithm and Fourier transformation

    Energy Technology Data Exchange (ETDEWEB)

    Solookinejad, Ghahraman, E-mail: ghsolooki@gmail.com [Department of Physics, University of Isfahan, Hezar Jarib Street, Isfahan 81746-73441 (Iran, Islamic Republic of); Rozatian, Amir Sayid Hassan [Department of Physics, University of Isfahan, Hezar Jarib Street, Isfahan 81746-73441 (Iran, Islamic Republic of); Habibi, Mohammad Hossein [Department of Chemistry, University of Isfahan, Hezar Jarib Street, Isfahan 81746-73441 (Iran, Islamic Republic of)

    2011-10-15

    Zinc oxide (ZnO) thin film was fabricated by sol-gel spin coating method on glass substrate. X-ray reflectivity (XRR) and its optimization have been used for characterization and extracting physical parameters of the film. Genetic algorithm (GA) has been applied for this optimization process. The model independent information was needed to establish data analyzing process for X-ray reflectivity before optimization process. Independent information was exploited from Fourier transform of Fresnel reflectivity normalized X-ray reflectivity. This Fourier transformation (Auto Correlation Function) yields thickness of each coated layer on substrate. This information is a keynote for constructing optimization process. Specular X-ray reflectivity optimization yields structural parameters such as thickness, roughness of surface and interface and electron density profile of the film. Acceptable agreement exists between results obtained from Fourier transformation and X-ray reflectivity fitting.

  19. High-resolution x-ray scatter and reflectivity study of sputtered IR surfaces

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; Abdali, S.; Hornstrup, Allan

    1993-01-01

    In recent years there has been an increased interest in the possible use of Ir as the reflecting surface in X-ray telescope programs. An X-ray study of such surfaces produced by sputtering of Ir on highly polished Zerodur flats is presented here. The study was performed using Fe K(alpha) 1 (6.......404 Kev) and Cu K(alpha) 1 (8.048 keV) and includes measurement of total external reflection and scattering. The scattering measurement was made with three different instruments arrangements; one employed a 1D position sensitive detector for low resolution studies giving approximately 30 arcsec resolution...... (FWHM), and the other two arrangements employed channel cut crystals providing resolutions (FWHM) of 5 arcsec and 1 arcsec, respectively at Cu K(alpha) 1. The reflectivity study revealed a very close correspondence with a theoretical model based on recently published optical constants. This important...

  20. The Comptonization of accretion disc X-ray emission: consequences for X-ray reflection and the geometry of AGN coronae

    Science.gov (United States)

    Wilkins, D. R.; Gallo, L. C.

    2015-03-01

    We consider the Comptonization of the photons that make up the relativistically blurred reflection that is commonly detected from the accretion discs of active galactic nuclei by the coronae of energetic particles believed to give rise to the powerful X-ray continua by the inverse-Compton scattering of thermal seed photons from the disc. Recent measurements of the emissivity profiles of accretion discs as well as reverberation time lags between the primary X-ray continuum and the reflection suggest that this corona is situated at a low height above the disc and extends radially, tens of gravitational radii over the disc surface, hence should also Compton scatter the reflected X-rays. We find that the detection of blurred reflection from as close in as the innermost stable circular orbits (ISCOs) of maximally rotating black holes is consistent with such coronae, but requires that the corona be patchy, consisting perhaps of a number of isolated flares throughout the region. Considering only the requirement that it be possible to detect reflection from the ISCO, we find that at any given moment, the covering fraction of the inner part of the accretion disc by the corona needs to be less than 85 per cent, although the detection of `reflection-dominated' spectra in which the total reflected flux exceeds that seen in the continuum requires covering fractions as low as 50 or 25 per cent.

  1. Structure of magainin and alamethicin in model membranes studied by x-ray reflectivity.

    Science.gov (United States)

    Li, C; Salditt, T

    2006-11-01

    We have investigated the structure of lipid bilayers containing varied molar ratios of different lipids and the antimicrobial peptides magainin and alamethicin. For this structural study, we have used x-ray reflectivity on highly aligned solid-supported multilamellar lipid membranes. The reflectivity curves have been analyzed by semi-kinematical reflectivity theory modeling the bilayer density profile rho(z). Model simulations of the reflectivity curves cover a large range of vertical momentum transfer q(z), and yield excellent agreement between data and theory. The structural changes observed as a function of the molar peptide/lipid concentration P/L are discussed in a comparative way.

  2. Structure of Magainin and Alamethicin in Model Membranes Studied by X-Ray Reflectivity

    Science.gov (United States)

    Li, C.; Salditt, T.

    2006-01-01

    We have investigated the structure of lipid bilayers containing varied molar ratios of different lipids and the antimicrobial peptides magainin and alamethicin. For this structural study, we have used x-ray reflectivity on highly aligned solid-supported multilamellar lipid membranes. The reflectivity curves have been analyzed by semi-kinematical reflectivity theory modeling the bilayer density profile ρ(z). Model simulations of the reflectivity curves cover a large range of vertical momentum transfer qz, and yield excellent agreement between data and theory. The structural changes observed as a function of the molar peptide/lipid concentration P/L are discussed in a comparative way. PMID:16920839

  3. [Application of in situ micro energy dispersive X-ray fluorescence analysis in mineralogy].

    Science.gov (United States)

    Yang, Hai; Ge, Liang-Quan; Gu, Yi; Zhang, Qing-Xian; Xiong, Sheng-Qing

    2013-11-01

    Thirteen rock samples were collected for studying the variation of element content in the mineral during the alteration process from Xinjiang, China. The IED-6000 in situ micro energy dispersive X-ray fluorescence developed by CDUT was applied to get chemical and physical data from minerals. The non-destructive spectrometer is based on a low-power Mo-anode X-ray tube and a Si-PIN peltier cooled X-ray detector. The unique design of the tube's probe allows very close coupling of polycapillary and makes the use of micro-area measurement feasible and efficient. The spectrometer can be integrated into any microscope for analysis. The long axis diameter of beam spot is about 110 microm. According to micro-EDXRF measurement, the tetrahedrite was corrected to pyrite, improving the efficiency and accuracy of the mineral identification. The feldspar of mineralized rock sample is rich in Cu and Zn which can be used as prospecting indicator elements. Element content of Cr, Mn and Co shows negative correlation with the degree of mineralization.

  4. Total Reflection X-ray Fluorescence Analysis (TXRF) using the high flux SAXS camera

    CERN Document Server

    Wobrauschek, P; Pepponi, G; Bergmann, A; Glatter, O

    2002-01-01

    Combining the high photon flux from a rotating anode X-ray tube with an X-ray optical component to focus and monochromatize the X-ray beam is the most promising instrumentation for best detection limits in the modern XRF laboratory. This is realized by using the design of a high flux SAXS camera in combination with a 4 kW high brilliant rotating Cu anode X-ray tube with a graded elliptically bent multilayer and including a new designed module for excitation in total reflection geometry within the beam path. The system can be evacuated thus reducing absorption and scattering of air and removing the argon peak in the spectra. Another novelty is the use of a Peltier cooled drift detector with an energy resolution of 148 eV at 5.9 keV and 5 mm sup 2 area. For Co detection limits of about 300 fg determined by a single element standard have been achieved. Testing a real sample NIST 1643d led to detection limits in the range of 300 ng/l for the medium Z.

  5. X-ray reflection from cold white dwarfs in magnetic cataclysmic variables

    Science.gov (United States)

    Hayashi, Takayuki; Kitaguchi, Takao; Ishida, Manabu

    2018-02-01

    We model X-ray reflection from white dwarfs (WDs) in magnetic cataclysmic variables (mCVs) using a Monte Carlo simulation. A point source with a power-law spectrum or a realistic post-shock accretion column (PSAC) source irradiates a cool and spherical WD. The PSAC source emits thermal spectra of various temperatures stratified along the column according to the PSAC model. In the point-source simulation, we confirm the following: a source harder and nearer to the WD enhances the reflection; higher iron abundance enhances the equivalent widths (EWs) of fluorescent iron Kα1, 2 lines and their Compton shoulder, and increases the cut-off energy of a Compton hump; significant reflection appears from an area that is more than 90° apart from the position right under the point X-ray source because of the WD curvature. The PSAC simulation reveals the following: a more massive WD basically enhances the intensities of the fluorescent iron Kα1, 2 lines and the Compton hump, except for some specific accretion rate, because the more massive WD makes a hotter PSAC from which higher-energy X-rays are preferentially emitted; a larger specific accretion rate monotonically enhances the reflection because it makes a hotter and shorter PSAC; the intrinsic thermal component hardens by occultation of the cool base of the PSAC by the WD. We quantitatively estimate the influences of the parameters on the EWs and the Compton hump with both types of source. We also calculate X-ray modulation profiles brought about by the WD spin. These depend on the angles of the spin axis from the line of sight and from the PSAC, and on whether the two PSACs can be seen. The reflection spectral model and the modulation model involve the fluorescent lines and the Compton hump and can directly be compared to the data, which allows us to estimate these geometrical parameters with unprecedented accuracy.

  6. Enhanced reflectance X-ray absorption fine structure sensitivity using a whispering-gallery waveguide

    CERN Document Server

    Chernov, V A; Kovalenko, N V; Zolotarev, K V

    2000-01-01

    A new technique of reflectance X-ray absorption fine structure (REFL-XAFS) utilizing waveguides where X-rays are reflected many times along the waveguide surface is discussed. The multiple total reflection (MTR) phenomenon highly increases X-ray interaction with the waveguide surface and hence offers higher sensitivity compared to conventional (single reflection) REFL-XAFS. On the one hand, this technique is a direct structural method for characterizing waveguides (e.g. capillaries) where the application of other methods is very difficult. On the other hand, the conventional thin wafer can be transformed to a whispering-gallery (WG) waveguide by bending to a curved mirror. Ray tracing calculations demonstrate that the WG waveguide is very suitable for REFL-XAFS measurements. This method was experimentally realized for a cylindrically bent silica wafer with the surface covered with a GeO sub 2 monolayer. The Ge K-edge REFL-XAFS measurements were performed using both MTR and conventional techniques. The MTR tec...

  7. In situ X-ray pair distribution function analysis of geopolymer gel nanostructure formation kinetics.

    Science.gov (United States)

    White, Claire E; Provis, John L; Bloomer, Breaunnah; Henson, Neil J; Page, Katharine

    2013-06-14

    With the ever-increasing environmentally-driven demand for technologically advanced structural materials, geopolymer cement is fast becoming a viable alternative to traditional cements due to its proven engineering characteristics and the reduction in CO2 emitted during manufacturing (as much as 80% less CO2 emitted in manufacture, compared to ordinary Portland cement). Nevertheless, much remains unknown regarding the kinetics of reaction responsible for nanostructural evolution during the geopolymerisation process. Here, in situ X-ray total scattering measurements and pair distribution function (PDF) analysis are used to quantify the extent of reaction as a function of time for alkali-activated metakaolin/slag geopolymer binders, including the impact of various activators (alkali hydroxide/silicate) on the kinetics of the geopolymerisation reaction. Quantifying the reaction process in situ from X-ray PDF data collected during the initial ten hours can provide an estimate of the total reaction extent, but when combined with data obtained at longer times (128 days here) enables more accurate determination of the overall rate of reaction. To further assess the initial stages of the geopolymerisation reaction process, a pseudo-single step first order rate equation is fitted to the extent of reaction data, which reveals important mechanistic information regarding the role of free silica in the activators in the evolution of the binder systems. Hence, it is shown that in situ X-ray PDF analysis is an ideal experimental local structure tool to probe the reaction kinetics of complex reacting systems involving transitions between disordered/amorphous phases, of which geopolymerisation is an important example.

  8. Integrated x-ray reflectivity measurements of elliptically curved pentaerythritol crystals.

    Science.gov (United States)

    Haugh, M J; Regan, S P; Jacoby, K D; Ross, P W; Magoon, J; Barrios, M A; Emig, J A; Shoup, M J; Fournier, K B

    2012-10-01

    The elliptically curved pentaerythritol (PET) crystals used in the Supersnout 2 x-ray spectrometer on the National Ignition Facility at Lawrence Livermore National Laboratory have been calibrated photometrically in the range of 5.5-16 keV. The elliptical geometry provides broad spectral coverage and minimizes the degradation of spectral resolution due to the finite source size. The reflectivity curve of the crystals was measured using a x-ray line source. The integrated reflectivity (R(I)) and width of its curve (ΔΘ) were the measurements of major interest. The former gives the spectrometer throughput, and the latter gives the spectrometer resolving power. Both parameters are found to vary considerably with the radius of curvature of the crystal and with spectral energy. The results are attributed to an enhanced mosaic effect due to the increase in curvature. There are also contributions from the crystal cleaving and gluing processes.

  9. Setup for in situ X-ray diffraction studies of thin film growth by magnetron sputtering

    CERN Document Server

    Ellmer, K; Weiss, V; Rossner, H

    2001-01-01

    A novel method is described for the in situ-investigation of nucleation and growth of thin films during magnetron sputtering. Energy dispersive X-ray diffraction with synchrotron light is used for the structural analysis during film growth. An in situ-magnetron sputtering chamber was constructed and installed at a synchrotron radiation beam line with a bending magnet. The white synchrotron light (1-70 keV) passes the sputtering chamber through Kapton windows and hits one of the substrates on a four-fold sample holder. The diffracted beam, observed under a fixed diffraction angle between 3 deg. and 10 deg., is energy analyzed by a high purity Ge-detector. The in situ-EDXRD setup is demonstrated for the growth of tin-doped indium oxide (ITO) films prepared by reactive magnetron sputtering from a metallic target.

  10. In Situ Soft X-ray Spectromicroscopy of Early Tricalcium Silicate Hydration

    Science.gov (United States)

    Bae, Sungchul; Kanematsu, Manabu; Hernández-Cruz, Daniel; Moon, Juhyuk; Kilcoyne, David; Monteiro, Paulo J. M.

    2016-01-01

    The understanding and control of early hydration of tricalcium silicate (C3S) is of great importance to cement science and concrete technology. However, traditional characterization methods are incapable of providing morphological and spectroscopic information about in situ hydration at the nanoscale. Using soft X-ray spectromicroscopy, we report the changes in morphology and molecular structure of C3S at an early stage of hydration. In situ C3S hydration in a wet cell, beginning with induction (~1 h) and acceleration (~4 h) periods of up to ~8 h, was studied and compared with ex situ measurements in the deceleration period after 15 h of curing. Analysis of the near-edge X-ray absorption fine structure showed that the Ca binding energy and energy splitting of C3S changed rapidly in the early age of hydration and exhibited values similar to calcium silicate hydrate (C–S–H). The formation of C–S–H nanoseeds in the C3S solution and the development of a fibrillar C–S–H morphology on the C3S surface were visualized. Following this, silicate polymerization accompanied by C–S–H precipitation produced chemical shifts in the peaks of the main Si K edge and in multiple scattering. However, the silicate polymerization process did not significantly affect the Ca binding energy of C–S–H. PMID:28774096

  11. In Situ Soft X-ray Spectromicroscopy of Early Tricalcium Silicate Hydration

    Directory of Open Access Journals (Sweden)

    Sungchul Bae

    2016-12-01

    Full Text Available The understanding and control of early hydration of tricalcium silicate (C3S is of great importance to cement science and concrete technology. However, traditional characterization methods are incapable of providing morphological and spectroscopic information about in situ hydration at the nanoscale. Using soft X-ray spectromicroscopy, we report the changes in morphology and molecular structure of C3S at an early stage of hydration. In situ C3S hydration in a wet cell, beginning with induction (~1 h and acceleration (~4 h periods of up to ~8 h, was studied and compared with ex situ measurements in the deceleration period after 15 h of curing. Analysis of the near-edge X-ray absorption fine structure showed that the Ca binding energy and energy splitting of C3S changed rapidly in the early age of hydration and exhibited values similar to calcium silicate hydrate (C–S–H. The formation of C–S–H nanoseeds in the C3S solution and the development of a fibrillar C–S–H morphology on the C3S surface were visualized. Following this, silicate polymerization accompanied by C–S–H precipitation produced chemical shifts in the peaks of the main Si K edge and in multiple scattering. However, the silicate polymerization process did not significantly affect the Ca binding energy of C–S–H.

  12. In situ X-ray ptychography imaging of high-temperature CO2 acceptor particle agglomerates

    DEFF Research Database (Denmark)

    Høydalsvik, Kristin; Fløystad, Jostein Bø; Zhao, Tiejun

    2014-01-01

    Imaging nanoparticles under relevant reaction conditions of high temperature and gas pressure is difficult because conventional imaging techniques, like transmission electron microscopy, cannot be used. Here we demonstrate that the coherent diffractive imaging technique of X-ray ptychography can...... be used for in situ phase contrast imaging in structure studies at atmospheric pressure and elevated temperatures. Lithium zirconate, a candidate CO2 capture material, was studied at a pressure of one atmosphere in air and in CO2, at temperatures exceeding 600 °C. Images with a spatial resolution better...

  13. In situ X-ray diffraction environments for high-pressure reactions

    DEFF Research Database (Denmark)

    R. S. Hansen, Bjarne; Møller, Kasper Trans; Paskevicius, Mark

    2015-01-01

    New sample environments and techniques specifically designed for in situ powder X-ray diffraction studies up to 1000 bar (1 bar = 105 Pa) gas pressure are reported and discussed. The cells can be utilized for multiple purposes in a range of research fields. Specifically, investigations of gas......–solid reactions and sample handling under inert conditions are undertaken here. Sample containers allowing the introduction of gas from one or both ends are considered, enabling the possibility of flow-through studies. Various containment materials are evaluated, e.g. capillaries of single-crystal sapphire (Al2O3...

  14. Local detection of X-ray spectroscopies with an in-situ AFM

    OpenAIRE

    Rodrigues, Mario; Dhez, Olivier; Le Denmat, Simon; Chevrier, Joël; Felici, Roberto; Comin, Fabio

    2008-01-01

    International audience; The in situ combination of Scanning Probe Microscopies (SPM) with X-ray microbeams adds a variety of new possibilities to the panoply of synchrotron radiation techniques. In this paper we describe an optics-free AFM/STM that can be directly installed on synchrotron radiation end stations for such combined experiments. The instrument can be used just for AFM imaging of the investigated sample or can be used for detection of photoemitted electrons with a sharp STM-like t...

  15. In-Situ Silver Acetylide Silver Nitrate Explosive Deposition Measurements Using X-Ray Fluorescence.

    Energy Technology Data Exchange (ETDEWEB)

    Covert, Timothy Todd

    2014-09-01

    The Light Initiated High Explosive facility utilized a spray deposited coating of silver acetylide - silver nitrate explosive to impart a mechanical shock into targets of interest. A diagnostic was required to measure the explosive deposition in - situ. An X - ray fluorescence spectrometer was deployed at the facility. A measurement methodology was developed to measure the explosive quantity with sufficient accuracy. Through the use of a tin reference material under the silver based explosive, a field calibration relationship has been developed with a standard deviation of 3.2 % . The effect of the inserted tin material into the experiment configuration has been explored.

  16. In-situ x-ray absorption study of copper films in ground watersolutions

    Energy Technology Data Exchange (ETDEWEB)

    Kvashnina, K.O.; Butorin, S.M.; Modin, A.; Soroka, I.; Marcellini, M.; Nordgren, J.; Guo, J.-H.; Werme, L.

    2007-10-29

    This study illustrates how the damage from copper corrosion can be reduced by modifying the chemistry of the copper surface environment. The surface modification of oxidized copper films induced by chemical reaction with Cl{sup -} and HCO{sub 3}{sup -} in aqueous solutions was monitored by in situ X-ray absorption spectroscopy. The results show that corrosion of copper can be significantly reduced by adding even a small amount of sodium bicarbonate. The studied copper films corroded quickly in chloride solutions, whereas the same solution containing 1.1 mM HCO{sub 3}{sup -} prevented or slowed down the corrosion processes.

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

    Science.gov (United States)

    Deich, Alex; Alex

    2018-01-01

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

  18. Studies of float glass surfaces by neutron and x-ray reflection

    CERN Document Server

    Dalgliesh, R

    2001-01-01

    applicability of current off-specular scattering models. A rich surface structure has been found which results in reflection effects that cannot be explained by these models. Model systems have also been developed in an attempt to combine x-ray fluorescence techniques with reflectivity. The surface of glass and glass coatings have been studied using x-ray and neutron scattering techniques. In particular, the effect of aqueous solutions and humid atmospheres on both the fire polished and the tin rich side of float glass have been investigated using neutron and x-ray reflection. Isotopic substitution has enabled the number density of water molecules within the float glass surface to be monitored with respect to immersion time, temperature and impurity content. A thin gel-like water-rich layer of thickness approx 30A is observed at the surface accompanied by a more deeply penetrating layer which increases in depth with time reaching approx 500A after 6 months. The rate of water ingression is higher than predicte...

  19. Iterative reconstruction of a refractive-index profile from x-ray or neutron reflectivity measurements.

    Science.gov (United States)

    Hohage, Thorsten; Giewekemeyer, Klaus; Salditt, Tim

    2008-05-01

    Analysis of x-ray and neutron reflectivity is usually performed by modeling the density profile of the sample and performing a least square fit to the measured (phaseless) reflectivity data. Here we address the uniqueness of the reflectivity problem as well as its numerical reconstruction. In particular, we derive conditions for uniqueness, which are applicable in the kinematic limit (Born approximation), and for the most relevant case of box model profiles with Gaussian roughness. At the same time we present an iterative method to reconstruct the profile based on regularization methods. The method is successfully implemented and tested both on simulated and real experimental data.

  20. X-ray reflection from the inner disc of the AGN Ton S180

    Science.gov (United States)

    Parker, M. L.; Miller, J. M.; Fabian, A. C.

    2018-02-01

    We analyse a long archival XMM-Newton observation of the narrow-line Seyfert 1 galaxy Ton S180, using the latest reflection models to explore the high quality X-ray spectrum. We find that the iron line is relatively narrow and sharp, and the soft excess is extremely smooth. We cannot find an acceptable reflection model that describes both components, and conclude that the soft excess cannot be produced by relativistic reflection. Fitting the 3-10 keV band with relativistic reflection to model the iron line strongly prefers low spin values (reflection. This gives a much better fit than a pure reflection model, which again prefers a low spin value. The photon index of the reflection component is intermediate between the two Comptonization components, suggesting that both illuminate the disc a similar amount and therefore both contribute to the reflection.

  1. Advanced analysis techniques for X-ray reflectivities. Theory and application

    Energy Technology Data Exchange (ETDEWEB)

    Zimmermann, Klaus Martin

    2005-07-01

    The first part of this thesis adresses the phase problem in X-ray reflectivity. The analytical properties of the reflection coefficient imply that the phase is completely determined by the Hilbert transform of the logarithm of the modulus and the zeros in the upper half complex plane (UHP). To account in addition for interfacial roughness, a new formula for the Hilbert-phase is derived.In the following, the conditions for which the reflection coefficient has zeros in the UHP is discussed and the existing sufficient condition is extended to rough multi-layer systems. Procedures for locating these zeros are developed. The second part of this thesis introduces a new iterative inversion method for X-ray reflectivity. It expands the profile in a set of eigenfunctions, which are discrete approximations of the eigenfunction of the classical reconstruction problem of a compact supported function from its partially known Fourier-transform. In this work, piecewise constant functions, polygons and second-order B-splines are used to expand the density profile. The eigenvalue problems for the calculation of the above mentioned approximations are stated and solved. The formalism for the calculation of the reflection coefficient for these profiles is developed in dynamical and single-scattering theory. In the experimental part of this work iterative inverse schemes are applied to the analysis of X-ray reflectivity. Different sample systems are investigated: For two titanium-carbon samples tiny details at the Ti/C interface such as the formation of a thin TiC layer can be observed.The density profiles obtained from the reflectivities taken from nickel-carbon samples show the formation of SiC inside the Si sub strate. Finally, the new inversion scheme is applied to a series of reflectivities from a 700 AaSiGe film on a substrate.

  2. Parameter study of self-absorption effects in Total Reflection X-ray Fluorescence-X-ray Absorption Near Edge Structure analysis of arsenic

    Science.gov (United States)

    Meirer, F.; Pepponi, G.; Streli, C.; Wobrauschek, P.; Kregsamer, P.; Zoeger, N.; Falkenberg, G.

    2008-12-01

    Total reflection X-ray Fluorescence (TXRF) analysis in combination with X-ray Absorption Near Edge Structure (XANES) analysis is a powerful method to perform chemical speciation studies at trace element levels. However, when measuring samples with higher concentrations and in particular standards, damping of the oscillations is observed. In this study the influence of self-absorption effects on TXRF-XANES measurements was investigated by comparing measurements with theoretical calculations. As(V) standard solutions were prepared at various concentrations and dried on flat substrates. The measurements showed a correlation between the damping of the oscillations and the As mass deposited. A Monte-Carlo simulation was developed using data of the samples shapes obtained from confocal white light microscopy. The results showed good agreement with the measurements; they confirmed that the key parameters are the density of the investigated atom in the dried residues and the shape of the residue, parameters that combined define the total mass crossed by a certain portion of the incident beam. The study presents a simple approach for an a priori evaluation of the self-absorption in TXRF X-ray absorption studies. The consequences for Extended X-ray Absorption Fine Structure (EXAFS) and XANES measurements under grazing incidence conditions are discussed, leading to the conclusion that the damping of the oscillations seems to make EXAFS of concentrated samples non feasible. For XANES "fingerprint" analysis samples should be prepared with a deposited mass and sample shape leading to an acceptable absorption for the actual investigation.

  3. The application of x-ray fluorescence analysis with total external reflection for determining the microelements in coal

    Energy Technology Data Exchange (ETDEWEB)

    Krasnolutskii, V.P.; Losev, N.F.; Poluyanova, G.I. [Rostov Don State University, Rostov na Donu (Russian Federation)

    1995-09-01

    The results of studying the metrological parameters of a small-size energy dispersive x-ray fluorescence spectrometer with total external reflection of primary radiation are presented. The results of direct x-ray fluorescence measurement of spectral intensities from coal powder sample 1 mg in mass using the spectrometer are in agreement with the data of neutron activation and atomic emission analysis.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-07-27

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

  5. Measured reflectance of graded multilayer mirrors designed for astronomical hard X-ray telescopes

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; Craig, W.W.; Windt, D.L.

    2000-01-01

    Future astronomical X-ray telescopes, including the balloon-borne High-Energy Focusing Telescope (HEFT) and the Constellation-X Hard X-ray Telescope (Con-X HXT) plan to incorporate depth-graded multilayer coatings in order to extend sensitivity into the hard X-ray (10 less than or similar to E less......-graded W/Si multilayers optimized for broadband performance up to 69.5 keV (WK-edge). These designs are ideal for both the HEFT and Con-X HXT applications. We compare the measurements to model calculations to demonstrate that the reflectivity can be well described by the intended power law distribution...... than or similar to 80 keV) band. In this paper, we present measurements of the reflectance in the 18-170 keV energy range of a cylindrical prototype nested optic taken at the European Synchrotron Radiation Facility (ESRF). The mirror segments, mounted in a single bounce stack, are coated with depth...

  6. Non-destructive in situ study of "Mad Meg" by Pieter Bruegel the Elder using mobile X-ray fluorescence, X-ray diffraction and Raman spectrometers

    Science.gov (United States)

    Van de Voorde, Lien; Van Pevenage, Jolien; De Langhe, Kaat; De Wolf, Robin; Vekemans, Bart; Vincze, Laszlo; Vandenabeele, Peter; Martens, Maximiliaan P. J.

    2014-07-01

    "Mad Meg", a figure of Flemish folklore, is the subject of a famous oil-on-panel painting by the Flemish renaissance artist Pieter Bruegel the Elder, exhibited in the Museum Mayer van den Bergh (Antwerp, Belgium). This article reports on the in situ chemical characterization of this masterpiece by using currently available state-of-the-art portable analytical instruments. The applied non-destructive analytical approach involved the use of a) handheld X-ray fluorescence instrumentation for retrieving elemental information and b) portable X-ray fluorescence/X-ray diffraction instrumentation and laser-based Raman spectrometers for obtaining structural/molecular information. Next to material characterization of the used pigments and of the different preparation layers of the painting, also the verification of two important historical iconographic hypotheses is performed concerning the economic way of painting by Brueghel, and whether or not he used blue smalt pigment for painting the boat that appears towards the top of the painting. The pigments identified are smalt pigment (65% SiO2 + 15% K2O + 10% CoO + 5% Al2O3) for the blue color present in all blue areas of the painting, probably copper resinate for the green colors, vermillion (HgS) as red pigment and lead white is used to form different colors. The comparison of blue pigments used on different areas of the painting gives no differences in the elemental fingerprint which confirms the existing hypothesis concerning the economic painting method by Bruegel.

  7. RASOR: An advanced instrument for soft x-ray reflectivity and diffraction

    Science.gov (United States)

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

    2010-07-01

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

  8. Trace element determination in amniotic fluid by total reflection X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Greaves, E.D.; Sajo-Bohus, L.; Castelli, C.; Borgerg, C. [Universidad Simon Bolivar, Caracas (Venezuela); Meitin, J.; Liendo, J.

    1995-03-01

    A new method is reported for the determination of Fe, Cu, Zn, and Br in amniotic fluid (AF) by Total Reflection X-Ray Fluorescence. The irradiation of AF samples with monochromatic X-Rays reduces the scattering background from the organic matrix and avoids the need for sample digestion. Sample manipulation is reduced to centrifuging and adding cobalt as internal standard. Lower detection limits obtained are 109, 53, 44 and 37 ppb for Fe, Cu, Zn and Br respectively. Measurement precision depends on element concentrations and can be as low as 1.5% SD. Results of the analysis of 34 AF samples from Venezuelan pregnant patients agree with previously reported ranges of Fe, Cu and Zn. Other elements observed but not quantified are Cl, K, Ca in all spectra and Pb and Sr in some of them. (author).

  9. Microlensing Constraints on Quasar Spins and X-ray Reflection Regions

    Science.gov (United States)

    Dai, Xinyu

    2017-08-01

    Gravitational microlensing provides a unique probe of the innermost parts of quasar accretion disks, close to the event horizon of supermassive black holes. Using Chandra monitoring data of six lenses from two Large Programs in Cycles 11 and 14/15, we identified two microlensing effects that can be used to constrain black hole spins and X-ray reflection regions for high redshift quasars. The first effect is the excess iron line equivalent widths of lensed quasars compared to normal AGN, and the second is the distribution of iron line peak energies of lensed quasars. A microlensing analysis of the iron line equivalent widths prefers high spin values and very steep iron line emissivity profiles for quasars at z~2. We will also discuss the prospect of measuring quasar spins with microlensing using the next generation of X-ray telescopes.

  10. Beer analysis by synchrotron radiation total reflection X-ray fluorescence (SR-TXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo. Dept. de Recursos Hidricos]. E-mail: silvana@fec.unicamp.br; Vives, Ana Elisa S. de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Nascimento Filho, Virgilio F. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear]. E-mail: virgilio@cena.usp.br; Zucchi, Orgheda L.D.A. [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas de Ribeirao Preto]. E-mail: olzucchi@fcfrp.usp.br

    2005-07-01

    In this work the concentrations of P, S, Cl, K, Ca, Mn, Fe, Zn and Br in twenty-nine brands of national and international beers were determined by Synchrotron Radiation Total Reflection X-Ray Fluorescence analysis (SR-TXRF). The results were compared with the limits established by the Brazilian Legislation and the nutritive values established by National Agricultural Library (NAL). The measurements were performed at the X-ray Fluorescence Beamline at Synchrotron Light Source Laboratory, in Campinas, Sao Paulo, Brazil, using a polychromatic beam for excitation. A small volume of 5 {mu}L of sample beers containing just an internal standard, used to correct geometry effects, were analyzed without any pre-treatment. The measuring time was 100 s and the detection limits obtained varied from 1{mu}g.L{sup -1} for Mn and Fe to 15{mu}g.L{sup -1} for P. (author)

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

    Science.gov (United States)

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

    2010-07-01

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

  12. In situ azimuthal rotation device for linear dichroism measurements in scanning transmission x-ray microscopy

    Science.gov (United States)

    Hernández-Cruz, D.; Hitchcock, A. P.; Tyliszczak, T.; Rousseau, M.-E.; Pézolet, M.

    2007-03-01

    A novel miniature rotation device used in conjunction with a scanning transmission x-ray microscope is described. It provides convenient in situ sample rotation to enable measurements of linear dichroism at high spatial resolution. The design, fabrication, and mechanical characterization are presented. This device has been used to generate quantitative maps of the spatial distribution of the orientation of proteins in several different spider and silkworm silks. Specifically, quantitative maps of the dichroic signal at the C 1s→π*amide transition in longitudinal sections of the silk fibers give information about the spatial orientation, degree of alignment, and spatial distribution of protein peptide bonds. A new approach for analyzing the dichroic signal to extract orientation distributions, in addition to magnitudes of aligned components, is presented and illustrated with results from Nephila clavipes dragline spider silk measured using the in situ rotation device.

  13. Advanced in situ metrology for x-ray beam shaping with super precision.

    Science.gov (United States)

    Wang, Hongchang; Sutter, John; Sawhney, Kawal

    2015-01-26

    We report a novel method for in situ metrology of an X-ray bimorph mirror by using the speckle scanning technique. Both the focusing beam and the "tophat" defocussed beam have been generated by optimizing the bimorph mirror in a single iteration. Importantly, we have demonstrated that the angular sensitivity for measuring the slope error of an optical surface can reach accuracy in the range of two nanoradians. When compared with conventional ex-situ metrology techniques, the method enables a substantial increase of around two orders of magnitude in the angular sensitivity and opens the way to a previously inaccessible region of slope error measurement. Such a super precision metrology technique will be beneficial for both the manufacture of polished mirrors and the optimization of beam shaping.

  14. Simultaneous measurements of X-ray reflectivity and grazing incidence fluorescence at BL-16 beamline of Indus-2.

    Science.gov (United States)

    Das, Gangadhar; Kane, S R; Khooha, Ajay; Singh, A K; Tiwari, M K

    2015-05-01

    A new multipurpose x-ray reflectometer station has been developed and augmented at the microfocus beamline (BL-16) of Indus-2 synchrotron radiation source to facilitate synchronous measurements of specular x-ray reflectivity and grazing incidence x-ray fluorescence emission from thin layered structures. The design and various salient features of the x-ray reflectometer are discussed. The performance of the reflectometer has been evaluated by analyzing several thin layered structures having different surface interface properties. The results reveal in-depth information for precise determination of surface and interface properties of thin layered materials demonstrating the immense potential of the combined measurements of x-ray reflectivity and grazing incidence fluorescence on a single reflectometer.

  15. Speckle-based portable device for in-situ metrology of x-ray mirrors at Diamond Light Source

    Science.gov (United States)

    Wang, Hongchang; Kashyap, Yogesh; Zhou, Tunhe; Sawhney, Kawal

    2017-09-01

    For modern synchrotron light sources, the push toward diffraction-limited and coherence-preserved beams demands accurate metrology on X-ray optics. Moreover, it is important to perform in-situ characterization and optimization of X-ray mirrors since their ultimate performance is critically dependent on the working conditions. Therefore, it is highly desirable to develop a portable metrology device, which can be easily implemented on a range of beamlines for in-situ metrology. An X-ray speckle-based portable device for in-situ metrology of synchrotron X-ray mirrors has been developed at Diamond Light Source. Ultra-high angular sensitivity is achieved by scanning the speckle generator in the X-ray beam. In addition to the compact setup and ease of implementation, a user-friendly graphical user interface has been developed to ensure that characterization and alignment of X-ray mirrors is simple and fast. The functionality and feasibility of this device is presented with representative examples.

  16. A flow cell for transient voltammetry and in situ grazing incidence X-ray diffraction characterization of electrocrystallized cadmium(II) tetracyanoquinodimethane

    Energy Technology Data Exchange (ETDEWEB)

    Veder, Jean-Pierre [Nanochemistry Research Institute, Department of Chemistry, Curtin University, GPO Box U1987, Perth, Western Australia 6845 (Australia); Nafady, Ayman [School of Chemistry, Monash University, Clayton, Victoria 3800 (Australia); Clarke, Graeme [Nanochemistry Research Institute, Department of Chemistry, Curtin University, GPO Box U1987, Perth, Western Australia 6845 (Australia); Williams, Ross P. [Centre for Materials Research, Department of Imaging and Applied Physics, Curtin University, GPO Box U1987, Perth, Western Australia 6845 (Australia); De Marco, Roland, E-mail: r.demarco@curtin.edu.a [Nanochemistry Research Institute, Department of Chemistry, Curtin University, GPO Box U1987, Perth, Western Australia 6845 (Australia); Bond, Alan M. [School of Chemistry, Monash University, Clayton, Victoria 3800 (Australia)

    2011-01-01

    An easy to fabricate and versatile cell that can be used with a variety of electrochemical techniques, also meeting the stringent requirement for undertaking cyclic voltammetry under transient conditions in in situ electrocrystallization studies and total external reflection X-ray analysis, has been developed. Application is demonstrated through an in situ synchrotron radiation-grazing incidence X-ray diffraction (SR-GIXRD) characterization of electrocrystallized cadmium (II)-tetracyanoquinodimethane material, Cd(TCNQ){sub 2}, from acetonitrile (0.1 mol dm{sup -3} [NBu{sub 4}][PF{sub 6}]). Importantly, this versatile cell design makes SR-GIXRD suitable for almost any combination of total external reflection X-ray analysis (e.g., GIXRF and GIXRD) and electrochemical perturbation, also allowing its application in acidic, basic, aqueous, non-aqueous, low and high flow pressure conditions. Nevertheless, the cell design separates the functions of transient voltammetry and SR-GIXRD measurements, viz., voltammetry is performed at high flow rates with a substantially distended window to minimize the IR (Ohmic) drop of the electrolyte, while SR-GIXRD is undertaken using stop-flow conditions with a very thin layer of electrolyte to minimize X-ray absorption and scattering by the solution.

  17. Combined evaluation of grazing incidence X-ray fluorescence and X-ray reflectivity data for improved profiling of ultra-shallow depth distributions.

    Science.gov (United States)

    Ingerle, D; Meirer, F; Pepponi, G; Demenev, E; Giubertoni, D; Wobrauschek, P; Streli, C

    2014-09-01

    The continuous downscaling of the process size for semiconductor devices pushes the junction depths and consequentially the implantation depths to the top few nanometers of the Si substrate. This motivates the need for sensitive methods capable of analyzing dopant distribution, total dose and possible impurities. X-ray techniques utilizing the external reflection of X-rays are very surface sensitive, hence providing a non-destructive tool for process analysis and control. X-ray reflectometry (XRR) is an established technique for the characterization of single- and multi-layered thin film structures with layer thicknesses in the nanometer range. XRR spectra are acquired by varying the incident angle in the grazing incidence regime while measuring the specular reflected X-ray beam. The shape of the resulting angle-dependent curve is correlated to changes of the electron density in the sample, but does not provide direct information on the presence or distribution of chemical elements in the sample. Grazing Incidence XRF (GIXRF) measures the X-ray fluorescence induced by an X-ray beam incident under grazing angles. The resulting angle dependent intensity curves are correlated to the depth distribution and mass density of the elements in the sample. GIXRF provides information on contaminations, total implanted dose and to some extent on the depth of the dopant distribution, but is ambiguous with regard to the exact distribution function. Both techniques use similar measurement procedures and data evaluation strategies, i.e. optimization of a sample model by fitting measured and calculated angle curves. Moreover, the applied sample models can be derived from the same physical properties, like atomic scattering/form factors and elemental concentrations; a simultaneous analysis is therefore a straightforward approach. This combined analysis in turn reduces the uncertainties of the individual techniques, allowing a determination of dose and depth profile of the implanted

  18. In situ X-ray diffraction study of crystallization process of GeSbTe thin films during heat treatment

    Energy Technology Data Exchange (ETDEWEB)

    Kato, Naohiko [Toyota Central R and D Labs., Inc., Nagakute, Aichi 480-1192 (Japan)]. E-mail: e0957@mosk.tytlabs.co.jp; Konomi, Ichiro [Toyota Central R and D Labs., Inc., Nagakute, Aichi 480-1192 (Japan); Seno, Yoshiki [Toyota Central R and D Labs., Inc., Nagakute, Aichi 480-1192 (Japan); Motohiro, Tomoyoshi [Toyota Central R and D Labs., Inc., Nagakute, Aichi 480-1192 (Japan)

    2005-05-15

    The crystallization processes of the Ge{sub 2}Sb{sub 2}Te{sub 5} thin film used for PD and DVD-RAM were studied in its realistic optical disk film configurations for the first time by X-ray diffraction using an intense X-ray beam of a synchrotron orbital radiation facility (SPring-8) and in situ quick detection with a Position-Sensitive-Proportional-Counter. The dependence of the amorphous-to-fcc phase-change temperature T{sub 1} on the rate of temperature elevation R{sub et} gave an activation energy E{sub a}: 0.93 eV much less than previously reported 2.2 eV obtained from a model sample 25-45 times thicker than in the real optical disks. The similar measurement on the Ge{sub 4}Sb{sub 1}Te{sub 5} film whose large reflectance change attains the readability by CD-ROM drives gave E{sub a}: 1.13 eV with larger T{sub 1} than Ge{sub 2}Sb{sub 2}Te{sub 5} thin films at any R{sub et} implying a lower sensitivity in erasing as well as a better data stability of the phase-change disk.

  19. An apparatus for in situ x-ray scattering measurements during polymer injection molding.

    Science.gov (United States)

    Rendon, Stanley; Fang, Jun; Burghardt, Wesley R; Bubeck, Robert A

    2009-04-01

    We report a novel instrument for synchrotron-based in situ x-ray scattering measurements during injection molding processing. It allows direct, real-time monitoring of molecular-scale structural evolution in polymer materials undergoing a complex processing operation. The instrument is based on a laboratory-scale injection molding machine, and employs customized mold tools designed to allow x-ray access during mold filling and subsequent solidification, while providing sufficient robustness to withstand high injection pressures. The use of high energy, high flux synchrotron radiation, and a fast detector allows sufficiently rapid data acquisition to resolve time-dependent orientation dynamics in this transient process. Simultaneous monitoring of temperature and pressure signals allows transient scattering data to be referenced to various stages of the injection molding cycle. Representative data on a commercial liquid crystalline polymer, Vectra(R) B950, are presented to demonstrate the features of this apparatus; however, it may find application in a wide range of polymeric materials such as nanocomposites, semicrystalline polymers and fiber-reinforced thermoplastics.

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

    Science.gov (United States)

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

    2017-11-01

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

  1. Characterization of ion-bombardment induced modifications of periodic La/B{sub 4}C-multilayer-mirrors for the reflection of soft X-ray radiation

    Energy Technology Data Exchange (ETDEWEB)

    Merschjohann, Fabian; Lass, Maike; Gorholt, Lennart; Sacher, Marc D.; Heinzmann, Ulrich [Molecular and Surface Physics, Bielefeld University (Germany); Schaefers, Franz [Helmholtz-Zentrum Berlin fuer Materialien und Energie, Elektronenspeicherring BESSY II (Germany)

    2010-07-01

    The applicability of reflective optical components for the soft X-Ray region depends on the existence of multilayer-optics. Therefore stacks of alternating layers of two materials with different refractive index are applied. For the photon energy range of 100-190 eV Lanthanum (La) is favoured as the absorber material and Boroncarbide (B{sub 4}C) as the spacer material. Thin periodic layer systems of those materials with double layer periods of 5.6 nm have been produced by UHV Electron Beam Evaporation. The layer thickness is controlled by in-situ X-Ray Reflectometry. The purity and the stoichiometry of the layers has been analyzed by electron beam induced in-situ Auger Spectroscopy. Ion Polishing of each interface should diminish the interface roughness and thus enhance the reflectivity. The modification of the La- and B{sub 4}C-layers due to ion bombardment has been investigated by the in-situ Auger Spectroscopy, ex-situ X-Ray Diffraction and at-wavelength reflectivity measurements by use of Synchrotron radiation at the BESSY II facility. Effects of compaction, mixing, sputter-etching and smoothing have been found. The modifications can be influenced by varying the kinetic energy of the ions and/or the duration of the treatment.

  2. Reflectivity Around the Gold M-Edges of X-ray Reflector of the Soft X-Ray Telescope Onboard ASTRO-H

    Science.gov (United States)

    Kurashimaa, Sho; Furuzawa, Akihiro; Sato, Toshiki; Kikuchia, Naomichi; Nakaniwaa, Nozomi; Maeda, Yoshitomo; Ishida, Manabu; Izuka, Ryo; Okajima, Takashi; Mori, Hideyuki; hide

    2016-01-01

    The X-ray astronomy satellite ASTRO-H are equipped with two equivalent soft X-ray telescopes (SXT-I and SXT-S) which cover the energy band 0.3-12 keV. The X-ray reflectors of the SXTs are coated with a gold monolayer by means of the replication technique. A series of gold M absorption edges in the 2-4 keV band causes complex structures in the energy response of the SXTs. In the same band, there are astrophysically important emission lines from Si, Ar and S. Since the SXS has unprecedentedly high spectral resolution, we have measured the reflectivity around the gold M-edges in an extremely fine energy pitch at the synchrotron radiation facility KEK PF BL11-B, with the 2 eV pitch in 2100 eV to 4100 eV band that covers the entire series of the absorption edges (M-I through M-V) at grazing incident angles to the reflectors of 0.5, 0.8, 1.0, 1.2, 1.4 degree, and with a finer pitch of 0.25 eV in the 2200 eV to 2350 eV band where the two deepest M-IV and M-V edges are included. In the resultant reflectivity curves, we have clearly identified the fine structures associated with all the M-edges. Using these data, we calculated atomic scattering factor f1 as a function of X-ray energy, with which we have built the mirror response function which can be applied to the Suzaku spectra. As a result, we have found that discrepancy of the spectral model to the Suzaku data of 4U1630-472 (a black hole transient) and the Crab nebula around the M-edges are significantly reduced from those with the official Suzaku response.

  3. Local and long range order in promoted iron-based Fischer–Tropsch catalysts: a combined in situ X-ray absorption spectroscopy/wide angle X-ray scattering study

    NARCIS (Netherlands)

    de Smit, E.|info:eu-repo/dai/nl/304824232; Beale, A.M.|info:eu-repo/dai/nl/325802068; Nikitenko, S.; Weckhuysen, B.M.|info:eu-repo/dai/nl/285484397

    2009-01-01

    The structural properties of three Fe-based Fischer–Tropsch synthesis (FTS) catalysts containing different amounts of Cu, K and SiO2 additives were investigated during pretreatment and FTS in a fixed bed-like reactor using combined in situ X-ray absorption fine structure (XAFS)/wide angle X-ray

  4. Structural investigations of self-assembled monolayers for organic electronics: results from X-ray reflectivity.

    Science.gov (United States)

    Khassanov, Artoem; Steinrück, Hans-Georg; Schmaltz, Thomas; Magerl, Andreas; Halik, Marcus

    2015-07-21

    Self-assembled monolayers (SAMs) have been established as crucial interlayers and electronically active layers in organic electronic devices, such as organic light emitting diodes (OLEDs), organic photovoltaics (OPVs), organic thin film transistors (OTFTs), and nonvolatile memories (NVMs). The use of self-assembling functionalized organic molecules is beneficial due to mainly three advantages compared with common thin film deposition approaches. (1) Molecular self-assembly occurs with surface selectivity, determined by the interaction between the functional anchor group of the organic molecules and the target surface. (2) The film thickness of the resulting layers is perfectly controllable on the angstrom scale, due to the self-terminating film formation to only a single molecular layer. And finally, (3) the wide variability in the chemical structure of such molecules enables different SAM functionalities for devices, ranging from electrical insulation to charge storage to charge transport. The SAM approach can be further expanded by employing several functionalized molecules to create mixed SAMs with consequently mixed properties. The function of SAMs in devices depends not only on the chemical structure of the molecules but also on their final arrangement and orientation on the surface. A reliable and nondestructive in-depth characterization of SAMs on nonconductive oxide surfaces is still challenging because of the very small thickness and the impracticality of methods such as scanning tunneling microscopy (STM) and X-ray photoelectron spectroscopy (XPS). In this Account, we illustrate how X-ray reflectivity (XRR) provides analytical access to major questions of SAM composition, morphology, and even formation by means of investigations of pure and mixed SAMs based on phosphonic acids (PAs) of various chain structures on flat alumina (AlOx) surfaces. XRR is an analytical method that provides access to spatially averaged structural depth profiles over a relatively

  5. Final Report on Developing Microstructure-Property Correlation in Reactor Materials using in situ High-Energy X-rays

    Energy Technology Data Exchange (ETDEWEB)

    Li, Meimei [Argonne National Lab. (ANL), Argonne, IL (United States); Almer, Jonathan D. [Argonne National Lab. (ANL), Argonne, IL (United States); Yang, Yong [Univ. of Florida, Gainesville, FL (United States); Tan, Lizhen [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2016-01-01

    This report provides a summary of research activities on understanding microstructure – property correlation in reactor materials using in situ high-energy X-rays. The report is a Level 2 deliverable in FY16 (M2CA-13-IL-AN_-0403-0111), under the Work Package CA-13-IL-AN_- 0403-01, “Microstructure-Property Correlation in Reactor Materials using in situ High Energy Xrays”, as part of the DOE-NE NEET Program. The objective of this project is to demonstrate the application of in situ high energy X-ray measurements of nuclear reactor materials under thermal-mechanical loading, to understand their microstructure-property relationships. The gained knowledge is expected to enable accurate predictions of mechanical performance of these materials subjected to extreme environments, and to further facilitate development of advanced reactor materials. The report provides detailed description of the in situ X-ray Radiated Materials (iRadMat) apparatus designed to interface with a servo-hydraulic load frame at beamline 1-ID at the Advanced Photon Source. This new capability allows in situ studies of radioactive specimens subject to thermal-mechanical loading using a suite of high-energy X-ray scattering and imaging techniques. We conducted several case studies using the iRadMat to obtain a better understanding of deformation and fracture mechanisms of irradiated materials. In situ X-ray measurements on neutron-irradiated pure metal and model alloy and several representative reactor materials, e.g. pure Fe, Fe-9Cr model alloy, 316 SS, HT-UPS, and duplex cast austenitic stainless steels (CASS) CF-8 were performed under tensile loading at temperatures of 20-400°C in vacuum. A combination of wide-angle X-ray scattering (WAXS), small-angle X-ray scattering (SAXS), and imaging techniques were utilized to interrogate microstructure at different length scales in real time while the specimen was subject to thermal-mechanical loading. In addition, in situ X-ray studies were

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

    Science.gov (United States)

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

    2015-12-23

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

  7. X-ray reflectivity measurement of interdiffusion in metallic multilayers during rapid heating

    Science.gov (United States)

    Liu, J. P.; Kirchhoff, J.; Zhou, L.; Zhao, M.; Grapes, M. D.; Dale, D. S.; Tate, M. D.; Philipp, H. T.; Gruner, S. M.; Weihs, T. P.; Hufnagel, T. C.

    2017-01-01

    A technique for measuring interdiffusion in multilayer materials during rapid heating using X-ray reflectivity is described. In this technique the sample is bent to achieve a range of incident angles simultaneously, and the scattered intensity is recorded on a fast high-dynamic-range mixed-mode pixel array detector. Heating of the multilayer is achieved by electrical resistive heating of the silicon substrate, monitored by an infrared pyrometer. As an example, reflectivity data from Al/Ni heated at rates up to 200 K s−1 are presented. At short times the interdiffusion coefficient can be determined from the rate of decay of the reflectivity peaks, and it is shown that the activation energy for interdiffusion is consistent with a grain boundary diffusion mechanism. At longer times the simple analysis no longer applies because the evolution of the reflectivity pattern is complicated by other processes, such as nucleation and growth of intermetallic phases. PMID:28664887

  8. X-ray reflectivity measurement of interdiffusion in metallic multilayers during rapid heating.

    Science.gov (United States)

    Liu, J P; Kirchhoff, J; Zhou, L; Zhao, M; Grapes, M D; Dale, D S; Tate, M D; Philipp, H T; Gruner, S M; Weihs, T P; Hufnagel, T C

    2017-07-01

    A technique for measuring interdiffusion in multilayer materials during rapid heating using X-ray reflectivity is described. In this technique the sample is bent to achieve a range of incident angles simultaneously, and the scattered intensity is recorded on a fast high-dynamic-range mixed-mode pixel array detector. Heating of the multilayer is achieved by electrical resistive heating of the silicon substrate, monitored by an infrared pyrometer. As an example, reflectivity data from Al/Ni heated at rates up to 200 K s-1 are presented. At short times the interdiffusion coefficient can be determined from the rate of decay of the reflectivity peaks, and it is shown that the activation energy for interdiffusion is consistent with a grain boundary diffusion mechanism. At longer times the simple analysis no longer applies because the evolution of the reflectivity pattern is complicated by other processes, such as nucleation and growth of intermetallic phases.

  9. Three-Dimensional X-ray Reflections from Anthracite and Meta-Anthracite.

    Science.gov (United States)

    Ergun, S; Mentser, M; O'donnell, H J

    1960-11-04

    Careful analysis of x-ray scattering intensities of demineralized metaanthracites and high-rank anthracites formed during the Pennsylvanian geological period has revealed the presence of three-dimensional (hkl) reflections of graphite, demonstrating unequivocally that coals graphitize with metamorphism. Graphitization has been observed also with a coal formed before the Cambrian period, much earlier than most coals. A significant degree of graphitization occurs by coalification when the graphite-like layers attain a size of 25 to 30 angstroms as compared to 100 A or more by the heat treatment of amorphous carbons.

  10. SARS E protein in phospholipid bilayers: an anomalous X-ray reflectivity study

    Science.gov (United States)

    Khattari, Z.; Brotons, G.; Arbely, E.; Arkin, I. T.; Metzger, T. H.; Salditt, T.

    2005-02-01

    We report on an anomalous X-ray reflectivity study to locate a labelled residue of a membrane protein with respect to the lipid bilayer. From such experiments, important constraints on the protein or peptide conformation can be derived. Specifically, our aim is to localize an iodine-labelled phenylalanine in the SARS E protein, incorporated in DMPC phospholipid bilayers, which are deposited in the form of thick multilamellar stacks on silicon surfaces. Here, we discuss the experimental aspects and the difficulties associated with the Fourier synthesis analysis that gives the electron density profile of the membranes.

  11. X-ray reflectivity study on the structure and phase stability of mixed phospholipid multilayers.

    Science.gov (United States)

    Jing, H Y; Hong, D H; Kwak, B D; Choi, D J; Shin, K; Yu, C J; Kim, J W; Noh, D Y; Seo, Y S

    2009-04-07

    Vertically oriented multilayers composed of two saturated phospholipids, 1,2-dipalmitoyl-sn-glycero-3-phosphocholine (DPPC) and 1,2-dipalmitoyl-sn-glycero-3-phosphoserine (DPPS), were deposited on silicon. X-ray reflectivity was used to investigate the structures of the variously mixed phospholipid multilayers as a function of composition. Then, the phase stability was investigated at various annealing temperatures under humid conditions. The results indicated that the lipid spacing of the mixed phospholipid multilayers varied systematically as a function of the DPPC/DPPS ratio and that no macroscopic phase separation occurred during the annealing process under both dry and humid conditions.

  12. Non-null full field X-ray mirror metrology using SCOTS: a reflection deflectometry approach.

    Science.gov (United States)

    Su, Peng; Wang, Yuhao; Burge, James H; Kaznatcheev, Konstantine; Idir, Mourad

    2012-05-21

    In a previous paper, the University of Arizona (UA) has developed a measurement technique called: Software Configurable Optical Test System (SCOTS) based on the principle of reflection deflectometry. In this paper, we present results of this very efficient optical metrology method applied to the metrology of X-ray mirrors. We used this technique to measure surface slope errors with precision and accuracy better than 100 nrad (rms) and ~200 nrad (rms), respectively, with a lateral resolution of few mm or less. We present results of the calibration of the metrology systems, discuss their accuracy and address the precision in measuring a spherical mirror.

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

    NARCIS (Netherlands)

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

    2016-01-01

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

  14. In situ X-ray polymerization: from swollen lamellae to polymer-surfactant complexes.

    Science.gov (United States)

    Agzenai, Yahya; Lindman, Björn; Alfredsson, Viveka; Topgaard, Daniel; Renamayor, Carmen S; Pacios, Isabel E

    2014-01-30

    The influence of the monomer diallyldimethylammonium chloride (D) on the lamellar liquid crystal formed by the anionic surfactant aerosol OT (AOT) and water is investigated, determining the lamellar spacings by SAXS and the quadrupolar splittings by deuterium NMR, as a function of the D or AOT concentrations. The cationic monomer D induces a destabilization of the AOT lamellar structure such that, at a critical concentration higher than 5 wt %, macroscopic phase separation takes place. When the monomer, which is dissolved in the AOT lamellae, is polymerized in situ by X-ray initiation, a new collapsed lamellar phase appears, corresponding to the complexation of the surfactant with the resulting polymer. A theoretical model is employed to analyze the variation of the interactions between the AOT bilayers and the stability of the lamellar structure.

  15. Reduction of variable-truncation artifacts from beam occlusion during in situ x-ray tomography

    DEFF Research Database (Denmark)

    Borg, Leise; Jørgensen, Jakob Sauer; Frikel, Jürgen

    2017-01-01

    Many in situ x-ray tomography studies require experimental rigs which may partially occlude the beam and cause parts of the projection data to be missing. In a study of fluid flow in porous chalk using a percolation cell with four metal bars drastic streak artifacts arise in the filtered...... discontinuities that are shown to be the source of the streaks. The ‘reduction to limited angle’ (RLA) method simply keeps only non-truncated projections; the ‘detector-directed smoothing’ (DDS) method smooths the discontinuities; while the ‘reflexive boundary condition’ (RBC) method enforces a zero derivative...... at the discontinuities. Experimental results using both simulated and real data show that the proposed methods effectively reduce variable-truncation artifacts. The RBC method is found to provide the best artifact reduction and preservation of image features using both visual and quantitative assessment. The analysis...

