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Sample records for surfaces synchrotron x-ray

  1. Reference-free total reflection X-ray fluorescence analysis of semiconductor surfaces with synchrotron radiation.

    PubMed

    Beckhoff, Burkhard; Fliegauf, Rolf; Kolbe, Michael; Müller, Matthias; Weser, Jan; Ulm, Gerhard

    2007-10-15

    Total reflection X-ray fluorescence (TXRF) analysis is a well-established method to monitor lowest level contamination on semiconductor surfaces. Even light elements on a wafer surface can be excited effectively when using high-flux synchrotron radiation in the soft X-ray range. To meet current industrial requirements in nondestructive semiconductor analysis, the Physikalisch-Technische Bundesanstalt (PTB) operates dedicated instrumentation for analyzing light element contamination on wafer pieces as well as on 200- and 300-mm silicon wafer surfaces. This instrumentation is also suited for grazing incidence X-ray fluorescence analysis and conventional energy-dispersive X-ray fluorescence analysis of buried and surface nanolayered structures, respectively. The most prominent features are a high-vacuum load-lock combined with an equipment front end module and a UHV irradiation chamber with an electrostatic chuck mounted on an eight-axis manipulator. Here, the entire surface of a 200- or a 300-mm wafer can be scanned by monochromatized radiation provided by the plane grating monochromator beamline for undulator radiation in the PTB laboratory at the electron storage ring BESSY II. This beamline provides high spectral purity and high photon flux in the range of 0.078-1.86 keV. In addition, absolutely calibrated photodiodes and Si(Li) detectors are used to monitor the exciting radiant power respectively the fluorescence radiation. Furthermore, the footprint of the excitation radiation at the wafer surface is well-known due to beam profile recordings by a CCD during special operation conditions at BESSY II that allow for drastically reduced electron beam currents. Thus, all the requirements of completely reference-free quantitation of TXRF analysis are fulfilled and are to be presented in the present work. The perspectives to arrange for reference-free quantitation using X-ray tube-based, table-top TXRF analysis are also addressed. PMID:17880182

  2. 3-D surface profile measurements of large x-ray synchrotron radiation mirrors using stitching interferometry.

    SciTech Connect

    Assoufid, L.; Bray, M.; Qian, J.; Shu, D.

    2002-09-12

    Stitching interferometry, using small-aperture, high-resolution, phase-measuring interferometry, has been proposed for quite some time now as a metrology technique to obtain 3-dimensional profiles of surfaces of oversized optical components and substrates. The aim of this work is to apply this method to the specific case of long grazing-incidence x-ray mirrors, such as those used in beamlines at synchrotron radiation facilities around the world. Both fabrication and characterization of these mirrors would greatly benefit from this technique because it offers the potential for providing measurements with accuracy and resolution better than those obtained using existing noncontact laser profilers, such as the long trace profiler (LTP). Measurement data can be used as feedback for computer-controlled fabrication processes to correct for possible topography errors. The data can also be used for simulating and predicting mirror performance under realistic conditions. A semiautomated stitching system was built and tested at the X-ray Optics Metrology Laboratory of the Advanced Photon Source at Argonne National Laboratory. The initial objective was to achieve a measurement sensitivity on the order of 1 {micro}rad rms. Preliminary tests on a 1 m-long x-ray mirror showed system repeatability of less than 0.6 {micro}rad rms. This value is comparable to that of a conventional LTP. The measurement accuracy was mostly affected by environmental perturbations and system calibration effects. With a fully automated and improved system (to be built in the near future), we expect to achieve measurement sensitivity on the order of 0.0 {micro}rad rms or better. In this paper, after a brief review of basic principles and general technical difficulties and challenges of the stitching technique, a detailed description of the measurement setup is given and preliminary results obtained with it are analyzed and discussed.

  3. Assessment of Barium Sulphate Formation and Inhibition at Surfaces with Synchrotron X-ray Diffraction (SXRD)

    SciTech Connect

    E Mavredaki; A Neville; K Sorbie

    2011-12-31

    The precipitation of barium sulphate from aqueous supersaturated solutions is a well-known problem in the oil industry often referred to as 'scaling'. The formation and growth of barite on surfaces during the oil extraction process can result in malfunctions within the oil facilities and serious damage to the equipment. The formation of barium sulphate at surfaces remains an important topic of research with the focus being on understanding the mechanisms of formation and means of control. In situ synchrotron X-ray diffraction (SXRD) was used to investigate the formation of barium sulphate on a stainless steel surface. The effect of Poly-phosphinocarboxylic acid (PPCA) and Diethylenetriamine-penta-methylenephosphonic acid (DETPMP) which are two commercial inhibitors for barium sulphate was examined. The in situ SXRD measurements allowed the identification of the crystal faces of the deposited barite in the absence and presence of the two inhibitors. The preferential effect of the inhibitors on some crystal planes is reported and the practical significance discussed.

  4. Ion distributions at charged aqueous surfaces: Synchrotron X-ray scattering studies

    SciTech Connect

    Bu, Wei

    2009-01-01

    Surface sensitive synchrotron X-ray scattering studies were performed to obtain the distribution of monovalent ions next to a highly charged interface at room temperature. To control surface charge density, lipids, dihexadecyl hydrogen-phosphate (DHDP) and dimysteroyl phosphatidic acid (DMPA), were spread as monolayer materials at the air/water interface, containing CsI at various concentrations. Five decades in bulk concentrations (CsI) are investigated, demonstrating that the interfacial distribution is strongly dependent on bulk concentration. We show that this is due to the strong binding constant of hydronium H3O+ to the phosphate group, leading to proton-transfer back to the phosphate group and to a reduced surface charge. Using anomalous reflectivity off and at the L3 Cs+ resonance, we provide spatial counterion (Cs+) distributions next to the negatively charged interfaces. The experimental ion distributions are in excellent agreement with a renormalized surface charge Poisson-Boltzmann theory for monovalent ions without fitting parameters or additional assumptions. Energy Scans at four fixed momentum transfers under specular reflectivity conditions near the Cs+ L3 resonance were conducted on 10-3 M CsI with DHDP monolayer materials on the surface. The energy scans exhibit a periodic dependence on photon momentum transfer. The ion distributions obtained from the analysis are in excellent agreement with those obtained from anomalous reflectivity measurements, providing further confirmation to the validity of the renormalized surface charge Poisson-Boltzmann theory for monovalent ions. Moreover, the dispersion corrections f0 and f00 for Cs+ around L3 resonance, revealing the local environment of a Cs+ ion in the solution at the interface, were extracted simultaneously with output of ion distributions.

  5. Effects of Surface Processing on the Response of CZT Gamma Detectors: Studies with a Collimated Synchrotron X-Ray Beam

    SciTech Connect

    Hossain,A.; Bolotnikov, A.; Camarda, G.; Cui, Y.; Babalola, S.; Burger, A.; James, R.

    2008-01-01

    Using a microscale X-ray mapping technique incorporating a synchrotron beam, we are able to reveal the fine details of the surface properties in cadmium zinc telluride (CZT) semiconductor detectors. A detector, with various degrees of surface roughness, was irradiated by a high-spatial-resolution X-ray beam. The detector's response was analyzed and displayed as a two-dimensional (2-D) map, and the charge collection was obtained from the peak positions in the spectra versus the beam's location, which reflects the local material properties. We noted the correlation between the 2-D image and the spectral response of the charge collection at different locations on the surface area, which indicates that a rough surface tends to contain trapping centers, thereby enhancing leakage current and distorting the signal. We also discuss our observations on the transition effect at the boundary area of a rough and a smooth surface under identical conditions.

  6. Fast in situ phase and stress analysis during laser surface treatment: a synchrotron x-ray diffraction approach.

    PubMed

    Kostov, V; Gibmeier, J; Wilde, F; Staron, P; Rössler, R; Wanner, A

    2012-11-01

    An in situ stress analysis by means of synchrotron x-ray diffraction was carried out during laser surface hardening of steel. A single exposure set-up that based on a special arrangement of two fast silicon strip line detectors was established, allowing for fast stress analysis according to the sin(2)ψ x-ray analysis method. For the in situ experiments a process chamber was designed and manufactured, which is described in detail. First measurements were carried out at the HZG undulator imaging beamline (IBL, beamline P05) at the synchrotron storage ring PETRA III, DESY, Hamburg (Germany). The laser processing was carried out using a 6 kW high power diode laser system. Two different laser optics were compared, a Gaussian optic with a focus spot of ø 3 mm and a homogenizing optic with a rectangular spot dimension of 8 × 8 mm(2). The laser processing was carried out using spot hardening at a heating-/cooling rate of 1000 K/s and was controlled via pyrometric temperature measurement using a control temperature of 1150 °C. The set-up being established during the measuring campaign allowed for this first realization data collection rates of 10Hz. The data evaluation procedure applied enables the separation of thermal from elastic strains and gains unprecedented insight into the laser hardening process. PMID:23206092

  7. Imaging the heterogeneity of mineral surface reactivity using Ag(I) and synchrotron X-ray microscopy

    SciTech Connect

    Amonette, James E.; Heald, Steve M.; Russell, Colleen K.

    2003-10-01

    Microscopic-scale imaging of reduced zones on the surfaces of minerals can be achieved by reaction with dilute Ag(I) solutions and subsequent analysis using synchrotron X-ray microscopy (XRM) above the Ag K-edge (25.5 keV). The principal reductant is Fe(II), but other reductants such as sulfide may contribute. Reduced zones may exist instrinsically, as in the structure of biotite and augite, or may be generated by reaction with chemical agents such as dithionite or treatment with sulfate-reducing bacteria (SRB). We demonstrate the method on flakes of specular hematite and biotite, as well as on thin sections of different rocks (arfvedsonitic granite, oolitic hematite, diabase, and quartz conglomerate) treated with SRB, and discuss possible artifacts that can occur. To our knowledge, this is the only microscopic technique that can image Fe(II) zones on the surface of an Fe-bearing mineral with monolayer sensitivity.

  8. Challenges for Synchrotron X-Ray Optics

    NASA Astrophysics Data System (ADS)

    Freund, Andreas K.

    2002-12-01

    It is the task of x-ray optics to adapt the raw beam generated by modern sources such as synchrotron storage rings to a great variety of experimental requirements in terms of intensity, spot size, polarization and other parameters. The very high quality of synchrotron radiation (source size of a few microns and beam divergence of a few micro-radians) and the extreme x-ray flux (power of several hundred Watts in a few square mm) make this task quite difficult. In particular the heat load aspect is very important in the conditioning process of the brute x-ray power to make it suitable for being used on the experimental stations. Cryogenically cooled silicon crystals and water-cooled diamond crystals can presently fulfill this task, but limits will soon be reached and new schemes and materials must be envisioned. A major tendency of instrument improvement has always been to concentrate more photons into a smaller spot utilizing a whole variety of focusing devices such as Fresnel zone plates, refractive lenses and systems based on bent surfaces, for example, Kirkpatrick-Baez systems. Apart from the resistance of the sample, the ultimate limits are determined by the source size and strength on one side, by materials properties, cooling, mounting and bending schemes on the other side, and fundamentally by the diffraction process. There is also the important aspect of coherence that can be both a nuisance and a blessing for the experiments, in particular for imaging techniques. Its conservation puts additional constraints on the quality of the optical elements. The overview of the present challenges includes the properties of present and also mentions aspects of future x-ray sources such as the "ultimate" storage ring and free electron lasers. These challenges range from the thermal performances of monochromators to the surface quality of mirrors, from coherence preservation of modern multilayers to short pulse preservation by crystals, and from micro- and nano

  9. X-ray microscopy using synchrotron radiation

    SciTech Connect

    Jones, K.W.; Gordon, B.M.; Hanson, A.L.; Pounds, J.G.; Rivers, M.L.; Schidlovsky, G.; Smith, J.V.; Spanne, P.; Sutton, S.R.

    1989-01-01

    The system for x-ray microscopy now being developed at the X-26 beam line of the Brookhaven National Synchrotron Light Source (NSLS) is described here. Examples of the use of x-ray microscopy for trace element geochemistry, biology and medicine, and materials investigations are given to emphasize the scientific applications of the technique. Future directions for the improvement and further development of the X-26 microscope and of the x-ray microscopy field in general are discussed. 11 refs., 7 figs.

  10. Synchrotron beamlines for x-ray lithography

    NASA Astrophysics Data System (ADS)

    Trippe, Anthony P.; Pearce, W. J.

    1994-02-01

    Louisiana State University established the J. Bennett Johnston, Sr., Center for Advanced Microstructures and Devices (CAMD). Designed and constructed by the Brobeck Division of Maxwell Laboratories, the CAMD synchrotron light source is the first electron storage ring to be built by a commercial company in the United States. The synchrotron x-ray radiation generated at CAMD is an extremely useful exposure source for both thin and thick film lithography. Passing through a beamline containing two plane mirrors, the synchrotron light is used to expose thin resists for lithography of patterns with feature sizes of 0.25 micron and smaller. Two thick-resist beamlines, one using a single aspheric (collimating) mirror and one using a plane mirror, provide the higher flux photons required for miniaturization in silicon to produce microscopic mechanical devices including gears, motors, filters, and valves.

  11. Synchrotron X-ray emission from old pulsars

    NASA Astrophysics Data System (ADS)

    Kisaka, Shota; Tanaka, Shuta J.

    2014-09-01

    We study the synchrotron radiation as the observed non-thermal emission by the X-ray satellites from old pulsars (≳1-10 Myr) to investigate the particle acceleration in their magnetospheres. We assume that the power-law component of the observed X-ray spectra is caused by the synchrotron radiation from electrons and positrons in the magnetosphere. We consider two pair-production mechanisms of X-ray emitting particles, the magnetic and the photon-photon pair productions. High-energy photons, which ignite the pair production, are emitted via the curvature radiation of the accelerated particles. We use the analytical description for the radiative transfer and estimate the luminosity of the synchrotron radiation. We find that for pulsars with the spin-down luminosity Lsd ≲ 1033 erg s-1, the locations of the particle acceleration and the non-thermal X-ray emission are within ≲107 cm from the centre of the neutron star, where the magnetic pair production occurs. For pulsars with the spin-down luminosity Lsd ≲ 1031 erg s-1 such as J0108-1431, the synchrotron radiation is difficult to explain the observed non-thermal component even if we consider the existence of the strong and small-scale surface magnetic field structures.

  12. Synchrotron X-ray imaging applied to solar photovoltaic silicon

    NASA Astrophysics Data System (ADS)

    Lafford, T. A.; Villanova, J.; Plassat, N.; Dubois, S.; Camel, D.

    2013-03-01

    Photovoltaic (PV) cell performance is dictated by the material of the cell, its quality and purity, the type, quantity, size and distribution of defects, as well as surface treatments, deposited layers and contacts. A synchrotron offers unique opportunities for a variety of complementary X-ray techniques, given the brilliance, spectrum, energy tunability and potential for (sub-) micron-sized beams. Material properties are revealed within in the bulk and at surfaces and interfaces. X-ray Diffraction Imaging (X-ray Topography), Rocking Curve Imaging and Section Topography reveal defects such as dislocations, inclusions, misorientations and strain in the bulk and at surfaces. Simultaneous measurement of micro-X-Ray Fluorescence (μ-XRF) and micro-X-ray Beam Induced Current (μ-XBIC) gives direct correlation between impurities and PV performance. Together with techniques such as microscopy and Light Beam Induced Current (LBIC) measurements, the correlation between structural properties and photovoltaic performance can be deduced, as well as the relative influence of parameters such as defect type, size, spatial distribution and density (e.g [1]). Measurements may be applied at different stages of solar cell processing in order to follow the evolution of the material and its properties through the manufacturing process. Various grades of silicon are under study, including electronic and metallurgical grades in mono-crystalline, multi-crystalline and mono-like forms. This paper aims to introduce synchrotron imaging to non-specialists, giving example results on selected solar photovoltaic silicon samples.

  13. Measuring Cavitation with Synchrotron X-Rays

    NASA Astrophysics Data System (ADS)

    Duke, Daniel; Kastengren, Alan; Powell, Chris; X-Ray Fuel Spray Group, Energy Systems Division Team

    2012-11-01

    Cavitation plays an important role in the formation of sprays from small nozzles such as those found in fuel injection systems. A sharp-edged inlet from the sac into the nozzle of a diesel fuel injector is shown to inititate a strong sheet-like cavitation along the boundary layer of the nozzle throat, which is difficult to measure and can lead to acoustic damage. To investigate this phenomenon, a diagnostic technique capable of mapping the density field of the nozzle through regions of intense cavitation is required. Available visible-light techniques are limited to qualitative observations of the outer extent of cavitation zones. However, brilliant X-rays from a synchrotron source have negligible refraction and are capable of penetrating the full extent of cavitation zones. We present the early results of a novel application of line-of-sight, time-resolved X-ray radiography on a cavitating model nozzle. Experiments were conducted at Sector 7-BM of the Advanced Photon Source. Density and vapor distribution are measured from the quantitative absorption of monochromatic X-rays. The density field can then be tomographically reconstructed from the projections. The density is then validated against a range of compressible and incompressible numerical simulations. This research was performed at the 7-BM beamline of the Advanced Photon Source. We acknowledge the support of the U.S. Department of Energy under Contract No. DE-AC02-06CH11357 and the DOE Vehicle Technologies Program (DOE-EERE).

  14. Structure analysis of the Ag (001) surface at 25 K by synchrotron x-ray crystal truncation rod scattering

    SciTech Connect

    Sakata, O.; Shimada, Y.; Walker, C.J.; Yi, M.-S.; Imai, Y.

    2004-05-12

    We have commissioned an ultra-high vacuum chamber for surface structure determination at an undulator beamline BL13XU, SPring-8. As a test experiment, a structure of a Ag (001) surface at a temperature of 25 K has been studied by analyzing x-ray scattering intensities along several surface crystal truncation rods (CTR). Results of least-squares fits to the CTR data show that the top atomic layer was shifted inwards by 0.0011 nm {+-} 0.0003 nm relative to the bulk position.

  15. X-ray studies of multilayer semiconductors using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Huang, Shiwen

    X-ray scattering and absorption techniques utilizing synchrotron radiation have been used to study a variety of multilayer semiconductors. The angular-dependent x-ray scattering at grazing incidence angles (grazing incidence x-ray scattering, GIXS) provides structural information of interfaces in these materials, such as rms interfacial roughness, cross- and lateral-correlation lengths, etc. Long-range order structures in material are probed by large-angle scattering (x-ray diffraction), in which strain and lattice constant as well as crystallinity of the epilayers are measured. Local structural variations in materials including local bond length, coordination number, and local disorder are obtained quantitatively by examining the modulation in the x-ray absorption spectrum some 40 eV above the absorption edge (extended x-ray absorption fine structure, EXAFS). Materials studied in the present work are SiGe/Si heterostructures, MnAs/GaAs ferromagnetic-semiconductor films, solar cell films, ZnSe-based II-VI semiconductor thin films, InGaAs/GaAs and GaAs/AlAs superlattices. Results obtained have shown (i) evidence for strain-induced surface/interface morphology variations in SiGe/Si heterostructures, (ii) template-dependent microstructures in MnAs/GaAs, (iii) changes in interface structures for films of different formations in solar cell films, (iv) differences between samples prepared by different epitaxial growth methods in II-VI semiconductor films, (v) observation of lateral structural ordering in one of the InGaAs/GaAs superlattices, (vi) differences in interfacial microstructures between MBE-grown samples with different interrupts in GaAs/AlAs superlattices. Most of all, x- rays are found to be a very useful nondestructive tool for probing microscopic structures in various multilayer semiconductor materials.

  16. X-ray reflectivity and surface roughness

    SciTech Connect

    Ocko, B.M.

    1988-01-01

    Since the advent of high brightness synchrotron radiation sources there has been a phenomenal growth in the use of x-rays as a probe of surface structure. The technique of x-ray reflectivity is particularly relevant to electrochemists since it is capable of probing the structure normal to an electrode surface in situ. In this paper the theoretical framework for x-ray reflectivity is reviewed and the results from previous non-electrochemistry measurements are summarized. These measurements are from the liquid/air interface (CCl/sub 4/), the metal crystal vacuum interface (Au(100)), and from the liquid/solid interface(liquid crystal/silicon). 34 refs., 5 figs.

  17. EVOLUTION OF SYNCHROTRON X-RAYS IN SUPERNOVA REMNANTS

    SciTech Connect

    Nakamura, Ryoko; Bamba, Aya; Dotani, Tadayasu; Ishida, Manabu; Kohri, Kazunori

    2012-02-20

    A systematic study of the synchrotron X-ray emission from supernova remnants (SNRs) has been conducted. We selected a total of 12 SNRs whose synchrotron X-ray spectral parameters are available in the literature with reasonable accuracy and studied how their luminosities change as a function of radius. It is found that the synchrotron X-ray luminosity tends to drop especially when the SNRs become larger than {approx}5 pc, despite large scatter. This may be explained by the change of spectral shape caused by the decrease of the synchrotron roll-off energy. A simple evolutionary model of the X-ray luminosity is proposed and is found to reproduce the observed data approximately, with reasonable model parameters. According to the model, the total energy of accelerated electrons is estimated to be 10{sup 47-48} erg, which is well below the supernova explosion energy. The maximum energies of accelerated electrons and protons are also discussed.

  18. The metrology of spherical shells using synchrotron x ray microtomography

    NASA Technical Reports Server (NTRS)

    Hmelo, Anthony B.; Allen, James L.; Damico, Kevin L.

    1990-01-01

    With recent advances in solid state imaging technology and the increasing availability of synchrotron x-ray radiation sources, synchrotron x-ray microtomography is emerging as a nondestructive technique for the evaluation of the structure and composition of small specimens with spatial resolution in the micron range. Synchrotron radiation offers the following advantages over conventional x-ray sources: high brightness, continuous emission which is tunable over a large energy range, faster data collection rates, and a highly collimated beam of large cross section permitting the illumination of large specimens. Synchrotron x-ray microtomography enables the structure of individual spheres to be evaluated in order to reveal the concentricity and sphericity of the internal void and the uniformity of the shell wall in the case of high quality spherical shells for Sandia National Laboratories' Inertial Confinement Fusion project.

  19. X-ray fluorescence imaging with synchrotron radiation

    SciTech Connect

    Rivers, M.L.

    1987-01-01

    The micro-distribution of trace elements is of great interest in fields such as geochemistry, biology and material science. The synchrotron x-ray fluorescence microprobe provides a technique to quantitatively measure trace element compositions at individual points and to construct semiquantitative two dimensional maps of trace element compositions. This paper describes an x-ray fluorescence system used at the National Synchrotron Light Source.

  20. Synchrotron X-ray techniques for fluid dynamics

    NASA Astrophysics Data System (ADS)

    Kastengren, Alan; Powell, Christopher F.

    2014-03-01

    X-ray diagnostics have the potential for making quantitative measurements in many flowfields where optical diagnostics are challenging, especially multiphase flows. In the past, many such measurements have been taken with laboratory-scale X-ray sources. This review describes the measurements that are possible with synchrotron X-ray sources, which can provide high-flux, tunable, monochromatic X-ray beams that cannot be created with laboratory sources. The relevant properties of X-rays and their interactions with matter are described. The types and capabilities of various X-ray optics and sources are discussed. Finally, four major X-ray diagnostics are described in detail. X-ray radiography provides quantitative measurements of density in variable-density flows. X-ray phase-contrast imaging is used to visualize multiphase flows with high spatial and temporal resolution. X-ray fluorescence spectroscopy shows significant promise to study mixing in single-phase and multiphase flows. Small-angle X-ray scattering is a powerful technique to examine small-scale particles in flows.

  1. Synchrotron-Radiation Induced X-Ray Emission (SRIXE)

    SciTech Connect

    Jones, Keith W.

    1999-09-01

    Elemental analysis using emission of characteristic x rays is a well-established scientific method. The success of this analytical method is highly dependent on the properties of the source used to produce the x rays. X-ray tubes have long existed as a principal excitation source, but electron and proton beams have also been employed extensively. The development of the synchrotron radiation x-ray source that has taken place during the past 40 years has had a major impact on the general field of x-ray analysis. Even tier 40 years, science of x-ray analysis with synchrotron x-ray beams is by no means mature. Improvements being made to existing synchrotron facilities and the design and construction of new facilities promise to accelerate the development of the general scientific use of synchrotron x-ray sources for at least the next ten years. The effective use of the synchrotron source technology depends heavily on the use of high-performance computers for analysis and theoretical interpretation of the experimental data. Fortunately, computer technology has advanced at least as rapidly as the x-ray technology during the past 40 years and should continue to do so during the next decade. The combination of these technologies should bring about dramatic advances in many fields where synchrotron x-ray science is applied. It is interesting also to compare the growth and rate of acceptance of this particular research endeavor to the rates for other technological endeavors. Griibler [1997] cataloged the time required for introduction, diffusion,and acceptance of technological, economic, and social change and found mean values of 40 to 50 years. The introduction of the synchrotron source depends on both technical and non-technical factors, and the time scale at which this seems to be occurring is quite compatible with what is seen for other major innovations such as the railroad or the telegraph. It will be interesting to see how long the present rate of technological change

  2. Synchrotron x-ray scattering study on the evolution of surface morphology of the InN/Al2O3)(0001 system

    NASA Astrophysics Data System (ADS)

    Lee, Ik Jae; Kim, Jin Woo; Hur, Tae-Bong; Hwang, Yoon-Hwae; Kim, Hyung-Kook

    2002-07-01

    Dynamic scaling behavior was studied for InN films grown on sapphire(0001) substrates using high-resolution synchrotron x-ray reflectivity and atomic force microscopy measurements. In the early stage of growth, highly strained planar InN films were grown. As the film thickness approaches an effective critical thickness, the growth gradually crosses over to the island growth. Concurrently, the relaxation of the lattice strain begins and the growth front becomes rougher. The roughness increases mostly during the intermediate crossover regime where the strain is relieved. In this regime, the dynamic scaling exponent, beta, is estimated as 1.754plus-or-minus0.071. The evolution of the surface roughness in the final-stage growth can be described by the dynamic scaling exponent of 0.236plus-or-minus0.022.

  3. Lead adsorption at the calcite-water interface: Synchrotron x-ray standing wave and x-ray reflectivity studies

    SciTech Connect

    Sturchio, N.C.; Chiarello, R.P.; You, Hoydoo

    1997-01-01

    By combining synchrotron X-ray standing wave (XSW) measurements with synchrotron X-ray reflectivity measurements, we have determined: (1) the precise three-dimensional location within the calcite unit cell of submonolayer Pb ions adsorbed at the calcite (104) surface from dilute aqueous solutions, and (2) the precise one-dimensional location of these unit cells relative to the calcite surface. Our XSW measurements, using three separate calcite Bragg reflections for triangulation, show that most adsorbed Pb ions occupy Ca sites in the calcite lattice with an ordered coverage of 0.05 equivalent monolayers, while the remaining Pb ions are disordered with a coverage of 0.03 equivalent monolayers. Our X-ray reflectivity measurements show that the ordered Ph ions occur primarily (>70%) in the surface atomic layer of calcite. Atomic force microscopy (AFM) was used to characterize the topography of the calcite (104) surface under conditions similar to the X-ray experiments. The quantitative morphological information obtained by AFM was used to develop realistic models of the calcite surface. The calculated X-ray reflectivities for these model surfaces were compared with the measured X-ray reflectivities. The new combined X-ray method that we have developed can be used to determine the atomic-scale structure of other metals adsorbed at mineral-water interfaces. Such high-resolution structural determinations are essential before detailed conceptual and theoretical models can be further developed to understand and predict the behavior of dissolved metals in mineral-water systems. 60 refs., 8 figs., 3 tabs.

  4. Synchrotron x-ray modification of nanoparticle superlattice formation

    NASA Astrophysics Data System (ADS)

    Lu, Chenguang; Akey, Austin J.; Herman, Irving P.

    2012-09-01

    The synchrotron x-ray radiation used to perform small angle x-ray scattering (SAXS) during the formation of three-dimensional nanoparticle superlattices by drop casting nanoparticle solutions affects the structure and the local crystalline order of the resulting films. The domain size decreases due to the real-time SAXS analysis during drying and more macroscopic changes are visible to the eye.

  5. Phase-contrast x-ray tomography using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Bonse, Ulrich; Beckmann, Felix; Bartscher, Markus; Biermann, Theodor; Busch, Frank; Guennewig, Olaf

    1997-10-01

    The principle and experimental l realization of x-ray phase- contrast in compute assisted microtomography ((mu) CT) at the micrometer resolution level is described. The camera used is a modification of a setup previously developed by us for attenuation-contrast (mu) CT using synchrotron x-rays. Phase detection is accomplished by employing the x-ray interferometer. By using x-ray phase contrast it is possible to image structural details in low-z biological tissues much better than with absorption contrast. The advantage of phase over attenuation contrast is not limited to light element or to low x-ray energies. Examples of applying phase contrast (mu) CT to the structural investigation of rat trigeminal nerve are given.

  6. X-ray and synchrotron studies of porous silicon

    SciTech Connect

    Sivkov, V. N.; Lomov, A. A.; Vasil'ev, A. L.; Nekipelov, S. V.; Petrova, O. V.

    2013-08-15

    The results of comprehensive studies of layers of porous silicon of different conductivity types, grown by anodizing standard Si(111) substrates in an electrolyte based on fluoric acid and ethanol with the addition of 5% of iodine and kept in air for a long time, are discussed. Measurements are performed by scanning electron microscopy, high-resolution X-ray diffraction, and ultrasoft X-ray spectroscopy using synchrotron radiation. The structural parameters of the layers (thickness, strain, and porosity) and atomic and chemical composition of the porous-silicon surface are determined. It is found that an oxide layer 1.5-2.3-nm thick is formed on the surface of the silicon skeleton. The near-edge fine structure of the Si 2p absorption spectrum of this layer corresponds to the fine structure of the 2p spectrum of well coordinated SiO{sub 2}. In this case, the fine structure in the Si 2p-edge absorption region of the silicon skeleton is identical to that of the 2p absorption spectrum of crystalline silicon.

  7. Synchrotron X-ray footprinting on tour

    PubMed Central

    Bohon, Jen; D’Mello, Rhijuta; Ralston, Corie; Gupta, Sayan; Chance, Mark R.

    2014-01-01

    Synchrotron footprinting is a valuable technique in structural biology for understanding macromolecular solution-state structure and dynamics of proteins and nucleic acids. Although an extremely powerful tool, there is currently only a single facility in the USA, the X28C beamline at the National Synchrotron Light Source (NSLS), dedicated to providing infrastructure, technology development and support for these studies. The high flux density of the focused white beam and variety of specialized exposure environments available at X28C enables footprinting of highly complex biological systems; however, it is likely that a significant fraction of interesting experiments could be performed at unspecialized facilities. In an effort to investigate the viability of a beamline-flexible footprinting program, a standard sample was taken on tour around the nation to be exposed at several US synchrotrons. This work describes how a relatively simple and transportable apparatus can allow beamlines at the NSLS, CHESS, APS and ALS to be used for synchrotron footprinting in a general user mode that can provide useful results. PMID:24365913

  8. Synchrotron x-ray reticulography: principles and applications

    NASA Astrophysics Data System (ADS)

    Lang, A. R.; Makepeace, A. P. W.

    1999-05-01

    Synchrotron x-ray reticulography is a versatile new technique for mapping misorientations in single crystals. It is nearly as simple to perform as conventional single-crystal Laue topography, yet it yields quantitative data on misorientations that would demand long sequences of images if the double-crystal technique were applied. In reticulography a fine-scale x-ray absorbing mesh is placed between a Laue-diffracting crystal specimen and the topograph-recording photographic plate. The mesh splits the diffracted beam into an array of individually identifiable microbeams. Direction differences between microbeams, which give the orientation differences between the crystal elements reflecting them, are measured from their relative shifts within the array when mesh-to-plate distance is changed. The angular sensitivity of reticulography depends upon the angular size of the x-ray source. At Station 7.6 at the SRS, Daresbury, 80 m from the tangent point, and with source size FWHM (full width half maximum) = 0.23 mm vertically, the incidence angular range in the vertical plane is only 0.6 arcsec, and misorientations down to this magnitude are measurable. Applications of reticulography to three quite different problems are described, illustrating the method's versatility. The problems are: (1) measuring surface lattice-plane tilts due to an array of dislocations in a large synthetic diamond; (2) determining the sense of the Burgers vector of a giant screw dislocation in SiC; and (3) measuring lattice curvature above an energetic ion implant in a natural diamond.

  9. 3D synchrotron x-ray microtomography of paint samples

    NASA Astrophysics Data System (ADS)

    Ferreira, Ester S. B.; Boon, Jaap J.; van der Horst, Jerre; Scherrer, Nadim C.; Marone, Federica; Stampanoni, Marco

    2009-07-01

    Synchrotron based X-ray microtomography is a novel way to examine paint samples. The three dimensional distribution of pigment particles, binding media and their deterioration products as well as other features such as voids, are made visible in their original context through a computing environment without the need of physical sectioning. This avoids manipulation related artefacts. Experiments on paint chips (approximately 500 micron wide) were done on the TOMCAT beam line (TOmographic Microscopy and Coherent rAdiology experimenTs) at the Paul Scherrer Institute in Villigen, CH, using an x-ray energy of up to 40 keV. The x-ray absorption images are obtained at a resolution of 350 nm. The 3D dataset was analysed using the commercial 3D imaging software Avizo 5.1. Through this process, virtual sections of the paint sample can be obtained in any orientation. One of the topics currently under research are the ground layers of paintings by Cuno Amiet (1868- 1961), one of the most important Swiss painters of classical modernism, whose early work is currently the focus of research at the Swiss Institute for Art Research (SIK-ISEA). This technique gives access to information such as sample surface morphology, porosity, particle size distribution and even particle identification. In the case of calcium carbonate grounds for example, features like microfossils present in natural chalks, can be reconstructed and their species identified, thus potentially providing information towards the mineral origin. One further elegant feature of this technique is that a target section can be selected within the 3D data set, before exposing it to obtain chemical data. Virtual sections can then be compared with cross sections of the same samples made in the traditional way.

  10. X-ray polarization splitting by a single crystal evaluated with synchrotron x-rays

    SciTech Connect

    Pereira, N. R.; Presura, R.; Wallace, M.; Kastengren, A.

    2014-07-15

    In hexagonal crystals such as quartz, an asymmetric Bragg reflection from two equivalent internal crystal planes can separate unpolarized x-rays into two linearly polarized components. The perfectly polarized and tunable x-rays from a synchrotron are ideal to evaluate polarization spitting in detail. One unanticipated feature is that additional reflections from the crystal affect the diffraction intensity of the two polarized components, an effect that is unlikely to matter in polarization spectroscopy of radiating plasmas for which the crystal is intended.

  11. Wavelength dispersive analysis with the synchrotron x ray fluorescence microprobe

    NASA Technical Reports Server (NTRS)

    Rivers, M. L.; Thorn, K. S.; Sutton, S. R.; Jones, K. W.; Bajt, S.

    1993-01-01

    A wavelength dispersive spectrometer (WDS) was tested on the synchrotron x ray fluorescence microprobe at Brookhaven National Laboratory. Compared to WDS spectra using an electron microprobe, the synchrotron WDS spectra have much better sensitivity and, due to the absence of bremsstrahlung radiation, lower backgrounds. The WDS spectrometer was successfully used to resolve REE L fluorescence spectra from standard glasses and transition metal K fluorescence spectra from kamacite.

  12. X-ray imaging detectors for synchrotron and XFEL sources

    PubMed Central

    Hatsui, Takaki; Graafsma, Heinz

    2015-01-01

    Current trends for X-ray imaging detectors based on hybrid and monolithic detector technologies are reviewed. Hybrid detectors with photon-counting pixels have proven to be very powerful tools at synchrotrons. Recent developments continue to improve their performance, especially for higher spatial resolution at higher count rates with higher frame rates. Recent developments for X-ray free-electron laser (XFEL) experiments provide high-frame-rate integrating detectors with both high sensitivity and high peak signal. Similar performance improvements are sought in monolithic detectors. The monolithic approach also offers a lower noise floor, which is required for the detection of soft X-ray photons. The link between technology development and detector performance is described briefly in the context of potential future capabilities for X-ray imaging detectors. PMID:25995846

  13. X-Ray Absorption Spectra of Uranium by Synchrotron Radiation

    NASA Astrophysics Data System (ADS)

    Adachi, Hirohiko; Fujima, Kazumi; Taniguchi, Kazuo; Miyake, Chie; Imoto, Shosuke

    1981-08-01

    The X-ray absorption spectra of U, UO2 and UCl4 near the U OIV and OV thresholds have been measured by use of synchrotron radiation. The absorption peaks at about 100 eV and 110 eV are observed for all of these materials. However, the detailed structure of the spectra depend on the chemical state.

  14. TOPICAL REVIEW: Medical applications of synchrotron radiation x-rays

    NASA Astrophysics Data System (ADS)

    Lewis, R.

    1997-07-01

    The use of synchrotron radiation is not widespread in the field of medicine and in fact few health-care professionals have even heard of it. It is the purpose of this article to explain what it is and to give some examples of how it can contribute to medical science. X-rays have been used for diagnostic medical imaging for more than 100 years and, whilst new techniques such as computed tomography have been developed, the means of producing x-rays has altered little during that time. Synchrotron radiation sources provide multiple, extremely intense and tuneable beams of photons over a huge range of energies from infrared through to hard x-rays. Their advent has revolutionized many experimental techniques and synchrotron radiation is being applied across many fields from imaging to molecular dynamics. It has spawned several methods for studying live and wet tissue samples, yielding information on both structure and composition on all length scales down to atomic resolution. Such techniques have played a crucial role in the development of molecular biology and the solution of protein structures. The application of synchrotron radiation in the field of radiography is now expanding and it is clear that very substantial improvements in image quality and patient dose can be realized. Following an overview of the production and properties of synchrotron radiation, some of the ways in which this remarkable tool has already been exploited for medical research are reviewed and some potential clinical opportunities highlighted.

  15. Applications of synchrotron x-ray fluorescence to extraterrestrial materials

    SciTech Connect

    Sutton, S.R.; Rivers, M.L.; Smith, J.V.

    1986-01-01

    Synchrotron x-ray fluorescence (SXRF) is a valuable technique for trace element analyses of extraterrestrial materials permitting minimum detection limits less than 1 ppM for 20 micrometer spots. SXRF measurements have been performed on iron meteorites and micrometeorites using white synchrotron radiation and an energy dispersive x-ray detector at the National Synchrotron Light Source (X-26C), Brookhaven National Laboratory (NY). Partitioning of Cu between troilite (FeS) and metal in the nine iron meteorites studied suggests sub-solidus re-equilibration in these objects. A technique has been developed for determining self-absorption corrections for filtered, continuum excitation of small specimens, such as stratospheric particles and refractory inclusions in meteorites.

  16. X-ray multilayer optics for Indus synchrotrons application

    NASA Astrophysics Data System (ADS)

    Nayak, Maheswar; Pradhan, P. C.; Lodha, G. S.

    2015-06-01

    We present the state-of-the-art X-ray multilayer optics fabrication facilities at Indus synchrotrons complex. The facilities are regularly used for fabrication of high quality x-ray multilayer structures. The results on two representative materials combination of Mo/Si and W/B4C are presented. In Mo/Si multilayer system, we have achieved ˜70% of reflectivity (near normal incidence angle) at soft x-ray region. Large area (300mm×50mm) Mo/Si multilayers are also successively fabricated for monochromator application in hard x-ray region. Whereas in W/B4C system, we demonstrate the capability of these facilities to fabricate ultra short period multilayer (periodicity ˜15-20 Å) with large number of layer pairs in the range of 200-400 for transmission polarizer near Fe L-edge and for monochromator application in hard x-ray region. Hard x-ray reflectivity of ˜54% is achieved from W/B4C MLs with periodicity ˜20 Å and number of layer pairs 300.

  17. SYNCHROTRON X-RAY BASED CHARACTERIZATION OF CDZNTE CRYSTALS

    SciTech Connect

    Duff, M

    2006-09-28

    Synthetic CdZnTe or 'CZT' crystals can be used for the room temperature-based detection of {gamma}-radiation. Structural/morphological heterogeneities within CZT, such as twinning, inclusions, and polycrystallinity can affect detector performance. We used a synchrotron-based X-ray technique, specifically extended X-ray absorption fine-structure (EXAFS) spectroscopy, to determine whether there are differences on a local structural level between intact CZT of high and low radiation detector performance. These studies were complemented by data on radiation detector performance and transmission IR imaging. The EXAFS studies revealed no detectable local structural differences between the two types of CZT materials.

  18. Three-dimensional characterization of electrodeposited lithium microstructures using synchrotron X-ray phase contrast imaging.

    PubMed

    Eastwood, David S; Bayley, Paul M; Chang, Hee Jung; Taiwo, Oluwadamilola O; Vila-Comamala, Joan; Brett, Daniel J L; Rau, Christoph; Withers, Philip J; Shearing, Paul R; Grey, Clare P; Lee, Peter D

    2015-01-01

    The electrodeposition of metallic lithium is a major cause of failure in lithium batteries. The 3D microstructure of electrodeposited lithium 'moss' in liquid electrolytes has been characterised at sub-micron resolution for the first time. Using synchrotron X-ray phase contrast imaging we distinguish mossy metallic lithium microstructures from high surface area lithium salt formations by their contrasting X-ray attenuation. PMID:24898258

  19. Synchrotron x-ray scattering studies of rapidly evolving nanoscale interfacial systems

    NASA Astrophysics Data System (ADS)

    Dai, Yeling

    In light of the development of third-generation synchrotron sources which deliver extremely bright radiation beam over a board energy band, tremendous progress has been made in x-ray science and the diverse range of disciplines that can be studied with x-ray. The special properties of synchrotron-produced x-ray such as coherence, polarization, etc., combined with different extreme experimental conditions, can meet almost any requirement of the research for material characterization, imaging, molecular dynamics, surface/interface physics and so on. In this work we will demonstrate how outstanding properties of synchrotron x-ray can be use to study the structural and dynamic properties of rapidly evolving nano-scale interfacial systems. A large part of this thesis is devoted to the investigation of the surface capillary fluctuations of laterally confined supported polystyrene films using x-ray photon correlation spectroscopy (XPCS), a young coherent scattering technique that can probes the dynamics of matter. The structural evolution of interfacial/surface system, such as the self-assembled nanoparticle film at water-air interface and the nano-imprinted polystyrene pattern, can be studied by different time-resolved x-ray small angle scattering techniques in grazing incidence geometry (GISAXS,GIXOS,GID), as well as the conventional specular reflectivity (XR) measurement. Particularly in the case of the liquid surface research, special efforts have been made to improve a recently developed diffuse scattering technique Grazing incidence off-specular x-ray scattering (GIXOS) for probing the structure at liquid interface with much better temporal resolution compared with that of XR. In this work We will present all the experimental results together with conclusive data analysis from the studies of these evolving systems with x-ray scattering techniques. In comparison to the reciprocal space studies with x-ray scattering tools, part of this thesis is devoted to the

  20. Synchrotron x-ray reflectivity study of oxidation/passivation of copper and silicon.

    SciTech Connect

    Chu, Y.; Nagy, Z.; Parkhutik, V.; You, H.

    1999-07-21

    Synchrotron x-ray-scattering technique studies of copper and silicon electrochemical interfaces are reported. These two examples illustrate the application of synchrotron x-ray techniques for oxidation, passivation, and dissolution of metals and semiconductors.

  1. Note: Dynamic strain field mapping with synchrotron X-ray digital image correlation

    SciTech Connect

    Lu, L.; Fan, D.; Luo, S. N.; Bie, B. X.; Ran, X. X.; Qi, M. L.; Parab, N.; Sun, J. Z.; Liao, H. J.; Hudspeth, M. C.; Claus, B.; Fezzaa, K.; Sun, T.; Chen, W.; Gong, X. L.

    2014-07-15

    We present a dynamic strain field mapping method based on synchrotron X-ray digital image correlation (XDIC). Synchrotron X-ray sources are advantageous for imaging with exceptional spatial and temporal resolutions, and X-ray speckles can be produced either from surface roughness or internal inhomogeneities. Combining speckled X-ray imaging with DIC allows one to map strain fields with high resolutions. Based on experiments on void growth in Al and deformation of a granular material during Kolsky bar/gas gun loading at the Advanced Photon Source beamline 32ID, we demonstrate the feasibility of dynamic XDIC. XDIC is particularly useful for dynamic, in-volume, measurements on opaque materials under high strain-rate, large, deformation.

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

    SciTech Connect

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

    2011-07-01

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

  3. Calcified-tissue investigations using synchrotron x-ray microscopy

    SciTech Connect

    Jones, K.W.; Spanne, P.; Schidlovsky, G.; Dejun, X. ); Bockman, R.S. . Medical Coll.); Rabinowitz, M.B. ); Hammond, P.B.; Bornschein, R.L. ); Hoeltzel, D.A. )

    1990-10-01

    Synchrotron x-ray microscopy (SXRM) in both emission and absorption modes has been used to examine elemental distributions in specimens of rat tibia, human deciduous teeth, and an orthopedic implant phantom. The work was performed with a spatial resolution of 8 {mu}m for the emission work and 25 {mu}m for the absorption work. The results illustrate the usefulness of SXRM for measurements of different types of calcified tissue. 3 figs.

  4. Ray tracing homogenizing mirrors for synchrotron x-ray lithography

    NASA Astrophysics Data System (ADS)

    Homer, Michael; Rosser, Roy J.; Speer, R. J.

    1991-12-01

    Saddle toroid array mirrors (STAMs) are novel grazing-incidence mirrors. They have been proposed as the optical component that most efficiently matches synchrotron orbital radiation (SOR) to the needs of proximity x-ray lithography. However, STAMs have yet to be accepted by the synchrotron lithography community because of the lack of detailed data on their expected performance, due primarily to the difficulty of raytracing such mirrors using existing optical raytrace programs. A raytracing package written especially to study the design and optimization of these unusually shaped mirrors and the very encouraging results obtained with the package to date are described. The optimum STAM designs turn out to be the most effective way of homogeneously illuminating a rectangular proximity x-ray lithography mask, improving on existing scanning mirror systems by at least a factor of four. They have the added advantage of being stationary, which should lead to greater reliability--a quality of considerable value in the production environment these mirrors are intended for, namely the ultra-high vacuum of a synchrotron beamline. Based on the results of the raytracing, a prototype STAM has been constructed, and preparations are being made for an x-ray test of the device.

  5. High counting rates of x-ray photon detection using APD detectors on synchrotron machines

    SciTech Connect

    Kakuno, E. M.; Giacomolli, B. A.; Scorzato, C. R.

    2012-05-17

    In this work we show the results of 10 x 10 mm{sup 2} Si-APD detector's test with guard ring detecting x-rays. The result of mapping surface is also exhibited. We show and discuss the difficulty of single photon detection in high counting rate experiments in synchrotrons machines.

  6. X-ray diffraction microtomography using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Barroso, R. C.; Lopes, R. T.; de Jesus, E. F. O.; Oliveira, L. F.

    2001-09-01

    The X-ray diffraction computed tomography technique is based on the interference phenomena of the coherent scatter. For low-momentum transfer, it is most probable that the scattering interaction will be coherent. A selective discrimination of a given element in a scanned specimen can be realized by fixing the Bragg angle which produces an interference peak and then, to carry out the computed tomography in the standard mode. The image reconstructed exalts the presence of this element with respect to other ones in a sample. This work reports the feasibility of a non-destructive synchrotron radiation X-ray diffraction imaging technique. This research was performed at the X-ray Diffraction beam line of the National Synchrotron Light Laboratory (LNLS) in Brazil. The coherent scattering properties of different tissue and bone substitute materials were evaluated. Furthermore, diffraction patterns of some polycrystalline solids were studied due to industrial and environmental human exposure to these metals. The obtained diffraction patterns form the basis of a selective tomography technique. Preliminary images are presented.

  7. Synchrotron X-ray Enhanced Scanning Tunneling Microscopy

    NASA Astrophysics Data System (ADS)

    Rose, Volker; Freeland, John

    2011-03-01

    Proper understanding of complex phenomena occurring in nanostructures requires tools with both the ability to resolve the nanometer scale as well as provide detailed information about chemical, electronic, and magnetic structure. Scanning tunneling microscopy (STM) achieves the requisite high spatial resolution; however, direct elemental determination is not easily accomplished. X-ray microscopies, on the other hand, provide elemental selectivity, but currently have spatial resolution only of tens of nanometers. We present a novel and radically different concept that employs detection of local synchrotron x-ray interactions utilizing a STM that provides spatial resolution, and x-ray absorption directly yields chemical, electronic, and magnetic sensitivity. If during tunneling the sample is simultaneously illuminated with monochromatic x-rays, characteristic absorption will arise. Electrons that are excited into unoccupied levels close to the Fermi level modulate the tunneling current giving rise to elemental contrast. This work was supported by the U. S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under contract DE-AC02-06CH11357.

  8. Miniature pulsed magnet system for synchrotron x-ray measurements

    SciTech Connect

    Linden, Peter J. E. M. van der; Mathon, Olivier; Strohm, Cornelius; Sikora, Marcin

    2008-07-15

    We have developed a versatile experimental apparatus for synchrotron x-ray measurements in pulsed high magnetic fields. The apparatus consists of a double cryostat incorporating a liquid nitrogen bath to cool the miniature pulsed coil and an independent helium flow cryostat allowing sample temperatures from 4 up to 250 K. The high duty cycle miniature pulsed coils can generate up to 38 T. During experiments at 30 T a repetition rate of 6 pulses/min was routinely reached. Using a 4 kJ power supply, the pulse duration was between 500 {mu}s and 1 ms. The setup was used for nuclear forward scattering measurements on {sup 57}Fe up to 25 T on the ESRF beamline ID18. In another experiment, x-ray magnetic circular dichroism was measured up to 30 T on the ESRF energy dispersive beamline ID24.

  9. Fabrication of nested elliptical KB mirrors using profile coating for synchrotron radiation X-ray focusing

    SciTech Connect

    Liu, Chian; Ice, Gene E; Liu, Wenjun; Assoufid, Lahsen; Qian, J; Shi, B.; Khachatryan, Ruben; Wieczorek, M.; Zschack, P.; Tischler, Jonathan Zachary

    2012-01-01

    This paper describes fabrication methods used to demonstrate the advantages of nested or Montel optics for micro/nanofocusing of synchrotron X-ray beams. A standard Kirkpatrick-Baez (KB) mirror system uses two separated elliptical mirrors at glancing angles to the X-ray beam and sequentially arranged at 90{sup o} to each other to focus X-rays successively in the vertical and horizontal directions. A nested KB mirror system has the two mirrors positioned perpendicular and side-by-side to each other. Compared to a standard KB mirror system, Montel optics can focus a larger divergence and the mirrors can have a shorter focal length. As a result, nested mirrors can be fabricated with improved demagnification factor and ultimately smaller focal spot, than with a standard KB arrangement. The nested system is also more compact with an increased working distance, and is more stable, with reduced complexity of mirror stages. However, although Montel optics is commercially available for laboratory X-ray sources, due to technical difficulties they have not been used to microfocus synchrotron radiation X-rays, where ultra-precise mirror surfaces are essential. The main challenge in adapting nested optics for synchrotron microfocusing is to fabricate mirrors with a precise elliptical surface profile at the very edge where the two mirrors meet and where X-rays scatter. For example, in our application to achieve a sub-micron focus with high efficiency, a surface figure root-mean-square (rms) error on the order of 1 nm is required in the useable area along the X-ray footprint with a {approx} 0.1 mm-diameter cross section. In this paper we describe promising ways to fabricate precise nested KB mirrors using our profile coating technique and inexpensive flat Si substrates.

  10. Contrasting of biological samples for X-ray synchrotron microtomography.

    PubMed

    Efimova, O I; Khlebnikov, A S; Senin, R A; Voronin, P A; Anokhin, K V

    2013-08-01

    The method of contrasting with iodine ions was developed to obtain high-resolution 3D images of large biological specimens using a synchrotron X-ray microtomography unit. It was shown that the samples (late mouse embryos) treated with 50% Lugol solution with addition of 25% ethanol for 48 h followed by a 48-h washout in phosphate buffered saline had maximum contrast and lowest compression artifacts. Processing of samples by this protocol allowed detecting zones of active proliferation. Incubation of brain samples for 120 h in 7.6% meglumine/sodium diatrizoate without washout ensured the best contrast during myelin identification. PMID:24143358

  11. Synchrotron Area X-ray Detectors, Present and Future

    SciTech Connect

    Gruner, Sol M.

    2010-06-23

    X-ray experiments are very frequently detector limited at today's storage ring synchrotron radiation (SR) sources, and will be even more so at future Energy Recovery Linac and X-ray Free Electron Laser sources. Image plate and phosphor-coupled CCD detectors that predominate at present-day sources were outgrowths of technologies initially developed for the medical and astronomical communities, respectively, with resultant limitations for SR. These limitations are enumerated. The growth of commercial silicon foundries and design tools enabling the production of large, customized integrated circuits is beginning to have a profound impact on SR detectors and is ushering in the age of 'designer detectors'. Novel area Pixel Array Detectors (PADs) are starting to appear in which each pixel has dedicated, complex circuitry capable of high speed and, in some cases, significant data processing power for specific applications. PADs now at, or near the horizon will be described. Integrated circuit methods continue to develop at a rapid pace. Implications for future x-ray detectors will be discussed.

  12. On-Line Mirror Surfacing Monitored by X-ray Shearing Interferometry and X-ray Scattering

    SciTech Connect

    Ziegler, E.; Peverini, L.; Kozhevnikov, I. V.; Weitkamp, T.; David, C.

    2007-01-19

    We propose a novel fabrication scheme combining a mirror surfacing tool and an on-line metrology instrument, the latter capable of controlling both figure and finish of an X-ray mirror with an accuracy matching the challenging specifications of nanofocusing reflective optics for synchrotron and FEL X-ray beams. This approach will be complementary to the present technologies. The paper reviews some recent achievements and presents pertinent examples of on-line diagnostics performed at the ESRF BM05 beamline for which X-rays prove to be a unique probe.

  13. Synchrotron x-ray photoemission study of soft x-ray processed ultrathin glycine-water ice films

    SciTech Connect

    Tzvetkov, George; Netzer, Falko P.

    2011-05-28

    Ultrathin glycine-water ice films have been prepared in ultrahigh vacuum by condensation of H{sub 2}O and glycine at 90 K on single crystalline alumina surfaces and processed by soft x-ray (610 eV) exposure for up to 60 min. The physicochemical changes in the films were monitored using synchrotron x-ray photoemission spectroscopy. Two films with different amounts of H{sub 2}O have been considered in order to evaluate the influence of the water ice content on the radiation-induced effects. The analysis of C1s, N1s, and O1s spectral regions together with the changes in the valence band spectra indicates that amino acid degradation occurs fast mainly via decarboxylation and deamination of pristine molecules. Enrichment of the x-ray exposed surfaces with fragments with carbon atoms without strong electronegative substituents (C-C and C-H) is documented as well. In the thinner glycine-water ice film (six layers of glycine + six layers of water) the 3D ice suffers strongly from the x-rays and is largely removed from the sample. The rate of photodecomposition of glycine in this film is about 30% higher than for glycine in the thicker film (6 layers of glycine + 60 layers of water). The photoemission results suggest that the destruction of amino acid molecules is caused by the direct interaction with the radiation and that no chemical attack of glycine by the species released by water radiolysis is detected.

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

    PubMed

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

    2012-08-01

    We present an experimental setup for the simultaneous measurement of surface plasmon resonance (SPR) and x-ray absorption spectroscopy (XAS) on metallic thin films at a synchrotron beamline. The system allows measuring in situ and in real time the effect of x-ray irradiation on the SPR curves to explore the interaction of x-rays with matter. It is also possible to record XAS spectra while exciting SPR in order to study changes in the films induced by the excitation of surface plasmons. Combined experiments recording simultaneously SPR and XAS curves while scanning different parameters can be also carried out. The relative variations in the SPR and XAS spectra that can be detected with this setup range from 10(-3) to 10(-5), depending on the particular experiment. PMID:22938268

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

    SciTech Connect

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

    2012-08-15

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

  16. Anomalous X-ray diffraction with soft X-ray synchrotron radiation.

    PubMed

    Carpentier, P; Berthet-Colominas, C; Capitan, M; Chesne, M L; Fanchon, E; Lequien, S; Stuhrmann, H; Thiaudière, D; Vicat, J; Zielinski, P; Kahn, R

    2000-07-01

    Anomalous diffraction with soft X-ray synchrotron radiation opens new possibilities in protein crystallography and materials science. Low-Z elements like silicon, phosphorus, sulfur and chlorine become accessible as new labels in structural studies. Some of the heavy elements like uranium exhibit an unusually strong dispersion at their M(V) absorption edge (lambdaMV = 3.497 A, E(MV) = 3545 eV) and so does thorium. Two different test experiments are reported here showing the feasibility of anomalous X-ray diffraction at long wavelengths with a protein containing uranium and with a salt containing chlorine atoms. With 110 electrons the anomalous scattering amplitude of uranium exceeds by a factor of 4 the resonance scattering of other strong anomalous scatterers like that of the lanthanides at their L(III) edge. The resulting exceptional phasing power of uranium is most attractive in protein crystallography using the multi-wavelength anomalous diffraction (MAD) method. The anomalous dispersion of an uranium derivative of asparaginyl-tRNA synthetase (hexagonal unit cell; a = 123.4 A, c = 124.4 A) has been measured for the first time at 4 wavelengths near the M(V) edge using the beamline ID1 of ESRF (Grenoble, France). The present set up allowed to measure only 30% of the possible reflections at a resolution of 4 A, mainly because of the low sensitivity of the CCD detector. In the second experiment, the dispersion of the intensity of 5 X-ray diffraction peaks from pentakismethylammonium undecachlorodibismuthate (PMACB, orthorhombic unit cell; a = 13.003 A, b = 14.038 A, c = 15.450 A) has been measured at 30 wavelengths near the K absorption edge of chlorine (lambdaK = 4.397 A, EK= 2819.6 eV). All reflections within the resolution range from 6.4 A to 3.4 A expected in the 20 degree scan were observed. The chemical state varies between different chlorine atoms of PMACB, and so does the dispersion of different Bragg peaks near the K-edge of chlorine. The results reflect

  17. Synchrotron X-ray diffraction characterization of healthy and fluorotic human dental enamel

    NASA Astrophysics Data System (ADS)

    Colaço, M. V.; Barroso, R. C.; Porto, I. M.; Gerlach, R. F.; Costa, F. N.; Braz, D.; Droppa, R.; de Sousa, F. B.

    2012-10-01

    With the introduction of fluoride as the main anticaries agent used in preventive dentistry, and perhaps an increase in fluoride in our food chain, dental fluorosis has become an increasing world-wide problem. Visible signs of fluorosis begin to become obvious on the enamel surface as opacities, implying some porosity in the tissue. The mechanisms that conduct the formation of fluorotic enamel are unknown, but should involve modifications in the basic physical-chemistry reactions of demineralization and remineralisation of the enamel of the teeth, which is the same reaction of formation of the enamel's hydroxyapatite (HAp) in the maturation phase. The increase of the amount of fluoride inside of the apatite will result in gradual increase of the lattice parameters. The aim of this work is to characterize the healthy and fluorotic enamel in human tooth using Synchrotron X-ray diffraction. All the scattering profile measurements were carried out at the X-ray diffraction beamline (XRD1) at the Brazilian Synchrotron Light Laboratory—LNLS, Campinas, Brazil. X-ray diffraction experiments were performed both in powder samples and polished surfaces. The powder samples were analyzed to obtain the characterization of a typical healthy enamel pattern. The polished surfaces were analyzed in specific areas that have been identified as fluorotic ones. X-ray diffraction data were obtained for all samples and these data were compared with the control samples and also with the literature data.

  18. The first microbeam synchrotron X-ray fluorescence beamline at the Siam Photon Laboratory.

    PubMed

    Tancharakorn, Somchai; Tanthanuch, Waraporn; Kamonsutthipaijit, Nuntaporn; Wongprachanukul, Narupon; Sophon, Methee; Chaichuay, Sarunyu; Uthaisar, Chunmanus; Yimnirun, Rattikorn

    2012-07-01

    The first microbeam synchrotron X-ray fluorescence (µ-SXRF) beamline using continuous synchrotron radiation from Siam Photon Source has been constructed and commissioned as of August 2011. Utilizing an X-ray capillary half-lens allows synchrotron radiation from a 1.4 T bending magnet of the 1.2 GeV electron storage ring to be focused from a few millimeters-sized beam to a micrometer-sized beam. This beamline was originally designed for deep X-ray lithography (DXL) and was one of the first two operational beamlines at this facility. A modification has been carried out to the beamline in order to additionally enable µ-SXRF and synchrotron X-ray powder diffraction (SXPD). Modifications included the installation of a new chamber housing a Si(111) crystal to extract 8 keV synchrotron radiation from the white X-ray beam (for SXPD), a fixed aperture and three gate valves. Two end-stations incorporating optics and detectors for µ-SXRF and SXPD have then been installed immediately upstream of the DXL station, with the three techniques sharing available beam time. The µ-SXRF station utilizes a polycapillary half-lens for X-ray focusing. This optic focuses X-ray white beam from 5 mm × 2 mm (H × V) at the entrance of the lens down to a diameter of 100 µm FWHM measured at a sample position 22 mm (lens focal point) downstream of the lens exit. The end-station also incorporates an XYZ motorized sample holder with 25 mm travel per axis, a 5× ZEISS microscope objective with 5 mm × 5 mm field of view coupled to a CCD camera looking to the sample, and an AMPTEK single-element Si (PIN) solid-state detector for fluorescence detection. A graphic user interface data acquisition program using the LabVIEW platform has also been developed in-house to generate a series of single-column data which are compatible with available XRF data-processing software. Finally, to test the performance of the µ-SXRF beamline, an elemental surface profile has been obtained for

  19. Synchrotron x-ray sources and new opportunities in the soil and environmental sciences

    SciTech Connect

    Schulze, D. ); Anderson, S. ); Mattigod, S. )

    1990-07-01

    This report contains the following papers: characteristics of the advanced photon source and comparison with existing synchrotron facilities; x-ray absorption spectroscopy: EXAFS and XANES -- A versatile tool to study the atomic and electronic structure of materials; applications of x-ray spectroscopy and anomalous scattering experiments in the soil and environmental sciences; X-ray fluorescence microprobe and microtomography.

  20. High pressure x-ray diffraction techniques with synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Jing, Liu

    2016-07-01

    This article summarizes the developments of experimental techniques for high pressure x-ray diffraction (XRD) in diamond anvil cells (DACs) using synchrotron radiation. Basic principles and experimental methods for various diffraction geometry are described, including powder diffraction, single crystal diffraction, radial diffraction, as well as coupling with laser heating system. Resolution in d-spacing of different diffraction modes is discussed. More recent progress, such as extended application of single crystal diffraction for measurements of multigrain and electron density distribution, time-resolved diffraction with dynamic DAC and development of modulated heating techniques are briefly introduced. The current status of the high pressure beamline at BSRF (Beijing Synchrotron Radiation Facility) and some results are also presented. Project supported by the National Natural Science Foundation of China (Grant Nos. 10875142, 11079040, and 11075175). The 4W2 beamline of BSRF was supported by the Chinese Academy of Sciences (Grant Nos. KJCX2-SW-N20, KJCX2-SW-N03, and SYGNS04).

  1. Synchrotron X-ray CT characterization of titanium parts fabricated by additive manufacturing. Part I. Morphology.

    PubMed

    Scarlett, Nicola Vivienne Yorke; Tyson, Peter; Fraser, Darren; Mayo, Sheridan; Maksimenko, Anton

    2016-07-01

    Synchrotron X-ray tomography has been applied to the study of titanium parts fabricated by additive manufacturing (AM). The AM method employed here was the Arcam EBM(®) (electron beam melting) process which uses powdered titanium alloy, Ti64 (Ti alloy with approximately 6%Al and 4%V), as the feed and an electron beam for the sintering/welding. The experiment was conducted on the Imaging and Medical Beamline of the Australian Synchrotron. Samples were chosen to examine the effect of build direction and complexity of design on the surface morphology and final dimensions of the piece. PMID:27359150

  2. Surface-Enhanced X-Ray Fluorescence

    NASA Technical Reports Server (NTRS)

    Anderson, Mark

    2010-01-01

    Surface-enhanced x-ray fluorescence (SEn-XRF) spectroscopy is a form of surface- enhanced spectroscopy that was conceived as a means of obtaining greater sensitivity in x-ray fluorescence (XRF) spectroscopy. As such, SEn-XRF spectroscopy joins the ranks of such other, longer-wavelength surface-enhanced spectroscopies as those based on surface-enhanced Raman scattering (SERS), surface-enhanced resonance Raman scattering (SERRS), and surfaceenhanced infrared Raman absorption (SEIRA), which have been described in previous NASA Tech Briefs articles. XRF spectroscopy has been used in analytical chemistry for determining the elemental compositions of small samples. XRF spectroscopy is rapid and quantitative and has been applied to a variety of metal and mineralogical samples. The main drawback of XRF spectroscopy as practiced heretofore is that sensitivity has not been as high as required for some applications. In SEn-XRF as in the other surface-enhanced spectroscopies, one exploits several interacting near-field phenomena, occurring on nanotextured surfaces, that give rise to local concentrations of incident far-field illumination. In this case, the far-field illumination comes from an x-ray source. Depending on the chemical composition and the geometry of a given nanotextured surface, these phenomena could include the lightning-rod effect (concentration of electric fields at the sharpest points on needlelike surface features), surface plasmon resonances, and grazing incidence geometric effects. In the far field, the observable effect of these phenomena is an increase in the intensity of the spectrum of interest - in this case, the x-ray fluorescence spectrum of chemical elements of interest that may be present within a surface layer at distances no more than a few nanometers from the surface.

  3. Synchrotron X-ray microtomographic study of tablet swelling.

    PubMed

    Laity, P R; Cameron, R E

    2010-06-01

    Tablet swelling behaviour was investigated by following the movements of embedded glass microsphere tracers, using X-ray microtomography (XmicroT) with intense illumination from a synchrotron. Specimens were prepared using combinations of hydroxypropyl-methyl-cellulose (HPMC) and microcrystalline cellulose (MCC) or pre-gelatinised starch (PGS), three materials commonly used as excipients for compacted tablets. The results revealed significant differences in swelling behaviour due to excipient type and compaction conditions. In particular, a sudden change was observed from gel-forming behaviour of formulations containing PGS or high HPMC content, to more rapid expansion and disintegration for formulations above 70% MCC. Although some radial expansion was observable with the higher PGS formulations and during later stages of swelling, axial expansion (i.e. the reverse of the compaction process) appeared to dominate in most cases. This was most pronounced for the 10/90 HPMC/MCC specimens, which rapidly increased in thickness, while the diameter remained almost unchanged. The expansion appeared to be initiated by hydration and may be due to the relaxation of residual compaction stress. This occurred within 'expansion zones', which initially appeared as thin bands close to the compacted (upper and lower) faces, but gradually advanced towards the centre and spread around the sides of the tablets. These zones exhibited lower X-ray absorbance, probably because they contained significant amounts of bubbles, which were formed by air released from the swelling excipients. Although, in most cases, these bubbles were too small to be resolved (<60 microm), larger bubbles (diameter up to 1mm) were clearly evident in the rapidly swelling 10/90 HPMC/MCC specimens. It is suggested that the presence of these bubbles may affect subsequent water ingress, by increasing the tortuosity and occluding part of the gel, which may affect the apparent diffusion kinetics (i.e. Fickian or Case II

  4. Geoscience Applications of Synchrotron X-ray Computed Microtomography

    NASA Astrophysics Data System (ADS)

    Rivers, M. L.

    2009-05-01

    Computed microtomography is the extension to micron spatial resolution of the CAT scanning technique developed for medical imaging. Synchrotron sources are ideal for the method, since they provide a monochromatic, parallel beam with high intensity. High energy storage rings such as the Advanced Photon Source at Argonne National Laboratory produce x-rays with high energy, high brilliance, and high coherence. All of these factors combine to produce an extremely powerful imaging tool for earth science research. Techniques that have been developed include: - Absorption and phase contrast computed tomography with spatial resolution approaching one micron - Differential contrast computed tomography, imaging above and below the absorption edge of a particular element - High-pressure tomography, imaging inside a pressure cell at pressures above 10GPa - High speed radiography, with 100 microsecond temporal resolution - Fluorescence tomography, imaging the 3-D distribution of elements present at ppm concentrations. - Radiographic strain measurements during deformation at high confining pressure, combined with precise x- ray diffraction measurements to determine stress. These techniques have been applied to important problems in earth and environmental sciences, including: - The 3-D distribution of aqueous and organic liquids in porous media, with applications in contaminated groundwater and petroleum recovery. - The kinetics of bubble formation in magma chambers, which control explosive volcanism. - Accurate crystal size distributions in volcanic systems, important for understanding the evolution of magma chambers. - The equation-of-state of amorphous materials at high pressure using both direct measurements of volume as a function of pressure and also by measuring the change x-ray absorption coefficient as a function of pressure. - The formation of frost flowers on Arctic sea-ice, which is important in controlling the atmospheric chemistry of mercury. - The distribution of

  5. K-Edge Subtraction Angiography with Synchrotron X-Rays

    SciTech Connect

    Giacomini, John C.

    1996-12-31

    The purpose of this project was to utilize dual energy, monochromatic X-rays produced from synchrotrons radiation in order to obtain noninvasive medical imaging. The application of synchrotrons radiation to medical imaging is based on the principle of iodine dichromography, first described by Bertil Jacobson of the Karolinska Institute in 1953. Medical imaging using synchrotrons radiation and K-edge dichromography was pioneered at Stanford University under the leadership of Dr. Ed Rubenstein, and the late Nobel Laureate in Physics, Dr. Robert Hofstadter. With progressive refinements in hardware, clinical-quality images were obtained of human coronary arteries utilizing peripheral injections of iodinated contrast agent. These images even now are far superior to those being presented by investigators using MRI as an imaging tool for coronary arteries. However, new supplies and instruments in the cardiac catheterization laboratory have served to transform coronary angiography into an outpatient procedure, with relatively little morbidity. We extended the principles learned with coronary angiography to noninvasive imaging of the human bronchial tree. For these images, we utilized xenon as the contrast agent, as it has a K-edge very similar to that of iodine. In this case, there is no true competing diagnostic test, and pulmonary neoplasm is an enormous public health concern. In early experiments, we demonstrated remarkably clear images of the human bronchial tree. These images have been shown internationally; however, funding difficulties primarily with the Department of Energy have not allowed for progression of this promising avenue of research. One potential criticism of the project is that in order to obtain these images, we utilized national laboratories. Some have questioned whether this would lead to a practical imaging modality. However, we have shown that the technology exists to allow for construction of a miniature storage ring, with a superconducting

  6. CH 3Cl adsorption on a Si(100)2 × 1 surface modified by alkali metal overlayer studied by soft X-ray photoemission using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Gentle, T. M.; Soukiassian, P.; Schuette, K. P.; Bakshi, M. H.; Hurych, Z.