  16. In Situ X ray scattering for investing morphology of bottle brush BCP with Solvent annealing

    Science.gov (United States)

    Jeong, Gajin; Russell, Thomas P.; Sveinbjornsson, Benjamin R.; Grubbs, Robert H.; Univ of Mass-Amherst Collaboration; California Institute of Technology Collaboration

    2014-03-01

    We investigated the morphology of bottle-brush block copolymer (BrBCPs) thin films using solvent vapor annealing (SVA) in a specially designed chamber for in situgrazing incidence x-ray scattering. BrBCPs with polystyrene (PS) and poly(lactic acid) (PLA) side chains and a norbornene backbone were studied SVA using THF, a good solvent for PS and PLA, a controlled swelling and deswelling rate were achieved with N2 carrier gas. Film thickness was monitored by optical interferometry. The interference maximum, characteristic of the microdomain morphology, was found to vary linearly with molecular weight. The in situGISAXS measuremens were used to elucidate the evolution of the morphology in the thin films.

  17. In-situ x-ray characterization of wurtzite formation in GaAs nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Krogstrup, Peter; Hannibal Madsen, Morten; Nygaard, Jesper; Feidenhans' l, Robert [Nano-Science Center, Niels Bohr Institute, University of Copenhagen, Copenhagen (Denmark); Hu Wen [Quantum Beam Science Directorate, Japan Atomic Energy Agency, 1-1-1 Koto, Sayo, Hyogo 679-5148 (Japan); Kozu, Miwa; Nakata, Yuka [University of Hyogo, 3-2-1 Koto, Kamigori, Hyogo 678-1297 (Japan); Takahasi, Masamitu [Quantum Beam Science Directorate, Japan Atomic Energy Agency, 1-1-1 Koto, Sayo, Hyogo 679-5148 (Japan); University of Hyogo, 3-2-1 Koto, Kamigori, Hyogo 678-1297 (Japan)

    2012-02-27

    In-situ monitoring of the crystal structure formation during Ga-assisted GaAs nanowire growth on Si(111) substrates has been performed in a combined molecular beam epitaxy growth and x-ray characterization experiment. Under Ga rich conditions, we show that an increase in the V/III ratio increases the formation rate of the wurtzite structure. Moreover, the response time for changes in the structural phase formation to changes in the beam fluxes is observed to be much longer than predicted time scales of adatom kinetics and liquid diffusion. This suggests that the morphology of the growth interface plays the key role for the relative growth structure formation rates.

  18. Tensile behavior of orthorhombic alpha ''-titanium alloy studied by in situ X-ray diffraction

    DEFF Research Database (Denmark)

    Wang, X.D.; Lou, H.B.; Ståhl, Kenny

    2010-01-01

    The tensile behavior of a Ti-11%Zr-14%Nb-10%Sn alloy with pure orthorhombic alpha '' phase was studied by in situ X-ray diffraction using synchrotron radiation. It is found that no phase transformation happens during the whole tensile process. The "double-yielding" platforms of this alloy...... are indeed due to a low stress yielding (similar to 400 MPa) followed with a significant work-hardening before necking and fracture. In this process, the [0 2 2] orientation of grains more approaches the tensile direction and the [2 0 0] moves to the transverse, causing the lattice parameter a to be shrunk......, and b and c elongated, and the formation of texture. The similar texture can also be produced upon cold rolling by which the yield strength of the alpha '' phase is largely improved to be over 900 MPa....

  19. Hydride reorientation in Zircaloy-4 examined by in situ synchrotron X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Weekes, H.E. [Department of Materials, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2BP (United Kingdom); Jones, N.G. [Department of Materials Science and Metallurgy, University of Cambridge, 27 Charles Babbage Road, Cambridge CB3 0FS (United Kingdom); Lindley, T.C. [Department of Materials, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2BP (United Kingdom); Dye, D., E-mail: david.dye@imperial.ac.uk [Department of Materials, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2BP (United Kingdom)

    2016-09-15

    The phenomenon of stress-reorientation has been investigated using in situ X-ray diffraction during the thermomechanical cycling of hydrided Zircaloy-4 tensile specimens. Results have shown that loading along a sample’s transverse direction (TD) leads to a greater degree of hydride reorientation when compared to rolling direction (RD)-aligned samples. The elastic lattice micro-strains associated with radially oriented hydrides have been revealed to be greater than those oriented circumferentially, a consequence of strain accommodation. Evidence of hydride redistribution after cycling, to α-Zr grains oriented in a more favourable orientation when under an applied stress, has also been observed and its behaviour has been found to be highly dependent on the loading axis. Finally, thermomechanical loading across multiple cycles has been shown to reduce the difference in terminal solid solubility of hydrogen during dissolution (TSS{sub D,H}) and precipitation (TSS{sub P,H}).

  20. Reduction of variable-truncation artifacts from beam occlusion during in situ x-ray tomography

    Science.gov (United States)

    Borg, Leise; Jørgensen, Jakob S.; Frikel, Jürgen; Sporring, Jon

    2017-12-01

    Many in situ x-ray tomography studies require experimental rigs which may partially occlude the beam and cause parts of the projection data to be missing. In a study of fluid flow in porous chalk using a percolation cell with four metal bars drastic streak artifacts arise in the filtered backprojection (FBP) reconstruction at certain orientations. Projections with non-trivial variable truncation caused by the metal bars are the source of these variable-truncation artifacts. To understand the artifacts a mathematical model of variable-truncation data as a function of metal bar radius and distance to sample is derived and verified numerically and with experimental data. The model accurately describes the arising variable-truncation artifacts across simulated variations of the experimental setup. Three variable-truncation artifact-reduction methods are proposed, all aimed at addressing sinogram discontinuities that are shown to be the source of the streaks. The ‘reduction to limited angle’ (RLA) method simply keeps only non-truncated projections; the ‘detector-directed smoothing’ (DDS) method smooths the discontinuities; while the ‘reflexive boundary condition’ (RBC) method enforces a zero derivative at the discontinuities. Experimental results using both simulated and real data show that the proposed methods effectively reduce variable-truncation artifacts. The RBC method is found to provide the best artifact reduction and preservation of image features using both visual and quantitative assessment. The analysis and artifact-reduction methods are designed in context of FBP reconstruction motivated by computational efficiency practical for large, real synchrotron data. While a specific variable-truncation case is considered, the proposed methods can be applied to general data cut-offs arising in different in situ x-ray tomography experiments.

  1. In situ X-ray diffraction measurement of shock-wave-driven twinning and lattice dynamics

    Science.gov (United States)

    Wehrenberg, C. E.; McGonegle, D.; Bolme, C.; Higginbotham, A.; Lazicki, A.; Lee, H. J.; Nagler, B.; Park, H.-S.; Remington, B. A.; Rudd, R. E.; Sliwa, M.; Suggit, M.; Swift, D.; Tavella, F.; Zepeda-Ruiz, L.; Wark, J. S.

    2017-10-01

    Pressure-driven shock waves in solid materials can cause extreme damage and deformation. Understanding this deformation and the associated defects that are created in the material is crucial in the study of a wide range of phenomena, including planetary formation and asteroid impact sites, the formation of interstellar dust clouds, ballistic penetrators, spacecraft shielding and ductility in high-performance ceramics. At the lattice level, the basic mechanisms of plastic deformation are twinning (whereby crystallites with a mirror-image lattice form) and slip (whereby lattice dislocations are generated and move), but determining which of these mechanisms is active during deformation is challenging. Experiments that characterized lattice defects have typically examined the microstructure of samples after deformation, and so are complicated by post-shock annealing and reverberations. In addition, measurements have been limited to relatively modest pressures (less than 100 gigapascals). In situ X-ray diffraction experiments can provide insights into the dynamic behaviour of materials, but have only recently been applied to plasticity during shock compression and have yet to provide detailed insight into competing deformation mechanisms. Here we present X-ray diffraction experiments with femtosecond resolution that capture in situ, lattice-level information on the microstructural processes that drive shock-wave-driven deformation. To demonstrate this method we shock-compress the body-centred-cubic material tantalum—an important material for high-energy-density physics owing to its high shock impedance and high X-ray opacity. Tantalum is also a material for which previous shock compression simulations and experiments have provided conflicting information about the dominant deformation mechanism. Our experiments reveal twinning and related lattice rotation occurring on the timescale of tens of picoseconds. In addition, despite the common association between twinning

  2. In situ X-ray diffraction measurement of shock-wave-driven twinning and lattice dynamics.

    Science.gov (United States)

    Wehrenberg, C E; McGonegle, D; Bolme, C; Higginbotham, A; Lazicki, A; Lee, H J; Nagler, B; Park, H-S; Remington, B A; Rudd, R E; Sliwa, M; Suggit, M; Swift, D; Tavella, F; Zepeda-Ruiz, L; Wark, J S

    2017-10-25

    Pressure-driven shock waves in solid materials can cause extreme damage and deformation. Understanding this deformation and the associated defects that are created in the material is crucial in the study of a wide range of phenomena, including planetary formation and asteroid impact sites, the formation of interstellar dust clouds, ballistic penetrators, spacecraft shielding and ductility in high-performance ceramics. At the lattice level, the basic mechanisms of plastic deformation are twinning (whereby crystallites with a mirror-image lattice form) and slip (whereby lattice dislocations are generated and move), but determining which of these mechanisms is active during deformation is challenging. Experiments that characterized lattice defects have typically examined the microstructure of samples after deformation, and so are complicated by post-shock annealing and reverberations. In addition, measurements have been limited to relatively modest pressures (less than 100 gigapascals). In situ X-ray diffraction experiments can provide insights into the dynamic behaviour of materials, but have only recently been applied to plasticity during shock compression and have yet to provide detailed insight into competing deformation mechanisms. Here we present X-ray diffraction experiments with femtosecond resolution that capture in situ, lattice-level information on the microstructural processes that drive shock-wave-driven deformation. To demonstrate this method we shock-compress the body-centred-cubic material tantalum-an important material for high-energy-density physics owing to its high shock impedance and high X-ray opacity. Tantalum is also a material for which previous shock compression simulations and experiments have provided conflicting information about the dominant deformation mechanism. Our experiments reveal twinning and related lattice rotation occurring on the timescale of tens of picoseconds. In addition, despite the common association between twinning and

  3. Total reflection X-ray fluorescence and archaeometry: Application in the Argentinean cultural heritage

    Energy Technology Data Exchange (ETDEWEB)

    Vazquez, Cristina [Comision Nacional de Energia Atomica, Av. Gral Paz 1499 (B1650KNA) San Martin, Buenos Aires (Argentina); Laboratorio de Quimica de Sistemas Heterogeneos, Facultad de Ingenieria, Universidad de Buenos Aires, P. Colon 850 (C1063ACU), Buenos Aires (Argentina)], E-mail: Cristina.Vazquez@cnea.gov.ar; Albornoz, Ana [Agencia Rio Negro Cultura, Museo de la Patagonia F.P.Moreno, Centro Civico s/n Bariloche, Rio Negro (Argentina); Hajduk, Adam [CONICET, Museo de la Patagonia F.P.Moreno, Centro Civico s/n Bariloche, Rio Negro (Argentina); Elkin, Dolores [CONICET Instituto Nacional de Antropologia y Pensamiento Latinoamericano, 3 de febrero 1378 (C1426AEL) Buenos Aires (Argentina); Custo, Graciela; Obrustky, Alba [Comision Nacional de Energia Atomica, Av. Gral Paz 1499 (B1650KNA) San Martin, Buenos Aires (Argentina)

    2008-12-15

    Archaeometry is an interdisciplinary research area involved in the development and use of scientific methods in order to answer questions concerned with the human history. In this way the knowledge of archaeological objects through advanced chemical and physical analyses permits a better preservation and conservation of the cultural heritage and also reveals materials and technologies used in the past. In this sense, analytical techniques play an important role in order to provide chemical information about cultural objects. Considering the non destructive characteristic of this study, analytical techniques must be adequate in order to prevent any alteration or damage and in addition to allow the conservation of their integrity. Taking into account the irreplaceable character of the archaeological and artistic materials considered in this study, analytical techniques must be adequate in order to prevent any alteration or damage and in addition to allow the conservation of their integrity. Total Reflection X-ray Fluorescence Spectrometry as a geometric variant of conventional X-ray fluorescence is a proved microanalytical technique considering the small amount of sample required for the analysis. A few micrograms are enough in order to reveal valuable information about elemental composition and in this context it is highly recommended for artwork studies. In this paper a case study is presented in which Total Reflection X-Ray Fluorescence Spectrometry has been successfully employed in the archaeometry field. Examples from Argentinean cultural heritage sites related with the determination of pigments in paintings on canvas and in rock sites as well as in underwater archaeology research are shown.

  4. In-Situ Synchrotron X-ray Study of the Phase and Texture Evolution of Ceria and Superconductor Films Deposited by Chemical Solution Method

    DEFF Research Database (Denmark)

    Yue, Zhao; Grivel, Jean-Claude; He, Dong

    2012-01-01

    In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry/differential ther......In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry...

  5. X-ray reflectivity reveals ionic structure at liquid crystal-aqueous interfaces.

    Science.gov (United States)

    Hallett, James E; Hayward, Dominic W; Arnold, Thomas; Bartlett, Paul; Richardson, Robert M

    2017-08-23

    Here X-ray reflectivity has been used to determine the structure of liquid crystal monolayers for different cyanobiphenyl homologues supported on aqueous solutions of two different salt species. Sodium iodide induces homeotropic ordering for all of the monolayer forming liquid crystal homologues studied here, and forms a Stern layer of iodide ions at the liquid crystal cyano headgroup, similar to the case of lipids or surfactants supported on electrolyte solutions. The liquid crystal headgroups were also found to penetrate into the water surface when binding with iodide ions. Sodium bromide, however, does not form the same localisation of ions close to a liquid crystal monolayer, and instead appears to produce no noticeable change in the scattering length density of the liquid crystal monolayer compared to pure water. However, on further compression the X-ray reflectivity dramatically changes, revealing the emergence of the so-called "trilayer" structure for 5CB and 8CB. This transition occurs at a lower areal density for sodium bromide than for pure water, and unlike for the uncompressed film, a layer of bromide ions was found at the trilayer-water interface.

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

    Science.gov (United States)

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

    2017-08-01

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

  7. In situ hydration of sulphoaluminate cement mixtures monitored by synchrotron x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Turrillas, X. [Institut de Ciencia de Materials de Barcelona (ICMAB-CSIC), Barcelona (Spain); Martinez, L.G.; Carvalho, A.M.; Carezzato, G.L. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Rossetto, C.M. [Faculdade de Tecnologia de Sao Paulo (FATEC), SP (Brazil)

    2016-07-01

    Full text: The hydration of calcium sulpho-aluminate cement mixtures was studied in situ by synchrotron X-ray diffraction at the XRD1 beamline of the Laboratorio Nacional de Luz Sincrotron (LNLS) in Campinas, SP. The powder specimens were introduced in borosilicate glass capillary tubes of 0.7 mm of internal diameter and imbued with deionized water. As the hydration reaction is very fast the capillaries were placed on the goniometer and the data collection was started after two minutes of mixing with water. The X-ray energy chosen to get an adequate flux for these short time acquisitions was 12 keV or more precisely 1.033258 Å, determined with polycrystalline corundum standard. Diffraction patterns were collected sequentially every 35 seconds for several hours at temperatures ranging from 40 degC to 55 degC with an accuracy better than 0.1 degC attained with the help of a hot air blower. The diffracted signal was collected with an array of twenty-four Mythen detectors at 760 mm from the capillary tube. The diffraction patterns had appropriate statistics to determine the kinetics of the reaction either by quantitative Rietveld analysis or by fitting isolated diffraction peaks to Gaussian curves as a function of time. The most important phases involved in the hydration are Klein´s salt, also known as Ye’elimite, Ca4(AlO2)6SO4, and gypsum, CaSO4.2H2O to yield Ettringite, Ca6Al2(SO4)3(OH)12 - 26H2O, phase responsible for the mechanical properties. (author)

  8. Multiple-wave diffraction in high energy resolution back-reflecting x-ray optics.

    Science.gov (United States)

    Stetsko, Yuri P; Keister, J W; Coburn, D S; Kodituwakku, C N; Cunsolo, A; Cai, Y Q

    2011-10-07

    We have studied the effects of multiple-wave diffraction in a novel optical scheme recently published by Shvyd'ko et al. utilizing Bragg diffraction of x rays in backscattering geometry from asymmetrically cut crystals for achieving energy resolutions beyond the intrinsic width of the Bragg reflection. By numerical simulations based on dynamic x-ray diffraction and by experimentation involving two-dimensional angular scans of the back-reflecting crystal, multiple-wave diffraction was found to contribute up to several tens percent loss of efficiency but can be avoided without degrading the energy resolution of the original scheme by careful choice of azimuthal orientation of the diffracting crystal surface and by tilting of the crystal perpendicular to the dispersion plane.

  9. Modelless approach in X-ray reflectivity of multilayer nanoheterostructure Fe/Cr

    Science.gov (United States)

    Babanov, Yu A.; Devyaterikov, D. I.; Ustinov, V. V.

    2017-10-01

    A new modelless method of determining the element concentration profile of metallic multilayer nanoheterostructures for low-contrast systems is applied to study periodical and aperiodical multilayer Fe/Cr system by X-ray reflectivity. As a special case, we discuss a cluster-layered Fe/Cr film with Kondo-like behavior of the resistance. The method does not require any a priori information on the structure of the multilayer nanostructures, such as position and width of interfaces, as well as, their shape. The method is based on solution of the Fredholm integral equation of the first kind, which relates the reflection coefficient and the concentration profile of the chemical elements of the sample. The ill-posed inverse problem of determination of the element concentration profile is solved by the regularization method. Efficiency of the method is confirmed by model calculations.

  10. Recent Developments in the X-Ray Reflectivity Analysis for Rough Surfaces and Interfaces of Multilayered Thin Film Materials

    Directory of Open Access Journals (Sweden)

    Yoshikazu Fujii

    2013-01-01

    Full Text Available X-ray reflectometry is a powerful tool for investigations on rough surface and interface structures of multilayered thin film materials. The X-ray reflectivity has been calculated based on the Parratt formalism, accounting for the effect of roughness by the theory of Nevot-Croce conventionally. However, in previous studies, the calculations of the X-ray reflectivity often show a strange effect where interference effects would increase at a rough surface. And estimated surface and interface roughnesses from the X-ray reflectivity measurements did not correspond to the TEM image observation results. The strange result had its origin in a used equation due to a serious mistake in which the Fresnel transmission coefficient in the reflectivity equation is increased at a rough interface because of a lack of consideration of diffuse scattering. In this review, a new accurate formalism that corrects this mistake is presented. The new accurate formalism derives an accurate analysis of the X-ray reflectivity from a multilayer surface of thin film materials, taking into account the effect of roughness-induced diffuse scattering. The calculated reflectivity by this accurate reflectivity equation should enable the structure of buried interfaces to be analyzed more accurately.

  11. NuSTAR Spectroscopy of Multi-Component X-Ray Reflection from NGC 1068

    DEFF Research Database (Denmark)

    Bauer, Franz E.; Arevalo, Patricia; Walton, Dominic J.

    2015-01-01

    We report on high-energy X-ray observations of the Compton-thick Seyfert 2 galaxy NGC 1068 with NuSTAR, which provide the best constraints to date on its >10 keV spectral shape. The NuSTAR data are consistent with those from past and current instruments to within cross-calibration uncertainties......, and we find no strong continuum or line variability over the past two decades, which is in line with its X-ray classification as a reflection-dominated Compton-thick active galactic nucleus. The combined NuSTAR, Chandra, XMM-Newton, and Swift BAT spectral data set offers new insights into the complex......, inconsistent viewing angles, or poor fits to the spatially resolved spectra). A multi-component reflector with three distinct column densities (e.g., with best-fit values of N-H of 1.4 x 10(23), 5.0 x 10(24), and 10(25) cm(-2)) provides a more reasonable fit to the spectral lines and Compton hump, with near...

  12. Soft X-ray reflectivity: from quasi-perfect mirrors to accelerator walls

    CERN Document Server

    Schäfers, F.

    2013-04-22

    Reflection of light from surfaces is a very common, but complex phenomenon not only in science and technology, but in every day life. The underlying basic optical principles have been developed within the last five centuries using visible light available from the sun or other laboratory light sources. X-rays were detected in 1895, and the full potential of soft- and hard-x ray radiation as a probe for the electronic and geometric properties of matter, for material analysis and its characterisation is available only since the advent of synchrotron radiation sources some 50 years ago. On the other hand high-brilliance and high power synchrotron radiation of present-days 3rd and 4th generation light sources is not always beneficial. Highenergy machines and accelerator-based light sources can suffer from a serious performance drop or limitations due to interaction of the synchrotron radiation with the accelerator walls, thus producing clouds of photoelectrons (e-cloud) which in turn interact with the accelerated ...

  13. X-ray reflectivity analysis of titanium dioxide thin films grown by cathodic arc deposition.

    Science.gov (United States)

    Kleiman, A; Lamas, D G; Craievich, A F; Márquez, A

    2014-05-01

    TiO2 thin films deposited by a vacuum arc on a glass substrate were characterized by X-ray reflectivity (XRR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and atomic force microscopy (AFM). Several thin films with different amounts of deposited TiO2 mass and different deposition and annealing temperatures were studied. A qualitative analysis of the XRD patterns indicated the presence of the anatase and/or rutile crystalline phases in most of the studied samples. From the analysis of the experimental XRR curves--which exhibited a wide angular range of oscillatory behavior--the thickness, mass density and interface roughness were determined. All XRR patterns were well fitted by modeled curves that assume the presence of a single and homogeneous TiO2 layer over which a very thin H2O layer is adsorbed. The thickest H2O adsorption layers were developed in films with the highest anatase content. Our overall results of the XRR analyses are consistent with those derived from the imaging techniques (SEM and AFM).

  14. In situ coherent x-ray scattering and STM studies of hexagonally reconstructed Au(001) in Electrolytes

    Science.gov (United States)

    Pierce, Michael S.; Komanicky, Vladimir; Barbour, Andi; Hennessy, Daniel; Su, Jun-Dar; Sandy, Alec; You, Hoydoo

    2011-03-01

    We have studied the dynamics of Au(001) and Au(111) surfaces in situ in 0.1 M HClO4 electrolyte solution using coherent x-ray scattering experiments and STM microscopy. Our coherent x-ray scattering experiments measure a correlation time for the surface as a function of applied potentials. Coherent x-ray scattering differs from the ordinary x-ray diffraction in sensitivity to the structural and temporal details. The correlation times were obtained from measurements conducted while the surface is in equilibrium and the ordinary surface scattering intensity is constant. The correlation time changes from high 103 seconds to low 102 seconds. The correlation times of reconstructed surfaces at low potential are at least an order of magnitude smaller than those measured at the reconstructed surfaces in vacuum. The correlation times also change dramatically in response to the applied potential. These experiments also represent the first successful application of coherent x-ray scattering to the study of electrochemical interfaces in situ. Work at ANL is supported by DOE-BES and work at SU by VEGA.

  15. A compact high vacuum heating chamber for in-situ x-ray scattering studies

    Energy Technology Data Exchange (ETDEWEB)

    Bertram, F.; Deiter, C.; Pflaum, K.; Seeck, O. H. [Hamburger Synchrotronstrahlungslabor am Deutschen Elektronen-Synchrotron, Notkestr. 85, 22607 Hamburg (Germany)

    2012-08-15

    A very compact multi purpose high vacuum heating chamber for x-ray scattering techniques was developed. The compact design allows the chamber to be installed on high precision diffractometers which usually cannot support heavy and/or large equipment. The chamber is covered by a Be dome allowing full access to the hemisphere above the sample which is required for in-plane grazing incident x-ray diffraction and out-off plane wide angle x-ray diffraction.

  16. In situ x-ray absorption of Co/Mn/TiO2 catalysts for Fischer-Tropsch synthesis

    NARCIS (Netherlands)

    Morales, F; de Groot, FMF|info:eu-repo/dai/nl/08747610X; Glatzel, P; Kleimenov, E; Bluhm, H; Havecker, M; Knop-Gericke, A; Weckhuysen, BM|info:eu-repo/dai/nl/285484397

    2004-01-01

    The reduction behavior of Co/TiO2 and Co/Mn/TiO2 catalysts for Fischer-Tropsch synthesis has been investigated by soft X-ray absorption spectroscopy (XAS). In situ XAS measurements of the L-2,L-3 edges of Co and Mn have been carried out during reduction treatments of the samples in H-2 at a pressure

  17. In-situ real-time x-ray scattering for probing the processing-structure-performance relation

    KAUST Repository

    Smilgies, Detlef-M.

    2014-01-01

    © 2014 Materials Research Society. In-situ X-ray scattering methodology is discussed, in order to analyze the microstructure development of soft functional materials during coating, annealing, and drying processes in real-time. The relevance of a fundamental understanding of coating processes for future industrial production is pointed out.

  18. Total reflection X-ray fluorescence and energy-dispersive X-ray fluorescence analysis of runoff water and vegetation from abandoned mining of Pb-Zn ores

    Energy Technology Data Exchange (ETDEWEB)

    Marques, A.F.; Queralt, I.; Carvalho, M.L. E-mail: luisa@cii.fc.ul.pt; Bordalo, M

    2003-12-15

    The present work reports on the heavy metal content: Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Cd and Pb in running waters and vegetation around abandoned mining areas. Two species of mosses (Dicranum sp. and Pleurocarpus sp.) and three different species of wild grass (Bromus sp., Rumex sp. and Pseudoavena sp.) growing on the surrounding areas of old lead-zinc mines (Aran Valley, Pyrenees, NE Spain) have been analyzed. Both water and vegetation were collected in two different sampling places: (a) near the mine gallery water outlets and (b) on the landfill close to the abandoned mineral concentration factories. For the heavy metal content determination, two different techniques were used: total reflection X-ray fluorescence for water analysis and energy-dispersive X-ray fluorescence for vegetation study. Surface waters around mine outlets exhibit anomalous content of Co, Ni, Zn, Cd. Stream waters running on mining landfills exhibit higher Cu, Zn, Cd and Pb than those of the waters at the mine gallery outlets. The results allow us to assess the extent of the environmental impact of the mining activities on the water quality. The intake of these elements by vegetation was related with the sampling place, reflecting the metal water content and the substrate chemistry. Accumulation of metals in mosses is higher than those exhibited in wild grasses. Furthermore, different levels of accumulation were found in different wild grass. Rumex sp. presented the lowest metal concentrations, while Pseudoavena sp. reported the highest metal content.

  19. Reflectivity Around the Gold L-Edges of X-Ray Reflector of the Soft X-Ray Telescope Onboard ASTRO-H

    Science.gov (United States)

    Maeda, Yoshitomo; Kikuchi, Naomichi; Kurashima, Sho; Ishida, Manabu; Iizuka, Ryo; Hayashi, Takayuki; Okajima, Takashi; Matsumoto, Hironori; Mitsuishi, Ikuyuki; Saji, Shigetaka; hide

    2016-01-01

    We report the atomic scattering factor in the 11.215.4 keV for the ASTRO-H Soft X-ray Telescope (SXT) obtained in the ground based measurements. The large effective area of the SXT covers above 10 keV. In fact, the flight data show the spectra of the celestical objects in the hard X-ray band. In order to model the area, the reflectivity measurements in the 11.2-15.4 keV band with the energy pitch of 0.4-0.7 eV were made in the synchrotron beamline Spring-8 BL01B1. We obtained atomic scattering factors f1 and f2 by the curve fitting to the reflectivities of our witness sample. The edges associated with the golds L-I, II, and III transitions are identified, of which the depths are found to be roughly 60 percent shallower than those expected from the Henke's atomic scattering factor.

  20. In-situ X-ray Nanocharacterization of Defect Kinetics in Chalcogenide Solar Cell Materials

    Energy Technology Data Exchange (ETDEWEB)

    Bertoni, Mariana [Arizona State Univ., Tempe, AZ (United States); Lai, Barry [Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS); Masser, Jorg [Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS); Buonassisi, Tonio [Massachusetts Inst. of Technology (MIT), Cambridge, MA (United States)

    2016-09-21

    ) correlate positively, and In negatively with charge collection efficiency for cells with low Ga content, both at grain boundaries and in grain cores. For cells with high Ga content, the charge collection efficiency depends to much lesser extent on the elemental distribution. The objective is three folded: (1) develop an x-ray in-situ microscopy capability to simulate growth and processing conditions, (2) apply it to elucidate performance-governing defect kinetics in chalcogenide solar cell materials, and (3) to study approaches to engineer materials from the nanoscale up. The development of these capabilities will enable experimental characterization to take place under actual processing and operating conditions and it will have impact well beyond the proposed research, enabling future studies on a large variety of materials system where electronic properties depend on underlying structural or chemical inhomogeneities.

  1. First Total Reflection X-Ray Fluorescence round-robin test of water samples: Preliminary results

    Energy Technology Data Exchange (ETDEWEB)

    Borgese, Laura; Bilo, Fabjola [Chemistry for Technologies Laboratory, University of Brescia, Brescia (Italy); Tsuji, Kouichi [Graduate School of Engineering, Osaka City University, Osaka (Japan); Fernández-Ruiz, Ramón [Servicio Interdepartamental de Investigación (SIdI), Laboratorio de TXRF, Universidad Autónoma de Madrid, Madrid (Spain); Margui, Eva [Department of Chemistry, University of Girona, Girona (Spain); Streli, Christina [TU Wien, Atominstitut,Radiation Physics, Vienna (Austria); Pepponi, Giancarlo [Fondazione Bruno Kessler, Povo, Trento (Italy); Stosnach, Hagen [Bruker Nano GmbH, Berlin (Germany); Yamada, Takashi [Rigaku Corporation, Takatsuki, Osaka (Japan); Vandenabeele, Peter [Department of Archaeology, Ghent University, Ghent (Belgium); Maina, David M.; Gatari, Michael [Institute of Nuclear Science and Technology, University of Nairobi, Nairobi (Kenya); Shepherd, Keith D.; Towett, Erick K. [World Agroforestry Centre (ICRAF), Nairobi (Kenya); Bennun, Leonardo [Laboratorio de Física Aplicada, Departamento de Física, Universidad de Concepción (Chile); Custo, Graciela; Vasquez, Cristina [Gerencia Química, Laboratorio B025, Centro Atómico Constituyentes, San Martín (Argentina); Depero, Laura E., E-mail: laura.depero@unibs.it [Chemistry for Technologies Laboratory, University of Brescia, Brescia (Italy)

    2014-11-01

    Total Reflection X-Ray Fluorescence (TXRF) is a mature technique to evaluate quantitatively the elemental composition of liquid samples deposited on clean and well polished reflectors. In this paper the results of the first worldwide TXRF round-robin test of water samples, involving 18 laboratories in 10 countries are presented and discussed. The test was performed within the framework of the VAMAS project, interlaboratory comparison of TXRF spectroscopy for environmental analysis, whose aim is to develop guidelines and a standard methodology for biological and environmental analysis by means of the TXRF analytical technique. - Highlights: • The discussion of the first worldwide TXRF round-robin test of water samples (18 laboratories of 10 countries) is reported. • Drinking, waste, and desalinated water samples were tested. • Data dispersion sources were identified: sample concentration, preparation, fitting procedure, and quantification. • The protocol for TXRF analysis of drinking water is proposed.

  2. Metals determination in coffee sample by total reflection X-ray fluorescence analysis (TXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Vives, Ana Elisa Sirito de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo]. E-mail: Silvana@fec.unicamp.br; Brienza, Sandra Maria Boscolo [ Universidade Metodista de Piracicaba (UNIMEP), Piracicaba, SP (Brazil). Faculdade de Ciencias Matematicas, da Natureza e de Tecnologia da Informacao]. E-mail: sbrienza@unimep.br; Zucchi, Orgheda Luiza Araujo Domingues [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas]. E-mail: olzucchi@fcfrp.usp.br; Nascimento Filho, Virgilio Franco do [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil)]. E-mail: virgilio@cena.usp.br

    2005-07-01

    The objective of this study was to evaluate the inorganic concentration in five brands of coffee, three of them nationally marketed and the others of an exportation kind. The samples were prepared by infusion with deionized water. To carry out the calibration, standard solutions were prepared with different concentrations of Al, Si, K, Ca, Ti, Cr, Fe, Ni, Zn and Se. The measurements were carried out using a white beam of synchrotron radiation for excitation and a Si (Li) semiconductor detector for detection. By employing Synchrotron Radiation Total Reflection X-Ray Fluorescence Analysis (SR-TXRF) it was possible to evaluate the concentrations of P, S, Cl, K, Ca, Mn, Fe, Cu, Zn, Rb and Ba. The detection limits for 300 s counting time were in the range of 0.03 (Ca) to 30 ng.g{sup -1} (Rb), respectively. (author)

  3. Probing the protic ionic liquid surface using X-ray reflectivity.

    Science.gov (United States)

    Wakeham, Deborah; Nelson, Andrew; Warr, Gregory G; Atkin, Rob

    2011-12-14

    The structure of the free liquid surface of three protic ionic liquids, ethylammonium nitrate (EAN), propylammonium nitrate (PAN), and ethylammonium formate (EAF), has been elucidated using X-ray reflectivity. The results show all three liquids have an extended interfacial region, spanning at least five ion pairs, which can be divided into two parts. Adjacent to the gas phase are aggregates consisting of multiple cations and anions. Below this are layers oriented parallel to the macroscopic surface that are alternately enriched and depleted in cation alkyl chains and polar domains of cation ammonium groups and their anions, gradually decaying to the isotropic sponge-like bulk structure. The most pronounced layering is observed for PAN, driven by strong solvophobic interactions, while reduced hydrogen bonding in EAF results in the least structured and least extensive interfacial region.

  4. Multielement-analysis of city waste incineration ash with total reflection X-ray fluorescence (TXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Gerwinski, W.; Goetz, D.; Koelling, S.; Kunze, J.

    1987-06-01

    The toal reflection X-ray fluorescence technique (TXRF) was used for the routine analysis of city waste incineration ash. Subjects of these analyses were digested ashes (a) and aqueous leaching solutions (b). The accuracy of TXRF was estimated in comparison with atomic absorption spectroscopy (AAS) and atomic emission spectroscopy (ICP-AES) measurements. Satisfactory agreement was found between the results of the different methods for both types of samples. In addition to the direct measurements without prior sample preparation sample type (b) was used to compare three different extraction methods. In each case a dithiocarbamate derivative was used as complexing agent. The separation of the precipitate was performed with a silicagel column, by liquid/liquid extraction and by leaching the sample on a quartz target. Satisfying agreement was found between direct measurements and the different extraction methods.

  5. A triple axis double crystal multiple reflection camera for ultra small angle X-ray scattering

    Science.gov (United States)

    Lambard, Jacques; Lesieur, Pierre; Zemb, Thomas

    1992-06-01

    To extend the domain of small angle X-ray scattering requires multiple reflection crystals to collimate the beam. A double crystal, triple axis X-ray camera using multiple reflection channel cut crystals is described. Procedures for measuring the desmeared scattering cross-section on absolute scale are described as well as the measurement from several typical samples : fibrils of collagen, 0.3 μm diameter silica spheres, 0.16 μm diameter interacting latex spheres, porous lignite coal, liquid crystals in a surfactant-water system, colloidal crystal of 0.32 μm diameter silica spheres. L'extension du domaine de diffusion des rayons-X vers les petits angles demande l'emploi de cristaux à réflexions multiples pour collimater le faisceau. Nous décrivons une caméra à rayons-X à trois axes où les réflexions multiples sont réalisées dans deux cristaux à gorge. Nous donnons ensuite les procédures de déconvolution pour obtenir la section efficace de diffusion en échelle absolue, ainsi que les résultats des mesures effectuées avec plusieurs échantillons typiques : fibres de collagène, sphères de silice de 0,3 μm de diamètre, sphères de latex de 0,16 μm de diamètre en interaction, charbon lignite poreux, cristaux liquides formés dans un système eau-tensioactif, solution colloïdale de sphères de silice de 0,32 μm de diamètre.

  6. A rotational and axial motion system load frame insert for in situ high energy x-ray studies

    Energy Technology Data Exchange (ETDEWEB)

    Shade, Paul A., E-mail: paul.shade.1@us.af.mil; Schuren, Jay C.; Turner, Todd J. [Materials and Manufacturing Directorate, Air Force Research Laboratory, Wright-Patterson AFB, Ohio 45433 (United States); Blank, Basil [PulseRay, Beaver Dams, New York 14812 (United States); Kenesei, Peter; Goetze, Kurt; Lienert, Ulrich; Almer, Jonathan [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Suter, Robert M. [Carnegie Mellon University, Pittsburgh, Pennsylvania 15213 (United States); Bernier, Joel V.; Li, Shiu Fai [Engineering Directorate, Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Lind, Jonathan [Carnegie Mellon University, Pittsburgh, Pennsylvania 15213 (United States); Engineering Directorate, Lawrence Livermore National Laboratory, Livermore, California 94550 (United States)

    2015-09-15

    High energy x-ray characterization methods hold great potential for gaining insight into the behavior of materials and providing comparison datasets for the validation and development of mesoscale modeling tools. A suite of techniques have been developed by the x-ray community for characterizing the 3D structure and micromechanical state of polycrystalline materials; however, combining these techniques with in situ mechanical testing under well characterized and controlled boundary conditions has been challenging due to experimental design requirements, which demand new high-precision hardware as well as access to high-energy x-ray beamlines. We describe the design and performance of a load frame insert with a rotational and axial motion system that has been developed to meet these requirements. An example dataset from a deforming titanium alloy demonstrates the new capability.

  7. Electrochemistry and in-situ x-ray diffraction of InSb in lithium batteries.

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, C. S.; Vaughey, J. T.; Thackeray, M. M.; Sarakonsri, T.; Hackney, S. A.; Fransson, L.; Edstrom, K.; Thomas, J. O.; Chemical Engineering

    2000-08-01

    The electrochemical reactions of lithium with the intermetallic compound, InSb, were studied in lithium coin cells using laminate electrodes fabricated from either single-crystal InSb wafers or ball-milled samples. In-situ X-ray diffraction data show that the InSb zinc-blende framework is unstable to extensive reaction with lithium; In is extruded from a fixed Sb lattice during 'discharge' and is partially incorporated back into the lattice during 'charge'. Despite the loss of some In from the structure, the indium antimonide electrode provides capacities in excess of 300 mAh/g with excellent reversibility. Cyclic voltammetry was used to study the electrochemical processes in greater detail. Lithiated indium products are formed below {approx}600 mV versus Li. The electrode can be discharged at high rates, delivering 150 mAh/g at 3.6 mA/cm{sub 2} between 1.2 and 0.2 V versus Li. These data hold exciting prospects for the development of intermetallic insertion electrodes for practical room-temperature Li-ion cells.

  8. Versatile in situ powder X-ray diffraction cells for solid-gas investigations

    Energy Technology Data Exchange (ETDEWEB)

    Jensen, Torben R.; Nielsen, Thomas K.; Joergensen, Jens-Erik [Aarhus Univ. (Denmark). Center for Energy Materials, Center for Materials Crystallography; Filinchuk, Yaroslav [European Synchrotron Radiation Facility, Grenoble (France). Swiss-Norwegian Beam Lines; Cerenius, Yngve [Lund Univ. (Sweden). MAX-lab; Gray, Evan MacA.; Webb, Colin J. [Griffith Univ., Nathan, Brisbane (Australia). Queensland Micro- and Nanotechnology Centre

    2010-12-15

    This paper describes new sample cells and techniques for in situ powder X-ray diffraction specifically designed for gas absorption studies up to ca 300 bar (1 bar = 100 000 Pa) gas pressure. The cells are for multipurpose use, in particular the study of solid-gas reactions in dosing or flow mode, but can also handle samples involved in solid-liquid-gas studies. The sample can be loaded into a single-crystal sapphire (Al{sub 2}O{sub 3}) capillary, or a quartz (SiO{sub 2}) capillary closed at one end. The advantages of a sapphire single-crystal cell with regard to rapid pressure cycling are discussed, and burst pressures are calculated and measured to be {proportional_to}300 bar. An alternative and simpler cell based on a thin-walled silicate or quartz glass capillary, connected to a gas source via a VCR fitting, enables studies up to {proportional_to}100 bar. Advantages of the two cell types are compared and their applications are illustrated by case studies. (orig.)

  9. Kinetics of methane hydrate decomposition studied via in situ low temperature X-ray powder diffraction.

    Science.gov (United States)

    Everett, S Michelle; Rawn, Claudia J; Keffer, David J; Mull, Derek L; Payzant, E Andrew; Phelps, Tommy J

    2013-05-02

    Gas hydrate is known to have a slowed decomposition rate at ambient pressure and temperatures below the melting point of ice. As hydrate exothermically decomposes, gas is released and water of the clathrate cages transforms into ice. Based on results from the decomposition of three nominally similar methane hydrate samples, the kinetics of two regions, 180-200 and 230-260 K, within the overall decomposition range 140-260 K, were studied by in situ low temperature X-ray powder diffraction. The kinetic rate constants, k(a), and the reaction mechanisms, n, for ice formation from methane hydrate were determined by the Avrami model within each region, and activation energies, E(a), were determined by the Arrhenius plot. E(a) determined from the data for 180-200 K was 42 kJ/mol and for 230-260 K was 22 kJ/mol. The higher E(a) in the colder temperature range was attributed to a difference in the microstructure of ice between the two regions.

  10. In situ alkali-silica reaction observed by x-ray microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Kurtis, K.E.; Monteiro, P.J.M. [Univ. of California, Berkeley, CA (United States); Brown, J.T.; Meyer-Ilse, W. [Ernest Orlando Lawrence Berkeley National Lab., CA (United States)

    1997-04-01

    In concrete, alkali metal ions and hydroxyl ions contributed by the cement and reactive silicates present in aggregate can participate in a destructive alkali-silica reaction (ASR). This reaction of the alkalis with the silicates produces a gel that tends to imbibe water found in the concrete pores, leading to swelling of the gel and eventual cracking of the affected concrete member. Over 104 cases of alkali-aggregate reaction in dams and spillways have been reported around the world. At present, no method exists to arrest the expansive chemical reaction which generates significant distress in the affected structures. Most existing techniques available for the examination of concrete microstructure, including ASR products, demand that samples be dried and exposed to high pressure during the observation period. These sample preparation requirements present a major disadvantage for the study of alkali-silica reaction. Given the nature of the reaction and the affect of water on its products, it is likely that the removal of water will affect the morphology, creating artifacts in the sample. The purpose of this research is to observe and characterize the alkali-silica reaction, including each of the specific reactions identified previously, in situ without introducing sample artifacts. For observation of unconditioned samples, x-ray microscopy offers an opportunity for such an examination of the alkali-silica reaction. Currently, this investigation is focusing on the effect of calcium ions on the alkali-silica reaction.

  11. In situ X-ray Scattering and Dynamical Modeling of Pd Catalyst Nanoparticles Formed in Flames

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Juan; Seifert, Sönke; Winans, Randall E.; Tolmachoff, Erik; Xin, Yuxuan; Chen, Dongping; Wang, Hai; Anderson, Scott L.

    2015-08-20

    It has previously been demonstrated that organopalladium precursors can break down under combustion conditions, forming nanoparticles that catalyze ignition. Here, we use in situ small-angle X-ray scattering (SAXS) to probe the formation and growth of palladium nanoparticles in an ethylene fl ame doped with 28 ppm (mol) of Pd(acetate) 2 . The particles appear to nucleate in the fl ame front and are observed by SAXS to grow in size and mass in the high-temperature region of the fl ame ( ~ 2200 K) with median diameters that evolve from 1.5 to 3.0 nm. Transmission electron microscopy of particles collected on a grid located outside the fl ame shows that the particles are metallic palladium with sizes comparable to those determined by SAXS. Molecular dynamics simulation of particles of selected sizes indicates that at the fl ame temperature the particles are molten and the average mass density of the particle material is notably smaller than that of bulk, liquid Pd at the melting point. Both experimental and computational results point to homogeneous nucleation and particle - particle coalescence as mechanisms for particle formation and growth. Aerosol dynamics simulation reproduces the time evolution of the particle size distribution and suggests that a substantial fraction of the particles must be electrically charged during their growth process.

  12. Hybrid X-ray and {gamma}-ray spectrometer for in-situ planetary science missions

    Energy Technology Data Exchange (ETDEWEB)

    Skidmore, M.S. [Space Research Centre, Department of Physics and Astronomy, University of Leicester, University Road, Leicester LE1 7RH (United Kingdom)], E-mail: mss16@star.le.ac.uk; Ambrosi, R.M. [Space Research Centre, Department of Physics and Astronomy, University of Leicester, University Road, Leicester LE1 7RH (United Kingdom); Simon, H. [Eurorad, 2, rue Ettore Bugatti, 67201 Eckbolsheim (France)

    2009-06-11

    {gamma}-Ray spectroscopy, X-ray spectroscopy and {gamma}-ray backscatter densitometry for planetary science applications are three complementary analytical techniques that can be used to determine surface and sub-surface composition, constrain heat flow through a planetary regolith and hence understand more about the processes that formed planetary bodies. Evaluating different detector types and configurations in order to achieve these scientific objectives is a key enabling step for a successful flight instrument development programme. In this study, we evaluate and compare different detector solutions and configurations including: planar and hemispherical CdTe, a CsI(Tl) scintillator, a LaBr{sub 3}(Ce) scintillator and a HPGe detector. The LaBr{sub 3}(Ce) detector was chosen as the most suitable detector for an in-situ planetary science mission due to its high-radiation tolerance, low mass compared with HPGe detector systems, its comparable resolution ({approx}3.4% at 662 keV) to compound semiconductors (planar CdTe {approx}2.4% at 662 keV) and high efficiency.

  13. Scanning of Adsorption Hysteresis In Situ with Small Angle X-Ray Scattering

    Science.gov (United States)

    Mitropoulos, Athanasios Ch.; Favvas, Evangelos P.; Stefanopoulos, Konstantinos L.; Vansant, Etienne F.

    2016-01-01

    Everett’s theorem-6 of the domain theory was examined by conducting adsorption in situ with small angle x-ray scattering (SAXS) supplemented by the contrast matching technique. The study focuses on the spectrum differences of a point to which the system arrives from different scanning paths. It is noted that according to this theorem at a common point the system has similar macroscopic properties. Furthermore it was examined the memory string of the system. We concluded that opposite to theorem-6: a) at a common point the system can reach in a finite (not an infinite) number of ways, b) a correction for the thickness of the adsorbed film prior to capillary condensation is necessary, and c) the scattering curves although at high-Q values coincide, at low-Q values are different indicating different microscopic states. That is, at a common point the system holds different metastable states sustained by hysteresis effects. These metastable states are the ones which highlight the way of a system back to a return point memory (RPM). Entering the hysteresis loop from different RPMs different histories are implanted to the paths toward the common point. Although in general the memory points refer to relaxation phenomena, they also constitute a characteristic feature of capillary condensation. Analogies of the no-passing rule and the adiabaticity assumption in the frame of adsorption hysteresis are discussed. PMID:27741263

  14. Examining molecular clouds in the Galactic Centre region using X-ray reflection spectra simulations

    Science.gov (United States)

    Walls, M.; Chernyakova, M.; Terrier, R.; Goldwurm, A.

    2016-12-01

    In the centre of our Galaxy lies a supermassive black hole, identified with the radio source Sagittarius A⋆. This black hole has an estimated mass of around 4 million solar masses. Although Sagittarius A⋆ is quite dim in terms of total radiated energy, having a luminosity that is a factor of 1010 lower than its Eddington luminosity, there is now compelling evidence that this source was far brighter in the past. Evidence derived from the detection of reflected X-ray emission from the giant molecular clouds in the Galactic Centre region. However, the interpretation of the reflected emission spectra cannot be done correctly without detailed modelling of the reflection process. Attempts to do so can lead to an incorrect interpretation of the data. In this paper, we present the results of a Monte Carlo simulation code we developed in order to fully model the complex processes involved in the emerging reflection spectra. The simulated spectra can be compared to real data in order to derive model parameters and constrain the past activity of the black hole. In particular, we apply our code to observations of Sagittarius B2, in order to constrain the position and density of the cloud and the incident luminosity of the central source. The results of the code have been adapted to be used in XSPEC by a large community of astronomers.

  15. NuSTAR SPECTROSCOPY OF MULTI-COMPONENT X-RAY REFLECTION FROM NGC 1068

    Energy Technology Data Exchange (ETDEWEB)

    Bauer, Franz E. [Pontificia Universidad Católica de Chile, Instituto de Astrofísica, Casilla 306, Santiago 22 (Chile); Arévalo, Patricia [EMBIGGEN Anillo, Concepción (Chile); Walton, Dominic J.; Baloković, Mislav; Brightman, Murray; Harrison, Fiona A. [Cahill Center for Astronomy and Astrophysics, California Institute of Technology, Pasadena, CA 91125 (United States); Koss, Michael J. [Institute for Astronomy, Department of Physics, ETH Zurich, Wolfgang-Pauli-Strasse 27, CH-8093 Zurich (Switzerland); Puccetti, Simonetta [ASDC-ASI, Via del Politecnico, I-00133 Roma (Italy); Gandhi, Poshak [School of Physics and Astronomy, University of Southampton, Highfield, Southampton SO17 1BJ (United Kingdom); Stern, Daniel [Jet Propulsion Laboratory, California Institute of Technology, 4800 Oak Grove Drive, Pasadena, CA 91109 (United States); Alexander, David M.; Moro, Agnese Del [Department of Physics, Durham University, South Road, Durham, DH1 3LE (United Kingdom); Boggs, Steve E.; Craig, William W. [Space Sciences Laboratory, University of California, Berkeley, CA 94720 (United States); Brandt, William N.; Luo, Bin [Department of Astronomy and Astrophysics, The Pennsylvania State University, 525 Davey Lab, University Park, PA 16802 (United States); Christensen, Finn E. [DTU Space, National Space Institute, Technical University of Denmark, Elektrovej 327, DK-2800 Lyngby (Denmark); Comastri, Andrea [INAF-Osservatorio Astronomico di Bologna, via Ranzani 1, I-40127 Bologna (Italy); Hailey, Charles J. [Columbia Astrophysics Laboratory, Columbia University, New York, NY 10027 (United States); Hickox, Ryan [Department of Physics and Astronomy, Dartmouth College, 6127 Wilder Laboratory, Hanover, NH 03755 (United States); and others

    2015-10-20

    We report on high-energy X-ray observations of the Compton-thick Seyfert 2 galaxy NGC 1068 with NuSTAR, which provide the best constraints to date on its >10 keV spectral shape. The NuSTAR data are consistent with those from past and current instruments to within cross-calibration uncertainties, and we find no strong continuum or line variability over the past two decades, which is in line with its X-ray classification as a reflection-dominated Compton-thick active galactic nucleus. The combined NuSTAR, Chandra, XMM-Newton, and Swift BAT spectral data set offers new insights into the complex secondary emission seen instead of the completely obscured transmitted nuclear continuum. The critical combination of the high signal-to-noise NuSTAR data and the decomposition of the nuclear and extranuclear emission with Chandra allow us to break several model degeneracies and greatly aid physical interpretation. When modeled as a monolithic (i.e., a single N{sub H}) reflector, none of the common Compton reflection models are able to match the neutral fluorescence lines and broad spectral shape of the Compton reflection hump without requiring unrealistic physical parameters (e.g., large Fe overabundances, inconsistent viewing angles, or poor fits to the spatially resolved spectra). A multi-component reflector with three distinct column densities (e.g., with best-fit values of N{sub H} of 1.4 × 10{sup 23}, 5.0 × 10{sup 24}, and 10{sup 25} cm{sup −2}) provides a more reasonable fit to the spectral lines and Compton hump, with near-solar Fe abundances. In this model, the higher N{sub H} component provides the bulk of the flux to the Compton hump, while the lower N{sub H} component produces much of the line emission, effectively decoupling two key features of Compton reflection. We find that ≈30% of the neutral Fe Kα line flux arises from >2″ (≈140 pc) and is clearly extended, implying that a significant fraction (and perhaps most) of the <10 keV reflected component

  16. Effect of C16TMA contents on the thermal stability of organo-bentonites: In situ X-ray diffraction analysis

    Energy Technology Data Exchange (ETDEWEB)

    Kooli, Fethi, E-mail: fkooli@taibahu.edu.sa [Taibah University, Department of Chemistry, PO Box 30002, Al-Madinah Al-Munawwarah (Saudi Arabia)

    2013-01-10

    Highlights: Black-Right-Pointing-Pointer Organo-bentonites were prepared at C16TMABr/CEC ratios up to 11. Black-Right-Pointing-Pointer Disorder configuration of C16TMA cations was observed at higher C16TMABr/CEC ratios. Black-Right-Pointing-Pointer The evolved gases during the calcinations of organoclays were analyzed by MS-TG. Black-Right-Pointing-Pointer In situ XRD technique detected clearly the phase disorder in the range 50-150 Degree-Sign C. Black-Right-Pointing-Pointer Collapse of organoclays depended on the temperature and the used atmospheres. - Abstract: Different concentrations of cetyl trimethylammonium bromide solutions were cation exchanged with bentonite clay mineral, at room temperature. The resulting organoclays were characterized by elemental analysis C and N, X-ray diffraction and thermal gravimetric analysis. The evolved gases during the calcination of organoclays were identified by online mass spectrometry coupled with thermal gravimetry technique. Meanwhile, in situ X-ray diffraction was used to have insight on the thermal stability of the organoclays in air atmosphere. X-ray diffraction at room temperature indicated that a disorder transition phase from bilayer to paraffin configuration occurred at higher surfactant-cation exchange capacity ratios, with two phases at 3.25 and 2.00 nm, respectively. The in situ X-ray diffraction confirmed the presence of these two phases with improved reflections intensities in the range of 100-200 Degree-Sign C. Above this temperature, both phases collapsed due to the decomposition of the surfactants as recorded by mass spectrometry thermal gravimetric analysis.

  17. Study of archaeological ceramics by total-reflection X-ray fluorescence spectrometry: Semi-quantitative approach

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez-Ruiz, R. [Universidad Autonoma de Madrid, Facultad de Ciencias, Servicio Interdepartamental de Investigacion, Modulo C-9, Laboratorio de TXRF, Crta. Colmenar, Km 15, Cantoblanco, E-28049, Madrid (Spain)], E-mail: ramon.fernandez@uam.es; Garcia-Heras, M. [Instituto de Historia-CSIC, C/Serrano, 13. E-28001, Madrid (Spain); CENIM-CSIC, Avda. Gregorio del Amo, 8. E-28040, Madrid (Spain)

    2007-10-15

    Total-reflection X-ray fluorescence spectrometry has been compared with Instrumental Neutron Activation Analysis in order to test its potential application to the study of archaeological ceramics in the archaeometric field. Two direct solid non-chemical sample preparation procedures have been checked: solid sedimentation and solid chemical homogenization. For sedimentation procedure, total-reflection X-ray fluorescence allows the analysis of the elemental composition with respect to the size fraction but not the average evaluation of the composition. For solid chemical homogenization procedure, total-reflection X-ray fluorescence provides precise (from 0.8% to 27% of coefficient of variation) and accurate results (from 91% to 110% of recovery) for 15 elements (Cr, Hf, Ni, Rb, Al, Ba, Ca, K, Mn, Ti, V, Cu, Ga, Y and Fe) with an easy sample preparation process of the solid clay and without previous chemical treatment. The influence of the particle sizes has been checked by total-reflection X-ray fluorescence sample angle scans and anomalous behaviors have been found for three additional detected elements: As, Sr and Zn, which can be attributed to interference effects of the mineral grain sizes of their associated chemical phases in the total-reflection X-ray fluorescence interference region. The solid chemical homogenization procedure produces data useful for archaeological interpretation, which is briefly illustrated by a case-study. Finally, the decantation procedure data can be also useful for size chemical speciation and, consequently, for alternative environmental total-reflection X-ray fluorescence applications.

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

    Science.gov (United States)

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

    2018-01-01

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

  19. Self-assembled iron oxide nanoparticle multilayer: x-ray and polarized neutron reflectivity.

    Science.gov (United States)

    Mishra, D; Benitez, M J; Petracic, O; Badini Confalonieri, G A; Szary, P; Brüssing, F; Theis-Bröhl, K; Devishvili, A; Vorobiev, A; Konovalov, O; Paulus, M; Sternemann, C; Toperverg, B P; Zabel, H

    2012-02-10

    We have investigated the structure and magnetism of self-assembled, 20 nm diameter iron oxide nanoparticles covered by an oleic acid shell for scrutinizing their structural and magnetic correlations. The nanoparticles were spin-coated on an Si substrate as a single monolayer and as a stack of 5 ML forming a multilayer. X-ray scattering (reflectivity and grazing incidence small-angle scattering) confirms high in-plane hexagonal correlation and a good layering property of the nanoparticles. Using polarized neutron reflectivity we have also determined the long range magnetic correlations parallel and perpendicular to the layers in addition to the structural ones. In a field of 5 kOe we determine a magnetization value of about 80% of the saturation value. At remanence the global magnetization is close to zero. However, polarized neutron reflectivity reveals the existence of regions in which magnetic moments of nanoparticles are well aligned, while losing order over longer distances. These findings confirm that in the nanoparticle assembly the magnetic dipole-dipole interaction is rather strong, dominating the collective magnetic properties at room temperature.

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

    Science.gov (United States)

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

    2010-06-01

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

  1. X-ray reflectivity measurements of layer-by-layer films at the solid/liquid interface.

    Science.gov (United States)

    Erokhina, Svetlana; Berzina, Tatiana; Cristofolini, Luigi; Erokhin, Victor; Folli, Claudia; Konovalov, Oleg; Marino, Iari-Gabriel; Fontana, M P

    2008-11-04

    In this Letter, we present a method for the decoration of layer-by-layer (LbL) structures by heavy metal ions, which allows X-ray reflectivity (XRR) measurements at the solid/water interface. The improved contrast has allowed us to obtain well-structured X-ray reflectivity curves from samples at the liquid/solid interface that can be used for the film structure modeling. The developed technique was also used to follow the formation of complexes between DNA and the LbL multilayer. The XRR data are confirmed by independent null-ellipsometric measurements at the solid/liquid interface on the very same architectures.

  2. X-Ray Reflected Spectra from Accretion Disk Models. III. A Complete Grid of Ionized Reflection Calculations

    Science.gov (United States)

    García, J.; Dauser, T.; Reynolds, C. S.; Kallman, T. R.; McClintock, J. E.; Wilms, J.; Eikmann, W.