    1988-08-01

    We present the first study of the effect of an alkali metal overlayer on the adsorption of an organic molecule, methylchloride, on a Si(100)2 × 1 surface. In strong contrast to the behavior of molecular oxygen or nitrogen which were found to react with the silicon substrate, there was no significant interaction between methylchloride and silicon, rather, the formation of alkali-chlorine bonds was observed. Core level and valence band spectroscopies using synchrotron radiation were used to study these systems. Sodium was found to exhibit the strongest interaction with mehtylchloride which was dissociated, while the effects produced by K and Cs were weaker.

  7. Microbial biofilm study by synchrotron X-ray microscopy

    NASA Astrophysics Data System (ADS)

    Pennafirme, S.; Lima, I.; Bitencourt, J. A.; Crapez, M. A. C.; Lopes, R. T.

    2015-11-01

    Microbial biofilm has already being used to remove metals and other pollutants from wastewater. In this sense, our proposal was to isolate and cultivate bacteria consortia from mangrove's sediment resistant to Zn (II) and Cu (II) at 50 mg L-1 and to observe, through synchrotron X-ray fluorescence microscopy (microXRF), whether the biofilm sequestered the metal. The biofilm area analyzed was 1 mm2 and a 2D map was generated (pixel size 20×20 μm2, counting time 5 s/point). The biofilm formation and retention followed the sequence Zn>Cu. Bacterial consortium zinc resistant formed dense biofilm and retained 63.83% of zinc, while the bacterial consortium copper resistant retained 3.21% of copper, with lower biofilm formation. Dehydrogenase activity of Zn resistant bacterial consortium was not negatively affect by 50 mg ml-1 zinc input, whereas copper resistant bacterial consortium showed a significant decrease on dehydrogenase activity (50 mg mL-1 of Cu input). In conclusion, biofilm may protect bacterial cells, acting as barrier against metal toxicity. The bacterial consortia Zn resistant, composed by Nitratireductor spp. and Pseudomonas spp formed dense biofilm and sequestered metal from water, decreasing the metal bioavailability. These bacterial consortia can be used in bioreactors and in bioremediation programs.

  8. Measuring and interpreting X-ray fluorescence from planetary surfaces.

    PubMed

    Owens, Alan; Beckhoff, Burkhard; Fraser, George; Kolbe, Michael; Krumrey, Michael; Mantero, Alfonso; Mantler, Michael; Peacock, Anthony; Pia, Maria-Grazia; Pullan, Derek; Schneider, Uwe G; Ulm, Gerhard

    2008-11-15

    As part of a comprehensive study of X-ray emission from planetary surfaces and in particular the planet Mercury, we have measured fluorescent radiation from a number of planetary analog rock samples using monochromatized synchrotron radiation provided by the BESSY II electron storage ring. The experiments were carried out using a purpose built X-ray fluorescence (XRF) spectrometer chamber developed by the Physikalisch-Technische Bundesanstalt, Germany's national metrology institute. The XRF instrumentation is absolutely calibrated and allows for reference-free quantitation of rock sample composition, taking into account secondary photon- and electron-induced enhancement effects. The fluorescence data, in turn, have been used to validate a planetary fluorescence simulation tool based on the GEANT4 transport code. This simulation can be used as a mission analysis tool to predict the time-dependent orbital XRF spectral distributions from planetary surfaces throughout the mapping phase. PMID:18855420

  9. Synchrotron Radiation from Outer Space and the Chandra X-Ray Observatory

    NASA Technical Reports Server (NTRS)

    Weisskopf, M. C.

    2006-01-01

    The universe provides numerous extremely interesting astrophysical sources of synchrotron X radiation. The Chandra X-ray Observatory and other X-ray missions provide powerful probes of these and other cosmic X-ray sources. Chandra is the X-ray component of NASA's Great Observatory Program which also includes the Hubble Space telescope, the Spitzer Infrared Telescope Facility, and the now defunct Compton Gamma-Ray Observatory. The Chandra X-Ray Observatory provides the best angular resolution (sub-arcsecond) of any previous, current, or planned (for the foreseeable near future) space-based X-ray instrumentation. We present here a brief overview of the technical capability of this X-Ray observatory and some of the remarkable discoveries involving cosmic synchrotron sources.

  10. X-ray absorption spectroscopy of liquid surface

    NASA Astrophysics Data System (ADS)

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

    1997-09-01

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

  11. Fast synchrotron X-ray tomography study of the rod packing structures

    SciTech Connect

    Zhang Xiaodan; Xia Chengjie; Sun Haohua; Wang Yujie

    2013-06-18

    We present a fast synchrotron X-ray tomography study of the packing structures of rods under tapping. Utilizing the high flux of the X-rays generated from the third-generation synchrotron source, we can complete a tomography scan within several seconds, after which the three-dimensional (3D) packing structure can be obtained for the subsequent structural analysis. Due to the high-energy nature of the X-ray beam, special image processing steps including image phase-retrieval has been implemented. Overall, this study suggests the possibility of acquiring statistically significant static packing structures within a reasonable time scale using high-intensity X-ray sources.

  12. Combined synchrotron X-ray tomography and X-ray powder diffraction using a fluorescing metal foil

    SciTech Connect

    Kappen, P.; Arhatari, B. D.; Luu, M. B.; Balaur, E.; Caradoc-Davies, T.

    2013-06-15

    This study realizes the concept of simultaneous micro-X-ray computed tomography and X-ray powder diffraction using a synchrotron beamline. A thin zinc metal foil was placed in the primary, monochromatic synchrotron beam to generate a divergent wave to propagate through the samples of interest onto a CCD detector for tomographic imaging, thus removing the need for large beam illumination and high spatial resolution detection. Both low density materials (kapton tubing and a piece of plant) and higher density materials (Egyptian faience) were investigated, and elemental contrast was explored for the example of Cu and Ni meshes. The viability of parallel powder diffraction using the direct beam transmitted through the foil was demonstrated. The outcomes of this study enable further development of the technique towards in situ tomography/diffraction studies combining micrometer and crystallographic length scales, and towards elemental contrast imaging and reconstruction methods using well defined fluorescence outputs from combinations of known fluorescence targets (elements).

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

    SciTech Connect

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

    1995-06-01

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

  14. Optoelectronic measurement of x-ray synchrotron pulses: A proof of concept demonstration

    SciTech Connect

    Durbin, Stephen M.; Caffee, Marc; Savikhin, Sergei; Mahmood, Aamer; Dufresne, Eric M.; Wen, Haidan; Li, Yuelin

    2013-02-04

    Optoelectronic detection using photoconductive coplanar stripline devices has been applied to measuring the time profile of x-ray synchrotron pulses, a proof of concept demonstration that may lead to improved time-resolved x-ray studies. Laser sampling of current vs time delay between 12 keV x-ray and 800 nm laser pulses reveal the {approx}50 ps x-ray pulse width convoluted with the {approx}200 ps lifetime of the conduction band carriers. For GaAs implanted with 8 MeV protons, a time profile closer to the x-ray pulse width is observed. The protons create defects over the entire depth sampled by the x-rays, trapping the x-ray excited conduction electrons and minimizing lifetime broadening of the electrical excitation.

  15. Synchrotron Vacuum Ultraviolet Light and Soft X-Ray Radiation Effects on Aluminized Teflon FEP Investigated

    NASA Technical Reports Server (NTRS)

    Dever, Joyce A.; Townsend, Jacqueline A.; Gaier, James R.; Jalics, Alice I.

    1999-01-01

    Since the Hubble Space Telescope (HST) was deployed in low Earth orbit in April 1990, two servicing missions have been conducted to upgrade its scientific capabilities. Minor cracking of second-surface metalized Teflon FEP (DuPont; fluorinated ethylene propylene) surfaces from multilayer insulation (MLI) was first observed upon close examination of samples with high solar exposure retrieved during the first servicing mission, which was conducted 3.6 years after deployment. During the second HST servicing mission, 6.8 years after deployment, astronaut observations and photographic documentation revealed significant cracks in the Teflon FEP layer of the MLI on both the solar- and anti-solar-facing surfaces of the telescope. NASA Goddard Space Flight Center directed the efforts of the Hubble Space Telescope MLI Failure Review Board, whose goals included identifying the low-Earth-orbit environmental constituent(s) responsible for the cracking and embrittling of Teflon FEP which was observed during the second servicing mission. The NASA Lewis Research Center provided significant support to this effort. Because soft x-ray radiation from solar flares had been considered as a possible cause for the degradation of the mechanical properties of Teflon FEP (ref. 1), the effects of soft xray radiation and vacuum ultraviolet light on Teflon FEP were investigated. In this Lewisled effort, samples of Teflon FEP with a 100-nm layer of vapor-deposited aluminum (VDA) on the backside were exposed to synchrotron radiation of various vacuum ultraviolet and soft x-ray wavelengths between 18 nm (69 eV) and 0.65 nm (1900 eV). Synchrotron radiation exposures were conducted using the National Synchrotron Light Source at Brookhaven National Laboratory. Samples of FEP/VDA were exposed with the FEP surface facing the synchrotron beam. Doses and fluences were compared with those estimated for the 20-yr Hubble Space Telescope mission.

  16. Recent advances in X-ray nanolithography using synchrotron radiation at Super-ACO

    NASA Astrophysics Data System (ADS)

    Rousseaux, F.; Chen, Y.; Haghiri-Gosnet, A. M.; Launois, H.

    1995-02-01

    This paper describes our recent advances in high resolution synchrotron radiation lithography. Fabrication processes of high resolution X-ray masks based on our current {SiC}/{W} technology have been optimized to be compatible with a commercial Karl Süss stepper. As a result, well defined 50 nm wide isolated lines and small gratings of period down to 100 nm have been fabricated and tested in proximity X-ray lithography with the stepper. Replication tests were done with a minimum gap setting down to 5 μm. Results show that proximity X-ray lithography using synchrotron radiation is a viable technology for printing 50 nm linewidth features.

  17. X-ray phase-contrast tomography with a compact laser-driven synchrotron source

    PubMed Central

    Eggl, Elena; Schleede, Simone; Bech, Martin; Achterhold, Klaus; Loewen, Roderick; Ruth, Ronald D.; Pfeiffer, Franz

    2015-01-01

    Between X-ray tubes and large-scale synchrotron sources, a large gap in performance exists with respect to the monochromaticity and brilliance of the X-ray beam. However, due to their size and cost, large-scale synchrotrons are not available for more routine applications in small and medium-sized academic or industrial laboratories. This gap could be closed by laser-driven compact synchrotron light sources (CLS), which use an infrared (IR) laser cavity in combination with a small electron storage ring. Hard X-rays are produced through the process of inverse Compton scattering upon the intersection of the electron bunch with the focused laser beam. The produced X-ray beam is intrinsically monochromatic and highly collimated. This makes a CLS well-suited for applications of more advanced––and more challenging––X-ray imaging approaches, such as X-ray multimodal tomography. Here we present, to our knowledge, the first results of a first successful demonstration experiment in which a monochromatic X-ray beam from a CLS was used for multimodal, i.e., phase-, dark-field, and attenuation-contrast, X-ray tomography. We show results from a fluid phantom with different liquids and a biomedical application example in the form of a multimodal CT scan of a small animal (mouse, ex vivo). The results highlight particularly that quantitative multimodal CT has become feasible with laser-driven CLS, and that the results outperform more conventional approaches. PMID:25902493

  18. X-ray phase-contrast tomography with a compact laser-driven synchrotron source.

    PubMed

    Eggl, Elena; Schleede, Simone; Bech, Martin; Achterhold, Klaus; Loewen, Roderick; Ruth, Ronald D; Pfeiffer, Franz

    2015-05-01

    Between X-ray tubes and large-scale synchrotron sources, a large gap in performance exists with respect to the monochromaticity and brilliance of the X-ray beam. However, due to their size and cost, large-scale synchrotrons are not available for more routine applications in small and medium-sized academic or industrial laboratories. This gap could be closed by laser-driven compact synchrotron light sources (CLS), which use an infrared (IR) laser cavity in combination with a small electron storage ring. Hard X-rays are produced through the process of inverse Compton scattering upon the intersection of the electron bunch with the focused laser beam. The produced X-ray beam is intrinsically monochromatic and highly collimated. This makes a CLS well-suited for applications of more advanced--and more challenging--X-ray imaging approaches, such as X-ray multimodal tomography. Here we present, to our knowledge, the first results of a first successful demonstration experiment in which a monochromatic X-ray beam from a CLS was used for multimodal, i.e., phase-, dark-field, and attenuation-contrast, X-ray tomography. We show results from a fluid phantom with different liquids and a biomedical application example in the form of a multimodal CT scan of a small animal (mouse, ex vivo). The results highlight particularly that quantitative multimodal CT has become feasible with laser-driven CLS, and that the results outperform more conventional approaches. PMID:25902493

  19. Thermal management of next-generation contact-cooled synchrotron x-ray mirrors

    SciTech Connect

    Khounsary, A.

    1999-10-29

    In the past decade, several third-generation synchrotrons x-ray sources have been constructed and commissioned around the world. Many of the major problems in the development and design of the optical components capable of handling the extremely high heat loads of the generated x-ray beams have been resolved. It is expected, however, that in the next few years even more powerful x-ray beams will be produced at these facilities, for example, by increasing the particle beam current. In this paper, the design of a next generation of synchrotron x-ray mirrors is discussed. The author shows that the design of contact-cooled mirrors capable of handing x-ray beam heat fluxes in excess of 500 W/mm{sup 2} - or more than three times the present level - is well within reach, and the limiting factor is the thermal stress rather then thermally induced slope error.

  20. Development and applications of an epifluorescence module for synchrotron x-ray fluorescence microprobe imaging

    SciTech Connect

    Miller, Lisa M.; Smith, Randy J.; Ruppel, Meghan E.; Ott, Cassandra H.; Lanzirotti, Antonio

    2005-06-15

    Synchrotron x-ray fluorescence (XRF) microprobe is a valuable analysis tool for imaging trace element composition in situ at a resolution of a few microns. Frequently, epifluorescence microscopy is beneficial for identifying the region of interest. To date, combining epifluorescence microscopy with x-ray microprobe has involved analyses with two different microscopes. We report the development of an epifluorescence module that is integrated into a synchrotron XRF microprobe beamline, such that visible fluorescence from a sample can be viewed while collecting x-ray microprobe images simultaneously. This unique combination has been used to identify metal accumulation in Alzheimer's disease plaques and the mineral distribution in geological samples. The flexibility of this accessory permits its use on almost any synchrotron x-ray fluorescence microprobe beamline and applications in many fields of science can benefit from this technology.

  1. X-ray assisted chemical modification of silicon surfaces

    NASA Astrophysics Data System (ADS)

    Pinhero, Patrick Joseph

    Interest in surface photochemistry induced by x-irradiation has received a renaissance with the construction of new synchrotron radiation facilities worldwide. There are three general pathways that a x-ray excited gas-surface system can follow that will lead to reaction. These are: (1) direct excitation, (2) excitation by emitted secondary electrons, and (3) reactions induced by hot electrons at the surface. Two chemical systems are studied in a modified x-ray photoelectron spectrometer (XPS) that allows for reactions to be studied in situ. The systems studied were (1) Nsb2/Si(100) and (2) the SFsb6/Si system. The motivation for studying these two compounds is: they are both relatively inert, i.e. no spontaneous reactions; they both are technologically interesting, possible silicon nitride formation in the case of Nsb2, and SFsb6 is a popular etchant gas in the semiconductor industry; and these two compounds have the potential to exhibit contrasting behavior. Besides its etching qualities, SFsb6 possesses a large x-ray absorption cross section and it has a large electron capture cross section. Both systems are primarily studied by XPS. XPS has the quality of providing quantifiable information about the composition of the surface and details about the chemical environment of each constituent element present. Atomic force microscopy (AFM) is used with the SFsb6 system to observe any structural changes that may occur after reaction. In the Nsb2/Si(100) system, a silicon nitride is formed at very long exposures. This is first observed after 24 hours of simultaneous exposure to Nsb2 and x-irradiation. In the SFsb6 experiments, several subsystems are examined: (1) simultaneous exposure of a Si(100) surface to SFsb6 and x-irradiation at 298K; (2) x-irradiation of a SFsb6 film adsorbed on Si(100) at 100K; (3) simultaneous exposure of a natively oxidized Si surface to SFsb6 and x-rays at 298K; and (4) x-irradiation of a SFsb6 film adsorbed on natively oxidized Si at 100K

  2. Interactions between synchrotron radiation X-ray and biological tissues — theoretical and clinical significance

    PubMed Central

    Chen, Heyu; He, Xin; Sheng, Caibin; Ma, Yingxin; Nie, Hui; Xia, Weiliang; Ying, Weihai

    2011-01-01

    Synchrotron radiation (SR) X-ray has great potential for its applications in both diagnosis and treatment of diseases, due to its characteristic properties including coherence, collimation, monochromaticity, and exceptional brightness. Great advances have been made regarding potential medical applications of SR X-ray in recent years, particularly with the development of the third generation of SR light sources. However, multiple studies have also suggested damaging effects of SR X-ray on biological samples ranging from protein crystals to cells and biological tissues. It has become increasingly important to conduct comprehensive studies on two closely related topics regarding SR X-ray in medical applications: The safety issues regarding the medical applications of SR X-ray and the fundamental mechanisms underlying the interactions between SR X-ray and biological tissues. In this article, we attempted to provide an overview of the literatures regarding these two increasingly significant topics. We also proposed our hypothesis that there are significant differences between the biological tissue-damaging mechanisms of SR X-ray and those of normal X-ray, due to the characteristic properties of SR X-ray such as high dose rate. Future studies are warranted to test this hypothesis, which may profoundly improve our understanding regarding the fundamental mechanisms underlying the interactions between light and matter. These studies would also constitute an essential basis for establishing the safety standard for the medical applications of SR X-ray. PMID:22162780

  3. Synchrotron X-ray measurement techniques for thermal barrier coated cylindrical samples under thermal gradients

    SciTech Connect

    Siddiqui, Sanna F.; Knipe, Kevin; Manero, Albert; Raghavan, Seetha; Meid, Carla; Wischek, Janine; Bartsch, Marion; Okasinski, John; Almer, Jonathan; Karlsson, Anette M.

    2013-08-15

    Measurement techniques to obtain accurate in situ synchrotron strain measurements of thermal barrier coating systems (TBCs) applied to hollow cylindrical specimens are presented in this work. The Electron Beam Physical Vapor Deposition coated specimens with internal cooling were designed to achieve realistic temperature gradients over the TBC coated material such as that occurring in the turbine blades of aeroengines. Effects of the circular cross section on the x-ray diffraction (XRD) measurements in the various layers, including the thermally grown oxide, are investigated using high-energy synchrotron x-rays. Multiple approaches for beam penetration including collection, tangential, and normal to the layers, along with variations in collection parameters are compared for their ability to attain high-resolution XRD data from the internal layers. This study displays the ability to monitor in situ, the response of the internal layers within the TBC, while implementing a thermal gradient across the thickness of the coated sample. The thermal setup maintained coating surface temperatures in the range of operating conditions, while monitoring the substrate cooling, for a controlled thermal gradient. Through variation in measurement location and beam parameters, sufficient intensities are obtained from the internal layers which can be used for depth resolved strain measurements. Results are used to establish the various techniques for obtaining XRD measurements through multi-layered coating systems and their outcomes will pave the way towards goals in achieving realistic in situ testing of these coatings.

  4. Synchrotron X-ray and optical studies of the DNA-mediated growth of plasmonic nanostructures

    NASA Astrophysics Data System (ADS)

    Chen, Gang; Wang, Geng; Zhang, Xiaonan; Geng, Heping; Xu, Lifeng; Li, Wenqin; Liu, Xin

    2015-03-01

    Reproducible and controllable growth of nanostructures with well-defined physical and chemical properties is a longstanding problem in nanoscience. A key step to address this issue is to understand their underlying growth mechanism, which is often entangled in the complexity of growth environments and obscured by rapid reaction speeds. Synchrotron x-rays, because of their specific wavelengths (nanometers) and advantages of large flux, high penetration and adjustable photon energy, have a particularly important position in structural and electronic characterizations of nanomaterials. Herein, we demonstrate that the evolution of size, surface morphology, and the optical properties of plasmonic nanostructures could be quantitatively intercepted by dynamic and stoichiometric control of the DNA-mediated growth. By combining synchrotron-based small-angle X-ray scattering with transmission electron microscopy, we reliably obtained quantitative structural parameters for these fine nanostructures that correlate well with their optical properties as identified by UV/Vis absorption and dark-field scattering spectroscopy. We report growth mechanisms for SERS active plasmonic nanostructures, and the remarkable interplay between their morphology and plasmonic properties. Work supported by NNSF of China (11375256) and Sci. and Tech. Commission of Shanghai Municipality (14JC1493300).

  5. Synchrotron X-ray measurement techniques for thermal barrier coated cylindrical samples under thermal gradients.

    PubMed

    Siddiqui, Sanna F; Knipe, Kevin; Manero, Albert; Meid, Carla; Wischek, Janine; Okasinski, John; Almer, Jonathan; Karlsson, Anette M; Bartsch, Marion; Raghavan, Seetha

    2013-08-01

    Measurement techniques to obtain accurate in situ synchrotron strain measurements of thermal barrier coating systems (TBCs) applied to hollow cylindrical specimens are presented in this work. The Electron Beam Physical Vapor Deposition coated specimens with internal cooling were designed to achieve realistic temperature gradients over the TBC coated material such as that occurring in the turbine blades of aeroengines. Effects of the circular cross section on the x-ray diffraction (XRD) measurements in the various layers, including the thermally grown oxide, are investigated using high-energy synchrotron x-rays. Multiple approaches for beam penetration including collection, tangential, and normal to the layers, along with variations in collection parameters are compared for their ability to attain high-resolution XRD data from the internal layers. This study displays the ability to monitor in situ, the response of the internal layers within the TBC, while implementing a thermal gradient across the thickness of the coated sample. The thermal setup maintained coating surface temperatures in the range of operating conditions, while monitoring the substrate cooling, for a controlled thermal gradient. Through variation in measurement location and beam parameters, sufficient intensities are obtained from the internal layers which can be used for depth resolved strain measurements. Results are used to establish the various techniques for obtaining XRD measurements through multi-layered coating systems and their outcomes will pave the way towards goals in achieving realistic in situ testing of these coatings. PMID:24007076

  6. Direct surface magnetometry with photoemission magnetic x-ray dichroism

    SciTech Connect

    Tobin, J.G.; Goodman, K.W.; Schumann, F.O.

    1997-04-01

    Element specific surface magnetometry remains a central goal of synchrotron radiation based studies of nanomagnetic structures. One appealing possibility is the combination of x-ray absorption dichroism measurements and the theoretical framework provided by the {open_quotes}sum rules.{close_quotes} Unfortunately, sum rule analysis are hampered by several limitations including delocalization of the final state, multi-electronic phenomena and the presence of surface dipoles. An alternative experiment, Magnetic X-Ray Dichroism in Photoelectron Spectroscopy, holds out promise based upon its elemental specificity, surface sensitivity and high resolution. Computational simulations by Tamura et al. demonstrated the relationship between exchange and spin orbit splittings and experimental data of linear and circular dichroisms. Now the authors have developed an analytical framework which allows for the direct extraction of core level exchange splittings from circular and linear dichroic photoemission data. By extending a model initially proposed by Venus, it is possible to show a linear relation between normalized dichroism peaks in the experimental data and the underlying exchange splitting. Since it is reasonable to expect that exchange splittings and magnetic moments track together, this measurement thus becomes a powerful new tool for direct surface magnetometry, without recourse to time consuming and difficult spectral simulations. The theoretical derivation will be supported by high resolution linear and circular dichroism data collected at the Spectromicroscopy Facility of the Advanced Light Source.

  7. Neutron and Synchrotron X-Ray Scattering Studies of Superconductors

    SciTech Connect

    Tranquada,J.M.

    2008-09-01

    Superconductors hold the promise for a more stable and efficient electrical grid, but new isotropic, high-temperature superconductors are needed in order to reduce cable manufacturing costs. The effort to understand high-temperature superconductivity, especially in the layered cuprates, provides guidance to the search for new superconductors. Neutron scattering has long provided an important probe of the collective excitations that are involved in the pairing mechanism. For the cuprates, neutron and x-ray diffraction techniques also provide information on competing types of order, such as charge and spin stripes, that appear to be closely connected to the superconductivity. Recently, inelastic x-ray scattering has become competitive for studying phonons and may soon provide valuable information on electronic excitations. Examples of how these techniques contribute to our understanding of superconductivity are presented.

  8. 3D-analysis of plant microstructures: advantages and limitations of synchrotron X-ray microtomography

    NASA Astrophysics Data System (ADS)

    Matsushima, U.; Graf, W.; Zabler, S.; Manke, I.; Dawson, M.; Choinka, G.; Hilger, A.; Herppich, W. B.

    2013-01-01

    Synchrotron X-ray computer microtomography was used to analyze the microstructure of rose peduncles. Samples from three rose cultivars, differing in anatomy, were scanned to study the relation between tissue structure and peduncles mechanical strength. Additionally, chlorophyll fluorescence imaging and conventional light microscopy was applied to quantify possible irradiation-induced damage to plant physiology and tissue structure. The spatial resolution of synchrotron X-ray computer microtomography was sufficiently high to investigate the complex tissues of intact rose peduncles without the necessity of any preparation. However, synchrotron X-radiation induces two different types of damage on irradiated tissues. First, within a few hours after first X-ray exposure, there is a direct physical destruction of cell walls. In addition, a slow and delayed destruction of chlorophyll and, consequently, of photosynthetic activity occurred within hours/ days after the exposure. The results indicate that synchrotron X-ray computer microtomography is well suited for three-dimensional visualization of the microstructure of rose peduncles. However, in its current technique, synchrotron X-ray computer microtomography is not really non-destructive but induce tissue damage. Hence, this technique needs further optimization before it can be applied for time-series investigations of living plant materials

  9. X-ray Synchrotron Radiation in a Plasma Wiggler

    SciTech Connect

    Wang, Shuoquin; /UCLA /SLAC, SSRL

    2005-09-27

    A relativistic electron beam can radiate due to its betatron motion inside an ion channel. The ion channel is induced by the electron bunch as it propagates through an underdense plasma. In the theory section of this thesis the formation of the ion channel, the trajectories of beam electrons inside the ion channel, the radiation power and the radiation spectrum of the spontaneous emission are studied. The comparison between different plasma wiggler schemes is made. The difficulties in realizing stimulated emission as the beam traverses the ion channel are investigated, with particular emphasis on the bunching mechanism, which is important for the ion channel free electron laser. This thesis reports an experiment conducted at the Stanford Linear Accelerator Center (SLAC) to measure the betatron X-ray radiations for the first time. They first describe the construction and characterization of the lithium plasma source. In the experiment, the transverse oscillations of the SLAC 28.5 GeV electron beam traversing through a 1.4 meter long lithium plasma source are clearly seen. These oscillations lead to a quadratic density dependence of the spontaneously emitted betatron X-ray radiation. The divergence angle of the X-ray radiation is measured. The absolute photon yield and the spectral brightness at 14.2 KeV photon energy are estimated and seen to be in reasonable agreement with theory.

  10. Synthesis of metallic nanoparticles through X-ray radiolysis using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Yamaguchi, Akinobu; Okada, Ikuo; Fukuoka, Takao; Sakurai, Ikuya; Utsumi, Yuichi

    2016-05-01

    The potential to fabricate metallic nanoparticles directly on silicon substrates from liquid solutions is ideal for three-dimensional lithography systems, drug delivery materials, and sensing applications. Here, we report the successful synthesis of Au, Cu, and Fe nanoparticles from the corresponding liquid solutions [gold(I) trisodium disulphite, copper(II) sulfate, and potassium ferricyanide] by synchrotron (SR) X-ray irradiation. The deposition of gold nanoparticles in the gold(I) trisodium disulphite solution was performed by monochromatic X-ray exposure from synchrotron radiation. The use of ethanol as an additive enabled the nucleation and growth of Cu particles, while no Cu particles were produced in the copper sulfate solution without ethanol with polychromatic SR X-ray irradiation. Fe particles were generated by direct polychromatic SR X-ray irradiation. These results demonstrate the behavior of three-dimensional printers, enabling us to build composite material structures with metallic and plastic materials.

  11. DEVELOPMENTS IN SYNCHROTRON X-RAY COMPUTED MICROTOMOGRAPHY AT THE NATIONAL SYNCHROTRON LIGHT SOURCE.

    SciTech Connect

    DOWD,B.A.

    1999-07-23

    Last year, the X27A beamline at the National Synchrotron Light Source (NSLS) became dedicated solely to X-Ray Computed Microtomography (XCMT). This is a third-generation instrument capable of producing tomographic volumes of 1-2 micron resolution over a 2-3mm field of view. Recent enhancements will be discussed. These have focused on two issues: the desire for real-time data acquisition and processing and the need for highly monochromatic beam (.1 % energy bandpass). The latter will permit k-edge subtraction studies and will provide improved image contrast from below the Cr (6 keV) up to the Cs (36 keV) k-edge. A range of applications that benefit from these improvements will be discussed as well. These two goals are somewhat counterproductive, however; higher monochromaticity yields a lower flux forcing longer data acquisition times. To balance the two, a more efficient scintillator for X-ray conversion is being developed. Some testing of a prototype scintillator has been performed; preliminary results will be presented here. In the meantime, data reconstruction times have been reduced, and the entire tomographic acquisition, reconstruction and volume rendering process streamlined to make efficient use of synchrotron beam time. A Fast Filtered Back Transform (FFBT) reconstruction program recently developed helped to reduce the time to reconstruct a volume of 150 x 150 x 250 pixels{sup 3} (over 5 million voxels) from the raw camera data to 1.5 minutes on a dual R10,000 CPU. With these improvements, one can now obtain a ''quick look'' of a small tomographic volume ({approximately}10{sup 6}voxels) in just over 15 minutes from the start of data acquisition.

  12. Fluctuation x-ray scattering from biological particles in frozen solution by using synchrotron radiation.

    PubMed Central

    Kam, Z; Koch, M H; Bordas, J

    1981-01-01

    Determination of the structure of biological particles, randomly oriented in solution, from spatial correlation analysis of fluctuations in x-ray scattering has recently been proposed. The feasibility of scattering fluctuation measurements was evaluated by using an x-ray synchrotron radiation camera to obtain the spatial correlation for a solution of tobacco mosaic virus along a line. The experimental system, analysis of data, and requirements for the determination of structures in solution are discussed using this example. PMID:6943555

  13. Ultra-high vacuum compatible optical chopper system for synchrotron x-ray scanning tunneling microscopy

    NASA Astrophysics Data System (ADS)

    Chang, Hao; Cummings, Marvin; Shirato, Nozomi; Stripe, Benjamin; Rosenmann, Daniel; Preissner, Curt; Freeland, John W.; Kersell, Heath; Hla, Saw-Wai; Rose, Volker

    2016-01-01

    High-speed beam choppers are a crucial part of time-resolved x-ray studies as well as a necessary component to enable elemental contrast in synchrotron x-ray scanning tunneling microscopy (SX-STM). However, many chopper systems are not capable of operation in vacuum, which restricts their application to x-ray studies with high photon energies, where air absorption does not present a significant problem. To overcome this limitation, we present a fully ultra-high vacuum (UHV) compatible chopper system capable of operating at variable chopping frequencies up to 4 kHz. The lightweight aluminum chopper disk is coated with Ti and Au films to provide the required beam attenuation for soft and hard x-rays with photon energies up to about 12 keV. The chopper is used for lock-in detection of x-ray enhanced signals in SX-STM.

  14. International Conference on Surface X-ray and Neutron Scattering (SXNS-11)

    SciTech Connect

    Michael J. Bedzyk

    2011-06-17

    The 11th International Surface X-ray and Neutron Scattering (SXNS) Conference was held on July 13-17, 2010, on the Northwestern University (NU) campus, in Evanston Illinois and hosted by the NU Materials Research Science and Engineering Center. This biennial conference brought together a community of 164 attendees from 16 countries. The field now makes use of a broad range of new experimental capabilities that have been made possible through the development of increasingly brilliant X-ray and neutron sources around the world, including third generation synchrotron sources, neutron reactor and spallation sources, as well as the recent development of X-ray lasers.

  15. Comparison of Synchrotron X-Ray Fluorescence Mapping and Micro-XANES to Bulk X-Ray Absorption Spectra in Metal-Contaminated Sediments

    SciTech Connect

    O'Day, P; Carroll, S A; Bajt, S

    2003-01-16

    Synchrotron X-ray absorption spectroscopy (XAS) is one of the few techniques that can supply molecular-scale information for a variety of elements at concentrations relevant to natural systems in non-vacuum conditions. Bulk XAS analysis supplies the dominant chemical bonding mode(s) for a specific element. In complex materials such as natural soils and sediments, however, the dominant mode may not necessarily be the most reactive because changes in speciation at surfaces may results in changes in reactivity. Our previous work at Naval Air Station (NAS) Alameda (CA) focused on in situ metal chemistry in surface and deep sediments, and the impact of metal mobility by sediment oxidation. Estuary sediments at the Alameda Naval Station Air in California have elevated metal concentrations that increase with increasing depth. The metal concentrations in these sediments are: Cd (10-350 ppm), Cr (200-1000 ppm), Cu (100-230 ppm), Pb (200-1200 ppm) and Zn (250-600 ppm). We have extensively characterized these sediments using bulk XAS and other non-synchrotron supporting methods [ 1]. In this experiment, we collected fluorescence element maps using synchrotron X-ray microprobe of unreacted and seawater-oxidized sediment samples from Alameda NAS to determine the spatial distribution and correlation of lead, zinc, and iron. We then compared micro-XANES spectra for lead and zinc collected with the X-ray microprobe to previously collected bulk XANES spectra. The results from our bulk XAS characterization of the sediments showed both oxide and sulfide components for the trace metals. However, the bulk XAS data were not able to identify the composition of the oxide component (i.e. carbonate or hydroxide), nor could absorbed species or solid solutions be definitively identified. Our objective in using micro-XANES and fluorescence element maps was to attempt a more precise identification of metal speciation in or on individual particles.

  16. Report of the second workshop on synchrotron radiation sources for x-ray lithography

    SciTech Connect

    Barton, M.Q.; Craft, B.; Williams, G.P.

    1986-01-01

    The reported workshop is part of an effort to implement a US-based x-ray lithography program. Presentations include designs for three storage rings (one superconducting and two conventional) and an overview of a complete lithography program. The background of the effort described, the need for synchrotron radiation, and the international competition in the area are discussed briefly. The technical feasibility of x-ray lithography is discussed, and synchrotron performance specifications and construction options are given, as well as a near-term plan. It is recommended that a prototype synchrotron source be built as soon as possible, and that a research and development plan on critical technologies which could improve cost effectiveness of the synchrotron source be established. It is further recommended that a small number of second generation prototype synchrotrons be distributed to IC manufacturing centers to expedite commercialization. (LEW)

  17. Microbeam, timing and signal-resolved studies of nuclear materials with synchrotron X-ray sources

    SciTech Connect

    Ice, Gene E; Specht, Eliot D

    2012-01-01

    The development of ultra-brilliant synchrotron X-ray sources enables characterization methods that are particularly important for nuclear materials. Here we discuss emerging synchrotron methods with unprecedented signal-to-noise, spatial and time resolution. Microprobe methods are discussed that extend virtually any X-ray characterization measurement to ultra-small sample volumes. This ability is critical to resolve heterogeneities in nuclear materials and for studies on volumes with vastly lower activity than are needed for traditional X-ray characterization. Specific methods discussed include microdiffraction for the characterization of local crystal structure and micro-spectroscopy techniques that allow for characterization of elemental distributions with sensitivity for daughter products, oxidation states and diffusion through buffer layers. Opportunities are also discussed that exploit the high brilliance and pulsed nature of synchrotron radiation to reduce backgrounds from sample radiation and to study materials dynamics.