    2013-05-01

    We present a new and complete library of synthetic spectra for modeling the component of emission that is reflected from an illuminated accretion disk. The spectra were computed using an updated version of our code XILLVER that incorporates new routines and a richer atomic database. We offer in the form of a table model an extensive grid of reflection models that cover a wide range of parameters. Each individual model is characterized by the photon index Γ of the illuminating radiation, the ionization parameter ξ at the surface of the disk (i.e., the ratio of the X-ray flux to the gas density), and the iron abundance A Fe relative to the solar value. The ranges of the parameters covered are 1.2 XSPEC. Detailed comparisons with previous reflection models illustrate the improvements incorporated in this version of XILLVER.

  3. Methodology for in situ synchrotron X-ray studies in the laser-heated diamond anvil cell

    DEFF Research Database (Denmark)

    Mezouar, M.; Giampaoli, R.; Garbarino, G.

    2017-01-01

    in the case of elemental tantalum. Preliminary results of a comparison between reflective and refractive optics for high temperature measurements in the laser-heated diamond anvil cell are briefly discussed. Finally, the importance of the size and relative alignment of X-ray and laser beams for quantitative X...

  4. Alignment of off-plane X-ray reflection gratings using optical light

    Science.gov (United States)

    Tutt, James; McEntaffer, Randall; Donovan, Benjamin; Schultz, Ted; DeRoo, Casey; Hertz, Edward; Allured, Ryan

    2017-08-01

    The next generation of high resolution soft X-ray spectrometers require large effective areas and high resolving capability. This can be achieved through the use of off-plane reflection gratings. X-rays will only reflect if they are incident onto a surface at a shallow graze angle; therefore, arrays of off-plane gratings are placed into the converging beam of a telescope to achieve the necessary effective area. To maintain the high resolving power of a single grating across this array, the gratings have to be very precisely aligned to one another and fanned so that they match the convergence of the telescope.Leveraging previous work that co-aligned 4 state of the art gratings into a module, 26 gratings will be co-aligned into a module that will be launched on the sub-orbital rocket WRX-R. The alignment procedure is unchanged, but improvements have been made to stabilize the setup. The alignment procedure was found to be highly temperature dependent and the opto-mechanics suffered from mechanical instabilities. To solve these issues, the new setup uses a high precision temperature control unit and a larger optical bench allowing the setup to be simplified.The alignment method is based around the generation of a light wavefront which reflects off the grating surface. This wavefront is measured using a Shack-Hartmann sensor, which allows the gratings orientation relative to the sensor normal to be found. A hexapod is then used to move the grating, allowing the grating surface to be aligned in pitch, roll and yaw. The x, y and z positions for each grating are constrained through the mechanical tolerance of the alignment mount and high precision stages. The aligned gratings are mounted into an Invar module and a theodolite is used to measure the relative position of the module to the known position of the grating.This poster discusses the improvements made to the grating alignment process and the proposed path towards producing the array of 26 co-aligned gratings that

  5. Integrated X-ray testing of the electro-optical breadboard model for the XMM reflection grating spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Bixler, J.V.; Craig, W.; Decker, T. [Lawrence Livermore National Lab., CA (United States); Aarts, H.; Boggende, T. den; Brinkman, A.C. [Space Research Organization Netherlands, Utrecht (Netherlands); Burkert, W.; Brauninger, H. [Max-Planck Institute fur Extraterrestische Physik, Testanlage (Germany); Branduardi-Raymont, G. [Univ. College London (United Kingdom); Dubbeldam, L. [Space Research Organization Netherlands, Leiden (Netherlands)] [and others

    1994-07-12

    X-ray calibration of the Electro-Optical Breadboard Model (EOBB) of the XXM Reflection Grating Spectrometer has been carried out at the Panter test facility in Germany. The EOBB prototype optics consisted of a four-shell grazing incidence mirror module followed by an array of eight reflection gratings. The dispersed x-rays were detected by an array of three CCDs. Line profile and efficiency measurements where made at several energies, orders, and geometric configurations for individual gratings and for the grating array as a whole. The x-ray measurements verified that the grating mounting method would meet the stringent tolerances necessary for the flight instrument. Post EOBB metrology of the individual gratings and their mountings confirmed the precision of the grating boxes fabrication. Examination of the individual grating surface`s at micron resolution revealed the cause of anomalously wide line profiles to be scattering due to the crazing of the replica`s surface.

  6. Geological Carbon Sequestration: new insights from in-situ Synchrotron X-ray Microtomography

    Science.gov (United States)

    Voltolini, M.; Kwon, T.; Ajo Franklin, J. B.

    2012-12-01

    In a world with rapidly increasing atmospheric CO2 concentrations, a variety of scalable technologies are being considered to mitigate emissions from the combustion of fossil fuels; among these approaches, geological carbon storage (GCS) is being actively tested at a variety of subsurface sites. Despite these activities, a mechanistic understanding of multiphase flow in scCO2/brine systems at the pore scale is still being developed. The distribution of scCO2 in the pore space controls a variety of processes at the continuum scale including CO2 dissolution rate (by way of brine/CO2 contact area), capillary trapping, and residual brine fraction. Virtually no dynamic measurements of the pore-scale distribution of scCO2 in real geological samples have been made in three dimensions leaving models describing multi-phase fluid dynamics, reactive transport, and geophysical properties reliant on analog systems (often using fewer spatial dimensions, different fluids, or lower pressures) or theoretical models describing phase configurations. We present dynamic pore-scale imagery of scCO2 invasion dynamics in a 3D geological sample, in this case a quartz-rich sandstone core extracted from the Domengine Fm, a regionally extensive unit which is currently a target for future GCS operations in the Sacramento Basin. This dataset, acquired using synchrotron X-ray micro tomography (SXR-μCT) and high speed radiography, was made possible by development of a controlled P/T flow-through triaxial cell compatible with X-ray imaging in the 8-40 keV range. These experiments successfully resolved scCO2 and brine phases at a spatial resolution of 4.47 μm while the sample was kept at in situ conditions (45°C, 9 MPa pore pressure, 14 MPa hydrostatic confining stress) during drainage and imbibition cycles. Image volumes of the dry, brine saturated, and partially scCO2 saturated sample were captured and were used to correlate aspects of rock microstructure to development of the invasion front

  7. In situ MEMS testing: correlation of high-resolution X-ray diffraction with mechanical experiments and finite element analysis.

    Science.gov (United States)

    Schifferle, Andreas; Dommann, Alex; Neels, Antonia

    2017-01-01

    New methods are needed in microsystems technology for evaluating microelectromechanical systems (MEMS) because of their reduced size. The assessment and characterization of mechanical and structural relations of MEMS are essential to assure the long-term functioning of devices, and have a significant impact on design and fabrication. Within this study a concept for the investigation of mechanically loaded MEMS materials on an atomic level is introduced, combining high-resolution X-ray diffraction (HRXRD) measurements with finite element analysis (FEA) and mechanical testing. In situ HRXRD measurements were performed on tensile loaded single crystal silicon (SCSi) specimens by means of profile scans and reciprocal space mapping (RSM) on symmetrical (004) and (440) reflections. A comprehensive evaluation of the rather complex XRD patterns and features was enabled by the correlation of measured with simulated, 'theoretical' patterns. Latter were calculated by a specifically developed, simple and fast approach on the basis of continuum mechanical relations. Qualitative and quantitative analysis confirmed the admissibility and accuracy of the presented method. In this context [001] Poisson's ratio was determined providing an error of less than 1.5% with respect to analytical prediction. Consequently, the introduced procedure contributes to further going investigations of weak scattering being related to strain and defects in crystalline structures and therefore supports investigations on materials and devices failure mechanisms.

  8. Direct and quantitative comparison of pixelated density profiles with high-resolution X-ray reflectivity data.

    Science.gov (United States)

    Fenter, P; Lee, S S; Skelton, A A; Cummings, P T

    2011-03-01

    A method for comparing pixelated density profiles (e.g. obtained from molecular dynamics or other computational techniques) with experimental X-ray reflectivity data both directly and quantitatively is described. The conditions under which such a comparison can be made quantitatively (e.g. with errors X-ray reflectivity calculations for binned density profiles is defined in terms of the inter-relationships between resolution of the X-ray reflectivity data (i.e. its range in momentum transfer), the chosen bin size and the width of the intrinsic density profile. These factors play a similar role in the application of any structure-factor calculations that involve the use of pixelated density profiles, such as those obtained from iterative phasing algorithms for inverting structures from X-ray reflectivity and coherent diffraction imaging data. Finally, it is shown how simulations of a quartz-water interface can be embedded into an exact description of the `bulk' phases (including the substrate crystal and the fluid water, below and above the actual interface) to quantitatively reproduce the experimental reflectivity data of a solid-liquid interface.

  9. Quantifying the Nucleation and Growth Kinetics of Microwave Nanochemistry Enabled by in Situ High-Energy X-ray Scattering.

    Science.gov (United States)

    Liu, Qi; Gao, Min-Rui; Liu, Yuzi; Okasinski, John S; Ren, Yang; Sun, Yugang

    2016-01-13

    The fast reaction kinetics presented in the microwave synthesis of colloidal silver nanoparticles was quantitatively studied, for the first time, by integrating a microwave reactor with in situ X-ray diffraction at a high-energy synchrotron beamline. Comprehensive data analysis reveals two different types of reaction kinetics corresponding to the nucleation and growth of the Ag nanoparticles. The formation of seeds (nucleation) follows typical first-order reaction kinetics with activation energy of 20.34 kJ/mol, while the growth of seeds (growth) follows typical self-catalytic reaction kinetics. Varying the synthesis conditions indicates that the microwave colloidal chemistry is independent of concentration of surfactant. These discoveries reveal that the microwave synthesis of Ag nanoparticles proceeds with reaction kinetics significantly different from the synthesis present in conventional oil bath heating. The in situ X-ray diffraction technique reported in this work is promising to enable further understanding of crystalline nanomaterials formed through microwave synthesis.

  10. X-RAY REFLECTED SPECTRA FROM ACCRETION DISK MODELS. III. A COMPLETE GRID OF IONIZED REFLECTION CALCULATIONS

    Energy Technology Data Exchange (ETDEWEB)

    Garcia, J.; McClintock, J. E. [Harvard-Smithsonian Center for Astrophysics, 60 Garden Street, Cambridge, MA 02138 (United States); Dauser, T.; Wilms, J.; Eikmann, W. [Dr. Karl Remeis-Observatory and Erlangen Centre for Astroparticle Physics, Sternwartstr. 7, D-96049 Bamberg (Germany); Reynolds, C. S. [Department of Astronomy, University of Maryland, College Park, MD (United States); Kallman, T. R., E-mail: javier@head.cfa.harvard.edu, E-mail: jem@cfa.harvard.edu, E-mail: chris@astro.umd.edu, E-mail: thomas.dauser@sternwarte.uni-erlangen.de, E-mail: joern.wilms@sternwarte.uni-erlangen.de, E-mail: wiebke.eikmann@sternwarte.uni-erlangen.de, E-mail: timothy.r.kallman@nasa.gov [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States)

    2013-05-10

    We present a new and complete library of synthetic spectra for modeling the component of emission that is reflected from an illuminated accretion disk. The spectra were computed using an updated version of our code XILLVER that incorporates new routines and a richer atomic database. We offer in the form of a table model an extensive grid of reflection models that cover a wide range of parameters. Each individual model is characterized by the photon index {Gamma} of the illuminating radiation, the ionization parameter {xi} at the surface of the disk (i.e., the ratio of the X-ray flux to the gas density), and the iron abundance A{sub Fe} relative to the solar value. The ranges of the parameters covered are 1.2 {<=} {Gamma} {<=} 3.4, 1 {<=} {xi} {<=} 10{sup 4}, and 0.5 {<=} A{sub Fe} {<=} 10. These ranges capture the physical conditions typically inferred from observations of active galactic nuclei, and also stellar-mass black holes in the hard state. This library is intended for use when the thermal disk flux is faint compared to the incident power-law flux. The models are expected to provide an accurate description of the Fe K emission line, which is the crucial spectral feature used to measure black hole spin. A total of 720 reflection spectra are provided in a single FITS file (http://hea-www.cfa.harvard.edu/{approx}javier/xillver/) suitable for the analysis of X-ray observations via the atable model in XSPEC. Detailed comparisons with previous reflection models illustrate the improvements incorporated in this version of XILLVER.

  11. In-situ X-ray CT results of damage evolution in L6 ordinary chondrite meteorites

    Energy Technology Data Exchange (ETDEWEB)

    Cuadra, Jefferson A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Hazeli, Kavan [Univ. of Alabama, Huntsville, AL (United States); Ramesh, K. T. [Johns Hopkins Univ., Baltimore, MD (United States). Hopkins Extreme Materials Inst.; Martz, Harry [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States). Nondestructive Characterization Inst.

    2016-06-17

    These are slides about in-situ X-ray CT results of damage evolution in L6 ordinary chondrite meteorites. The following topics are covered: mechanical and thermal damage characterization, list of Grosvenor Mountain (GRO) meteorite samples, in-situ x-ray compression test setup, GRO-chipped reference at 0 N - existing cracks, GRO-chipped loaded at 1580 N, in-situ x-ray thermal fatigue test setup, GRO-B14 room temperature reference, GRO-B14 Cycle 47 at 200°C, GRO-B14 Cycle 47 at room temperature, conclusions from qualitative analysis, future work and next steps. Conclusions are the following: Both GRO-Chipped and GRO-B14 had existing voids and cracks within the volume. These sites with existing damage were selected for CT images from mechanically and thermally loaded scans since they are prone to damage initiation. The GRO-Chipped sample was loaded to 1580 N which resulted in a 14% compressive engineering strain, calculated using LVDT. Based on the CT cross sectional images, the GRO-B14 sample at 200°C has a thermal expansion of approximately 96 μm in height (i.e. ~1.6% engineering strain).

  12. Development of off-line layer chromatographic and total reflection X-ray fluorescence spectrometric methods for arsenic speciation

    Energy Technology Data Exchange (ETDEWEB)

    Mihucz, Victor G. [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary); Hungarian Satellite Centre of Trace Elements Institute to UNESCO, P. O. Box 32, H-1518 Budapest (Hungary); Moricz, Agnes M. [L. Eoetvoes University, Department of Chemical Technology and Environmental Chemistry, P.O. Box 32, H-1518 Budapest (Hungary); Kroepfl, Krisztina [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary); Szikora, Szilvia [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary); Tatar, Eniko [Hungarian Satellite Centre of Trace Elements Institute to UNESCO, P. O. Box 32, H-1518 Budapest (Hungary); L. Eoetvoes University, Department of Inorganic and Analytical Chemistry, P.O. Box 32, H-1518 Budapest (Hungary); Parra, Lue Meru Marco [Universidad Centro-occidental Lisandro Alvarado, Decanato de Agronomia, Departamento de Quimica y Suelos Unidad de Analisis Instrumental, Apartado Postal 4076, Cabudare 3023 (Venezuela); Zaray, Gyula [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary) and Hungarian Satellite Centre of Trace Elements Institute to UNESCO, P. O. Box 32, H-1518 Budapest (Hungary) and L. Eoetvoes University, Department of Inorganic and Analytical Chemistry, P.O. Box 32, H-1518 Budapest (Hungary)]. E-mail: zaray@ludens.elte.hu

    2006-11-15

    Rapid and low cost off-line thin layer chromatography-total reflection X-ray fluorescence spectrometry and overpressured thin layer chromatography-total reflection X-ray fluorescence spectrometry methods have been developed for separation of 25 ng of each As(III), As(V), monomethyl arsonic acid and dimethylarsinic acid applying a PEI cellulose stationary phase on plastic sheets and a mixture of acetone/acetic acid/water = 2:1:1 (v/v/v) as eluent system. The type of eluent systems, the amounts (25-1000 ng) of As species applied to PEI cellulose plates, injection volume, development distance, and flow rate (in case of overpressured thin layer chromatography) were taken into consideration for the development of the chromatographic separation. Moreover, a microdigestion method employing nitric acid for the As spots containing PEI cellulose scratched from the developed plates divided into segments was developed for the subsequent total reflection X-ray fluorescence spectrometry analysis. The method was applied for analysis of root extracts of cucumber plants grown in As(III) containing modified Hoagland nutrient solution. Both As(III) and As(V) were detected by applying the proposed thin layer chromatography/overpressured thin layer chromatography-total reflection X-ray fluorescence spectrometry methods.

  13. Reconstruction of interfaces of periodic multilayers from X-ray reflectivity using a free-form approach

    NARCIS (Netherlands)

    Zameshin, Andrey; Makhotkin, Igor Alexandrovich; Yakunin, Sergey N.; van de Kruijs, Robbert Wilhelmus Elisabeth; Yakshin, Andrey; Bijkerk, Frederik

    2016-01-01

    Grazing-incidence X-ray reflectivity (GIXRR) is a widely used analysis method for thin films and multilayer structures. However, conventional so-called model-based approaches of structural reconstruction from GIXRR data lack flexibility when dealing with very thin structures (down to the nanometre

  14. Structure of a liquid/liquid interface during solvent extraction combining X-ray and neutron reflectivity measurements.

    Science.gov (United States)

    Scoppola, E; Watkins, E; Li Destri, G; Porcar, L; Campbell, R A; Konovalov, O; Fragneto, G; Diat, O

    2015-06-21

    We have resolved the molecular structure of a bulk oil/water interface that contains amphiphilic ligand molecules using a combination of X-ray and neutron reflectivity measurements for the first time. This new capability can greatly impact future work in the field of ion separation by phase transfer, i.e. liquid/liquid extraction.

  15. Hydrogen concentration and mass density of diamondlike carbon films obtained by x-ray and neutron reflectivity

    DEFF Research Database (Denmark)

    Findeisen, E.; Feidenhans'l, R.; Vigild, Martin Etchells

    1994-01-01

    Specular reflectivity of neutrons and x rays can be used to determine the scattering length density profile of a material perpendicular to its surface. We have applied these techniques to study amorphous, diamondlike, hydrocarbon films. By the combination of these two techniques we obtain not only...

  16. Structure and Growth of Vapor-Deposited n-Dotriacontane Films Studied by X-ray Reflectivity

    DEFF Research Database (Denmark)

    del Campo, V.; Cisternas, E.; Taub, H.

    2009-01-01

    We have used synchrotron X-ray reflectivity measurements to investigate the structure of n-dotriacontane (n-C32H66 or C32) films deposited from the vapor phase onto a SiO2-coated Si(100) surface. Our primary motivation was to determine whether the structure and growth mode of these films differ...

  17. Nanocalorimeter platform for in situ specific heat measurements and x-ray diffraction at low temperature

    Energy Technology Data Exchange (ETDEWEB)

    Willa, K. [Materials Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA; Diao, Z. [Department of Physics, Stockholm University, SE-106 91 Stockholm, Sweden; Laboratory of Mathematics, Physics and Electrical Engineering, Halmstad University, P.O. Box 823, SE-301 18 Halmstad, Sweden; Campanini, D. [Department of Physics, Stockholm University, SE-106 91 Stockholm, Sweden; Welp, U. [Materials Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA; Divan, R. [Center for Nanoscale Materials, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA; Hudl, M. [Department of Physics, Stockholm University, SE-106 91 Stockholm, Sweden; Islam, Z. [X-ray Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA; Kwok, W. -K. [Materials Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA; Rydh, A. [Department of Physics, Stockholm University, SE-106 91 Stockholm, Sweden

    2017-12-01

    Recent advances in electronics and nanofabrication have enabled membrane-based nanocalorimetry for measurements of the specific heat of microgram-sized samples. We have integrated a nanocalorimeter platform into a 4.5 T split-pair vertical-field magnet to allow for the simultaneous measurement of the specific heat and x-ray scattering in magnetic fields and at temperatures as low as 4 K. This multi-modal approach empowers researchers to directly correlate scattering experiments with insights from thermodynamic properties including structural, electronic, orbital, and magnetic phase transitions. The use of a nanocalorimeter sample platform enables numerous technical advantages: precise measurement and control of the sample temperature, quantification of beam heating effects, fast and precise positioning of the sample in the x-ray beam, and fast acquisition of x-ray scans over a wide temperature range without the need for time-consuming re-centering and re-alignment. Furthermore, on an YBa2Cu3O7-delta crystal and a copper foil, we demonstrate a novel approach to x-ray absorption spectroscopy by monitoring the change in sample temperature as a function of incident photon energy. Finally, we illustrate the new insights that can be gained from in situ structural and thermodynamic measurements by investigating the superheated state occurring at the first-order magneto-elastic phase transition of Fe2P, a material that is of interest for magnetocaloric applications.

  18. In situ electrochemical high-energy X-ray diffraction using a capillary working electrode cell geometry.

    Science.gov (United States)

    Young, Matthias J; Bedford, Nicholas M; Jiang, Naisheng; Lin, Deqing; Dai, Liming

    2017-07-01

    The ability to generate new electrochemically active materials for energy generation and storage with improved properties will likely be derived from an understanding of atomic-scale structure/function relationships during electrochemical events. Here, the design and implementation of a new capillary electrochemical cell designed specifically for in situ high-energy X-ray diffraction measurements is described. By increasing the amount of electrochemically active material in the X-ray path while implementing low-Z cell materials with anisotropic scattering profiles, an order of magnitude enhancement in diffracted X-ray signal over traditional cell geometries for multiple electrochemically active materials is demonstrated. This signal improvement is crucial for high-energy X-ray diffraction measurements and subsequent Fourier transformation into atomic pair distribution functions for atomic-scale structural analysis. As an example, clear structural changes in LiCoO2 under reductive and oxidative conditions using the capillary cell are demonstrated, which agree with prior studies. Accurate modeling of the LiCoO2 diffraction data using reverse Monte Carlo simulations further verifies accurate background subtraction and strong signal from the electrochemically active material, enabled by the capillary working electrode geometry.

  19. X-ray absorption and reflection as probes of the GaN conduction bands: Theory and experiments

    Energy Technology Data Exchange (ETDEWEB)

    Lambrecht, W.R.L.; Rashkeev, S.N.; Segall, B. [Case Western Reserve Univ., Cleveland, OH (United States)] [and others

    1997-04-01

    X-ray absorption measurements are a well-known probe of the unoccupied states in a material. The same information can be obtained by using glancing angle X-ray reflectivity. In spite of several existing band structure calculations of the group III nitrides and previous optical studies in UV range, a direct probe of their conduction band densities of states is of interest. The authors performed a joint experimental and theoretical investigation using both of these experimental techniques for wurtzite GaN.

  20. A large-volume gas cell for high-energy X-ray reflectivity investigations of interfaces under pressure.

    Science.gov (United States)

    Venturini, Federica; Schöder, Sebastian; Kuhs, Werner F; Honkimäki, Veijo; Melesi, Louis; Reichert, Harald; Schober, Helmut; Thomas, Frederic

    2011-03-01

    A cell for the investigation of interfaces under pressure is presented. Given the pressure and temperature specifications of the cell, P ≤ 100 bar and 253 K ≤ T ≤ 323 K, respectively, high-energy X-rays are required to penetrate the thick Al(2)O(3) windows. The CH(4)(gas)/H(2)O(liquid) interface has been chosen to test the performance of the new device. The measured dynamic range of the high-energy X-ray reflectivity data exceeds 10(-8), thereby demonstrating the validity of the entire experimental set-up.

  1. An access to buried interfaces: the X-ray reflectivity set-up of BL9 at DELTA.

    Science.gov (United States)

    Paulus, Michael; Lietz, Daniela; Sternemann, Christian; Shokuie, Kaveh; Evers, Florian; Tolan, Metin; Czeslik, Claus; Winter, Roland

    2008-11-01

    An X-ray reflectivity set-up to study buried interfaces at beamline BL9 of the electron storage ring DELTA is presented. The structure of solid-gas and solid-liquid interfaces can be investigated using X-rays with incident energies of about 27 keV. A detailed description of the set-up is given and its performance is demonstrated by a discussion of selected applications, i.e. protein adsorption at the solid-liquid interface and gas adsorption at the solid-gas interface at elevated pressures.

  2. X-Ray Diffraction and Reflectivity Validation of the Depletion Attraction in the Competitive Adsorption of Lung Surfactant and Albumin

    DEFF Research Database (Denmark)

    Stenger, Patric C.; Wu, Guohui; Miller, Chad E.

    2009-01-01

    Lung surfactant (LS) and albumin compete for the air-water interface when both are present in solution. Equilibrium favors LS because it has a lower equilibrium surface pressure, but the smaller albumin is kinetically favored by faster diffusion. Albumin at the interface creates an energy barrier...... to subsequent LS adsorption that can be overcome by the depletion attraction induced by polyethylene glycol (PEG) in solution. A combination of grazing incidence x-ray diffraction (GIXD), x-ray reflectivity (XR), and pressure-area isotherms provides molecular-resolution information on the location...

  3. Determination of element levels in human serum: Total reflection X-ray fluorescence applications

    Science.gov (United States)

    Majewska, U.; Łyżwa, P.; Łyżwa, K.; Banaś, D.; Kubala-Kukuś, A.; Wudarczyk-Moćko, J.; Stabrawa, I.; Braziewicz, J.; Pajek, M.; Antczak, G.; Borkowska, B.; Góźdź, S.

    2016-08-01

    Deficiency or excess of elements could disrupt proper functioning of the human body and could lead to several disorders. Determination of their concentrations in different biological human fluids and tissues should become a routine practice in medical treatment. Therefore the knowledge about appropriate element concentrations in human organism is required. The purpose of this study was to determine the concentration of several elements (P, S, Cl, K, Ca, Cr, Fe, Cu, Zn, Se, Br, Rb, Pb) in human serum and to define the reference values of element concentration. Samples of serum were obtained from 105 normal presumably healthy volunteers (66 women aged between 15 and 78 years old; 39 men aged between 15 and 77 years old). Analysis has been done for the whole studied population and for subgroups by sex and age. It is probably first so a wide study of elemental composition of serum performed in the case of Świętokrzyskie region. Total reflection X-ray fluorescence (TXRF) method was used to perform the elemental analysis. Spectrometer S2 Picofox (Bruker AXS Microanalysis GmbH) was used to identify and measure elemental composition of serum samples. Finally, 1st and 3rd quartiles were accepted as minimum and maximum values of concentration reference range.

  4. X-ray reflectivity investigation of Newton and common black films

    Science.gov (United States)

    Benattar, J. J.; Schalchli, A.; Bélorgey, O.

    1992-06-01

    In the present paper we show that X-ray reflectivity provides a new means of studying black films of soap which are the ultimate stage of thinning soap films. We have thus solved a structural problem which dates is back over three centuries old: the Newton black film has a sandwich structure which does not contain an aqueous core but only contains a hydration layer of the polar heads. We have also investigated the thicker common black films as a function of the ionic strength and of the drainage of water on a nanometric scale. Dans cet article nous montrons que la réflectivité des rayons X est un nouveau moyen d'aborder l'étude des films noirs de savon qui sont les étapes ultimes d'une bulle après l'écoulement de l'eau. Nous avons pu résoudre ainsi un problème structural qui date de plus de trois sièlces: le film noir de Newton est une structure sandwich qui ne contient pas d'eau mais une couche d'hydratation des têtes polaires. Nous avons également étudié les films noirs communs, plus épais, en fonction de la force ionique ainsi que les problèmes d'écoulement à une échelle nanométrique.

  5. Total reflection X-ray fluorescence as a fast multielemental technique for human placenta sample analysis

    Science.gov (United States)

    Marguí, E.; Ricketts, P.; Fletcher, H.; Karydas, A. G.; Migliori, A.; Leani, J. J.; Hidalgo, M.; Queralt, I.; Voutchkov, M.

    2017-04-01

    In the present contribution, benchtop total reflection X-ray fluorescence spectrometry (TXRF) has been evaluated as a cost-effective multielemental analytical technique for human placenta analysis. An easy and rapid sample preparation consisting of suspending 50 mg of sample in 1 mL of a Triton 1% solution in deionized water showed to be the most suitable for this kind of samples. However, for comparison purposes, an acidic microwave acidic digestion procedure was also applied. For both sample treatment methodologies, limits of detection for most elements were in the low mg/kg level. Accurate and precise results were obtained using internal standardization as quantification approach and applying a correction factor to compensate for absorption effects. The correction factor was based on the proportional ratio between the slurry preparation results and those obtained for the analysis of a set of human placenta samples analysed by microwave acidic digestion and ICP-AES analysis. As a study case, the developed TXRF methodology was applied for multielemental analysis (K, Ca, Fe, Cu, Zn, As, Se, Br, Rb and Sr) of several healthy women's placenta samples from two regions in Jamaica.

  6. Understanding properties of engineered catalyst supports using contact angle measurements and X-ray reflectivity.

    Science.gov (United States)

    Amama, Placidus B; Islam, Ahmad E; Saber, Sammy M; Huffman, Daniel R; Maruyama, Benji

    2016-02-07

    There is significant interest in broadening the type of catalyst substrates that support the growth of high-quality carbon nanotube (CNT) carpets. In this study, ion beam bombardment has been utilized to modify catalyst substrates for CNT carpet growth. Using a combination of contact angle measurements (CAMs) and X-ray reflectivity (XRR) for the first time, new correlations between the physicochemical properties of pristine and engineered catalyst substrates and CNT growth behavior have been established. The engineered surfaces obtained after exposure to different degrees of ion beam damage have distinct physicochemical properties (porosity, layer thickness, and acid-base properties). The CAM data were analyzed using the van Oss-Chaudhury-Good model, enabling the determination of the acid-base properties of the substrate surfaces. For the XRR data, a Fourier analysis of the interference patterns enabled extraction of layer thickness, while the atomic density and interfacial roughness were extracted by analyzing the amplitude of the interference oscillations. The dramatic transformation of the substrate from "inactive" to "active" is attributed to a combined effect of substrate porosity or damage depth and Lewis basicity. The results reveal that the efficiency of catalyst substrates can be further improved by increasing the substrate basicity, if the minimum surface porosity is established. This study advances the use of a non-thermochemical approach for catalyst substrate engineering, as well as demonstrates the combined utility of CAM and XRR as a powerful, nondestructive, and reliable tool for rational catalyst design.

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

    Science.gov (United States)

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

    2017-10-01

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

  8. X-ray reflectivity studies at the mercury/electrolyte interface

    Energy Technology Data Exchange (ETDEWEB)

    Elsen, Annika; Murphy, Bridget M.; Magnussen, Olaf M. [Institut fuer Experimentelle und Angewandte Physik, CAU, D-24105 Kiel (Germany); Ocko, Ben M. [Department of Physics, BNL, Upton, New York 11973 (United States); Tamam, Lilach; Deutsch, Moshe [Department of Physics, Bar-Ilan University, Ramat Gan 52900 (Israel); Kuzmenko, Ivan [CMC-CAT, APS, ANL, Argonne, Illinois 60439 (United States)

    2010-07-01

    The interface between the liquid mercury electrode and an electrolyte solution is one of the most extensively studied electrochemical systems. It was fundamental for verifying traditional and modern theories of the electrochemical double layer. Although the metal contributes significant to the double layer capacity, with its interface structure playing an important role, up to now there is almost no knowledge about this structure. Here we present the first X-ray reflectivity studies at the liquid mercury electrode in electrolyte solution (0.01M NaF), allowing to clarify the interface structure. The experiments exhibited atomic layering of the mercury perpendicular to the surface similar to that found for the mercury vapour interface. We found a significant influence on the width of the interface electron density profile which can be referred to two effects: first of all the potential dependent change in the surface tension causes a change in the capillary wave induced interface roughness. Secondly another potential controlled effect was found due to the intrinsic change in the electron density distribution because of interface polarisation.

  9. Total reflection X-ray fluorescence analysis of pollen as an indicator for atmospheric pollution

    Energy Technology Data Exchange (ETDEWEB)

    Pepponi, G. E-mail: pepponi@itc.it; Lazzeri, P.; Coghe, N.; Bersani, M.; Gottardini, E.; Cristofolini, F.; Clauser, G.; Torboli, A

    2004-08-31

    The viability of pollen is affected by environmental pollution and its use as a bio-indicator is proposed. Such effects can be observed and quantified by biological tests. However, a more accurate identification of the agents affecting the viability is required in order to validate the biological assay for environmental monitoring. The chemical analysis of pollen is meant to ascertain the existence of a correlation between its reduced biological functions and the presence of pollutants. Moreover, such biological systems act as accumulators and allow the detection and quantification of species present in the environment at low concentrations. Total reflection X-ray fluorescence analysis (TXRF) has been chosen for the investigation due to its high sensitivity, multielement capability and wide dynamic range. Corylus avellana L. (hazel) pollen has been collected in areas with different anthropic impact in the province of Trento, Italy. For the TXRF measurements, a liquid sample is needed, especially if a quantitative analysis is required. In the present work, the analysis after a microwave digestion has been compared with the analysis of a suspension of the pollen samples. In both cases, an internal standard has been used for the quantification. The concentrations of 17 elements ranging from Al to Pb have been determined in 13 samples. Analysis of the suspensions showed to be comparable to that of digested samples in terms of spectral quality, but the latter preparation method gave better reproducibility. Sub-ppm lowest limits of detection were obtained for iron and heavier elements detected.

  10. Development of a total reflection X-ray fluorescence spectrometer for ...

    Indian Academy of Sciences (India)

    Unknown

    TXRF) spectrometer has been designed, constructed and realized. The spectrometer is capable of ultra-trace multielement analysis as well as performs surface characterization of thin films. The TXRF setup comprises of an X-ray generator, a slit-.

  11. In Situ X-ray Microtomography of Stress Corrosion Cracking and Corrosion Fatigue in Aluminum Alloys

    Science.gov (United States)

    Singh, Sudhanshu S.; Stannard, Tyler J.; Xiao, Xianghui; Chawla, Nikhilesh

    2017-08-01

    Structural materials are subjected to combinations of stress and corrosive environments that work synergistically to cause premature failure. Therefore, studies on the combined effect of stress and corrosive environments on material behavior are required. Existing studies have been performed in two dimensions that are inadequate for full comprehension of the three-dimensional (3D) processes related to stress corrosion cracking (SCC) and corrosion-fatigue (CF) behavior. Recently, x-ray synchrotron tomography has evolved as an excellent technique to obtain the microstructure in 3D. Moreover, being nondestructive in nature, x-ray synchrotron tomography is well suited to study the evolution of microstructure with time (4D, or fourth dimension in time). This article presents our recent 4D studies on SCC and CF of Al 7075 alloys using x-ray synchrotron tomography.

  12. High reflectance Cr/C multilayer at 250 eV for soft X-ray polarimetry

    Energy Technology Data Exchange (ETDEWEB)

    Wen, Mingwu; Jiang, Li; Zhang, Zhong; Huang, Qiushi [MOE Key Laboratory of Advanced Micro-Structured Materials, Institute of Precision Optical Engineering (IPOE), School of Physics Science and Engineering, Tongji University, Shanghai 200092 (China); Wang, Zhanshan, E-mail: wangzs@tongji.edu.cn [MOE Key Laboratory of Advanced Micro-Structured Materials, Institute of Precision Optical Engineering (IPOE), School of Physics Science and Engineering, Tongji University, Shanghai 200092 (China); She, Rui; Feng, Hua [Department of Engineering Physics, Tsinghua University, Beijing (China); Wang, Hongchang [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE (United Kingdom)

    2015-10-01

    X-ray reflection near 45° via multilayer mirrors can be used for astronomical polarization measurements. A Cr/C multilayer mirror (designed for X-ray polarimetry at 250 eV), with a period thickness of 3.86 nm and a bi-layer number of 100, was fabricated using direct current magnetron sputtering. Grazing incidence X-ray reflectometry at 8 keV and transmission electron microscopy were used to investigate the multilayer structure. Different models were introduced to fit the hard X-ray reflectivity curve, which indicates that the layer thickness of two materials slightly drifts from the bottom to the top of the stack. Both the chromium and carbon layers are amorphous with asymmetric interfaces, while the Cr-on-C interface is slightly wider. Based on the good quality of the multilayer structure, a high reflectivity of 21.8% for the s-polarized light was obtained at 250 eV at a grazing incidence angle of 40.7°. The fabricated Cr/C multilayer mirror exhibits high reflectivity and polarization levels in the energy region of 240 eV–260 eV. - Highlights: • We fabricated Cr/C multilayer with 3.8 nm d-spacing. • X-ray reflectometry was used to determine the exact structure of Cr/C multilayer. • A high reflectivity of 21.8% for the s-polarized light was obtained at 250 eV. • Both Cr and C were found to be amorphous with slightly asymmetric interfaces. • A 4-layer model was used to fit and explain the results.

  13. X-ray Reflectivity Study of Ionic Liquids at Electrified Surfaces

    Science.gov (United States)

    Chu, Miaoqi

    X-ray reflectivity (XRR) versatile technique that characterize the surface structures. However, due to the lack of phase information of X-ray data, the reconstruction of electron density profile (EDP) from XRR data is an ill-posed inverse problem that requires extra attention. In Chapter 1, several key concepts in XRR data analysis are reviewed. The typical XRR data acquisition procedure and methods of modeling electron density are introduced. The widely used logarithm form of merit function is justified with mathematical deduction and numerical experiment. A scheme that generates artificial reflectivity data with theoretical statistical error but not systematical error is proposed. With the methods and schemes described in Chapter 1, simulated reflectivity data of a simple one-slab model is generated and fitted to test the efficient of EDP reconstruction. By isolating the parameters, the effects of slab width, electron density contrast and maximal wave transfer are studied individually. It?s demonstrated that best-fit/global minima, result reported by most XRR studies, don?t necessary reflect the real EDP. By contrast, mapping the merit function in the parametric space can capture much more details. Additionally, the widely accepted concept about the XRR theoretical spatial resolution (pi/q_{max}) as well the using Patterson function are brought to test. In the perspective of XRR data analysis, this chapter puts forward general rules to design and optimize XRR experiments. It also demonstrates how susceptible the fitting result will be if it?s not done carefully. In Chapter 3, the interface between hydrophobic OTS film and several solvents is studied with XRR in a transmission-cell setup. The solvents, from water, acetone, to alcohol (methanol, ethanol, 1-propanol), to alkane (pentane, hexane and heptane), vary significantly in terms of polarity and hydrogen bonding. However, the XRR data from different solvents are subtle. The methods and principles elicited in

  14. 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.

  15. 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.

  16. RefleX: X-ray absorption and reflection in active galactic nuclei for arbitrary geometries

    Science.gov (United States)

    Paltani, S.; Ricci, C.

    2017-11-01

    Reprocessed X-ray radiation carries important information about the structure and physical characteristics of the material surrounding the supermassive black hole (SMBH) in active galactic nuclei (AGN). We report here on a newly developed simulation platform, RefleX, which allows to reproduce absorption and reflection by quasi-arbitrary geometries. We show here the reliability of our approach by comparing the results of our simulations with existing spectral models such as pexrav, MYTorus and BNTorus. RefleX implements both Compton scattering on free electrons and Rayleigh scattering and Compton scattering on bound electrons. We show the effect of bound-electron corrections on a torus geometry simulated like in MYTorus. We release with this paper the RefleX executable, as well as RXTorus, a model that assumes absorption and reflection from a torus with a varying ratio of the minor to major axis of the torus. To allow major flexibility RXTorus is also distributed in three components: absorbed primary emission, scattered radiation and fluorescent lines. RXTorus is provided for different values of the abundance, and with (atomic configuration) or without (free-electron configuration) taking into account Rayleigh scattering and bound electrons. We apply the RXTorus model in both configurations on the XMM-Newton and NuSTAR spectrum of the Compton-thick AGN NGC 424 and find that the models are able to reproduce very well the observations, but that the assumption on the bound or free state of the electrons has significant consequences on the fit parameters. RefleX executable, user manual and example models are available at http://www.astro.unige.ch/reflex. A copy of the RefleX executable is also available at the CDS via anonymous ftp to http://cdsarc.u-strasbg.fr (http://130.79.128.5) or via http://cdsarc.u-strasbg.fr/viz-bin/qcat?J/A+A/607/A31

  17. Nustar and Suzaku X-Ray Spectroscopy Of Ngc 4151: Evidence For Reflection From The Inner Accretion Disk

    DEFF Research Database (Denmark)

    Keck, M. L.; Brenneman, L. W.; Ballantyne, D. R.

    2015-01-01

    We present X-ray timing and spectral analyses of simultaneous 150 ks Nuclear Spectroscopic Telescope Array (NuSTAR) and Suzaku X-ray observations of the Seyfert 1.5 galaxy NGC 4151. We disentangle the continuum emission, absorption, and reflection properties of the active galactic nucleus (AGN......) by applying inner accretion disk reflection and absorption-dominated models. With a time-averaged spectral analysis, we find strong evidence for relativistic reflection from the inner accretion disk. We find that relativistic emission arises from a highly ionized inner accretion disk with a steep emissivity...... profile, which suggests an intense, compact illuminating source. We find a preliminary, near-maximal black hole spin accounting for statistical and systematic modeling errors. We find a relatively moderate reflection fraction with respect to predictions for the lamp post geometry, in which...

  18. An ultrahigh-vacuum goniometer for in situ soft X-ray standing-wave analysis of semiconductor surfaces.

    Science.gov (United States)

    Sugiyama, M; Maeyama, S

    1998-05-01

    An ultrahigh-vacuum goniometer was developed for in situ X-ray standing-wave (XSW) analysis of semiconductor surfaces prepared by molecular-beam epitaxy (MBE). Although two ultrahigh-vacuum motors for chi and phi rotating axes are inside the analysis chamber, low-energy photoelectrons can still be collected as the magnetic field is sufficiently suppressed by using metal shields. Furthermore, the sample can be annealed at temperatures higher than 870 K on the goniometer in the analysis chamber. This goniometer is used at beamline 1A (BL-1A) at the Photon Factory, where both monochromated soft X-rays and UV radiation are available. This analysis system was shown to be suitable not only for in situ soft-XSW and X-ray absorption near-edge structure (XANES) studies but also for synchrotron radiation photoelectron spectroscopy (SRPES) studies. The annealing effects on an S-adsorbed GaAs(001) surface could be studied by SRPES, XANES and XSW using this new goniometer.

  19. In situ microfluidic dialysis for biological small-angle X-ray scattering

    DEFF Research Database (Denmark)

    Skou, Magda; Skou, Soren; Jensen, Thomas Glasdam

    2014-01-01

    for simultaneous SAXS and ultraviolet absorption measurements during protein dialysis, integrated directly on a SAXS beamline. Microfluidic dialysis can be used for monitoring structural changes in response to buffer exchange or, as demonstrated, protein concentration. By collecting X-ray data during...

  20. In situ study of the Porticello Bronzes by portable X-ray fluorescence and laser-induced breakdown spectroscopy

    Science.gov (United States)

    Ferretti, M.; Cristoforetti, G.; Legnaioli, S.; Palleschi, V.; Salvetti, A.; Tognoni, E.; Console, E.; Palaia, P.

    2007-12-01

    This paper reports the results of a measurement campaign performed at the National Museum of Magna Grecia in Reggio Calabria (Italy). Portable X-Ray Fluorescence (XRF) and Laser-Induced Breakdown Spectroscopy (LIBS) instrumentation allowed in situ analysis of several bronze pieces belonging to the group of the so-called Porticello Bronzes. The find occurred at sea, off the village of Porticello (Reggio Calabria) in 1969 and consists of a number of fragments, including a bearded head, pertaining to at least two statues. The use of X-Ray Fluorescence and Laser-Induced Breakdown Spectroscopy techniques allowed for a classification of the fragments according to their elemental composition. The fragments appear to belong to at least two different statues; although, in general, the compositional classification agrees well with the stylistic analysis of the fragments, significant improvements with respect to previous achievements emerge from the joint results of the two techniques used.

  1. In situ study of the Porticello Bronzes by portable X-ray fluorescence and laser-induced breakdown spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Ferretti, M. [Istituto per le Tecnologie Applicate ai Beni Culturali, Via Salaria, km 29.300, c.p.10, 00016 Monterotondo St. - Roma (Italy); Cristoforetti, G.; Legnaioli, S. [Applied Laser Spectroscopy Laboratory, Istituto per i Processi Chimico Fisici del CNR, Area di Ricerca di Pisa, Via G.Moruzzi, 1-56124 Pisa (Italy); Palleschi, V. [Applied Laser Spectroscopy Laboratory, Istituto per i Processi Chimico Fisici del CNR, Area di Ricerca di Pisa, Via G.Moruzzi, 1-56124 Pisa (Italy); Salvetti, A.; Tognoni, E. [Applied Laser Spectroscopy Laboratory, Istituto per i Processi Chimico Fisici del CNR, Area di Ricerca di Pisa, Via G.Moruzzi, 1-56124 Pisa (Italy); Console, E. [T.E.A. s.a.s., Via Luigi Pascali, 23/25-88100 Catanzaro (Italy)], E-mail: elena@teacz.191.it; Palaia, P. [T.E.A. s.a.s., Via Luigi Pascali, 23/25-88100 Catanzaro (Italy)

    2007-12-15

    This paper reports the results of a measurement campaign performed at the National Museum of Magna Grecia in Reggio Calabria (Italy). Portable X-Ray Fluorescence (XRF) and Laser-Induced Breakdown Spectroscopy (LIBS) instrumentation allowed in situ analysis of several bronze pieces belonging to the group of the so-called Porticello Bronzes. The find occurred at sea, off the village of Porticello (Reggio Calabria) in 1969 and consists of a number of fragments, including a bearded head, pertaining to at least two statues. The use of X-Ray Fluorescence and Laser-Induced Breakdown Spectroscopy techniques allowed for a classification of the fragments according to their elemental composition. The fragments appear to belong to at least two different statues; although, in general, the compositional classification agrees well with the stylistic analysis of the fragments, significant improvements with respect to previous achievements emerge from the joint results of the two techniques used.

  2. X-Ray Polarimetry

    OpenAIRE

    Kaaret, Philip

    2014-01-01

    We review the basic principles of X-ray polarimetry and current detector technologies based on the photoelectric effect, Bragg reflection, and Compton scattering. Recent technological advances in high-spatial-resolution gas-filled X-ray detectors have enabled efficient polarimeters exploiting the photoelectric effect that hold great scientific promise for X-ray polarimetry in the 2-10 keV band. Advances in the fabrication of multilayer optics have made feasible the construction of broad-band ...

  3. A novel heavy-atom label for side-specific peptide iodination: synthesis, membrane incorporation and X-ray reflectivity.

    Science.gov (United States)

    Schneggenburger, Philipp E; Beerlink, André; Worbs, Brigitte; Salditt, Tim; Diederichsen, Ulf

    2009-07-13

    Structural parameters, such as conformation, orientation and penetration depth of membrane-bound peptides and proteins that may function as channels, pores or biocatalysts, are of persistent interest and have to be probed in the native fluid state of a membrane. X-ray scattering in combination with heavy-atom labeling is a powerful and highly appropriate method to reveal the position of a certain amino acid residue within a lipid bilayer with respect to the membrane normal axis up to a resolution of several Angstrøm. Herein, we report the synthesis of a new iodine-labeled amino acid building block. This building block is intended for peptide incorporation to provide high intensities for electron density difference analysis of X-ray reflectivity data and improve the labeling potential for the lipid bilayer head-group and water region. The novel building block as well as the commercially available non-iodinated analogue, required for X-ray scattering, was implemented in a transmembrane peptide motif via manual solid-phase peptide synthesis (SPPS) following the fluorenylmethyloxycarbonyl (Fmoc)-strategy. The derived peptides were reconstituted in lipid vesicles as well as in highly aligned multilamellar lipid stacks and investigated via circular dichroism (CD) and X-ray reflectivity. Thereby, it has been revealed that the bulky iodine probe neither causes conformational change of the peptide structure nor lamellar disordering of the membrane complexes.

  4. The effect of surface texture on total reflection of neutrons and X-rays from modified interfaces

    DEFF Research Database (Denmark)

    Goldar, A.; Roser, S.J.; Hughes, A.

    2002-01-01

    X-ray and neutron scattering from macroscopically rough surfaces and interfaces is considered and a new method of analysis based on the variation of the shape of the total reflection edge in the reflectivity profile is proposed. It was shown that in the limit that the correlation length...... and the height of the surface roughness are larger than the wavelength (at least 100 times bigger) of the incoming beam, the total reflection edge in the reflection profile becomes rounded. This technique allows direct analysis of the variation of the reflectivity pro le in terms of the structure of the surface...

  5. Determination of trace elements in freshwater rotifers and ciliates by total reflection X-ray fluorescence spectrometry

    Science.gov (United States)

    Woelfl, S.; Óvári, M.; Nimptsch, J.; Neu, T. R.; Mages, M.

    2016-02-01

    Element determination in plankton is important for the assessment of metal contamination of aquatic environments. Until recently, it has been difficult to determine elemental content in rotifers or ciliates derived from natural plankton samples because of the difficulty in handling and separation of these fragile organisms. The aim of this study was to evaluate methods for separation of rotifers and large ciliates from natural plankton samples (μg range dry weight) and subsequent analysis of their elemental content using total-reflection X-ray fluorescence spectrometry (TXRF). Plankton samples were collected from different aquatic environments (three lakes, one river) in Chile, Argentina and Hungary. From one to eighty specimens of five rotifer species (Brachionus calyciflorus, Brachionus falcatus, Asplanchna sieboldii, Asplanchna sp., Philodina sp.) and four to twelve specimens of one large ciliate (Stentor amethystinus) were prepared according to the dry method originally developed for microcrustaceans, and analysed by TRXF following in situ microdigestion. Our results demonstrated that it possible to process these small and fragile organisms (individual dry mass: 0.17-9.39 μg ind- 1) via careful washing and preparation procedures. We found species-dependent differences of the element mass fractions for some of the elements studied (Cr, Mn, Fe, Ni, Cu, Zn, As, Pb), especially for Cu, Fe and Mn. One large rotifer species (A. sieboldii) also showed a negative correlation between individual dry weight and the element content for Pb, Ni and Cr. We conclude that our application of the in situ microdigestion-TRXF method is suitable even for rotifers and ciliates, greatly expanding the possibilities for use of plankton in biomonitoring of metal contamination in aquatic environments.

  6. Reflectivity around the gold L-edges of X-ray reector of the soft X-ray telescope onboard ASTRO-H

    DEFF Research Database (Denmark)

    Maeda, Yoshitomo; Kikuchi, Naomichi; Kurashima, Sho

    2017-01-01

    We report the atomic scattering factor in the 11.2-15.4 keV for the ASTRO-H Soft X-ray Telescope (SXT)9 obtained in the ground based measurements. The large effective area of the SXT covers above 10 keV. In fact, the flight data show the spectra of the celestical objects in the hard X-ray band. I...

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

    NARCIS (Netherlands)

    Mesu, J. Gerbrand; Beale, Andrew M.|info:eu-repo/dai/nl/325802068; de Groot, Frank M. F.|info:eu-repo/dai/nl/08747610X; Weckhuysen, Bert M.|info:eu-repo/dai/nl/285484397

    2006-01-01

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

  8. In situ analyses of Ag speciation in tissues of cucumber and wheat using synchrotron-based X-ray absorption spectroscopy

    Data.gov (United States)

    U.S. Environmental Protection Agency — In situ analyses of Ag speciation in tissues of cucumber and wheat using synchrotron-based X-ray absorption spectroscopy showing spectral fitting and linear...

  9. Evaluation of the soft x-ray reflectivity of micropore optics using anisotropic wet etching of silicon wafers.

    Science.gov (United States)

    Mitsuishi, Ikuyuki; Ezoe, Yuichiro; Koshiishi, Masaki; Mita, Makoto; Maeda, Yoshitomo; Yamasaki, Noriko Y; Mitsuda, Kazuhisa; Shirata, Takayuki; Hayashi, Takayuki; Takano, Takayuki; Maeda, Ryutaro

    2010-02-20

    The x-ray reflectivity of an ultralightweight and low-cost x-ray optic using anisotropic wet etching of Si (110) wafers is evaluated at two energies, C K(alpha)0.28 keV and Al K(alpha)1.49 keV. The obtained reflectivities at both energies are not represented by a simple planar mirror model considering surface roughness. Hence, an geometrical occultation effect due to step structures upon the etched mirror surface is taken into account. Then, the reflectivities are represented by the theoretical model. The estimated surface roughness at C K(alpha) (approximately 6 nm rms) is significantly larger than approximately 1 nm at Al K(alpha). This can be explained by different coherent lengths at two energies.

  10. A Next-Generation Hard X-Ray Nanoprobe Beamline for In Situ Studies of Energy Materials and Devices

    Energy Technology Data Exchange (ETDEWEB)

    Maser, Jong [Argonne National Lab. (ANL), Argonne, IL (United States); Lai, Barry [Argonne National Lab. (ANL), Argonne, IL (United States); Buonassisi, Toni [Massachusetts Inst. of Technology (MIT), Cambridge, MA (United States); Cai, Zhonghou [Argonne National Lab. (ANL), Argonne, IL (United States); Chen, Si [Argonne National Lab. (ANL), Argonne, IL (United States); Finney, Lydia [Argonne National Lab. (ANL), Argonne, IL (United States); Gleber, Sophie-Charlotte [Argonne National Lab. (ANL), Argonne, IL (United States); Jacobsen, Chris [Argonne National Lab. (ANL), Argonne, IL (United States); Preissner, Curt [Argonne National Lab. (ANL), Argonne, IL (United States); Roehrig, Chris [Argonne National Lab. (ANL), Argonne, IL (United States); Rose, Volker [Argonne National Lab. (ANL), Argonne, IL (United States); Shu, Deming [Argonne National Lab. (ANL), Argonne, IL (United States); Vine, David [Argonne National Lab. (ANL), Argonne, IL (United States); Vogt, Stefan [Argonne National Lab. (ANL), Argonne, IL (United States)

    2013-08-20

    The Advanced Photon Source is developing a suite of new X-ray beamlines to study materials and devices across many length scales and under real conditions. One of the flagship beamlines of the APS upgrade is the In Situ Nanoprobe (ISN) beamline, which will provide in situ and operando characterization of advanced energy materials and devices under varying temperatures, gas ambients, and applied fields, at previously unavailable spatial resolution and throughput. Examples of materials systems include inorganic and organic photovoltaic systems, advanced battery systems, fuel cell components, nanoelectronic devices, advanced building materials and other scientifically and technologically relevant systems. To characterize these systems at very high spatial resolution and trace sensitivity, the ISN will use both nanofocusing mirrors and diffractive optics to achieve spots sizes as small as 20 nm. Nanofocusing mirrors in Kirkpatrick–Baez geometry will provide several orders of magnitude increase in photon flux at a spatial resolution of 50 nm. Diffractive optics such as zone plates and/or multilayer Laue lenses will provide a highest spatial resolution of 20 nm. Coherent diffraction methods will be used to study even small specimen features with sub-10 nm relevant length scale. A high-throughput data acquisition system will be employed to significantly increase operations efficiency and usability of the instrument. The ISN will provide full spectroscopy capabilities to study the chemical state of most materials in the periodic table, and enable X-ray fluorescence tomography. In situ electrical characterization will enable operando studies of energy and electronic devices such as photovoltaic systems and batteries. We also describe the optical concept for the ISN beamline, the technical design, and the approach for enabling a broad variety of in situ studies. Furthermore, we discuss the application of hard X-ray microscopy to study defects in multi-crystalline solar

  11. In-situ high-P, T X-ray microtomographic imaging during large deformation

    DEFF Research Database (Denmark)

    Wang, Y; Lesher, Charles

    2011-01-01

    We have examined the microstructural evolution of a two-phase composite (olivine + Fe-Ni-S) during large shear deformation, using a newly developed high-pressure X-ray tomography microscope. Two samples were examined: a load-bearing framework–type texture, where the alloy phase (Fe-Ni-S) was pres......We have examined the microstructural evolution of a two-phase composite (olivine + Fe-Ni-S) during large shear deformation, using a newly developed high-pressure X-ray tomography microscope. Two samples were examined: a load-bearing framework–type texture, where the alloy phase (Fe...... deformation at temperatures up to 800 K. Shear strains were introduced by twisting the samples at high pressure and high temperature. At each imposed shear strain, samples were cooled to ambient temperature and tomographic images collected. The three-dimensional tomographic images were analyzed for textural...

  12. Determination of observable depth of dislocations in 4H-SiC by X-ray topography in back reflection

    Science.gov (United States)

    Ishiji, Kotaro; Kawado, Seiji; Hirai, Yasuharu; Nagamachi, Shinji

    2017-10-01

    We performed X-ray topography using the asymmetric \\bar{1}\\bar{1}28 back-reflection by changing the incident X-ray energy (E) in order to evaluate the observable depth (t obs) of dislocations in 4H-SiC(0001) wafers with a 4° off-axis angle toward the [11\\bar{2}0]-direction. Since the incident angle (ω) of the X-rays satisfying the Bragg condition changed along with E, the observable length of the straight segment of the basal plane dislocation (BPD) on the X-ray topographs also changed. The t obs values were determined from the observable length of the straight BPD segment, and consequently, plots of t obs versus E, and t obs versus ω were obtained. We discussed the relationships between t obs and the absorption depth (t μ), between t obs and the extinction depth (t Λ), and between t obs and t Λ/t μ as criteria of the dislocation visibility, and we found that the plot of t obs versus t μ was described as t obs ∼ 0.75t μ with good linearity.

  13. Structure of synthetic transmembrane lipid membranes at the solid/liquid interface studied by specular X-ray reflectivity.

    Science.gov (United States)

    Schubert, Thomas; Seitz, Peter C; Schneck, Emanuel; Nakamura, Makoto; Shibakami, Motonari; Funari, Sergio S; Konovalov, Oleg; Tanaka, Motomu

    2008-08-14

    We fabricated a new class of supported membranes based on monolayers of artificial bola (transmembrane) lipids. The lipids used in this study are symmetric bola lipids with two phosphocholine head groups, which resemble natural archaea lipids. To prevent bending of the hydrocarbon chains, stiff triple bonds are inserted in the middle of the hydrocarbon cores. The formation of homogeneous "monolayers" of transmembrane lipids over macroscopic areas can be monitored with fluorescence microscopy. Structures of such supported monolayers in bulk water were characterized with specular X-ray reflectivity using high energy X-ray radiation, which guarantees a high transmission through bulk water. Here, the vertical structure of single monolayers could be resolved from reconstructed electron density profiles. To verify the structural model suggested by the specular reflectivity, we also performed small- and wide-angle X-ray scattering of transmembrane lipid suspensions. The wide-angle patterns reflect a distorted chain-chain correlation, while the small-angle scattering allowed us to model an electron density profile which is consistent with the profile calculated from specular reflectivity.

  14. Enhancement of soft X-ray reflectivity and interface stability in nitridated Pd/Y multilayer mirrors.

    Science.gov (United States)

    Xu, Dechao; Huang, Qiushi; Wang, Yiwen; Li, Pin; Wen, Mingwu; Jonnard, Philippe; Giglia, Angelo; Kozhevnikov, Igor V; Wang, Kun; Zhang, Zhong; Wang, Zhanshan

    2015-12-28

    Pd/Y multilayer mirrors operating in the soft X-ray region are characterized by a high theoretical reflectance, reaching 65% at normal incidence in the 8-12 nm wavelength range. However, a severe intermixing of neighboring Pd and Y layers results in an almost total disappearance of the interfaces inside the multilayer structures fabricated by direct current magnetron sputtering and thus a dramatic reflectivity decrease. Based on grazing incidence X-ray reflectometry and X-ray photoelectron spectroscopy, we demonstrate that the stability of the interfaces in Pd/Y multilayer structures can be essentially improved by adding a small amount of nitrogen (4-8%) to the working gas (Ar). High resolution transmission electron microscopy shows that the interlayer width is only 0.9 nm and 0.6 nm for Y(N)-on-Pd(N) and Pd(N)-on-Y(N) interfaces, respectively. A well-defined crystalline texture of YN (200) is observed on the electron diffraction pattern. As a result, the measured reflectance of the Pd(N)/Y(N) multilayer achieves 30% at λ = 9.3 nm. The peak reflectivity value is limited by the remaining interlayers and the formation of the YN compound inside the yttrium layers, resulting in an increased absorption.

  15. Amorphous iron-(hydr) oxide networks at liquid/vapor interfaces: in situ X-ray scattering and spectroscopy studies.

    Science.gov (United States)

    Wang, Wenjie; Pleasants, Jacob; Bu, Wei; Park, Rebecca Y; Kuzmenko, Ivan; Vaknin, David

    2012-10-15

    Surface sensitive X-ray reflectivity (XR), fluorescence (XF), and grazing incidence X-ray diffraction (GIXD) experiments were conducted to determine the accumulation of ferric iron Fe (III) or ferrous iron Fe (II) under dihexadecyl phosphate (DHDP) or arachidic acid (AA) Langmuir monolayers at liquid/vapor interfaces. Analysis of the X-ray reflectivity and fluorescence data of monolayers on the aqueous subphases containing FeCl(3) indicates remarkably high levels of surface-bound Fe (III) in number of Fe(3+) ions per molecule (DHDP or AA) that exceed the amount necessary to neutralize a hypothetically completely deprotonated monolayer (DHDP or AA). These results suggest that nano-scale iron (hydr) oxide complexes (oxides, hydroxides or oxyhydroxides) bind to the headgroups and effectively overcompensate the maximum possible charges at the interface. The lack of evidence of in-plane ordering in GIXD measurements and strong effects on the surface-pressure versus molecular area isotherms indicate that an amorphous network of iron (hydr) oxide complexes contiguous to the headgroups is formed. Similar experiments with FeCl(2) generally resulted with the oxidation of Fe (II)-Fe (III) which consequently leads to ferric Fe (III) complexes binding albeit with less iron at the interface. Controlling the oxidation of Fe (II) changes the nature and amount of binding significantly. The implications to biomineralization of iron (hydr) oxides are briefly discussed. Copyright © 2012 Elsevier Inc. All rights reserved.

  16. Amorphous iron-(hydr) oxide networks at liquid/vapor interfaces: In situ X-ray scattering and spectroscopy studies

    Energy Technology Data Exchange (ETDEWEB)

    Wang, W.; Pleasants, J.; Bu, W.; Park, R.Y.; Kuzmenko, I.; Vaknin, D.

    2012-06-23

    Surface sensitive X-ray reflectivity (XR), fluorescence (XF), and grazing incidence X-ray diffraction (GIXD) experiments were conducted to determine the accumulation of ferric iron Fe (III) or ferrous iron Fe (II) under dihexadecyl phosphate (DHDP) or arachidic acid (AA) Langmuir monolayers at liquid/vapor interfaces. Analysis of the X-ray reflectivity and fluorescence data of monolayers on the aqueous subphases containing FeCl3 indicates remarkably high levels of surface-bound Fe (III) in number of Fe3þ ions per molecule (DHDP or AA) that exceed the amount necessary to neutralize a hypothetically completely deprotonated monolayer (DHDP or AA). These results suggest that nano-scale iron (hydr) oxide complexes (oxides, hydroxides or oxyhydroxides) bind to the headgroups and effectively overcompensate the maximum possible charges at the interface. The lack of evidence of in-plane ordering in GIXD measurements and strong effects on the surface-pressure versus molecular area isotherms indicate that an amorphous network of iron (hydr) oxide complexes contiguous to the headgroups is formed. Similar experiments with FeCl2 generally resulted with the oxidation of Fe (II)–Fe (III) which consequently leads to ferric Fe (III) complexes binding albeit with less iron at the interface. Controlling the oxidation of Fe (II) changes the nature and amount of binding significantly. The implications to biomineralization of iron (hydr) oxides are briefly discussed.

  17. Differentiation of Deformation Modes in Nanocrystalline Pd Films Inferred from Peak Asymmetry Evolution Using In Situ X-Ray Diffraction

    Science.gov (United States)

    Lohmiller, Jochen; Baumbusch, Rudolf; Kraft, Oliver; Gruber, Patric A.

    2013-02-01

    Synchrotron-based in situ tensile testing was used to study the dominant deformation mechanisms of nanocrystalline Pd thin films on a compliant substrate. An x-ray diffraction peak profile analysis reveals an (hkl) independent deformation induced peak asymmetry. It is argued that the asymmetry is caused by a broad distribution of elastic strains among individual grains and the complexity of accommodation processes. The reversal of peak asymmetry manifests the transition from heterogeneous microplasticity to dislocation-based macroplasticity. Independently, stress-driven grain boundary migration is active.

  18. Ultra-fast in-situ X-ray studies of evolving columnar dendrites in solidifying steel weld pools

    OpenAIRE

    Mirihanage, W.U.; Di Michiel, M.; Mathiesen, R.H.

    2015-01-01

    High-brilliance polychromatic synchrotron radiation has been used to conduct in-situ studies of the solidification microstructure evolution during simulated welding. The welding simulations were realized by rapidly fusing ~ 5 mm spot in Fe-Cr-Ni steel. During the solid- liquid-solid phase transformations, a section of the weld pool was placed in an incident 50-150 keV polychromatic synchrotron X-ray beam, in a near-horizontal position at a very low inclination angle. Multiple high-resolution ...

  19. In-situ study of the growth of CuO nanowires by energy dispersive X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Srivastava, Himanshu; Ganguli, Tapas; Deb, S. K. [Indus Synchrotrons Utilization Division, Raja Ramanna Centre for Advanced technology, Indore-452013 (India); Sant, Tushar; Poswal, Himanshu; Sharma, S. M. [High Pressure and Synchrotron Physics Division, Bhabha Atomic Research Centre, Mumbai (India)

    2013-02-05

    Growth of CuO nanowires by annealing method has been studied in-situ by grazing incidence Energy Dispersive X-ray Diffraction (EDXRD) technique on Indus-2. It was observed that Cu slowly oxidized to Cu{sub 2}O and finally to CuO. The data was taken as a function of time at two annealing temperatures 500 Degree-Sign C where nanowires form and 300 Degree-Sign C where nanowires don't form. We found that the strain in the CuO layer may be a principal factor for the spontaneous growth of nanowires in annealing method.

  20. Strength of shock-loaded single-crystal tantalum [100] determined using in situ broadband x-ray Laue diffraction.

    Science.gov (United States)

    Comley, A J; Maddox, B R; Rudd, R E; Prisbrey, S T; Hawreliak, J A; Orlikowski, D A; Peterson, S C; Satcher, J H; Elsholz, A J; Park, H-S; Remington, B A; Bazin, N; Foster, J M; Graham, P; Park, N; Rosen, P A; Rothman, S R; Higginbotham, A; Suggit, M; Wark, J S

    2013-03-15

    The strength of shock-loaded single crystal tantalum [100] has been experimentally determined using in situ broadband x-ray Laue diffraction to measure the strain state of the compressed crystal, and elastic constants calculated from first principles. The inferred strength reaches 35 GPa at a shock pressure of 181 GPa and is in excellent agreement with a multiscale strength model [N. R. Barton et al., J. Appl. Phys. 109, 073501 (2011)], which employs a hierarchy of simulation methods over a range of length scales to calculate strength from first principles.

  1. Combination of grazing incidence x-ray fluorescence with x-ray reflectivity in one table-top spectrometer for improved characterization of thin layer and implants on/in silicon wafers.

    Science.gov (United States)

    Ingerle, D; Schiebl, M; Streli, C; Wobrauschek, P

    2014-08-01

    As Grazing Incidence X-ray Fluorescence (GIXRF) analysis does not provide unambiguous results for the characterization of nanometre layers as well as nanometre depth profiles of implants in silicon wafers by its own, the approach of providing additional information using the signal from X-ray Reflectivity (XRR) was tested. As GIXRF already uses an X-ray beam impinging under grazing incidence and the variation of the angle of incidence, a GIXRF spectrometer was adapted with an XRR unit to obtain data from the angle dependent fluorescence radiation as well as data from the reflected beam. A θ-2θ goniometer was simulated by combining a translation and tilt movement of a Silicon Drift detector, which allows detecting the reflected beam over 5 orders of magnitude. HfO2 layers as well as As implants in Silicon wafers in the nanometre range were characterized using this new setup. A just recently published combined evaluation approach was used for data evaluation.

  2. Pigment particles analysis with a total reflection X-ray fluorescence spectrometer: study of influence of instrumental parameters

    Energy Technology Data Exchange (ETDEWEB)

    Coccato, Alessia; Vandenabeele, Peter [Ghent University, Department of Archaeology, Ghent (Belgium); Vekemans, Bart; Vincze, Laszlo; Moens, Luc [Ghent University, Department of Analytical Chemistry, Ghent (Belgium)

    2016-12-15

    Total reflection X-ray fluorescence (TXRF) analysis is an excellent tool to determine major, minor and trace elements in minuscule amounts of samples, making this technique very suitable for pigment analysis. Collecting minuscule amounts of pigment material from precious works of art by means of a cotton swab is a well-accepted sampling method, but poses specific challenges when TXRF is to be used for the characterization of the unknown material. (orig.)

  3. Insight on the silver catalyst distribution during silicon nanowire array formation: an X-ray reflectivity study.

    Science.gov (United States)

    Kremenak, Jesse W; Arendse, Christopher J; Cummings, Franscious R; Chen, Yiyao; Miceli, Paul F

    2017-12-14

    Although metal-catalysts are commonly used to create nanoscale materials at surfaces, little is quantitatively known or understood about the depth distribution profile of the catalyst during the growth process. Using X-ray reflectivity, we report the first quantitative investigation, with nanoscale resolution, of the Ag metal-catalyst depth distribution profile during metal-assisted chemical etch (MACE) growth of Si nanowire (SiNW) arrays on Si(100). Given the very low optical reflectivity of these nanowire arrays, specular reflection from these materials in the X-ray region is extremely challenging to measure because it probes interfaces on the nanoscale. Nevertheless, we demonstrate that with suitable investigation, X-ray specular reflection can be measured and utilized to obtain unique structural information about the composition profile of both Ag and Si. The measurements, which also include X-ray diffraction and complementary electron microscopy, reveal that the Ag nanoparticles distribute along the length of the nanowires upon etching with a Ag density that increases towards the etch front. The Ag nanoparticles coarsen with etch time, indicating a high mobility of Ag ions even though we also find that the Ag does not migrate from the SiNW region into the etch bath during etching. The Ag density gradient and the Ag mobility suggest the existence of a strong chemical force that attracts Ag towards the etch front. These results provide unique and important new insight into the growth process for creating SiNWs from wet chemical etching using metal-catalysts.

  4. In situ X-ray investigations of oxygen precipitation in semiconductor silicon; In-situ-Roentgenuntersuchungen der Sauerstoffpraezipitation in Halbleitersilizium

    Energy Technology Data Exchange (ETDEWEB)

    Grillenberger, Hannes

    2011-03-04

    The precipitation of oxygen in Czochralski grown semiconductor silicon is investigated in situ during thermal treatments up to 1000 C with high energy X-rays. All investigations are performed with a focusing Laue diffractometer. The parameters of the diffraction curve are the relative full width at half maximum (rFHWM) and the enhancement of the integral intensity (EII). A readout software has been developed to extract these automatically from the detector image for the measured 220, -220 and 040 Bragg peaks. The sample thickness is set to 15 mm as this enhances the sensitivity of the method and the samples are processed after the strain-field diffraction (SFD) experiments to wafers for an ex situ characterization demanding wafers. Three experimental series with a total of 21 in situ SFD experiments with different thermal treatments have been performed. The slope of the initial temperature ramp is set to 1 K/min in the first and the third series to generate a high precipitate (Bulk Micro Defect, BMD) density. In the second series the slope is chosen as 10 K/min to generate a lower density in the same silicon material. It is shown with all experiments and with preliminary works that the built up of strain during the heat treatment is caused by BMDs during the high temperature period of the treatment. The detection limit of series 1 is found at 7 nm at a density of 10{sup 13}/cm{sup 3}, of series 2 at 40 nm at a density of 2 x 10{sup 8}/cm{sup 3}, and at 8 nm at a density of 4.8 x 10{sup 12}/cm{sup 3} for series 3. The local maximum of the EII at 450 C, which emerges coincident with a local minimum of the rFWHM in series 2 may be caused by thermal donors (TD). With the experiments is shown that SFD operates in the infrared-laser scattering tomography detection range, but also reaches in a region covered only by transmission electron microscopy (TEM) so far. In contrast to these methods SFD is not limited to low temperatures and in situ experiments can be done. Thus

  5. Pressure-induced amorphization of cubic Zr W2 O8 studied in situ and ex situ by synchrotron x-ray diffraction and absorption

    Science.gov (United States)

    Varga, Tamas; Wilkinson, Angus P.; Jupe, Andrew C.; Lind, Cora; Bassett, William A.; Zha, Chang-Sheng

    2005-07-01

    The behavior of cubic ZrW2O8 on compression in a DAC to 7.6GPa was examined in situ by a combination of synchrotron x-ray diffraction and x-ray absorption spectroscopy (XAS). These data were compared with x-ray absorption measurements on an amorphous sample of ZrW2O8 recovered from 7.5GPa in a multianvil apparatus. The in situ diffraction data show the complete formation of orthorhombic ZrW2O8 at low pressure (2.4GPa with completion at <7.6GPa . The corresponding in situ XAS data suggest a continuous evolution of the local tungsten coordination environment on compression after forming the orthorhombic phase, with the average WO bond length increasing, indicating an increase in the average coordination number, and the W LI pre-edge peak decreasing in magnitude, indicating a movement toward tungsten coordination that is closer to centrosymmetric These observations are inconsistent with a model for the amorphization that simply involves a loss of orientational/positional order among existing coordination polyhedra. The XANES data for the amorphous sample recovered from the multianvil apparatus are unlike any of the XANES seen in the in situ measurements, suggesting that the local structure in the glassy material relaxes on decompression. The XANES for the recovered sample are very similar to those for ammonium paratungstate, a material that contains tungsten in a variety of heavily distorted octahedral environments.

  6. Coupling X-Ray Reflectivity and In Silico Binding to Yield Dynamics of Membrane Recognition by Tim1.

    Science.gov (United States)

    Tietjen, Gregory T; Baylon, Javier L; Kerr, Daniel; Gong, Zhiliang; Henderson, J Michael; Heffern, Charles T R; Meron, Mati; Lin, Binhua; Schlossman, Mark L; Adams, Erin J; Tajkhorshid, Emad; Lee, Ka Yee C

    2017-10-03

    The dynamic nature of lipid membranes presents significant challenges with respect to understanding the molecular basis of protein/membrane interactions. Consequently, there is relatively little known about the structural mechanisms by which membrane-binding proteins might distinguish subtle variations in lipid membrane composition and/or structure. We have previously developed a multidisciplinary approach that combines molecular dynamics simulation with interfacial x-ray scattering experiments to produce an atomistic model for phosphatidylserine recognition by the immune receptor Tim4. However, this approach requires a previously determined protein crystal structure in a membrane-bound conformation. Tim1, a Tim4 homolog with distinct differences in both immunological function and sensitivity to membrane composition, was crystalized in a closed-loop conformation that is unlikely to support membrane binding. Here we have used a previously described highly mobile membrane mimetic membrane in combination with a conventional lipid bilayer model to generate a membrane-bound configuration of Tim1 in silico. This refined structure provided a significantly improved fit of experimental x-ray reflectivity data. Moreover, the coupling of the x-ray reflectivity analysis with both highly mobile membrane mimetic membranes and conventional lipid bilayer molecular dynamics simulations yielded a dynamic model of phosphatidylserine membrane recognition by Tim1 with atomic-level detail. In addition to providing, to our knowledge, new insights into the molecular mechanisms that distinguish the various Tim receptors, these results demonstrate that in silico membrane-binding simulations can remove the requirement that the existing crystal structure be in the membrane-bound conformation for effective x-ray reflectivity analysis. Consequently, this refined methodology has the potential for much broader applicability with respect to defining the atomistic details of membrane

  7. X-ray Reflected Spectra from Accretion Disk Models. I. Constant Density Atmospheres

    Science.gov (United States)

    Garcia, Javier; Kallman, Timothy R.

    2009-01-01

    We present new models for illuminated accretion disks, their structure and reprocessed emission. We consider the effects of incident X-rays on the surface of an accretion disk by solving simultaneously the equations of radiative transfer, energy balance and ionization equilibrium over a large range of column densities. We assume plane-parallel geometry and azimuthal symmetry, such that each calculation corresponds to a ring at a given distance from the central object. Our models include recent and complete atomic data for K-shell of the iron and oxygen isonuclear sequences. We examine the effect on the spectrum of fluorescent Ka line emission and absorption in the emitted spectrum. We also explore the dependence of the spectrum on the strength of the incident X-rays and other input parameters, and discuss the importance of Comptonization on the emitted spectrum.

  8. Improved theory of noncomplanar diffraction of X-Rays under specular reflection conditions

    CERN Document Server

    Balyan, M K

    2000-01-01

    In two-wave approximation the equations describing the dynamical diffraction of X-ray spatially modulated waves in ideal and deformed crystals in grazing noncomplanar incidence geometry are obtained. The solutions of obtained equations for diffraction of arbitrary spatially modulated incidence wave in ideal half-infinite crystal are found. As a special case of the obtained solutions, the diffraction of incidence spherical wave under small grazing angle is briefly considered.

  9. Interface characterization of B4C-based multilayers by X-ray grazing-incidence reflectivity and diffuse scattering.

    Science.gov (United States)

    Jiang, Hui; Wang, Zhanshan; Zhu, Jingtao

    2013-05-01

    B4C-based multilayers have important applications for soft to hard X-rays. In this paper, X-ray grazing-incidence reflectivity and diffuse scattering, combining various analysis methods, were used to characterize the structure of B4C-based multilayers including layer thickness, density, interfacial roughness, interdiffusion, correlation length, etc. Quantitative results for W/B4C, Mo/B4C and La/B4C multilayers were compared. W/B4C multilayers show the sharpest interfaces and most stable structures. The roughness replications of La/B4C and Mo/B4C multilayers are not strong, and oxidations and structure expansions are found in the aging process. This work provides guidance for future fabrication and characterization of B4C-based multilayers.

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

    Science.gov (United States)

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

    1997-01-01

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

  11. In situ observation of dynamic electrodeposition processes by soft x-ray fluorescence microspectroscopy and keyhole coherent diffractive imaging

    Science.gov (United States)

    Bozzini, Benedetto; Kourousias, George; Gianoncelli, Alessandra

    2017-03-01

    This paper describes two novel in situ microspectroscopic approaches to the dynamic study of electrodeposition processes: x-ray fluorescence (XRF) mapping with submicrometric space resolution and keyhole coherent diffractive imaging (kCDI) with nanometric lateral resolution. As a case study, we consider the pulse-plating of nanocomposites with polypyrrole matrix and Mn x Co y O z dispersoids, a prospective cathode material for zinc-air batteries. This study is centred on the detailed measurement of the elemental distributions developing in two representative subsequent growth steps, based on the combination of in situ identical-location XRF microspectroscopy—accompanied by soft-x ray absorption microscopy—and kCDI. XRF discloses space and time distributions of the two electrodeposited metals and kCDI on the one hand allows nanometric resolution and on the other hand provides complementary absorption as well as phase contrast modes. The joint information derived from these two microspectroscopies allows measurement of otherwise inaccessible observables that are a prerequisite for electrodeposition modelling and control accounting for dynamic localization processes.

  12. Quantitative study of particle size distribution in an in-situ grown Al–TiB{sub 2} composite by synchrotron X-ray diffraction and electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Tang, Y. [State Key Laboratory of Metal Matrix Composites, Shanghai Jiao Tong University, Shanghai 200240 (China); Chen, Z., E-mail: zhe.chen@sjtu.edu.cn [State Key Laboratory of Metal Matrix Composites, Shanghai Jiao Tong University, Shanghai 200240 (China); Borbély, A. [SMS Materials Center, LGF-CNRS UMR 5307, Ecole des Mines de Saint Etienne, 158, Cours Fauriel, 42023 Saint Etienne (France); Ji, G. [Unité Matériaux et Transformations, CNRS UMR 8207, Université Lille 1, Villeneuve d' Ascq 59655 (France); Zhong, S.Y. [State Key Laboratory of Metal Matrix Composites, Shanghai Jiao Tong University, Shanghai 200240 (China); Schryvers, D. [Electron Microscopy for Materials Science (EMAT), University of Antwerp, Groenenborgerlaan 171, 2020 Antwerp (Belgium); Ji, V. [ICMMO/LEMHE, UMR CNRS 8182, Université Paris-Sud 11, Orsay Cedex 91405, France. (France); Wang, H.W. [State Key Laboratory of Metal Matrix Composites, Shanghai Jiao Tong University, Shanghai 200240 (China)

    2015-04-15

    Synchrotron X-ray diffraction and transmission electron microscopy (TEM) were applied to quantitatively characterize the average particle size and size distribution of free-standing TiB{sub 2} particles and TiB{sub 2} particles in an in-situ grown Al–TiB{sub 2} composite. The detailed evaluations were carried out by X-ray line profile analysis using the restricted moment method and multiple whole profile fitting procedure (MWP). Both numerical methods indicate that the formed TiB{sub 2} particles are well crystallized and free of crystal defects. The average particle size determined from different Bragg reflections by the restricted moment method ranges between 25 and 55 nm, where the smallest particle size is determined using the 110 reflection suggesting the highest lateral-growth velocity of (110) facets. The MWP method has shown that the in-situ grown TiB{sub 2} particles have a very low dislocation density (~ 10{sup 11} m{sup −} {sup 2}) and their size distribution can be described by a log-normal distribution. Good agreement was found between the results obtained from the restricted moment and MWP methods, which was further confirmed by TEM. - Highlights: • Accurate quantitative characterization of in-situ grown T{sub i}B{sub 2} particles has been achieved. • Particle size anisotropy was revealed indicating 110 facets being largest during T{sub i}B{sub 2} growth. • A wide size distribution was observed for T{sub i}B{sub 2} particles with a dominant size smaller than 100 nm.

  13. X-ray micro-beam focusing system for in situ investigation of single nanowire during MBE growth

    Science.gov (United States)

    Hu, Wen; Takahasi, Masamitu; Kozu, Miwa; Nakata, Yuka

    2013-03-01

    A ternary Fresnel zone plate (FZP) has been fabricated and installed at the beamline 11XU of SPring-8, in the aim of in situ studies on the growth of semiconductor nanostructures. The FZP is designed for an X-ray energy of 9.5 keV for the first-order diffraction, which is isolated by an order sorting aperture (OSA) inserted 450 mm after the FZP. The focal length of this FZP is 650 mm. The full width at half maximum of the focused beam profile was estimated to be 1.17 μm (H) × 1.38 μm (V) by the dark-field knife-edge scan. Using this FZP, micro-beam diffraction of an as-grown single InAs NW was carried out to show the feasibility of in situ study during growth.

  14. Ex-situ X-ray computed tomography data for a non-crimp fabric based glass fibre composite under fatigue loading

    Directory of Open Access Journals (Sweden)

    Kristine M. Jespersen

    2017-12-01

    Full Text Available The data published with this article are high resolution X-ray computed tomography (CT data obtained during an ex-situ fatigue test of a coupon test specimen made from a non-crimp fabric based glass fibre composite similar to those used for wind turbine blades. The fatigue test was interrupted four times for X-ray CT examination during the fatigue life of the considered specimen. All the X-ray CT experiments were performed in the region where unidirectional fibre fractures first became visible, and thereby include the damage progression in 3D in this specific region during fatigue loading of the specimen.

  15. Ex-situ X-ray computed tomography data for a non-crimp fabric based glass fibre composite under fatigue loading

    DEFF Research Database (Denmark)

    Jespersen, Kristine Munk; Mikkelsen, Lars Pilgaard

    2017-01-01

    The data published with this article are high resolution X-ray computed tomography (CT) data obtained during an ex-situ fatigue test of a coupon test specimen made from a non-crimp fabric based glass fibre composite similar to those used for wind turbine blades. The fatigue test was interrupted...... four times for X-ray CT examination during the fatigue life of the considered specimen. All the X-ray CT experiments were performed in the region where unidirectional fibre fractures first became visible, and thereby include the damage progression in 3D in this specific region during fatigue loading...

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

    Science.gov (United States)

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

    1999-01-01

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

  17. Anisotropy of x-ray reflectivity: chemical and structural effects on K-shell excitations in hexagonal BN crystal

    CERN Document Server

    Filatova, E O

    2002-01-01

    The experimental investigation of the B and N K-reflection spectra using both s-polarized synchrotron radiation and unpolarized radiation for different crystal orientations with respect to the electric field vector E was carried out. The absorption spectra calculated from the reflection spectra using Kramers-Kronig analysis are presented. A strong orientation dependence of both reflection and absorption spectra is exhibited. Analysis of the orientation dependences of the x-ray reflection and absorption spectra near both edges strongly supports a possibility of tracing the role of each excitation canal in the formation of fine structure. The high sensitivity of the reflection spectra fine structure to the vibronic interaction connected with Jahn-Teller distortions as well to the core-hole relaxation is discussed. A very strong dependence of the absolute values of the reflectivity on planar crystal anisotropy was discovered.

  18. The X-Ray Reflection Spectrum of the Radio-loud Quasar 4C 74.26

    DEFF Research Database (Denmark)

    Lohfink, Anne M.; Fabian, Andrew C.; Ballantyne, David R.

    2017-01-01

    The relativistic jets created by some active galactic nuclei are important agents of AGN feedback. In spite of this, our understanding of what produces these jets is still incomplete. X-ray observations, which can probe the processes operating in the central regions in the immediate vicinity...... of the supermassive black hole, the presumed jet launching point, are potentially particularly valuable in illuminating the jet formation process. Here, we present the hard X-ray NuSTAR observations of the radio-loud quasar 4C 74.26 in a joint analysis with quasi-simultaneous, soft X-ray Swift observations. Our...... spectral analysis reveals a high-energy cutoff of   keV and confirms the presence of ionized reflection in the source. From the average spectrum we detect that the accretion disk is mildly recessed, with an inner radius of Rin = 4-180 Rg. However, no significant evolution of the inner radius is seen during...

  19. The X-Ray Reflection Spectrum of the Radio-loud Quasar 4C 74.26

    Science.gov (United States)

    Lohfink, Anne M.; Fabian, Andrew C.; Ballantyne, David R.; Boggs, S. E.; Boorman, Peter; Christensen, F. E.; Craig, W. W.; Farrah, Duncan; García, Javier; Hailey, C. J.; Harrison, F. A.; Ricci, Claudio; Stern, Daniel; Zhang, W. W.

    2017-06-01

    The relativistic jets created by some active galactic nuclei are important agents of AGN feedback. In spite of this, our understanding of what produces these jets is still incomplete. X-ray observations, which can probe the processes operating in the central regions in the immediate vicinity of the supermassive black hole, the presumed jet launching point, are potentially particularly valuable in illuminating the jet formation process. Here, we present the hard X-ray NuSTAR observations of the radio-loud quasar 4C 74.26 in a joint analysis with quasi-simultaneous, soft X-ray Swift observations. Our spectral analysis reveals a high-energy cutoff of {183}-35+51 keV and confirms the presence of ionized reflection in the source. From the average spectrum we detect that the accretion disk is mildly recessed, with an inner radius of R in = 4-180 R g. However, no significant evolution of the inner radius is seen during the three months covered by our NuSTAR campaign. This lack of variation could mean that the jet formation in this radio-loud quasar differs from what is observed in broad-line radio galaxies.

  20. NUSTAR and Suzaku x-ray spectroscopy of NGC 4151: Evidence for reflection from the inner accretion disk

    Energy Technology Data Exchange (ETDEWEB)

    Keck, M. L.; Brenneman, L. W.; Ballantyne, D. R.; Bauer, F.; Boggs, S. E.; Christensen, F. E.; Craig, W. W.; Dauser, T.; Elvis, M.; Fabian, A. C.; Fuerst, F.; García, J.; Grefenstette, B. W.; Hailey, C. J.; Harrison, F. A.; Madejski, G.; Marinucci, A.; Matt, G.; Reynolds, C. S.; Stern, D.; Walton, D. J.; Zoghbi, A.

    2015-06-15

    We present X-ray timing and spectral analyses of simultaneous 150 ks Nuclear Spectroscopic Telescope Array (NuSTAR) and Suzaku X-ray observations of the Seyfert 1.5 galaxy NGC 4151. We disentangle the continuum emission, absorption, and reflection properties of the active galactic nucleus (AGN) by applying inner accretion disk reflection and absorption-dominated models. With a time-averaged spectral analysis, we find strong evidence for relativistic reflection from the inner accretion disk. We find that relativistic emission arises from a highly ionized inner accretion disk with a steep emissivity profile, which suggests an intense, compact illuminating source. We find a preliminary, near-maximal black hole spin $a\\gt 0.9$ accounting for statistical and systematic modeling errors. We find a relatively moderate reflection fraction with respect to predictions for the lamp post geometry, in which the illuminating corona is modeled as a point source. Through a time-resolved spectral analysis, we find that modest coronal and inner disk reflection (IDR) flux variation drives the spectral variability during the observations. We discuss various physical scenarios for the IDR model and we find that a compact corona is consistent with the observed features.

  1. MapX An In Situ, Full-frame X-Ray Spectroscopic Imager for Planetary Science and Astrobiology

    Science.gov (United States)

    Blake, David; Sarrazin, Philippe; Thompson, Kathleen; Bristow, Thomas

    2017-01-01

    Microbial life exploits micron-scale disequilibria at boundaries where valence, chemical potential, pH, Eh, etc. vary on a length scale commensurate with the organisms - 10's to 100's of microns. The detection of accumulations of the biogenic elements C,N,O,P,S at appropriate concentrations on or in a mineral/ice substrate would constitute permissive evidence of extant life, but context is also required. Does the putative biosignature exist under habitable conditions? Under what conditions of P, T, and chemical potential was the host mineralogy formed? MapX is an in situ robotic spacecraft instrument that images the biogenic elements C, N, O, P, S, as well as the cations of the rock-forming minerals (Na, Mg, Al, Si, K, Ca, Ti, Cr, Mn, Fe) and important anions such as Cl, Fl. MapX provides element maps with less than or equal to100 microns resolution over a 2.5 cm X 2.5 cm area, as well as quantitative XRF spectra from ground- or instrument-selected Regions of Interest (ROI). XRF spectra are converted to mineralogies using ground- or instrument-based algorithms. Either X-ray tube or radioisotope sources such as 244Cm (Alpha-particle and gamma- ray fluorescence) can be used. Fluoresced sample Xrays are imaged onto an X-ray sensitive CCD through an X-ray MicroPore Optic (MPO). The MapX design as well as baseline performance requirements for a MapX instrument intended for life detection / identification of habitable environments will be presented.

  2. In situ and ex situ electron microscopy and X-ray diffraction characterization of the evolution of a catalytic system - from synthesis to deactivation

    DEFF Research Database (Denmark)

    Gardini, Diego

    the understanding of the structural properties and mechanisms at the origin of catalytic activity. This thesis presents the potential and uniqueness of ex situ and in situ transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques in the characterization of several supported material systems...... TEM (HRTEM) and electron energy loss spectroscopy (EELS) revealed the degradation of the supported carbide particles probably due to the formation of volatile molybdenum hydroxide species. The activity of silver nanoparticles as catalyst for soot oxidation was studied in operative conditions...

  3. Role of Bi promotion and solvent in platinum-catalyzed alcohol oxidation probed by in situ X-ray absorption and ATR-IR spectroscopy

    DEFF Research Database (Denmark)

    Mondelli, C.; Grunwaldt, Jan-Dierk; Ferri, D.

    2010-01-01

    the catalysts under working conditions using in situ X-ray absorption spectroscopy (XAS) and attenuated total reflection infrared spectroscopy (ATR-IR), aiming at uncovering the roles of the metal promoter and the reaction medium. XAS confirms that Bi is oxidized more easily than Pt, maintaining the catalytic....... This behaviour is not observed in the presence of Bi, whose geometric effect (site blocking) is interpreted as additionally limiting the adsorption of toluene and the premature deactivation of Pt. ATR-IR spectroscopy during CO adsorption on Pt and during reaction indicates that Bi is located rather on extended...... surfaces than on step or kink sites. Side products, CO and benzoate species, appearing during the reaction reveal that the geometric suppression of undesired reactions does not occur to the same extent on Pt-based catalysts as on Pd, suggesting that decarbonylation of the produced aldehyde on Pt may occur...

  4. Microstructures of a Pt/Ni/C multilayer system: an X-ray reflectivity and ion scattering study.

    Science.gov (United States)

    Roy, Sumalay; Bera, S; Dev, B N

    2007-06-01

    Microstructural characterization of a synthetic periodic and graded Pt/Ni/C multilayer system by X-ray reflectivity and ion scattering techniques is presented. The experimental reflectivity data are fitted with a theoretical multi-trilayer model with graded periodicity which increases from substrate to film surface along the surface normal direction. The increase in periodicity is found to be due to a linear increase in C-layer thickness from the bottom to the top, with a change of slope nearly at the middle of the multilayer stack. The thicknesses of Pt and Ni layers, the variation of C-layer thickness with depth, interface roughness of Pt/Ni, Ni/C, C/Pt interfaces are determined from the analysis of the reflectivity data. Rutherford backscattering spectrometry measurements were also made on the same sample. Simulated Rutherford back scattering spectrometry data using the parameters obtained from the analysis of the X-ray reflectivity data agree well with the measured Rutherford backscattering spectrum.

  5. Center for X-Ray Optics, 1992

    Energy Technology Data Exchange (ETDEWEB)

    1993-08-01

    This report discusses the following topics: Center for X-Ray Optics; Soft X-Ray Imaging wit Zone Plate Lenses; Biological X-Ray microscopy; Extreme Ultraviolet Lithography for Nanoelectronic Pattern Transfer; Multilayer Reflective Optics; EUV/Soft X-ray Reflectometer; Photoemission Microscopy with Reflective Optics; Spectroscopy with Soft X-Rays; Hard X-Ray Microprobe; Coronary Angiography; and Atomic Scattering Factors.

  6. The Simultaneous Combination of Phase Contrast Imaging with In Situ X-ray diffraction from Shock Compressed Matter

    Science.gov (United States)

    McBride, Emma Elizabeth; Seiboth, Frank; Cooper, Leora; Frost, Mungo; Goede, Sebastian; Harmand, Marion; Levitan, Abe; McGonegle, David; Miyanishi, Kohei; Ozaki, Norimasa; Roedel, Melanie; Sun, Peihao; Wark, Justin; Hastings, Jerry; Glenzer, Siegfried; Fletcher, Luke

    2017-10-01

    Here, we present the simultaneous combination of phase contrast imaging (PCI) techniques with in situ X-ray diffraction to investigate multiple-wave features in laser-driven shock-compressed germanium. Experiments were conducted at the Matter at Extreme Conditions end station at the LCLS, and measurements were made perpendicular to the shock propagation direction. PCI allows one to take femtosecond snapshots of magnified real-space images of shock waves as they progress though matter. X-ray diffraction perpendicular to the shock propagation direction provides the opportunity to isolate and identify different waves and determine the crystal structure unambiguously. Here, we combine these two powerful techniques simultaneously, by using the same Be lens setup to focus the fundamental beam at 8.2 keV to a size of 1.5 mm on target for PCI and the 3rd harmonic at 24.6 keV to a spot size of 2 um on target for diffraction.

  7. Tuning of colossal dielectric constant in gold-polypyrrole composite nanotubes using in-situ x-ray diffraction techniques

    Directory of Open Access Journals (Sweden)

    Abhisakh Sarma

    2014-09-01

    Full Text Available In-situ x-ray diffraction technique has been used to study the growth process of gold incorporated polypyrrole nanotubes that exhibit colossal dielectric constant due to existence of quasi-one-dimensional charge density wave state. These composite nanotubes were formed within nanopores of a polycarbonate membrane by flowing pyrrole monomer from one side and mixture of ferric chloride and chloroauric acid from other side in a sample cell that allows collection of x-ray data during the reaction. The size of the gold nanoparticle embedded in the walls of the nanotubes was found to be dependent on chloroauric acid concentration for nanowires having diameter more than 100 nm. For lower diameter nanotubes the nanoparticle size become independent of chloroauric acid concentration and depends on the diameter of nanotubes only. The result of this study also shows that for 50 nm gold-polypyrrole composite nanotubes obtained with 5.3 mM chloroauric acid gives colossal dielectric constant of about 107. This value remain almost constant over a frequency range from 1Hz to 106 Hz even at 80 K temperature.

  8. In situ observation of water distribution and behaviour in a polymer electrolyte fuel cell by synchrotron X-ray imaging.

    Science.gov (United States)

    Mukaide, Taihei; Mogi, Satoshi; Yamamoto, Jun; Morita, Akira; Koji, Shinnosuke; Takada, Kazuhiro; Uesugi, Kentaro; Kajiwara, Kentaro; Noma, Takashi

    2008-07-01

    In situ visualization of the distribution and behaviour of water in a polymer electrolyte fuel cell during power generation has been demonstrated using a synchrotron X-ray imaging technique. Images were recorded using a CCD detector combined with a scintillator (Gd(2)O(2)S:Tb) and relay lens system, which were placed at 2.0 m or 2.5 m from the fuel cell. The images were measured continuously before and during power generation, and data on cell performance was recorded. The change of water distribution during power generation was obtained from X-ray images normalized with the initial state of the fuel cell. Compared with other techniques for visualizing the water in fuel cells, this technique enables the water distribution and behaviour in the fuel cell to be visualized during power generation with high spatial resolution. In particular, the effects of the specifications of the gas diffusion layer on the cathode side of the fuel cell on the distribution of water were efficiently identified. This is a very powerful technique for investigating the mechanism of water flow within the fuel cell and the relationship between water behaviour and cell performance.

  9. Aerodynamic levitator for in situ x-ray structure measurements on high temperature and molten nuclear fuel materials

    Energy Technology Data Exchange (ETDEWEB)

    Weber, J. K. R.; Alderman, O. L. G. [Materials Development, Inc., Arlington Heights, Illinois 60004 (United States); Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Tamalonis, A.; Sendelbach, S. [Materials Development, Inc., Arlington Heights, Illinois 60004 (United States); Benmore, C. J. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Hebden, A.; Williamson, M. A. [Nuclear Engineering Division, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

    2016-07-15

    An aerodynamic levitator with carbon dioxide laser beam heating was integrated with a hermetically sealed controlled atmosphere chamber and sample handling mechanism. The system enabled containment of radioactive samples and control of the process atmosphere chemistry. The chamber was typically operated at a pressure of approximately 0.9 bars to ensure containment of the materials being processed. Samples 2.5-3 mm in diameter were levitated in flowing gas to achieve containerless conditions. Levitated samples were heated to temperatures of up to 3500 °C with a partially focused carbon dioxide laser beam. Sample temperature was measured using an optical pyrometer. The sample environment was integrated with a high energy (100 keV) x-ray synchrotron beamline to enable in situ structure measurements to be made on levitated samples as they were heated, melted, and supercooled. The system was controlled from outside the x-ray beamline hutch by using a LabVIEW program. Measurements have been made on hot solid and molten uranium dioxide and binary uranium dioxide-zirconium dioxide compositions.

  10. Tuning of colossal dielectric constant in gold-polypyrrole composite nanotubes using in-situ x-ray diffraction techniques

    Energy Technology Data Exchange (ETDEWEB)

    Sarma, Abhisakh; Sanyal, Milan K., E-mail: milank.sanyal@saha.ac.in [Saha Institute of Nuclear Physics, 1/AF Bidhannagar, Kolkata 700 064 (India)

    2014-09-15

    In-situ x-ray diffraction technique has been used to study the growth process of gold incorporated polypyrrole nanotubes that exhibit colossal dielectric constant due to existence of quasi-one-dimensional charge density wave state. These composite nanotubes were formed within nanopores of a polycarbonate membrane by flowing pyrrole monomer from one side and mixture of ferric chloride and chloroauric acid from other side in a sample cell that allows collection of x-ray data during the reaction. The size of the gold nanoparticle embedded in the walls of the nanotubes was found to be dependent on chloroauric acid concentration for nanowires having diameter more than 100 nm. For lower diameter nanotubes the nanoparticle size become independent of chloroauric acid concentration and depends on the diameter of nanotubes only. The result of this study also shows that for 50 nm gold-polypyrrole composite nanotubes obtained with 5.3 mM chloroauric acid gives colossal dielectric constant of about 10{sup 7}. This value remain almost constant over a frequency range from 1Hz to 10{sup 6} Hz even at 80 K temperature.

  11. Aerodynamic levitator for in situ x-ray structure measurements on high temperature and molten nuclear fuel materials.

    Science.gov (United States)

    Weber, J K R; Tamalonis, A; Benmore, C J; Alderman, O L G; Sendelbach, S; Hebden, A; Williamson, M A

    2016-07-01

    An aerodynamic levitator with carbon dioxide laser beam heating was integrated with a hermetically sealed controlled atmosphere chamber and sample handling mechanism. The system enabled containment of radioactive samples and control of the process atmosphere chemistry. The chamber was typically operated at a pressure of approximately 0.9 bars to ensure containment of the materials being processed. Samples 2.5-3 mm in diameter were levitated in flowing gas to achieve containerless conditions. Levitated samples were heated to temperatures of up to 3500 °C with a partially focused carbon dioxide laser beam. Sample temperature was measured using an optical pyrometer. The sample environment was integrated with a high energy (100 keV) x-ray synchrotron beamline to enable in situ structure measurements to be made on levitated samples as they were heated, melted, and supercooled. The system was controlled from outside the x-ray beamline hutch by using a LabVIEW program. Measurements have been made on hot solid and molten uranium dioxide and binary uranium dioxide-zirconium dioxide compositions.

  12. Multiferroic CuCrO₂ under high pressure: In situ X-ray diffraction and Raman spectroscopic studies

    Energy Technology Data Exchange (ETDEWEB)

    Garg, Alka B., E-mail: alkagarg@barc.gov.in; Mishra, A. K.; Pandey, K. K.; Sharma, Surinder M. [High Pressure and Synchrotron Radiation Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 (India)

    2014-10-07

    The compression behavior of delafossite compound CuCrO₂ has been investigated by in situ x-ray diffraction (XRD) and Raman spectroscopic measurements up to 23.2 and 34 GPa, respectively. X-ray diffraction data show the stability of ambient rhombohedral structure up to ~23 GPa. Material shows large anisotropy in axial compression with c-axis compressibility, κ{sub c} = 1.26 × 10⁻³(1) GPa⁻¹ and a-axis compressibility, κ{sub a} = 8.90 × 10⁻³(6) GPa⁻¹. Our XRD data show an irreversible broadening of diffraction peaks. Pressure volume data when fitted to 3rd order Birch-Murnaghan equation of state give the value of bulk modulus, B₀ = 156.7(2.8) GPa with its pressure derivative, B₀{sup ’} as 5.3(0.5). All the observed vibrational modes in Raman measurements show hardening with pressure. Appearance of a new mode at ~24 GPa indicates the structural phase transition in the compound. Our XRD and Raman results indicate that CuCrO{sub 2} may be transforming to an ordered rocksalt type structure under compression.

  13. In-situ X-ray observations of creep behavior during the olivine-spinel transformation in fayalite

    Science.gov (United States)

    Kubo, T.; Doi, N.; Imamura, M.; Kato, T.; Higo, Y.; Tange, Y.

    2016-12-01

    Most of constituent minerals in subducting slab cause high-pressure transformations in mantle transition zone, which largely affects rheology of the deep slab. Previous studies have suggested that the grain-size reduction due to non-equilibrium olivine-spinel transformation leads to weakening and shear instability in the slab, which may be responsible for the slab stagnation and deep earthquakes. However, there have been few experimental studies to examine the coupling process between transformation and deformation at high pressure quantitatively. Here we report preliminary results on in-situ X-ray observations of creep behaviors during the olivine-spinel transformation in fayalite (Fe2SiO4). High-pressure deformation experiments were conducted using Deformation-DIA apparatus in the beamline of BL04B1 at the synchrotron facility of SPring-8. Monochromatic X-ray (energy 50-60 keV) was used as the incident beam. We measured time-resolved two-dimensional X-ray diffraction patterns and X-ray radiography images to obtain stress-strain and transformation-time (strain) curves, simultaneously. After annealing polycrystalline fayalite at 3.5 GP and 1173 K for 2 hours, we observed the olivine-spinel transformation at 5-9 GPa and 873-1173 K with and without deformation (in uniaxial compression with constant strain rate of 4-5 x 10-5 s-1). Overpressures needed for the transformation increased with decreasing temperature from 1.5 GPa and 1173 K to 3.8 GPa at 973 K in the case of no deformation. When the sample was deformed, the overpressures decreased by 0.5-1 GPa compared to the case of no deformation, suggesting the enhancement of spinel nucleation. Transformation was not observed at 873 K even when the overpressure reached to 4 GPa with deformation. Stress in olivine, spinel, and the bulk sample (from stress marker arranged in tandem) were similar at the initial stage, and then spinel becomes dominant deformation phase at around 50% transformation. During the

  14. Hydraulic Properties of Fractured Rock Samples at In-Situ Conditions - Insights from Lab Experiments Using X-Ray Tomography

    Science.gov (United States)

    Nehler, Mathias; Stöckhert, Ferdinand; Duda, Mandy; Renner, Jörg; Bracke, Rolf

    2017-04-01

    The hydraulic properties of low-porosity rock formations are controlled by the geometry of open fractures, joints and faults. Aperture, surface roughness, accessible length, and thus, the volume available for fluids associated of such interfaces are strongly affected by their state of stress. Moreover, these properties may evolve with time in particular due to processes involving chemically active fluids. Understanding the physico-chemical interactions of rocks with fluids at reservoir conditions will help to predict the long-term reservoir development and to increase the efficiency of geothermal power plants. We designed an x-ray transparent flow-through cell. Confining pressure can be up to 50 MPa and pore fluid can currently be circulated through the sample with pressures of up to 25 MPa. All wetted parts are made of PEEK to avoid corrosion when using highly saline fluids. Laboratory experiments were performed to investigate hydraulic properties of fractured low-porosity samples under reservoir conditions while x-rays transmit the sample. The cell is placed inside a µCT scanner with a 225 kV multifocal x-ray tube for high resolution x-ray tomography. Samples measure 10 mm in diameter and 25 mm in length resulting in a voxel resolution of approximately 10 µm. Samples with single natural as well as artificial fractures were subjected to various confining pressures ranging from 2.5 MPa to 25 MPa. At each pressure level, effective permeability was determined from steady-state flow relying on Darcy's law. In addition, a full 3D image was recorded by the µCT scanner to gain information on the fracture aperture and geometry. Subvolumes (400x400x400 voxels) of the images were analyzed to reduce computational cost. The subvolumes were filtered in 3D with an edge preserving non-local means filter. Further quantification algorithms were implemented in Matlab. Segmentation into pore space and minerals was done automatically for all datasets by a peak finder algorithm

  15. Testing the Performance and Accuracy of the RELXILL Model for the Relativistic X-Ray Reflection from Accretion Disks

    Science.gov (United States)

    Choudhury, Kishalay; García, Javier A.; Steiner, James F.; Bambi, Cosimo

    2017-12-01

    The reflection spectroscopic model RELXILL is commonly implemented in studying relativistic X-ray reflection from accretion disks around black holes. We present a systematic study of the model’s capability to constrain the dimensionless spin and ionization parameters from ∼6000 Nuclear Spectroscopic Telescope Array (NuSTAR) simulations of a bright X-ray source employing the lamp-post geometry. We employ high-count spectra to show the limitations in the model without being confused with limitations in signal-to-noise. We find that both parameters are well-recovered at 90% confidence with improving constraints at higher reflection fraction, high spin, and low source height. We test spectra across a broad range—first at 106–107 and then ∼105 total source counts across the effective 3–79 keV band of NuSTAR, and discover a strong dependence of the results on how fits are performed around the starting parameters, owing to the complexity of the model itself. A blind fit chosen over an approach that carries some estimates of the actual parameter values can lead to significantly worse recovery of model parameters. We further stress the importance to span the space of nonlinear-behaving parameters like {log} ξ carefully and thoroughly for the model to avoid misleading results. In light of selecting fitting procedures, we recall the necessity to pay attention to the choice of data binning and fit statistics used to test the goodness of fit by demonstrating the effect on the photon index Γ. We re-emphasize and implore the need to account for the detector resolution while binning X-ray data and using Poisson fit statistics instead while analyzing Poissonian data.

  16. Spherical analyzers and monochromators for resonant inelastic hard X-ray scattering: a compilation of crystals and reflections

    Energy Technology Data Exchange (ETDEWEB)

    Gog, Thomas, E-mail: gog@aps.anl.gov; Casa, Diego M.; Said, Ayman H.; Upton, Mary H.; Kim, Jungho; Kuzmenko, Ivan; Huang, XianRong; Khachatryan, Ruben [Advanced Photon Source, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439 (United States)

    2013-01-01

    Resonant inelastic X-ray scattering (RIXS) experiments require special sets of near-backscattering spherical diced analyzers and high-resolution monochromators for every distinct absorption-edge energy or emission line. For the purpose of aiding the design and planning of efficient RIXS experiments, a compilation of suitable crystal materials and viable reflections for hard X-rays, together with energy resolution and throughput information, is presented. Resonant inelastic X-ray scattering (RIXS) experiments require special sets of near-backscattering spherical diced analyzers and high-resolution monochromators for every distinct absorption-edge energy and emission line. For the purpose of aiding the design and planning of efficient RIXS experiments, comprehensive lists of suitable analyzer reflections for silicon, germanium, α-quartz, sapphire and lithium niobate crystals were compiled for a multitude of absorption edges and emission lines. Analyzers made from lithium niobate, sapphire or α-quartz offer many choices of reflections with intrinsic resolutions currently unattainable from silicon or germanium. In some cases these materials offer higher intensities at comparable resolutions. While lithium niobate, sapphire or α-quartz analyzers are still in an early stage of development, the present compilation can serve as a computational basis for assessing expected and actual performance. With regard to high-resolution monochromators, bandpass and throughput calculations for combinations of double-crystal, high-heat-load and near-backscattering high-resolution channel-cuts were assembled. The compilation of these analyzer and monochromator data is publicly available on a website.

  17. In-situ characterization of highly reversible phase transformation by synchrotron X-ray Laue microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Xian [Department of Mechanical and Aerospace Engineering, Hong Kong University of Science and Technology, Clear Water Bay (Hong Kong); Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, California 94720 (United States); Tamura, Nobumichi; MacDowell, Alastair [Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, California 94720 (United States); James, Richard D. [Department of Aerospace Engineering and Mechanics, University of Minnesota, Minneapolis, Minnesota 55455 (United States)

    2016-05-23

    The alloy Cu{sub 25}Au{sub 30}Zn{sub 45} undergoes a huge first-order phase transformation (6% strain) and shows a high reversibility under thermal cycling and an unusual martensitc microstructure in sharp contrast to its nearby compositions. This alloy was discovered by systematically tuning the composition so that its lattice parameters satisfy the cofactor conditions (i.e., the kinematic conditions of compatibility between phases). It was conjectured that satisfaction of these conditions is responsible for the enhanced reversibility as well as the observed unusual fluid-like microstructure during transformation, but so far, there has been no direct evidence confirming that these observed microstructures are those predicted by the cofactor conditions. To verify this hypothesis, we use synchrotron X-ray Laue microdiffraction to measure the orientations and structural parameters of variants and phases near the austenite/martensite interface. The areas consisting of both austenite and multi-variants of martensite are scanned by microLaue diffraction. The cofactor conditions have been examined from the kinematic relation of lattice vectors across the interface. The continuity condition of the interface is precisely verified from the correspondent lattice vectors between two phases.

  18. Optical properties of zirconium carbide in 60-200 Å wavelength region using x-ray reflectivity technique.

    Science.gov (United States)

    Singh, Amol; Modi, Mohammed H; Lodha, G S

    2015-01-10

    Optical constants of zirconium carbide (ZrC) have been determined in the soft x-ray region of 60-200 Å wavelength using angle-dependent x-ray reflectivity measurements. Reflectivity measurements are carried out at the reflectivity beamline of the Indus-1 synchrotron radiation source. Derived optical constants (δ and β) are compared with the tabulated values [At. Data Nucl. Data Tables 54, 181 (1993)]. The optical constants are 15%-35% lower than bulk values in the 60-200 Å wavelength region. Near the Zr M4 edge 187 eV (66.3 Å), the δ values were close to bulk values with a deviation of 5%-10%. A large deviation of ∼20% was found in beta values especially near the Zr M4 edge region, whereas it was in close agreement in the wavelength range away from the edge. To the best of our knowledge, this paper gives the first reported experimental values of optical constants for zirconium carbide in the 60-200 Å wavelength region.

  19. Sample Handling System for in-situ Powder X-ray Diffraction Instruments. Project

    Data.gov (United States)

    National Aeronautics and Space Administration — The proposed innovation is a Powder Handling System (PHS) that will deliver powdered samples to in situ planetary XRD instruments and provide unique means of...

  20. A flow cell for the study of gas-solid reactions via in situ powder X-ray diffraction

    Science.gov (United States)

    Scarlett, Nicola V. Y.; Hewish, Damien; Pattel, Rachel; Webster, Nathan A. S.

    2017-10-01

    This paper describes the development and testing of a novel capillary flow cell for use in in situ powder X-ray diffraction experiments. It is designed such that it achieves 200° of rotation of the capillary whilst still allowing the flow of gas through the sample and the monitoring of off gas via mass spectrometry, gas chromatography, or other such analytical techniques. This high degree of rotation provides more uniform heating of the sample than can be achieved in static cells or those with lower rotational ranges and consequently also improves particle statistics. The increased uniformity of heating provides more accurate temperature calibration of the experimental setup as well. The cell is designed to be held in a standard goniometer head and is therefore suitable for use in many laboratory and synchrotron instruments.

  1. In-situ early stage electromigration study in Al line using synchrotron polychromatic X-ray microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Kai; Tamura, Nobumichi; Tu, King-Ning

    2007-10-31

    Electromigration is a phenomenon that has attracted much attention in the semiconductor industry because of its deleterious effects on electronic devices (such as interconnects) as they become smaller and current density passing through them increases. However, the effect of the electric current on the microstructure of interconnect lines during the very early stage of electromigration is not well documented. In the present report, we used synchrotron radiation based polychromatic X-ray microdiffraction for the in-situ study of the electromigration induced plasticity effects on individual grains of an Al (Cu) interconnect test structure. Dislocation slips which are activated by the electric current stressing are analyzed by the shape change of the diffraction peaks. The study shows polygonization of the grains due to the rearrangement of geometrically necessary dislocations (GND) in the direction of the current. Consequences of these findings are discussed.

  2. In-situ stress measurement of single and multilayer thin-films used in x-ray astronomy optics applications

    Science.gov (United States)

    Broadway, David M.; Ramsey, Brian D.; O'Dell, Stephen L.; Gurgew, Danielle

    2017-09-01

    We present in-situ stress measurement results for single and multilayer thin-films deposited by magnetron sputtering. In particular, we report on the influence of the material interfaces on the ensuing stress in both the transient and steady-state regimes of film growth. This behavior is used to determine the appropriate thicknesses of the constituent layers that will result in a net tensile stress in multilayers composed of various material combinations. These multilayers can then be used to compensate the compressive integrated stress in single and multilayer EUV and x-ray optical coatings. The use of multilayers to compensate the integrated stress might be advantageous because, unlike single layers of chromium, the roughness is not expected to increase with the total thickness of the multilayer. In this paper, we demonstrate the technique for W/Si and Mo/Si multilayers and discuss its application to other material combinations.

  3. Probing the electron beam induced reduction of graphite oxide by in situ X-ray photoelectron spectroscopy/mass spectrometer

    Science.gov (United States)

    Zhu, Chunhua; Hao, Xiaofei; Liu, Yu; Wu, Yeping; Wang, Jianhua

    2018-01-01

    The graphite oxide (GO) was reduced successfully by electron-beam irradiation without solution chemistry and high temperature, where the chemical structural changes and gaseous species released during the exposure was monitored directly by X-ray photoelectron spectroscopy/mass spectrometer. The degree of reduction of GO can be tuned effectively by way of electron beam intensity and irradiation time, resulting a high C/O ratio of 5.27. The evolution of C 1s spectra with irradiation time was also investigated. The CO, CO2, H2 molecules and several organic species were detected during the irradiation, confirmed that the electron beam induced the photoreduction of GO. The combined chemical structure evolution and gas species analysis make the XPS-MS highly desirable as a powerful in situ analytical instrument for tracking the reaction process. The electron-beam-induced reduction described in detail here provides potential way to fabricate graphene device from GO in one step.