  18. Nitride-MBE system for in situ synchrotron X-ray measurements

    NASA Astrophysics Data System (ADS)

    Sasaki, Takuo; Ishikawa, Fumitaro; Yamaguchi, Tomohiro; Takahasi, Masamitu

    2016-05-01

    A molecular beam epitaxy (MBE) chamber dedicated to nitride growth was developed at the synchrotron radiation facility SPring-8. This chamber has two beryllium windows for incident and outgoing X-rays, and is directly connected to an X-ray diffractometer, enabling in situ synchrotron X-ray measurements during the nitride growth. Experimental results on initial growth dynamics in GaN/SiC, AlN/SiC, and InN/GaN heteroepitaxy were presented. We achieved high-speed and high-sensitivity reciprocal space mapping with a thickness resolution of atomic-layer scale. This in situ measurement using the high-brilliance synchrotron light source will be useful for evaluating structural variations in the initial growth stage of nitride semiconductors.

  19. High Resolution X-Ray Diffraction of Macromolecules with Synchrotron Radiation

    NASA Technical Reports Server (NTRS)

    Stojanoff, Vivian; Boggon, Titus; Helliwell, John R.; Judge, Russell; Olczak, Alex; Snell, Edward H.; Siddons, D. Peter; Rose, M. Franklin (Technical Monitor)

    2000-01-01

    We recently combined synchrotron-based monochromatic X-ray diffraction topography methods with triple axis diffractometry and rocking curve measurements: high resolution X-ray diffraction imaging techniques, to better understand the quality of protein crystals. We discuss these methods in the light of results obtained on crystals grown under different conditions. These non destructive techniques are powerful tools in the characterization of the protein crystals and ultimately will allow to improve, develop, and understand protein crystal growth. High resolution X-ray diffraction imaging methods will be discussed in detail in light of recent results obtained on Hen Egg White Lysozyme crystals and other proteins.

  20. Omega Dante Soft X-Ray Power Diagnostic Component Calibration at the National Synchrotron Light Source

    SciTech Connect

    Campbell, K; Weber, F; Dewald, E; Glenzer, S; Landen, O; Turner, R; Waide, P

    2004-04-15

    The Dante soft x-ray spectrometer installed on the Omega laser facility at the Laboratory for Laser Energetics, University of Rochester is a twelve-channel filter-edge defined x-ray power diagnostic. It is used to measure the absolute flux from direct drive, indirect drive (hohlraums) and other plasma sources. Calibration efforts using two beam lines, U3C (50eV-1keV) and X8A (1keV-6keV) at the National Synchrotron Light Source (NSLS) have been implemented to insure the accuracy of these measurements. We have calibrated vacuum x-ray diodes, mirrors and filters.

  1. Omega Dante soft x-ray power diagnostic component calibration at the National Synchrotron Light Source

    SciTech Connect

    Campbell, K.M.; Weber, F.A.; Dewald, E.L.; Glenzer, S.H.; Landen, O.L.; Turner, R.E.; Waide, P.A.

    2004-10-01

    The Dante soft x-ray spectrometer, installed on the Omega laser facility at the Laboratory for Laser Energetics, University of Rochester, is a 12-channel filter-edge defined soft x-ray power diagnostic. It is used to measure the spectrally resolved, absolute flux from direct drive, indirect drive (hohlraums) and other plasma sources. Dante component calibration efforts using two beam lines, U3C (50 eV-1 keV) and X8A (1-6 keV) at the National Synchrotron Light Source have been implemented to improve the accuracy of these measurements. We have calibrated metallic vacuum x-ray diodes, mirrors and filters.

  2. X-ray microtomography with monochromatic synchrotron radiation

    SciTech Connect

    D'Amico, K. L.; Deckman, H. W.; Dunsmuir, J. H.; Flannery, B. P.; Roberge, W. G.

    1989-07-01

    We review results obtained with the Exxon Microtomography apparatus. The technique is based on tomographic methods widely used in medicine and nondestructive evaluation. When used with a tunable x-ray source, it is a powerful diagnostic and research tool for a wide variety of materials problems. It is capable of producing maps of the interior structure and chemical composition of samples approximately 0.5--1.0 mm in size, with spatial resolution in the map of the density variations approaching 10.0 /mu/m.

  3. Synchrotron soft X-ray absorption spectroscopy study of carbon and silicon nanostructures for energy applications.

    PubMed

    Zhong, Jun; Zhang, Hui; Sun, Xuhui; Lee, Shuit-Tong

    2014-12-10

    Carbon and silicon materials are two of the most important materials involved in the history of the science and technology development. In the last two decades, C and Si nanoscale materials, e.g., carbon nanotubes, graphene, and silicon nanowires, and quantum dots, have also emerged as the most interesting nanomaterials in nanoscience and nanotechnology for their myriad promising applications such as for electronics, sensors, biotechnology, etc. In particular, carbon and silicon nanostructures are being utilized in energy-related applications such as catalysis, batteries, solar cells, etc., with significant advances. Understanding of the nature of surface and electronic structures of nanostructures plays a key role in the development and improvement of energy conversion and storage nanosystems. Synchrotron soft X-ray absorption spectroscopy (XAS) and related techniques, such as X-ray emission spectroscopy (XES) and scanning transmission X-ray microscopy (STXM), show unique capability in revealing the surface and electronic structures of C and Si nanomaterials. In this review, XAS is demonstrated as a powerful technique for probing chemical bonding, the electronic structure, and the surface chemistry of carbon and silicon nanomaterials, which can greatly enhance the fundamental understanding and also applicability of these nanomaterials in energy applications. The focus is on the unique advantages of XAS as a complementary tool to conventional microscopy and spectroscopy for effectively providing chemical and structural information about carbon and silicon nanostructures. The employment of XAS for in situ, real-time study of property evolution of C and Si nanostructures to elucidate the mechanisms in energy conversion or storage processes is also discussed. PMID:25204894

  4. Cell for simultaneous synchrotron radiation X-ray and electrochemical corrosion measurements on cultural heritage metals and other materials.

    PubMed

    Dowsett, Mark G; Adriaens, Annemie

    2006-05-15

    We describe the construction of an electrochemical cell of the Bragg type suitable for in situ synchrotron X-ray measurements on rough, heterogeneous metals such as cultural heritage alloys and simulants with corroding or passivated surfaces. The cell features a working electrode, which may be moved under remote control from a position close to an X-ray window to full immersion in the electrolyte. A pocket of electrolyte in contact with the bulk can be maintained on the working electrode surface at all times. Its thickness (typically 100-200 microm) can be controlled by adjusting the working electrode position and, independently, altering the conformation of the X-ray window with hydrostatic pressure. Alternatively, the electrode may be lowered into the bulk of the electrolyte. Early results from the cell showing a time-resolved study of the reduction of nantokite to cuprite in sodium sesquicarbonate, accompanied by corrosion potential measurements obtained in parallel, are presented here. PMID:16689538

  5. Evaluation of different synchrotron beamline configurations for X-ray fluorescence analysis of environmental samples.

    PubMed

    Barberie, Sean R; Iceman, Christopher R; Cahill, Catherine F; Cahill, Thomas M

    2014-08-19

    Synchrotron radiation X-ray fluorescence (SR-XRF) is a powerful elemental analysis tool, yet synchrotrons are large, multiuser facilities that are generally not amenable to modification. However, the X-ray beamlines from synchrotrons can be modified by simply including X-ray filters or removing monochromators to improve the SR-XRF analysis. In this study, we evaluated four easily applied beamline configurations for the analysis of three representative environmental samples, namely a thin aerosol sample, an intermediate thickness biological sample, and a thick rare earth mineral specimen. The results showed that the "white beam" configuration, which was simply the full, polychromatic output of the synchrotron, was the optimal configuration for the analysis of thin samples with little mass. The "filtered white beam" configuration removed the lower energy X-rays from the excitation beam so it gave better sensitivity for elements emitting more energetic X-rays. The "filtered white beam-filtered detector" configuration sacrifices the lower energy part of the spectrum (<15 keV) for improved sensitivity in the higher end (∼26 to 48 keV range). The use of a monochromatic beam, which tends to be the standard mode of operation for most SR-XRF analyses reported in the literature, gave the least sensitive analysis. PMID:25025342

  6. Micro-structural characterization of materials using synchrotron hard X-ray imaging techniques

    SciTech Connect

    Agrawal, Ashish Singh, Balwant; Kashyap, Yogesh; Sarkar, P. S.; Shukla, Mayank; Sinha, Amar

    2015-06-24

    X-ray imaging has been an important tool to study the materials microstructure with the laboratory based sources however the advent of third generation synchrotron sources has introduced new concepts in X-ray imaging such as phase contrast imaging, micro-tomography, fluorescence imaging and diffraction enhance imaging. These techniques are being used to provide information of materials about their density distribution, porosity, geometrical and morphological characteristics at sub-micron scalewith improved contrast. This paper discusses the development of various imaging techniques at synchrotron based imaging beamline Indus-2 and few recent experiments carried out at this facility.

  7. Absolute x-ray dosimetry on a synchrotron medical beam line with a graphite calorimeter

    SciTech Connect

    Harty, P. D. Ramanathan, G.; Butler, D. J.; Johnston, P. N.; Lye, J. E.; Hall, C. J.; Stevenson, A. W.

    2014-05-15

    Purpose: The absolute dose rate of the Imaging and Medical Beamline (IMBL) on the Australian Synchrotron was measured with a graphite calorimeter. The calorimetry results were compared to measurements from the existing free-air chamber, to provide a robust determination of the absolute dose in the synchrotron beam and provide confidence in the first implementation of a graphite calorimeter on a synchrotron medical beam line. Methods: The graphite calorimeter has a core which rises in temperature when irradiated by the beam. A collimated x-ray beam from the synchrotron with well-defined edges was used to partially irradiate the core. Two filtration sets were used, one corresponding to an average beam energy of about 80 keV, with dose rate about 50 Gy/s, and the second filtration set corresponding to average beam energy of 90 keV, with dose rate about 20 Gy/s. The temperature rise from this beam was measured by a calibrated thermistor embedded in the core which was then converted to absorbed dose to graphite by multiplying the rise in temperature by the specific heat capacity for graphite and the ratio of cross-sectional areas of the core and beam. Conversion of the measured absorbed dose to graphite to absorbed dose to water was achieved using Monte Carlo calculations with the EGSnrc code. The air kerma measurements from the free-air chamber were converted to absorbed dose to water using the AAPM TG-61 protocol. Results: Absolute measurements of the IMBL dose rate were made using the graphite calorimeter and compared to measurements with the free-air chamber. The measurements were at three different depths in graphite and two different filtrations. The calorimetry measurements at depths in graphite show agreement within 1% with free-air chamber measurements, when converted to absorbed dose to water. The calorimetry at the surface and free-air chamber results show agreement of order 3% when converted to absorbed dose to water. The combined standard uncertainty is 3

  8. Soft X-Ray Spectrometer Using 100-Pixel STJ Detectors for Synchrotron Radiation

    SciTech Connect

    Shiki, Shigetomo; Zen, Nobuyuki; Ukibe, Masahiro; Ohkubo, Masataka

    2009-12-16

    Fluorescent X-ray absorption fine structure (XAFS) is an important tool for material analysis, especially for the measurement of chemical states or local structures of elements. Semiconductor detectors are usually used for separating the fluorescent of elements in question from background fluorescence. However, the semiconductor detectors cannot always discriminate K-lines of light elements and L-lines of various elements as different X-ray peaks at an energy range below about 3 keV. Superconducting tunnel junction (STJ) detectors are promising device for the soft X-ray at synchrotron radiation beam lines because of excellent energy resolution, high detection efficiency, and high counting rate. We are constructing a fluorescent X-ray spectrometer having 100-pixel array of STJs with 200 {mu}m square. The array detector is mounted on a liquid cryogen-free {sup 3}He cryostat. The sensitive area is the largest among the superconducting X-ray spectrometers operating at synchrotron beam lines. Each pixel is connected to a room temperature readout circuit that consists of a charge sensitive amplifier and a pulse height analyzer. The spectrometer will achieve a total solid angle of {approx}0.01 sr and a maximum counting rate of more than 1 M count per second. The present status of developments of our fluorescent X-ray spectrometer was reported.

  9. Diamond for high-heat-load synchrotron x-ray applications

    SciTech Connect

    Lee, Wah-Keat

    1994-12-31

    Synchrotron facilities worldwide provide scientists with useful radiation in the ultraviolet to the x-ray regime. Third-generation synchrotron sources win deliver photon fluxes in the 10{sup 15} photons/s/0.1%BW range, with brilliance on the order of 10{sup 18} photons/s/0.1%BW/mrad{sup 2}/mm{sup 2}. Along with the increase in flux and brilliance is an increase in the power and power densities of the x-ray beam. Depending on the particular insertion device, the x-ray beam can have total power in excess of 10 kW and peak power, density of more than 400 W/mm{sup 2}. Such high heat loads are a major challenge in the design and fabrication of x-ray beamline components. The superior thermal and mechanical properties of diamond make it a good candidate as material in these components. Single crystal diamonds can be used as x-ray monochromators, while polycrystalline or CVD diamonds can be used in a variety of ways on the front-end beamline components. This paper discusses the issues regarding the feasibility of using diamond in third-generation synchrotron beamline components.

  10. Contemporary X-ray electron-density studies using synchrotron radiation

    PubMed Central

    Jørgensen, Mads R. V.; Hathwar, Venkatesha R.; Bindzus, Niels; Wahlberg, Nanna; Chen, Yu-Sheng; Overgaard, Jacob; Iversen, Bo B.

    2014-01-01

    Synchrotron radiation has many compelling advantages over conventional radiation sources in the measurement of accurate Bragg diffraction data. The variable photon energy and much higher flux may help to minimize critical systematic effects such as absorption, extinction and anomalous scattering. Based on a survey of selected published results from the last decade, the benefits of using synchrotron radiation in the determination of X-ray electron densities are discussed, and possible future directions of this field are examined. PMID:25295169

  11. Combining operando synchrotron X-ray tomographic microscopy and scanning X-ray diffraction to study lithium ion batteries.

    PubMed

    Pietsch, Patrick; Hess, Michael; Ludwig, Wolfgang; Eller, Jens; Wood, Vanessa

    2016-01-01

    We present an operando study of a lithium ion battery combining scanning X-ray diffraction (SXRD) and synchrotron radiation X-ray tomographic microscopy (SRXTM) simultaneously for the first time. This combination of techniques facilitates the investigation of dynamic processes in lithium ion batteries containing amorphous and/or weakly attenuating active materials. While amorphous materials pose a challenge for diffraction techniques, weakly attenuating material systems pose a challenge for attenuation-contrast tomography. Furthermore, combining SXRD and SRXTM can be used to correlate processes occurring at the atomic level in the crystal lattices of the active materials with those at the scale of electrode microstructure. To demonstrate the benefits of this approach, we investigate a silicon powder electrode in lithium metal half-cell configuration. Combining SXRD and SRXTM, we are able to (i) quantify the dissolution of the metallic lithium electrode and the expansion of the silicon electrode, (ii) better understand the formation of the Li15Si4 phase, and (iii) non-invasively probe kinetic limitations within the silicon electrode. A simple model based on the 1D diffusion equation allows us to qualitatively understand the observed kinetics and demonstrates why high-capacity electrodes are more prone to inhomogeneous lithiation reactions. PMID:27324109

  12. Combining operando synchrotron X-ray tomographic microscopy and scanning X-ray diffraction to study lithium ion batteries

    PubMed Central

    Pietsch, Patrick; Hess, Michael; Ludwig, Wolfgang; Eller, Jens; Wood, Vanessa

    2016-01-01

    We present an operando study of a lithium ion battery combining scanning X-ray diffraction (SXRD) and synchrotron radiation X-ray tomographic microscopy (SRXTM) simultaneously for the first time. This combination of techniques facilitates the investigation of dynamic processes in lithium ion batteries containing amorphous and/or weakly attenuating active materials. While amorphous materials pose a challenge for diffraction techniques, weakly attenuating material systems pose a challenge for attenuation-contrast tomography. Furthermore, combining SXRD and SRXTM can be used to correlate processes occurring at the atomic level in the crystal lattices of the active materials with those at the scale of electrode microstructure. To demonstrate the benefits of this approach, we investigate a silicon powder electrode in lithium metal half-cell configuration. Combining SXRD and SRXTM, we are able to (i) quantify the dissolution of the metallic lithium electrode and the expansion of the silicon electrode, (ii) better understand the formation of the Li15Si4 phase, and (iii) non-invasively probe kinetic limitations within the silicon electrode. A simple model based on the 1D diffusion equation allows us to qualitatively understand the observed kinetics and demonstrates why high-capacity electrodes are more prone to inhomogeneous lithiation reactions. PMID:27324109

  13. In situ synchrotron X-ray diffraction investigation of the evolution of a PbO₂/PbSO₄ surface layer on a copper electrowinning Pb anode in a novel electrochemical flow cell.

    PubMed

    Clancy, Marie; Styles, Mark J; Bettles, Colleen J; Birbilis, Nick; Chen, Miao; Zhang, Yansheng; Gu, Qinfen; Kimpton, Justin A; Webster, Nathan A S

    2015-03-01

    This paper describes the quantitative measurement, by in situ synchrotron X-ray diffraction (S-XRD) and subsequent Rietveld-based quantitative phase analysis and thickness calculations, of the evolution of the PbO2 and PbSO4 surface layers formed on a pure lead anode under simulated copper electrowinning conditions in a 1.6 M H2SO4 electrolyte at 318 K. This is the first report of a truly in situ S-XRD study of the surface layer evolution on a Pb substrate under cycles of galvanostatic and power interruption conditions, of key interest to the mining, solvent extraction and lead acid battery communities. The design of a novel reflection geometry electrochemical flow cell is also described. The in situ S-XRD results show that β-PbO2 forms immediately on the anode under galvanostatic conditions, and undergoes continued growth until power interruption where it transforms to PbSO4. The kinetics of the β-PbO2 to PbSO4 conversion decrease as the number of cycles increases, whilst the amount of residual PbO2 increases with the number of cycles due to incomplete conversion to PbSO4. Conversely, complete transformation of PbSO4 to β-PbO2 was observed in each cycle. The results of layer thickness calculations demonstrate a significant volume change upon PbSO4 to β-PbO2 transformation. PMID:25723938

  14. Soft X-ray synchrotron radiation investigations of actinidematerials systems utilizing X-ray emission spectroscopy and resonantinelastic X-ray scattering

    SciTech Connect

    Shuh, D.K.; Butorin, S.M.; Guo, J.-H.; Nordgren, J.

    2004-01-03

    Synchrotron radiation (SR) methods have been utilized with increasing frequency over the past several years to study topics in actinide science, ranging from those of a fundamental nature to those that address a specifically-targeted technical need. In particular, the emergence of microspectroscopic and fluorescence-based techniques have permitted investigations of actinide materials at sources of soft x-ray SR. Spectroscopic techniques with fluorescence-based detection are useful for actinide investigations since they are sensitive to small amounts of material and the information sampling depth may be varied. These characteristics also serve to simplify both sample preparation and safety considerations. Examples of investigations using these fluorescence techniques will be described along with their results, as well as the prospects for future investigations utilizing these methodologies.

  15. Biomedical elemental analysis and imaging using synchrotron x-ray microscopy

    SciTech Connect

    Jones, K.W.; Gordon, B.M.; Schidlovsky, G.; Spanne, P.; Dejun, Xue ); Bockman, R.S. ); Saubermann, A.J. . Health Science Center)

    1990-01-01

    The application of synchrotron x-ray microscopy to biomedical research is currently in progress at the Brookhaven National Synchrotron Light Source (NSLS). The current status of the x-ray microscope (XRM) is reviewed from a technical standpoint. Some of the items considered are photon flux, spatial resolution, quantitation, minimum detection limits, and beam-induced specimen damage. Images can be produced by measurement of fluorescent x rays or of the attenuation of the incident beam by the specimen. Maps of the elemental distributions or linear attenuation of the incident beam by the specimen. Maps of the elemental distributions or linear attenuation coefficients can be made by scanning the specimen past the beam. Computed microtomography (CMT) can be used for non- destructive images through the specimen in either the emission or absorption mode. Examples of measurements made with the XRM are given.

  16. Synchrotron radiation induced x-ray micro analysis: A realistic alternative for electron- and ion beam microscopy?

    SciTech Connect

    Janssens, K.; Adams, F.; Rivers, M.L.; Jones, K.W.

    1992-10-01

    Synchrotron Radiation induced X-ray micro Fluorescence analysis ({mu}-SRXRF) is compared with more conventional microanalytical techniques such as Secondary Ion Microscopy (SIMS) and Electron Probe X-ray Microanalysis (EPXMA) for two typical microanalytical applications. SRXRF and EPXMA are employed for the analysis of individual particles, showing the complementary character of both techniques. By means of element mapping of trace constituents in a heterogeneous feldspar, the strong and weak points of SRXRF in comparison to EPXMA and SIMS are illustrated. The most striking difference between SRXRF and the other two microanalytical methods is the ability of SRXRF to probe deep into the investigated Material, whereas SIMS and EPXMA only investigate the upper surface of the material. The possibilities of SRXRF at third generation synchrotron rings is also briefly discussed.

  17. Synchrotron radiation induced x-ray micro analysis: A realistic alternative for electron- and ion beam microscopy

    SciTech Connect

    Janssens, K.; Adams, F. . Dept. of Chemistry); Rivers, M.L.; Jones, K.W. )

    1992-01-01

    Synchrotron Radiation induced X-ray micro Fluorescence analysis ([mu]-SRXRF) is compared with more conventional microanalytical techniques such as Secondary Ion Microscopy (SIMS) and Electron Probe X-ray Microanalysis (EPXMA) for two typical microanalytical applications. SRXRF and EPXMA are employed for the analysis of individual particles, showing the complementary character of both techniques. By means of element mapping of trace constituents in a heterogeneous feldspar, the strong and weak points of SRXRF in comparison to EPXMA and SIMS are illustrated. The most striking difference between SRXRF and the other two microanalytical methods is the ability of SRXRF to probe deep into the investigated Material, whereas SIMS and EPXMA only investigate the upper surface of the material. The possibilities of SRXRF at third generation synchrotron rings is also briefly discussed.

  18. Comparison of synchrotron x-ray microanalysis with electron and proton microscopy for individual particle analysis

    SciTech Connect

    Janssens, K.H.; van Langevelde, F.; Adams, F.C.; Vis, R.D.; Sutton, S.R.; Rivers, M.L.; Jones, K.W.; Bowen, D.K.

    1991-12-31

    This paper is concerned with the evaluation of the use of synchrotron/radiation induced x-ray fluorescences ({mu}-SRXRF) as implemented at two existing X-ray microprobes for the analysis of individual particles. As representative environmental particulates, National Institutes of Science and Technology (NIST) K227, K309, K441 and K961 glass microspheres were analyzed using two types of X-ray micro probes: the white light microprobe at beamline X26A of the monochromatic (15 keV) X-ray microprobe at station 7.6 of the SRS. For reference, the particles were also analyzed with microanalytical techniques more commonly employed for individual particles analysis such as EPMA and micro-PIXE.

  19. Comparison of synchrotron x-ray microanalysis with electron and proton microscopy for individual particle analysis

    SciTech Connect

    Janssens, K.H.; van Langevelde, F.; Adams, F.C. ); Vis, R.D. ); Sutton, S.R.; Rivers, M.L. ); Jones, K.W. ); Bowen, D.K. )

    1991-01-01

    This paper is concerned with the evaluation of the use of synchrotron/radiation induced x-ray fluorescences ({mu}-SRXRF) as implemented at two existing X-ray microprobes for the analysis of individual particles. As representative environmental particulates, National Institutes of Science and Technology (NIST) K227, K309, K441 and K961 glass microspheres were analyzed using two types of X-ray micro probes: the white light microprobe at beamline X26A of the monochromatic (15 keV) X-ray microprobe at station 7.6 of the SRS. For reference, the particles were also analyzed with microanalytical techniques more commonly employed for individual particles analysis such as EPMA and micro-PIXE.

  20. Initial feasibility study of a dedicated synchrotron radiation light source for ultrafast X-ray science

    SciTech Connect

    Corlett, John N.; DeSantis, S.; Hartman, N.; Heimann, P.; LaFever, R.; Li, D.; Padmore, H.; Rimmer, R.; Robinson, K.; Schoenlein, R.; Tanabe, J.; Wang, S.; Zholents, A.; Kairan, D.

    2001-10-26

    We present an initial feasibility summary of a femtosecond synchrotron radiation x-ray source based on a flat-beam rf gun and a recirculating superconducting linac that provides beam to an array of undulators and bend magnets. Optical pulse durations of < 100 fs are obtained by a combination of electron pulse compression, transverse temporal correlation of the electrons, and x-ray pulse compression. After an introduction and initial scientific motivation, we cover the following aspects of the design: layout and lattice, ultra-fast x-ray pulse production, flat electron-beam production, the rf gun, rf systems, cryogenic systems, collective effects, photon production, and synchronization of x-ray and laser pulses. We conclude with a summary of issues and areas of development that remain to be addressed.

  1. CCD (charge-coupled device) sensors in synchrotron x-ray detectors

    SciTech Connect

    Strauss, M.G.; Naday, I.; Sherman, I.S.; Kraimer, M.R.; Westbrook, E.M.; Zaluzec, N.J.

    1987-01-01

    The intense photon flux from advanced synchrotron light sources, such as the 7-GeV synchrotron being designed at Argonne, require integrating-type detectors. Charge-coupled devices (CCDs) are well suited as synchrotron x-ray detectors. When irradiated indirectly via a phosphor followed by reducing optics, diffraction patterns of 100 cm/sup 2/ can be imaged on a 2 cm/sup 2/ CCD. With a conversion efficiency of approx.1 CCD electron/x-ray photon, a peak saturation capacity of >10/sup 6/ x rays can be obtained. A programmable CCD controller operating at a clock frequency of 20 MHz has been developed. The readout rate is 5 x 10/sup 6/ pixels/s and the shift rate in the parallel registers is 10/sup 6/ lines/s. The test detector was evaluated in two experiments. In protein crystallography diffraction patterns have been obtained from a lysozyme crystal using a conventional rotating anode x-ray generator. Based on these results we expect to obtain at a synchrotron diffraction images at the rate of approx.1 frame/s or a complete 3-dimensional data set from a single crystal in approx.2 min. 16 refs., 16 figs., 2 tabs.

  2. Fracture mechanics by three-dimensional crack-tip synchrotron X-ray microscopy.

    PubMed

    Withers, P J

    2015-03-01

    To better understand the relationship between the nucleation and growth of defects and the local stresses and phase changes that cause them, we need both imaging and stress mapping. Here, we explore how this can be achieved by bringing together synchrotron X-ray diffraction and tomographic imaging. Conventionally, these are undertaken on separate synchrotron beamlines; however, instruments capable of both imaging and diffraction are beginning to emerge, such as ID15 at the European Synchrotron Radiation Facility and JEEP at the Diamond Light Source. This review explores the concept of three-dimensional crack-tip X-ray microscopy, bringing them together to probe the crack-tip behaviour under realistic environmental and loading conditions and to extract quantitative fracture mechanics information about the local crack-tip environment. X-ray diffraction provides information about the crack-tip stress field, phase transformations, plastic zone and crack-face tractions and forces. Time-lapse CT, besides providing information about the three-dimensional nature of the crack and its local growth rate, can also provide information as to the activation of extrinsic toughening mechanisms such as crack deflection, crack-tip zone shielding, crack bridging and crack closure. It is shown how crack-tip microscopy allows a quantitative measure of the crack-tip driving force via the stress intensity factor or the crack-tip opening displacement. Finally, further opportunities for synchrotron X-ray microscopy are explored. PMID:25624521

  3. Multiple powder diffraction data for an accurate charge density study using synchrotron radiation x-ray

    NASA Astrophysics Data System (ADS)

    Kasai, Hidetaka; Nishibori, Eiji

    2016-04-01

    In recent years multiple synchrotron radiation (SR) powder x-ray diffraction profiles have been successfully applied to advanced structural studies such as an accurate charge density study and a structure determination from powder diffraction. The results have been presented with several examples. Abilities and future prospects have been discussed using state of the art powder diffraction data.

  4. Variable magnification with Kirkpatrick-Baez optics for synchrotron X-ray microscopy

    DOE PAGESBeta

    Jach, Terrence; Bakulin, Alex S.; Durbin, Stephen M.; Pedulla, Joseph; Macrander, Albert

    2006-05-01

    In this study, we describe the distinction between the operation of a short focal length x-ray microscope forming a real image with a laboratory source (convergent illumination) and with a highly collimated intense beam from a synchrotron light source (Kohler illumination).

  5. Atomic physics with hard X-rays from high brilliance synchrotron light sources

    SciTech Connect

    Southworth, S.; Gemmell, D.

    1996-08-01

    A century after the discovery of x rays, the experimental capability for studying atomic structure and dynamics with hard, bright synchrotron radiation is increasing remarkably. Tempting opportunities arise for experiments on many-body effects, aspects of fundamental photon-atom interaction processes, and relativistic and quantum-electrodynamic phenomena. Some of these possibilities are surveyed in general terms.

  6. Fracture mechanics by three-dimensional crack-tip synchrotron X-ray microscopy

    PubMed Central

    Withers, P. J.

    2015-01-01

    To better understand the relationship between the nucleation and growth of defects and the local stresses and phase changes that cause them, we need both imaging and stress mapping. Here, we explore how this can be achieved by bringing together synchrotron X-ray diffraction and tomographic imaging. Conventionally, these are undertaken on separate synchrotron beamlines; however, instruments capable of both imaging and diffraction are beginning to emerge, such as ID15 at the European Synchrotron Radiation Facility and JEEP at the Diamond Light Source. This review explores the concept of three-dimensional crack-tip X-ray microscopy, bringing them together to probe the crack-tip behaviour under realistic environmental and loading conditions and to extract quantitative fracture mechanics information about the local crack-tip environment. X-ray diffraction provides information about the crack-tip stress field, phase transformations, plastic zone and crack-face tractions and forces. Time-lapse CT, besides providing information about the three-dimensional nature of the crack and its local growth rate, can also provide information as to the activation of extrinsic toughening mechanisms such as crack deflection, crack-tip zone shielding, crack bridging and crack closure. It is shown how crack-tip microscopy allows a quantitative measure of the crack-tip driving force via the stress intensity factor or the crack-tip opening displacement. Finally, further opportunities for synchrotron X-ray microscopy are explored. PMID:25624521

  7. X-ray photonic microsystems for the manipulation of synchrotron light

    SciTech Connect

    Mukhopadhyay, D.; Walko, D. A.; Jung, I. W.; Schwartz, C. P.; Wang, Jin; López, D.; Shenoy, G. K.

    2015-05-05

    In this study, photonic microsystems played an essential role in the development of integrated photonic devices, thanks to their unique spatiotemporal control and spectral shaping capabilities. Similar capabilities to markedly control and manipulate X-ray radiation are highly desirable but practically impossible due to the massive size of the silicon single-crystal optics currently used. Here we show that micromechanical systems can be used as X-ray optics to create and preserve the spatial, temporal and spectral correlation of the X-rays. We demonstrate that, as X-ray reflective optics they can maintain the wavefront properties with nearly 100% reflectivity, and as a dynamic diffractive optics they can generate nanosecond time windows with over 100-kHz repetition rates. Since X-ray photonic microsystems can be easily incorporated into lab-based and next-generation synchrotron X-ray sources, they bring unprecedented design flexibility for future dynamic and miniature X-ray optics for focusing, wavefront manipulation, multicolour dispersion, and pulse slicing.

  8. Phase-contrast X-ray imaging with synchrotron radiation for materials science applications

    NASA Astrophysics Data System (ADS)

    Stevenson, A. W.; Gureyev, T. E.; Paganin, D.; Wilkins, S. W.; Weitkamp, T.; Snigirev, A.; Rau, C.; Snigireva, I.; Youn, H. S.; Dolbnya, I. P.; Yun, W.; Lai, B.; Garrett, R. F.; Cookson, D. J.; Hyodo, K.; Ando, M.

    2003-01-01

    Since Röntgen's discovery of X-rays just over a century ago the vast majority of radiographs have been collected and interpreted on the basis of absorption contrast and geometrical (ray) optics. Recently the possibility of obtaining new and complementary information in X-ray images by utilizing phase-contrast effects has received considerable attention, both in the laboratory context and at synchrotron sources (where much of this activity is a consequence of the highly coherent X-ray beams which can be produced). Phase-contrast X-ray imaging is capable of providing improved information from weakly absorbing features in a sample, together with improved edge definition. Four different experimental arrangements for achieving phase contrast in the hard X-ray regime, for the purpose of non-destructive characterization of materials, will be described. Two of these, demonstrated at ESRF in France and AR in Japan, are based on parallel-beam geometry; the other two, demonstrated at PLS in Korea and APS in USA, are based on spherical-beam geometry. In each case quite different X-ray optical arrangements were used. Some image simulations will be employed to demonstrate salient features of hard X-ray phase-contrast imaging and examples of results from each of the experiments will be shown.

  9. X-ray photonic microsystems for the manipulation of synchrotron light

    DOE PAGESBeta

    Mukhopadhyay, D.; Walko, D. A.; Jung, I. W.; Schwartz, C. P.; Wang, Jin; López, D.; Shenoy, G. K.

    2015-05-05

    In this study, photonic microsystems played an essential role in the development of integrated photonic devices, thanks to their unique spatiotemporal control and spectral shaping capabilities. Similar capabilities to markedly control and manipulate X-ray radiation are highly desirable but practically impossible due to the massive size of the silicon single-crystal optics currently used. Here we show that micromechanical systems can be used as X-ray optics to create and preserve the spatial, temporal and spectral correlation of the X-rays. We demonstrate that, as X-ray reflective optics they can maintain the wavefront properties with nearly 100% reflectivity, and as a dynamic diffractivemore » optics they can generate nanosecond time windows with over 100-kHz repetition rates. Since X-ray photonic microsystems can be easily incorporated into lab-based and next-generation synchrotron X-ray sources, they bring unprecedented design flexibility for future dynamic and miniature X-ray optics for focusing, wavefront manipulation, multicolour dispersion, and pulse slicing.« less

  10. X-ray photonic microsystems for the manipulation of synchrotron light

    PubMed Central

    Mukhopadhyay, D.; Walko, D. A.; Jung, I. W.; Schwartz, C. P.; Wang, Jin; López, D.; Shenoy, G. K.