  4. REFLECTION-DOMINATED NUCLEAR X-RAY EMISSION IN THE EARLY-TYPE GALAXY ESO 565-G019

    Energy Technology Data Exchange (ETDEWEB)

    Gandhi, P.; Takahashi, T. [Institute of Space and Astronautical Science (ISAS), Japan Aerospace Exploration Agency, 3-1-1 Yoshinodai, Chuo-ku, Sagamihara, Kanagawa 252-5210 (Japan); Terashima, Y. [Department of Physics, Ehime University, 2-5 Bunkyo-cho, Matsuyama, Ehime 790-8577 (Japan); Yamada, S. [Cosmic Radiation Laboratory, Institute of Physical and Chemical Research (RIKEN), Wako, Saitama 351-0198 (Japan); Mushotzky, R. F. [Department of Astronomy, University of Maryland College Park, College Park, MD 20742 (United States); Ueda, Y. [Department of Astronomy, Kyoto University, Kitashirakawa-Oiwake-cho, Sakyo-ku, Kyoto 606-8502 (Japan); Baumgartner, W. H. [NASA/Goddard Space Flight Center, Astrophysics Science Division, Greenbelt, MD 20771 (United States); Alexander, D. M.; Done, C. [Department of Physics, Durham University, Durham DH1-3LE (United Kingdom); Malzac, J. [Universite de Toulouse, UPS-OMP, IRAP, F-31028 Toulouse (France); Vaghmare, K. [IUCAA, Post Bag 4, Ganeshkhind, Pune 411007 (India)

    2013-08-10

    We present the discovery of a reflection-dominated active galactic nucleus (AGN) in the early-type radio-quiet galaxy ESO 565-G019 with Suzaku and Swift/Burst Alert Telescope. The source X-ray spectrum below 10 keV is characteristic of other Compton-thick (CT) AGNs, clearly showing an inverted continuum and prodigious fluorescence iron emission above {approx}3 keV. A Compton shoulder to the neutral Fe K{alpha} line also appears to be present. There is evidence for long-term hard X-ray flux variability that we associate with changes in the intrinsic AGN power law. More of such reflection-dominated AGNs should be uncovered in the near future with the increased sensitivity of ongoing and new hard X-ray surveys. ESO 565-G019 is hosted in an early-type galaxy whose morphology has been variously classified as either type E or type S0. Only about 20 bona fide CT-AGNs have been identified in the local universe so far, and all exist in host galaxies with late Hubble types (S0 or later). CT columns of nuclear obscuring gas are uncommon in early-type galaxies in the local universe, so confirmation of the exact morphological class of ESO 565-G019 is important. Infrared photometry also shows the presence of large quantities of cool dust in the host, indicative of significant ongoing star formation. ESO 565-G019 may be the first identified local example of minor-merger-driven CT-AGN growth in an early-type host, or may be the result of interaction with its neighboring galaxy ESO 565-G018 in a wide pair.

  5. Measuring twinning and slip in shock-compressed Ta from in-situ x-ray diffraction

    Science.gov (United States)

    Wehrenberg, Christopher; McGonegle, David; Sliwa, Marcin; Suggit, Matt; Wark, Justin; Lee, Hae Ja; Nagler, Bob; Tavella, Franz; Remington, Bruce; Rudd, Rob; Lazicki, Amy; Park, Hye-Sook; Swift, Damian; Zepeda-Ruiz, Louis; Higginbotham, Andrew; Bolme, Cindy

    2017-06-01

    A fundamental understanding of high-pressure and high-strain-rate deformation rests on grasping the underlying microstructural processes, such as twinning and dislocation generation and transport (slip), yet simulations and ex-post-facto recovery experiments provide conflicting answers to these basic issues. Here, we report direct, in-situ observation of twinning and slip in shock compressed Ta using in-situ x-ray diffraction. A series of shock experiments were performed on the Matter in Extreme Conditions end station at LCLS. Direct laser ablation was used to drive a shock, ranging in pressure from 10-300 GPa, into a Ta sample with an initial (110) fiber texture. The subsequent changes in texture were observed in-situ by examining the azimuthal distribution of the diffraction intensity and found to match twinning and lattice rotation. Measurements of the twin fraction and lattice rotation were used to calculate the equivalent plastic strain from twinning and slip. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract No. DE-AC52-07NA27344.

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

    Science.gov (United States)

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

    2017-04-01

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

  7. Effects of growth conditions on the GaAs/AlAs superlattices by grazing incidence X-ray reflectivity.

    Science.gov (United States)

    Ren, Lingling; Gao, Huifang; Yuan, Aili

    2013-02-01

    The effects of growth conditions on the structural properties of the GaAs/AlAs superlattices were investigated by grazing incidence X-ray reflectivity (GIXRR), transmission electron microscopy (TEM), Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS). The GaAs/AlAs superlattices were prepared by molecular beam epitaxy (MBE) at different growth temperatures (500 degrees C, 600 degrees C and 660 degrees C) and growth rates (1.0 microm/h and 0.7 microm/h for GaAs). And the thicknesses, surface/interface roughnesses and densities of the GaAs/AlAs superlattices were obtained by GIXRR by fitting the whole spectral reflectance curves based on the Parratt recurrence formula. The homogeneity of samples was also studied at different growth conditions. The results indicate that the superlattices grown at a high temperature and large growth rate ratio (rate of AlAs to that of GaAs) possess better structure and more homogeneity.

  8. Quantitative resonant soft x-ray reflectivity of ultrathin anisotropic organic layers: Simulation and experiment of PTCDA on Au.

    Science.gov (United States)

    Capelli, R; Mahne, N; Koshmak, K; Giglia, A; Doyle, B P; Mukherjee, S; Nannarone, S; Pasquali, L

    2016-07-14

    Resonant soft X-ray reflectivity at the carbon K edge, with linearly polarized light, was used to derive quantitative information of film morphology, molecular arrangement, and electronic orbital anisotropies of an ultrathin 3,4,9,10-perylene tetracarboxylic dianhydride (PTCDA) film on Au(111). The experimental spectra were simulated by computing the propagation of the electromagnetic field in a trilayer system (vacuum/PTCDA/Au), where the organic film was treated as an anisotropic medium. Optical constants were derived from the calculated (through density functional theory) absorption cross sections of the single molecule along the three principal molecular axes. These were used to construct the dielectric tensor of the film, assuming the molecules to be lying flat with respect to the substrate and with a herringbone arrangement parallel to the substrate plane. Resonant soft X-ray reflectivity proved to be extremely sensitive to film thickness, down to the single molecular layer. The best agreement between simulation and experiment was found for a film of 1.6 nm, with flat laying configuration of the molecules. The high sensitivity to experimental geometries in terms of beam incidence and light polarization was also clarified through simulations. The optical anisotropies of the organic film were experimentally determined and through the comparison with calculations, it was possible to relate them to the orbital symmetry of the empty electronic states.

  9. In situ X-ray crystallographic study of the structural evolution of colloidal crystals upon heating

    NARCIS (Netherlands)

    Zozulya, A.V.; Meijer, J.M.; Shabalin, A.; Ricci, A.; Westermeier, F.; Kurta, R.P.; Lorenz, U.; Singer, A.; Yefanow, O.; Petukhov, A.V.; Sprung, M.; Vartanyants, I. A.

    2013-01-01

    The structural evolution of colloidal crystals made of polystyrene hard spheres has been studied in situ upon incremental heating of a crystal in a temperature range below and above the glass transition temperature of polystyrene. Thin films of colloidal crystals having different particle sizes were

  10. Total reflection X-ray fluorescence analysis of trace-elements in candies marketed in Mexico

    Science.gov (United States)

    Martinez, T.; Lartigue, J.; Zarazua, G.; Avila-Perez, P.; Navarrete, M.; Tejeda, S.

    2010-06-01

    Trace metals concentrations in food are significant for nutrition, due either to their nature or toxicity. Sweets, including chewing gum and candies, are not exactly a food, but they usually are unwearied consumed by children, the most vulnerable age-group to any kind of metal contamination in the food chain. The presence of relatively high concentrations of heavy metals such as Lead elicits concern since children are highly susceptible to heavy metals poisoning. Trace-metals concentrations were determined for six different flavors of a Mexican candy by means of Total X-ray Fluorescence Spectrometry. Triplicate samples of the various candy's flavours (strawberry, pineapple, lemon, blackberry, orange and chilli) were digested in 8 mL of a mix of supra-pure HNO 3 and H 2O 2 (6 mL: 2 mL) in a microwave oven MARS-X. Results show the presence of essential and toxic elements such as Ti, Cr, Mn, Fe, Ni, Cu, Zn, Br, Rb, Sr, and Pb. All metal concentrations were higher and significantly different ( α = 0.05) in chilli candy, compared to other candy flavours. Lead concentration fluctuated in the range of 0.102 to 0.342 μg g - 1 . A discussion about risk consumption and concentration allowed by Mexican and International Norms is made. As a part of the Quality Control Program, a NIST standard of "Citrus Leaves" and a blank were treated in the same way.

  11. Building Polyelectrolyte Multilayers with Calmodulin: A Neutron and X-ray Reflectivity Study.

    Science.gov (United States)

    Cinar, Süleyman; Möbitz, Simone; Al-Ayoubi, Samy; Seidlhofer, Beatrix-Kamelia; Czeslik, Claus

    2017-04-25

    We have studied the formation and functional properties of polyelectrolyte multilayers where calmodulin (CaM) is used as a polyanion. CaM is known to populate distinct conformational states upon binding Ca2+ and small ligand molecules. Therefore, we have also probed the effects of Ca2+ ions and trifluoperazine (TFP) as ligand molecule on the interfacial structures. Multilayers with the maximum sequence PEI-(PSS-PAH)x-CaM-PAH-CaM-PAH have been deposited on silicon wafers and characterized by X-ray and neutron reflectometry. From the analysis of all data, several remarkable conclusions can be drawn. When CaM is deposited for the second time, a much thicker sublayer is produced than in the first CaM deposition step. However, upon rinsing with PAH, very thin CaM-PAH sublayers remain. There are no indications that ligand TFP can be involved in the multilayer buildup due to strong CaM-PAH interactions. However, there is a significant increase in the multilayer thickness upon removal of Ca2+ ions from holo-CaM and an equivalent decrease in the multilayer thickness upon subsequent saturation of apo-CaM with Ca2+ ions. Presumably, CaM can still be toggled between an apo and a holo state, when it is embedded in polyelectrolyte multilayers, providing an approach to design bioresponsive interfaces.

  12. Exploring Pore Formation of Atomic Layer-Deposited Overlayers by in Situ Small- and Wide-Angle X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Li, Tao; Karwal, Saurabh; Aoun, Bachir; Zhao, Haiyan; Ren, Yang; Canlas, Christian P.; Elam, Jeffrey W.; Winans, Randall E.

    2016-10-11

    In this work, we explore the pore structure of overcoated materials by in situ synchrotron small- and wide-angle X-ray scattering (SAXS)/(WAXS). Thin films of aluminum oxide (Al2O3) and titanium dioxide (TiO2) with thicknesses of 4.9 and 2.5 nm, respectively, are prepared by atomic layer deposition (ALD) on non-porous nanoparticles. In situ X-ray measurements reveal that porosity is induced in the ALD films by annealing the samples at high temperature. Moreover, this pore formation can be attributed to densification resulting from an amorphous to crystalline phase transition of the ALD films as confirmed by high resolution X-ray diffraction (XRD) and pair distribution function (PDF). Simultaneous SAXS/WAXS results not only show the porosity is formed by the phase transition but also that the pore size increases with temperature.

  13. Exploring Pore Formation of Atomic Layer-Deposited Overlayers by in Situ Small- and Wide-Angle X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Li, Tao; Karwal, Saurabh; Aoun, Bachir; Zhao, Haiyan; Ren, Yang; Canlas, Christian P.; Elam, Jeffrey W.; Winans, Randall E.

    2016-10-11

    In this work, we explore the pore structure of overcoated materials by in situ synchrotron small- and wide-angle X-ray scattering (SAXS)/(WAXS). Thin films of aluminum oxide (Al2O3) and titanium dioxide (TiO2) with thicknesses of 4.9 and 2.5 nm, respectively, are prepared by atomic layer deposition (ALD) on non-porous nanoparticles. In situ X-ray measurements reveal that porosity is induced in the ALD films by annealing the samples at high temperature. Moreover, this pore formation can be attributed to densification resulting from an amorphous to crystalline phase transition of the ALD films as confirmed by high resolution X-ray diffraction (XRD) and pair distribution function (PDF). Simultaneous SAXS/WAXS results not only show that the porosity is formed by this phase transition but also that the pore size increases with temperature.

  14. Mapping strain fields induced in Zr-based bulk metallic glasses during in-situ nanoindentation by X-ray nanodiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Gamcová, J.; Bednarčík, J.; Franz, H. [DESY, Notkestraße 85, Hamburg 22547 (Germany); Mohanty, G.; Wehrs, J.; Michler, J. [Empa, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for Mechanics of Materials and Nanostructures, Feuerwerkerstraße 39, Thun 3602 (Switzerland); Michalik, Š. [Institute of Physics ASCR, Na Slovance 2, Praha 18221 (Czech Republic); Krywka, C. [HZG, Institut für Werkstoffforschung, Notkestraße 85, Hamburg 22547 (Germany); Breguet, J. M. [Empa, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for Mechanics of Materials and Nanostructures, Feuerwerkerstraße 39, Thun 3602 (Switzerland); Alemnis GmbH, Feuerwerkerstraße 39, Thun 3602 (Switzerland)

    2016-01-18

    A pioneer in-situ synchrotron X-ray nanodiffraction approach for characterization and visualization of strain fields induced by nanoindentation in amorphous materials is introduced. In-situ nanoindentation experiments were performed in transmission mode using a monochromatic and highly focused sub-micron X-ray beam on 40 μm thick Zr-based bulk metallic glass under two loading conditions. Spatially resolved X-ray diffraction scans in the deformed volume of Zr-based bulk metallic glass covering an area of 40 × 40 μm{sup 2} beneath the pyramidal indenter revealed two-dimensional map of elastic strains. The largest value of compressive elastic strain calculated from diffraction data at 1 N load was −0.65%. The region of high elastic compressive strains (<−0.3%) is located beneath the indenter tip and has radius of 7 μm.

  15. In situ structural investigation of iron phthalocyanine monolayer adsorbed on electrode surface by X-ray absorption fine structure

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Sung Hyun [Konkuk Univ., Seoul (Korea, Republic of); Ohta, Toshiaki [Tokyo Univ., Tokyo (Japan); Kwag, Gwang Hoon [Kumho Petrochemical Co., Taejon(Korea, Republic of)

    2000-06-01

    Structural changes of an iron phthalocyanine (FePC) monolayer induced by adsorption and externally applied potential on high area carbon surface have been investigated in situ by iron K-edge X-ray absorption fine structure (XAFS) in 0.5 M H{sub 2}SO{sub 4}. Fine structures shown in the X-ray absorption near edge structure (XANES) for microcrystalline FePC decreased upon adsorption and further diminished under electrochemical conditions. Fe(II)PC(-2) showed a 1s{yields}4p transition as poorly resolved shoulder to the main absorption edge rather than a distinct peak and a weak 1s{yields}3d transition. The absorption edge position measured at half maximum was shifted from 7121.8 eV for Fe(II)PC(-2) to 7124.8 eV for [Fe(III)PC(-2)]{sup +} as well as the 1s{yields}3d pre-edge peak being slightly enhanced. However, essentially no absorption edge shift was observed by the 1-electron reduction of Fe(II)PC(-2), indicating that the species formed is [Fe(II)PC(-3)]{sup -}. Structural parameters were obtained by analyzing extended X-ray absorption fine structure (EXAFS) oscillations with theoretical phases and amplitudes calculated from FEFF 6.01 using multiple-scattering theory. When applied to the powder FePC, the average iron-to-phthalocyanine nitrogen distance, d(Fe-N{sub p}) and the coordination number were found to be 1.933 A and 3.2, respectively, and these values are the same, within experimental error, as those reported (1.927 A and 4). Virtually no structural changes were found upon adsorption except for the increased Debye-Waller factor of 0.005 A{sup 2} from 0.003 A{sup 2}. Oxidation of Fe(II)PC(-2) to [Fe(III)PC(-2)]{sup +} yielded an increased d(Fe-N{sub p}) (1.98 A) and Debye-Waller factor (0.005 A{sup 2}). The formation of [Fe(II)PC(-3)]{sup -}, however, produced a shorter d(Fe-N{sub p}) of 1.91 A, the same as that of crystalline FePC within experimental error, and about the same Debye-Waller factor (0.006 A{sup 2})

  16. Induction of in situ DNA double-strand breaks and apoptosis by 200 MeV protons and 10 MV X-rays in human tumour cell lines.

    Science.gov (United States)

    Gerelchuluun, Ariungerel; Hong, Zhengshan; Sun, Lue; Suzuki, Kenshi; Terunuma, Toshiyuki; Yasuoka, Kiyoshi; Sakae, Takeji; Moritake, Takashi; Tsuboi, Koji

    2011-01-01

    To clarify the properties of clinical high-energy protons by comparing with clinical high-energy X-rays. Human tumor cell lines, ONS76 and MOLT4, were irradiated with 200 MeV protons or 10 MV X-rays. In situ DNA double-strand breaks (DDSB) induction was evaluated by immunocytochemical staining of phosphorylated histone H2AX (γ-H2AX). Apoptosis was measured by flow-cytometry after staining with Annexin V. The relative biological effectiveness (RBE) was obtained by clonogenic survival assay. DDSB induction was significantly higher for protons than X-rays with average ratios of 1.28 (ONS76) and 1.59 (MOLT4) at 30 min after irradiation. However the differences became insignificant at 6 h. Also, apoptosis induction in MOLT4 cells was significantly higher for protons than X-rays with an average ratio of 2.13 at 12 h. However, the difference became insignificant at 20 h. RBE values of protons to X-rays at 10% survival were 1.06 ± 0.04 and 1.02 ± 0.15 for ONS76 and MOLT4, respectively. Cell inactivation may differ according to different timings and/or endpoints. Proton beams demonstrated higher cell inactivation than X-rays in the early phases. These data may facilitate the understanding of the biological properties of clinical proton beams.

  17. X-ray reflectivity at polarized liquid-Hg-aqueous-electrolyte interface: challenging macroscopic approaches for ion-specificity issues.

    Science.gov (United States)

    Duval, Jérôme F L; Bera, Sambhunath; Michot, Laurent J; Daillant, Jean; Belloni, Luc; Konovalov, Oleg; Pontoni, Diego

    2012-05-18

    We report Angstrom-resolved x-ray reflectivity analysis of externally polarized liquid-Hg surface in contact with molar LiCl, LiBr, and MgSO4 aqueous electrolytes. Interpretation of reflectivity curves demonstrates a dependence of Hg-surface layering on both applied potential and ion nature. It further highlights how interfacial polarization degree impacts electron density profiles at a molecular scale. These profiles indicate accumulation of anions and cations at the Hg surface. Upon decrease of the potential from the point of zero charge, anions are gradually expelled from the Hg surface. The study challenges traditional thermodynamic approaches for deriving countercharge composition at the Hg-electrolyte-solution interface from macroscopic Hg-surface tension data. It further dismisses the long-standing approximation that assimilates the Hg surface to a smooth, perfect chemically inert conductor with a uniformly smeared-out surface charge density.

  18. Compact Roll-to-Roll Coater for in Situ X-ray Diffraction Characterization of Organic Electronics Printing.

    Science.gov (United States)

    Gu, Xiaodan; Reinspach, Julia; Worfolk, Brian J; Diao, Ying; Zhou, Yan; Yan, Hongping; Gu, Kevin; Mannsfeld, Stefan; Toney, Michael F; Bao, Zhenan

    2016-01-27

    We describe a compact roll-to-roll (R2R) coater that is capable of tracking the crystallization process of semiconducting polymers during solution printing using X-ray scattering at synchrotron beamlines. An improved understanding of the morphology evolution during the solution-processing of organic semiconductor materials during R2R coating processes is necessary to bridge the gap between "lab" and "fab". The instrument consists of a vacuum chuck to hold the flexible plastic substrate uniformly flat for grazing incidence X-ray scattering. The time resolution of the drying process that is achievable can be tuned by controlling two independent motor speeds, namely, the speed of the moving flexible substrate and the speed of the printer head moving in the opposite direction. With this novel design, we are able to achieve a wide range of drying time resolutions, from tens of milliseconds to seconds. This allows examination of the crystallization process over either fast or slow drying processes depending on coating conditions. Using regioregular poly(3-hexylthiophene-2,5-diyl) (P3HT) and phenyl-C61-butyric acid methyl ester (PCBM) inks based on two different solvents as a model system, we demonstrate the capability of our in situ R2R printing tool by observing two distinct crystallization processes for inks drying from the solvents with different boiling points (evaporation rates). We also observed delayed on-set point for the crystallization of P3HT polymer in the 1:1 P3HT/PCBM BHJ blend, and the inhibited crystallization of the P3HT during the late stage of the drying process.

  19. The internal structure of PMETAC brush/gold nanoparticle composites: a neutron and X-ray reflectivity study.

    Science.gov (United States)

    Kesal, D; Christau, S; Trapp, M; Krause, P; von Klitzing, R

    2017-11-22

    This work addresses the pH-triggered distribution and relocation of charge-stabilized gold nanoparticles (AuNPs) incorporated into strong polyelectrolyte brushes. Brush/particle composite materials were investigated under aqueous conditions and at different humidities using neutron and X-ray reflectivity, respectively. X-ray reflectivity measurements complement neutron reflectivity measurements and reveal results that could not be observed by neutron reflectivity measurements. Both methods allow scanning the particle density profile, but due to different contrasts, they are sensitive to different regions within the brush. More specifically, 3-mercaptopropionic acid (MPA)-coated AuNPs were incorporated into poly-[2-(methacryloyloxy)ethyl]trimethylammonium chloride (PMETAC) polyelectrolyte brushes at different pH values. The pH value triggers a change in the AuNP surface charge caused by the pH-sensitivity of the MPA ligands, while the charge of the PMETAC brush is not affected by pH variations. The particle number density as well as the particle distribution depend strongly on the pH value of the incubation medium: a rather non-homogeneous assembly (2D assembly) is found when the PMETAC brush is incubated in AuNP suspension at pH 4, while a more homogeneous assembly (3D assembly) is found when the PMETAC brush is incubated in AuNP suspension at pH 8. The main factor dominating the formation of 2D or 3D assembly is assigned to the particle-particle interaction and not to the particle-polymer interaction. No significant relocation of AuNPs within the brush can be found by changing the environmental conditions. The control of particle amount and distribution within the polymer brush has a strong impact on the optical properties of those composite materials, which is crucial for the fabrication of colorimetric sensors.

  20. On the characterization of ultra-precise X-ray optical components: advances and challenges in ex situ metrology.

    Science.gov (United States)

    Siewert, F; Buchheim, J; Zeschke, T; Störmer, M; Falkenberg, G; Sankari, R

    2014-09-01

    To fully exploit the ultimate source properties of the next-generation light sources, such as free-electron lasers (FELs) and diffraction-limited storage rings (DLSRs), the quality requirements for gratings and reflective synchrotron optics, especially mirrors, have significantly increased. These coherence-preserving optical components for high-brightness sources will feature nanoscopic shape accuracies over macroscopic length scales up to 1000 mm. To enable high efficiency in terms of photon flux, such optics will be coated with application-tailored single or multilayer coatings. Advanced thin-film fabrication of today enables the synthesis of layers on the sub-nanometre precision level over a deposition length of up to 1500 mm. Specifically dedicated metrology instrumentation of comparable accuracy has been developed to characterize such optical elements. Second-generation slope-measuring profilers like the nanometre optical component measuring machine (NOM) at the BESSY-II Optics laboratory allow the inspection of up to 1500 mm-long reflective optical components with an accuracy better than 50 nrad r.m.s. Besides measuring the shape on top of the coated mirror, it is of particular interest to characterize the internal material properties of the mirror coating, which is the domain of X-rays. Layer thickness, density and interface roughness of single and multilayer coatings are investigated by means of X-ray reflectometry. In this publication recent achievements in the field of slope measuring metrology are shown and the characterization of different types of mirror coating demonstrated. Furthermore, upcoming challenges to the inspection of ultra-precise optical components designed to be used in future FEL and DLSR beamlines are discussed.

  1. Total reflection X-ray fluorescence analysis of trace-elements in candies marketed in Mexico

    Energy Technology Data Exchange (ETDEWEB)

    Martinez, T., E-mail: tmc@servidor.unam.m [Facultad de Quimica, Departamento de Quimica Inorganica y Nuclear. Universidad Nacional Autonoma de Mexico, Mexico D.F. 04510 (Mexico); Lartigue, J. [Facultad de Quimica, Departamento de Quimica Inorganica y Nuclear. Universidad Nacional Autonoma de Mexico, Mexico, D.F. 04510 (Mexico); Zarazua, G.; Avila-Perez, P. [National Institute of Nuclear Research. Ocoyoacac, Edo. de Mexico, 05045 (Mexico); Navarrete, M. [Facultad de Quimica, Departamento de Quimica Inorganica y Nuclear. Universidad Nacional Autonoma de Mexico, Mexico, D.F. 04510 (Mexico); Tejeda, S. [National Institute of Nuclear Research. Ocoyoacac, Edo. de Mexico, 05045 (Mexico)

    2010-06-15

    Trace metals concentrations in food are significant for nutrition, due either to their nature or toxicity. Sweets, including chewing gum and candies, are not exactly a food, but they usually are unwearied consumed by children, the most vulnerable age-group to any kind of metal contamination in the food chain. The presence of relatively high concentrations of heavy metals such as Lead elicits concern since children are highly susceptible to heavy metals poisoning. Trace-metals concentrations were determined for six different flavors of a Mexican candy by means of Total X-ray Fluorescence Spectrometry. Triplicate samples of the various candy's flavours (strawberry, pineapple, lemon, blackberry, orange and chilli) were digested in 8 mL of a mix of supra-pure HNO{sub 3} and H{sub 2}O{sub 2} (6 mL: 2 mL) in a microwave oven MARS-X. Results show the presence of essential and toxic elements such as Ti, Cr, Mn, Fe, Ni, Cu, Zn, Br, Rb, Sr, and Pb. All metal concentrations were higher and significantly different ({alpha} = 0.05) in chilli candy, compared to other candy flavours. Lead concentration fluctuated in the range of 0.102 to 0.342 {mu}g g{sup -1}. A discussion about risk consumption and concentration allowed by Mexican and International Norms is made. As a part of the Quality Control Program, a NIST standard of 'Citrus Leaves' and a blank were treated in the same way.

  2. X-ray magnetic circular dichroism and reflection anisotropy spectroscopy Kerr effect studies of capped magnetic nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Cunniffe, J. P.; McNally, D.E.; Liberati, M.; Arenholz, E.; McGuinness, C.; McGilp, J. F.

    2010-03-02

    Aligned Co wires grown on Pt(997) under ultra-high vacuum conditions have been capped successfully by the epitaxial growth of Au monolayers (ML) at room temperature. The samples were kept under vacuum except when transferring between apparatus or when making some of the measurements. No degradation of the Co wires was detected during the measurements. The magneto-optic response of the system was measured using X-ray magnetic circular dichroism (XMCD) at the Co L{sub 2,3} edge and reflection anisotropy spectroscopy (RAS) at near normal incidence, which is sensitive to the normal component of the out-of-plane magnetization via the Kerr effect (MOKE). Capping the wires significantly impacts their magnetic properties. Comparison of the magneto-optic response of the system at X-ray and optical energies reveals small differences that are attributed to the induced moment in the Pt substrate and Au capping layer not picked up by the element specific XMCD measurements. The sensitivity of RAS-MOKE is sufficient to allow the determination of the easy axis direction of the capped wires to within a few degrees. The results for a 6-atom-wide Co wire sample, capped with 6 ML of Au, are consistent with the capped wires possessing perpendicular magnetization.

  3. Improved multivariate analysis for fast and selective monitoring of structural dynamics by in situ X-ray powder diffraction.

    Science.gov (United States)

    Guccione, Pietro; Palin, Luca; Milanesio, Marco; Belviso, Benny Danilo; Caliandro, Rocco

    2017-11-06

    The development of two solid-state reactions, Xe absorption into MFI and molecular complex formation, where samples are affected by changes of crystal lattice due to temperature or pressure variation was structurally monitored through in situ or in operando X-ray powder diffraction experiments. Consequent variations of the peak positions prevent collective analysis of measured patterns, aiming at investigating structural changes occurring within the crystal cell. Moreover, an intrinsic and variable error in peak position is unavoidable when using the Bragg-Brentano geometry and, in some cases (sticky, bulky, aggregate samples) the sample mounting can increase the error within a dataset. Here we present a general multivariate analysis method to process in a fast and automatic way in situ XRPD data collected on charge transfer complexes and porous materials, with the capacity of disentangling peak shifts from intensity and shape variations in diffraction signals, thus allowing an efficient separation of the contribution of crystal lattice changes from structural changes. The peak shift correction allowed an improved PCA analysis that turned out to be more sensible than the traditional single pattern Rietveld analysis. The developed algorithms allowed, with respect to the traditional approach, the location of two new Xe positions into MFI with a better interpretation of the experimental data, while a much faster and more efficient recovery of the reaction coordinate was achieved in the molecular complex formation reaction.

  4. Hydrogen Absorption in Metal Thin Films and Heterostructures Investigated in Situ with Neutron and X-ray Scattering

    Directory of Open Access Journals (Sweden)

    Sara J. Callori

    2016-05-01

    Full Text Available Due to hydrogen possessing a relatively large neutron scattering length, hydrogen absorption and desorption behaviors in metal thin films can straightforwardly be investigated by neutron reflectometry. However, to further elucidate the chemical structure of the hydrogen absorbing materials, complementary techniques such as high resolution X-ray reflectometry and diffraction remain important too. Examples of work on such systems include Nb- and Pd-based multilayers, where Nb and Pd both have strong affinity to hydrogen. W/Nb and Fe/Nb multilayers were measured in situ with unpolarized and polarized neutron reflectometry under hydrogen gas charging conditions. The gas-pressure/hydrogen-concentration dependence, the hydrogen-induced macroscopic film swelling as well as the increase in crystal lattice plane distances of the films were determined. Ferromagnetic-Co/Pd multilayers were studied with polarized neutron reflectometry and in situ ferromagnetic resonance measurements to understand the effect of hydrogen absorption on the magnetic properties of the system. This electronic effect enables a novel approach for hydrogen sensing using a magnetic readout scheme.

  5. In situ x-ray diffraction of solution-derived ferroelectric thin films for quantitative phase and texture evolution measurement

    Science.gov (United States)

    Nittala, Krishna; Mhin, Sungwook; Jones, Jacob L.; Robinson, Douglas S.; Ihlefeld, Jon F.; Brennecka, Geoff L.

    2012-11-01

    An in situ measurement technique is developed and presented, which utilizes x-rays from a synchrotron source with a two-dimensional detector to measure thin film microstructural and crystallographic evolution during heating. A demonstration experiment is also shown wherein the measured diffraction patterns are used to describe phase and texture evolution during heating and crystallization of solution-derived thin films. The diffraction images are measured sequentially while heating the thin film with an infrared lamp. Data reduction methodologies and representations are also outlined to extract phase and texture information from the diffraction images as a function of time and temperature. These techniques and data reduction methods are demonstrated during crystallization of solution-derived lead zirconate titanate ferroelectric thin films heated at a rate of 30 °C/min and using an acquisition time of 8 s. During heating and crystallization, a PtxPb type phase was not observed. A pyrochlore phase was observed prior to the formation and growth of the perovskite phase. The final crystallized films are observed to have both 111 and 100 texture components. The in situ measurement methodology developed in this work allows for acquiring diffraction images in times as low as 0.25 s and can be used to investigate changes during crystallization at faster heating rates. Moreover, the experiments are shown to provide unique information during materials processing.

  6. Beamline electrostatic levitator for in situ high energy x-ray diffraction studies of levitated solids and liquids

    Energy Technology Data Exchange (ETDEWEB)

    Gangopadhyay, A.K.; Lee, G.W.; Kelto, K.F.; Rogers, J.R.; Goldman, A.I.; Robinson, D.S.; Rathz, T.J.; Hyers, R.W. (WU); (UAB); (NASA); (UMASS, Amherst)

    2010-07-19

    Determinations of the phase formation sequence, crystal structures and the thermo-physical properties of materials at high temperatures are hampered by contamination from the sample container and environment. Containerless processing techniques, such as electrostatic (ESL), electromagnetic, aerodynamic, and acoustic levitation, are most suitable for these studies. An adaptation of ESL for in situ structural studies of a wide range of materials using high energy (30-130 keV) x rays at a synchrotron source is described here. This beamline ESL (BESL) allows the in situ determination of the atomic structures of equilibrium solid and liquid phases, undercooled liquids and time-resolved studies of solid-solid and liquid-solid phase transformations. The use of area detectors enables the rapid acquisition of complete diffraction patterns over a wide range (0.5-14 {angstrom}{sup -1}) of reciprocal space. The wide temperature range (300-2500 K), containerless processing environment under high vacuum (10{sup -7}-10{sup -8} Torr), and fast data acquisition capability, make BESL particularly well suited for phase stability studies of high temperature solids and liquids. An additional, but important, feature of BESL is the capability for simultaneous measurements of a host of thermo-physical properties including the specific heat, enthalpy of transformation, solidus and liquidus temperatures, density, viscosity, and surface tension, all on the same sample during the structural measurements.

  7. Strategies for in situ laser heating in the diamond anvil cell at an X-ray diffraction beamline.

    Science.gov (United States)

    Petitgirard, Sylvain; Salamat, Ashkan; Beck, Pierre; Weck, Gunnar; Bouvier, Pierre

    2014-01-01

    An overview of several innovations regarding in situ laser-heating techniques in the diamond anvil cell at the high-pressure beamline ID27 of the European Synchrotron Radiation Facility is presented. Pyrometry measurements have been adapted to allow simultaneous double-sided temperature measurements with the installation of two additional online laser systems: a CO2 and a pulsed Nd:YAG laser system. This reiteration of laser-heating advancements at ID27 is designed to pave the way for a new generation of state-of-the-art experiments that demand the need for synchrotron diffraction techniques. Experimental examples are provided for each major development. The capabilities of the double pyrometer have been tested with the Nd:YAG continuous-wave lasers but also in a time-resolved configuration using the nanosecond-pulsed Nd:YAG laser on a Fe sample up to 180 GPa and 2900 K. The combination of time-resolved X-ray diffraction with in situ CO2 laser heating is shown with the crystallization of a high-pressure phase of the naturally found pyrite mineral MnS2 (11 GPa, 1100-1650 K).

  8. Formation and texture of palladium germanides studied by in situ X-ray diffraction and pole figure measurements

    Energy Technology Data Exchange (ETDEWEB)

    Geenen, F.A., E-mail: Filip.Geenen@UGent.be [Ghent University, Department of Solid-State Sciences, Krijgslaan 281 (S1), 9000 Gent (Belgium); Knaepen, W.; De Keyser, K. [Ghent University, Department of Solid-State Sciences, Krijgslaan 281 (S1), 9000 Gent (Belgium); Opsomer, K. [Interuniversitair Micro-Electronica Centrum (IMEC), Kapeldreef 75, 3001 Leuven (Belgium); Vanmeirhaeghe, R.L. [Ghent University, Department of Solid-State Sciences, Krijgslaan 281 (S1), 9000 Gent (Belgium); Jordan-Sweet, J.; Lavoie, C. [IBM T.J. Watson Research Center, Yorktown (United States); Detavernier, C. [Ghent University, Department of Solid-State Sciences, Krijgslaan 281 (S1), 9000 Gent (Belgium)

    2014-01-31

    The solid state reaction between 30 nm Pd films and various Ge substrates (Ge(100), Ge(111), polycrystalline Ge and amorphous Ge) was studied by means of in situ X-ray diffraction and in situ sheet resistance measurements. The reported phase sequence of Pd{sub 2}Ge followed by PdGe was verified on all substrates. The texture of the germanides was analysed by pole figure measurements on samples quenched in the Pd{sub 2}Ge and in the PdGe phase on both Ge(100) and (111) substrates. We report an epitaxial growth of Pd{sub 2}Ge on Ge(111) and on Ge(100). The formed PdGe has an axiotaxial alignment on Ge(111). On Ge(100), the axiotaxial texture is observed together with a fibre texture. The higher formation temperature of PdGe on Ge(111) could be related to the epitaxial alignment of the Pd{sub 2}Ge parent phase on Ge(111). - Highlights: • Solid-state reaction is studied on a Pd film with Ge substrates. • Pd2Ge grains have an epitaxial texture on both Ge 100 and Ge 111. • PdGe grains are found to grow with an axiotaxial texture. • Retarded PdGe formation on Ge111 is related with strong epitaxy of Pd2Ge.

  9. Strategies for in situ laser heating in the diamond anvil cell at an X-ray diffraction beamline

    Science.gov (United States)

    Petitgirard, Sylvain; Salamat, Ashkan; Beck, Pierre; Weck, Gunnar; Bouvier, Pierre

    2014-01-01

    An overview of several innovations regarding in situ laser-heating techniques in the diamond anvil cell at the high-pressure beamline ID27 of the European Synchrotron Radiation Facility is presented. Pyrometry measurements have been adapted to allow simultaneous double-sided temperature measurements with the installation of two additional online laser systems: a CO2 and a pulsed Nd:YAG laser system. This reiteration of laser-heating advancements at ID27 is designed to pave the way for a new generation of state-of-the-art experiments that demand the need for synchrotron diffraction techniques. Experimental examples are provided for each major development. The capabilities of the double pyrometer have been tested with the Nd:YAG continuous-wave lasers but also in a time-resolved configuration using the nanosecond-pulsed Nd:YAG laser on a Fe sample up to 180 GPa and 2900 K. The combination of time-resolved X-ray diffraction with in situ CO2 laser heating is shown with the crystallization of a high-pressure phase of the naturally found pyrite mineral MnS2 (11 GPa, 1100–1650 K). PMID:24365921

  10. 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

    Lithium ion battery technology is the heart in operating modern technology devices such as mobile phones and laptops. However, as our society is moving towards the utilization of sustainable energy sources, batteries can be foreseen to become an even more important part of the energy infrastructure...... the obtainable power density and battery life time. A challenging and important task is to obtain in situ information about the formation and evolution of interfaces in an operating battery system. This work addresses these challenges and for this purpose we have developed a special microcapillary battery cell...

  11. X-ray-induced reduction of Au ions in an aqueous solution in the presence of support materials and in situ time-resolved XANES measurements

    Energy Technology Data Exchange (ETDEWEB)

    Ohkubo, Yuji, E-mail: okubo@upst.eng.osaka-u.ac.jp; Nakagawa, Takashi; Seino, Satoshi; Kugai, Junichiro; Yamamoto, Takao A. [Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871 (Japan); Nitani, Hiroaki; Niwa, Yasuhiro [High Energy Accelerator Research Organization (KEK), 1-1 Oho, Tsukuba, Ibaraki 305-0801 (Japan)

    2014-07-31

    In situ time-resolved XANES measurements of Au ions in an aqueous solution in the presence of support materials were performed under synchrotron X-ray irradiation. The synchrotron X-ray-induced reduction of Au ions leads to the formation of Au nanoparticles on the carbon particles, acrylic cell or polyimide window. The deposited Au metallic spots were affected by the wettability of carbon particles. Synchrotron X-ray-induced reduction of Au ions in an aqueous solution with or without support materials is reported. To clarify the process of radiation-induced reduction of metal ions in aqueous solutions in the presence of carbon particles as support materials, in situ time-resolved XANES measurements of Au ions were performed under synchrotron X-ray irradiation. XANES spectra were obtained only when hydrophobic carbon particles were added to the precursor solution containing Au ions. Changes in the shape of the XANES spectra indicated a rapid reduction from ionic to metallic Au in the precursor solution owing to synchrotron X-ray irradiation. In addition, the effects of the wettability of the carbon particles on the deposited Au metallic spots were examined. The deposited Au metallic spots were different depending on the relationship of surface charges between metal precursors and support materials. Moreover, a Au film was obtained as a by-product only when hydrophilic carbon particles were added to the precursor solution containing the Au ions.

  12. Characterization of beryllium deformation using in-situ x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Magnuson, Eric Alan [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Brown, Donald William [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Clausen, Bjorn [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Sisneros, Thomas A. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Park, Jun-Sang [Argonne National Lab. (ANL), Argonne, IL (United States)

    2015-08-24

    Beryllium’s unique mechanical properties are extremely important in a number of high performance applications. Consequently, accurate models for the mechanical behavior of beryllium are required. However, current models are not sufficiently microstructure aware to accurately predict the performance of beryllium under a range of processing and loading conditions. Previous experiments conducted using the SMARTS and HIPPO instruments at the Lujan Center(LANL), have studied the relationship between strain rate and texture development, but due to the limitations of neutron diffraction studies, it was not possible to measure the response of the material in real-time. In-situ diffraction experiments conducted at the Advanced Photon Source have allowed the real time measurement of the mechanical response of compressed beryllium. Samples of pre-strained beryllium were reloaded orthogonal to their original load path to show the reorientation of already twinned grains. Additionally, the in-situ experiments allowed the real time tracking of twin evolution in beryllium strained at high rates. The data gathered during these experiments will be used in the development and validation of a new, microstructure aware model of the constitutive behavior of beryllium.

  13. The application of in-situ 3D X-ray diffraction in annealing experiments: First interpretation of substructure development in deformed NaCl

    DEFF Research Database (Denmark)

    Borthwick, Verity; Schmidt, Søren; Piazolo, Sandra

    2012-01-01

    In-situ 3D X-ray diffraction (3DXRD) annealing experiments were conducted at the ID-11 beamline at the European Synchrotron Radiation Facility in Grenoble. This allowed us to nondestructively document and subsequently analyse the development of substructures during heating, without the influence ...

  14. 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...

  15. Structural Investigation of Sodium Layered Oxides Via in Situ Synchrotron X-Ray Diffraction

    DEFF Research Database (Denmark)

    Jung, Young Hwa; Christiansen, Ane Sælland; Johnsen, Rune

    2015-01-01

    Sodium layered oxides with mixed transition metals have received significant attention as positive electrode candidates for sodium-ion batteries due to high reversible capacity. Sodium layered oxides would be more promising candidates than lithium-compounds in terms of high stability of MO2 slabs...... after extraction of Na induced from larger ionic size of Na. In addition, rich crystal chemistry for sodium layered compounds is available since larger Na+ ion is stable in more spacious prismatic site as compared to Li+ ion. In view of this, the phase transformation of layered compounds during......-situ synchrotron XRD experiments. A capillary Na-based cell is designed to minimize interference in other substances such as a separator or external battery parts. This approach could give us to obtain clear diffraction patterns with high intensity during electrochemical reaction in a short period of time without...

  16. Seasonal variation in trace and minor elements in Brazilian honey by total reflection X-ray fluorescence.

    Science.gov (United States)

    de Oliveira Resende Ribeiro, Roberta; Mársico, Eliane Teixeira; da Silva Carneiro, Carla; Simoes, Julia Siqueira; da Silva Ferreira, Micheli; de Jesus, Edgar Francisco Oliveira; Almeida, Eduardo; Junior, Carlos Adam Conte

    2015-03-01

    Honey is used as an alternative medicine and is a constituent of a healthy diet worldwide. Its composition is associated with botanical origin and, to some extent, geographical origin because soil and climate characteristics determine the melliferous flora. Also, the elements content in honey samples could give an indication of environmental pollution or geographical origin. The main purpose of this study was to evaluate seasonal patterns of essential elements of Brazilian honey. Honey was collected during spring, summer, autumn, and winter for 2 years to quantify K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Se, Br, and Sr using total reflection X-ray fluorescence spectroscopy (TXRF). Our results indicate no seasonal differences in concentration of Cr, Ni, Se, and Ti, although there were significant seasonal patterns in the composition of essential elements in honey, with higher concentrations of minor and trace elements, especially K and Ca of samples collected in spring and summer.

  17. CO adsorption on Pd(100) studied by multimodal ambient pressure X-ray photoelectron and infrared reflection absorption spectroscopies

    Science.gov (United States)

    Head, Ashley R.; Karslıoǧlu, Osman; Gerber, Timm; Yu, Yi; Trotochaud, Lena; Raso, Joseph; Kerger, Philipp; Bluhm, Hendrik

    2017-11-01

    The adsorption of CO on Pd(100) was investigated using simultaneous ambient pressure X-ray photoelectron spectroscopy (APXPS) and infrared reflection absorption infrared spectroscopy (IRRAS). The measurements were performed as a function of CO partial pressures from ultra-high vacuum to 0.5 Torr. Total CO coverages estimated from the complementary APXPS and IRRAS measurements are in good agreement. A signal for atop CO, which is uncommon for Pd(100), was observed in the IRRAS data and was used to identify the C 1 s binding energy of this species. Discerning this binding configuration of CO on the Pd(100) surface at elevated pressures has significance for catalytic reactions involving CO, where bridging CO is often the only configuration considered. We also detail the combined APXPS/IRRAS instrumentation and discuss ways to improve these multimodal measurements, which should have wide applicability across many areas of surface and interface science.

  18. Multielemental analysis in organic products and seed of linum by X-ray total reflection fluorescence with synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Serpa, Renata F.B.; Jesus, Edgar F.O. de; Lopes, Ricardo T. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Coordenacao dos Programas de Pos-graduacao de Engenharia. Lab. de Instrumentacao Nuclear]. E-mail: renata@lin.ufrj.br; Carmo, Maria da Graca T. do [Universidade Federal, Rio de Janeiro, RJ (Brazil). Inst. de Nutricao; Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil]. E-mail: silvana@fec.com.br

    2005-07-01

    The main goal of this study is to determining the trace and major elements levels in organic seeds samples, like soy, rice, bean and in Brazilian and Canadian linum seed by X-ray Total Reflection Fluorescence with Synchrotron Radiation (SR-TXRF). The measurements were carried out in the XRF beamline at the Light Synchrotron National Laboratory (Campinas, Brazil). The organic soy presented major concentrations of P, Ca, Ti, Fe, Ni, Cu, Zn, Br, Rb and Sr than organic bean and rice. Brazilian linum samples presented higher concentrations of S, P, Ca, Ni, Cu, Sr, Zr and Mo than Canadian one, even than organic samples. However potassium, iron and zinc were more pronounced in the Canadian seed of linum (author)

  19. Application of x-ray reflectivity measurement to monitoring of chemical reactions at 'buried' interface

    Energy Technology Data Exchange (ETDEWEB)

    Ishii, Masashi; Nakao, Aiko [RIKEN, 2-1, Hirosawa, Wako, Saitama 351-0198 (Japan); Sakurai, Kenji [National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan)

    2007-10-15

    A metal/yttria interface reaction by low temperature treatment at 100 {sup 0}C was chased by X-ray reflectivity measurement (XRR). Since the soft reaction did not affect surface morphology, it was not detectable by atomic force microscopy. The XRR results indicated that the structural change at Au/Y{sub 2}O{sub 3} interface was more significant than Pr/Y{sub 2}O{sub 3}. This difference can be explained by non-oxidization property of Au; the Au/Y{sub 2}O{sub 3} interface easily releases O atom, resulting in instability at the interface. The soft reaction of metal/Y{sub 2}O{sub 3} would be applicable to post-formation of nano-interface structures. For electronic device applications, since monitoring of microscopic reaction is mandatory, {mu}-XRR should be developed.

  20. Fish samples as bioindicator of environmental quality: synchrotron radiation total reflection X-ray fluorescence analysis (SR-TXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Vives, Ana Elisa Sirito de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: Silvana@fec.unicamp.br; Brienza, Sandra Maria Boscolo [Universidade Metodista de Piracicaba (UNIMEP), SP (Brazil). Faculdade de Ciencias Matematicas, da Natureza e de Tecnologia da Informacao]. E-mail: sbrienza@unimep.br; Zucchi, Orgheda Luiza Araujo Domingues [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas]. E-mail: olzucchi@fcfrp.usp.br; Nascimento Filho, Virgilio Franco do [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil)]. E-mail: virgilio@cena.usp.br

    2005-07-01

    In this study fish were used as bioindicators of environmental contamination. The species were collected in Piracicaba River, Sao Paulo state, Brazil and the toxic elements concentrations were determined in muscle tissue and viscus (liver, intestine and stomach) by Synchrotron Radiation Total Reflection X-Ray Fluorescence Analysis (SR-TXRF). Were determined the elements Ti, Cr, Mn, Fe, Ni, Cu, Zn and Ba. The results were compared with values established by Brazilian Legislation for general food. The elements concentrations evidenced potential risk to human health and environmental quality alteration of the studied area. The measurements were realized at the 'Laboratorio Nacional de Luz Sincrotron' (LNLS) located in Campinas, Sao Paulo State, Brazil. (author)

  1. Determination of multilayer thicknesses of GaAs/AlAs superlattice by grazing incidence X-ray reflectivity

    Directory of Open Access Journals (Sweden)

    Ren L.L.

    2013-01-01

    Full Text Available The grazing incidence X-ray reflectivity is used to determine the multilayer thickness of GaAs/AlAs supperlattice. The measurement process includes the fitting model and the measurement conditions (different powers of 45 kV × 40 mA, 40 kV × 40 mA and 35 kV × 40 mA, different step sizes of 0.005°, 0.008° and 0.010°, and different times per step of 1 s, 2 s, 3 s. In order to obtain the valid measurement process, the combined standard deviation is used as the normal of the fitting results selection. As a result, the measurement condition of 0.008° step size and 2 s time per step with the power 40 kV × 40 mA is selectable with the operation stability of facilities and smaller error.

  2. Diffusion of Ag into organic semiconducting materials: a combined analytical study using transmission electron microscopy and X-ray reflectivity.

    Science.gov (United States)

    Fladischer, Stefanie; Neuhold, Alfred; Kraker, Elke; Haber, Thomas; Lamprecht, Bernhard; Salzmann, Ingo; Resel, Roland; Grogger, Werner

    2012-10-24

    This study shows that the morphology of organic/metal interfaces strongly depends on process parameters and the involved materials. The interface between organic n-type blocking layer materials and the top Ag cathode within an organic photodiode was investigated. Ag was deposited on either amorphous tris-8-hydroxyquinolinato-aluminum (Alq(3)) or crystalline 4,7-diphenyl-1,10-phenanthroline (Bphen) using different deposition techniques such as electron beam deposition, ion beam sputtering, and vacuum thermal evaporation at various deposition rates. The interfaces were studied by transmission electron microscopy and X-ray reflectivity. It was found that Bphen does not show any Ag diffusion no matter which deposition technique was used, whereas the Ag diffusion into Alq(3) depends on the deposition technique and the deposition rate. The highest amount of Ag diffusion into Alq(3) occurred by using thermal vacuum deposition at low deposition rates.

  3. On the origin of the hydrophobic water gap: An X-ray reflectivity and MD simulation study.

    Science.gov (United States)

    Mezger, Markus; Sedlmeier, Felix; Horinek, Dominik; Reichert, Harald; Pontoni, Diego; Dosch, Helmut

    2010-05-19

    The density deficit of water at hydrophobic interfaces, frequently called the hydrophobic gap, has been the subject of numerous experimental and theoretical studies in the past decade. Recent experiments give values for the interfacial depletion that consistently correspond to less than a monolayer of water. The main question which remained so far unanswered is its origin and the mechanisms affected by the chemistry and molecular geometry of a particular hydrophobic coating. In this work, we present a combined high-energy X-ray reflectivity and molecular dynamics simulation study of the water depletion at a perfluorinated hydrophobic interface with a spatial resolution on the molecular scale. A comparison of our experimental and computational results elucidates the underlying mechanisms that affect the extent of the interfacial depletion. The complex interplay between surface chemistry and topography precludes the existence of a direct and universal relation between the macroscopic contact angle and the nanoscopic water depletion.

  4. Insight into the structure of Pd/ZrO2 during the total oxidation of methane using combined in situ XRD, X.-ray absorption and Raman spectroscopy

    DEFF Research Database (Denmark)

    Grunwaldt, Jan-Dierk; van Vegten, Niels; Baiker, Alfons

    2009-01-01

    The structure of palladium during the total combustion of methane has been studied by a combination of the complementary in situ techniques X-ray absorption spectroscopy, Raman spectroscopy and X-ray diffraction. The study demonstrates that finely dispersed and oxidized palladium is most active...... for the oxidation of methane. Upon heating in the reaction mixture a sudden reduction accompanied by strong sintering of the palladium particles occurs leading to a less active catalyst. Raman spectroscopy combined with XAS shows that palladium is re-oxidized during cooling but is not as finely dispersed as in its...

  5. Submicrometer-resolution in situ imaging of the focus pattern of a soft x-ray laser by color center formation in LiF crystal.

    Science.gov (United States)

    Faenov, A Ya; Kato, Y; Tanaka, M; Pikuz, T A; Kishimoto, M; Ishino, M; Nishikino, M; Fukuda, Y; Bulanov, S V; Kawachi, T

    2009-04-01

    We demonstrate high quality, single-shot in situ imaging of the focused Ag x-ray laser (XRL) at 13.9 nm with 700 nm spatial resolution by color center formation in LiF. The flux and intensity for the color center formation in LiF are evaluated from the experimental data. Comparisons with previous reports show that the threshold x-ray flux for the color center formation in LiF for the 13.9 nm, 7 ps Ag XRL is 3 orders of magnitude less than that with the 46.9 nm, 2 ns capillary discharge Ar XRL.

  6. In-situ small-angle x-ray scattering study of nanoparticles in the plasma plume induced by pulsed laser irradiation of metallic targets

    Energy Technology Data Exchange (ETDEWEB)

    Lavisse, L.; Jouvard, J.-M.; Girault, M.; Potin, V.; Andrzejewski, H.; Marco de Lucas, M. C.; Bourgeois, S. [Laboratoire Interdisciplinaire Carnot de Bourgogne (ICB), UMR 6303 CNRS-Universite de Bourgogne, 9 Avenue A. Savary, BP 47870-21078 Dijon Cedex (France); Le Garrec, J.-L.; Carles, S.; Mitchell, J. B. A. [Institut de Physique de Rennes, UMR 6251 CNRS-Universite de Rennes 1, 35042 Rennes Cedex (France); Hallo, L. [CEA CESTA, 15 Avenue des Sablieres CS 60001, 33116 Le Barp Cedex (France); Perez, J. [Synchrotron SOLEIL, L' Orme des Merisiers, Saint-Aubin, F-91192 Gif-sur-Yvette Cedex (France); Decloux, J. [Kaluti System, Optique et Laser, Centre Scientifique d' Orsay, 91400 Orsay (France)

    2012-04-16

    Small angle x-ray scattering was used to probe in-situ the formation of nanoparticles in the plasma plume generated by pulsed laser irradiation of a titanium metal surface under atmospheric conditions. The size and morphology of the nanoparticles were characterized as function of laser irradiance. Two families of nanoparticles were identified with sizes on the order of 10 and 70 nm, respectively. These results were confirmed by ex-situ transmission electron microscopy experiments.

  7. In-Situ Additive Manufacturing Platform for Neutron, X-ray and Proton Beamlines

    Science.gov (United States)

    Cooley, Jason C.; Brown, Donald B.; Carpenter, John S.; Clausen, Bjorn; Cross, Carl E.; Lienert, Thomas J.; Bernal, John E.; Losko, Adrian S.

    Advanced manufacturing offers the promise to make high value components with complex shapes without complex machining or significant material waste on short notice. There are however significant technical barriers to overcome with focused research and development. In the case of metallic parts made by melting and depositing wire or powder, additive manufacturing results in repetitive heating and cooling of the deposited material. The thermal gradients imposed are significantly higher than typically encountered during casting. These gradients produce residual stresses we cannot currently predict and can cause the formation of undesirable secondary phases. Efforts to accurately predict the final state of materials manufactured additively will require an understanding of the time evolution of the microstructure which includes intertwined residual stresses, texture, and chemical inhomogeneity. The best way to understand these linked effects is to measure their evolution in-situ during the deposition process. In order to do this a prototype device for making quasi 1-D features while making real time beamline measurements (radiography and diffraction) has been built and recently tested. Work funded by the Department of Energy under Contract Number DEAC5206NA25396.

  8. Analysis of neutron and x-ray reflectivity data by constrained least-squares methods

    DEFF Research Database (Denmark)

    Pedersen, J.S.; Hamley, I.W.

    1994-01-01

    Two methods for the determination of scattering length density profiles from specular reflectivity data are discussed. For either method kinematical or dynamical theory can be used to calculate the reflectivity. In the first method the scattering density is parametrized using cubic splines...... of the higher harmonics in the Fourier series. The two methods for analyzing reflectivity data have been applied to sets of simulated data based on examples from the literature. The two methods work equally well in most situations, and they are able to recover the original profiles. In general, the method using...

  9. Non-destructive in situ study of “Mad Meg” by Pieter Bruegel the Elder using mobile X-ray fluorescence, X-ray diffraction and Raman spectrometers

    Energy Technology Data Exchange (ETDEWEB)

    Van de Voorde, Lien, E-mail: lien.vandevoorde@ugent.be [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Van Pevenage, Jolien [Ghent University, Department of Analytical Chemistry, Raman Spectroscopy Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); De Langhe, Kaat [Ghent University, Department of Archaeology, Archaeometry Research Group, Sint-Pietersnieuwstraat 35, B-9000 Gent (Belgium); De Wolf, Robin; Vekemans, Bart; Vincze, Laszlo [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Vandenabeele, Peter [Ghent University, Department of Archaeology, Archaeometry Research Group, Sint-Pietersnieuwstraat 35, B-9000 Gent (Belgium); Martens, Maximiliaan P.J. [Ghent University, Department of Art, Music and Theatre Sciences, Blandijnberg 2, B-9000 Gent (Belgium)

    2014-07-01

    “Mad Meg”, a figure of Flemish folklore, is the subject of a famous oil-on-panel painting by the Flemish renaissance artist Pieter Bruegel the Elder, exhibited in the Museum Mayer van den Bergh (Antwerp, Belgium). This article reports on the in situ chemical characterization of this masterpiece by using currently available state-of-the-art portable analytical instruments. The applied non-destructive analytical approach involved the use of a) handheld X-ray fluorescence instrumentation for retrieving elemental information and b) portable X-ray fluorescence/X-ray diffraction instrumentation and laser-based Raman spectrometers for obtaining structural/molecular information. Next to material characterization of the used pigments and of the different preparation layers of the painting, also the verification of two important historical iconographic hypotheses is performed concerning the economic way of painting by Brueghel, and whether or not he used blue smalt pigment for painting the boat that appears towards the top of the painting. The pigments identified are smalt pigment (65% SiO{sub 2} + 15% K{sub 2}O + 10% CoO + 5% Al{sub 2}O{sub 3}) for the blue color present in all blue areas of the painting, probably copper resinate for the green colors, vermillion (HgS) as red pigment and lead white is used to form different colors. The comparison of blue pigments used on different areas of the painting gives no differences in the elemental fingerprint which confirms the existing hypothesis concerning the economic painting method by Bruegel. - Highlights: • In situ, non-destructive investigation of a famous painting by Pieter Bruegel. • Use of a new, commercial available, portable XRF/XRD instrumentation. • Multi-methodological approach: make also use of a mobile Raman spectrometer. • Used pigments and different preparation layers of the painting are characterized. • The verification of two important historical iconographic hypotheses are performed.