    2015-01-01

    Photonic microsystems played an essential role in the development of integrated photonic devices, thanks to their unique spatiotemporal control and spectral shaping capabilities. Similar capabilities to markedly control and manipulate X-ray radiation are highly desirable but practically impossible due to the massive size of the silicon single-crystal optics currently used. Here we show that micromechanical systems can be used as X-ray optics to create and preserve the spatial, temporal and spectral correlation of the X-rays. We demonstrate that, as X-ray reflective optics they can maintain the wavefront properties with nearly 100% reflectivity, and as a dynamic diffractive optics they can generate nanosecond time windows with over 100-kHz repetition rates. Since X-ray photonic microsystems can be easily incorporated into lab-based and next-generation synchrotron X-ray sources, they bring unprecedented design flexibility for future dynamic and miniature X-ray optics for focusing, wavefront manipulation, multicolour dispersion, and pulse slicing. PMID:25940542

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

    NASA Technical Reports Server (NTRS)

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

    1999-01-01

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

  12. Real world issues for the new soft x-ray synchrotron sources

    SciTech Connect

    Kincaid, B.M.

    1991-05-01

    A new generation of synchrotron radiation light sources covering the VUV, soft x-ray and hard x-ray spectral regions is under construction in several countries. They are designed specifically to use periodic magnetic undulators and low-emittance electron or positron beams to produce high-brightness near-diffraction-limited synchrotron radiation beams. An introduction to the properties of undulator radiation is followed by a discussion of some of the challenges to be faced at the new facilities. Examples of predicted undulator output from the Advanced Light Source, a third generation 1--2 GeV storage ring optimized for undulator use, are used to highlight differences from present synchrotron radiation sources, including high beam power, partial coherence, harmonics, and other unusual spectral and angular properties of undulator radiation. 8 refs., 2 figs.

  13. Real time synchrotron x-ray diffraction measurements to determine material strength of shocked single crystals following compression and release

    SciTech Connect

    Turneaure, Stefan J.; Gupta, Y.M.

    2009-09-15

    We present a method to use real time, synchrotron x-ray diffraction measurements to determine the strength of shocked single crystals following compression and release during uniaxial strain loading. Aluminum and copper single crystals shocked along [111] were examined to peak stresses ranging from 2 to 6 GPa. Synchrotron x rays were used to probe the longitudinal lattice strains near the rear free surface (16 and 5 {micro}m depths for Al and Cu, respectively) of the metal crystals following shock compression and release. The 111 diffraction peaks showed broadening indicating a heterogeneous microstructure in the released state. The diffraction peaks also shifted to lower Bragg angles relative to the ambient Bragg angle; the magnitude of the shift increased with increasing impact stress. The Bragg angle shifts and appropriate averaging procedures were used to determine the macroscopic or continuum strength following compression and release. For both crystals, the strengths upon release increased with increasing impact stress and provide a quantitative measure of the strain hardening that occurs in Al(111) and Cu(111) during the shock and release process. Our results for Al(111) are in reasonable agreement with a previous determination based solely on continuum measurements. Two points are noteworthy about the developments presented here: Synchrotron x rays are needed because they provide the resolution required for analyzing the data in the released state; the method presented here can be extended to the shocked state but will require additional measurements.

  14. Synchrotron-based Scattered Radiation from Phantom Materials used in X-ray CT

    SciTech Connect

    Rao, D.; Swapna, M; Cesareo, R; Brunetti, A; Akatsuka, T; Yuasa, T; Takeda, T; Gigante, G

    2010-01-01

    Synchrotron-based scattered radiation form low-contrast phantom materials prepared from polyethylene, polystyrene, nylon, and Plexiglas is used as test objects in X-ray CT was examined with 8, 10 and 12 keV X-rays. These phantom materials of medical interest will contains varying proportions of low atomic number elements. The assessment will allowed us to estimate the fluorescence to total scattered radiation. Detected the fluorescence spectra and the associated scattered radiation from calcium hydroxyapatite phantom with 8, 10 and 12 keV synchrotron X-rays. Samples with Bonefil (60% and 70% of calcium hydroxyapatite) and Bone cream (35-45% of calcium hydroxyapatite), were used. Utilized the X-ray micro-spectroscopy beamline facility, X27A, available at NSLS, BNL, USA. The primary beam with a spot size of the order of {approx}10 {micro}m, has been used for focusing. With this spatial resolution and high flux throuput, the synchrotron-based scattered radiation from the phantom materials were measured using a liquid-nitrogen-cooled 13-element energy-dispersive high-purity germanium detector.

  15. New possibilities in nanoscale surface structure diagnostics using X-ray standing waves under conditions of continuous resonant X-ray Raman scattering

    NASA Astrophysics Data System (ADS)

    Zel'Tser, I. A.; Kukushkin, S. A.; Moos, E. N.

    2008-07-01

    The main principles, new possibilities, and instrumental implementations of a structure-sensitive spectroscopy of the surface of condensed media probed by X-ray standing waves (XSWs) are considered in the case of electron emission under the action of continuous resonant X-ray Raman scattering. It is shown that prospects for the development and use of the new possibilities offered by the XSW method for surface investigations are related to the creation of a set of specific experimental equipment and special sources of synchrotron radiation.

  16. Dosimetry of Microdistributed Dose-Enhancing Agents in X-ray Synchrotron Binary Therapy

    NASA Astrophysics Data System (ADS)

    Hugtenburg, Richard P.

    2010-07-01

    Monte Carlo based modelling of the dose distribution in the vicinity of concentrates of iodine (I) and gold (Au) binary radiotherapy agents has been performed for monochromatised synchrotron X-rays. While the KERMA approximation, which ignores electron transport, is often acceptable for kilovoltage X-ray dosimetry in X-ray binary therapy, the range of photoelectrons and Auger electrons may be significant when compared to the microdostributed structure of the binary compound in which case corrections to the approximation may be necessary. Dose is calculated using EGSnrc for microdistributions associated with X-ray radiation synovecotomy, where iodine is taken up in the synovial lining. Dose as a function of the volume of aggregation for an Au-based contrast agent such as Au nanoparticles, ranging in diameter from 5 micron to 100 micron, were calculated using EGSnrc and Penelope, showing that the dose varies slowly for 90 keV X-rays, where much of the dose delivered by short range photoelectrons while 80 keV X-rays, just below the K-edge of Au (80.729 keV) increases linearly with diameter. In general the dose varies slowly as a function of volume suggesting that only small corrections will be needed to account for effects due to the failure of electronic equilibrium.

  17. Dosimetry of Microdistributed Dose-Enhancing Agents in X-ray Synchrotron Binary Therapy

    SciTech Connect

    Hugtenburg, Richard P.

    2010-07-23

    Monte Carlo based modelling of the dose distribution in the vicinity of concentrates of iodine (I) and gold (Au) binary radiotherapy agents has been performed for monochromatised synchrotron X-rays. While the KERMA approximation, which ignores electron transport, is often acceptable for kilovoltage X-ray dosimetry in X-ray binary therapy, the range of photoelectrons and Auger electrons may be significant when compared to the microdostributed structure of the binary compound in which case corrections to the approximation may be necessary. Dose is calculated using EGSnrc for microdistributions associated with X-ray radiation synovecotomy, where iodine is taken up in the synovial lining. Dose as a function of the volume of aggregation for an Au-based contrast agent such as Au nanoparticles, ranging in diameter from 5 micron to 100 micron, were calculated using EGSnrc and Penelope, showing that the dose varies slowly for 90 keV X-rays, where much of the dose delivered by short range photoelectrons while 80 keV X-rays, just below the K-edge of Au (80.729 keV) increases linearly with diameter. In general the dose varies slowly as a function of volume suggesting that only small corrections will be needed to account for effects due to the failure of electronic equilibrium.

  18. The recent development of an X-ray grating interferometer at Shanghai Synchrotron Radiation Facility

    NASA Astrophysics Data System (ADS)

    Sun, Haohua; Kou, Bingquan; Xi, Yan; Qi, Juncheng; Sun, Jianqi; Mohr, Jürgen; Börner, Martin; Zhao, Jun; Xu, Lisa X.; Xiao, Tiqiao; Wang, Yujie

    2012-07-01

    An X-ray grating interferometer has been installed at Shanghai Synchrotron Radiation Facility (SSRF). Three sets of phase gratings were designed to cover the wide X-ray energy range needed for biological and soft material imaging capabilities. The performance of the grating interferometer has been evaluated by a tomography study of a PMMA particle packing and a new born mouse chest. In the mouse chest study, the carotid artery and carotid vein inside the mouse can be identified in situ without contrast agents.

  19. Synchrotron-based X-ray computed tomography during compression loading of cellular materials

    DOE PAGESBeta

    Cordes, Nikolaus L.; Henderson, Kevin; Stannard, Tyler; Williams, Jason J.; Xiao, Xianghui; Robinson, Mathew W. C.; Schaedler, Tobias A.; Chawla, Nikhilesh; Patterson, Brian M.

    2015-04-29

    Three-dimensional X-ray computed tomography (CT) of in situ dynamic processes provides internal snapshot images as a function of time. Tomograms are mathematically reconstructed from a series of radiographs taken in rapid succession as the specimen is rotated in small angular increments. In addition to spatial resolution, temporal resolution is important. Thus temporal resolution indicates how close together in time two distinct tomograms can be acquired. Tomograms taken in rapid succession allow detailed analyses of internal processes that cannot be obtained by other means. This article describes the state-of-the-art for such measurements acquired using synchrotron radiation as the X-ray source.

  20. The recent development of an X-ray grating interferometer at Shanghai Synchrotron Radiation Facility

    SciTech Connect

    Sun Haohua; Kou Bingquan; Xi Yan; Qi Juncheng; Sun Jianqi; Mohr, Juergen; Boerner, Martin; Zhao Jun; Xu, Lisa X.; Xiao Tiqiao; Wang Yujie

    2012-07-31

    An X-ray grating interferometer has been installed at Shanghai Synchrotron Radiation Facility (SSRF). Three sets of phase gratings were designed to cover the wide X-ray energy range needed for biological and soft material imaging capabilities. The performance of the grating interferometer has been evaluated by a tomography study of a PMMA particle packing and a new born mouse chest. In the mouse chest study, the carotid artery and carotid vein inside the mouse can be identified in situ without contrast agents.

  1. Synchrotron-based X-ray computed tomography during compression loading of cellular materials

    SciTech Connect

    Cordes, Nikolaus L.; Henderson, Kevin; Stannard, Tyler; Williams, Jason J.; Xiao, Xianghui; Robinson, Mathew W. C.; Schaedler, Tobias A.; Chawla, Nikhilesh; Patterson, Brian M.

    2015-04-29

    Three-dimensional X-ray computed tomography (CT) of in situ dynamic processes provides internal snapshot images as a function of time. Tomograms are mathematically reconstructed from a series of radiographs taken in rapid succession as the specimen is rotated in small angular increments. In addition to spatial resolution, temporal resolution is important. Thus temporal resolution indicates how close together in time two distinct tomograms can be acquired. Tomograms taken in rapid succession allow detailed analyses of internal processes that cannot be obtained by other means. This article describes the state-of-the-art for such measurements acquired using synchrotron radiation as the X-ray source.

  2. Dynamics of barite growth in porous media quantified by in situ synchrotron X-ray tomography

    NASA Astrophysics Data System (ADS)

    Godinho, jose; Gerke, kirill

    2016-04-01

    Current models used to formulate mineral sequestration strategies of dissolved contaminants in the bedrock often neglect the effect of confinement and the variation of reactive surface area with time. In this work, in situ synchrotron X-ray micro-tomography is used to quantify barite growth rates in a micro-porous structure as a function of time during 13.5 hours with a resolution of 1 μm. Additionally, the 3D porous network at different time frames are used to simulate the flow velocities and calculate the permeability evolution during the experiment. The kinetics of barite growth under porous confinement is compared with the kinetics of barite growth on free surfaces in the same fluid composition. Results are discussed in terms of surface area normalization and the evolution of flow velocities as crystals fill the porous structure. During the initial hours the growth rate measured in porous media is similar to the growth rate on free surfaces. However, as the thinner flow paths clog the growth rate progressively decreases, which is correlated to a decrease of local flow velocity. The largest pores remain open, enabling growth to continue throughout the structure. Quantifying the dynamics of mineral precipitation kinetics in situ in 4D, has revealed the importance of using a time dependent reactive surface area and accounting for the local properties of the porous network, when formulating predictive models of mineral precipitation in porous media.

  3. X-Ray Synchrotron-emitting Fe-rich Ejecta in Supernova Remnant RCW 86

    NASA Astrophysics Data System (ADS)

    Rho, Jeonghee; Dyer, Kristy K.; Borkowski, Kazimierz J.; Reynolds, Stephen P.

    2002-12-01

    Supernova remnants may exhibit both thermal and nonthermal X-ray emission. In a previous study with ASCA data, we found that the middle-aged supernova remnant RCW 86 showed evidence for both processes, and we predicted that observations with much higher spatial resolution would distinguish harder X-rays, which we proposed were primarily synchrotron emission, from softer, thermal X-rays. Here we describe Chandra observations that amply confirm our predictions. Striking differences in the morphology of X-rays below 1 keV and above 2 keV point to a different physical origin. Hard X-ray emission is correlated fairly well with the edges of regions of radio emission, suggesting that these are the locations of shock waves at which both short-lived X-ray-emitting electrons and longer lived radio-emitting electrons are accelerated. Soft X-rays are spatially well correlated with optical emission from nonradiative shocks, which are almost certainly portions of the outer blast wave. These soft X-rays are well fitted with simple thermal plane-shock models. Harder X-rays show Fe Kα emission and are well described with a similar soft thermal component, but a much stronger synchrotron continuum dominating above 2 keV, and a strong Fe Kα line. Quantitative analysis of this line and the surrounding continuum shows that it cannot be produced by thermal emission from a cosmic-abundance plasma; the ionization time is too short, as shown by both the low centroid energy (6.4 keV) and the absence of oxygen lines below 1 keV. Instead, a model of a plane shock in Fe-rich ejecta, with a synchrotron continuum, provides a natural explanation. This requires that reverse shocks in ejecta be accelerating electrons to energies of order 50 TeV. We show that maximum energies of this order can be produced by radiation-limited diffusive shock acceleration at the reverse shocks. In the Appendix, we demonstrate that an explanation of the continuum as being due to nonthermal bremsstrahlung is unlikely.

  4. Hard-X-ray magnetic microscopy and local magnetization analysis using synchrotron radiation.

    PubMed

    Suzuki, Motohiro

    2014-11-01

    X-ray measurement offers several useful features that are unavailable from other microscopic means including electron-based techniques. By using X-rays, one can observe the internal parts of a thick sample. This technique basically requires no high vacuum environment such that measurements are feasible for wet specimens as well as under strong electric and magnetic fields and even at a high pressure. X-ray spectroscopy using core excitation provides element-selectivity with significant sensitivities to the chemical states and atomic magnetic moments in the matter. Synchrotron radiation sources produce a small and low-divergent X-ray beam, which can be converged to a spot with the size of a micrometer or less using X-ray focusing optics. The recent development in the focusing optics has been driving X-ray microscopy, which has already gone into the era of X-ray nanoscopy. With the use of the most sophisticated focusing devices, an X-ray beam of 7-nm size has successfully been achieved [1]. X-ray microscopy maintains above-mentioned unique features of X-ray technique, being a perfect complement to electron microscopy.In this paper, we present recent studies on magnetic microscopy and local magnetic analysis using hard X-rays. The relevant instrumentation developments are also described. The X-ray nanospectroscopy station of BL39XU at SPring-8 is equipped with a focusing optics consisting of two elliptic mirrors, and a focused X-ray beam with the size of 100 × 100 nm(2) is available [2]. Researchers can perform X-ray absorption spectroscopy: nano-XAFS (X-ray absorption fine structure) using the X-ray beam as small as 100 nm. The available X-ray energy is from 5 to 16 keV, which allows nano-XAFS study at the K edges of 3d transition metals, L edges of rare-earth elements and 5d noble metals. Another useful capability of the nanoprobe is X-ray polarization tunability, enabling magnetic circular dichroism (XMCD) spectroscopy with a sub-micrometer resolution. Scanning

  5. Antioxidant protects blood-testis barrier against synchrotron radiation X-ray-induced disruption

    PubMed Central

    Zhang, Tingting; Liu, Tengyuan; Shao, Jiaxiang; Sheng, Caibin; Hong, Yunyi; Ying, Weihai; Xia, Weiliang

    2015-01-01

    Synchrotron radiation (SR) X-ray has wide biomedical applications including high resolution imaging and brain tumor therapy due to its special properties of high coherence, monochromaticity and high intensity. However, its interaction with biological tissues remains poorly understood. In this study, we used the rat testis as a model to investigate how SR X-ray would induce tissue responses, especially the blood-testis barrier (BTB) because BTB dynamics are critical for spermatogenesis. We irradiated the male gonad with increasing doses of SR X-ray and obtained the testicles 1, 10 and 20 d after the exposures. The testicle weight and seminiferous tubule diameter reduced in a dose- and time-dependent manner. Cryosections of testes were stained with tight junction (TJ) component proteins such as occludin, claudin-11, JAM-A and ZO-1. Morphologically, increasing doses of SR X-ray consistently induced developing germ cell sloughing from the seminiferous tubules, accompanied by shrinkage of the tubules. Interestingly, TJ constituent proteins appeared to be induced by the increasing doses of SR X-ray. Up to 20 d after SR X-ray irradiation, there also appeared to be time-dependent changes on the steady-state level of these protein exhibiting differential patterns at 20-day after exposure, with JAM-A/claudin-11 still being up-regulated whereas occludin/ZO-1 being down-regulated. More importantly, the BTB damage induced by 40 Gy of SR X-ray could be significantly attenuated by antioxidant N-Acetyl-L-Cysteine (NAC) at a dose of 125 mg/kg. Taken together, our studies characterized the changes of TJ component proteins after SR X-ray irradiation, illustrating the possible protective effects of antioxidant NAC to BTB integrity. PMID:26413412

  6. Energy dispersive X-ray diffraction in the diamond anvil, high-pressure apparatus - Comparison of synchrotron and conventional X-ray sources

    NASA Technical Reports Server (NTRS)

    Spain, I. L.; Black, D. R.

    1985-01-01

    The use of both conventional fixed-anode X-ray sources and synchrotron radiation to carry out energy-dispersive X-ray diffraction experiments at high pressure in a diamond anvil cell, is discussed. The photon flux at the sample and at the detector for the two cases are compared and the results are presented in graphs. It is shown that synchrotron radiation experiments can be performed with nearly two orders of magnitude increase in data rate if superior detectors and detector electronics are available.

  7. Inclined-incidence quasi-Fresnel lens for prefocusing of synchrotron radiation x-ray beams

    NASA Astrophysics Data System (ADS)

    Kagoshima, Yasushi; Takano, Hidekazu; Takeda, Shingo

    2012-10-01

    An inclined-incidence quasi-Fresnel lens made of acrylic resin has been developed for prefocusing in synchrotron radiation x-ray beamlines. By inclining the lens, the grating aspect ratio is large enough for x-ray use. As it operates in transmission mode with negligible beam deflection and offset, little additional equipment is needed to introduce it into existing beamlines. It is fabricated by sheet-press forming, enabling inexpensive mass production. The prototype was able to focus a 730-μm-wide beam to a width of 80 μm with a photon flux density gain of 5.6 at an x-ray energy of 10 keV.

  8. Inclined-incidence quasi-Fresnel lens for prefocusing of synchrotron radiation x-ray beams

    SciTech Connect

    Kagoshima, Yasushi; Takano, Hidekazu; Takeda, Shingo

    2012-10-15

    An inclined-incidence quasi-Fresnel lens made of acrylic resin has been developed for prefocusing in synchrotron radiation x-ray beamlines. By inclining the lens, the grating aspect ratio is large enough for x-ray use. As it operates in transmission mode with negligible beam deflection and offset, little additional equipment is needed to introduce it into existing beamlines. It is fabricated by sheet-press forming, enabling inexpensive mass production. The prototype was able to focus a 730-{mu}m-wide beam to a width of 80 {mu}m with a photon flux density gain of 5.6 at an x-ray energy of 10 keV.

  9. Optimizing Monocapillary Optics for Synchrotron X-ray Diffraction, Fluorescence Imaging, and Spectroscopy Applications

    SciTech Connect

    Bilderback, Donald H.; Kazimirov, Alexander; Gillilan, Richard; Cornaby, Sterling; Woll, Arthur; Zha, Chang-Sheng; Huang Rong

    2007-01-19

    A number of synchrotron x-ray applications such as powder diffraction in diamond anvil cells, microbeam protein crystallography, x-ray fluorescence imaging, etc. can benefit from using hollow glass monocapillary optics to improve the flux per square micron on a sample. We currently draw glass tubing into the desired elliptical shape so that only one-bounce under total reflection conditions is needed to bring the x-ray beam to a focus at a 25 to 50 mm distance beyond the capillary tip. For modest focal spot sizes of 10 to 20 microns, we can increase the intensity per square micron by factors of 10 to 1000. We show some of the results obtained at CHESS and Hasylab with capillaries focusing 5 to 40 keV radiation, their properties, and how even better the experimental results could be if more ideal capillaries were fabricated in the future.

  10. Diamond monochromator for high heat flux synchrotron x-ray beams

    SciTech Connect

    Khounsary, A.M.; Smither, R.K.; Davey, S.; Purohit, A.

    1993-01-28

    Single crystal silicon has been the material of choice for x-ray monochromators for the past several decades. However, the need for suitable monochromators to handle the high heat load of the next generation synchrotron x-ray beams on the one hand and the rapid and on-going advances in synthetic diamond technology on the other make a compelling case for the consideration of a diamond monochromator system. In this paper, we consider various aspects, advantages and disadvantages, and promises and pitfalls of such a system and evaluate the comparative performance of a diamond monochromator subjected to the high heat load of the most powerful x-ray beam that will become available in the next few years. The results of experiments performed to evaluate the diffraction properties of a currently available synthetic single crystal diamond are also presented. Fabrication of a diamond-based monochromator is within present technical means.

  11. Diamond monochromator for high heat flux synchrotron x-ray beams

    SciTech Connect

    Khounsary, A.M.; Smither, R.K.; Davey, S.; Purohit, A.

    1992-12-01

    Single crystal silicon has been the material of choice for x-ray monochromators for the past several decades. However, the need for suitable monochromators to handle the high heat load of the next generation synchrotron x-ray beams on the one hand and the rapid and on-going advances in synthetic diamond technology on the other make a compelling case for the consideration of a diamond mollochromator system. In this Paper, we consider various aspects, advantage and disadvantages, and promises and pitfalls of such a system and evaluate the comparative an monochromator subjected to the high heat load of the most powerful x-ray beam that will become available in the next few years. The results of experiments performed to evaluate the diffraction properties of a currently available synthetic single crystal diamond are also presented. Fabrication of diamond-based monochromator is within present technical means.

  12. Optimizing Monocapillary Optics for Synchrotron X-ray Diffraction, Fluorescence Imaging, and Spectroscopy Applications

    NASA Astrophysics Data System (ADS)

    Bilderback, Donald H.; Kazimirov, Alexander; Gillilan, Richard; Cornaby, Sterling; Woll, Arthur; Zha, Chang-Sheng; Huang, Rong

    2007-01-01

    A number of synchrotron x-ray applications such as powder diffraction in diamond anvil cells, microbeam protein crystallography, x-ray fluorescence imaging, etc. can benefit from using hollow glass monocapillary optics to improve the flux per square micron on a sample. We currently draw glass tubing into the desired elliptical shape so that only one-bounce under total reflection conditions is needed to bring the x-ray beam to a focus at a 25 to 50 mm distance beyond the capillary tip. For modest focal spot sizes of 10 to 20 microns, we can increase the intensity per square micron by factors of 10 to 1000. We show some of the results obtained at CHESS and Hasylab with capillaries focusing 5 to 40 keV radiation, their properties, and how even better the experimental results could be if more ideal capillaries were fabricated in the future.

  13. Nanoscale chemical imaging using synchrotron x-ray enhanced scanning tunneling microscopy

    SciTech Connect

    Rose, Volker; Freeland, John W.

    2010-06-23

    The combination of synchrotron radiation with scanning tunneling microscopy provides a promising new concept for chemical imaging of nanoscale structures. It employs detection of local x-ray absorption, which directly yields chemical, electronic, and magnetic sensitivity. The study of the tip current in the far field (800 nm tip/sample separation) shows that insulator-coated tips have to be considered in order to reduce the background from stray photoelectron. A picture of the different channels contributing to the x-ray enhanced STM process is proposed. If during electron tunneling the sample is illuminated with monochromatic x-rays, characteristic absorption will arise, and core electrons are excited, which might modulate the conventional tunnel current and facilitate chemical imaging at the nanoscale.

  14. Concentration of synchrotron beams by means of monolithic polycapillary x-ray optics

    SciTech Connect

    Ullrich, J.B.; Klotzko, I.L. |; Huang, K.G.; Owens, S.M.; Aloisi, D.C.; Hofmann, F.A.; Gao, N.; Gibson, W.M.

    1995-08-01

    Capillary Optics have proven to be a valuable tool for concentrating synchrotron radiation. Single tapered capillaries are used at several facilities. However, most of these optics collect only over a small area. this can be overcome by using larger capillary structures. Polycapillary optics can deflect x-rays by larger angles than other x-ray optics that use only one or two reflections. Conventional x-ray optics that achieve similar deflections, are much more energy selective than capillaries. Therefore, capillaries achieve very short focal distances for a wide range of energies. The measurements shown here represent first tests performed with polycapillaries of large input diameter. The performance with respect to transmission efficiency and spot size was evaluated for a set of four very different prototypes. It is shown that a significant gain may be achieved if a spot size of the order of 0.1 mm is required. Further, some characteristics of the different optics are discussed.

  15. In-situ observations of catalytic surface reactions with soft x-rays under working conditions

    NASA Astrophysics Data System (ADS)

    Toyoshima, Ryo; Kondoh, Hiroshi

    2015-03-01

    Catalytic chemical reactions proceeding on solid surfaces are an important topic in fundamental science and industrial technologies such as energy conversion, pollution control and chemical synthesis. Complete understanding of the heterogeneous catalysis and improving its efficiency to an ultimate level are the eventual goals for many surface scientists. Soft x-ray is one of the prime probes to observe electronic and structural information of the target materials. Most studies in surface science using soft x-rays have been performed under ultra-high vacuum conditions due to the technical limitation, though the practical catalytic reactions proceed under ambient pressure conditions. However, recent developments of soft x-ray based techniques operating under ambient pressure conditions have opened a door to the in-situ observation of materials under realistic environments. The near-ambient-pressure x-ray photoelectron spectroscopy (NAP-XPS) using synchrotron radiation enables us to observe the chemical states of surfaces of condensed matters under the presence of gas(es) at elevated pressures, which has been hardly conducted with the conventional XPS technique. Furthermore, not only the NAP-XPS but also ambient-pressure compatible soft x-ray core-level spectroscopies, such as near-edge absorption fine structure (NEXAFS) and x-ray emission spectroscopy (XES), have been significantly contributing to the in-situ observations. In this review, first we introduce recent developments of in-situ observations using soft x-ray techniques and current status. Then we present recent new findings on catalytically active surfaces using soft x-ray techniques, particularly focusing on the NAP-XPS technique. Finally we give a perspective on the future direction of this emerging technique.

  16. Image Alignment for Tomography Reconstruction from Synchrotron X-Ray Microscopic Images

    PubMed Central

    Cheng, Chang-Chieh; Chien, Chia-Chi; Chen, Hsiang-Hsin; Hwu, Yeukuang; Ching, Yu-Tai

    2014-01-01

    A synchrotron X-ray microscope is a powerful imaging apparatus for taking high-resolution and high-contrast X-ray images of nanoscale objects. A sufficient number of X-ray projection images from different angles is required for constructing 3D volume images of an object. Because a synchrotron light source is immobile, a rotational object holder is required for tomography. At a resolution of 10 nm per pixel, the vibration of the holder caused by rotating the object cannot be disregarded if tomographic images are to be reconstructed accurately. This paper presents a computer method to compensate for the vibration of the rotational holder by aligning neighboring X-ray images. This alignment process involves two steps. The first step is to match the “projected feature points” in the sequence of images. The matched projected feature points in the - plane should form a set of sine-shaped loci. The second step is to fit the loci to a set of sine waves to compute the parameters required for alignment. The experimental results show that the proposed method outperforms two previously proposed methods, Xradia and SPIDER. The developed software system can be downloaded from the URL, http://www.cs.nctu.edu.tw/~chengchc/SCTA or http://goo.gl/s4AMx. PMID:24416264

  17. High resolution hard x-ray microscope on a second generation synchrotron source

    SciTech Connect

    Tian Yangchao; Li Wenjie; Chen Jie; Liu Longhua; Liu Gang; Tian Jinping; Xiong Ying; Tkachuk, Andrei; Gelb, Jeff; Hsu, George; Yun Wenbing

    2008-10-15

    A full-field, transmission x-ray microscope (TXM) operating in the energy range of 7-11 keV has been installed at the U7A beamline at the National Synchrotron Radiation Laboratory, a second generation synchrotron source operating at 0.8 GeV. Although the photon flux at sample position in the operating energy range is significantly low due to its relatively large emittance, the TXM can get high quality x-ray images with a spatial resolution down to 50 nm with acceptable exposure time. This TXM operates in either absorption or Zernike phase contrast mode with similar resolution. This TXM is a powerful analytical tool for a wide range of scientific areas, especially studies on nanoscale phenomena and structural imaging in biology, materials science, and environmental science. We present here the property of the x-ray source, beamline design, and the operation and key optical components of the x-ray TXM. Plans to improve the throughput of the TXM will be discussed.

  18. High resolution hard x-ray microscope on a second generation synchrotron source.

    PubMed

    Tian, Yangchao; Li, Wenjie; Chen, Jie; Liu, Longhua; Liu, Gang; Tkachuk, Andrei; Tian, Jinping; Xiong, Ying; Gelb, Jeff; Hsu, George; Yun, Wenbing

    2008-10-01

    A full-field, transmission x-ray microscope (TXM) operating in the energy range of 7-11 keV has been installed at the U7A beamline at the National Synchrotron Radiation Laboratory, a second generation synchrotron source operating at 0.8 GeV. Although the photon flux at sample position in the operating energy range is significantly low due to its relatively large emittance, the TXM can get high quality x-ray images with a spatial resolution down to 50 nm with acceptable exposure time. This TXM operates in either absorption or Zernike phase contrast mode with similar resolution. This TXM is a powerful analytical tool for a wide range of scientific areas, especially studies on nanoscale phenomena and structural imaging in biology, materials science, and environmental science. We present here the property of the x-ray source, beamline design, and the operation and key optical components of the x-ray TXM. Plans to improve the throughput of the TXM will be discussed. PMID:19044720

  19. High resolution hard x-ray microscope on a second generation synchrotron source

    NASA Astrophysics Data System (ADS)

    Tian, Yangchao; Li, Wenjie; Chen, Jie; Liu, Longhua; Liu, Gang; Tkachuk, Andrei; Tian, Jinping; Xiong, Ying; Gelb, Jeff; Hsu, George; Yun, Wenbing

    2008-10-01

    A full-field, transmission x-ray microscope (TXM) operating in the energy range of 7-11 keV has been installed at the U7A beamline at the National Synchrotron Radiation Laboratory, a second generation synchrotron source operating at 0.8 GeV. Although the photon flux at sample position in the operating energy range is significantly low due to its relatively large emittance, the TXM can get high quality x-ray images with a spatial resolution down to 50 nm with acceptable exposure time. This TXM operates in either absorption or Zernike phase contrast mode with similar resolution. This TXM is a powerful analytical tool for a wide range of scientific areas, especially studies on nanoscale phenomena and structural imaging in biology, materials science, and environmental science. We present here the property of the x-ray source, beamline design, and the operation and key optical components of the x-ray TXM. Plans to improve the throughput of the TXM will be discussed.

  20. Fast response amplitude scintillation detector for X-ray synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Dementyev, E. N.; Sheromov, M. A.; Sokolov, A. S.

    1986-05-01

    The present paper describes a scintillation detector for X-ray synchrotron radiation. This detector has been created on the basis of a scintillator and a photoelectron multiplier (FEU-130) and its construction allows one to use the specific features of the time characteristics of synchrotron radiation from the electron storage ring. In a given range of amplitudes, the detector electronics makes a 64-channel amplitude analysis of the FEU-130 signal strobed by the revolution frequency of an electron bunch in the storage ring ( f0 = 818 kHz). There is the possibility of operating the detector at high intensities of the monochromatic radiation incident on the scintillator. Such a possibility is directly provided by the time structure of SR and is not realizable with the use of other X-ray sources. The detector will find wide application in studies on X-ray structural analysis, transmission and fluorescent EXAFS- and XANES-spectroscopy, transmission scanning microscopy and microtomography, calibration of X-ray detectors and as a monitor on SR beams from the storage ring VEPP-4.

  1. Progress in Cell Marking for Synchrotron X-ray Computed Tomography

    SciTech Connect

    Hall, Christopher; Sturm, Erica; Schultke, Elisabeth; Arfelli, Fulvia; Astolfo, Alberto; Menk, Ralf-Hendrik; Juurlink, Bernhard H. J.

    2010-07-23

    Recently there has been an increase in research activity into finding ways of marking cells in live animals for pre-clinical trials. Development of certain drugs and other therapies crucially depend on tracking particular cells or cell types in living systems. Therefore cell marking techniques are required which will enable longitudinal studies, where individuals can be examined several times over the course of a therapy or study. The benefits of being able to study both disease and therapy progression in individuals, rather than cohorts are clear. The need for high contrast 3-D imaging, without harming or altering the biological system requires a non-invasive yet penetrating imaging technique. The technique will also have to provide an appropriate spatial and contrast resolution. X-ray computed tomography offers rapid acquisition of 3-D images and is set to become one of the principal imaging techniques in this area. Work by our group over the last few years has shown that marking cells with gold nano-particles (GNP) is an effective means of visualising marked cells in-vivo using x-ray CT. Here we report the latest results from these studies. Synchrotron X-ray CT images of brain lesions in rats taken using the SYRMEP facility at the Elettra synchrotron in 2009 have been compared with histological examination of the tissues. Some deductions are drawn about the visibility of the gold loaded cells in both light microscopy and x-ray imaging.

  2. Progress in Cell Marking for Synchrotron X-ray Computed Tomography

    NASA Astrophysics Data System (ADS)

    Hall, Christopher; Sturm, Erica; Schultke, Elisabeth; Arfelli, Fulvia; Menk, Ralf-Hendrik; Astolfo, Alberto; Juurlink, Bernhard H. J.

    2010-07-01

    Recently there has been an increase in research activity into finding ways of marking cells in live animals for pre-clinical trials. Development of certain drugs and other therapies crucially depend on tracking particular cells or cell types in living systems. Therefore cell marking techniques are required which will enable longitudinal studies, where individuals can be examined several times over the course of a therapy or study. The benefits of being able to study both disease and therapy progression in individuals, rather than cohorts are clear. The need for high contrast 3-D imaging, without harming or altering the biological system requires a non-invasive yet penetrating imaging technique. The technique will also have to provide an appropriate spatial and contrast resolution. X-ray computed tomography offers rapid acquisition of 3-D images and is set to become one of the principal imaging techniques in this area. Work by our group over the last few years has shown that marking cells with gold nano-particles (GNP) is an effective means of visualising marked cells in-vivo using x-ray CT. Here we report the latest results from these studies. Synchrotron X-ray CT images of brain lesions in rats taken using the SYRMEP facility at the Elettra synchrotron in 2009 have been compared with histological examination of the tissues. Some deductions are drawn about the visibility of the gold loaded cells in both light microscopy and x-ray imaging.