  10. Development of a new micro-furnace for "in situ" high-temperature single crystal X-ray diffraction measurements

    Science.gov (United States)

    Alvaro, Matteo; Angel, Ross J.; Marciano, Claudio; Zaffiro, Gabriele; Scandolo, Lorenzo; Mazzucchelli, Mattia L.; Milani, Sula; Rustioni, Greta; Domeneghetti, Chiara M.; Nestola, Fabrizio

    2015-04-01

    Several experimental methods to reliably determine elastic properties of minerals at non-ambient conditions have been developed. In particular, different techniques for generating high-pressure and high-temperature have been successfully adopted for single-crystal and powder X-ray diffraction measurements. High temperature devices for "in-situ" measurements should provide the most controlled isothermal environment as possible across the entire sample. It is intuitive that in general, thermal gradients across the sample increase as the temperature increases. Even if the small isothermal volume required for single-crystal X-ray diffraction experiments makes such phenomena almost negligible, the design of a furnace should also aim to reduce thermal gradients by including a large thermal mass that encloses the sample. However this solution often leads to complex design that results in a restricted access to reciprocal space or attenuation of the incident or diffracted intensity (with consequent reduction of the accuracy and/or precision in lattice parameter determination). Here we present a newly-developed H-shaped Pt-Pt/Rh resistance microfurnace for in-situ high-temperature single-crystal X-ray diffraction measurements. The compact design of the furnace together with the long collimator-sample-detector distance allows us to perform measurements up to 2θ = 70° with no further restrictions on any other angular movement. The microfurnace is equipped with a water cooling system that allows a constant thermal gradient to be maintained that in turn guarantees thermal stability with oscillations smaller than 5°C in the whole range of operating T of room-T to 1200°C. The furnace has been built for use with a conventional 4-circle Eulerian geometry equipped with point detector and automated with the SINGLE software (Angel and Finger 2011) that allows the effects of crystal offsets and diffractometer aberrations to be eliminated from the refined peak positions by the 8

  11. In situ surface X-ray diffraction studies of the copper-electrolyte interface. Atomic structure and homoepitaxial grwoth

    Energy Technology Data Exchange (ETDEWEB)

    Golks, Frederik

    2011-05-19

    Copper electrodeposition is the predominantly used technique for on-chip wiring in the fabrication of ultra-large scale integrated (ULSI) microchips. In this 'damascene copper electroplating' process, multicomponent electrolytes containing organic additives realize void-free filling of trenches with high aspect ratio ('superconformal deposition'). Despite manifold studies, motivated by the continuous trend to shrink wiring dimensions and thus the demand of optimized plating baths, detailed knowledge on the growth mechanism - in presence and absence of additives - is still lacking. Using a recently developed hanging meniscus X-ray transmission cell, brilliant synchrotron x-rays and a fast, one-dimensional detector system, unique real-time in situ surface X-ray diffraction studies of copper electrodeposition were performed under realistic reaction conditions, approaching rates of technological relevance. Preparatory measurements of the electrochemical dissolution of Au(001) in chloride-containing electrolyte demonstrated the capability of this powerful technique, specifically the possibility to follow atomic-scale deposition or dissolution processes with a time resolution down to five milliseconds. The electrochemical as well as structural characterization of the Cu(001)- and Cu(111)-electrolyte interfaces provided detailed insight into the complex atomic-scale structures in presence of specifically adsorbed chloride on these surfaces. The interface of Cu(001) in chloride-containing electrolyte exhibits a continuous surface phase transition of a disordered Cl adlayer to a c(2 x 2) Cl adlayer with increasing potential. The latter was found to induce a small vertical corrugation of substrate atoms, which can be ascribed to lattice relaxations induced by the presence of coadsorbed water molecules and cations in the outer part of the electrochemical double layer. The study of the specific adsorption of chloride on Cu(111) from acidic aqueous

  12. Capillary-based micro-battery cell for in situ X-ray powder diffraction studies of working batteries: a study of the initial intercalation and deintercalation of lithium into graphite

    DEFF Research Database (Denmark)

    Johnsen, Rune; Norby, Poul

    2013-01-01

    to obtain diffraction from a single electrode at a time, which facilitates detailed structural and microstructural studies of the electrode materials. The micro-battery cell is potentially also applicable for in situ X-ray absorption spectroscopy and smallangle X-ray scattering experiments. The in situ XRPD...

  13. Room temperature redox reaction by oxide ion migration at carbon/Gd-doped CeO2 heterointerface probed by an in situ hard x-ray photoemission and soft x-ray absorption spectroscopies

    Directory of Open Access Journals (Sweden)

    Takashi Tsuchiya, Shogo Miyoshi, Yoshiyuki Yamashita, Hideki Yoshikawa, Kazuya Terabe, Keisuke Kobayashi and Shu Yamaguchi

    2013-01-01

    Full Text Available In situ hard x-ray photoemission spectroscopy (HX-PES and soft x-ray absorption spectroscopy (SX-XAS have been employed to investigate a local redox reaction at the carbon/Gd-doped CeO2 (GDC thin film heterointerface under applied dc bias. In HX-PES, Ce3d and O1s core levels show a parallel chemical shift as large as 3.2 eV, corresponding to the redox window where ionic conductivity is predominant. The window width is equal to the energy gap between donor and acceptor levels of the GDC electrolyte. The Ce M-edge SX-XAS spectra also show a considerable increase of Ce3+ satellite peak intensity, corresponding to electrochemical reduction by oxide ion migration. In addition to the reversible redox reaction, two distinct phenomena by the electrochemical transport of oxide ions are observed as an irreversible reduction of the entire oxide film by O2 evolution from the GDC film to the gas phase, as well as a vigorous precipitation of oxygen gas at the bottom electrode to lift off the GDC film. These in situ spectroscopic observations describe well the electrochemical polarization behavior of a metal/GDC/metal capacitor-like two-electrode cell at room temperature.

  14. Solid state synthesis of layered sodium manganese oxide for sodium-ion battery by in-situ high energy X-ray diffraction and X-ray absorption near edge spectroscopy

    Science.gov (United States)

    Ma, Tianyuan; Xu, Gui-Liang; Zeng, Xiaoqiao; Li, Yan; Ren, Yang; Sun, Chengjun; Heald, Steve M.; Jorne, Jacob; Amine, Khalil; Chen, Zonghai

    2017-02-01

    In situ high energy X-ray diffraction (HEXRD) and in situ X-ray absorption near edge spectroscopy (XANES) were carried out to understand the solid state synthesis of NaxMnO2, with particular interest on the synthesis of P2 type Na2/3MnO2. It was found that there were multi intermediate phases formed before NaMnO2 appeared at about 600 °C. And the final product after cooling process is a combination of O‧3 NaMnO2 with P2 Na2/3MnO2. A P2 type Na2/3MnO2 was synthesized at reduced temperature (600 °C). The influence of Na2CO3 impurity on the electrochemical performance of P2 Na2/3MnO2 was thoroughly investigated in our work. It was found that the content of Na2CO3 can be reduced by optimizing Na2CO3/MnCO3 ratio during the solid state reaction or other post treatment such as washing with water. We expected our results could provide a good guide for future development of high performance cathode materials for sodium-ion batteries.

  15. Electrochemical (de)lithiation of silver ferrite and composites: mechanistic insights from ex situ, in situ, and operando X-ray techniques.

    Science.gov (United States)

    Durham, Jessica L; Brady, Alexander B; Cama, Christina A; Bock, David C; Pelliccione, Christopher J; Zhang, Qing; Ge, Mingyuan; Li, Yue Ru; Zhang, Yiman; Yan, Hanfei; Huang, Xiaojing; Chu, Yong; Takeuchi, Esther S; Takeuchi, Kenneth J; Marschilok, Amy C

    2017-08-23

    The structure of pristine AgFeO2 and phase makeup of Ag0.2FeO1.6 (a one-pot composite comprised of nanocrystalline stoichiometric AgFeO2 and amorphous γ-Fe2O3 phases) was investigated using synchrotron X-ray diffraction. A new stacking-fault model was proposed for AgFeO2 powder synthesized using the co-precipitation method. The lithiation/de-lithiation mechanisms of silver ferrite, AgFeO2 and Ag0.2FeO1.6 were investigated using ex situ, in situ, and operando characterization techniques. An amorphous γ-Fe2O3 component in the Ag0.2FeO1.6 sample is quantified. Operando XRD of electrochemically reduced AgFeO2 and Ag0.2FeO1.6 composites demonstrated differences in the structural evolution of the nanocrystalline AgFeO2 component. As complimentary techniques to XRD, ex situ X-ray Absorption Spectroscopy (XAS) provided insight into the short-range structure of the (de)lithiated nanocrystalline electrodes, and a novel in situ high energy X-ray fluorescence nanoprobe (HXN) mapping measurement was applied to spatially resolve the progression of discharge. Based on the results, a redox mechanism is proposed where the full reduction of Ag(+) to Ag(0) and partial reduction of Fe(3+) to Fe(2+) occur on reduction to 1.0 V, resulting in a Li1+yFe(III)Fe(II)yO2 phase. The Li1+yFe(III)Fe(II)yO2 phase can then reversibly cycle between Fe(3+) and Fe(2+) oxidation states, permitting good capacity retention over 50 cycles. In the Ag0.2FeO1.6 composite, a substantial amorphous γ-Fe2O3 component is observed which discharges to rock salt LiFe2O3 and Fe(0) metal phase in the 3.5-1.0 V voltage range (in parallel with the AgFeO2 mechanism), and reversibly reoxidizes to a nanocrystalline iron oxide phase.

  16. Performance Evaluation of a Microchannel Plate based X-ray Camera with a Reflecting Grid

    Science.gov (United States)

    Visco, A.; Drake, R. P.; Harding, E. C.; Rathore, G. K.

    2006-10-01

    Microchannel Plates (MCPs) are used in a variety of imaging systems as a means of amplifying the incident radiation. Using a microchannel plate mount recently developed at the University of Michigan, the effects of a metal reflecting grid are explored. Employing the reflecting grid, we create a potential difference above the MCP input surface that forces ejected electrons back into the pores, which may prove to increase the quantum efficiency of the camera. We investigate the changes in the pulse height distribution, modular transfer function, and Quantum efficiency of MCPs caused by the introduction of the reflecting grid. Work supported by the Naval Research Laboratory, National Nuclear Security Administration under the Stewardship Science Academic Alliances program through DOE Research Grant DE-FG52-03NA00064, and through DE FG53 2005 NA26014, and Livermore National Laboratory.

  17. In situ x-ray diffraction studies of alkyl quaternary ammonium montmorillonite in a CO2 environment

    Science.gov (United States)

    Thompson, M. R.; Balogh, M. P.; Speer, R. L.; Fasulo, P. D.; Rodgers, W. R.

    2009-01-01

    An in situ study was conducted using an x-ray diffractometer and a specially designed high pressure cell to examine the effects of carbon dioxide at different pressures and temperatures on three different modified montmorillonite species. These organoclays possessed organic pillars of quaternary ammonium surfactant with either one, two, or three long (C16-C18) alkyl chains attached to expand the galleries of the clay mineral. The three clay species were tested between 50 °C and 200 °C with carbon dioxide pressures between 0.1 and 8.4 MPa. Under these conditions, the three organoclays exhibited marked differences in their basal spacing depending on the surfactant used. The physical state of the intercalated surfactant was found to be of critical importance, with no changes in basal spacing noted until the organic component began to melt, in spite of CO2 being present. A pressure effect was also noted which delayed melting of the surfactants as the pressure of the system increased. In all cases, further cation exchange with residual sodium cation present in the galleries was observed in the presence of CO2 and above the melting state of the surfactant. The study included examination of the effect of rapid depressurization on the clay structure, which produced only a small change in basal spacing.

  18. In situ compressibility of carbonated hydroxyapatite in tooth dentine measured under hydrostatic pressure by high energy X-ray diffraction.

    Science.gov (United States)

    Forien, Jean-Baptiste; Fleck, Claudia; Krywka, Christina; Zolotoyabko, Emil; Zaslansky, Paul

    2015-10-01

    Tooth dentine and other bone-like materials contain carbonated hydroxyapatite nanoparticles within a network of collagen fibrils. It is widely assumed that the elastic properties of biogenic hydroxyapatites are identical to those of geological apatite. By applying hydrostatic pressure and by in situ measurements of the a- and c- lattice parameters using high energy X-ray diffraction, we characterize the anisotropic deformability of the mineral in the crowns and roots of teeth. The collected data allowed us to calculate the bulk modulus and to derive precise estimates of Young׳s moduli and Poisson׳s ratios of the biogenic mineral particles. The results show that the dentine apatite particles are about 20% less stiff than geological and synthetic apatites and that the mineral has an average bulk modulus K=82.7 GPa. A 5% anisotropy is observed in the derived values of Young׳s moduli, with E11≈91 GPa and E33≈96 GPa, indicating that the nanoparticles are only slightly stiffer along their long axis. Poisson׳s ratio spans ν≈0.30-0.35, as expected. Our findings suggest that the carbonated nanoparticles of biogenic apatite are significantly softer than previously thought and that their elastic properties can be considered to be nearly isotropic. Copyright © 2015 Elsevier Ltd. All rights reserved.

  19. In Situ Ambient Pressure X-ray Photoelectron Spectroscopy of Cobalt Perovskite Surfaces under Cathodic Polarization at High Temperatures

    KAUST Repository

    Crumlin, Ethan J.

    2013-08-08

    Heterostructured oxide interfaces have demonstrated enhanced oxygen reduction reaction rates at elevated temperatures (∼500-800 C); however, the physical origin underlying this enhancement is not well understood. By using synchrotron-based in situ ambient pressure X-ray photoelectron spectroscopy (APXPS), we focus on understanding the surface electronic structure, elemental composition, and chemical nature of epitaxial La0.8Sr 0.2CoO3-δ (LSC113), (La 0.5Sr0.5)2CoO4±δ (LSC214), and LSC214-decorated LSC113 (LSC 113/214) thin films as a function of applied electrical potentials (0 to -800 mV) at 520 C and p(O2) of 1 × 10-3 atm. Shifts in the top of the valence band binding energy and changes in the Sr 3d and O 1s spectral components under applied bias reveal key differences among the film chemistries, most notably in the degree of Sr segregation to the surface and quantity of active oxygen sites in the perovskite termination layer. These differences help to identify important factors governing the enhanced activity of oxygen electrocatalysis observed for the LSC113/214 heterostructured surface. © 2013 American Chemical Society.

  20. Temperature Assisted in-Situ Small Angle X-ray Scattering Analysis of Ph-POSS/PC Polymer Nanocomposite

    Science.gov (United States)

    Yadav, Ramdayal; Naebe, Minoo; Wang, Xungai; Kandasubramanian, Balasubramanian

    2016-07-01

    Inorganic/organic nanofillers have been extensively exploited to impart thermal stability to polymer nanocomposite via various strategies that can endure structural changes when exposed a wide range of thermal environment during their application. In this abstraction, we have utilized temperature assisted in-situ small angle X-ray scattering (SAXS) to examine the structural orientation distribution of inorganic/organic nanofiller octa phenyl substituted polyhedral oligomeric silsesquioxane (Ph-POSS) in Polycarbonate (PC) matrix from ambient temperature to 180 °C. A constant interval of 30 °C with the heating rate of 3 °C/min was utilized to guise the temperature below and above the glass transition temperature of PC followed by thermal gravimetric, HRTEM, FESEM and hydrophobic analysis at ambient temperature. The HRTEM images of Ph-POSS nano unit demonstrated hyperrectangular structure, while FESEM image of the developed nano composite rendered separated phase containing flocculated and overlapped stacking of POSS units in the PC matrix. The phase separation in polymer nanocomposite was further substantiated by thermodynamic interaction parameter (χ) and mixing energy (Emix) gleaned via Accelrys Materials studio. The SAXS spectra has demonstrated duplex peak at higher scattering vector region, postulated as a primary and secondary segregated POSS domain and followed by abundance of secondary peak with temperature augmentation.

  1. Grazing incidence reflectivity and total electron yield effects in soft x-ray absorption spectroscopy

    NARCIS (Netherlands)

    Alders, D; Hibma, T; Sawatzky, G.A; Cheung, K.C.; van Dorssen, G.E.; Roper, M.D.; Padmore, H.A.; van der Laan, G.; Vogel, J; Sacchi, M.

    1997-01-01

    We report on a study of grazing incidence absorption and reflection spectra of NiO in the region of the Ni 2p edge. The aim is to evaluate the distortion of the near edge spectrum by the critical angle behavior of individual components within the spectrum. This can be used to improve the separation

  2. Portable energy dispersive X-ray fluorescence and X-ray diffraction and radiography system for archaeometry

    Energy Technology Data Exchange (ETDEWEB)

    Mendoza Cuevas, Ariadna, E-mail: ariadna@mail.or [Archaeometry Laboratory, Colegio Universitario San Geronimo de La Habana, Obispo, entre San Ignacio y Mercaderes, Habana Vieja, cp 10 100, Havana (Cuba); Perez Gravie, Homero, E-mail: homero.perezgravie@mail.co [Archaeometry Laboratory, Colegio Universitario San Geronimo de La Habana, Obispo, entre San Ignacio y Mercaderes, Habana Vieja, cp 10 100, Havana (Cuba)

    2011-03-21

    Starting on a laboratory developed portable X-ray fluorescence (PXRF) spectrometer; three different analytical results can be performed: analysis of chemical elements, analysis of major chemical crystalline phase and structural analysis, which represents a contribution to a new, low cost development of portable X-ray analyzer; since these results are respectively obtained with independent equipments for X-ray fluorescence, X-ray diffraction and radiography. Detection limits of PXRF were characterized using standard reference materials for ceramics, glass, bronze and bones, which are the main materials requiring quantitative analysis in art and archeological objects. A setup for simultaneous energy dispersive X-ray fluorescence and diffraction (ED (XRF-XRD)) in the reflection mode has been tested for in situ and non-destructive analysis according to the requirements of art objects inspection. The system uses a single low power X-ray tube and an X-ray energy dispersive detector to measure X-ray diffraction spectrum at a fixed angle. Application to the identification of jadeite-jade mineral in archeological objects by XRD is presented. A local high resolution radiography image obtained with the same low power X-ray tube allows for studies in painting and archeological bones.

  3. X-ray diffraction and reflectivity validation of the depletion attraction in the competitive adsorption of lung surfactant and albumin.

    Science.gov (United States)

    Stenger, Patrick C; Wu, Guohui; Miller, Chad E; Chi, Eva Y; Frey, Shelli L; Lee, Ka Yee C; Majewski, Jaroslaw; Kjaer, Kristian; Zasadzinski, Joseph A

    2009-08-05

    Lung surfactant (LS) and albumin compete for the air-water interface when both are present in solution. Equilibrium favors LS because it has a lower equilibrium surface pressure, but the smaller albumin is kinetically favored by faster diffusion. Albumin at the interface creates an energy barrier to subsequent LS adsorption that can be overcome by the depletion attraction induced by polyethylene glycol (PEG) in solution. A combination of grazing incidence x-ray diffraction (GIXD), x-ray reflectivity (XR), and pressure-area isotherms provides molecular-resolution information on the location and configuration of LS, albumin, and polymer. XR shows an average electron density similar to that of albumin at low surface pressures, whereas GIXD shows a heterogeneous interface with coexisting LS and albumin domains at higher surface pressures. Albumin induces a slightly larger lattice spacing and greater molecular tilt, similar in effect to a small decrease in the surface pressure. XR shows that adding PEG to the LS-albumin subphase restores the characteristic LS electron density profile at the interface, and confirms that PEG is depleted near the interface. GIXD shows the same LS Bragg peaks and Bragg rods as on a pristine interface, but with a more compact lattice corresponding to a small increase in the surface pressure. These results confirm that albumin adsorption creates a physical barrier that inhibits LS adsorption, and that PEG in the subphase generates a depletion attraction between the LS aggregates and the interface that enhances LS adsorption without substantially altering the structure or properties of the LS monolayer.

  4. A novel vacuum spectrometer for total reflection x-ray fluorescence analysis with two exchangeable low power x-ray sources for the analysis of low, medium, and high Z elements in sequence.

    Science.gov (United States)

    Wobrauschek, P; Prost, J; Ingerle, D; Kregsamer, P; Misra, N L; Streli, C

    2015-08-01

    The extension of the detectable elemental range with Total Reflection X-ray Fluorescence (TXRF) analysis is a challenging task. In this paper, it is demonstrated how a TXRF spectrometer is modified to analyze elements from carbon to uranium. Based on the existing design of a vacuum TXRF spectrometer with a 12 specimen sample changer, the following components were renewed: the silicon drift detector with 20 mm(2) active area and having a special ultra-thin polymer window allowing the detection of elements from carbon upwards. Two exchangeable X-ray sources guarantee the efficient excitation of both low and high Z elements. These X-ray sources were two light-weighted easily mountable 35 W air-cooled low-power tubes with Cr and Rh anodes, respectively. The air cooled tubes and the Peltier-cooled detector allowed to construct a transportable tabletop spectrometer with compact dimensions, as neither liquid nitrogen cooling for the detector nor a water cooling circuit and a bulky high voltage generator for the X-ray tubes are required. Due to the excellent background conditions as a result of the TXRF geometry, detection limits of 150 ng for C, 12 ng for F, and 3.3 ng for Na have been obtained using Cr excitation in vacuum. For Rh excitation, the detection limits of 90 pg could be achieved for Sr. Taking 10 to 20 μl of sample volume, extrapolated detection limits in the ng/g (ppb) range are resulting in terms of concentration.

  5. A novel vacuum spectrometer for total reflection x-ray fluorescence analysis with two exchangeable low power x-ray sources for the analysis of low, medium, and high Z elements in sequence

    Energy Technology Data Exchange (ETDEWEB)

    Wobrauschek, P., E-mail: wobi@ati.ac.at; Prost, J.; Ingerle, D.; Kregsamer, P.; Streli, C. [Atominstitut, TU Wien, Stadionallee 2, 1020 Vienna (Austria); Misra, N. L. [Fuel Chemistry Division, Bhabha Atomic Research Centre (BARC), Mumbai 400085 (India)

    2015-08-15

    The extension of the detectable elemental range with Total Reflection X-ray Fluorescence (TXRF) analysis is a challenging task. In this paper, it is demonstrated how a TXRF spectrometer is modified to analyze elements from carbon to uranium. Based on the existing design of a vacuum TXRF spectrometer with a 12 specimen sample changer, the following components were renewed: the silicon drift detector with 20 mm{sup 2} active area and having a special ultra-thin polymer window allowing the detection of elements from carbon upwards. Two exchangeable X-ray sources guarantee the efficient excitation of both low and high Z elements. These X-ray sources were two light-weighted easily mountable 35 W air-cooled low-power tubes with Cr and Rh anodes, respectively. The air cooled tubes and the Peltier-cooled detector allowed to construct a transportable tabletop spectrometer with compact dimensions, as neither liquid nitrogen cooling for the detector nor a water cooling circuit and a bulky high voltage generator for the X-ray tubes are required. Due to the excellent background conditions as a result of the TXRF geometry, detection limits of 150 ng for C, 12 ng for F, and 3.3 ng for Na have been obtained using Cr excitation in vacuum. For Rh excitation, the detection limits of 90 pg could be achieved for Sr. Taking 10 to 20 μl of sample volume, extrapolated detection limits in the ng/g (ppb) range are resulting in terms of concentration.

  6. The Effects of High Density on the X-ray Spectrum Reflected from Accretion Discs Around Black Holes

    Science.gov (United States)

    Garcia, Javier A.; Fabian, Andrew C.; Kallman, Timothy R.; Dauser, Thomas; Parker, Micahel L.; McClintock, Jeffrey E.; Steiner, James F.; Wilms, Jorn

    2016-01-01

    Current models of the spectrum of X-rays reflected from accretion discs around black holes and other compact objects are commonly calculated assuming that the density of the disc atmosphere is constant within several Thomson depths from the irradiated surface. An important simplifying assumption of these models is that the ionization structure of the gas is completely specified by a single, fixed value of the ionization parameter (xi), which is the ratio of the incident flux to the gas density. The density is typically fixed at n(sub e) = 10(exp 15) per cu cm. Motivated by observations, we consider higher densities in the calculation of the reflected spectrum. We show by computing model spectra for n(sub e) approximately greater than 10(exp 17) per cu cm that high-density effects significantly modify reflection spectra. The main effect is to boost the thermal continuum at energies 2 approximately less than keV. We discuss the implications of these results for interpreting observations of both active galactic nuclei and black hole binaries. We also discuss the limitations of our models imposed by the quality of the atomic data currently available.

  7. Interferometric enhancement of x-ray reflectivity from unperturbed Langmuir monolayers of amphiphiles at the liquid-gas interface.

    Science.gov (United States)

    Krishnan, Venkata; Strzalka, Joseph; Liu, Jing; Liu, Chian; Kuzmenko, Ivan; Gog, Thomas; Blasie, J Kent

    2010-02-01

    Langmuir monolayers provide an important system for the investigation of the intramolecular structure and intermolecular ordering of organic and bio-organic macromolecular amphiphiles at an interface between polar and nonpolar media, e.g., the liquid-gas interface. Specular x-ray and neutron reflectivity have contributed substantially to these investigations. However, these reflectivity techniques are generally limited by the absence of crucial phase information, the relatively small contribution of the amphiphile to the scattering-length density contrast across the interface, and the relatively limited range of momentum transfer available perpendicular to the interface. Although several procedures have been developed to provide model-independent solutions to the phase problem, there remains a limited ability to distinguish features of slightly differing contrast (i.e., the "sensitivity") as well as their minimum allowable separation (i.e., the "spatial resolution") along the length of the scattering-length density profile derived from the reflectivity data via solution to the phase problem. Here, we demonstrate how the well-known interferometric approach can be extended to the structural investigation of otherwise unperturbed Langmuir monolayers of these amphiphiles to provide a direct solution to the phase problem and importantly, substantially enhance both the sensitivity and the spatial resolution in the derived profiles.

  8. Stability of a Bifunctional Cu-Based Core@Zeolite Shell Catalyst for Dimethyl Ether Synthesis Under Redox Conditions Studied by Environmental Transmission Electron Microscopy and In Situ X-Ray Ptychography

    DEFF Research Database (Denmark)

    Baier, Sina; Damsgaard, Christian Danvad; Klumpp, Michael

    2017-01-01

    gas. The catalyst stability was studied in a hierarchical manner by complementary environmental transmission electron microscopy (ETEM), scanning electron microscopy (SEM) and in situ hard X-ray ptychography with a specially designed in situ cell. Both reductive activation and reoxidation were applied....... The core-shell interface was found to be stable during reducing and oxidizing treatment at 250°C as observed by ETEM and in situ X-ray ptychography, although strong changes occurred in the core on a 10 nm scale due to the reduction of copper oxide to metallic copper particles. At 350°C, in situ X-ray...

  9. In Situ Synchrotron X-Ray Diffraction and Small Angle X-Ray Scattering Studies on Rapidly Heated and Cooled Ti-Al and Al-Cu-Mg Alloys Using Laser-Based Heating

    Science.gov (United States)

    Kenel, C.; Schloth, P.; Van Petegem, S.; Fife, J. L.; Grolimund, D.; Menzel, A.; Van Swygenhoven, H.; Leinenbach, C.

    2016-03-01

    Beam-based additive manufacturing (AM) typically involves high cooling rates in a range of 103-104 K/s. Therefore, new techniques are required to understand the non-equilibrium evolution of materials at appropriate time scales. Most technical alloys have not been optimized for such rapid solidification, and microstructural, phase, and elemental solubility behavior can be very different. In this work, the combination of complementary in situ synchrotron micro-x-ray diffraction (microXRD) and small angle x-ray scattering (SAXS) studies with laser-based heating and rapid cooling is presented as an approach to study alloy behavior under processing conditions similar to AM techniques. In rapidly solidified Ti-48Al, the full solidification and phase transformation sequences are observed using microXRD with high temporal resolution. The high cooling rates are achieved by fast heat extraction. Further, the temperature- and cooling rate-dependent precipitation of sub-nanometer clusters in an Al-Cu-Mg alloy can be studied by SAXS. The sensitivity of SAXS on the length scales of the newly formed phases allows their size and fraction to be determined. These techniques are unique tools to help provide a deeper understanding of underlying alloy behavior and its influence on resulting microstructures and properties after AM. Their availability to materials scientists is crucial for both in-depth investigations of novel alloys and also future production of high-quality parts using AM.

  10. New structural studies of liquid crystal by reflectivity and resonant X-ray diffraction; Nouvelles etudes structurales de cristaux liquides par reflectivite et diffraction resonante des rayons X

    Energy Technology Data Exchange (ETDEWEB)

    Fernandes, P

    2007-04-15

    This memory presents three structural studies of smectic Liquid Crystals by reflectivity and resonant diffraction of X-rays. It is divided in five chapters. In the first a short introduction to Liquid Crystals is given. In particular, the smectic phases that are the object of this study are presented. The second chapter is consecrated to the X-ray experimental techniques that were used in this work. The three last chapters present the works on which this thesis can be divided. Chapter three demonstrates on free-standing films of MHPOBC (historic liquid crystal that possesses the antiferroelectric sub-phases) the possibility to extend the technique of resonant X-ray diffraction to liquid crystals without resonant element. In the fourth chapter the structure of the B{sub 2} liquid crystal phase of bent-core molecules (or banana molecules) is elucidated by using resonant X-ray diffraction combined with polarization analysis of the diffracted beam. A model of the polarization of the resonant beam diffracted by four different structures proposed for the B{sub 2} phase is developed in this chapter. In the fifth chapter a smectic binary mixture presenting a very original critical point of phase separation is studied by X-ray reflectivity and optical microscopy. A concentration gradient in the direction perpendicular to the plane of the film seems to be induced by the free-standing film geometry. The results of a simplified model of the system are compatible with this interpretation.

  11. Resonant soft X-ray reflectivity of ultrathin polymer films at the C-edge: A direct approach

    Directory of Open Access Journals (Sweden)

    Alain Gibaud

    2016-09-01

    Full Text Available The use of resonant soft X-ray reflectivity (RSXRR in s-polarization is presented with the aim to show how far it is possible to go in the understanding the evolution of the refractive index n(E=1−δ(E−iβ(E of a ultrathin polystyrene film when the RSXRR is measured through the C-edge. We evidence that a direct fit to the data provides a very good estimation of δ(E and β(E in a large range of energies. Nevertheless, at some specific energy close to C-edge we observe that it is not possible to obtain a satisfactory fit to the data though the same formalism is applied to calculate the reflectivity. We show that even though we take into account the energy resolution of the incident beam, we still end up with a poor fit at these energies. Incorporating the strong contribution of 2nd order photons appeared near C-edge we could not eliminate the discrepancy. Probably the data normalisations have some impacts on such discrepancies at some specific energies.

  12. Parratt-based and model-independent X-ray reflectivity fitting procedure for nanoscale thin film characterization.

    Science.gov (United States)

    Yu, Chung-Jong; Kim, Euikwoun; Kim, Jae-Yong

    2011-05-01

    A general-purpose fitting procedure is presented for X-ray reflectivity data. The Parratt formula was used to fit the low-angle region of the reflectivity data and the resulting electron density profile (continuous base EDP or cbEDP) was then divided into a series of electron density slabs of width 1 angstroms (discrete base EDP or dbEDP), which is then easily incorporated into the Distorted Wave Born Approximation (DWBA). An additional series of density slabs of resolution-limited width are overlapped to the dbEDP, and the density value of the each additional slab is allowed to vary to further fit the data model-independently using DWBA. Because this procedure combines the Parratt formula and the model-independent DWBA fitting, each fitting method can always be employed depending on the type of thin film. Moreover, it provides a way to overcome the difficulties when both fitting methods do not work well for certain types of thin films. Simulations show that this procedure is suitable for nanoscale thin film characterization.

  13. Spherical analyzers and monochromators for resonant inelastic hard X-ray scattering: a compilation of crystals and reflections.

    Science.gov (United States)

    Gog, Thomas; Casa, Diego M; Said, Ayman H; Upton, Mary H; Kim, Jungho; Kuzmenko, Ivan; Huang, XianRong; Khachatryan, Ruben

    2013-01-01

    Resonant inelastic X-ray scattering (RIXS) experiments require special sets of near-backscattering spherical diced analyzers and high-resolution monochromators for every distinct absorption-edge energy and emission line. For the purpose of aiding the design and planning of efficient RIXS experiments, comprehensive lists of suitable analyzer reflections for silicon, germanium, α-quartz, sapphire and lithium niobate crystals were compiled for a multitude of absorption edges and emission lines. Analyzers made from lithium niobate, sapphire or α-quartz offer many choices of reflections with intrinsic resolutions currently unattainable from silicon or germanium. In some cases these materials offer higher intensities at comparable resolutions. While lithium niobate, sapphire or α-quartz analyzers are still in an early stage of development, the present compilation can serve as a computational basis for assessing expected and actual performance. With regard to high-resolution monochromators, bandpass and throughput calculations for combinations of double-crystal, high-heat-load and near-backscattering high-resolution channel-cuts were assembled. The compilation of these analyzer and monochromator data is publicly available on a website.

  14. Determination of heavy metals in macrozoobenthos from the rivers Tisza and Szamos by total reflection X-ray fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Woelfl, S. [Universidad Austral de Chile, Instituto de Zoologia, Casilla 567, Valdivia (Chile)]. E-mail: swoelfl@uach.cl; Mages, M. [Helmhotz Centre for Environmental Research (UFZ), Department of River Ecology, Brueckstrasse 3a, D-39114, Magdeburg (Germany); Ovari, M. [Ovari, M. Eoetvoes University, Department of Organic Chemistry, H-1117, Budapest, Pazmany P. stny. 1/a (Hungary); Geller, W. [Helmhotz Centre for Environmental Research (UFZ), Department of River Ecology, Brueckstrasse 3a, D-39114, Magdeburg (Germany)

    2006-11-15

    In 2000, accidents in the Romanian mining industry in key catchment areas led to heavy metal contamination of the Hungarian rivers Tisza and Szamos resulting in substantial heavy metal loads in several sediments of the upper river basins. This enhanced metal content might have been bioaccumulated in benthic organisms during the following years. Therefore, the aim of this study was to test, whether the zoobenthic fauna showed an enhanced metal content 3 years after the industrial accident. Macrozoobenthic insect larvae (chironomids) were sampled 100 m below and above the confluent site of the rivers Tisza and Szamos during summer 2003 and for comparison purpose also in the river Maros, a tributary of the Tisza river, during 2005. In order to determine their heavy metal content, single specimens were prepared and analysed by Total Reflection X-ray Fluorescence Spectrometry (TRXF) according to the modified dry method. Fe was much lower and Mn and Zn much higher concentrated in benthos from the more contaminated Szamos river compared to the Tisza and Maros rivers. In this sense, the benthic organisms reflected very well the enhanced metal concentrations in the contaminated rivers being suitable as bioindicators of metal contamination. However, the sediment bioaccumulation factor was low at all sampling sites indicating a low bioavailability of trace metals for benthic organisms.

  15. High-pressure, high-temperature deformation of dunite, eclogite, clinopyroxenite and garnetite using in situ X-ray diffraction

    Science.gov (United States)

    Farla, R.; Rosenthal, A.; Bollinger, C.; Petitgirard, S.; Guignard, J.; Miyajima, N.; Kawazoe, T.; Crichton, W. A.; Frost, D. J.

    2017-09-01

    The rheology of eclogite, garnetite and clinopyroxenite in the peridotitic upper mantle was experimentally investigated in a large volume press combined with in situ synchrotron X-ray diffraction techniques to study the impact on mantle convection resulting from the subduction of oceanic lithosphere. Experiments were carried out over a range of constant strain rates (2 ×10-6- 3 ×10-5 s-1), pressures (4.3 to 6.7 GPa) and temperatures (1050 to 1470 K). Results show substantial strength variations among eclogitic garnet and clinopyroxene and peridotitic olivine. At low temperatures (1400 K) eclogite is weaker than dunite by 0.2 GPa or more. Garnetite and clinopyroxenite exhibit higher strength than dunite at approximately 1200 K. However, at higher temperature (1370 K), clinopyroxenite is significantly weaker than garnetite (and dunite) by more than a factor of five. We explain these observations by transitions in deformation mechanisms among the mineral phases. In clinopyroxene, high temperature dislocation creep resulting in a strength reduction replaces low temperature twinning. Whereas garnet remains very rigid at all experimental conditions when nominally anhydrous ('dry'). Microstructural observations show phase segregation of clinopyroxene and garnet, development of a crystallographic and shape preferred orientation in the former but not in the latter, suggesting an overall weak seismic anisotropy. Detection of eclogite bodies in the peridotite-dominated mantle may only be possible via observation of high VP /VS1 ratios. A comparable or weaker rheology of eclogite to dunite suggests effective stirring and mixing of eclogite in the convecting mantle.

  16. Intrinsic stress in ZrN thin films: Evaluation of grain boundary contribution from in situ wafer curvature and ex situ x-ray diffraction techniques

    Energy Technology Data Exchange (ETDEWEB)

    Koutsokeras, L. E. [Departement Physique et Mecanique des Materiaux, Institut Pprime, CNRS-Universite de Poitiers-ENSMA, UPR 3346, SP2MI, Teleport 2, Bd M et P Curie, F 86962 Chasseneuil-Futuroscope (France); Department of Materials Science and Engineering, University of Ioannina, Ioannina 45110 (Greece); Abadias, G. [Departement Physique et Mecanique des Materiaux, Institut Pprime, CNRS-Universite de Poitiers-ENSMA, UPR 3346, SP2MI, Teleport 2, Bd M et P Curie, F 86962 Chasseneuil-Futuroscope (France)

    2012-05-01

    Low-mobility materials, like transition metal nitrides, usually undergo large residual stress when sputter-deposited as thin films. While the origin of stress development has been an active area of research for high-mobility materials, atomistic processes are less understood for low-mobility systems. In the present work, the contribution of grain boundary to intrinsic stress in reactively magnetron-sputtered ZrN films is evaluated by combining in situ wafer curvature measurements, providing information on the overall biaxial stress, and ex situ x-ray diffraction, giving information on elastic strain (and related stress) inside crystallites. The thermal stress contribution was also determined from the in situ stress evolution during cooling down, after deposition was stopped. The stress data are correlated with variations in film microstructure and growth energetics, in the 0.13-0.42 Pa working pressure range investigated, and discussed based on existing stress models. At low pressure (high energetic bombardment conditions), a large compressive stress is observed due to atomic peening, which induces defects inside crystallites but also promotes incorporation of excess atoms in the grain boundary. Above 0.3-0.4 Pa, the adatom surface mobility is reduced, leading to the build-up of tensile stress resulting from attractive forces between under-dense neighbouring column boundary and possible void formation, while crystallites can still remain under compressive stress.

  17. In situ characterization of delamination and crack growth of a CGO–LSM multi-layer ceramic sample investigated by X-ray tomographic microscopy

    DEFF Research Database (Denmark)

    Bjørk, Rasmus; Esposito, Vincenzo; Lauridsen, Erik Mejdal

    2014-01-01

    The densification, delamination and crack growth behavior in a Ce0.9Gd0.1O1.95 (CGO) and (La0.85Sr0.15)0.9MnO3 (LSM) multi-layer ceramic sample was studied using in situ X-ray tomographic microscopy (microtomography) to investigate the critical dynamics of crack propagation and delamination...... and delamination only accelerates when sintering occurs....

  18. An in situ x-ray photoelectron spectroscopy study of the initial stages of rf magnetron sputter deposition of indium tin oxide on p-type Si substrate

    Energy Technology Data Exchange (ETDEWEB)

    Rein, M. H.; Holt, A. O. [Institute for Energy Technology, Department of Solar Energy, Instituttveien 18, 2008 Kjeller (Norway); Hohmann, M. V.; Klein, A. [Technische Universitaet Darmstadt, Institute of Materials Science, Surface Science Division, Petersenstrasse 32, D-64287 Darmstadt (Germany); Thogersen, A. [SINTEF-Materials and Chemistry Syntesis and Properties, Forskningsveien 1, Pb. 124 Blindern, 0314 Oslo (Norway); Mayandi, J. [Department of Materials Science, School of Chemistry, Madurai Kamaraj University, Tamil Nadu, Madurai (India); Monakhov, E. V. [Institute for Energy Technology, Department of Solar Energy, Instituttveien 18, 2008 Kjeller (Norway); Department of Physics/Centre for Materials Science and Nanotechnology, University of Oslo, 0316 Oslo (Norway)

    2013-01-14

    The interface between indium tin oxide and p-type silicon is studied by in situ X-ray photoelectron spectroscopy (XPS). This is done by performing XPS without breaking vacuum after deposition of ultrathin layers in sequences. Elemental tin and indium are shown to be present at the interface, both after 2 and 10 s of deposition. In addition, the silicon oxide layer at the interface is shown to be composed of mainly silicon suboxides rather than silicon dioxide.

  19. In situ X-ray diffraction of catalysts. Phase transformations of Cu/Cr-oxides with different initial structure under redox conditions

    Energy Technology Data Exchange (ETDEWEB)

    Krieger, T.A.; Plyasova, L.M.; Yurieva, T.M. [Boreskov Inst. of Catalysis, Novosibirsk (Russian Federation)

    2000-07-01

    The installation design and a chamber-reactor were proposed for laboratory-scale in situ X-ray diffraction studies of solid phase transformations. Dynamics of phase transformations was studied for low-temperature copper chromite under the action of the reaction medium. Common and distinctive features of the behavior of low- and high-temperature copper chromites under redox conditions at the temperature below 300 C were revealed. (orig.)

  20. CO2-selective methanol steam reforming on In-doped Pd studied by in situ X-ray photoelectron spectroscopy

    Science.gov (United States)

    Rameshan, Christoph; Lorenz, Harald; Mayr, Lukas; Penner, Simon; Zemlyanov, Dmitry; Arrigo, Rosa; Haevecker, Michael; Blume, Raoul; Knop-Gericke, Axel; Schlögl, Robert; Klötzer, Bernhard

    2012-01-01

    In situ X-ray photoelectron spectroscopy (in situ XPS) was used to study the structural and catalytic properties of Pd–In near-surface intermetallic phases in correlation with previously studied PdZn and PdGa. Room temperature deposition of ∼4 monolayer equivalents (MLEs) of In metal on Pd foil and subsequent annealing to 453 K in vacuum yields a ∼1:1 Pd/In near-surface multilayer intermetallic phase. This Pd1In1 phase exhibits a similar “Cu-like” electronic structure and indium depth distribution as its methanol steam reforming (MSR)-selective multilayer Pd1Zn1 counterpart. Catalytic characterization of the multilayer Pd1In1 phase in MSR yielded a CO2-selectivity of almost 100% between 493 and 550 K. In contrast to previously studied In2O3-supported PdIn nanoparticles and pure In2O3, intermediate formaldehyde is only partially converted to CO2 using this Pd1In1 phase. Strongly correlated with PdZn, on an In-diluted PdIn intermetallic phase with “Pd-like” electronic structure, prepared by thermal annealing at 623 K, methanol steam reforming is suppressed and enhanced CO formation via full methanol dehydrogenation is observed. To achieve CO2-TOF values on the isolated Pd1In1 intermetallic phase as high as on supported PdIn/In2O3, at least 593 K reaction temperature is required. A bimetal-oxide synergism, with both bimetallic and oxide synergistically contributing to the observed catalytic activity and selectivity, manifests itself by accelerated formaldehyde-to-CO2 conversion at markedly lowered temperatures as compared to separate oxide and bimetal. Combination of suppression of full methanol dehydrogenation to CO on Pd1In1 inhibited inverse water–gas-shift reaction on In2O3 and fast water activation/conversion of formaldehyde is the key to the low-temperature activity and high CO2-selectivity of the supported catalyst. PMID:23226689

  1. CO(2)-selective methanol steam reforming on In-doped Pd studied by in situ X-ray photoelectron spectroscopy.

    Science.gov (United States)

    Rameshan, Christoph; Lorenz, Harald; Mayr, Lukas; Penner, Simon; Zemlyanov, Dmitry; Arrigo, Rosa; Haevecker, Michael; Blume, Raoul; Knop-Gericke, Axel; Schlögl, Robert; Klötzer, Bernhard

    2012-11-01

    In situ X-ray photoelectron spectroscopy (in situ XPS) was used to study the structural and catalytic properties of Pd-In near-surface intermetallic phases in correlation with previously studied PdZn and PdGa.Room temperature deposition of ∼4 monolayer equivalents (MLEs) of In metal on Pd foil and subsequent annealing to 453 K in vacuum yields a ∼1:1 Pd/In near-surface multilayer intermetallic phase. This Pd(1)In(1) phase exhibits a similar "Cu-like" electronic structure and indium depth distribution as its methanol steam reforming (MSR)-selective multilayer Pd(1)Zn(1) counterpart.Catalytic characterization of the multilayer Pd(1)In(1) phase in MSR yielded a CO(2)-selectivity of almost 100% between 493 and 550 K. In contrast to previously studied In(2)O(3)-supported PdIn nanoparticles and pure In(2)O(3), intermediate formaldehyde is only partially converted to CO(2) using this Pd(1)In(1) phase. Strongly correlated with PdZn, on an In-diluted PdIn intermetallic phase with "Pd-like" electronic structure, prepared by thermal annealing at 623 K, methanol steam reforming is suppressed and enhanced CO formation via full methanol dehydrogenation is observed.To achieve CO(2)-TOF values on the isolated Pd(1)In(1) intermetallic phase as high as on supported PdIn/In(2)O(3), at least 593 K reaction temperature is required. A bimetal-oxide synergism, with both bimetallic and oxide synergistically contributing to the observed catalytic activity and selectivity, manifests itself by accelerated formaldehyde-to-CO(2) conversion at markedly lowered temperatures as compared to separate oxide and bimetal. Combination of suppression of full methanol dehydrogenation to CO on Pd(1)In(1) inhibited inverse water-gas-shift reaction on In(2)O(3) and fast water activation/conversion of formaldehyde is the key to the low-temperature activity and high CO(2)-selectivity of the supported catalyst.

  2. Following the kinetics of a chemical reaction in ultrathin supported polymer films by reliable mass density determination with X-ray reflectivity.

    Science.gov (United States)

    Kontturi, Eero; Lankinen, Aapo

    2010-03-24

    Numerous modern functionalities with ultrathin polymer films involve chemical reactions within the films. X-ray reflectivity can be used to quantitatively follow these chemical reactions by a reliable determination of mass density, which is feasible within certain thickness constraints (e.g., 5-17 nm thickness for common polymer films).

  3. Ion distributions at the water/1,2-dichloroethane interface: potential of mean force approach to analyzing X-ray reflectivity and interfacial tension measurements.

    Science.gov (United States)

    Hou, Binyang; Laanait, Nouamane; Yu, Hao; Bu, Wei; Yoon, Jaesung; Lin, Binhua; Meron, Mati; Luo, Guangming; Vanysek, Petr; Schlossman, Mark L

    2013-05-02

    We present X-ray reflectivity and interfacial tension measurements of the electrified liquid/liquid interface between two immiscible electrolyte solutions for the purpose of understanding the dependence of interfacial ion distributions on the applied electric potential difference across the interface. The aqueous phase contains alkali-metal chlorides, including LiCl, NaCl, RbCl, or CsCl, and the organic phase is a 1,2-dichloroethane solution of bis(triphenylphosphor anylidene) ammonium tetrakis(pentafluorophenyl)borate (BTPPATPFB). Selected data for a subset of electric potential differences are analyzed to determine the potentials of mean force for Li(+), Rb(+), Cs(+), BTPPA(+), and TPFB(-). These potentials of mean force are then used to analyze both X-ray reflectivity and interfacial tension data measured over a wide range of electric potential differences. Comparison of X-ray reflectivity data for strongly hydrated alkali-metal ions (Li(+) and Na(+)), for which ion pairing to TPFB(-) ions across the interface is not expected, to data for weakly hydrated alkali-metal ions (Rb(+) and Cs(+)) indicates that the Gibbs energy of adsorption due to ion pairing at the interface must be small (X-ray reflectivity measurements that probe the nanoscale ion distribution and the consequences of these underlying distributions for thermodynamic studies, such as interfacial tension measurements, that yield quantities related to the integrated ion distribution.

  4. In situ electrochemical high-energy X-ray diffraction using a capillary working electrode cell geometry

    Energy Technology Data Exchange (ETDEWEB)

    Young, Matthias J.; Bedford, Nicholas M.; Jiang, Naisheng; Lin, Deqing; Dai, Liming

    2017-05-26

    The ability to generate new electrochemically active materials for energy generation and storage with improved properties will likely be derived from an understanding of atomic-scale structure/function relationships during electrochemical events. Here, the design and implementation of a new capillary electrochemical cell designed specifically forin situhigh-energy X-ray diffraction measurements is described. By increasing the amount of electrochemically active material in the X-ray path while implementing low-Zcell materials with anisotropic scattering profiles, an order of magnitude enhancement in diffracted X-ray signal over traditional cell geometries for multiple electrochemically active materials is demonstrated. This signal improvement is crucial for high-energy X-ray diffraction measurements and subsequent Fourier transformation into atomic pair distribution functions for atomic-scale structural analysis. As an example, clear structural changes in LiCoO2under reductive and oxidative conditions using the capillary cell are demonstrated, which agree with prior studies. Accurate modeling of the LiCoO2diffraction data using reverse Monte Carlo simulations further verifies accurate background subtraction and strong signal from the electrochemically active material, enabled by the capillary working electrode geometry.

  5. Inorganic pigment study of the San Pedro Gonzalez Telmo Sibyls using total reflection X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Vazquez, Cristina, E-mail: vazquez@cnea.gov.a [Universidad de Buenos Aires, Facultad de Ingenieria, Paseo Colon 850. C1063ACU, Buenos Aires (Argentina); Comision Nacional de Energia Atomica, Gerencia Quimica, Av. Gral Paz 1499, B1650KNA, San Martin (Argentina); Custo, Graciela, E-mail: custo@cnea.gov.a [Comision Nacional de Energia Atomica, Gerencia Quimica, Av. Gral Paz 1499, B1650KNA, San Martin (Argentina); Barrio, Nestor, E-mail: nbarrio@unsam.edu.a [CEIRCAB-TAREA, Universidad Nacional de San Martin (UNSAM), Escuela de Humanidades, Campus Miguelete, 25 de Mayo y Francia, B1650KNA, San Martin (Argentina); Burucua, Jose, E-mail: gburucua@unsam.edu.a [CEIRCAB-TAREA, Universidad Nacional de San Martin (UNSAM), Escuela de Humanidades, Campus Miguelete, 25 de Mayo y Francia, B1650KNA, San Martin (Argentina); Boeykens, Susana [Universidad de Buenos Aires, Facultad de Ingenieria, Paseo Colon 850. C1063ACU, Buenos Aires (Argentina); Marte, Fernando, E-mail: fmarte@unsam.edu.a [CEIRCAB-TAREA, Universidad Nacional de San Martin (UNSAM), Escuela de Humanidades, Campus Miguelete, 25 de Mayo y Francia, B1650KNA, San Martin (Argentina)

    2010-09-15

    This article describes the study carried out on a series of oil paintings on canvas from the eighteenth century that were restored at Centro de Produccion e Investigacion en Restauracion y Conservacion Artistica y Bibliografica - Tarea (CEIRCAB-Tarea), Buenos Aires, Argentina: the San Pedro Gonzalez Telmo Sibyls. Experimental study was undertaken to identify inorganic pigments and the technique used in their confection; and, in this way, try to add information about their local origin. Therefore special emphasis was put to infer technologies used in the manufacturing of these paintings. Elemental analysis was performed by total reflection X-ray fluorescence spectrometry (TXRF) and complemented by optical and polarized light microscopy. Microsampling was carefully done over areas of the paintings which were damaged and where a small additional loss will not be noticed. This investigation has shown that a variety of pigments were used, namely earth pigments (red and yellow ochres), white lead, vermilion, etc., and they were used either pure or in mixtures. This characterization helped conservators in their decisions regarding a better understanding of the deterioration processes. In addition, this research about the material composition allowed the art historians and restorers the possibility to obtain information about where, when or by whom The San Pedro Gonzalez Telmo Sibyls may have been painted.

  6. Inorganic pigment study of the San Pedro Gonzalez Telmo Sibyls using total reflection X-ray fluorescence

    Science.gov (United States)

    Vázquez, Cristina; Custo, Graciela; Barrio, Néstor; Burucúa, José; Boeykens, Susana; Marte, Fernando

    2010-09-01

    This article describes the study carried out on a series of oil paintings on canvas from the eighteenth century that were restored at Centro de Producción e Investigación en Restauración y Conservación Artística y Bibliográfica - Tarea (CEIRCAB-Tarea), Buenos Aires, Argentina: the San Pedro González Telmo Sibyls. Experimental study was undertaken to identify inorganic pigments and the technique used in their confection; and, in this way, try to add information about their local origin. Therefore special emphasis was put to infer technologies used in the manufacturing of these paintings. Elemental analysis was performed by total reflection X-ray fluorescence spectrometry (TXRF) and complemented by optical and polarized light microscopy. Microsampling was carefully done over areas of the paintings which were damaged and where a small additional loss will not be noticed. This investigation has shown that a variety of pigments were used, namely earth pigments (red and yellow ochres), white lead, vermilion, etc., and they were used either pure or in mixtures. This characterization helped conservators in their decisions regarding a better understanding of the deterioration processes. In addition, this research about the material composition allowed the art historians and restorers the possibility to obtain information about where, when or by whom The San Pedro González Telmo Sibyls may have been painted.

  7. Total reflection X-ray fluorescence as a convenient tool for determination of trace elements in microscale gasoline and diesel

    Science.gov (United States)

    Zhang, Airui; Jin, Axiang; Wang, Hai; Wang, Xiaokang; Zha, Pengfei; Wang, Meiling; Song, Xiaoping; Gao, Sitian

    2018-03-01

    Quantitative determination of trace elements like S, Fe, Cu, Mn and Pb in gasoline and S in diesel is of great importance due to the growing concerns over air pollution, human health and engine failure caused by utilization of gasoline and diesel with these harmful elements. A method of total reflection X-ray fluorescence (TXRF) was developed to measure these harmful trace elements in gasoline and diesel. A variety of factors to affect measurement results, including TXRF parameters, microwave-assisted digestion conditions and internal standard element and its addition, were examined to optimize these experimental procedures. The hydrophobic treatment of the surface of quartz reflectors to support the analyte with neutral silicone solutions could prepare thin films of gasoline and diesel digestion solutions for subsequent TXRF analysis. The proposed method shows good potential and reliability to determine the content of harmful trace elements in gasoline and diesel with high sensitivity and accuracy without drawing different standard calibration curves, and can be easily employed to screen gasoline and diesel in routine quality control and assurance.

  8. Determination of arsenic in water samples by Total Reflection X-Ray Fluorescence using pre-concentration with alumina

    Energy Technology Data Exchange (ETDEWEB)

    Barros, Haydn [Laboratorio de Fisica Nuclear, Dpto. De Fisica, Universidad Simon Bolivar, Sartenejas, Baruta (Venezuela, Bolivarian Republic of); Marco Parra, Lue-Meru, E-mail: luemerumarco@yahoo.e [Universidad Centroccidental Lisandro Alvarado, Dpto. Quimica y Suelos, Decanato de Agronomia, Tarabana, Cabudare, Edo.Lara (Venezuela, Bolivarian Republic of); Bennun, Leonardo [Universidad de Concepcion, Concepcion (Chile); Greaves, Eduardo D. [Laboratorio de Fisica Nuclear, Dpto. De Fisica, Universidad Simon Bolivar, Sartenejas, Baruta (Venezuela, Bolivarian Republic of)

    2010-06-15

    The determination of arsenic in water samples requires techniques of high sensitivity. Total Reflection X-Ray Fluorescence (TXRF) allows the determination but a prior separation and pre-concentration procedure is necessary. Alumina is a suitable substrate for the selective separation of the analytes. A method for separation and pre-concentration in alumina, followed by direct analysis of the alumina is evaluated. Quantification was performed using the Al-K{alpha} and Co-K{alpha} lines as internal standard in samples prepared on an alumina matrix, and compared to a calibration with aqueous standards. Artificial water samples of As (III) and As (V) were analyzed after the treatment. Fifty milliliters of the sample at ppb concentration levels were mixed with 10 mg of alumina. The pH, time and temperature were controlled. The alumina was separated from the slurry by centrifugation, washed with de-ionized water and analyzed directly on the sample holder. A pre-concentration factor of 100 was found, with detection limit of 0.7 {mu}gL{sup -1}. The percentage of recovery was 98% for As (III) and 95% for As (V) demonstrating the suitability of the procedure.

  9. Temperature dependence of multilayering at the free surface of ionic liquids probed by X-ray reflectivity measurements.

    Science.gov (United States)

    Nishi, Naoya; Uruga, Tomoya; Tanida, Hajime; Kakiuchi, Takashi

    2011-06-21

    The effect of the temperature on the surface layering of ionic liquids has been studied for two ionic liquids, trioctylmethylammonium bis(nonafluorobutanesulfonyl)amide([TOMA(+)][C(4)C(4)N(-)]) and trihexyltetradecylphosphonium bis(nonafluorobutanesulfonyl)amide ([THTDP(+)][C(4)C(4)N(-)]), using X-ray reflectivity measurements at 285, 300, and 315 K. Both [TOMA(+)][C(4)C(4)N(-)] and [THTDP(+)][C(4)C(4)N(-)] develop multilayers at the surface. The structure of the multilayers at the [TOMA(+)][C(4)C(4)N(-)] surface shows little temperature-dependent change, whereas that at the [THTDP(+)][C(4)C(4)N(-)] surface clearly becomes diffused with increasing temperature. The different temperature dependence seems to be related to the difference in the recently reported ultraslow dynamics of the interfacial structure of [TOMA(+)][C(4)C(4)N(-)] and [THTDP(+)][C(4)C(4)N(-)] at the ionic liquid|water interface. © 2011 American Chemical Society

  10. Effect of cholesterol and ergosterol on the antibiotic amphotericin B interactions with dipalmitoylphosphatidylcholine monolayers: X-ray reflectivity study.