  3. Image alignment for tomography reconstruction from synchrotron X-ray microscopic images.

    PubMed

    Cheng, Chang-Chieh; Chien, Chia-Chi; Chen, Hsiang-Hsin; Hwu, Yeukuang; Ching, Yu-Tai

    2014-01-01

    A synchrotron X-ray microscope is a powerful imaging apparatus for taking high-resolution and high-contrast X-ray images of nanoscale objects. A sufficient number of X-ray projection images from different angles is required for constructing 3D volume images of an object. Because a synchrotron light source is immobile, a rotational object holder is required for tomography. At a resolution of 10 nm per pixel, the vibration of the holder caused by rotating the object cannot be disregarded if tomographic images are to be reconstructed accurately. This paper presents a computer method to compensate for the vibration of the rotational holder by aligning neighboring X-ray images. This alignment process involves two steps. The first step is to match the "projected feature points" in the sequence of images. The matched projected feature points in the x-θ plane should form a set of sine-shaped loci. The second step is to fit the loci to a set of sine waves to compute the parameters required for alignment. The experimental results show that the proposed method outperforms two previously proposed methods, Xradia and SPIDER. The developed software system can be downloaded from the URL, http://www.cs.nctu.edu.tw/~chengchc/SCTA or http://goo.gl/s4AMx. PMID:24416264

  4. Apparatus and Techniques for Time-resolved Synchrotron X-ray Diffraction using Diamond Anvil Cells

    NASA Astrophysics Data System (ADS)

    Smith, J.; Sinogeikin, S. V.; Lin, C.; Rod, E.; Bai, L.; Shen, G.

    2015-12-01

    Complementary advances in synchrotron sources, x-ray optics, area detectors, and sample environment control have recently made possible many time-resolved experimental techniques for studying materials at extreme pressure and temperature conditions. The High Pressure Collaborative Access Team (HPCAT) at the Advanced Photon Source has made a sustained effort to assemble a powerful collection of high-pressure apparatus for time-resolved research, and considerable time has been invested in developing techniques for collecting high-quality time-resolved x-ray scattering data. Herein we present key aspects of the synchrotron beamline and ancillary equipment, including source considerations, rapid (de)compression apparatus, high frequency imaging detectors, and software suitable for processing large volumes of data. A number of examples are presented, including fast equation of state measurements, compression rate dependent synthesis of metastable states in silicon and germanium, and ultrahigh compression rates using a piezoelectric driven diamond anvil cell.

  5. National Synchrotron Light Source users manual: Guide to the VUV and x-ray beam lines

    SciTech Connect

    Gmuer, N.F.; White-DePace, S.M.

    1987-08-01

    The success of the National Synchrotron Light Source in the years to come will be based, in large part, on the size of the users community and the diversity of the scientific disciplines represented by these users. In order to promote this philosophy, this National Synchrotron Light Source (NSLS) Users Manual: Guide to the VUV and X-Ray Beam Lines, has been published. This manual serves a number of purposes. In an effort to attract new research, it will present to the scientific community-at-large the current and projected architecture and capabilities of the various VUV and x-ray beam lines and storage rings. We anticipate that this publication will be updated periodically in order to keep pace with the constant changes at the NSLS.

  6. Synchrotron X-Ray Reciprocal Space Mapping, Topography and Diffraction Resolution Studies of Macromolecular Crystal Quality

    NASA Technical Reports Server (NTRS)

    Boggon, T. J.; Helliwell, J. R.; Judge, Russell A.; Siddons, D. P.; Snell, Edward H.; Stojanoff, V.

    2000-01-01

    A comprehensive study of microgravity and ground grown chicken egg white lysozyme crystals is presented using synchrotron X-ray reciprocal space mapping, topography techniques and diffraction resolution. Microgravity crystals displayed, on average, reduced intrinsic mosaicities but no differences in terms of stress over their earth grown counterparts. Topographic analysis revealed that in the microgravity case the majority of the crystal was contributing to the peak of the reflection at the appropriate Bragg angle. In the earth case at the diffraction peak only a small volume of the crystal contributed to the intensity. The techniques prove to be highly complementary with the reciprocal space mapping providing a quantitative measure of the crystal mosaicity and stress (or variation in lattice spacing) and topography providing a qualitative overall assessment of the crystal in terms of its X-ray diffraction properties. Structural data collection was also carried out both at the synchrotron and in the laboratory.

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

    SciTech Connect

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

    2012-03-13

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

  8. Tracing X-rays through an L-shaped laterally graded multilayer mirror: a synchrotron application.

    PubMed

    Honnicke, Marcelo Goncalves; Huang, Xianrong; Keister, Jeffrey W; Kodituwakku, Chaminda Nalaka; Cai, Yong Q

    2010-05-01

    A theoretical model to trace X-rays through an L-shaped (nested or Montel Kirkpatrick-Baez mirrors) laterally graded multilayer mirror to be used in a synchrotron application is presented. The model includes source parameters (size and divergence), mirror figure (parabolic and elliptic), multilayer parameters (reflectivity, which depends on layer material, thickness and number of layers) and figure errors (slope error, roughness, layer thickness fluctuation Deltad/d and imperfection in the corners). The model was implemented through MATLAB/OCTAVE scripts, and was employed to study the performance of a multilayer mirror designed for the analyzer system of an ultrahigh-resolution inelastic X-ray scattering spectrometer at National Synchrotron Light Source II. The results are presented and discussed. PMID:20400833

  9. Characterization of Nano and Mesoscale Deformation Structures with Intense X-ray Synchrotron Sources

    SciTech Connect

    Ice, G.E.; Barabash, R.I.; Walker, F.J.

    2010-07-19

    Advanced polychromatic microdiffraction is sensitive to the organization of dislocations and other defects that rotate the lattice planes. Using ultra-brilliant third-generation synchrotron sources and non-dispersive X-ray focusing optics, it is now possible to analyze individual dislocation cells and walls at a submicron scale that cannot be probed by traditional methods. The method is applied to an Ir weld sample to illustrate how microdiffraction can be used to determine the locally active dislocation system.

  10. Synchrotron X-ray Investigations of Mineral-Microbe-Metal Interactions

    SciTech Connect

    Kemner, Kenneth M.; O'Loughlin, Edward J.; Kelly, Shelly D.; Boyanov, Maxim I.

    2008-06-06

    Interactions between microbes and minerals can play an important role in metal transformations (i.e. changes to an element's valence state, coordination chemistry, or both), which can ultimately affect that element's mobility. Mineralogy affects microbial metabolism and ecology in a system; microbes, in turn, can affect the system's mineralogy. Increasingly, synchrotron-based X-ray experiments are in routine use for determining an element's valence state and coordination chemistry, as well as for examining the role of microbes in metal transformations.

  11. Synchrotron X-ray and ab initio studies of beta-Si3N4.

    PubMed

    du Boulay, D; Ishizawa, N; Atake, T; Streltsov, V; Furuya, K; Munakata, F

    2004-08-01

    Almost absorption- and extinction-free single-crystal synchrotron X-ray diffraction data were measured at 150, 200 and 295 K for beta-Si3N4, silicon nitride, at a wavelength of 0.7 A. The true symmetry of this material has been the subject of minor controversy for several decades. No compelling evidence favouring the low-symmetry P6(3) model was identified in this study. PMID:15258397

  12. Applications of synchrotron x-ray fluorescence microprobe techniques to photochromic materials

    SciTech Connect

    Perry, D.L.

    1996-12-31

    Applications of synchrotron x-ray fluorescence microprobe techniques to photochromic materials are presented regarding dopant metal ions in the crystal matrices. Types of samples that are amenable to the technique will be discussed, along with sample format and experimental conditions. The chemical information that one can obtain from samples will be presented, and examples of copant contaminant studies in crystals will be given. New types of samples that are possible to study using this technique will be presented.

  13. A tunable wedge-shaped absorber for hard X-ray synchrotron applications.

    PubMed

    Krywka, C; Brix, M; Müller, M

    2014-07-01

    The concept of a concave aluminium wedge-shaped absorber for hard X-ray synchrotron beamlines is presented. Unlike the commonly used absorber types (fixed-thickness absorber sheets or binary exchangers of individual fixed absorbers), this concept allows a compact system, controlled with a single linear positioner, and provides a wide attenuation range as well as a precise tunability over a large energy range. Data were recorded at the Nanofocus Endstation of the MINAXS beamline, PETRA III, Hamburg, Germany. PMID:24971979

  14. Formation of secondary porosity in 4D Synchrotron X-ray tomography experiments

    NASA Astrophysics Data System (ADS)

    Fusseis, Florian; Liu, Jie; de Carlo, Francesco; Regenauer-Lieb, Klaus; Schrank, Christoph; Hough, Robert; Gessner, Klaus; Llana-Fúnez, Sergio; Faulkner, Dan; Wheeler, John

    2010-05-01

    Synchrotron X-ray tomography at the Advanced Photon Source (APS) allows to investigate secondary porosity in three dimensions on the nano- to microscale. We utilised the key advantage of the technique, the rapid data acquisition time (seconds to about half an hour/data set), to study the formation of porosity in natural rock samples in real time (4D). The spacious instrument setup in the experimental hutch allowed us to install an X-ray transparent furnace to heat millimetre-sized samples up to 230 °C (>400 °C in the next generation) in the X-ray beam. We focused on two porosity-generating mechanisms: thermal expansion cracking in Westerly granite and dehydration (volume loss/hydraulic fracturing) of Volterra gypsum. The spatial resolution was 1.3 micron in both experiments. We heated a 2mm diameter cylinder of Westerly Granite stepwise from 50 °C to 230 °C and then quenched it to investigate the effects of thermal expansion cracking on the three-dimensional porosity architecture. The sample was scanned after increasing the temperature in 10 °C steps to record the cracks formed during each heating interval. Preliminary analysis of the heterogeneous 4D displacement fields proved that the approach works well. We documented the opening and closing as well as interconnection of grain boundary- and intragranular cracks. A full quantification is currently under way. This experiment also serves to benchmark numerical simulations of thermal cracking that will be used to upscale the permeability evolution during heating (see abstract of Schrank et al.). A second heating experiment aimed at documenting the fluid escape pathways during the dehydration of gypsum to bassanite. We heated a gypsum sample to 115 °C for increasing periods of time. The reaction progress was directly observed in two-dimensional tomographic projections, 3D tomographic datasets were collected during cooling at 50 °C in between the heating intervals. The experiment demonstrated how a permeable

  15. Tracking picosecond molecular dynamics in solution using a suite of synchrotron-x-ray spectroscopic tools

    NASA Astrophysics Data System (ADS)

    March, Anne Marie; Doumy, Gilles; Kanter, Elliot P.; Lehmann, Stefan; Moonshiram, Dooshaye; Southworth, Stephen H.; Young, Linda; Assefa, Tadesse A.; Bressler, Christian; Gawelda, Wojciech; Németh, Zoltán; Vankó, György

    2015-03-01

    Laser-pump, X-ray-probe techniques are powerful tools for exploring molecular structural changes that occur in complex environments such as solutions, during a photo-initiated reaction. We are developing such methods using hard x-rays from the Advanced Photon Source, combining x-ray emission spectroscopy and x-ray absorption spectroscopy as probes of electronic and geometric structure and using high-power, MHz lasers as pumps. The high-duty-cycle pump-probe measurements efficiently utilize the synchrotron x-ray flux and enable high-fidelity measurements of the structures of transient intermediates. We present measurements on the model system [Fe(II)(CN)6]4- (ferrocyanide) in an aqueous solution after excitation with 355 nm and 266 nm laser light. The system undergoes two wavelength dependent reactions: photooxidation and photoaquation. Iron K-edge absorption spectra were obtained along with iron emission spectra. Our data support the presence of a previously unobserved pentacoordinated intermediate species in the photoaquation reaction. Its lifetime has been measured to be 4.6 ns and details of its structure will be discussed. The work was supported by the U.S. Department of Energy, Office of Science, Chemical Sciences, Geosciences, and Biosciences Division.

  16. High-energy synchrotron radiation x-ray microscopy: Present status and future prospects

    SciTech Connect

    Jones, K.W.; Gordon, B.M.; Spanne, P. ); Rivers, M.L.; Sutton, S.R. )

    1991-01-01

    High-energy radiation synchrotron x-ray microscopy is used to characterize materials of importance to the chemical and materials sciences and chemical engineering. The x-ray microscope (XRM) forms images of elemental distributions fluorescent x rays or images of mass distributions by measurement of the linear attenuation coefficient of the material. Distributions of sections through materials are obtained non-destructively using the technique of computed microtomography. The energy range of the x rays used for the XRM ranges from a few keV at the minimum value to more than 100 keV, which is sufficient to excite the K-edge of all naturally occurring elements. The work in progress at the Brookhaven NSLS X26 and X17 XRM is described in order to show the current status of the XRM. While there are many possible approaches to the XRM instrumentation, this instrument gives state-of-the-art performance in most respects and serves as a reasonable example of the present status of the instrumentation in terms of the spatial resolution and minimum detection limits obtainable. The examples of applications cited give an idea of the types of research fields that are currently under investigation. They can be used to illustrate how the field of x-ray microscopy will benefit from the use of bending magnets and insertion devices at the Advanced Photon Source. 8 refs., 5 figs.

  17. Synchrotron X-ray muprobe and its application to human hair analysis

    NASA Astrophysics Data System (ADS)

    Iida, Atsuo; Noma, Takashi

    1993-07-01

    A synchrotron X-ray muprobe system based on Kirkpatrick-Baez optics has been developed. Double-crystal and synthetic multilayer monochromators are used for high energy resolution experiments and for highly sensitive X-ray fluorescence analysis, respectively. The characteristics of the X-ray muprobe were experimentally examined. A beam size of around 5 μm was obtained; the X-ray photon flux at the storage ring current of 300 mA is of the order of 10 7-8 photons/s and 10 9-10 photons/s for the double-crystal and multilayer monochromators, respectively. The concentration distributions of trace elements in cross sections of human hair were measured using an X-ray mubeam with the multilayer monochromator. Inhomogeneous distributions of trace elements in thin cross-section samples show that two-dimensional imaging is effective and indispensable both for the determination of the elemental concentration in hair and for investigating the incorporation mechanism of trace elements into hair from the body.

  18. POLARIZATION STUDIES OF CdZnTe DETECTORS USING SYNCHROTRON X-RAY RADIATION.

    SciTech Connect

    CAMARDA,G.S.; BOLOTNIKOV, A.E.; CUI, Y.; HOSSAIN, A.; JAMES, R.B.

    2007-07-01

    New results on the effects of small-scale defects on the charge-carrier transport in single-crystal CdZnTe (CZT) material were produced. We conducted detailed studies of the role of Te inclusions in CZT by employing a highly collimated synchrotron x-ray radiation source available at Brookhaven's National Synchrotron Light Source (NSLS). We were able to induce polarization effects by irradiating specific areas with the detector. These measurements allowed the first quantitative comparison between areas that are free of Te inclusions and those with a relatively high concentration of inclusions. The results of these polaration studies will be reported.

  19. Synchrotron based X-ray fluorescence activities at Indus-2: An overview

    SciTech Connect

    Tiwari, M. K.

    2014-04-24

    X-Ray fluorescence (XRF) spectrometry is a powerful non-destructive technique for elemental analysis of materials at bulk and trace concentration levels. Taking into consideration several advantages of the synchrotron based XRF technique and to fulfill the requirements of Indian universities users we have setup a microfocus XRF beamline (BL-16) on Indus-2 synchrotron light source. The beamline offers a wide range of usages – both from research laboratories and industries; and for researchers working in diverse fields. A brief overview of the measured performance of the beamline, design specifications including various attractive features and recent research activities carried out on the BL-16 beamline are presented.

  20. A setup for synchrotron-radiation-induced total reflection X-ray fluorescence and X-ray absorption near-edge structure recently commissioned at BESSY II BAMline.

    PubMed

    Fittschen, U; Guilherme, A; Böttger, S; Rosenberg, D; Menzel, M; Jansen, W; Busker, M; Gotlib, Z P; Radtke, M; Riesemeier, H; Wobrauschek, P; Streli, C

    2016-05-01

    An automatic sample changer chamber for total reflection X-ray fluorescence (TXRF) and X-ray absorption near-edge structure (XANES) analysis in TXRF geometry was successfully set up at the BAMline at BESSY II. TXRF and TXRF-XANES are valuable tools for elemental determination and speciation, especially where sample amounts are limited (<1 mg) and concentrations are low (ng ml(-1) to µg ml(-1)). TXRF requires a well defined geometry regarding the reflecting surface of a sample carrier and the synchrotron beam. The newly installed chamber allows for reliable sample positioning, remote sample changing and evacuation of the fluorescence beam path. The chamber was successfully used showing accurate determination of elemental amounts in the certified reference material NIST water 1640. Low limits of detection of less than 100 fg absolute (10 pg ml(-1)) for Ni were found. TXRF-XANES on different Re species was applied. An unknown species of Re was found to be Re in the +7 oxidation state. PMID:27140163

  1. Recent progress on synchrotron-based in-situ soft X-ray spectroscopy for energy materials.

    PubMed

    Liu, Xiaosong; Yang, Wanli; Liu, Zhi

    2014-12-10

    Soft X-ray spectroscopy (SXS) techniques such as photoelectron spectroscopy, soft X-ray absorption spectroscopy and X-ray emission spectroscopy are efficient and direct tools to probe electronic structures of materials. Traditionally, these surface sensitive soft X-ray techniques that detect electrons or photons require high vacuum to operate. Many recent in situ instrument developments of these techniques have overcome this vacuum barrier. One can now study many materials and model devices under near ambient, semi-realistic, and operando conditions. Further developments of integrating the realistic sample environments with efficient and high resolution detection methods, particularly at the high brightness synchrotron light sources, are making SXS an important tool for the energy research community. In this progress report, we briefly describe the basic concept of several SXS techniques and discuss recent development of SXS instruments. We then present several recent studies, mostly in situ SXS experiments, on energy materials and devices. Using these studies, we would like to highlight that the integration of SXS and in situ environments can provide in-depth insight of material's functionality and help researchers in new energy material developments. The remaining challenges and critical research directions are discussed at the end. PMID:24799004

  2. Tetrameric assembly of full-sequence protein zero myelin glycoprotein by synchrotron x-ray scattering.

    PubMed Central

    Inouye, H; Tsuruta, H; Sedzik, J; Uyemura, K; Kirschner, D A

    1999-01-01

    Highly purified myelin P0 glycoprotein was solubilized to 1-8 mg/ml in 0.1% sodium dodecyl sulfate (SDS), and the solution structure of the P0 assembly was studied using synchrotron x-ray scattering. The full-length P0, which was isolated from bovine intradural roots, included both the extracellular and cytoplasmic domains of the molecule. At the higher concentrations (4, 6, and 8 mg/ml, respectively), an x-ray intensity maximum was observed at 316 A, 245 A, and 240 A Bragg spacing. Because the position of this intensity depended on P0 concentration, it is most likely due to interparticle interference. By contrast, the position of a second intensity maximum, which was at approximately 40 A Bragg spacing, was invariant with P0 concentration. This latter intensity was accounted for by monodispersed, 80 A-diameter particles that are composed of eight, approximately 30 A-diameter spheres. Chemical parameters suggest that the 80 A particles correspond to the size of a tetramer of P0 molecules. Therefore, the approximately 30 A spheres would correspond to the sizes of the extracellular and cytoplasmic domains for each of the P0 monomers. The invariance of the second intensity maximum with P0 concentration indicates that the structure of the 80 A-diameter, tetrameric particles is unaltered. According to the liquid model for interparticle interference from charged spheres, the 80 A-diameter particle has 10 negative surface charges which likely arise from negatively charged SDS molecules bound to the transmembrane domain of P0. This binding, however, apparently does not alter the tetrameric assembly of P0, suggesting that intermolecular interactions involving extracellular domains and cytoplasmic domains likely stabilize this assembly. Some of our results have been published in abstract form (Inouye, H., H. Tsuruta, D. A. Kirschner, J. Sedzik, and K. Uyemura. Abstracts of the 4th International School and Symposium on Synchrotron Radiation in Natural Science, June 15

  3. Taking X-ray Diffraction to the Limit: Macromolecular Structures from Femtosecond X-ray Pulses and Diffraction Microscopy of Cells with Synchrotron Radiation

    SciTech Connect

    Chapman, H N; Miao, J; Kirz, J; Sayre, D; Hodgson, K O

    2003-10-01

    The methodology of X-ray crystallography has recently been successfully extended to the structure determination of non-crystalline specimens. The phase problem was solved by using the oversampling method, which takes advantage of ''continuous'' diffraction pattern from non-crystalline specimens. Here we review the principle of this newly developed technique and discuss the ongoing experiments of imaging non-periodic objects, like cells and cellular structures using coherent and bright X-rays from the 3rd generation synchrotron radiation. In the longer run, the technique may be applied to image single biomolecules by using the anticipated X-ray free electron lasers. Computer simulations have so far demonstrated two important steps: (1) by using an extremely intense femtosecond X-ray pulse, a diffraction pattern can be recorded from a macromolecule before radiation damage manifests itself, and (2) the phase information can be ab initio retrieved from a set of calculated noisy diffraction patterns of single protein molecules.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    SciTech Connect

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

    2015-11-15

    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 Er{sub 2}O{sub 3} ALD on amorphous ALD alumina and single crystalline sapphire.

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

    SciTech Connect

    Klug, Jeffrey A.; Weimer, Matthew S.; Emery, Jonathan D.; Yanguas-Gil, Angel; Seifert, Sonke; Schleputz, 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 \\textit{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.

  7. On the surface shape of an X-ray monochromator

    SciTech Connect

    Pleshakov, V. F.

    2008-07-15

    It is established that the surface of a monochromator for a point X-ray source in diffractometers is the surface of revolution of a circle arc around the straight line connecting the X-ray source and detector. It is shown that scattering occurs at the points of intersection of the monochromator surface with the set of ellipsoids of revolution, in whose focuses the X-ray source and detector are located. A formula is obtained for calculating the misorientation angle of mosaic blocks. The limits of variation in the angle for FeK{sub {alpha}} {sub 1}, CuK{sub {alpha}} {sub 1} and MoK{sub {alpha}} {sub 1} radiations are determined. It is shown that there is no unified continuous reflecting monochromator surface, and the true reflecting surface is fractal.

  8. DIFFUSE HARD X-RAY EMISSION IN STARBURST GALAXIES AS SYNCHROTRON FROM VERY HIGH ENERGY ELECTRONS

    SciTech Connect

    Lacki, Brian C.; Thompson, Todd A.

    2013-01-01

    The origin of the diffuse hard X-ray (2-10 keV) emission from starburst galaxies is a long-standing problem. We suggest that synchrotron emission of 10-100 TeV electrons and positrons (e {sup {+-}}) can contribute to this emission, because starbursts have strong magnetic fields. We consider three sources of e {sup {+-}} at these energies: (1) primary electrons directly accelerated by supernova remnants, (2) pionic secondary e {sup {+-}} created by inelastic collisions between cosmic ray (CR) protons and gas nuclei in the dense interstellar medium of starbursts, and (3) pair e {sup {+-}} produced between the interactions between 10 and 100 TeV {gamma}-rays and the intense far-infrared (FIR) radiation fields of starbursts. We create one-zone steady-state models of the CR population in the Galactic center (R {<=} 112 pc), NGC 253, M82, and Arp 220's nuclei, assuming a power-law injection spectrum for electrons and protons. We consider different injection spectral slopes, magnetic field strengths, CR acceleration efficiencies, and diffusive escape times, and include advective escape, radiative cooling processes, and secondary and pair e {sup {+-}}. We compare these models to extant radio and GeV and TeV {gamma}-ray data for these starbursts, and calculate the diffuse synchrotron X-ray and inverse Compton (IC) luminosities of these starbursts in the models which satisfy multiwavelength constraints. If the primary electron spectrum extends to {approx}PeV energies and has a proton/electron injection ratio similar to the Galactic value, we find that synchrotron emission contributes 2%-20% of their unresolved, diffuse hard X-ray emission. However, there is great uncertainty in this conclusion because of the limited information on the CR electron spectrum at these high energies. IC emission is likewise a minority of the unresolved X-ray emission in these starbursts, from 0.1% in the Galactic center to 10% in Arp 220's nuclei, with the main uncertainty being the starbursts

  9. Diffuse Hard X-Ray Emission in Starburst Galaxies as Synchrotron from Very High Energy Electrons

    NASA Astrophysics Data System (ADS)

    Lacki, Brian C.; Thompson, Todd A.

    2013-01-01

    The origin of the diffuse hard X-ray (2-10 keV) emission from starburst galaxies is a long-standing problem. We suggest that synchrotron emission of 10-100 TeV electrons and positrons (e ±) can contribute to this emission, because starbursts have strong magnetic fields. We consider three sources of e ± at these energies: (1) primary electrons directly accelerated by supernova remnants, (2) pionic secondary e ± created by inelastic collisions between cosmic ray (CR) protons and gas nuclei in the dense interstellar medium of starbursts, and (3) pair e ± produced between the interactions between 10 and 100 TeV γ-rays and the intense far-infrared (FIR) radiation fields of starbursts. We create one-zone steady-state models of the CR population in the Galactic center (R <= 112 pc), NGC 253, M82, and Arp 220's nuclei, assuming a power-law injection spectrum for electrons and protons. We consider different injection spectral slopes, magnetic field strengths, CR acceleration efficiencies, and diffusive escape times, and include advective escape, radiative cooling processes, and secondary and pair e ±. We compare these models to extant radio and GeV and TeV γ-ray data for these starbursts, and calculate the diffuse synchrotron X-ray and inverse Compton (IC) luminosities of these starbursts in the models which satisfy multiwavelength constraints. If the primary electron spectrum extends to ~PeV energies and has a proton/electron injection ratio similar to the Galactic value, we find that synchrotron emission contributes 2%-20% of their unresolved, diffuse hard X-ray emission. However, there is great uncertainty in this conclusion because of the limited information on the CR electron spectrum at these high energies. IC emission is likewise a minority of the unresolved X-ray emission in these starbursts, from 0.1% in the Galactic center to 10% in Arp 220's nuclei, with the main uncertainty being the starbursts' magnetic field. We also model generic starbursts, including

  10. SYNCHROTRON X-RAY MICROTOMOGRAPHY, ELECTRON PROBE MICROANALYSIS, AND NMR OF TOLUENE WASTE IN CEMENT.

    SciTech Connect

    BUTLER,L.G.

    1999-07-22

    Synchrotron X-ray microtomography shows vesicular structures for toluene/cement mixtures, prepared with 1.22 to 3.58 wt% toluene. Three-dimensional imaging of the cured samples shows spherical vesicles, with diameters ranging from 20 to 250 {micro}m; a search with EPMA for vesicles in the range of 1-20 {micro}m proved negative. However, the total vesicle volume, as computed from the microtomography images, accounts for less than 10% of initial toluene. Since the cements were cured in sealed bottles, the larger portion of toluene must be dispersed within the cement matrix. Evidence for toluene in the cement matrix comes from {sup 29}Si MAS NMR spectroscopy, which shows a reduction in chain silicates with added toluene. Also, {sup 2}H NMR of d{sub 8}-toluene/cement samples shows high mobility for all, toluene and thus no toluene/cement binding. A model that accounts for all observations follows: For loadings below about 3 wt%, most toluene is dispersed in the cement matrix, with a small fraction of the initial toluene phase separating from the cement paste and forming vesicular structures that are preserved in the cured cement. Furthermore, at loadings above 3 wt%, the abundance of vesicles formed during toluene/cement paste mixing leads to macroscopic phase separation (most toluene floats to the surface of the cement paste).

  11. High-resolution synchrotron X-ray analysis of bioglass-enriched hydrogels.

    PubMed

    Gorodzha, Svetlana; Douglas, Timothy E L; Samal, Sangram K; Detsch, Rainer; Cholewa-Kowalska, Katarzyna; Braeckmans, Kevin; Boccaccini, Aldo R; Skirtach, Andre G; Weinhardt, Venera; Baumbach, Tilo; Surmeneva, Maria A; Surmenev, Roman A

    2016-05-01

    Enrichment of hydrogels with inorganic particles improves their suitability for bone regeneration by enhancing their mechanical properties, mineralizability, and bioactivity as well as adhesion, proliferation, and differentiation of bone-forming cells, while maintaining injectability. Low aggregation and homogeneous distribution maximize particle surface area, promoting mineralization, cell-particle interactions, and homogenous tissue regeneration. Hence, determination of the size and distribution of particles/particle agglomerates in the hydrogel is desirable. Commonly used techniques have drawbacks. High-resolution techniques (e.g., SEM) require drying. Distribution in the dry state is not representative of the wet state. Techniques in the wet state (histology, µCT) are of lower resolution. Here, self-gelling, injectable composites of Gellan Gum (GG) hydrogel and two different types of sol-gel-derived bioactive glass (bioglass) particles were analyzed in the wet state using Synchrotron X-ray radiation, enabling high-resolution determination of particle size and spatial distribution. The lower detection limit volume was 9 × 10(-5) mm(3) . Bioglass particle suspensions were also studied using zeta potential measurements and Coulter analysis. Aggregation of bioglass particles in the GG hydrogels occurred and aggregate distribution was inhomogeneous. Bioglass promoted attachment of rat mesenchymal stem cells (rMSC) and mineralization. PMID:26749323

  12. Time-resolved coherent X-ray diffraction imaging of surface acoustic waves

    PubMed Central

    Nicolas, Jan-David; Reusch, Tobias; Osterhoff, Markus; Sprung, Michael; Schülein, Florian J. R.; Krenner, Hubert J.; Wixforth, Achim; Salditt, Tim

    2014-01-01

    Time-resolved coherent X-ray diffraction experiments of standing surface acoustic waves, illuminated under grazing incidence by a nanofocused synchrotron beam, are reported. The data have been recorded in stroboscopic mode at controlled and varied phase between the acoustic frequency generator and the synchrotron bunch train. At each time delay (phase angle), the coherent far-field diffraction pattern in the small-angle regime is inverted by an iterative algorithm to yield the local instantaneous surface height profile along the optical axis. The results show that periodic nanoscale dynamics can be imaged at high temporal resolution in the range of 50 ps (pulse length). PMID:25294979

  13. X-Tream quality assurance in synchrotron X-ray microbeam radiation therapy.

    PubMed

    Fournier, Pauline; Cornelius, Iwan; Donzelli, Mattia; Requardt, Herwig; Nemoz, Christian; Petasecca, Marco; Bräuer-Krisch, Elke; Rosenfeld, Anatoly; Lerch, Michael

    2016-09-01

    Microbeam radiation therapy (MRT) is a novel irradiation technique for brain tumours treatment currently under development at the European Synchrotron Radiation Facility in Grenoble, France. The technique is based on the spatial fractionation of a highly brilliant synchrotron X-ray beam into an array of microbeams using a multi-slit collimator (MSC). After promising pre-clinical results, veterinary trials have recently commenced requiring the need for dedicated quality assurance (QA) procedures. The quality of MRT treatment demands reproducible and precise spatial fractionation of the incoming synchrotron beam. The intensity profile of the microbeams must also be quickly and quantitatively characterized prior to each treatment for comparison with that used for input to the dose-planning calculations. The Centre for Medical Radiation Physics (University of Wollongong, Australia) has developed an X-ray treatment monitoring system (X-Tream) which incorporates a high-spatial-resolution silicon strip detector (SSD) specifically designed for MRT. In-air measurements of the horizontal profile of the intrinsic microbeam X-ray field in order to determine the relative intensity of each microbeam are presented, and the alignment of the MSC is also assessed. The results show that the SSD is able to resolve individual microbeams which therefore provides invaluable QA of the horizontal field size and microbeam number and shape. They also demonstrate that the SSD used in the X-Tream system is very sensitive to any small misalignment of the MSC. In order to allow as rapid QA as possible, a fast alignment procedure of the SSD based on X-ray imaging with a low-intensity low-energy beam has been developed and is presented in this publication. PMID:27577773

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

    PubMed

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

    2016-05-01

    The short pulse duration, small effective source size and high flux of synchrotron radiation is ideally suited for probing a wide range of transient deformation processes in materials under extreme conditions. In this paper, the challenges of high-resolution time-resolved indirect X-ray detection are reviewed in the context of dynamic synchrotron experiments. In particular, the discussion is targeted at two-dimensional integrating detector methods, such as those focused on dynamic radiography and diffraction experiments. The response of a scintillator to periodic synchrotron X-ray excitation is modelled and validated against experimental data collected at the Diamond Light Source (DLS) and European Synchrotron Radiation Facility (ESRF). An upper bound on the dynamic range accessible in a time-resolved experiment for a given bunch separation is calculated for a range of scintillators. New bunch structures are suggested for DLS and ESRF using the highest-performing commercially available crystal LYSO:Ce, allowing time-resolved experiments with an interframe time of 189 ns and a maximum dynamic range of 98 (6.6 bits). PMID:27140147

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

    PubMed Central

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

    2016-01-01

    The short pulse duration, small effective source size and high flux of synchrotron radiation is ideally suited for probing a wide range of transient deformation processes in materials under extreme conditions. In this paper, the challenges of high-resolution time-resolved indirect X-ray detection are reviewed in the context of dynamic synchrotron experiments. In particular, the discussion is targeted at two-dimensional integrating detector methods, such as those focused on dynamic radiography and diffraction experiments. The response of a scintillator to periodic synchrotron X-ray excitation is modelled and validated against experimental data collected at the Diamond Light Source (DLS) and European Synchrotron Radiation Facility (ESRF). An upper bound on the dynamic range accessible in a time-resolved experiment for a given bunch separation is calculated for a range of scintillators. New bunch structures are suggested for DLS and ESRF using the highest-performing commercially available crystal LYSO:Ce, allowing time-resolved experiments with an interframe time of 189 ns and a maximum dynamic range of 98 (6.6 bits). PMID:27140147

  16. Microstructural Characterization and Corrosion Behavior of Al 7075 Alloys Using X-ray Synchrotron Tomography

    NASA Astrophysics Data System (ADS)

    Singh, Sudhanshu Shekhar

    Al 7075 alloys are used in a variety of structural applications, such as aircraft wings, automotive components, fuselage, spacecraft, missiles, etc. The mechanical and corrosion behavior of these alloys are dependent on their microstructure and the environment. Therefore, a comprehensive study on microstructural characterization and stress-environment interaction is necessary. Traditionally, 2D techniques have been used to characterize microstructure, which are inaccurate and inadequate since the research has shown that the results obtained in the bulk are different from those obtained on the surface. There now exist several techniques in 3D, which can be used to characterize the microstructure. Al 7075 alloys contain second phase particles which can be classified as Fe-bearing inclusions, Si-bearing inclusions and precipitates. The variation in mechanical and corrosion properties of aluminum alloys has been attributed to the size, shape, distribution, corrosion properties and mechanical behavior of these precipitates and constituent particles. Therefore, in order to understand the performance of Al 7075 alloys, it is critical to investigate the size and distribution of inclusions and precipitates in the alloys along with their mechanical properties, such as Young's modulus, hardness and stress-strain behavior. X-ray tomography and FIB tomography were used to visualize and quantify the microstructure of constituent particles (inclusions) and precipitates, respectively. Microscale mechanical characterization techniques, such as nanoindentation and micropillar compression, were used to obtain mechanical properties of inclusions. Over the years, studies have used surface measurements to understand corrosion behavior of materials. More recently, in situ mechanical testing has become more attractive and advantageous, as it enables visualization and quantification of microstructural changes as a function of time (4D). In this study, in situ X-ray synchrotron tomography

  17. Conical geometry for sagittal focusing as applied to X rays from synchrotrons

    SciTech Connect

    Ice, G.E.; Sparks, C.J.