    Science.gov (United States)

    Kamiński, Daniel M; Czernel, Grzegorz; Murphy, Bridget; Runge, Benjamin; Magnussen, Olaf M; Gagoś, Mariusz

    2014-11-01

    Amphotericin B is a Streptomyces nodosus metabolite and one of the oldest polyene antibiotics used in the treatment of invasive systemic fungal infections. Despite its over 50-year existence in clinical practice and the recognition of amphotericin B as the gold standard in the treatment of serious systemic mycosis, it still remains one of the most toxic pharmaceuticals. Understanding of the processes at the molecular levels and the interactions between amphotericin B with lipid membranes containing sterols should elucidate the mechanisms of the action and toxicity of this widely used antibiotic. In this work, we use X-ray reflectivity to study the structural changes on a molecular scale after amphotericin B incorporation. These changes are accompanied by an increase in monolayer surface pressure which is more pronounced for ergosterol - rather than cholesterol-rich membranes. The data indicate that this difference is not due to the higher affinity of amphotericin B towards ergosterol-containing membranes but is rather due to a ~3Angstrom corrugation of the monolayer. Furthermore, the total quantity of amphotericin B incorporated into lipid monolayers containing cholesterol and ergosterol is the same. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Asymmetric Structural Features in Single Supported Lipid Bilayers Containing Cholesterol and GM1 Resolved with Synchrotron X-Ray Reflectivity

    Science.gov (United States)

    Reich, Christian; Horton, Margaret R.; Krause, Bärbel; Gast, Alice P.; Rädler, Joachim O.; Nickel, Bert

    2008-01-01

    The cell membrane comprises numerous protein and lipid molecules capable of asymmetric organization between leaflets and liquid-liquid phase separation. We use single supported lipid bilayers (SLBs) to model cell membranes, and study how cholesterol and asymmetrically oriented ganglioside receptor GM1 affect membrane structure using synchrotron x-ray reflectivity. Using mixtures of cholesterol, sphingomyelin, and 1,2-dioleoyl-sn-glycero-3-phosphocholine, we characterize the structure of liquid-ordered and liquid-disordered SLBs in terms of acyl-chain density, headgroup size, and leaflet thickness. SLBs modeling the liquid-ordered phase are 10 Å thicker and have a higher acyl-chain electron density (〈ρchain〉 = 0.33 e−/Å3) compared to SLBs modeling the liquid-disordered phase, or pure phosphatidylcholine SLBs (〈ρchain〉 = 0.28 e−/Å3). Incorporating GM1 into the distal bilayer leaflet results in membrane asymmetry and thickening of the leaflet of 4–9 Å. The structural effect of GM1 is more complex in SLBs of cholesterol/sphingomyelin/1,2-dioleoyl-sn-glycero-3-phosphocholine, where the distal chains show a high electron density (〈ρchain〉 = 0.33 e−/Å3) and the lipid diffusion constant is reduced by ∼50%, as measured by fluorescence microscopy. These results give quantitative information about the leaflet asymmetry and electron density changes induced by receptor molecules that penetrate a single lipid bilayer. PMID:18375517

  12. On the Determination of the Spin of the Black Hole in Cyg X-1 from X-Ray Reflection Spectra

    Science.gov (United States)

    Fabian, A. C.; Wilkins, D.; Miller, J. M.; Reis, R. C.; Reynolds, C. S.; Cackett, E. M.; Nowak, M. A.; Pooley, G.; Pottschmidt, K.; Sanders, J. S.; hide

    2012-01-01

    The spin of Cygnus X-I is measured by fitting reflection models to Suzaku data covering the energy band 0.9-400 keY. The inner radius of the accretion disc is found to lie within 2 gravitational radii (rg = GM/c(exp 2)) and a value for the dimensionless black hole spin is obtained of 0.97(sup .0.14) (sup -0.02). This agrees with recent measurements using the continuum fitting method by Gou et al. and of the broad iron line by Duro et al. The disc inclination is measured at 23.7(sup +6.7) (sup -5.4) deg. which is consistent with the recent optical measurement of the binary system inclination by Orosz et al of 27+/- 0.8 deg. We pay special attention to the emissivity profile caused by irradiation of the inner disc by the hard power-law source. 1be X-ray observations and simulations show that the index q of that profile deviates from the commonly used, Newtonian, value of 3 within 3r(sub g), steepening considerably within 2r(sub g). as expected in the strong gravity regime.

  13. A novel total reflection X-ray fluorescence procedure for the direct determination of trace elements in petrochemical products

    Energy Technology Data Exchange (ETDEWEB)

    Cinosi, Amedeo [Sasol Italy SpA, Paderno Dugnano (Italy); GNR srl, Agrate Conturbia, Novara (Italy); Andriollo, Nunzio [Sasol Italy SpA, Paderno Dugnano (Italy); Pepponi, Giancarlo [Fondazione Bruno Kessler, Povo, Trento (Italy); Monticelli, Damiano [Universita degli Studi dell' Insubria - sede di Como, Dipartimento di Scienze Chimiche e Ambientali, Como, CO (Italy)

    2011-01-15

    A total reflection X-ray fluorescence (TXRF) procedure was developed for the determination of metal traces in petrochemical end products or intermediates for surfactant synthesis. The method combines a fast and straightforward sample preparation, i.e. deposition on the sample holder and evaporation of the sample matrix, with an efficient quantification method based on internal standardization (organic gallium standard). The method developed showed detection limits below 0.05 {mu}g g{sup -1} and in most cases below 0.005 {mu}g g{sup -1}. Fifteen elements (Ca, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Rh, Sn, Sr, V and Zn) were determined in matrices such as paraffins, n-olefins, linear alkylbenzenes, long-chain alkyl alcohols and esters: typical metal contents were below 1 {mu}g g{sup -1}. The results were compared with the reference method ASTM D5708 (test method B) based on inductively coupled plasma optical emission spectroscopy: advantages and drawbacks of the two procedures were critically evaluated. The TXRF method developed showed comparable precision and absence of bias with respect to the reference method. A comparison of the performances of the two methods is presented. (orig.)

  14. Trace metal determinations by total-reflection x-ray fluorescence analysis in the open Atlantic Ocean

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt, D.; Gerwinski, W.; Radke, I. (Bundesamt fuer Seeschiffahrt und Hydrographie, Hamburg (Germany))

    1993-02-01

    The Intergovernmental Oceanographic Commission (IOC), as a major component of its programme ''Global Investigation of Pollution in the Marine Environment'' (GIPME), maintains a long-standing project on ''Open Ocean Baseline Studies of Trace Contaminants''. Initially, the Atlantic Ocean and trace metals were selected. Four deep-water stations in the Cape Basin, Angola Basin, Cape Verde Abyssal Plain and Seine Abyssal Plain were regularly sampled for at least 36 depths. Additional samples were taken between stations. Samples were distributed to participants and a similar number of additional laboratories. As a central part of our own contribution to the project, we determined the trace heavy metals manganese, nickel, copper, zinc and lead and the lighter selenium by total-reflection X-ray fluorescence analysis. For the TXRF, the pre-enrichment of the trace metals and the separation from the salt matrix were performed by complexation with sodium dibenzyldithiocarbamate and reverse-phase chromatography. Generally, very low levels of trace elements were found in filtered and unfiltered water samples from these remote areas of the open Atlantic Ocean. Typical examples of the distributions of trace metal concentrations on depth profiles from the four deep-water stations as well as intercomparisons between the stations are presented. (author).

  15. Total reflection x-ray fluorescence spectroscopy as a tool for evaluation of iron concentration in ferrofluids and yeast samples

    Energy Technology Data Exchange (ETDEWEB)

    Kulesh, N.A., E-mail: nikita.kulesh@urfu.ru [Ural Federal University, Mira 19, 620002 Ekaterinburg (Russian Federation); Novoselova, I.P. [Ural Federal University, Mira 19, 620002 Ekaterinburg (Russian Federation); Immanuel Kant Baltic Federal University, 236041 Kaliningrad (Russian Federation); Safronov, A.P. [Ural Federal University, Mira 19, 620002 Ekaterinburg (Russian Federation); Institute of Electrophysics UD RAS, Amundsen 106, 620016 Ekaterinburg (Russian Federation); Beketov, I.V.; Samatov, O.M. [Institute of Electrophysics UD RAS, Amundsen 106, 620016 Ekaterinburg (Russian Federation); Kurlyandskaya, G.V. [Ural Federal University, Mira 19, 620002 Ekaterinburg (Russian Federation); University of the Basque Country UPV-EHU, 48940 Leioa (Spain); Morozova, M. [Ural Federal University, Mira 19, 620002 Ekaterinburg (Russian Federation); Denisova, T.P. [Irkutsk State University, Karl Marks 1, 664003 Irkutsk (Russian Federation)

    2016-10-01

    In this study, total reflection x-ray fluorescent (TXRF) spectrometry was applied for the evaluation of iron concentration in ferrofluids and biological samples containing iron oxide magnetic nanoparticles obtained by the laser target evaporation technique. Suspensions of maghemite nanoparticles of different concentrations were used to estimate the limitation of the method for the evaluation of nanoparticle concentration in the range of 1–5000 ppm in absence of organic matrix. Samples of single-cell yeasts grown in the nutrient media containing maghemite nanoparticles were used to study the nanoparticle absorption mechanism. The obtained results were analyzed in terms of applicability of TXRF for quantitative analysis in a wide range of iron oxide nanoparticle concentrations for biological samples and ferrofluids with a simple established protocol of specimen preparation. - Highlights: • Ferrofluids and yeasts samples were analysed by TXRF spectroscopy. • Simple protocol for iron quantification by means of TXRF was proposed. • Results were combined with magnetic, structural, and morphological characterization. • Preliminary conclusion on nanoparticles uptake mechanism was made.

  16. Determination of platinum group metal catalyst residues in active pharmaceutical ingredients by means of total reflection X-ray spectrometry

    Science.gov (United States)

    Marguí, Eva; Queralt, Ignasi; Hidalgo, Manuela

    2013-08-01

    The control of metal catalyst residues (i.e., platinum group metals (PGMs)) in different stages of the manufacturing processes of the active pharmaceutical ingredients (APIs) and, especially, in the final product is crucial. For API specimens, there are strict guidelines to limit the levels of metal residues based on their individual levels of safety concern. For PGMs the concentration limit has been established at 10 mg/kg in the API. Therefore great effort is currently being devoted to the development of new and simple procedures to control metals in pharmaceuticals. In the present work, an analytical methodology based on benchtop total reflection X-ray fluorescence spectrometry (TXRF) has been developed for the rapid and simple determination of some PGM catalyst impurities (Rh, Pd, Ir and Pt) in different types of API samples. An evaluation of different sample treatments (dissolution and digestion of the solid pharmaceutical samples) has been carried out and the developed methodologies have been validated according to the analytical parameters to be considered and acceptance criteria for PGM determination according to the United States Pharmacopeia (USP). Limits of quantification obtained for PGM metals were in the range of 2-4 mg/kg which are satisfactory according to current legislation. From the obtained results it is shown that the developed TXRF method can be implemented in the pharmaceutical industries to increase productivity of the laboratory; offering an interesting and complementary analytical tool to other atomic spectroscopic methods.

  17. Analytical capabilities of total reflection X-ray fluorescence spectrometry for silver nanoparticles determination in soil adsorption studies

    Science.gov (United States)

    Torrent, Laura; Iglesias, Mònica; Hidalgo, Manuela; Marguí, Eva

    2016-12-01

    In recent years, the production of silver nanoparticles (AgNPs) has grown due to their antibacterial properties. This fact enhances the release of these particles into the environment, especially in soils that are the major sink. To better understand adsorption processes in soils, usually batch kinetic studies are carried out. In this context, we tested the possibilities of using total reflection X-ray fluorescence spectrometry (TXRF) to monitor the silver content in soil adsorption kinetic studies. It was found that the lower limit of detection for Ag (through Ag-Kα detection) in aqueous solutions was around 37 μg·L- 1, which was suitable to carry out this kind of studies. Moreover, the direct analysis of Ag adsorbed onto soil after the kinetic studies was investigated. In this case, the limit of detection for Ag was around 1.7 mg·kg- 1. All TXRF results were compared with those obtained by inductively coupled plasma optic emission spectrometry and good agreement was found. The batch adsorption tests performed showed that 98% of polyvinylpyrrolidone coated AgNPs were retained on the tested soils in < 6 h.

  18. Interfacial properties and iron binding to bacterial proteins that promote the growth of magnetite nanocrystals: X-ray reflectivity and surface spectroscopy studies.

    Science.gov (United States)

    Wang, Wenjie; Bu, Wei; Wang, Lijun; Palo, Pierre E; Mallapragada, Surya; Nilsen-Hamilton, Marit; Vaknin, David

    2012-03-06

    Surface sensitive X-ray scattering and spectroscopic studies have been conducted to determine structural properties of Mms6, the protein in Magnetospirillum magneticum AMB-1 that is implicated as promoter of magnetite nanocrystals growth. Surface pressure versus molecular area isotherms indicate Mms6 forms stable monolayers at the aqueous/vapor interface that are strongly affected by ionic conditions of the subphase. Analysis of X-ray reflectivity from the monolayers shows that the protein conformation at the interface depends on surface pressure and on the presence of ions in the solutions, in particular of iron ions and its complexes. X-ray fluorescence at grazing angles of incidence from the same monolayers allows quantitative determination of surface bound ions to the protein showing that ferric iron binds to Mms6 at higher densities compared to other ions such as Fe(2+) or La(3+) under similar buffer conditions.

  19. Normalizing a Relativistic Model of X-Ray Reflection Definition of the Reflection Fraction and Its Implementation in relxill

    Science.gov (United States)

    Dauser, T.; Garcia, J.; Walton, D. J.; Eikmann, W.; Kallman, T.; McClintock, J.; Wilms, J.

    2016-01-01

    Aims. The only relativistic reflection model that implements a parameter relating the intensity incident on an accretion disk to the observed intensity is relxill. The parameter used in earlier versions of this model, referred to as the reflection strength, is unsatisfactory; it has been superseded by a parameter that provides insight into the accretion geometry, namely the reflection fraction. The reflection fraction is defined as the ratio of the coronal intensity illuminating the disk to the coronal intensity that reaches the observer. Methods. The relxill model combines a general relativistic ray-tracing code and a photoionization code to compute the component of radiation reflected from an accretion that is illuminated by an external source. The reflection fraction is a particularly important parameter for relativistic models with well-defined geometry, such as the lamp post model, which is a focus of this paper. Results. Relativistic spectra are compared for three inclinations and for four values of the key parameter of the lamp post model,namely the height above the black hole of the illuminating, on-axis point source. In all cases, the strongest reflection is produced for low source heights and high spin. A low-spin black hole is shown to be incapable of producing enhanced relativistic reflection. Results for the relxill model are compared to those obtained with other models and a Monte Carlo simulation. Conclusions. Fitting data by using the relxill model and the recently implemented reflection fraction, the geometry of a system can be constrained. The reflection-fraction is independent of system parameters such as inclination and black hole spin. The reflection-fraction parameter was implemented with the name reflec_frac all flavours of the relxill model, and the non-relativistic reflection model xillver, in v0.4a (18 January 2016).

  20. In situ liquid water visualization in polymer electrolyte membrane fuel cells with high resolution synchrotron x-ray radiography

    Energy Technology Data Exchange (ETDEWEB)

    Chevalier, S.; Banerjee, R.; Lee, J.; Ge, N.; Lee, C.; Bazylak, A., E-mail: abazylak@mie.utoronto.ca [Dept. of Mechanical & Industrial Engineering, Faculty of Applied Science & Engineering, University of Toronto, Toronto, Ontario (Canada); Wysokinski, T. W.; Belev, G.; Webb, A.; Miller, D.; Zhu, N. [Canadian Light Source, Saskatoon, Saskatchewan (Canada); Tabuchi, Y.; Kotaka, T. [EV System Laboratory, Research Division 2, Nissan Motor Co., Ltd., Yokosuka, Kanagawa (Japan)

    2016-07-27

    In this work, we investigated the dominating properties of the porous materials that impact water dynamics in a polymer electrolyte membrane fuel cell (PEMFC). Visualizations of liquid water in an operating PEMFC were performed at the Canadian Light Source. A miniature fuel cell was specifically designed for X-ray imaging investigations, and an in-house image processing algorithm based on the Beer-Lambert law was developed to extract quantities of liquid water thicknesses (cm) from raw X-ray radiographs. The X-ray attenuation coefficient of water at 24 keV was measured with a calibration device to ensure accurate measurements of the liquid water thicknesses. From this experiment, the through plane distribution of the liquid water in the fuel cell was obtained.

  1. Method for spatially modulating X-ray pulses using MEMS-based X-ray optics

    Science.gov (United States)

    Lopez, Daniel; Shenoy, Gopal; Wang, Jin; Walko, Donald A.; Jung, Il-Woong; Mukhopadhyay, Deepkishore

    2015-03-10

    A method and apparatus are provided for spatially modulating X-rays or X-ray pulses using microelectromechanical systems (MEMS) based X-ray optics. A torsionally-oscillating MEMS micromirror and a method of leveraging the grazing-angle reflection property are provided to modulate X-ray pulses with a high-degree of controllability.

  2. X-Ray Reflection and an Exceptionally Long Thermonuclear Helium Burst from IGR J17062-6143

    Science.gov (United States)

    Keek, L.; Iwakiri, W.; Serino, M.; Ballantyne, D. R.; in’t Zand, J. J. M.; Strohmayer, T. E.

    2017-01-01

    Thermonuclear X-ray bursts from accreting neutron stars power brief but strong irradiation of their surroundings, providing a unique way to study accretion physics. We analyze MAXI/Gas Slit Camera and Swift/XRT spectra of a day-long flash observed from IGR J17062-6143 in 2015. It is a rare case of recurring bursts at a low accretion luminosity of 0.15% Eddington. Spectra from MAXI, Chandra, and NuSTAR observations taken between the 2015 burst and the previous one in 2012 are used to determine the accretion column. We find it to be consistent with the burst ignition column of 5x10(exp 10) g cm (exp -2), which indicates that it is likely powered by burning in a deep helium layer. The burst flux is observed for over a day, and decays as a straight power law: F gamma t (exp -1.15). The burst and persistent spectra are well described by thermal emission from the neutron star, Comptonization of this emission in a hot optically thin medium surrounding the star, and reflection off the photoionized accretion disk. At the burst peak, the Comptonized component disappears, when the burst may dissipate the Comptonizing gas, and it returns in the burst tail. The reflection signal suggests that the inner disk is truncated at approximately 102 gravitational radii before the burst, but may move closer to the star during the burst. At the end of the burst, the flux drops below the burst cooling trend for 2 days, before returning to the pre-burst level.

  3. Novel micro-reactor flow cell for investigation of model catalysts using in situ grazing-incidence X-ray scattering

    DEFF Research Database (Denmark)

    Kehres, Jan; Pedersen, Thomas; Masini, Federico

    2016-01-01

    at synchrotron facilities are performed utilizing the micro-reactor and a designed transportable gas feed and analysis system. The feasibility of simultaneous in situ GISAXS/GIWAXS experiments in the novel micro-reactor flow cell was confirmed with CO oxidation over mass-selected Ru nanoparticles.......The design, fabrication and performance of a novel and highly sensitive micro-reactor device for performing in situ grazing-incidence X-ray scattering experiments of model catalyst systems is presented. The design of the reaction chamber, etched in silicon on insulator (SIO), permits grazing...

  4. On symmetric X-ray beam splitting with high efficiency by use of reflection gratings with rectangular profile in the extreme off-plane configuration.

    Science.gov (United States)

    Jark, Werner; Eichert, Diane

    2015-08-24

    In order to be reflected or diffracted off a surface structure soft X-rays and hard X-rays need to impinge at grazing angles of incidence onto the surface. In case of a reflection grating of highly symmetric structure with rectangular groove profile these grooves can be oriented parallel to the beam trajectory. In such a symmetric situation the distribution of the diffracted intensity with respect to the plane of incidence is then expected to be symmetric. This is indeed observed with symmetrically oriented diffraction peaks. It can be predicted that for appropriate structure parameters the intensity can be contained mostly in two symmetrically oriented diffraction peaks. This will also be the case for hard X-rays. The diffraction efficiency will be particularly high, when the angle of grazing incidence is chosen in the total reflection regime below the critical angle of the grating coating. These predictions were experimentally verified in this work for hard X-rays with photon energies between 4 keV and 12.4 keV. In the experiment of the order of 30% of the incident intensity was diffracted into the two first orders. This is to be compared to reflectivities of the order of 50% measured at the same coating in an unruled area of the substrate. Consequently the relative structural diffraction efficiency for each first order was about 30%, while ideally it could have been 40%. The presented grating structure will thus be a rather efficient amplitude beam splitter for hard X-rays, e.g. in the coherent beam from a free electron laser. In addition such object could then be used as the first component in Michelson interferometers for the beam characterisation or for introducing a time delay between two coherent beams.

  5. Quantitative determination on heavy metals in different stages of wine production by Total Reflection X-ray Fluorescence and Energy Dispersive X-ray Fluorescence: Comparison on two vineyards

    Energy Technology Data Exchange (ETDEWEB)

    Pessanha, Sofia [Centro Fisica Atomica, Departamento de Fisica, Faculdade de Ciencias, Universidade de Lisboa, Av. Prof. Gama Pinto, 2, 1649-003 Lisboa (Portugal); Carvalho, Maria Luisa, E-mail: luisa@cii.fc.ul.p [Centro Fisica Atomica, Departamento de Fisica, Faculdade de Ciencias, Universidade de Lisboa, Av. Prof. Gama Pinto, 2, 1649-003 Lisboa (Portugal); Becker, Maria; Bohlen, Alex von [Institute for analytical Sciences, Bunsen-Kirchhoff-Str. 11, 44139 Dortmund (Germany)

    2010-06-15

    The purpose of this study is to determine the elemental content, namely heavy metals, of samples of vine-leaves, grapes must and wine. In order to assess the influence of the vineyard age on the elemental content throughout the several stages of wine production, elemental determinations of trace elements were made on products obtained from two vineyards aged 6 and 14 years from Douro region. The elemental content of vine-leaves and grapes was determined by Energy Dispersive X-Ray Fluorescence (EDXRF), while analysis of the must and wine was performed by Total Reflection X-ray Fluorescence (TXRF). Almost all elements present in wine and must samples did not exceed the recommended values found in literature for wine. Bromine was present in the 6 years old wine in a concentration 1 order of magnitude greater than what is usually detected. The Cu content in vine-leaves from the older vineyard was found to be extremely high probably due to excessive use of Cu-based fungicides to control vine downy mildew. Higher Cu content was also detected in grapes although not so pronounced. Concerning the wine a slightly higher level was detected on the older vineyard, even so not exceeding the recommended value.

  6. Physical interactions of fish protamine and antisepsis peptide drugs with bacterial membranes revealed by combination of specular x-ray reflectivity and grazing-incidence x-ray fluorescence.

    Science.gov (United States)

    Abuillan, Wasim; Schneck, Emanuel; Körner, Alexander; Brandenburg, Klaus; Gutsmann, Thomas; Gill, Tom; Vorobiev, Alexei; Konovalov, Oleg; Tanaka, Motomu

    2013-07-01

    As a defined model of outer membranes of gram negative bacteria, we investigated the interaction of monolayers of lipopolysacchrides from Salmonella enterica rough strains R90 (LPS Ra) with natural and synthetic peptides. The fine structures perpendicular to the membrane plane and the ion distribution near the interface were determined by specular x-ray reflectivity (XRR) and grazing-incidence x-ray fluorescence (GIXF) in the presence and absence of divalent cations. The unique combination of XRR and GIXF allows for the quantitative identification of different modes of interactions in a high spatial resolution, which cannot be assessed by other experimental methods. Natural fish protamine disrupts the stratified membrane structures in the absence of Ca(2+) ions, while staying away from the membrane surface in the presence of Ca(2+) ions. In contrast, synthetic antisepsis peptide Pep 19-2.5 weakly adsorbs to the membrane and stays near the uncharged sugar units even in the absence of Ca(2+). In the presence of Ca(2+), Pep 19-2.5 can reach the negatively charged inner core without destroying the barrier capability against ions.

  7. Impact of Lipid Oxidization on Vertical Structures and Electrostatics of Phospholipid Monolayers Revealed by Combination of Specular X-ray Reflectivity and Grazing-Incidence X-ray Fluorescence.

    Science.gov (United States)

    Korytowski, Agatha; Abuillan, Wasim; Makky, Ali; Konovalov, Oleg; Tanaka, Motomu

    2015-07-30

    The influence of phospholipid oxidization of floating monolayers on the structure perpendicular to the global plane and on the density profiles of ions near the lipid monolayer has been investigated by a combination of grazing incidence X-ray fluorescence (GIXF) and specular X-ray reflectivity (XRR). Systematic variation of the composition of the floating monolayers unravels changes in the thickness, roughness and electron density of the lipid monolayers as a function of molar fraction of oxidized phospholipids. Simultaneous GIXF measurements enable one to qualitatively determine the element-specific density profiles of monovalent (K(+) or Cs(+)) and divalent ions (Ca(2+)) in the vicinity of the interface in the presence and absence of two types of oxidized phospholipids (PazePC and PoxnoPC) with high spatial accuracy (±5 Å). We found the condensation of Ca(2+) near carboxylated PazePC was more pronounced compared to PoxnoPC with an aldehyde group. In contrast, the condensation of monovalent ions could hardly be detected even for pure oxidized phospholipid monolayers. Moreover, pure phospholipid monolayers exhibited almost no ion specific condensation near the interface. The quantitative studies with well-defined floating monolayers revealed how the elevation of lipid oxidization level alters the structures and functions of cell membranes.

  8. Soft x-ray resonant magnetic reflectivity studies for in-and out-of-plane magnetization profile in ultra thin films

    Energy Technology Data Exchange (ETDEWEB)

    Tonnerre, J-M; Santis, M De; Tolentino, H C N; Grenier, S; Garaudee, S [Institut Neel, CNRS and Universite J. Fourier, F-38042 Grenoble (France); Jaouen, N [Synchrotron SOLEIL, L' Orme des Merisiers, Saint-Aubin, F-91192 Gif-sur-Yvette (France); Bontempi, E [Laboratorio di Chimica per le Tecnologie, Universita di Brescia, I-25123 Brescia (Italy); Carbone, D [ESRF, F-38043 Grenoble (France); Babonneau, D [Laboratoire de Physique des Materiaux (PHYMAT), CNRS, Universite de Poitiers, SP2MI, Teleport 2, Bvd M. et P Curie, F-86962 Futuroscope Chasseneuil (France); Staub, U, E-mail: jean-marc.tonnerre@grenoble.cnrs.f [Paul Scherrer Institut, Swiss Light Source, CH-5232 Villigen (Switzerland)

    2010-02-01

    The possibility to investigate complex magnetic profiles throughout an ultrathin magnetic film or an interface by soft x-ray resonant magnetic reflectivity is presented. The determination of in- and out-of-plane magnetic profile is shown to be possible with a subnanometer resolution by measuring the reflectivity over a wide angular range. The technique is applied to a granular magnetic multilayer and to a perpendicular exchange bias coupled system.

  9. In situ observation of fracture processes in high-strength concretes and limestone using high-speed X-ray phase-contrast imaging

    Energy Technology Data Exchange (ETDEWEB)

    Parab, Niranjan D.; Guo, Zherui; Hudspeth, Matthew; Claus, Benjamin; Lim, Boon Him; Sun, Tao; Xiao, Xianghui; Fezzaa, Kamel; Chen, Weinong W.

    2016-12-12

    The mechanical properties and fracture mechanisms of geomaterials and construction materials such as concrete are reported to be dependent on the loading rates. However, the in situ cracking inside such specimens cannot be visualized using traditional optical imaging methods since the materials are opaque. In this study, the in situ sub-surface failure/damage mechanisms in Cor-Tuf (a reactive powder concrete), a high-strength concrete (HSC) and Indiana limestone under dynamic loading were investigated using high-speed synchrotron X-ray phase-contrast imaging. Dynamic compressive loading was applied using a modified Kolsky bar and fracture images were recorded using a synchronized high-speed synchrotron X-ray imaging set-up. Three-dimensional synchrotron X-ray tomography was also performed to record the microstructure of the specimens before dynamic loading. In the Cor-Tuf and HSC specimens, two different modes of cracking were observed: straight cracking or angular cracking with respect to the direction of loading. In limestone, cracks followed the grain boundaries and voids, ultimately fracturing the specimen. Cracks in HSC were more tortuous than the cracks in Cor-Tuf specimens. The effects of the microstructure on the observed cracking behaviour are discussed. This article is part of the themed issue ‘Experimental testing and modelling of brittle materials at high strain rates’.

  10. In situ Raman spectroscopy and X-ray diffraction of pressure-induced phase transition in columbite CaNb{sub 2}O{sub 6}

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Jing [State Key Laboratory of Superhard Materials, Jilin University, Changchun 130012 (China); Feng, Guanlin [State Key Laboratory of Superhard Materials, Jilin University, Changchun 130012 (China); China Electronic Product Reliability and Environmental Testing Research Institute, Guangzhou 510610 (China); Li, Liang; Huang, Fengxian; Shen, Hongzhi; Yang, Hang [State Key Laboratory of Superhard Materials, Jilin University, Changchun 130012 (China); Wang, Wenquan [College of Physics, Jilin University, Changchun 130000 (China); Zhou, Qiang [State Key Laboratory of Superhard Materials, Jilin University, Changchun 130012 (China); College of Physics, Jilin University, Changchun 130000 (China); Xu, Dapeng, E-mail: xudp@jlu.edu.cn [State Key Laboratory of Superhard Materials, Jilin University, Changchun 130012 (China); College of Physics, Jilin University, Changchun 130000 (China)

    2013-12-05

    Highlights: •The phase transition of CaNb{sub 2}O{sub 6} was investigated for the first time under high pressure. •In situ Raman spectroscopy and Synchrotron X-ray diffraction were measured. •A pressure-induced reversible phase transition was observed below 23 GPa. •The orthorhombic columbite Pbcn transforms to monoclinic structure P2{sub 1}/c. •The lattice parameters of the new phase were obtained by the Pawley refinements. -- Abstract: The in situ high pressure studies of CaNb{sub 2}O{sub 6} have been performed using Raman spectroscopy and Synchrotron X-ray diffraction in a DAC up to 23 GPa. Raman experiments show that most Raman peaks decrease in intensity and shift toward high wave numbers with increasing pressure. Two turn points in the slope of frequency–pressure curve of the slopes of Raman modes turn up at the pressure around 8 and 15 GPa. ADXRD results display that the old peaks disappear and some new peaks appear above 9.4 GPa, and the patterns remain unchanged above 15 GPa. Both Raman and X-ray diffraction data provide evidence of a reversible phase transition beginning from about 8 GPa and completing at 15 GPa.

  11. Growth and structure of water on SiO2 films on Si investigated byKelvin probe microscopy and in situ X-ray Spectroscopies

    Energy Technology Data Exchange (ETDEWEB)

    Verdaguer, A.; Weis, C.; Oncins, G.; Ketteler, G.; Bluhm, H.; Salmeron, M.

    2007-06-14

    The growth of water on thin SiO{sub 2} films on Si wafers at vapor pressures between 1.5 and 4 torr and temperatures between -10 and 21 C has been studied in situ using Kelvin Probe Microscopy and X-ray photoemission and absorption spectroscopies. From 0 to 75% relative humidity (RH) water adsorbs forming a uniform film 4-5 layers thick. The surface potential increases in that RH range by about 400 mV and remains constant upon further increase of the RH. Above 75% RH the water film grows rapidly, reaching 6-7 monolayers at around 90% RH and forming a macroscopic drop near 100%. The O K-edge near-edge X-ray absorption spectrum around 75% RH is similar to that of liquid water (imperfect H-bonding coordination) at temperatures above 0 C and ice-like below 0 C.

  12. In-situ synchrotron x-ray studies of the microstructure and stability of In 2 O 3 epitaxial films

    Energy Technology Data Exchange (ETDEWEB)

    Highland, M. J.; Hruszkewycz, S. O.; Fong, D. D.; Thompson, Carol; Fuoss, P. H.; Calvo-Almazan, I.; Maddali, S.; Ulvestad, A.; Nazaretski, E.; Huang, X.; Yan, H.; Chu, Y. S.; Zhou, H.; Baldo, P. M.; Eastman, J. A.

    2017-10-16

    We report on the synthesis, stability, and local structure of In2O3 thin films grown via rf-magnetron sputtering and characterized by in-situ x-ray scattering and focused x-ray nanodiffraction. We find that In2O3 deposited onto (0 0 1)-oriented single crystal yttria-stabilized zirconia substrates adopts a Stranski-Krastanov growth mode at a temperature of 850 degrees C, resulting in epitaxial, truncated square pyramids with (1 1 1) side walls. We find that at this temperature, the pyramids evaporate unless they are stabilized by a low flux of In2O3 from the magnetron source. We also find that the internal lattice structure of one such pyramid is made up of differently strained volumes, revealing local structural heterogeneity that may impact the properties of In2O3 nanostructures and films.

  13. In situ observation of Cu-Ni alloy nanoparticle formation by X-ray diffraction, X-ray absorption spectroscopy, and transmission electron microscopy: Influence of Cu/Ni ratio

    DEFF Research Database (Denmark)

    Wu, Qiongxiao; Duchstein, Linus Daniel Leonhard; Chiarello, Gian Luca

    2014-01-01

    Silica-supported, bimetallic Cu-Ni nanomaterials were prepared with different ratios of Cu to Ni by incipient wetness impregnation without a specific calcination step before reduction. Different in situ characterization techniques, in particular transmission electron microscopy (TEM), X-ray diffr......Silica-supported, bimetallic Cu-Ni nanomaterials were prepared with different ratios of Cu to Ni by incipient wetness impregnation without a specific calcination step before reduction. Different in situ characterization techniques, in particular transmission electron microscopy (TEM), X......, which results in improved reducibility of the Ni species compared with monometallic Ni. At high Ni concentrations silica-supported Cu-Ni alloys form a homogeneous solid solution of Cu and Ni, whereas at lower Ni contents Cu and Ni are partly segregated and form metallic Cu and Cu-Ni alloy phases. Under...... the same reduction conditions, the particle sizes of reduced Cu-Ni alloys decrease with increasing Ni content. Estimates of the metal surface area from sulfur chemisorption and from the XRD particle size generally agree well on the trend across the composition range, but show some disparity in terms...

  14. Total reflection X-ray fluorescence analysis of oral fluids of women affected by osteoporosis and osteopenia

    Science.gov (United States)

    Sánchez, Héctor Jorge; Valentinuzzi, María Cecilia; Grenón, Miram; Abraham, José

    2008-12-01

    Osteoporosis is a disease characterized by low bone mass and microarchitectural deterioration of bone tissue, leading to bone fragility and an increased susceptibility to fractures; the early stage of decreased bone density is called osteopenia. More than 200 million people are affected and about 50% of post-menopausic women are expected to develop the disease. Osteoporosis, osteopenia and periodontal disease have in common several risk factors, being hyperthyroidism and smoking habits the most important ones. There is scarce information in the literature about the association between periodontal disease and osteoporosis and/or osteopenia. Some works suggest that osteoporotic women are susceptible to a higher loss of periodontal insertion, alveolar bones, and teeth. Thirty adult post-menopausic women were studied; some of them were healthy (control group) and the rest of them were undergoing some stage of osteoporosis or osteopenia. All the subjects were healthy, non-smokers, not having dental implants, and with communitarian periodontal index higher than 1(CPI > 1). Samples of saliva and gingival crevice fluid were extracted with calibrated micro-capillaries and deposited on Si reflectors. Known amounts of Ga were added to the samples in order to act as internal standard for quantification by the total reflection x-ray fluorescence technique. Experimental concentrations of several elements (P, S, Cl, K, Ca, Cr, Fe, NI, Cu, and Zn) were determined. The concentration of some elements in saliva showed different behavior as compared to gingival crevice fluid. Some critical elements of bone composition, such as Ca and Zn, present very distinguishable behavior. Improvements in the statistics are required for a better assessment of a routine method and to establish some correlation with periodontal disease. TXRF seems to be a promising method to evaluate the evolution of osteoporosis.

  15. X-ray and Neutron Reflectivity Study Shows That CLIC1 Undergoes Cholesterol-Dependent Structural Reorganization in Lipid Monolayers.

    Science.gov (United States)

    Hossain, Khondker R; Holt, Stephen A; Le Brun, Anton P; Al Khamici, Heba; Valenzuela, Stella M

    2017-10-31

    CLIC1 belongs to the ubiquitous family of chloride intracellular ion channel proteins that are evolutionarily conserved across species. The CLICs are unusual in that they exist mainly as soluble proteins but possess the intriguing property of spontaneous conversion from the soluble to an integral membrane-bound form. This conversion is regulated by the membrane lipid composition, especially by cholesterol, together with external factors such as oxidation and pH. However, the precise physiological mechanism regulating CLIC1 membrane insertion is currently unknown. In this study, X-ray and neutron reflectivity experiments were performed to study the interaction of CLIC1 with different phospholipid monolayers prepared using POPC, POPE, or POPS with and without cholesterol in order to better understand the regulatory role of cholesterol in CLIC1 membrane insertion. Our findings demonstrate for the first time two different structural orientations of CLIC1 within phospholipid monolayers, dependent upon the absence or presence of cholesterol. In phospholipid monolayers devoid of cholesterol, CLIC1 was unable to insert into the lipid acyl chain region. However, in the presence of cholesterol, CLIC1 showed significant insertion within the phospholipid acyl chains occupying an area per protein molecule of 6-7 nm2 with a total CLIC1 thickness ranging from ∼50 to 56 Å across the entire monolayer. Our data strongly suggests that cholesterol not only facilitates the initial docking or binding of CLIC1 to the membrane but also promotes deeper penetration of CLIC1 into the hydrophobic tails of the lipid monolayer.

  16. Total reflection X-ray fluorescence analysis of oral fluids of women affected by osteoporosis and osteopenia

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez, Hector Jorge [Facultad de Matematica Astronomia y Fisica, Universidad Nacional de Cordoba, 5000 Cordoba (Argentina)], E-mail: jsan@famaf.unc.edu.ar; Valentinuzzi, Maria Cecilia [Facultad de Matematica Astronomia y Fisica, Universidad Nacional de Cordoba, 5000 Cordoba (Argentina); Grenon, Miram [Facultad de Odontologia, Universidad Nacional de Cordoba, 5000 Cordoba (Argentina); Abraham, Jose [Facultad de Matematica Astronomia y Fisica, Universidad Nacional de Cordoba, 5000 Cordoba (Argentina)

    2008-12-15

    Osteoporosis is a disease characterized by low bone mass and microarchitectural deterioration of bone tissue, leading to bone fragility and an increased susceptibility to fractures; the early stage of decreased bone density is called osteopenia. More than 200 million people are affected and about 50% of post-menopausic women are expected to develop the disease. Osteoporosis, osteopenia and periodontal disease have in common several risk factors, being hyperthyroidism and smoking habits the most important ones. There is scarce information in the literature about the association between periodontal disease and osteoporosis and/or osteopenia. Some works suggest that osteoporotic women are susceptible to a higher loss of periodontal insertion, alveolar bones, and teeth. Thirty adult post-menopausic women were studied; some of them were healthy (control group) and the rest of them were undergoing some stage of osteoporosis or osteopenia. All the subjects were healthy, non-smokers, not having dental implants, and with communitarian periodontal index higher than 1(CPI > 1). Samples of saliva and gingival crevice fluid were extracted with calibrated micro-capillaries and deposited on Si reflectors. Known amounts of Ga were added to the samples in order to act as internal standard for quantification by the total reflection x-ray fluorescence technique. Experimental concentrations of several elements (P, S, Cl, K, Ca, Cr, Fe, NI, Cu, and Zn) were determined. The concentration of some elements in saliva showed different behavior as compared to gingival crevice fluid. Some critical elements of bone composition, such as Ca and Zn, present very distinguishable behavior. Improvements in the statistics are required for a better assessment of a routine method and to establish some correlation with periodontal disease. TXRF seems to be a promising method to evaluate the evolution of osteoporosis.

  17. Determination of As concentration in earthworm coelomic fluid extracts by total-reflection X-ray fluorescence spectrometry

    Science.gov (United States)

    Allegretta, Ignazio; Porfido, Carlo; Panzarino, Onofrio; Fontanella, Maria Chiara; Beone, Gian Maria; Spagnuolo, Matteo; Terzano, Roberto

    2017-04-01

    Earthworms are often used as sentinel organisms to study As bioavailability in polluted soils. Arsenic in earthworms is mainly sequestrated in the coelomic fluids whose As content can therefore be used to asses As bioavalability. In this work, a method for determining As concentration in coelomic fluid extracts using total-reflection X-ray fluorescence spectrometry (TXRF) is presented. For this purpose coelomic fluid extracts from earthworms living in three polluted soils and one non-polluted (control) soil have been collected and analysed. A very simple sample preparation was implemented, consisting of a dilution of the extracts with polyvinyl alcohol (PVA) using a 1:8 ratio and dropwise deposition of the sample on the reflector. A detection limit of 0.2 μg/l and quantification limit of 0.6 μg/l was obtained in the diluted samples, corresponding to 2 μg/l and 6 μg/l in the coelomic fluid extracts, respectively. This allowed to quantify As concentration in coelomic fluids extracted from earthworms living in soils polluted with As at concentrations higher than 20 mg/kg (considered as a pollution threshold for agricultural soils). The TXRF method has been validated by comparison with As concentrations in standards and by analysing the same samples by ICP-MS, after acid digestion of the sample. The low limit of detection, the proven reliability of the method and the little sample preparation make TXRF a suitable, cost-efficient and "green" technique for the analysis of As in earthworm coelomic fluid extracts for bioavailability studies.

  18. Quantitative analysis of total reflection X-ray fluorescence from finely layered structures using XeRay

    Energy Technology Data Exchange (ETDEWEB)

    Gong, Zhiliang [James Franck Institute, The University of Chicago, Chicago, Illinois 60637, USA; Department of Chemistry, The University of Chicago, Chicago, Illinois 60637, USA; Kerr, Daniel [Program in the Biophysical Sciences, Institute for Biophysical Dynamics, The University of Chicago, Chicago, Illinois 60637, USA; Hwang, Hyeondo Luke [James Franck Institute, The University of Chicago, Chicago, Illinois 60637, USA; Department of Chemistry, The University of Chicago, Chicago, Illinois 60637, USA; Henderson, J. Michael [James Franck Institute, The University of Chicago, Chicago, Illinois 60637, USA; Department of Chemistry, The University of Chicago, Chicago, Illinois 60637, USA; Suwatthee, Tiffany [The College, The University of Chicago, Chicago, Illinois 60637, USA; Slaw, Benjamin R. [James Franck Institute, The University of Chicago, Chicago, Illinois 60637, USA; Department of Chemistry, The University of Chicago, Chicago, Illinois 60637, USA; Cao, Kathleen D. [James Franck Institute, The University of Chicago, Chicago, Illinois 60637, USA; Department of Chemistry, The University of Chicago, Chicago, Illinois 60637, USA; Lin, Binhua [James Franck Institute, The University of Chicago, Chicago, Illinois 60637, USA; Center for Advanced Radiation Sources, The University of Chicago, Chicago, Illinois 60637, USA; Bu, Wei [Center for Advanced Radiation Sources, The University of Chicago, Chicago, Illinois 60637, USA; Lee, Ka Yee C. [James Franck Institute, The University of Chicago, Chicago, Illinois 60637, USA; Department of Chemistry, The University of Chicago, Chicago, Illinois 60637, USA; Center for Advanced Radiation Sources, The University of Chicago, Chicago, Illinois 60637, USA

    2017-03-01

    Total reflection x-ray fluorescence (TXRF) is a widely applicable experimental technique for studying chemical element distributions across finely layered structures at extremely high sensitivity. To promote and facilitate scientific discovery using TXRF, we developed a MATLAB-based software package with a graphical user interface, named XeRay, for quick, accurate, and intuitive data analysis. XeRay lets the user model any layered system, each layer with its independent chemical composition and thickness, and enables fine-tuned data fitting. The accuracy of XeRay has been tested in the analysis of TXRF data from both air/liquid interface and liquid/liquid interfacial studies and has been compared to literature results. In an air/liquid interface study, Ca2+ sequestration was measured at a Langmuir monolayer of 1-stearoyl-2-oleoyl-sn-glycero-3-phosphatidic acid (SOPA) on a buffer solution of 1 mM CaCl2 at pH 7.5. Data analysis with XeRay reveals that each 1 nm2 of interfacial area contains 2.38 ± 0.06 Ca2+ ions, which corresponds to a 1:1 ratio between SOPA headgroups and Ca2+ ions, consistent with several earlier reports. For the liquid/liquid interface study of Sr2+ enrichment at the dodecane/surfactant/water interface, analysis using XeRay gives a surface enrichment of Sr2+ at 68+6-568-5+6 Å2 per ion, consistent with the result published for the same dataset.

  19. X-ray in-situ study of copper electrodeposition on UHV prepared GaAs(001) surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Gruender, Yvonne

    2008-06-02

    For this work a unique setup for in-situ electrochemical studies was employed and improved. This setup permits UHV preparation of the GaAs(001) surface with a defined surface termination (arsenic-rich or gallium-rich) and its characterization by SXRD in UHV, under ambient pressure in inert gas and in electrolyte under potential control without passing through air. The GaAs(001) surfaces were capped by amorphous arsenic. This permitted to ship them through ambient air. Afterwards smooth well defined GaAs(001) surfaces could be recovered by thermal annealing in UHV. A first investigation of the arsenic capped sample was done by atomic force microscopy (AFM) and Surface X-Ray Diffraction (SXRD). The non bulk like termination of the arsenic buried GaAs(001) surface was revealed. For the electrochemical metal deposition, arsenic terminated (2 x 4) reconstructed and gallium terminated (4 x 2) reconstructed GaAs(001) surfaces were employed. These surfaces were characterized by STM, LEED and a first time by SXRD. The surfaces are smooth, however, a higher degree of disorder than for MBE prepared reconstructed GaAs(001) is found. After exposure of the sample to nitrogen, the surfaces were then again studied by SXRD. These two steps characterizing the bare GaAs(001) surfaces permitted us to get a better knowledge of the starting surface and its influence on the later electrodeposited copper. At ambient pressure both reconstructions are lifted, but the surface is not bulk-like terminated as can be deduced from the crystal truncation rods. Epitaxial copper clusters grow upon electrodeposition on the UHV prepared GaAs(001) surface. The copper lattice is rotated and inclined with respect to the GaAs substrate lattice, leading to eight symmetry equivalent domains. The influence of the surface termination as well as the nucleation potential on the structure of the electrodeposited copper were investigated. The tilt and rotation angles do not depend on the deposition potential but

  20. Ultra-short-period W/B4C multilayers for x-ray optics-microstructure limits on reflectivity

    Energy Technology Data Exchange (ETDEWEB)

    Walton, Christopher Charles [Univ. of California, Berkeley, CA (United States). Dept. of Materials Science and Mineral Engineering

    1997-12-01

    Multilayer thin films are used as Bragg reflectors for soft x-rays in the energy range 50eV < E < 1000eV in many x-ray optics applications such as x-ray microscopes and telescopes, reducing optics for extreme ultraviolet (EUV) lithography, and x-ray polarizers and phase retarders. Applications often depend critically on reflectivity, which has not been systematically characterized for multilayer periods below 20Å. For this study, W/B4C multilayers were fabricated by magnetron sputtering on Si(111), with periods from 48Å to as little as 4.7Å. The x-ray reflectivity measured at λ = 1.54Å and at 45° incidence (289 eV < E < 860 eV) was found to decrease sharply for multilayer periods less than 15-20Å. Examination by high-resolution transmission electron microscopy (HRTEM) showed an expansion of the thickness of the W-rich layers of 30-40% from the nominal values, consistent with intermixture of the two materials during sputter growth, and discontinuous W-rich layers for multilayer periods below about 15Å. The experimental data for the specular reflectivity in the hard and soft x-ray regimes and the diffuse scattering fit well to a model of multilayer roughness. The model is expressed as a power-law dependence of roughness on spatial frequency. Analysis of small-angle scattering in transmission from multilayers grown on freestanding Si3N4 membranes confirms the onset of discontinuity at periods between 14Å and 22Å. Spectroscopy studies by x-ray absorption (NEXAFS) and electron energy loss (EELS) at the boron K-edge (188eV) are consistent with changes in the average boron bonding environment, as the multilayer period decreases and the W-rich layers are increasingly thin and dispersed. A discrete W-rich phase is present for periods at least as small as 6.3Å.

  1. Joint x-ray

    Science.gov (United States)

    X-ray - joint; Arthrography; Arthrogram ... x-ray technologist will help you position the joint to be x-rayed on the table. Once in place, pictures are taken. The joint may be moved into other positions for more ...

  2. Online in situ x-ray diffraction setup for structural modification studies during swift heavy ion irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Grygiel, C.; Lebius, H.; Bouffard, S.; Quentin, A.; Ramillon, J. M.; Madi, T.; Guillous, S.; Been, T.; Guinement, P.; Lelievre, D.; Monnet, I. [CIMAP, CEA-CNRS-ENSICAEN-UCBN, BP 5133, 14070 Caen Cedex 5 (France)

    2012-01-15

    The high energy density of electronic excitations due to the impact of swift heavy ions can induce structural modifications in materials. We present an x-ray diffractometer called ALIX (''Analyse en Ligne sur IRRSUD par diffraction de rayons X''), which has been set up at the low-energy beamline (IRRadiation SUD - IRRSUD) of the Grand Accelerateur National d'Ions Lourds facility, to allow the study of structural modification kinetics as a function of the ion fluence. The x-ray setup has been modified and optimized to enable irradiation by swift heavy ions simultaneously to x-ray pattern recording. We present the capability of ALIX to perform simultaneous irradiation-diffraction by using energy discrimination between x-rays from diffraction and from ion-target interaction. To illustrate its potential, results of sequential or simultaneous irradiation-diffraction are presented in this article to show radiation effects on the structural properties of ceramics. Phase transition kinetics have been studied during xenon ion irradiation of polycrystalline MgO and SrTiO{sub 3}. We have observed that MgO oxide is radiation-resistant to high electronic excitations, contrary to the high sensitivity of SrTiO{sub 3}, which exhibits transition from the crystalline to the amorphous state during irradiation. By interpreting the amorphization kinetics of SrTiO{sub 3}, defect overlapping models are discussed as well as latent track characteristics. Together with a transmission electron microscopy study, we conclude that a single impact model describes the phase transition mechanism.

  3. Ion-Bombardment of Thin-Layers - the Effect on the Interface Roughness and Its X-Ray Reflectivity

    NARCIS (Netherlands)

    Puik, E. J.; van der Wiel, M. J.; Zeijlemaker, H.; Verhoeven, J.

    1992-01-01

    In this paper we report on experiments which indicate the necessity of the use of ion-beam bombardment for e-beam deposited multilayer x-ray coatings. Measurements are described in which ion bombardment (200-300 eV Ar+) is used to ion etch metal layers after initial deposition and during deposition

  4. Enhancement of Reflectivity of Multilayer Mirrors for Soft-X-Ray Projection Lithography by Temperature Optimization and Ion-Bombardment

    NARCIS (Netherlands)

    E. Louis,; Voorma, H. J.; Koster, N. B.; Shmaenok, L.; F. Bijkerk,; Schlatmann, R.; Verhoeven, J.; Platonov, Y. Y.; van Dorssen, G. E.; Padmore, H. A.

    1994-01-01

    In this paper we discuss two techniques to optimize the quality of multilayer x-ray mirrors, namely optimization of the temperature of the substrates during deposition and ion-bombardment of the layers. We produced Mo/Si multilayers applying both methods and present the effect on the near normal

  5. In situ micro-focused X-ray beam characterization with a lensless camera using a hybrid pixel detector.

    Science.gov (United States)

    Kachatkou, Anton; Marchal, Julien; van Silfhout, Roelof

    2014-03-01

    Results of studies on micro-focused X-ray beam diagnostics using an X-ray beam imaging (XBI) instrument based on the idea of recording radiation scattered from a thin foil of a low-Z material with a lensless camera are reported. The XBI instrument captures magnified images of the scattering region within the foil as illuminated by the incident beam. These images contain information about beam size, beam position and beam intensity that is extracted during dedicated signal processing steps. In this work the use of the device with beams for which the beam size is significantly smaller than that of a single detector pixel is explored. The performance of the XBI device equipped with a state-of-the-art hybrid pixel X-ray imaging sensor is analysed. Compared with traditional methods such as slit edge or wire scanners, the XBI micro-focused beam characterization is significantly faster and does not interfere with on-going experiments. The challenges associated with measuring micrometre-sized beams are described and ways of optimizing the resolution of beam position and size measurements of the XBI instrument are discussed.

  6. The behavior of single-crystal silicon to dynamic loading using in-situ X-ray diffraction and phase contrast imaging

    Science.gov (United States)

    Lee, Hae Ja; Xing, Zhou; Galtier, Eric; Arnold, Brice; Granados, Eduardo; Brown, Shaughnessy B.; Tavella, Franz; McBride, Emma; Fry, Alan; Nagler, Bob; Schropp, Andreas; Seiboth, Frank; Samberg, Dirk; Schroer, Christian; Gleason, Arianna E.; Higginbotham, Andrew

    Hydrostatic and uniaxial compression studies have revealed that crystalline silicon undergoes phase transitions from a cubic diamond structure to a variety of phases including orthorhombic Imma phase, body-centered tetragonal phase, and a hexagonal primitive phase. The dynamic response of silicon at high pressure, however, is not well understood. Phase contrast imaging has proven to be a powerful tool for probing density changes caused by the shock propagation into a material. In order to characterize the elastic and phase transitions, we image shock waves in Si with high spatial resolution using the LCLS X-ray free electron laser and Matter in Extreme Conditions instrument. In this study, the long pulse optical laser with pseudo-flat top shape creates high pressures up to 60 GPa. We measure the crystal structure by observing X-ray diffraction orthogonal to the shock propagation direction over a range of pressures. We describe the capability of simultaneously performing phase contrast imaging and in situ X-ray diffraction during shock loading and discuss the dynamic response of Si in high-pressure phases Use of the Linac Coherent Light Source (LCLS), SLAC National Accelerator Laboratory, is supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences under Contract No. DE-AC02-76SF00515. The MEC instrument is supported by.

  7. Direct analysis of blood serum by total reflection X-ray fluorescence spectrometry and application of an artificial neural network approach for cancer diagnosis*1

    Science.gov (United States)

    Hernández-Caraballo, Edwin A.; Marcó-Parra, Lué M.

    2003-12-01

    Iron, copper, zinc and selenium were determined directly in serum samples from healthy individuals ( n=33) and cancer patients ( n=27) by total reflection X-ray fluorescence spectrometry using the Compton peak as internal standard [L.M. Marcó P. et al., Spectrochim. Acta Part B 54 (1999) 1469-1480]. The standardized concentrations of these elements were used as input data for two-layer artificial neural networks trained with the generalized delta rule in order to classify such individuals according to their health status. Various artificial neural networks, comprising a linear function in the input layer, a hyperbolic tangent function in the hidden layer and a sigmoid function in the output layer, were evaluated for such a purpose. Of the networks studied, the (4:4:1) gave the highest estimation (98%) and prediction rates (94%). The latter demonstrates the potential of the total reflection X-ray fluorescence spectrometry/artificial neural network approach in clinical chemistry.

  8. Center for X-ray Optics, 1988

    Energy Technology Data Exchange (ETDEWEB)

    1989-04-01

    This report briefly reviews the following topics: soft-x-ray imaging; reflective optics for hard x-rays; coherent XUV sources; spectroscopy with x-rays; detectors for coronary artery imaging; synchrotron-radiation optics; and support for the advanced light source.

  9. Portable ultrahigh-vacuum sample storage system for polarization-dependent total-reflection fluorescence x-ray absorption fine structure spectroscopy

    OpenAIRE

    Watanabe, Yoshihide; Nishimura, Yusaku F.; Suzuki, Ryo; Uehara, Hiromitsu; Nimura, Tomoyuki; Beniya, Atsushi; Isomura, Noritake; Asakura, Kiyotaka; Takakusagi, Satoru

    2016-01-01

    A portable ultrahigh-vacuum sample storage system was designed and built to investigate the detailed geometric structures of mass-selected metal clusters on oxide substrates by polarization-dependent total-reflection fluorescence x-ray absorption fine structure spectroscopy (PTRF-XAFS). This ultrahigh-vacuum (UHV) sample storage system provides the handover of samples between two different sample manipulating systems. The sample storage system is adaptable for public transportation, facilitat...

  10. In-situ CdCl{sub 2}-treated CdTe film surface analysis by X-ray photoelectron spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Vamsi Krishna, K.; Dutta, V. [Centre for Energy Studies, Indian Institute of Technology Delhi, Hauz Khas, New Delhi 100 016 (India)

    2004-07-01

    CdTe thin films are deposited using a spray pyrolysis technique without and with in-situ CdCl{sub 2} treatment. An X-ray photoelectron spectroscopy technique is used to study the Cd, Te, O and Cl chemical environments and the valence-band spectra of the CdTe film surface. A shift in the Fermi-level position of {proportional_to}200 meV towards the valence-band maximum is observed in the CdTe film after the in-situ CdCl{sub 2} treatment, which is attributed to the increment of the Cl concentration and the improvement in the grain growth of the CdTe film. In addition to the increment of the Cl concentration, less surface oxidation is observed compared to that for ex-situ treatment. (copyright 2004 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  11. Atomic and electronic aspects of the coloration mechanism of gasochromic Pt/Mo-modified V2O5 smart films: an in situ X-ray spectroscopic study.