    1993-06-01

    The authors describe a method for simultaneously focusing and monochromatization of X rays from a fan of radiation having up to 15 mrad divergence in one dimension. This geometry is well suited to synchrotron radiation sources at magnifications of one-fifth to two and is efficient for X-ray energies between 3 and 40 keV (0.48 and 6.4 fJ). The method uses crystals bent to part of a cone for sagittal focusing and allows for the collection of a larger divergence with less mixing of the horizontal into the vertical divergence than is possible with X-ray mirrors. They describe the geometry required to achieve the highest efficiency when a conical crystal follows a flat crystal in a nondispersive two-crystal monochromator. At a magnification of one-third, the geometry is identical to a cylindrical focusing design described previously. A simple theoretical calculation is shown to agree well with ray-tracing results. Minimum aberrations are observed at magnifications near one. Applications of the conical focusing geometry to existing and future synchrotron radiation facilities are discussed.

  18. Investigation of internal structure of fine granules by microtomography using synchrotron X-ray radiation.

    PubMed

    Noguchi, Shuji; Kajihara, Ryusuke; Iwao, Yasunori; Fujinami, Yukari; Suzuki, Yoshio; Terada, Yasuko; Uesugi, Kentaro; Miura, Keiko; Itai, Shigeru

    2013-03-10

    Computed tomography (CT) using synchrotron X-ray radiation was evaluated as a non-destructive structural analysis method for fine granules. Two kinds of granules have been investigated: a bromhexine hydrochloride (BHX)-layered Celphere CP-102 granule coated with pH-sensitive polymer Kollicoat Smartseal 30-D, and a wax-matrix granule constructed from acetaminophen (APAP), dibasic calcium phosphate dehydrate, and aminoalkyl methacrylate copolymer E (AMCE) manufactured by melt granulation. The diameters of both granules were 200-300 μm. CT analysis of CP-102 granule could visualize the laminar structures of BHX and Kollicoat layers, and also visualize the high talc-content regions in the Kollicoat layer that could not be detected by scanning electron microscopy. Moreover, CT analysis using X-ray energies above the absorption edge of Br specifically enhanced the contrast in the BHX layer. As for granules manufactured by melt granulation, CT analysis revealed that they had a small inner void space due to a uniform distribution of APAP and other excipients. The distribution of AMCE revealed by CT analysis was also found to involve in the differences of drug dissolution from the granules as described previously. These observations demonstrate that CT analysis using synchrotron X-ray radiation is a powerful method for the detailed internal structure analysis of fine granules. PMID:23376507

  19. Synchrotron Small-Angle X-ray Scattering Study of Cross-Linked Polymeric Micelles.

    PubMed

    Kim, Hyun-Chul; Jin, Kyeong Sik; Lee, Se Guen; Kim, Eunjoo; Lee, Sung Jun; Jeong, Sang Won; Lee, Seung Woo; Kim, Kwang-Woo

    2016-06-01

    Polymeric micelles of methoxypoly(ethylene glycol)-b-poly(lactide) containing lysine units (mPEG-PLA-Lys4) were cross-linked by reacting of lysine moieties with a bifunctional bis(N-hydroxy-succinimide ester). The micelles were characterized in aqueous solution using dynamic light scattering, transmission electron microscopy, and synchrotron small-angle X-ray scattering. The mPEG-PLA-Lys4 was synthesized through the ring-opening polymerization of N6-carbobenzyloxy-L-lysine N-carboxyanhydride with amine-terminated mPEG-PLA and subsequent deprotection. The polymeric micelles showed enhanced micelle stability after cross-linking, which was confirmed by adding sodium dodecyl sulfate as a destabilizing agent. The average diameters measured via dynamic light scattering were 19.1 nm and 29.2 nm for non-cross-linked polymeric micelles (NCPMs) and cross-linked polymeric micelles (CPMs), respectively. The transmission electron microscopy images showed that the size of the polymeric micelles increased slightly due to cross-linking, which was in good agreement with the DLS measurements. The overall structures and internal structural changes of NCPMs and CPMs in aqueous solution were studied in detail using synchrotron X-ray scattering method. According to the structural parameters of X-ray scattering analysis, CPMs with a more densely packed core structure were formed by reacting bifunctional cross-linking agents with lysine amino groups located in the innermost core of the polymeric micelles. PMID:27427731

  20. Heat transfer issues in high-heat-load synchrotron x-ray beams

    SciTech Connect

    Khounsary, A.M.; Mills, D.M.

    1994-09-01

    In this paper, a short description of the synchrotron radiation x-ray sources and the associated power loads is given, followed by a brief description of typical synchrotron components and their heat load. It is emphasized that the design goals for most of these components is to limit (a) temperature, (b) stresses, or (c) strains in the system. Each design calls for a different geometry, material selection, and cooling scheme. Cooling schemes that have been utilized so far are primarily single phase and include simple macrochannel cooling, microchannel cooling, contact cooling, pin-post cooling, porous-flow cooling, jet cooling, etc. Water, liquid metals, and various cryogenic coolants have been used. Because the trend in x-ray beam development is towards brighter (i.e., more powerful) beams and assuming that no radical changes in the design of x-ray generating machines occurs in the next few years, it is fair to state that the utilization of various effective cooling schemes and, in particular, two-phase flow (e.g., subcooled boiling) warrants further investigation. This, however, requires a thorough examination of stability and reliability of two-phase flows for high-heat-flux components operating in ultrahigh vacuum with stringent reliability requirements.

  1. Trace element abundance determinations by Synchrotron X Ray Fluorescence (SXRF) on returned comet nucleus mineral grains

    NASA Technical Reports Server (NTRS)

    Flynn, G. J.; Sutton, S. R.

    1989-01-01

    Trace element analyses were performed on bulk cosmic dust particles by Proton Induced X Ray Emission (PIXE) and Synchrotron X Ray Fluorescence (SXRF). When present at or near chondritic abundances the trace elements K, Ti, Cr, Mn, Cu, Zn, Ga, Ge, Se, and Br are presently detectable by SXRF in particles of 20 micron diameter. Improvements to the SXRF analysis facility at the National Synchrotron Light Source presently underway should increase the range of detectable elements and permit the analysis of smaller samples. In addition the Advanced Photon Source will be commissioned at Argonne National Laboratory in 1995. This 7 to 8 GeV positron storage ring, specifically designed for high-energy undulator and wiggler insertion devices, will be an ideal source for an x ray microprobe with one micron spatial resolution and better than 100 ppb elemental sensitivity for most elements. Thus trace element analysis of individual micron-sized grains should be possible by the time of the comet nucleus sample return mission.

  2. Workshops on Science Enabled by a Coherent, CW, Synchrotron X-ray Source, June 2011

    SciTech Connect

    Brock, Joel

    2012-01-03

    In June of 2011 we held six two-day workshops called "XDL-2011: Science at the Hard X-ray Diffraction Limit". The six workshops covered (1) Diffraction-based imaging techniques, (2) Biomolecular structure from non-crystalline materials, (3) Ultra-fast science, (4) High-pressure science, (5) Materials research with nano-beams and (6) X-ray photon correlation spectroscopy (XPCS), In each workshop, invited speaker from around the world presented examples of novel experiments that require a CW, diffraction-limited source. During the workshop, each invited speaker provided a one-page description of the experiment and an illustrative graphic. The experiments identified by the workshops demonstrate the broad and deep scientific case for a CW coherent synchrotron x-ray source. The next step is to perform detailed simulations of the best of these ideas to test them quantitatively and to guide detailed x-ray beam-line designs. These designs are the first step toward developing detailed facility designs and cost estimates.

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

    PubMed

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

    2016-01-19

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

  4. Development of soft X-ray polarized light beamline on Indus-2 synchrotron radiation source

    SciTech Connect

    Phase, D. M. Gupta, Mukul Potdar, S. Behera, L. Sah, R. Gupta, Ajay

    2014-04-24

    This article describes the development of a soft x-ray beamline on a bending magnet source of Indus-2 storage ring (2.5 GeV) and some preliminary results of x-ray absorption spectroscopy (XAS) measurements using the same. The beamline layout is based on a spherical grating monochromator. The beamline is able to accept synchrotron radiation from the bending magnet port BL-1 of the Indus-2 ring with a wide solid angle. The large horizontal and vertical angular acceptance contributes to high photon flux and selective polarization respectively. The complete beamline is tested for ultrahigh vacuum (UHV) ∼ 10{sup −10} mbar. First absorption spectrum was obtained on HOPG graphite foil. Our performance test indicates that modest resolving power has been achieved with adequate photon flux to carry out various absorption experiments.

  5. Small-angle scattering studies of meso-scopic structures with synchrotron X-rays

    NASA Astrophysics Data System (ADS)

    Dore, J. C.; North, A. N.; Rigden, J. S.

    1995-03-01

    The use of small-angle X-ray scattering techniques for the study of spatial inhomogeneities over the range 20 Å to 2 μm is reviewed. The basic formalism for scattering by an inhomogeneous medium is developed with particular reference to liquid suspensions, porous solids and solid aggregates. The instrumentation available on the Synchrotron Radiation Source at the Daresbury Laboratory is briefly presented and the use of the Bonse-Hart method for studies at ultra-low scattering angles described. The extraction of structural information for a range of natural and synthetic materials is presented with particular reference to microemulsions, porous silicas, clays and composites. The complementarity of X-ray and neutron techniques is critically reviewed and prospects for future developments, particularly for the study of anisotropic systems, are discussed.

  6. Single-crystal sapphire microstructure for high-resolution synchrotron X-ray monochromators

    DOE PAGESBeta

    Asadchikov, Victor E.; Butashin, Andrey V.; Buzmakov, Alexey V.; Deryabin, Alexander N.; Kanevsky, Vladimir M.; Prokhorov, Igor A.; Roshchin, Boris S.; Volkov, Yuri O.; Zolotov, Dennis A.; Jafari, Atefeh; et al

    2016-03-22

    We report on the growth and characterization of several sapphire single crystals for the purpose of x-ray optics applications. Structural defects were studied by means of laboratory double-crystal X-ray diffractometry and white beam synchrotron-radiation topography. The investigations confirmed that the main defect types are dislocations. The best quality crystal was grown using the Kyropoulos technique with a dislocation density of 102-103 cm-2 and a small area with approximately 2*2 mm2 did not show dislocation contrast in many reflections and has suitable quality for application as a backscattering monochromator. As a result, a clear correlation between growth rate and dislocation densitymore » is observed, though growth rate is not the only parameter impacting the quality.« less

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

    NASA Astrophysics Data System (ADS)

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

    2015-06-01

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

  8. Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading.

    PubMed

    Fan, D; Huang, J W; Zeng, X L; Li, Y; E, J C; Huang, J Y; Sun, T; Fezzaa, K; Wang, Z; Luo, S N

    2016-05-01

    We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera's capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantify lattice deformation and fracture; fracture is dominated by splitting cracks followed by wing cracks, and diffraction peaks are broadened likely due to mosaic spread. Our results demonstrate the potential of such multiscale measurements for studying high strain-rate phenomena at dynamic extremes. PMID:27250438

  9. Development of a speckle-based portable device for in situ metrology of synchrotron X-ray mirrors.

    PubMed

    Kashyap, Yogesh; Wang, Hongchang; Sawhney, Kawal

    2016-09-01

    A portable device for in situ metrology of synchrotron X-ray mirrors based on the near-field speckle scanning technique has been developed. Ultra-high angular sensitivity is achieved by scanning a piece of abrasive paper or filter membrane 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 optimizing active X-ray mirrors is simple and fast. The functionality and feasibility of this device have been demonstrated by characterizing and optimizing X-ray mirrors. PMID:27577767

  10. Development of a speckle-based portable device for in situ metrology of synchrotron X-ray mirrors

    PubMed Central

    Kashyap, Yogesh; Wang, Hongchang; Sawhney, Kawal

    2016-01-01

    A portable device for in situ metrology of synchrotron X-ray mirrors based on the near-field speckle scanning technique has been developed. Ultra-high angular sensitivity is achieved by scanning a piece of abrasive paper or filter membrane 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 optimizing active X-ray mirrors is simple and fast. The functionality and feasibility of this device have been demonstrated by characterizing and optimizing X-ray mirrors. PMID:27577767

  11. Prospects for compact high-intensity laser synchrotron x-ray and gamma sources

    NASA Astrophysics Data System (ADS)

    Pogorelsky, I. V.

    1997-03-01

    A laser interacting with a relativistic electron beam behaves like a virtual wiggler of an extremely short period equal to half of the laser wavelength. This approach opens a route to relatively compact, high-brightness x-ray sources alternative or complementary to conventional synchrotron light sources. Although not new, the laser synchrotron source (LSS) concept is still waiting for a convincing demonstration. Available at the BNL Accelerator Test Facility (ATF), a high-brightness electron beam and the high-power CO2 laser may be used for prototype LSS demonstration. In a feasible demonstration experiment, 10-GW, 100-ps CO2 laser beam will be brought to a head-on collision with a 10-ps, 0.5-nC, 50 MeV electron bunch. Flashes of collimated 4.7 keV (2.6 Å) x-rays of 10-ps pulse duration, with a flux of ˜1019photons/sec, will be produced via linear Compton backscattering. The x-ray spectrum is tunable proportionally to the e-beam energy. A rational short-term extension of the proposed experiment would be further enhancement of the x-ray flux to the 1022 photons/sec level, after the ongoing ATF CO2 laser upgrade to 5 TW peak power and electron bunch shortening to 3 ps is realized. In the future, exploiting the promising approach of a high-gradient laser wake field accelerator, a compact "table-top" LSS of monochromatic gamma radiation may become feasible.

  12. Synchrotron-based small-angle X-ray scattering (SAXS) of proteins in solution

    PubMed Central

    Skou, Soren; Gillilan, Richard E

    2015-01-01

    Summary With recent advances in data analysis algorithms, X-ray detectors, and synchrotron sources, small-angle X-ray scattering (SAXS) has become much more accessible to the structural biology community than ever before. Although limited to ~10 Å resolution, SAXS can provide a wealth of structural information on biomolecules in solution and is compatible with a wide range of experimental conditions. SAXS is thus an attractive alternative when crystallography is not possible. Moreover, advanced usage of SAXS can provide unique insight into biomolecular behavior that can only be observed in solution, such as large conformational changes and transient protein-protein interactions. Unlike crystal diffraction data, however, solution scattering data are subtle in appearance, highly sensitive to sample quality and experimental errors, and easily misinterpreted. In addition, synchrotron beamlines that are dedicated to SAXS are often unfamiliar to the non-specialist. Here, we present a series of procedures that can be used for SAXS data collection and basic cross-checks designed to detect and avoid aggregation, concentration effects, radiation damage, buffer mismatch, and other common problems. The protein, human serum albumin (HSA), serves as a convenient and easily replicated example of just how subtle these problems can sometimes be, but also of how proper technique can yield pristine data even in problematic cases. Because typical data collection times at a synchrotron are only one to several days, we recommend that the sample purity, homogeneity, and solubility be extensively optimized prior to the experiment. PMID:24967622

  13. Experimental comparison between speckle and grating-based imaging technique using synchrotron radiation X-rays.

    PubMed

    Kashyap, Yogesh; Wang, Hongchang; Sawhney, Kawal

    2016-08-01

    X-ray phase contrast and dark-field imaging techniques provide important and complementary information that is inaccessible to the conventional absorption contrast imaging. Both grating-based imaging (GBI) and speckle-based imaging (SBI) are able to retrieve multi-modal images using synchrotron as well as lab-based sources. However, no systematic comparison has been made between the two techniques so far. We present an experimental comparison between GBI and SBI techniques with synchrotron radiation X-ray source. Apart from the simple experimental setup, we find SBI does not suffer from the issue of phase unwrapping, which can often be problematic for GBI. In addition, SBI is also superior to GBI since two orthogonal differential phase gradients can be simultaneously extracted by one dimensional scan. The GBI has less stringent requirements for detector pixel size and transverse coherence length when a second or third grating can be used. This study provides the reference for choosing the most suitable technique for diverse imaging applications at synchrotron facility. PMID:27505829

  14. Synchrotron x-ray fluorescence analyses of stratospheric cosmic dust: New results for chondritic and nickel-depleted particles

    SciTech Connect

    Flynn, G.J.; Sutton, S.R.

    1989-06-01

    Trace element abundance determinations were performed using synchrotron x-ray fluorescence on nine particles collected from the stratosphere and classified as ''cosmic''. Improvements to the Synchrotron Light Source allowed the detection of all elements between Cr and Mo, with the exceptions of Co and As, in our largest particle. The minor and trace element abundance patterns of three Ni-depleted particles were remarkably similar to those of extraterrestrial igneous rocks. Fe/Ni and Fe/Mn ratios suggest that one of these may be of lunar origin. All nine particles exhibited an enrichment in Br, ranging form 1.3 to 38 times the Cl concentration. Br concentrations were uncorrelated with particle size, as would be expected for a surface correlated component acquires from the stratosphere. 27 refs., 4 figs., 2 tabs.

  15. Simultaneous X-ray fluorescence and scanning X-ray diffraction microscopy at the Australian Synchrotron XFM beamline.

    PubMed

    Jones, Michael W M; Phillips, Nicholas W; van Riessen, Grant A; Abbey, Brian; Vine, David J; Nashed, Youssef S G; Mudie, Stephen T; Afshar, Nader; Kirkham, Robin; Chen, Bo; Balaur, Eugeniu; de Jonge, Martin D

    2016-09-01

    Owing to its extreme sensitivity, quantitative mapping of elemental distributions via X-ray fluorescence microscopy (XFM) has become a key microanalytical technique. The recent realisation of scanning X-ray diffraction microscopy (SXDM) meanwhile provides an avenue for quantitative super-resolved ultra-structural visualization. The similarity of their experimental geometries indicates excellent prospects for simultaneous acquisition. Here, in both step- and fly-scanning modes, robust, simultaneous XFM-SXDM is demonstrated. PMID:27577770

  16. Iron overload of human colon adenocarcinoma cells studied by synchrotron-based X-ray techniques.

    PubMed

    Mihucz, Victor G; Meirer, Florian; Polgári, Zsófia; Réti, Andrea; Pepponi, Giancarlo; Ingerle, Dieter; Szoboszlai, Norbert; Streli, Christina

    2016-04-01

    Fast- and slow-proliferating human adenocarcinoma colorectal cells, HT-29 and HCA-7, respectively, overloaded with transferrin (Tf), Fe(III) citrate, Fe(III) chloride and Fe(II) sulfate were studied by synchrotron radiation total-reflection X-ray spectrometry (TXRF), TXRF-X-ray absorption near edge structure (TXRF-XANES), and micro-X-ray fluorescence imaging to obtain information on the intracellular storage of overloaded iron (Fe). The determined TfR1 mRNA expression for the investigated cells correlated with their proliferation rate. In all cases, the Fe XANES of cells overloaded with inorganic Fe was found to be similar to that of deliquescent Fe(III) sulfate characterized by a distorted octahedral geometry. A fitting model using a linear combination of the XANES of Tf and deliquescent Fe(III) sulfate allowed to explain the near edge structure recorded for HT-29 cells indicating that cellular overload with inorganic Fe results in a non-ferritin-like fast Fe storage. Hierarchical cluster analysis of XANES spectra recorded for Fe overloaded HT-29 and HCA-7 cells was able to distinguish between Fe treatments performed with different Fe species with a 95 % hit rate, indicating clear differences in the Fe storage system. Micro-X-ray fluorescence imaging of Fe overloaded HT-29 cells revealed that Fe is primarily located in the cytosol of the cells. By characterizing the cellular Fe uptake, Fe/S content ratios were calculated based on the X-ray fluorescence signals of the analytes. These Fe/S ratios were dramatically lower for HCA-7 treated with organic Fe(III) treatments suggesting dissimilarities from the Tf-like Fe uptake. PMID:26759251

  17. Shedding new light on historical metal samples using micro-focused synchrotron X-ray fluorescence and spectroscopy

    NASA Astrophysics Data System (ADS)

    Grolimund, D.; Senn, M.; Trottmann, M.; Janousch, M.; Bonhoure, I.; Scheidegger, A. M.; Marcus, M.

    2004-10-01

    Synchrotron-based micro-X-ray fluorescence (micro-XRF) and micro-X-ray absorption spectroscopy (micro-XAS) were used in the present study to obtain spatially resolved micro-scale information on elemental composition, trace element distribution, chemical speciation and oxidation state and/or mineral phase distribution within historical iron artefacts dating from the Iron Age to early Medieval Times. Large area two-dimensional trace element distribution maps and oxidation state maps with micrometer spatial resolution were required to answer open archaeological questions in the context of ancient metal processing. The first set of examples was focusing on historical weapons and included two ancient iron sword blades. The micro-XRF maps revealed a distinct, highly correlated distribution pattern of trace elements such as As, Ni, Cu and Zn. Accordingly, the number of used raw materials could be determined unambiguously and key information concerning the used ancient smithing technique were gained. Further, the ability to record—in a fast manner—large area maps with high spatial resolution ('elemental screening') led to the discovery of a hitherto unknown enhanced occurrence of selected trace elements (Cu, Zn, and Au) at the blade surface. Complementary investigations by high resolution scanning electron microscopy were able to localize these trace metals within a carbon-rich matrix may be pointing towards an artifact induced during preservation. A second set of investigated artefacts is dealing with smithing waste products and related historical processing techniques and conditions. Synchrotron-based micro-XRF and micro-XAS were used to determine the structural composition as well as the spatial variation of the predominant Fe oxidation state and corresponding crystallographic phases. The study revealed the presence of distinct domains of Fe 0, Fe IIO (wustite), and α-Fe IIIOOH (goethite), separated by sharp domain boundaries. These findings help to gain new

  18. Probing deformation substructure by synchrotron X-ray diffraction and dislocation dynamics modelling.

    PubMed

    Korsunsky, Alexander M; Hofmann, Felix; Song, Xu; Eve, Sophie; Collins, Steve P

    2010-09-01

    Materials characterization at the nano-scale is motivated by the desire to resolve the structural aspects and deformation behavior at length scales relevant to those mechanisms that define the novel and unusual properties of nano-structured materials. A range of novel techniques has recently become accessible with the help of synchrotron X-ray beams that can be focused down to spot sizes of less than a few microns on the sample. The unique combination of tunability (energy selection), parallelism and brightness of synchrotron X-ray beams allows their use for high resolution diffraction (determination of crystal structure and transformations, analysis of dislocation sub-structures, orientation and texture analysis, strain mapping); small angle X-ray scattering (analysis of nano-scale voids and defects; orientation analysis) and imaging (radiography and tomography). After a brief review of the state-of-the-art capabilities for monochromatic and white beam synchrotron diffraction, we consider the usefulness of these techniques for the task of bridging the gap between experiment and modeling. Namely, we discuss how the experiments can be configured to provide information relevant to the validation and improvement of modeling approaches, and also how the results of various simulations can be post-processed to improve the possibility of (more or less) direct comparison with experiments. Using the example of some recent experiments carried out on beamline 116 at Diamond Light Source near Oxford, we discuss how such experimental results can be interpreted in view and in conjunction with numerical deformation models, particularly those incorporating dislocation effects, e.g., finite-element based pseudo-continuum strain gradient formulations, and discrete dislocation simulations. Post-processing of FE and discrete dislocation simulations is described, illustrating the kind of information that can be extracted from comparisons between modeling and experimental data. PMID

  19. Role of the Template in Model Biomineralization: Synchrotron X-ray Scattering Experiments

    NASA Astrophysics Data System (ADS)

    Uysal, Ahmet

    Synthesis of functional nanoparticles in cheap and environment friendly ways is one of the big challenges we face today. Interestingly, many biological systems are already expert at this task. Living organisms can grow nanocrystals of inorganic minerals with certain orientations and shapes and use them together with organic material to build structures with properties superior to the sum of their components. This process is called biomineralization. It has been previously shown that floating monolayers of amphiphilic molecules (Langmuir monolayers) can be used to simulate this process. This project covers the study of three different minerals, calcium oxalate, hydroxyapatite and gold, in an attempt to understand the role of the organic template in the model biomineralization experiments. We used in situ synchrotron x-ray scattering techniques to monitor the organic-inorganic interface during nucleation and growth of inorganic crystals. We also used scanning and transmission electron microscopy to study the structure of mature crystals ex situ . Although kidney stones (mostly calcium oxalate) are pathological in humans and animals, their microscopic structures exhibit considerable orientation and order, probably caused by organic molecules. Our x-ray scattering experiments revealed, first time, that in the early stages of the crystallization calcium oxalate crystals adapt a structure different from their known bulk structures. In the later stages, the crystals relax back to the bulk structure while changing the organization of the organic molecules next to them. We developed a model that explains these interactions in terms of the organic-inorganic interface potential energy. Hydroxyapatite is the main inorganic constituent of the vertebrate bone. In spite of the vast literature about bone mineralization, there is little known about the organic-inorganic interactions at the molecular level. In this thesis, we report the first in situ x-ray scattering experiments

  20. Load transfer in bovine plexiform bone determined by synchrotron x-ray diffraction.

    SciTech Connect

    Akhtar, R.; Daymond, M.; Almer, J.; Mummery, P.; The Univ. of Manchester; Queen's Univ.

    2008-02-01

    High-energy synchrotron x-ray diffraction (XRD) has been used to quantify load transfer in bovine plexiform bone. By using both wide-angle and small-angle XRD, strains in the mineral as well as the collagen phase of bone were measured as a function of applied compressive stress. We suggest that a greater proportion of the load is borne by the more mineralized woven bone than the lamellar bone as the applied stress increases. With a further increase in stress, load is shed back to the lamellar regions until macroscopic failure occurs. The reported data fit well with reported mechanisms of microdamage accumulation in bovine plexiform bone.

  1. The live lattices become visible in coherent synchrotron X-rays

    NASA Astrophysics Data System (ADS)

    Kohn, V.; Rau, C.; Sergienko, P. M.; Snigireva, I.; Snigirev, A.; Vazina, A.

    2005-05-01

    We demonstrate a great potential of the method of phase contrast imaging for a study of muscles and animal organism in normal and pathological states. The method is applied to image biological tissues that have the unique feature of structure-translation symmetry of 0.1-10 μm periodicity. The cross-striated muscle is the most interesting example of such objects. The experiment was done using high-brilliant coherent X-rays, delivered by synchrotron radiation source of third generation (ESRF, Grenoble), and high-resolution 2D-detector.

  2. Synchrotron total reflection X-ray fluorescence at BL-16 microfocus beamline of Indus-2

    NASA Astrophysics Data System (ADS)

    Tiwari, M. K.; Singh, A. K.; Das, Gangadhar; Chowdhury, Anupam; Lodha, G. S.

    2014-04-01

    Determination of ultra trace elements is important in many disciplines both in basic and applied sciences. Numerous applications show their importance in medical science, environmental science, materials science, food processing and semiconductor industries and in maintaining the quality control of ultra pure chemicals and reagents. We report commissioning of a synchrotron based total reflection x-ray fluorescence (TXRF) facility on the BL-16 microfocus beamline of Indus-2. This paper describes the performance of the BL-16 TXRF spectrometer and the detailed description of its capabilities through examples of measured results.

  3. Microscopy and elemental analysis in tissue samples using computed microtomography with synchrotron x-rays

    SciTech Connect

    Spanne, P.; Rivers, M.L.

    1988-01-01

    The initial development shows that CMT using synchrotron x-rays can be developed to ..mu..m spatial resolution and perhaps even better. This creates a new microscopy technique which is of special interest in morphological studies of tissues, since no chemical preparation or slicing of the sample is necessary. The combination of CMT with spatial resolution in the ..mu..m range and elemental mapping with sensitivity in the ppM range results in a new tool for elemental mapping at the cellular level. 7 refs., 1 fig.

  4. An x-ray fluorescence study of lake sediments from ancient Turkey using synchrotron radiation.

    SciTech Connect

    Alatas, A.; Alp, E. E.; Friedman, E. S.; Jennings, G.; Johnson, C. E.; Lai, B.; Mini, S. M.; Sato, Y.; Wilkinson, T. J.; Yener, K. A.

    1999-03-10

    Sediments from relic Lake Golbasi were analyzed by X-ray fluorescence with synchrotrons radiation to determine changes in element concentrations over time with selected elements serving as proxies for environmental change. Increases in Ca and Sr suggest soil formation during a dry period, from ca. 4500 BC to ca. 200 AD at which point K, Rb, Zr, Ti, and Y increase, indicating the return of a wet environment. Soil erosion, represented by Cr and Ni, increases ca. 7000 BC, probably as a consequence of environmental change, prior to suggested exploitation of natural resources by the newly urbanized society of the third millennium BC.

  5. Porosity characterization of fiber-reinforced ceramic matrix composite using synchrotron X-ray computed tomography

    NASA Astrophysics Data System (ADS)

    Zou, C.; Marrow, T. J.; Reinhard, C.; Li, B.; Zhang, C.; Wang, S.

    2016-03-01

    The pore structure and porosity of a continuous fiber reinforced ceramic matrix composite has been characterized using high-resolution synchrotron X-ray computed tomography (XCT). Segmentation of the reconstructed tomograph images reveals different types of pores within the composite, the inter-fiber bundle open pores displaying a "node-bond" geometry, and the intra-fiber bundle isolated micropores showing a piping shape. The 3D morphology of the pores is resolved and each pore is labeled. The quantitative filtering of the pores measures a total porosity 8.9% for the composite, amid which there is about 7.1~ 9.3% closed micropores.

  6. Compressible cake filtration: monitoring cake formation and shrinkage using synchrotron X-rays

    SciTech Connect

    Bierck, B.R.; Wells, S.A.; Dick, R.I.

    1988-05-01

    High energy, highly collimated X-rays produced at the Cornell High Energy Synchrotron Sources (CHESS) enabled real-time suspended solids concentration measurements each second with 0.5 mm vertical separation in a kaolin filter cake. Suspended solids concentration profiles reflected expected effects of cumulative fluid drag forces. Shrinkage caused a significant increase in average cake suspended solids concentration after expiration of the slurry, and the saturated cake ultimately formed was virtually homogeneous. Shrinkage is consolidation under compressive forces created when capillary menisci form at air/liquid interfaces, and has a significant effect on cake structure in latter stages of compressible cake filtration.

  7. A Optical Synchrotron Nebula around the X-Ray Pulsar 0540-693

    NASA Astrophysics Data System (ADS)

    Chanan, G.; Helfand, D.; Reynolds, S.

    The authors report the discovery of extended optical continuum emission around the recently discovered 50 ms X-ray pulsar in the supernova remnant 0540-693. Exposures in blue and red broadband filters made with the CTIO 4 m telescope and prime focus CCD show a center-brightened but clearly extended nebula about 4arcsec in diameter (FWHM), while an image in an [O III] filter shows an 8arcsec diameter shell (as reported earlier) which encloses the continuum source. 0540-693 is a system very similar to the Crab nebula and represents the second detection of optical synchrotron radiation in a supernova remnant.

  8. Synchrotron x-ray nano-tomography characterization of the sintering of multilayered systems

    NASA Astrophysics Data System (ADS)

    Yan, Zilin; Guillon, Olivier; Wang, Steve; Martin, Christophe L.; Lee, Chul-Seung; Bouvard, Didier

    2012-06-01

    Synchrotron x-ray nano-tomography was used to characterize the microstructures of multi-layer ceramic capacitors before and after sintering. 3D microstructures of the same sample were reconstructed and quantitatively analyzed. The discontinuities observed in inner electrodes were found to originate from initial heterogeneities of nickel powders in the electrodes. They are supposed to grow due to the constraint of adjacent dielectric layers. Dielectric layers show anisotropic shrinkage with a decrease in density as function of layer position in the multilayer.

  9. In-situ synchrotron x-ray transmission microscopy of the sintering of multilayers

    NASA Astrophysics Data System (ADS)

    Yan, Zilin; Guillon, Olivier; Martin, Christophe L.; Wang, Steve; Lee, Chul-Seung; Bouvard, Didier

    2013-06-01

    This letter reports on in-situ characterization of the high temperature sintering of multilayer ceramic capacitors by high-resolution synchrotron x-ray imaging. Microstructural evolution was obtained in real time by a continuous recording of 2-dimensional radiographs. Anisotropic strains were measured for different layers. Quantification of defects was conducted with 3-dimensional nano-computed tomography. These in-situ observations prove that electrode discontinuities occur at the early stage of sintering and originate from initial heterogeneities linked to the particulate nature of the starting powders.

  10. Poly (methyl methacrylate) Formation and Patterning Initiated by Synchrotron X-ray Illumination

    SciTech Connect

    Xiao, J.; Je, J. H.; Wang, C. H.; Yang, T. Y.; Hwu, Y.

    2007-01-19

    A facile radiation method was developed to obtain micro-sized poly (methyl methacrylate) (PMMA) particles and create patterned coating on different substrates by a synchrotron x-ray induced dispersion polymerization. The polymerization of MMA monomer and well defined patterning was successfully realized. The produced PMMA particles and patterning were characterized by Fourier transformation infrared (FTIR), 1H-Nuclear Magnetic Resonance (NMR), and Scanning Electron Microscope (SEM). The observed patterning contrast essentially derived from a variation of size, density and morphology of particles and the type of substrate materials used.

  11. Synchrotron total reflection X-ray fluorescence at BL-16 microfocus beamline of Indus-2

    SciTech Connect

    Tiwari, M. K. Singh, A. K. Das, Gangadhar Chowdhury, Anupam Lodha, G. S.

    2014-04-24

    Determination of ultra trace elements is important in many disciplines both in basic and applied sciences. Numerous applications show their importance in medical science, environmental science, materials science, food processing and semiconductor industries and in maintaining the quality control of ultra pure chemicals and reagents. We report commissioning of a synchrotron based total reflection x-ray fluorescence (TXRF) facility on the BL-16 microfocus beamline of Indus-2. This paper describes the performance of the BL-16 TXRF spectrometer and the detailed description of its capabilities through examples of measured results.

  12. A low-cost X-ray-transparent experimental cell for synchrotron-based X-ray microtomography studies under geological reservoir conditions.

    PubMed

    Fusseis, Florian; Steeb, Holger; Xiao, Xianghui; Zhu, Wen-lu; Butler, Ian B; Elphick, Stephen; Mäder, Urs

    2014-01-01

    A new modular X-ray-transparent experimental cell enables tomographic investigations of fluid rock interaction under natural reservoir conditions (confining pressure up to 20 MPa, pore fluid pressure up to 15 MPa, temperature ranging from 296 to 473 K). The portable cell can be used at synchrotron radiation sources that deliver a minimum X-ray flux density of 10(9) photons mm(-2) s(-1) in the energy range 30-100 keV to acquire tomographic datasets in less than 60 s. It has been successfully used in three experiments at the bending-magnet beamline 2BM at the Advanced Photon Source. The cell can be easily machined and assembled from off-the-shelf components at relatively low costs, and its modular design allows it to be adapted to a wide range of experiments and lower-energy X-ray sources. PMID:24365944

  13. Synchrotron X-ray imaging of nanomagnetism in meteoritic metal (Invited)

    NASA Astrophysics Data System (ADS)

    Bryson, J. F.; Herrero Albillos, J.; Kronast, F.; Tyliszczak, T.; Redfern, S. A.; van der Laan, G.; Harrison, R. J.