    Science.gov (United States)

    Lu, Ying-Rui; Hsu, Hsin-Hua; Chen, Jeng-Lung; Chang, Han-Wei; Chen, Chi-Liang; Chou, Wu-Ching; Dong, Chung-Li

    2016-02-21

    In this work, gasochromic pristine and Mo-modified V2O5 thin films were prepared by the sol-gel spin coating method. Both films exhibit excellent gasochromic coloration. Synchrotron grazing incidence X-ray diffraction reveals that the Mo-modified V2O5 thin film is more amorphous than the pristine V2O5 thin film. X-ray absorption spectroscopy (XAS) was utilized to elucidate the modifications of the local electronic and atomic structures that are caused by Mo. In situ soft-XAS and in situ hard-XAS were performed to monitor the effect of the adsorption of dihydrogen on the charge state of vanadium and local atomic rearrangement in the gasochromic thin films. The gasochromic V2O5 film has a significantly pyramid-like oxygen-coordinated environment. However, the Mo-modified film exhibits mixed pyramid- and octahedral-like structures. Analytic results indicate that upon gasochromic coloration, adsorption of hydrogen adds electrons to the V 3d t2g orbital, lowering the charge state of vanadium. The films undergo structural modification before the valence is changed. The Mo-modified V2O5 film exhibits faster coloration because the apical V-O bond differs from that in the pristine V2O5 film. This in situ XAS allows real-time monitoring of changes in the element-specific local atomic structure during the gasochromic reaction and enables the elucidation of the gasochromic mechanism.

  12. In situ synchrotron X-ray diffraction study of deformation behavior and load transfer in a Ti2Ni-NiTi composite

    Science.gov (United States)

    Zhang, Junsong; Liu, Yinong; Ren, Yang; Huan, Yong; Hao, Shijie; Yu, Cun; Shao, Yang; Ru, Yadong; Jiang, Daqiang; Cui, Lishan

    2014-07-01

    The deformation behavior and load transfer of a dual-phase composite composed of martensite NiTi embedded in brittle Ti2Ni matrices were investigated by using in situ synchrotron x-ray diffraction during compression. The composite exhibits a stage-wise deformation feature and a double-yielding phenomenon, which were caused by the interaction between Ti2Ni and NiTi with alternative microscopic deformation mechanism. No load transfer occurs from the soft NiTi dendrites to the hard Ti2Ni matrices during the pseudoplastic deformation (detwinning) of NiTi, which is significantly different from that previously reported in bulk metallic glasses matrices composites.

  13. In situ soft X-ray absorption spectroscopy investigation of electrochemical corrosion of copper in aqueous NaHCO3 solution

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Peng; Chen, Jeng-Lung; Borondics, Ferenc; Glans, Per-Anders; West, Mark W.; Chang, Ching-Lin; Salmeron, Miquel; Guo, Jinghua

    2010-03-31

    A novel electrochemical setup has been developed for soft x-ray absorption studies of the electronic structure of electrode materials during electrochemical cycling. In this communication we illustrate the operation of the cell with a study of the corrosion behavior of copper in aqueous NaHCO3 solution via the electrochemically induced changes of its electronic structure. This development opens the way for in situ investigations of electrochemical processes, photovoltaics, batteries, fuel cells, water splitting, corrosion, electrodeposition, and a variety of important biological processes.

  14. Potential controlled stripping of an amorphous As layer on GaAs(001) in an electrolyte: An in situ x-ray scattering study

    DEFF Research Database (Denmark)

    Scherb, G.; Kazimirov, A.; Zegenhagen, J.

    1997-01-01

    2SO4. we monitored the stripping process of the 50 nm As cap over a period of hours in situ with x-ray diffraction. Our results suggest that, using this potential controlled stripping, smooth and well ordered GaAs(001) surfaces can be obtained in an aqueous electrolyte. (C) 1997 American Institute......We demonstrate that an amorphous As layer deposited as protection on a GaAs(001) surface frown by molecular beam epitaxy can be removed via reductive etching in an electrolytical cell at sufficiently negative electrode potentials. Employing a specially constructed electrochemical cell filled with H...

  15. A rapid total reflection X-ray fluorescence protocol for micro analyses of ion profiles in Arabidopsis thaliana

    Science.gov (United States)

    Höhner, Ricarda; Tabatabaei, Samaneh; Kunz, Hans-Henning; Fittschen, Ursula

    2016-11-01

    The ion homeostasis of macro and micronutrients in plant cells and tissues is a fundamental requirement for vital biochemical pathways including photosynthesis. In nature, ion homeostasis is affected mainly by three processes: 1. Environmental stress factors, 2. Developmental effects, and 3. Loss or gain-of-function mutations in the plant genome. Here we present a rapid total reflection X-ray fluorescence (TXRF) protocol that allows for simultaneous quantification of several elements such as potassium (K), calcium (Ca), sulfur (S), manganese (Mn) and strontium (Sr) in Arabidopsis thaliana leaf specimens. Our procedure is cost-efficient and enables precise, robust and highly reproducible measurements on tissue samples as small as 0.3 mg dry weight. As shown here, we apply the TXRF procedure to detect accurately the early replacement of K by Na ions in leaves of plants exposed to soil salinity, a globally increasing abiotic stress factor. Furthermore, we were able to prove the existence of a leaf development-dependent ion gradient for K, Ca, and other divalent ions in A. thaliana; i.e. old leaves contain significantly lower K but higher Ca than young leaves. Lastly, we show that our procedure can be readily applied to reveal subtle differences in tissue-specific ion contents of plant mutants. We employed independent A. thaliana kea1kea2 loss-of-function mutants that lack KEA1 and KEA2, two highly active chloroplast K exchange proteins. We found significantly increased K levels specifically in kea1kea2 mutants, i.e. 55 mg ∗ g- 1 dry weight, compared to 40 mg ∗ g- 1 dry weight in wild type plants. The TXRF procedure can be supplemented with Flame atomic absorption (FAAS) and emission spectrometry (FAES) to expand the detection range to sodium (Na) and magnesium (Mg). Because of the small sample amounts required, this method is especially suited to probe individual leaves in single plants or even specific leaf areas. Therefore, TXRF represents a powerful method to

  16. In situ multi-element analyses by energy-dispersive X-ray fluorescence on varnishes of historical violins

    Energy Technology Data Exchange (ETDEWEB)

    Echard, Jean-Philippe [Laboratoire de recherche et de restauration, Musee de la musique, Cite de la musique, 221, avenue Jean-Jaures, 75019 Paris (France)]. E-mail: jpechard@cite-musique.fr

    2004-10-08

    Varnishes of Italian violins and other historical stringed instruments have been analyzed by energy-dispersive X-ray fluorescence (EDXRF). The instruments whose varnishes were to be analyzed were chosen from the collection kept in Musee de la Musique in Paris. Direct analyses were performed on instrument varnishes, without any sampling and non-destructively, showing inorganic elements such as lead, mercury and iron that could be related to siccatives or pigments. Analytical results and their comparison with old formulae or traditional recipes of violin varnishes, as with the few previous analytical results, will be discussed.

  17. The changing source of X-ray reflection in the radio-intermediate Seyfert 1 galaxy III Zw 2

    Science.gov (United States)

    Gonzalez, A. G.; Waddell, S. G. H.; Gallo, L. C.

    2018-03-01

    We report on X-ray observations of the radio-intermediate, X-ray bright Seyfert 1 galaxy, III Zw 2, obtained with XMM-Newton, Suzaku, and Swift over the past 17 yr. The source brightness varies significantly over yearly time-scales, but more modestly over periods of days. Pointed observations with XMM-Newton in 2000 and Suzaku in 2011 show spectral differences despite comparable X-ray fluxes. The Suzaku spectra are consistent with a power-law continuum and a narrow Gaussian emission feature at ˜6.4 keV, whereas the earlier XMM-Newton spectrum requires a broader Gaussian profile and soft-excess below ˜2 keV. A potential interpretation is that the primary power-law emission, perhaps from a jet base, preferentially illuminates the inner accretion disc in 2000, but the distant torus in 2011. The interpretation could be consistent with the hypothesized precessing radio jet in III Zw 2 that may have originated from disc instabilities due to an ongoing merging event.

  18. Rb+ and Sr2+ adsorption at the TiO2 (110)-electrolyte interface observed with resonant anomalous X-ray reflectivity.

    Science.gov (United States)

    Kohli, Vaibhav; Zhang, Zhan; Park, Changyong; Fenter, Paul

    2010-01-19

    We report the vertical density profiles of Rb(+) and Sr(2+) at the rutile TiO(2)(110)-electrolyte interface for the following bulk electrolyte conditions, [Rb(+)] = 1 mM at pH 11 and [Sr(2+)] = 0.1 mM at pH 10.3, using X-ray reflectivity and resonant anomalous X-ray reflectivity. We find that Rb(+) specifically adsorbs with a coverage of 0.080 +/- 0.003 monolayer (ML) and a height of 3.72 +/- 0.03 A above the surface Ti-O plane. In comparison, Sr(2+) adsorbs with a coverage of 0.40 +/- 0.07 ML and an average height of 3.05 +/- 0.16 A, but with a significant vertical distribution width (0.35 +/- 0.02 A). The Sr(2+) distribution in the presence of a background electrolyte ([Na(+)] = 30 mM) was also investigated, and it is found that, while the ion height and coverage are unchanged within the uncertainties of the measurements, the width of the distribution is apparently increased in the presence of Na(+). Comparison is made with previous results, including XR and X-ray standing waves (XSW) measurements, and molecular dynamics simulations. Our results are in excellent agreement with a recently proposed multisite adsorption mechanism that suggests simultaneous adsorption in two inner-sphere adsorption geometries, the tetradentate and the bidentate sites.

  19. Reflection optimization of nano-multilayer X-ray mirrors in three-edge energies: Cr-Kα, Co-Kα, and Ti-Kα

    Directory of Open Access Journals (Sweden)

    H Ghavidel

    2017-08-01

    Full Text Available In this paper, a practical simulation method for optimizing of x-ray reflection of nano-multilayer mirrors in three different edge energies: Cr-Kα, Co-Kα, and Ti-Kα is discussed in order to obtain the most reflection based on quarter-wave thickness method (QW. In this method, the reflected x-ray will have a constructive interference, and a peak, called Brag peak, will appear in reflection curve when the tickness of the layer is an odd multiple of the quarter-wave thickness. The quarter-wave thickness is dependent to on the angle and energy of the entrance photon beam. In the mentioned edge energies, for different nano-multilayer mirrors, and for incident angle ranges from  0.5 to 8 degrees, the QW thikness for each layer is estimated and the Brag peak reflected intensity was simulated for each angle by the IMD computational code. The details shows that the optimal reflection is accessible by plotting Brag peak reflection curves based on the related angles.

  20. A NuSTAR observation of the reflection spectrum of the low-mass X-ray binary 4U 1728-34

    DEFF Research Database (Denmark)

    Sleator, Clio C.; Tomsick, John A.; King, Ashley L.

    2016-01-01

    We report on a simultaneous NuSTAR and Swift observation of the neutron star low-mass X-ray binary 4U 1728-34. We identified and removed four Type I X-ray bursts during the observation in order to study the persistent emission. The continuum spectrum is hard and described well by a blackbody with k......T = 1.5 keV and a cutoff power law with Γ = 1.5, and a cutoff temperature of 25 keV. Residuals between 6 and 8 keV provide strong evidence of a broad Fe Kα line. By modeling the spectrum with a relativistically blurred reflection model, we find an upper limit for the inner disk radius of Rin≤2RISCO...

  1. Monitoring environmental pollution of trace elements in tree-rings by synchrotron radiation total reflection X-ray fluorescence analysis (SR-TXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo]. E-mail: Silvana@fec.unicamp.br; Vives, Ana Elisa S. de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Brienza, Sandra Maria B. [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil) Faculdade de Ciencias Matematicas, da Natureza e de Tecnologia da Informacao]. E-mail: sbrienza@unimep.br; Medeiros, Jean Gabriel S.; Tomazello Filho, Mario [Sao Paulo Univ., Piracicaba, SP (Brazil). Escola Superior de Agricultura Luiz de Queiroz]. E-mail: jeangm@esalq.usp.br; mtomazel@esalq.usp.br; Zucchi, Orgheda L.A.D. [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas]. E-mail: olzucchi@fcfrp.usp.br; Nascimento Filho, Virgilio F. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear]. E-mail: virgilio@cena.usp.br

    2005-07-01

    This paper aims to study the environmental pollution in the tree development, as a manner to evaluate its use as bioindicator in urban and country sides. The sample collecting was carry out in Piracicaba city, Sao Paulo State, that presents high level of environmental contamination of the water, soil and air, due industrial activities, vehicles combustion, sugar-cane leaves burning in the harvesting, etc. It was selected the Caesalpinia peltophoroides ('Sibipiruna') specie because its very used in urban arborization. It was employed the analytical technique named total reflection X-ray fluorescence (TXRF) to identify and quantify the elements and metals of nutritional and toxicological importance in the wood samples. The analysis was done in the Brazilian Synchrotron Light Laboratory, using a white beam for excitation and a Si(Li) detector for characteristic X-ray detection. It was quantified the P, K, Ca, Ti, Fe, Sr, Ba e Pb elements. (author)

  2. Fine structures in refractive index of sapphire at the L(II,III) absorption edge of aluminum determined by soft x-ray resonant reflectivity.

    Science.gov (United States)

    Das, Arijeet; Gupta, Rajkumar K; Modi, Mohammed H; Mukherjee, Chandrachur; Rai, Sanjay K; Bose, Aniruddha; Ganguli, Tapas; Joshi, Satish C; Lodha, Gyan S; Deb, Sudip K

    2012-10-20

    The optical constants of sapphire crystal (α-Al(2)O(3)) and amorphous Al(2)O(3) in the soft x-ray region (67-85 eV) around the aluminum LII,III absorption edge (73.1 eV) are determined by angle-dependent x-ray reflectivity. The differences between the optical constant values of both the samples are discussed. The fine structures obtained in the absorption of crystalline sapphire are explained. An absorption feature at 70.2 eV is observed for the first time for crystalline alumina. Both datasets are compared to the tabulated values of Henke et al. [At. Data Nucl. Data Tables 54, 181 (1993)], Weaver et al. [Physik Daten, Physics Data: Optical Properties of Metals (Fach-information zentrum, 1981), Vols. 18-1 and 18-2], and [Handbook of Optical Constants of Solids II (Academic, 1991)].

  3. Adding diffuse reflectance infrared Fourier transform spectroscopy capability to extended x-ray-absorption fine structure in a new cell to study solid catalysts in combination with a modulation approach

    Science.gov (United States)

    Chiarello, Gian Luca; Nachtegaal, Maarten; Marchionni, Valentina; Quaroni, Luca; Ferri, Davide

    2014-07-01

    We describe a novel cell used to combine in situ transmission X-ray absorption spectroscopy (XAS) with diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) in a single experiment. The novelty of the cell design compared to current examples is that both radiations are passed through an X-ray and IR transparent window in direct contact with the sample. This innovative geometry also offers a wide surface for IR collection. In order to avoid interference from the crystalline IR transparent materials (e.g., CaF2, MgF2, diamond) a 500 μm carbon filled hole is laser drilled in the center of a CaF2 window. The cell is designed to represent a plug flow reactor, has reduced dead volume in order to allow for fast exchange of gases and is therefore suitable for experiments under fast transients, e.g., according to the concentration modulation approach. High quality time-resolved XAS and DRIFTS data of a 2 wt.% Pt/Al2O3 catalyst are obtained in concentration modulation experiments where CO (or H2) pulses are alternated to O2 pulses at 150 °C. We show that additional information can be obtained on the Pt redox dynamic under working conditions thanks to the improved sensitivity given by the modulation approach followed by Phase Sensitive Detection (PSD) analysis. It is anticipated that the design of the novel cell is likely suitable for a number of other in situ spectroscopic and diffraction methods.

  4. Nucleation and growth of gold nanoparticles studied via in situ small angle X-ray scattering at millisecond time resolution.

    Science.gov (United States)

    Polte, Jörg; Erler, Robert; Thünemann, Andreas F; Sokolov, Sergey; Ahner, T Torsten; Rademann, Klaus; Emmerling, Franziska; Kraehnert, Ralph

    2010-02-23

    Gold nanoparticles (AuNP) were prepared by the homogeneous mixing of continuous flows of an aqueous tetrachloroauric acid solution and a sodium borohydride solution applying a microstructured static mixer. The online characterization and screening of this fast process ( approximately 2 s) was enabled by coupling a micromixer operating in continuous-flow mode with a conventional in-house small angle X-ray scattering (SAXS) setup. This online characterization technique enables the time-resolved investigation of the growth process of the nanoparticles from an average radius of ca. 0.8 nm to about 2 nm. To the best of our knowledge, this is the first demonstration of a continuous-flow SAXS setup for time-resolved studies of nanoparticle formation mechanisms that does not require the use of synchrotron facilities. In combination with X-ray absorption near edge structure microscopy, scanning electron microscopy, and UV-vis spectroscopy the obtained data allow the deduction of a two-step mechanism of gold nanoparticle formation. The first step is a rapid conversion of the ionic gold precursor into metallic gold nuclei, followed by particle growth via coalescence of smaller entities. Consequently it could be shown that the studied synthesis serves as a model system for growth driven only by coalescence processes.

  5. The condensation of the corona for the correlation between the hard X-ray photon index Γ and the reflection scaling factor ℜ in active galactic nuclei

    Science.gov (United States)

    Qiao, Erlin; Liu, B. F.

    2017-05-01

    Observationally, it is found that there is a strong correlation between the hard X-ray photon index Γ and the Compton reflection scaling factor ℜ in active galactic nuclei. In this paper, we propose that the Γ - ℜ correlation can be explained within the framework of the condensation of the hot corona on to the cold accretion disc around a supermassive black hole. In the model, it is presumed that, initially, a vertically extended hot gas (corona) is supplied to the central supermassive black hole by capturing the interstellar medium and stellar wind. In this scenario, when the initial mass accretion rate \\dot{M}/ \\dot{M}_Edd ≳ 0.01, at a critical radius rd, part of the hot gas begins to condense on to the equatorial disc plane of the black hole, forming an inner cold accretion disc. Then, the matter is accreted in the form of a disc-corona structure extending down to the innermost stable circular orbits of the black hole. The size of the inner disc is determined by the initial mass accretion rate. With the increase of the initial mass accretion rate, the size of the inner disc increases, which results in both the increase of the Compton reflection scaling factor ℜ and the increase of the hard X-ray photon index Γ. By comparing with a sample of Seyfert galaxies with well-fitted X-ray spectra, it is found that our model can roughly explain the observations. Finally, we discuss the possibility of applying our model to high-mass X-ray binaries, which are believed to be fuelled by hot winds from the companion stars.

  6. New developments in laser-heated diamond anvil cell with in situ synchrotron x-ray diffraction at High Pressure Collaborative Access Team.

    Science.gov (United States)

    Meng, Yue; Hrubiak, Rostislav; Rod, Eric; Boehler, Reinhard; Shen, Guoyin

    2015-07-01

    An overview of the in situ laser heating system at the High Pressure Collaborative Access Team, with emphasis on newly developed capabilities, is presented. Since its establishment at the beamline 16-ID-B a decade ago, laser-heated diamond anvil cell coupled with in situ synchrotron x-ray diffraction has been widely used for studying the structural properties of materials under simultaneous high pressure and high temperature conditions. Recent developments in both continuous-wave and modulated heating techniques have been focusing on resolving technical issues of the most challenging research areas. The new capabilities have demonstrated clear benefits and provide new opportunities in research areas including high-pressure melting, pressure-temperature-volume equations of state, chemical reaction, and time resolved studies.

  7. Competitive adsorption of strontium and fulvic acid at the muscovite-solution interface observed with resonant anomalous X-ray reflectivity

    Science.gov (United States)

    Lee, Sang Soo; Park, Changyong; Fenter, Paul; Sturchio, Neil C.; Nagy, Kathryn L.

    2010-03-01

    Molecular-scale distributions of Sr 2+ and fulvic acid (FA) adsorbed on the muscovite (0 0 1) surface were investigated using in situ specular X-ray reflectivity (XR) and resonant anomalous X-ray reflectivity (RAXR). The total amount of Sr 2+ adsorbed from a 1 × 10 -2 mol/kg SrCl 2 and 100 mg/kg Elliott Soil Fulvic Acid II (ESFA II) solution at pH 5.5 compensated 81 ± 5% of the muscovite surface charge, less than previously measured (118 ± 5%) in an ESFA II-free solution with the same Sr concentration and pH. Inner-sphere (IS) and outer-sphere (OS) Sr 2+ constituted 87% of the total adsorbed species in IS:OS proportions of 19:81 compared to 42:58 in the solution without FA, suggesting that adsorbed FA competes with the IS Sr 2+ for surface sites. The coverage of both IS and OS Sr 2+ decreased even more in a pH 3.5 solution containing the same concentration of FA and 0.5 × 10 -2 mol/kg Sr(NO 3) 2, whereas a significant amount of Sr 2+ accumulated farther from the surface in the FA layer. The amount of Sr 2+ incorporated in the ˜10 Å thick FA layer decreased by 79% with decreasing FA concentration (100 → 1 mg/kg) and increasing Sr 2+ concentration (0.5 × 10 -2 → 1 × 10 -2 mol/kg) and pH (3.5 → 3.6). These results indicate not only that adsorbed FA molecules (and perhaps also H 3O +) displace Sr 2+ near the muscovite surface, but also that the sorbed FA film provides binding sites for additional Sr 2+ away from the surface. When a muscovite crystal pre-coated with FA after reaction in a 100 mg/kg ESFA II solution for 50 h was subsequently reacted with a 0.5 × 10 -2 mol/kg Sr(NO 3) 2 and 100 mg/kg ESFA II solution at pH 3.7, a significant fraction of Sr 2+ was distributed in the outer part of the FA film similar to that observed on fresh muscovite reacted at pH 3.5 with a pre-mixed Sr-FA solution at the same concentrations. However, this Sr 2+ sorbed in the pre-adsorbed organic film was more widely distributed and had a lower coverage, suggesting that

  8. Grazing incidence diffraction and X-ray reflectivity studies of the interactions of inorganic mercury salts with membrane lipids in Langmuir monolayers at the air/water interface.

    Science.gov (United States)

    Broniatowski, Marcin; Flasiński, Michał; Dynarowicz-Łatka, Patrycja; Majewski, Jarosław

    2010-07-29

    The interactions of mercury ions with the membrane phospholipids are considered to be of great importance regarding the toxicity of this metal in living organisms. To obtain deeper insight into this problem, we performed systematic studies applying the Langmuir technique complemented with synchrotron X-ray scattering methods (grazing incidence X-ray diffraction (GIXD) and X-ray reflectivity (XR)). We focused our attention on the interactions of inorganic mercury salts dissolved in the aqueous subphase with lipid monolayers, formed by selected membrane phospholipids, namely, dipalmitoylphosphatidylglicerol (DPPG), dipalmitoylphosphatidylcholine (DPPC), 1-octadecyl 2-sn-phosphatidylcholine (lyso-PC), and sphingomyelin (SM). Two different inorganic mercury salts, one of a hydracid, HgCl(2), and the other of an oxacid, Hg(NO(3))(2), have been investigated. Our results proved that the elastic properties of phospholipid monolayers are a key factor regarding the interactions with mercury ions. Significant differences in mercury ions complexation are observed with double-chain phospholipids (such as DPPG and DPPC) forming fluid layers of low compressibility and phospholipids forming more compressible films (like SM and lyso-PC). Namely, important changes in the monolayer characteristic were observed only for the latter kind of lipids. This is an important finding taking into account the accumulation of mercury in the central nervous system and its neurotoxic effects. SM is one of the most abundant lipids in neurons shells and therefore can be considered as a target lipid complexing mercury ions.

  9. In situ probing calcium carbonate formation by combining fast controlled precipitation method and small-angle X-ray scattering.

    Science.gov (United States)

    Chao, Yanjia; Horner, Olivier; Vallée, Philippe; Meneau, Florian; Alos-Ramos, Olga; Hui, Franck; Turmine, Mireille; Perrot, Hubert; Lédion, Jean

    2014-04-01

    The initial stage of calcium carbonate nucleation and growth, found usually in "natural" precipitation conditions, is still not well understood. The calcium carbonate formation for moderate supersaturation level could be achieved by an original method called the fast controlled precipitation (FCP) method. FCP was coupled with SAXS (small-angle X-ray scattering) measurements to get insight into the nucleation and growth mechanisms of calcium carbonate particles in Ca(HCO3)2 aqueous solutions. Two size distributions of particles were observed. The particle size evolutions of these two distributions were obtained by analyzing the SAXS data. A nice agreement was obtained between the total volume fractions of CaCO3 obtained by SAXS analysis and by pH-resistivity curve modeling (from FCP tests).

  10. Native target chemistry during reactive dc magnetron sputtering studied by ex-situ x-ray photoelectron spectroscopy

    Science.gov (United States)

    Greczynski, G.; Mráz, S.; Schneider, J. M.; Hultman, L.

    2017-07-01

    We report x-ray photoelectron spectroscopy (XPS) analysis of native Ti target surface chemistry during magnetron sputtering in an Ar/N2 atmosphere. To avoid air exposure, the target is capped immediately after sputtering with a few-nm-thick Al overlayers; hence, information about the chemical state of target elements as a function of N2 partial pressure pN2 is preserved. Contrary to previous reports, which assume stoichiometric TiN formation, we present direct evidence, based on core-level XPS spectra and TRIDYN simulations, that the target surface is covered by TiNx with x varying in a wide range, from 0.27 to 1.18, depending on pN2. This has far-reaching consequences both for modelling of the reactive sputtering process and for everyday thin film growth where detailed knowledge of the target state is crucial.

  11. Elemental analysis of human amniotic fluid and placenta by total-reflection X-ray fluorescence and energy-dispersive X-ray fluorescence: child weight and maternal age dependence

    Science.gov (United States)

    Carvalho, M. L.; Custódio, P. J.; Reus, U.; Prange, A.

    2001-11-01

    This work is an attempt to evaluate the possible influence of the mother's age in trace element concentrations in human amniotic fluid and placenta and whether these concentrations are correlated to the weight of the newborn infants. Total-reflection X-ray fluorescence (TXRF) was used to analyze 16 amniotic fluid samples, and the placenta samples were analyzed by energy dispersive X-ray fluorescence (EDXRF). The whole samples were collected during delivery from healthy mothers and healthy infants and full-term pregnancies. According to the age of the mother, three different groups were considered: 20-25, 25-30 and 30-40 years old. Only two mothers were aged more than 35 years. The weight of the infants ranged from 2.56 to 4.05 kg and three groups were also considered: 2.5-3, 3-3.5 and 3.5-4 kg. The organic matrix of the amniotic fluid samples was removed by treatment with HNO 3 followed by oxygen plasma ashing. Yttrium was used as the internal standard for TXRF analysis. Placenta samples were lyophilized and analyzed by EDXRF without any chemical treatment. Very low levels of Ni and Sr were found in the amniotic fluid samples, and were independent of the age of the mother and weight of the child. Cr, Mn, Se and Pb were at the level of the detection limit. Zn, considered one of the key elements in neonatal health, was not significantly different in the samples analyzed; however, it was weakly related to birth weigh. The concentrations obtained ranged from 0.11 to 0.92 mg/l and 30 to 65 μg/g in amniotic fluid and placenta, respectively. The only two elements which seemed to be significantly correlated with mother's age and newborn weight were Ca and Fe for both types of sample: Ca levels were increased in heavier children and older mothers; however, Fe increased with increasing maternal age, but decreased for heavier babies. The same conclusions were obtained for placenta and amniotic fluid samples. Cu is closely associated with Fe in its function in the organism

  12. Ammonothermal Synthesis of Earth-Abundant Nitride Semiconductors ZnSiN2 and ZnGeN2 and Dissolution Monitoring by In Situ X-ray Imaging.

    Science.gov (United States)

    Häusler, Jonas; Schimmel, Saskia; Wellmann, Peter; Schnick, Wolfgang

    2017-09-07

    In this contribution, first synthesis of semiconducting ZnSiN2 and ZnGeN2 from solution is reported with supercritical ammonia as solvent and KNH2 as ammonobasic mineralizer. The reactions were conducted in custom-built high-pressure autoclaves made of nickel-based superalloy. The nitrides were characterized by powder X-ray diffraction and their crystal structures were refined by the Rietveld method. ZnSiN2 (a=5.24637(4), b=6.28025(5), c=5.02228(4) Å, Z=4, Rwp =0.0556) and isotypic ZnGeN2 (a=5.46677(10), b=6.44640(12), c=5.19080(10) Å, Z=4, Rwp =0.0494) crystallize in the orthorhombic space group Pna21 (no. 33). The morphology and elemental composition of the nitrides were examined by electron microscopy and energy-dispersive X-ray spectroscopy (EDX). Well-defined single crystals with a diameter up to 7 μm were grown by ammonothermal synthesis at temperatures between 870 and 1070 K and pressures up to 230 MPa. Optical properties have been analyzed with diffuse reflectance measurements. The band gaps of ZnSiN2 and ZnGeN2 were determined to be 3.7 and 3.2 eV at room temperature, respectively. In situ X-ray measurements were performed to exemplarily investigate the crystallization mechanism of ZnGeN2 . Dissolution in ammonobasic supercritical ammonia between 570 and 670 K was observed which is quite promising for the crystal growth of ternary nitrides under ammonothermal conditions. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Support Effects in Catalysis Studied by in-situ Sum Frequency Generation Vibrational Spectroscopy and in-situ X-Ray Spectroscopies

    Science.gov (United States)

    Kennedy, Griffin John

    which the molecule binds via the aldehyde group. These sites are believed to be the active sites for alcohol production. In the case of Co3O 4 ambient pressure x-ray photoelectron spectroscopy and x-ray absorption spectroscopy reveal a reduction of the oxide surface under reaction conditions indicating the adsorption sites on the oxide exist on a reduced surface, additional evidence for the site being an O-vacancy. Lastly a before undiscovered example of encapsulation of a metal particle by an oxide support is observed for the Pt/Co3O4 system by ambient pressure x-ray photoelectron spectroscopy. Under mild conditions an encapsulated state is reached in which the oxide covers the Pt surface, yet does not inhibit reactivity. In fact the total activity of the catalyst increases dramatically and a change in product selectivity was observed. (Abstract shortened by ProQuest.).

  14. 4D in situ visualization of electrode morphology changes during accelerated degradation in fuel cells by X-ray computed tomography

    Science.gov (United States)

    White, Robin T.; Wu, Alex; Najm, Marina; Orfino, Francesco P.; Dutta, Monica; Kjeang, Erik

    2017-05-01

    A four-dimensional visualization approach, featuring three dimensions in space and one dimension in time, is proposed to study local electrode degradation effects during voltage cycling in fuel cells. Non-invasive in situ micro X-ray computed tomography (XCT) with a custom fuel cell fixture is utilized to track the same cathode catalyst layer domain throughout various degradation times from beginning-of-life (BOL) to end-of-life (EOL). With this unique approach, new information regarding damage features and trends are revealed, including crack propagation and catalyst layer thinning being quantified by means of image processing and analysis methods. Degradation heterogeneities as a result of local environmental variations under land and channel are also explored, with a higher structural degradation rate under channels being observed. Density and compositional changes resulting from carbon corrosion and catalyst layer collapse and thinning are observed by changes in relative X-ray attenuation from BOL to EOL, which also indicate possible vulnerable regions where crack initiation and propagation may occur. Electrochemical diagnostics and morphological features observed by micro-XCT are correlated by additionally collecting effective catalyst surface area, double layer capacitance, and polarization curves prior to imaging at various stages of degradation.

  15. In situ X-ray absorption fine structure studies of a manganese dioxide electrode in a rechargeable MnO{sub 2}/Zn alkaline battery environment

    Energy Technology Data Exchange (ETDEWEB)

    Mo, Y.; Hu, Y.; Bae, I.T.; Miller, B.; Scherson, D.A. [Case Western Reserve Univ., Cleveland, OH (United States). Dept. of Chemistry; Antonio, M.R. [Argonne National Lab., IL (United States). Chemistry Div.

    1996-12-31

    Electronic and structural aspects of a MnO{sub 2} electrode in a rechargeable MnO{sub 2}/Zn battery environment have been investigated by in situ Mn K-edge X-ray absorption fine structure (XAFS). The relative amplitudes of the three major Fourier transform shells of the EXAFS (extended XAFS) function of the rechargeable MnO{sub 2} electrode in the undischarged state were found to be similar to those found for ramsdellite, a MnO{sub 2} polymorph with substantial corner-sharing linkages among the basic MnO{sub 6} octahedral units. The analyses of the background-subtracted pre-edge peaks and absorption edge regions for the nominally 1-e{sup {minus}} discharged electrode were consistent with Mn{sup 3+} as being the predominant constituent species, rather than a mixture of Mn{sup 4+} and Mn{sup 2+} sites. Furthermore, careful inspection of both the XANES (X-ray absorption near edge structure) and EXAFS indicated that the full recharge of MnO, which had been previously discharged either by a 1- or 2-equivalent corner-sharing linkages compared to the original undischarged MnO{sub 2}.

  16. Temperature effect of elastic anisotropy and internal strain development in advanced nanostructured alloys: An in-situ synchrotron X-ray investigation

    Energy Technology Data Exchange (ETDEWEB)

    Gan, Yingye; Mo, Kun; Yun, Di; Hoelzer, David T.; Miao, Yinbin; Liu, Xiang; Lan, Kuan-Che; Park, Jun-Sang; Almer, Jonathan; Chen, Tianyi; Zhao, Huijuan

    2017-04-01

    Nanostructured ferritic alloys (NFAs) are a promising structural material for advanced nuclear systems due to their exceptional radiation tolerance and high-temperature mechanical properties. Their remarkable properties result from the ultrafine ultrahigh density Y-Ti-O nanoclusters dispersed within the ferritic matrix. In this work, we performed in-situ synchrotron X-ray diffraction tests to study the tensile deformation process of the three types of NFAs: 9YWTV, 14YWT-sm13, and 14YWT-sm170 at both room temperature and elevated temperatures. A technique was developed, combining Kroner’s model and X-ray measurement, to determine the intrinsic monocrystal elastic-stiffness constants, and polycrystal Young’s modulus and Poisson’s ratio of the NFAs. Temperature dependence of elastic anisotropy was observed in the NFAs. An analysis of intergranular strain and strengthening factors determined that 14YWT-sm13 had a higher resistance to temperature softening compared to 9YWTV, attributed to the more effective nanoparticle strengthening during high-temperature mechanical loading.

  17. In situ observation of high-pressure phase transition in silicon carbide under shock loading using ultrafast x-ray diffraction

    Science.gov (United States)

    Tracy, Sally June

    2017-06-01

    SiC is an important high-strength ceramic material used for a range of technological applications, including lightweight impact shielding and abrasives. SiC is also relevant to geology and planetary science. It may be a host of reduced carbon in the Earth's interior and also occurs in meteorites and impact sites. SiC has also been put forward as a possible major constituent in the proposed class of extra-solar planets known as carbon planets. Previous studies have used wave profile measurements to identify a phase transition under shock loading near 1 Mbar, but lattice-level structural information was not obtained. Here we present the behavior of silicon carbide under shock loading as investigated through a series of time-resolved pump-probe x-ray diffraction measurements up to 200 GPa. Our experiments were conducted at the Materials in Extreme Conditions beamline of the Linac Coherent Light Source. In situ x-ray diffraction data on shock-compressed SiC was collected using a free electron laser source combined with a pulsed high-energy laser. These measurements allow for the determination of time-dependent atomic arrangements, demonstrating that the wurtzite phase of SiC transforms directly to the B1 structure. Our measurements also reveal details of the material texture evolution under shock loading and release.

  18. NuSTAR and Swift joint view of neutron star X-ray binary 4U 1728-34: disc reflection in the island and lower banana states

    Science.gov (United States)

    Mondal, Aditya S.; Pahari, Mayukh; Dewangan, G. C.; Misra, R.; Raychaudhuri, B.

    2017-04-01

    We analyse two simultaneous NuSTAR and Swift data of the Atoll-type neutron star (NS) X-ray binary 4U 1728-34 observed on 2013 October 1 and 3. We infer that the first and the second observations belong to the island state and the lower banana state, respectively. During island state, four type-I X-ray bursts are observed within 60 ks exposure. From the time-resolved spectral analysis of each burst with NuSTAR, the blackbody temperature kTbb are found to vary between 1.3 and 3.0 keV, while the blackbody normalizations (km/10 kpc)2 vary in the range 20-200, which translates to blackbody radii of 3.5-7.4 km for an assumed distance of 5 kpc. The persistent, joint energy spectra from Swift and NuSTAR for both observations in the energy band 1-79 keV are well described with thermal emission from the NS surface (kTbb ≃ 1-2.5 keV), Comptonized emission of thermal seed photons from the hot boundary layer/corona and the strong reflection component from the accretion disc. We detect a broad iron line in the 5-8 keV band and reflection hump in the 15-30 keV band modelled by the relxill reflection model. Joint spectral fitting constrains the inclination angle of the binary system and inner disc radius to be 22°-40° and (2.0-4.3) × RISCO, respectively. We estimate the magnetic field to be (1.8-6.5) × 108 G. The X-ray luminosity of the source during the island and lower banana states are found to be LX = 1.1 and 1.6 × 1037 erg s-1, respectively, which correspond to ˜6 per cent and ˜9 per cent of the Eddington luminosity.

  19. X-ray reflectivity studies of cPLA2{alpha}-C2 domains adsorbed onto Langmuir monolayers of SOPC.

    Science.gov (United States)

    Málková, Sárka; Long, Fei; Stahelin, Robert V; Pingali, Sai V; Murray, Diana; Cho, Wonhwa; Schlossman, Mark L

    2005-09-01

    X-ray reflectivity is used to study the interaction of C2 domains of cytosolic phospholipase A(2) (cPLA(2)alpha-C2) with a Langmuir monolayer of 1-stearoyl-2-oleoyl-sn-glycero-3-phosphocholine (SOPC) supported on a buffered aqueous solution containing Ca(2+). The reflectivity is analyzed in terms of the known crystallographic structure of cPLA(2)alpha-C2 domains and a slab model representing the lipid layer to yield an electron density profile of the lipid layer and bound C2 domains. This new method of analysis determines the angular orientation and penetration depth of the cPLA(2)alpha-C2 domains bound to the SOPC monolayer, information not available from the standard slab model analysis of x-ray reflectivity. The best-fit orientation places the protein-bound Ca(2+) ions within 1 A of the lipid phosphate group (with an accuracy of +/-3 A). Hydrophobic residues of the calcium-binding loops CBL1 and CBL3 penetrate deepest into the lipid layer, with a 2 A penetration into the tailgroup region. X-ray measurements with and without the C2 domain indicate that there is a loss of electrons in the headgroup region of the lipid monolayer upon binding of the domains. We suggest that this is due to a loss of water molecules bound to the headgroup. Control experiments with a non-calcium buffer and with domain mutants confirm that the cPLA(2)alpha-C2 binding to the SOPC monolayer is Ca(2+)-dependent and that the hydrophobic residues in the calcium-binding loops are critical for membrane binding. These results indicate that an entropic component (due to water loss) as well as electrostatic and hydrophobic interactions contributes to the binding mechanism.

  20. X-Ray Reflectivity Studies of cPLA2α-C2 Domains Adsorbed onto Langmuir Monolayers of SOPC

    Science.gov (United States)

    Málková, Šárka; Long, Fei; Stahelin, Robert V.; Pingali, Sai V.; Murray, Diana; Cho, Wonhwa; Schlossman, Mark L.

    2005-01-01

    X-ray reflectivity is used to study the interaction of C2 domains of cytosolic phospholipase A2 (cPLA2α-C2) with a Langmuir monolayer of 1-stearoyl-2-oleoyl-sn-glycero-3-phosphocholine (SOPC) supported on a buffered aqueous solution containing Ca2+. The reflectivity is analyzed in terms of the known crystallographic structure of cPLA2α-C2 domains and a slab model representing the lipid layer to yield an electron density profile of the lipid layer and bound C2 domains. This new method of analysis determines the angular orientation and penetration depth of the cPLA2α-C2 domains bound to the SOPC monolayer, information not available from the standard slab model analysis of x-ray reflectivity. The best-fit orientation places the protein-bound Ca2+ ions within 1 Å of the lipid phosphate group (with an accuracy of ±3 Å). Hydrophobic residues of the calcium-binding loops CBL1 and CBL3 penetrate deepest into the lipid layer, with a 2 Å penetration into the tailgroup region. X-ray measurements with and without the C2 domain indicate that there is a loss of electrons in the headgroup region of the lipid monolayer upon binding of the domains. We suggest that this is due to a loss of water molecules bound to the headgroup. Control experiments with a non-calcium buffer and with domain mutants confirm that the cPLA2α-C2 binding to the SOPC monolayer is Ca2+-dependent and that the hydrophobic residues in the calcium-binding loops are critical for membrane binding. These results indicate that an entropic component (due to water loss) as well as electrostatic and hydrophobic interactions contributes to the binding mechanism. PMID:15994899

  1. 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...

  2. Fullerene films and fullerene-dodecylamine adduct monolayers at air-water interfaces studied by neutron and x-ray reflection

    DEFF Research Database (Denmark)

    Wang, J.Y.; Vaknin, D.; Uphaus, R.A.

    1994-01-01

    Neutron and X-ray reflection measurements and surface pressure isotherms of spread films of the fullerene-dodecylamine adduct C60-[NH2(CH2)11CH3]x all indicate that this material may form monomolecular layers on water surfaces. The reflection data sets (neutron on both H2O and D2O) can be accounted...... stratum and the remainder alkyl tails are located close to both the air and the water interfaces. The alkyl moieties close to the aqueous substrate are hydrated. The reflection experiments and the isotherms suggest that on average 8 +/- 3 dodecylamine molecules are present per fullerene, consistent within...... error, with elemental analysis 5 +/- 2. By contrast, neutron reflection and surface pressure vs. area data of spread films of C60 fullerenes on aqueous surfaces indicate the formation of inhomogeneous multilayer films with a thickness and a surface roughness exceeding the molecular size...

  3. Chest X-Ray

    Medline Plus

    Full Text Available ... the most commonly performed x-ray exams and use a very small dose of ionizing radiation to ... to your health. While a chest x-ray use a tiny dose of ionizing radiation, the benefit ...

  4. Nanometer x-ray lithography

    Science.gov (United States)

    Hartley, Frank T.; Khan Malek, Chantal G.

    1999-10-01

    New developments for x-ray nanomachining include pattern transfer onto non-planar surfaces coated with electrodeposited resists using synchrotron radiation x-rays through extremely high-resolution mask made by chemically assisted focused ion beam lithography. Standard UV photolithographic processes cannot maintain sub-micron definitions over large variation in feature topography. The ability of x-ray printing to pattern thin or thick layers of photoresist with high resolution on non-planar surfaces of large and complex topographies with limited diffraction and scattering effects and no substrate reflection is known and can be exploited for patterning microsystems with non-planar 3D geometries as well as multisided and multilayered substrates. Thin conformal coatings of electro-deposited positive and negative tone photoresist have been shown to be x-ray sensitive and accommodate sub-micro pattern transfer over surface of extreme topographical variations. Chemically assisted focused ion beam selective anisotropic erosion was used to fabricate x-ray masks directly. Masks with feature sizes less than 20 nm through 7 microns of gold were made on bulk silicon substrates and x-ray mask membranes. The technique is also applicable to other high density materials. Such masks enable the primary and secondary patterning and/or 3D machining of Nano-Electro-Mechanical Systems over large depths or complex relief and the patterning of large surface areas with sub-optically dimensioned features.

  5. Magnetic confinement, Alfven wave reflection, and the origins of X-ray and mass-loss 'dividing lines' for late-type giants and supergiants

    Science.gov (United States)

    Rosner, R.; An, C.-H.; Musielak, Z. E.; Moore, R. L.; Suess, S. T.

    1991-01-01

    A simple qualitative model for the origin of the coronal and mass-loss dividing lines separating late-type giants and supergiants with and without hot, X-ray-emitting corona, and with and without significant mass loss is discussed. The basic physical effects considered are the necessity of magnetic confinement for hot coronal material on the surface of such stars and the large reflection efficiency for Alfven waves in cool exponential atmospheres. The model assumes that the magnetic field geometry of these stars changes across the observed 'dividing lines' from being mostly closed on the high effective temperature side to being mostly open on the low effective temperature side.

  6. A Versatile System for High-Throughput In Situ X-ray Screening and Data Collection of Soluble and Membrane-Protein Crystals

    Energy Technology Data Exchange (ETDEWEB)

    Broecker, Jana; Klingel, Viviane; Ou, Wei-Lin; Balo, Aidin R.; Kissick, David J.; Ogata, Craig M.; Kuo, Anling; Ernst, Oliver P.

    2016-10-12

    In recent years, in situ data collection has been a major focus of progress in protein crystallography. Here, we introduce the Mylar in situ method using Mylar-based sandwich plates that are inexpensive, easy to make and handle, and show significantly less background scattering than other setups. A variety of cognate holders for patches of Mylar in situ sandwich films corresponding to one or more wells makes the method robust and versatile, allows for storage and shipping of entire wells, and enables automated crystal imaging, screening, and goniometerbased X-ray diffraction data-collection at room temperature and under cryogenic conditions for soluble and membrane-protein crystals grown in or transferred to these plates. We validated the Mylar in situ method using crystals of the water-soluble proteins hen egg-white lysozyme and sperm whale myoglobin as well as the 7-transmembrane protein bacteriorhodopsin from Haloquadratum walsbyi. In conjunction with current developments at synchrotrons, this approach promises high-resolution structural studies of membrane proteins to become faster and more routine.

  7. In-Situ Coherent Grazing Incidence Small Angle X-ray Scattering (Co-GISAXS) Studies of Surface Fluctuations of Sputter Deposited WSi2 using X-ray Photon Correlation Spectroscopy (XPCS)

    Science.gov (United States)

    Dahal, Som; Ulbrandt, Jeffrey; Headrick, Randall; Demasi, Alexander; Ludwig, Karl

    2014-03-01

    We performed Coherent Grazing Incidence Small Angle X-ray Scattering (Co-GISAXS) studies of surface dynamics during magnetron sputtering deposited WSi2 amorphous thin films. The local dynamics of surface fluctuations was studied by X-ray Photon Correlation Spectroscopy (XPCS) in the late time regime where the static GIXAXS stops evolving. Our studies reveal that the correlation time of the sputtered species varies as a power law with the in-plane momentum transfer. The experimentally obtained results are compared with predictions from continuum models of surface growth.

  8. Dynamics of mineral crystallization from precipitated slab-derived fluid phase: first in situ synchrotron X-ray measurements

    Science.gov (United States)

    Malaspina, Nadia; Alvaro, Matteo; Campione, Marcello; Wilhelm, Heribert; Nestola, Fabrizio

    2015-03-01

    Remnants of the fluid phase at ultrahigh pressure (UHP) in subduction environments may be preserved as primary multiphase inclusions in UHP minerals. The mode of crystallization of daughter minerals during precipitation within the inclusion and/or the mechanism of interaction between the fluid at supercritical conditions and the host mineral are still poorly understood from a crystallographic point of view. A case study is represented by garnet-orthopyroxenites from the Maowu Ultramafic Complex (China) deriving from harzburgite precursors metasomatized at ~4 GPa, 750 °C by a silica- and incompatible trace element-rich fluid phase. This metasomatism produced poikilitic orthopyroxene and inclusion-rich garnet porphyroblasts. Solid multiphase primary inclusions in garnet display a size within a few tens of micrometres and negative crystal shapes. Infilling minerals (spinel: 10-20 vol%; amphibole, chlorite, talc, mica: 80-90 vol%) occur with constant volume proportions and derive from trapped solute-rich aqueous fluids. To constrain the possible mode of precipitation of daughter minerals, we performed for the first time a single-crystal X-ray diffraction experiment by synchrotron radiation at Diamond Light Source. In combination with electron probe microanalyses, this measurement allowed the unique identification of each mineral phase and reciprocal orientations. We demonstrated the epitaxial relationship between spinel and garnet and between some hydrous minerals. Such information is discussed in relation to the physico-chemical aspects of nucleation and growth, shedding light on the mode of mineral crystallization from a fluid phase trapped at supercritical conditions.

  9. Ionic multilayers at the free surface of an ionic liquid, trioctylmethylammonium bis(nonafluorobutanesulfonyl)amide, probed by x-ray reflectivity measurements.

    Science.gov (United States)

    Nishi, Naoya; Yasui, Yukinori; Uruga, Tomoya; Tanida, Hajime; Yamada, Tasuku; Nakayama, Shun-ichi; Matsuoka, Hideki; Kakiuchi, Takashi

    2010-04-28

    The presence of ionic multilayers at the free surface of an ionic liquid, trioctylmethylammonium bis(nonafluorobutanesulfonyl)amide ([TOMA(+)][C(4)C(4)N(-)]), extending into the bulk from the surface to the depth of approximately 60 A has been probed by x-ray reflectivity measurements. The reflectivity versus momentum transfer (Q) plot shows a broad peak at Q approximately 0.4 A(-1), implying the presence of ionic layers at the [TOMA(+)][C(4)C(4)N(-)] surface. The analysis using model fittings revealed that at least four layers are formed with the interlayer distance of 16 A. TOMA(+) and C(4)C(4)N(-) are suggested not to be segregated as alternating cationic and anionic layers at the [TOMA(+)][C(4)C(4)N(-)] surface. It is likely that the detection of the ionic multilayers with x-ray reflectivity has been realized by virtue of the greater size of TOMA(+) and C(4)C(4)N(-) and the high critical temperature of [TOMA(+)][C(4)C(4)N(-)].

  10. Hand x-ray

    Science.gov (United States)

    X-ray - hand ... A hand x-ray is taken in a hospital radiology department or your health care provider's office by an ... technician. You will be asked to place your hand on the x-ray table, and keep it ...

  11. X-Ray

    Science.gov (United States)

    ... show up on chest X-rays. Breast cancer. Mammography is a special type of X-ray test used to examine breast tissue. Enlarged heart. This sign of congestive heart failure shows up clearly on X-rays. Blocked blood vessels. Injecting a contrast material that contains iodine can help highlight sections ...

  12. Study of the mechanical behavior of the hydride blister/rim structure in Zircaloy-4 using in-situ synchrotron X-ray diffraction

    Science.gov (United States)

    Lin, Jun-li; Han, Xiaochun; Heuser, Brent J.; Almer, Jonathan D.

    2016-04-01

    High-energy synchrotron X-ray diffraction was utilized to study the mechanical response of the f.c.c δ hydride phase, the intermetallic precipitation with hexagonal C14 lave phase and the α-Zr phase in the Zircaloy-4 materials with a hydride rim/blister structure near one surface of the material during in-situ uniaxial tension experiment at 200 °C. The f.c.c δ was the only hydride phase observed in the rim/blister structure. The conventional Rietveld refinement was applied to measure the macro-strain equivalent response of the three phases. Two regions were delineated in the applied load versus lattice strain measurement: a linear elastic strain region and region that exhibited load partitioning. Load partitioning was quantified by von Mises analysis. The three phases were observed to have similar elastic modulus at 200 °C.

  13. Look fast: Crystallization of conjugated molecules during solution shearing probed in-situ and in real time by X-ray scattering

    KAUST Repository

    Smilgies, Detlef Matthias

    2012-12-20

    High-speed solution shearing, in which a drop of dissolved material is spread by a coating knife onto the substrate, has emerged as a versatile, yet simple coating technique to prepare high-mobility organic thin film transistors. Solution shearing and subsequent drying and crystallization of a thin film of conjugated molecules is probed in situ using microbeam grazing incidence wide-angle X-ray scattering (μGIWAXS). We demonstrate the advantages of this approach to study solution based crystal nucleation and growth, and identify casting parameter combinations to cast highly ordered and laterally aligned molecular thin films. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Performance of a size-selected nanocluster deposition facility and in situ characterization of grown films by x-ray photoelectron spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Mondal, Shyamal; Bhattacharyya, S. R., E-mail: satyar.bhattacharyya@saha.ac.in [Saha Institute of Nuclear Physics, 1/AF Bidhan Nagar, Kolkata 700 064 (India)

    2014-06-15

    We report here on a newly installed gas aggregation type nanocluster deposition unit based on magnetron sputtering ion source with mass selection of the clusters by quadrupole mass filter. The system is ultra high vacuum compatible and is equipped with an in situ X-ray Photoelectron Spectroscopy facility, giving compositional information of the films formed by nanoclusters deposition on a substrate. Detailed descriptions and working of the components of the system are presented. For the characterization of the nanocluster source and associated mass filter for size selected clusters, the dependence of output performance as a function of aggregation length, sputter gas flow and magnetron power of the cluster source have been studied. Copper nanoclusters deposited on Silicon (100) surface and on transmission electron microscope grids are, respectively, studied with scanning electron microscopy and transmission electron microscopy for the morphology.

  15. In situ synchrotron X-ray diffraction study of deformation behavior and load transfer in a Ti{sub 2}Ni-NiTi composite

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Junsong; Hao, Shijie; Yu, Cun; Shao, Yang; Ru, Yadong; Jiang, Daqiang; Cui, Lishan, E-mail: lscui@cup.edu.cn [Department of Materials Science and Engineering, China University of Petroleum-Beijing, Changping, Beijing 102249 (China); Liu, Yinong [School of Mechanical and Chemical Engineering, The University of Western Australia, Crawley, WA 6009 (Australia); Ren, Yang [X-ray Science Division, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Huan, Yong [State Key Laboratory of Nonlinear Mechanics (LNM), Institute of Mechanics, Chinese Academy of Sciences, Beijing 100190 (China)

    2014-07-28

    The deformation behavior and load transfer of a dual-phase composite composed of martensite NiTi embedded in brittle Ti{sub 2}Ni matrices were investigated by using in situ synchrotron x-ray diffraction during compression. The composite exhibits a stage-wise deformation feature and a double-yielding phenomenon, which were caused by the interaction between Ti{sub 2}Ni and NiTi with alternative microscopic deformation mechanism. No load transfer occurs from the soft NiTi dendrites to the hard Ti{sub 2}Ni matrices during the pseudoplastic deformation (detwinning) of NiTi, which is significantly different from that previously reported in bulk metallic glasses matrices composites.

  16. In-situ X-ray diffraction reveals the degradation of crystalline CH3NH3PbI3 by water-molecule collisions at room temperature

    Science.gov (United States)

    Hada, Masaki; Hasegawa, Yoichi; Nagaoka, Ryota; Miyake, Tomoya; Abdullaev, Ulugbek; Ota, Hiromi; Nishikawa, Takeshi; Yamashita, Yoshifumi; Hayashi, Yasuhiko

    2018-02-01

    We have developed a vacuum-compatible chamber for in-situ X-ray diffraction (XRD) studies and have used it to characterize the changing crystal structure of an inorganic–organic hybrid perovskite material, CH3NH3PbI3 (MAPbI3), during interactions with water vapor at room temperature. In the XRD spectra, we have observed the degradation of MAPbI3 and the creation of MAPbI3 hydrates, which follow simple rate equations. The time constant for the degradation of MAPbI3 during accelerated aging suggests that multiple collisions of water molecules with the MAPbI3 crystal trigger the degradation of the crystal.

  17. Evidence for Degradation of the Chrome Yellows in Van Gogh's Sunflowers: A Study Using Noninvasive In Situ Methods and Synchrotron-Radiation-Based X-ray Techniques.

    Science.gov (United States)

    Monico, Letizia; Janssens, Koen; Hendriks, Ella; Vanmeert, Frederik; Van der Snickt, Geert; Cotte, Marine; Falkenberg, Gerald; Brunetti, Brunetto Giovanni; Miliani, Costanza

    2015-11-16

    This paper presents firm evidence for the chemical alteration of chrome yellow pigments in Van Gogh's Sunflowers (Van Gogh Museum, Amsterdam). Noninvasive in situ spectroscopic analysis at several spots on the painting, combined with synchrotron-radiation-based X-ray investigations of two microsamples, revealed the presence of different types of chrome yellow used by Van Gogh, including the lightfast PbCrO4 and the sulfur-rich PbCr1-x Sx O4 (x≈0.5) variety that is known for its high propensity to undergo photoinduced reduction. The products of this degradation process, i.e., Cr(III) compounds, were found at the interface between the paint and the varnish. Selected locations of the painting with the highest risk of color modification by chemical deterioration of chrome yellow are identified, thus calling for careful monitoring in the future. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. In situ x-ray observations of the diamond formation process in the C-H sub 2 O-MgO system

    CERN Document Server

    Okada, T; Shimomura, O

    2002-01-01

    The diamond formation process in aqueous fluid catalyst under high-pressure and high-temperature conditions has been observed for the first time. Quench experiments and in situ x-ray diffraction experiments using synchrotron radiation have been performed upon a mixture of brucite (Mg(OH) sub 2) and graphite as the starting material. It was confirmed that brucite decomposed into periclase and H sub 2 O at 3.6 GPa and 1050 deg. C while its complete melting occurred at 6.2 GPa and 1150 deg. C, indicating that the solubility of MgO in H sub 2 O greatly increases with increasing pressure. The conversion of carbon from its graphite to its diamond form in aqueous fluid was observed at 7.7 GPa and 1835 deg. C.

  19. Hydrogen-Mediated Electron Doping of Gold Clusters As Revealed by In Situ X-ray and UV-vis Absorption Spectroscopy.

    Science.gov (United States)

    Ishida, Ryo; Hayashi, Shun; Yamazoe, Seiji; Kato, Kazuo; Tsukuda, Tatsuya

    2017-06-01

    We previously reported that small (∼1.2 nm) gold clusters stabilized by poly(N-vinyl-2-pyrrolidone) (Au:PVP) exhibited a localized surface plasmon resonance (LSPR) band at ∼520 nm in the presence of NaBH4. To reveal the mechanism of this phenomenon, the electronic structure of Au:PVP during the reaction with NaBH4 in air was examined by means of in situ X-ray absorption spectroscopy at Au L3-edge and UV-vis spectroscopy. These measurements indicated that the appearance of the LSPR band is not associated with the growth in size but is ascribed to electron doping to the Au sp band by the adsorbed H atoms.

  20. Solvent exchange in a metal–organic framework single crystal monitored by dynamic in situ X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Cox, Jordan M.; Walton, Ian M.; Bateman, Gage; Benson, Cassidy A.; Mitchell, Travis; Sylvester, Eric; Chen, Yu-Sheng; Benedict, Jason B. (UC); (Buffalo)

    2017-07-25

    Understanding the processes by which porous solid-state materials adsorb and release guest molecules would represent a significant step towards developing rational design principles for functional porous materials. To elucidate the process of liquid exchange in these materials, dynamicin situX-ray diffraction techniques have been developed which utilize liquid-phase chemical stimuli. Using these time-resolved diffraction techniques, the ethanol solvation process in a flexible metal–organic framework [Co(AIP)(bpy)0.5(H2O)]·2H2O was examined. The measurements provide important insight into the nature of the chemical transformation in this system including the presence of a previously unreported neat ethanol solvate structure.