    2013-12-01

    It is becoming increasingly apparent that a wealth of paleomagnetic information is stored at the nanoscale within natural samples. To date, this nanopaleomagetism has been investigated using high resolution magnetic microscopies, such as electron holography. Although unparalleled in its spatial resolution, electron holography produces images that are indirectly related to the magnetisation state of the sample, introducing ambiguity when interpreting magnetisation information. Holography also requires extensive off-line processing, making it unsuitable for studying dynamic processes, and the sample preparation negates the study of natural remanences. Here we demonstrate the capabilities of a new generation of nanomagnetic imaging methods using synchrotron X-ray radiation. X-rays tuned to an elemental absorption edge can display differing excitation probabilities depending on the orientation of an electron's magnetic moment relative to that of the X-ray beam. This is achieved by introducing an angular momentum to the photon through circular polarisation, resulting in an absorption signal that is proportional to the projection of the magnetic moment on to the X-ray beam direction. We introduce and compare two experimental set-ups capable of spatially resolving these signals to form a high-resolution magnetisation map: photoemission electron microscopy and scanning transmission electron microscopy. Both techniques provide measurements of magnetisation with 30-50nm resolution and elemental specificity. Photoemission electron microscopy can be used also to create maps of all three of the spatial components of magnetisation and investigate dynamic magnetic switching processes. The full capabilities of X-ray imaging are demonstrated through the application of both of these techniques to meteoritic metal. We show that the 'cloudy zone' within iron meteorites contains nanoscale islands of tetrataenite (FeNi) that are populated equally by all three possible magnetic easy axes

  14. The rf system of the Synchrotron X-ray Source at Argonne

    SciTech Connect

    Kustom, R.L.; Mavrogenes, G.; Nicholls, G.

    1987-01-01

    A Positron Storage Ring for the Synchrotron X-ray Source at Argonne is under design. The rf system is described. The rf system is divided into four stations, each using a one-megawatt klystron to excite four single-cell spherical cavities to a gap voltage of 761 kV at the operating frequency of 350.8 MHz. The same klystron also provides the beam power for synchrotron radiation losses of the position beam of up to 300 mA, the higher-order-mode power losses, the power losses in the beam due to the insertion devices, and the rf power transmission losses. The transmission waveguide system includes magic tees for splitting the power of each klystron to four cavities, isolators to protect the klystrons, harmonic and higher-order-mode absorbers, and mechanical phase shifters for fine phase tuning.

  15. Multilayer-based soft X-ray polarimeter at the Beijing Synchrotron Radiation Facility

    NASA Astrophysics Data System (ADS)

    Sun, Li-Juan; Cui, Ming-Qi; Zhu, Jie; Zhao, Yi-Dong; Zheng, Lei; Wang, Zhan-Shan; Zhu, Jing-Tao

    2013-07-01

    A compact high precision eight-axis automatism and two-axis manual soft-ray polarimeter with a multilayer has been designed, constructed, and installed in 3W1B at the Beijing Synchrotron Radiation Facility (BSRF). Four operational modes in the same device, which are double-reflection, double-transmission, front-reflection-behind-transmission and front-transmission-behind-reflection, have been realized. It can be used for the polarization analysis of synchrotron radiation. It also can be used to characterize the polarization properties of the optical elements in the soft X-ray energy range. Some experiments with Mo/Si and Cr/C multilayers have been performed by using this polarimeter with good results obtained.

  16. High Resolution X-Ray Microangiography of 4T1 Tumor in Mouse Using Synchrotron Radiation

    SciTech Connect

    Sun Jianqi; Liu Ping; Gu Xiang; Liu Xiaoxia; Zhao Jun; Xiao Tiqiao; Xu, Lisa X.

    2010-07-23

    Angiogenesis is very important in tumor growth and metastasis. But in clinic, only vessels lager than 200 {mu}m in diameter, can be observed using conventional medical imaging. Synchrotron radiation (SR) phase contrast imaging, whose spatial resolution can reach as high as 1 {mu}m, has great advantages in imaging soft tissue structures, such as blood vessels and tumor tissues. In this paper, the morphology of newly formed micro-vessels in the mouse 4T1 tumor samples was firstly studied with contrast agent. Then, the angiogenesis in nude mice tumor window model was observed without contrast agent using the SR phase contrast imaging at the beamline for X-ray imaging and biomedical applications, Shanghai Synchrotron Radiation Facility (SSRF). The images of tumors showed dense, irregular and tortuous tumor micro-vessels with the smallest size of 20-30 {mu}m in diameter.

  17. Synchrotron X-ray CT characterization of titanium parts fabricated by additive manufacturing. Part II. Defects.

    PubMed

    Scarlett, Nicola Vivienne Yorke; Tyson, Peter; Fraser, Darren; Mayo, Sheridan; Maksimenko, Anton

    2016-07-01

    Synchrotron X-ray tomography (SXRT) has been applied to the study of defects within three-dimensional printed titanium parts. These parts were made using the Arcam EBM(®) (electron beam melting) process which uses powdered titanium alloy, Ti64 (Ti alloy with approximately 6%Al and 4%V) as the feed and an electron beam for the sintering/welding. The experiment was conducted on the Imaging and Medical Beamline of the Australian Synchrotron. The samples represent a selection of complex shapes with a variety of internal morphologies. Inspection via SXRT has revealed a number of defects which may not otherwise have been seen. The location and nature of such defects combined with detailed knowledge of the process conditions can contribute to understanding the interplay between design and manufacturing strategy. This fundamental understanding may subsequently be incorporated into process modelling, prediction of properties and the development of robust methodologies for the production of defect-free parts. PMID:27359151

  18. Steady X-Ray Synchrotron Emission in the Northeastern Limb of SN 1006

    NASA Technical Reports Server (NTRS)

    Katsuda, Satoru; Petre, Robert; Mori, Koji; Reynolds, Stephen; Long, Knox; Winkler, P.; Tsunemi, Hiroshi

    2010-01-01

    We investigate time variations and detailed spatial structures of X-ray synchrotron emission in the northeastern limb of SN 1006, using two Chandra observations taken in 2000 and 2008. We extract spectra from a number of small ([approx]10'') regions. After taking account of proper motion and isolating the synchrotron from the thermal emission, we study time variations in the synchrotron emission in the small regions. We find that there are no regions showing strong flux variations. Our analysis shows an apparent flux decline in the overall synchrotron flux of [approx]4% at high energies, but we suspect that this is mostly a calibration effect, and that flux is actually constant to [approx]1%. This is much less than the variation found in other remnants where it was used to infer magnetic-field strengths up to 1 mG. We attribute the lack of variability to the smoothness of the synchrotron morphology, in contrast to the small-scale knots found to be variable in other remnants. The smoothness is to be expected for a Type Ia remnant encountering uniform material. Finally, we find a spatial correlation between the flux and the cutoff frequency in synchrotron emission. The simplest interpretation is that the cutoff frequency depends on the magnetic-field strength. This would require that the maximum energy of accelerated electrons is not limited by synchrotron losses, but by some other effect. Alternatively, the rate of particle injection and acceleration may vary due to some effect not yet accounted for, such as a dependence on shock obliquity.

  19. Spatially confined low-power optically pumped ultrafast synchrotron x-ray nanodiffraction

    SciTech Connect

    Park, Joonkyu; Zhang, Qingteng; Chen, Pice; Cosgriff, Margaret P.; Tilka, Jack A.; Evans, Paul G.; Adamo, Carolina; Schlom, Darrell G.; Wen, Haidan; Zhu, Yi

    2015-08-15

    The combination of ultrafast optical excitation and time-resolved synchrotron x-ray nanodiffraction provides unique insight into the photoinduced dynamics of materials, with the spatial resolution required to probe individual nanostructures or small volumes within heterogeneous materials. Optically excited x-ray nanobeam experiments are challenging because the high total optical power required for experimentally relevant optical fluences leads to mechanical instability due to heating. For a given fluence, tightly focusing the optical excitation reduces the average optical power by more than three orders of magnitude and thus ensures sufficient thermal stability for x-ray nanobeam studies. Delivering optical pulses via a scannable fiber-coupled optical objective provides a well-defined excitation geometry during rotation and translation of the sample and allows the selective excitation of isolated areas within the sample. Experimental studies of the photoinduced lattice dynamics of a 35 nm BiFeO{sub 3} thin film on a SrTiO{sub 3} substrate demonstrate the potential to excite and probe nanoscale volumes.

  20. CMOS Imaging Detectors as X-ray Detectors for Synchrotron Radiation Experiments

    SciTech Connect

    Yagi, Naoto; Uesugi, Kentaro; Inoue, Katsuaki

    2004-05-12

    CMOS imagers are matrix-addressed photodiode arrays, which have been utilized in devices such as commercially available digital cameras. The pixel size of CMOS imagers is usually larger than that of CCD and smaller than that of TFT, giving them a unique position. Although CMOS x-ray imaging devices have already become commercially available, they have not been used as an x-ray area detector in synchrotron radiation experiments. We tested performance of a CMOS detector from Rad-icon (Shad-o-Box1024) in medical imaging, small-angle scattering, and protein crystallography experiments. It has pixels of 0.048 mm square, read-out time of 0.45 sec, 12-bit ADC, and requires a frame grabber for image acquisition. The detection area is 5-cm square. It uses a Kodak Min-R scintillator screen as a phosphor. The sensitivity to x-rays with an energy less than 15 keV was low because of the thick window materials. Since the readout noise is high, the dynamic range is limited to 2000. The biggest advantages of this detector are cost-effectiveness (about 10,000 US dollars) and compactness (thickness < 3 cm, weight < 2 kg)

  1. Spatially confined low-power optically pumped ultrafast synchrotron x-ray nanodiffraction.

    PubMed

    Park, Joonkyu; Zhang, Qingteng; Chen, Pice; Cosgriff, Margaret P; Tilka, Jack A; Adamo, Carolina; Schlom, Darrell G; Wen, Haidan; Zhu, Yi; Evans, Paul G

    2015-08-01

    The combination of ultrafast optical excitation and time-resolved synchrotron x-ray nanodiffraction provides unique insight into the photoinduced dynamics of materials, with the spatial resolution required to probe individual nanostructures or small volumes within heterogeneous materials. Optically excited x-ray nanobeam experiments are challenging because the high total optical power required for experimentally relevant optical fluences leads to mechanical instability due to heating. For a given fluence, tightly focusing the optical excitation reduces the average optical power by more than three orders of magnitude and thus ensures sufficient thermal stability for x-ray nanobeam studies. Delivering optical pulses via a scannable fiber-coupled optical objective provides a well-defined excitation geometry during rotation and translation of the sample and allows the selective excitation of isolated areas within the sample. Experimental studies of the photoinduced lattice dynamics of a 35 nm BiFeO3 thin film on a SrTiO3 substrate demonstrate the potential to excite and probe nanoscale volumes. PMID:26329208

  2. Absorption and Phase Contrast X-Ray Imaging in Paleontology Using Laboratory and Synchrotron Sources.

    PubMed

    Bidola, Pidassa; Stockmar, Marco; Achterhold, Klaus; Pfeiffer, Franz; Pacheco, Mírian L A F; Soriano, Carmen; Beckmann, Felix; Herzen, Julia

    2015-10-01

    X-ray micro-computed tomography (μCT) is commonly used for imaging of samples in biomedical or materials science research. Owing to the ability to visualize a sample in a nondestructive way, X-ray μCT is perfectly suited to inspect fossilized specimens, which are mostly unique or rare. In certain regions of the world where important sedimentation events occurred in the Precambrian geological time, several fossilized animals are studied to understand questions related to their origin, environment, and life evolution. This article demonstrates the advantages of applying absorption and phase-contrast CT on the enigmatic fossil Corumbella werneri, one of the oldest known animals capable of building hard parts, originally discovered in Corumbá (Brazil). Different tomographic setups were tested to visualize the fossilized inner structures: a commercial laboratory-based μCT device, two synchrotron-based imaging setups using conventional absorption and propagation-based phase contrast, and a commercial X-ray microscope with a lens-coupled detector system, dedicated for radiography and tomography. Based on our results we discuss the strengths and weaknesses of the different imaging setups for paleontological studies. PMID:26306692

  3. Synchrotron x-ray study of the smectic layer directional instability

    PubMed

    Dierking; Glusen; Lagerwall; Ober

    2000-02-01

    We have investigated the phenomenon of field-induced smectic layer instability, as monitored by synchrotron x-ray scattering. This instability means that, upon application of time-asymmetric electric fields to chiral smectics, the layer direction seems to "rotate" locally around an axis given by the direction of the applied field. For moderate values of field amplitude and asymmetry, domains with a favored layer inclination grow at the expense of unfavored ones, while larger fields and asymmetries generally lead to a chaotic flow behavior. At moderate amplitudes, we have followed the process of the horizontal layer folding (or horizontal chevron domain formation) and the smectic C* layer reorientation of ferroelectric liquid crystals by applying symmetric and asymmetric wave forms, respectively, and performing time resolved x-ray measurements. The studies unambiguously show the formation of a horizontal (in-plane, i.e., in a plane parallel to the cell substrates) chevron domain structure from a nonoriented sample by application of a symmetric electric field of sufficient amplitude. It is then demonstrated that a transition from the horizontal chevron domain structure to an in-plane uniform smectic layer direction takes place on application of asymmetric electric wave forms. Reversal of the field asymmetry reverses the inclination direction and selects the other layer normal direction as the uniform end state. The in-plane smectic layer reorientation process is followed here as it evolves, and analyzed directly by means of x-ray scattering. PMID:11046442

  4. Absorption and Phase Contrast X-Ray Imaging in Paleontology Using Laboratory and Synchrotron Sources

    SciTech Connect

    Bidola, Pidassa; Stockmar, Marco; Achterhold, Klaus; Pfeiffer, Franz; Pacheco, Mirian L.A.F.; Soriano, Carmen; Beckmann, Felix; Herzen, Julia

    2015-10-01

    X-ray micro-computed tomography (CT) is commonly used for imaging of samples in biomedical or materials science research. Owing to the ability to visualize a sample in a nondestructive way, X-ray CT is perfectly suited to inspect fossilized specimens, which are mostly unique or rare. In certain regions of the world where important sedimentation events occurred in the Precambrian geological time, several fossilized animals are studied to understand questions related to their origin, environment, and life evolution. This article demonstrates the advantages of applying absorption and phase-contrast CT on the enigmatic fossil Corumbella werneri, one of the oldest known animals capable of building hard parts, originally discovered in Corumba (Brazil). Different tomographic setups were tested to visualize the fossilized inner structures: a commercial laboratory-based CT device, two synchrotron-based imaging setups using conventional absorption and propagation-based phase contrast, and a commercial X-ray microscope with a lens-coupled detector system, dedicated for radiography and tomography. Based on our results we discuss the strengths and weaknesses of the different imaging setups for paleontological studies.

  5. X-ray optics developments at the APS for third-generation synchrotron radiation sources

    SciTech Connect

    Mills, D.M.

    1996-09-01

    High brilliance third-generation synchrotron radiation sources simultaneously provide both a need and an opportunity for the development of new x-ray optical components. The high power and power densities of the x-ray beams produced by insertion devices have forced researchers to consider novel, and what may seem like exotic, approaches to the mitigation of thermal distortions that can dilute the beam brilliance delivered to the experiment or next optical component. Once the power has been filtered by such high heat load optical elements, specialized components can be employed that take advantage of the high degree of brilliance. This presentation reviews the performance of optical components that have been designed, fabricated, and tested at the Advanced Photon Source, starting with high heat load components and followed by examples of several specialized devices such as a milli-eV resolution (in-line) monochromator, a high energy x-ray phase retarder, and a phase zone plate with submicron focusing capability.

  6. Ice Recrystallization in a Solution of a Cryoprotector and Its Inhibition by a Protein: Synchrotron X-Ray Diffraction Study.

    PubMed

    Zakharov, Boris; Fisyuk, Alexander; Fitch, Andy; Watier, Yves; Kostyuchenko, Anastasia; Varshney, Dushyant; Sztucki, Michael; Boldyreva, Elena; Shalaev, Evgenyi

    2016-07-01

    Ice formation and recrystallization is a key phenomenon in freezing and freeze-drying of pharmaceuticals and biopharmaceuticals. In this investigation, high-resolution synchrotron X-ray diffraction is used to quantify the extent of disorder of ice crystals in binary aqueous solutions of a cryoprotectant (sorbitol) and a protein, bovine serum albumin. Ice crystals in more dilute (10 wt%) solutions have lower level of microstrain and larger crystal domain size than these in more concentrated (40 wt%) solutions. Warming the sorbitol-water mixtures from 100 to 228 K resulted in partial ice melting, with simultaneous reduction in the microstrain and increase in crystallite size, that is, recrystallization. In contrast to sorbitol solutions, ice crystals in the BSA solutions preserved both the microstrain and smaller crystallite size on partial melting, demonstrating that BSA inhibits ice recrystallization. The results are consistent with BSA partitioning into quasi-liquid layer on ice crystals but not with a direct protein-ice interaction and protein sorption on ice surface. The study shows for the first time that a common (i.e., not-antifreeze) protein can have a major impact on ice recrystallization and also presents synchrotron X-ray diffraction as a unique tool for quantification of crystallinity and disorder in frozen aqueous systems. PMID:27287516

  7. Melting curve of NaCl determined using synchrotron x-ray radiography

    NASA Astrophysics Data System (ADS)

    Chen, J.; Yu, T.; Long, H.; Wang, L.; Garai, J.

    2009-12-01

    NaCl has been widely used as a pressure calibrant in in-situ high pressure synchrotron x-ray study. The applicable pressure and temperature range of this calibrant is from ambient condition up to B1-B2 transition in pressure and to melting in temperature. Melting data of NaCl at high pressures are still very limited. We have conducted comparative experiments to study melting of NaCl using energy dispersive x-ray diffraction and radiographic imaging at high pressure up to 8.8GPa. The experiments were carried out using the cubic-type multi-anvil pressure (SAM85) at the X17B2 beamline of the National Synchrotron Light Source (NSLS). In the x-ray diffraction experiments, melting is inferred when disappearance of diffraction peak of NaCl from a mixture of NaCl+BN (to reduce possible grain growth) is observed. In the x-ray radiography experiment, a WC sphere is place in the top portion of pure NaCl sample; melting is inferred when the WC sphere start to drop in the sample. The experimental result indicates that the melting temperatures determined from the two types of observations may differ by 60°C at 5 GPa. Due to unavoidable grain growth near melting, x-ray diffraction signals may disappear from the point solid state detector even though the melting is not achieved. Therefore the radiography method may reflect more accurate measurement of melting temperature. Melting curve of NaCl was measured up to 1.8 GPa by Clark et al (1), and between 2 and 4 GPa by Pistorius (2). The new melting data are consistent with the previous results. All the experimental are in good agreement with theoretical prediction using Simon fusion equation (2) and the relation between melting temperature and Debye temperature (3). References: (1) Clark, Jr. Effect of Pressure on the Melting Points of Eight Alkali Halides, Journal of Chemical Physics 31 (6) 1526-1531 (1959). (2) Kraut and Kennedy, New Melting Law at High Pressures, Physical Review 151 (2) 668-675 (1966) (3) J. Garai, and J. Chen

  8. Structural characterization of sol-gel derived oxide nanostuctures using synchrotron x-ray techniques

    NASA Astrophysics Data System (ADS)

    Sun, Tao

    Ceramic oxides possess extraordinarily rich functionalities. With the advent of nanofabrication techniques, it is now possible to grow nanostructured oxides with precise control of composition, morphology, and microstructure, which has re-vitalized the research in the field of traditional ceramics. The unexpected behavior and enhanced properties of oxide nanostructures have been extensively reported. However, knowledge about the underlying mechanisms as well as structural implications is still quite limited. Therefore, it is imperative to develop and employ sophisticated characterization tools for unraveling the structure-property relationships for oxide nanostructures. The present thesis work aims at addressing the critical issues associated with fabrication, and more importantly, structural characterization of functional oxide nanostructures. The dissertation starts with introducing the strategy for synthesizing phase-pure and highly controlled oxide nanostructures using sol-gel deposition and an innovative approach called "soft" electron beam lithography. Some specific oxides are chosen for the present study, such as BiFeO3, CoFe2O4, and SnO2, because of their scientific and technological significance. Subsequent to fabrication of tailored oxide nanostructures, advanced synchrotron x-ray scattering techniques have been applied for structural characterization. The nucleation and growth behavior of BiFeO3 thin film was investigated using in situ grazing-incidence small-angle x-ray scattering (GISAXS) technique. The results reveal that the kinetics for early-stage nuclei growth are governed by the oriented-attachment model. Moreover, the porous structures of undoped and Pd-doped semiconducting SnOx thin films were quantitatively characterized using GISAXS. By correlating the structural parameters with H2 sensitivity of SnOx films, it is found out that the microstructure of doped film is favorable for gas sensing, but it is not the major reason for the overall

  9. Defect characterization and stress analysis by white beam synchrotron X-ray topography in single crystal semiconducting materials

    NASA Astrophysics Data System (ADS)

    Sarkar, Vishwanath

    Semiconductor devices are becoming increasingly more complex as the number of transistors increases in the same Integrated Circuit (IC) area. Due to the complexity in design; processing and packaging of the device plays a crucial role in the IC fabrication. Package induced residual stress are not only detrimental to device performance but can also lead to device failure. We propose a non-destructive method to determine the complete stress state at each point on a packaged Silicon device. Surface and edge defect created as a result of various manufacturing steps were characterized using different techniques, primarily X-ray diffraction topography, optical microscopy, SEM and TEM. Residual stress plays an important role in the performance and lifetime of single crystal device material. Here we present a novel technique using white beam synchrotron X-ray diffraction reticulography, Stress Mapping and Analysis via Ray Tracing (SMART) in order to determine residual stress level at an array of points over the entire crystal area. This method has a unique advantage compared with other stress measurement technique in that it can evaluate all six components of the stress tensor. The underlying experimental technique is based on white beam synchrotron X-ray diffraction topography and ray tracing. An array of X-ray micro-beam is illuminated on the single crystal sample and multiple reflections (reticulographs) are recorded simultaneously on a photographic film. Crystallographic plane normal vector at the location of each micro-beam in the crystal is calculated. The variation of the plane normal vector direction is due to residual strain (both sheer and dilatational) present in the crystal. By considering three different diffracting planes and corresponding reticulograph a complete state of stress is calculated. Principle, applications and limitations are discussed. White beam synchrotron reticulography is used in reflection geometry to evaluate complete residual stress tensor

  10. Real-time microstructure of shocked LiF crystals: Use of synchrotron x-rays

    NASA Astrophysics Data System (ADS)

    Turneaure, Stefan J.; Gupta, Y. M.; Zimmerman, K.; Perkins, K.; Yoo, C. S.; Shen, G.

    2009-03-01

    We describe the use of a third generation synchrotron facility to obtain in situ, real-time, x-ray diffraction measurements in plate impact experiments. Subnanosecond duration x-ray pulses were utilized to record diffraction data from pure and magnesium-doped LiF single crystals shocked along the [111] and [100] orientations. The peak stresses were 3.0 GPa for the [111] oriented LiF and between 3.0 and 5.0 GPa for the [100] oriented LiF. For these stresses, shock compression along [111] results in elastic deformation and shock compression along [100] results in elastic-plastic deformation. Because of the quality of the synchrotron x-ray pulses, both shifting and broadening of the diffraction data were obtained simultaneously. As expected, shifts for elastic compression and elastic-plastic compression in shocked LiF were consistent with uniaxial and isotropic lattice compression, respectively. More importantly, diffraction patterns from crystals shocked along [100] exhibited substantial broadening due to elastic-plastic deformation. The broadening indicates that the shocked LiF(100) crystals developed substructure with a characteristic size for coherently diffracting domains (0.1-10 μm) and a distribution of (100) microlattice-plane rotations (˜1° wide). In contrast to the LiF(100) results, broadening of the diffraction pattern did not occur for elastically deformed LiF(111). Another important finding was that the amount of lattice disorder for shocked LiF(100) depends on the loading history; the broadening was larger for the magnesium-doped LiF(100) (large elastic precursor) than for ultrapure LiF(100) (small elastic precursor) shocked to the same peak stress. The data are simulated by calculating the diffraction pattern from LiF(100) with a model microstructure consisting of coherently diffracting domains. The lattice orientation and longitudinal strain is assumed uniform within domains, but they vary from domain to domain with Gaussian distributions

  11. Solution Synchrotron X-ray Diffraction Reveals Structural Details of Lipid Domains in Ternary Mixtures

    SciTech Connect

    Yuan, J.; Kiss, A; Pramudya, Y; Nguyen, L; Hirst, L

    2009-01-01

    The influence of cholesterol on lipid bilayer structure is significant and the effect of cholesterol on lipid sorting and phase separation in lipid-raft-forming model membrane systems has been well investigated by microscopy methods on giant vesicles. An important consideration however is the influence of fluorescence illumination on the phase state of these lipids and this effect must be carefully minimized. In this paper, we show that synchrotron x-ray scattering on solution lipid mixtures is an effective alternative technique for the identification and characterization of the l o (liquid ordered) and l d (liquid disordered) phases. The high intensity of synchrotron x rays allows the observation of up to 5 orders of diffraction from the l o phase, whereas only two are clearly visible when the l d phase alone is present. This data can be collected in approximately 1 min/sample, allowing rapid generation of phase data. In this paper, we measure the lamellar spacing in both the liquid-ordered and liquid-disordered phases simultaneously, as a function of cholesterol concentration in two different ternary mixtures. We also observe evidence of a third gel-phaselike population at 10-12 mol % cholesterol and determine the thickness of the bilayer for this phase. Importantly we are able to look at phase coexistence in the membrane independent of photoeffects.

  12. Synchrotron X-ray CT characterization of friction-welded joints in tial turbocharger components

    NASA Astrophysics Data System (ADS)

    Sun, J. G.; Kropf, A. J.; Vissers, D. R.; Sun, W. M.; Katsoudas, J.; Yang, N.; Fei, D.

    2012-05-01

    Titanium aluminide (TiAl) is an advanced intermetallic material and is being investigated for application in turbocharger components for diesel engines. A TiAl turbocharger rotor consists of a cast TiAl turbine wheel and a Ti-alloy shaft that are joined by friction welding. Although friction welding is an established industrial process, it is still challenging to join dissimilar materials especially for brittle intermetallics. These joints are therefore required to be inspected using a nondestructive evaluation (NDE) method. In this study, synchrotron X-ray computed tomography (CT) developed at the Advanced Photon Source at Argonne National Laboratory was used for NDE characterization of friction-welded joint in three TiAl turbocharger rotors. The filtered synchrotron X-ray source has high peak energies to penetrate thick metallic materials, and the detector (imager) has high spatial resolutions to resolve small flaws. The CT inspections revealed detailed 3D crack distributions within poorly welded joints. The crack detection sensitivity and resolution was calibrated and found to be correlated well with destructive examination.

  13. Mapping Metal Elements of Shuangbai Dinosaur Fossil by Synchrotron X-ray Fluorescence Microprobe

    SciTech Connect

    Wang, Y.; Qun, Y; Ablett, J

    2008-01-01

    The metal elements mapping of Shuangbai dinosaur fossil, was obtained by synchrotron x-ray fluorescence (SXRF). Eight elements, Ca, Mn, Fe, Cu, Zn, As, Y and Sr were determined. Elements As and Y were detected for the first time in the dinosaur fossil. The data indicated that metal elements are asymmetrical on fossil section. This is different from common minerals. Mapping metals showed that metal element As is few. The dinosaur most likely belongs to natural death. This is different from Zigong dinosaurs which were found dead from poisoning. This method has been used to find that metals Fe and Mn are accrete, and the same is true for Sr and Y. This study indicated that colloid granule Fe and Mn, as well as Sr and Y had opposite electric charges in lithification process of fossils. By this analysis, compound forms can be ascertained. Synchrotron light source x-ray fluorescence is a complementary method that shows mapping of metal elements at the dinosaur fossil, and is rapid, exact and intuitionist. This study shows that dinosaur fossil mineral imaging has a potential in reconstructing the paleoenvironment and ancient geology.

  14. Synchrotron Powder X-ray Diffraction Study of the Structure and Dehydration Behavior of Sepiolite

    SciTech Connect

    Post,J.; Bish, D.; Heaney, P.

    2007-01-01

    Rietveld refinements using synchrotron powder X-ray diffraction data were used to study the crystal structure and dehydration behavior of sepiolite from Durango, Mexico. The room-temperature (RT) sepiolite structure in air compares well with previous models but reveals an additional zeolitic H{sub 2}O site. The RT structure under vacuum retained only {approx}1/8 of the zeolitic H{sub 2}O and the volume decreased by 1.3%. Real-time, temperature-resolved synchrotron powder X-ray diffraction data and Rietveld refinements were used to investigate the behavior of the sepiolite structure from 300 to 925 K. Rietveld refinements revealed that most of the zeolitic H{sub 2}O is lost by {approx}390 K, accompanied by a decrease in the a and c unit-cell parameters. Above {approx}600 K the sepiolite structure folds as one-half of the crystallographically bound H{sub 2}O is lost. Rietveld refinements of the 'anhydrous' sepiolite structure reveal that, in general, unit-cell parameters a and b and volume steadily decrease with increasing temperature; there is an obvious change in slope at {approx}820 K suggesting a phase transformation coinciding with the loss of the remaining bound H{sub 2}O molecule.

  15. Synchrotron radiation induced μ-X-ray fluorescence spectroscopy on municipal solid waste fly ashes

    NASA Astrophysics Data System (ADS)

    Camerani, Maria Caterina; Somogyi, Andrea; Drakopoulos, Mikael; Steenari, Britt-Marie

    2001-08-01

    The high brightness of synchrotron radiation sources of the 3rd generation and the development of focusing optical elements for X-rays make it possible to create beams of micrometer size with high intensity. These beams can be used to reveal spatially resolved information about structural and chemical properties of particles. Here, the possibility of using synchrotron radiation micro-X-ray fluorescence (μ-SRXRF) for the determination of the major and minor components and their distribution within municipal solid waste (MSW) fly ashes has been investigated. By using an excitation energy of 27.0 keV, trace elements of environmental concern, like Cd, Pb and Zn can be detected to their low concentrations (ppm) routinely. The aim of the work was to gain a better understanding of the factors that determine the environmental mobility of each trace element and, in particular, the potential for their dissolution and leaching. Such detailed investigation of the content and distribution of toxic metals on/in individual particles is a valuable complement to the usual elemental analysis of bulk samples.

  16. Pore level imaging of fluid transport using synchrotron x-ray microtomography

    SciTech Connect

    Coles, M.E.; Hazlett, R.D.; Muegge, E.L.; Spanne, P.; Soll, W.E.; Jones, K.W.

    1996-12-31

    Recently developed high resolution computed microtomography (CMI) using synchrotron X-ray sources is analogous to conventional medical Cr scanning and provides the ability to obtain three-dimensional images of specimens with a spatial resolution on the order of micrometers. Application of this technique to the study of core samples has previously been shown to provide excellent two- and three-dimensional high resolution descriptions of pore structure and mineral distributions of core material. Recently, computed microtomographic endpoint saturation images of a fluid filled sandstone core sample were obtained using a microtomographic apparatus and a high energy X-ray beam produced by a superconducting wiggler at the National Synchrotron Light Source at Brookhaven National Laboratory. Images of a 6 mm subsection of the one inch diameter core sample were obtained prior and subsequent to flooding to residual oil. Both oil and brine phases were observable within the imaged rock matrix. The rock matrix image data was used as input to a fluid transport simulator and the results compared with the end point saturation images and data. These high resolution images of the fluid filled pore space have not been previously available to researchers and will provide valuable insight to fluid flow, and provide data as input into and validation of high resolution porous media flow simulators, such as percolation-network and Lattice Boltzmann models.

  17. Ptychographic coherent x-ray surface scattering imaging

    NASA Astrophysics Data System (ADS)

    Kim, Jong Woo; Jiang, Zhang; Sun, Tao; Wang, Jin

    Lensless x-ray coherent diffraction imaging enables the determination of nano-scaled structures in physical and biological sciences. Several coherent diffractive imaging (CDI) methods have been developed in both transmission and reflection modes such as Bragg CDI, plane-wave CDI, Fresnel CDI, coherent surface scattering imaging (CSSI) and so on. The grazing-incidence coherent surface scattering (CSSI) technique, which is recently developed by T. Sun et al., takes advantage of enhanced x-ray surface scattering and interference near total external reflection, and thereby overcomes some limitations that the transmission mode have. However, the sample size can be investigated is limited by x-ray beam size because the sample is supposed to be isolated. We incorporated ptychographic algorithm with coherent surface scattering imaging to overcome this limitation and make it more useful and applicable. The ptychographic coherent surface scattering imaging technique enables us to measure 2D roughness of the flat surface such as thin film and silicon wafer regardless of the surface area. LDRD.

  18. Analysis of heat-affected zone phase transformations using in situ spatially resolved x-ray diffraction with synchrotron radiation

    SciTech Connect

    Elmer, J.W.; Wong, J.; Froeba, M.; Waide, P.A.; Larson, E.M.

    1996-03-01

    Spatially resolved X-ray diffraction (SRXRD) consists of producing a submillimeter size X-ray beam from an intense synchrotron radiation source to perform real-time diffraction measurements on solid materials. This technique was used int his study to investigate the crystal phases surrounding a liquid weld pool in commercial purity titanium and to determine the location of the phase boundary separating the high-temperature body-centered-cubic (bcc) {beta} phase from the low-temperature hexagonal-close-packed (hcp) {alpha} phase. The experiments were carried out at the Stanford Synchrotron Radiation Laboratory (SSRL) using a 0.25 x 0.50 mm X-ray probe that could be positioned with 10-{micro}m precision on the surface of a quasistationary gas tungsten arc weld (GTAW). The SRXRD results showed characteristic hcp, bcc, and liquid diffraction patterns at various points along the sample, starting from the base metal through the heat-affected zone (HAZ) and into the weld pool, respectively. Analyses of the SRXRD data show the coexistence of bcc and hcp phases in the partially transformed (outer) region of the HAZ and single-phase bcc in the fully transformed (inner) region of the HAZ. Postweld metallographic examinations of the HAZ, combined with a conduction-based thermal model of the weld, were correlated with the SRXRD results. Finally, analysis of the diffraction intensities of the hcp and bcc phases was performed on the SRXRD data to provide additional information about the microstructural conditions that may exist in the HAZ at temperature during welding. This work represents the first direct in situ mapping of phase boundaries in fusion welds.

  19. Evaluation of surface figure error profile of ellipsoidal mirror for soft x-ray focusing

    NASA Astrophysics Data System (ADS)

    Takeo, Yoko; Saito, Takahiro; Mimura, Hidekazu

    2015-08-01

    It is possible to achieve soft X-ray nanofocusing with a high efficiency and no chromatic aberration by using an ultraprecise ellipsoidal mirror. Surface figure metrology is key in the improvement of surface figure accuracy. In this study, we propose a ptychographic phase retrieval method using a visible light laser to measure the surface figure error profile of an ellipsoidal mirror. We introduce a simple experimental system for ptychographic phase retrieval and demonstrate the basic performance of the proposed system. Obtainable wavefront information provides both the figure error and the alignment of the ellipsoidal mirror that yield the best focusing. This developed method is required for offline adjustments when an ellipsoidal mirror is installed in the beamline of synchrotron radiation or X-ray free-electron laser light sources.

  20. Real-time, high-resolution x-ray diffraction measurements on shocked crystals at a synchrotron facility

    NASA Astrophysics Data System (ADS)

    Gupta, Y. M.; Turneaure, Stefan J.; Perkins, K.; Zimmerman, K.; Arganbright, N.; Shen, G.; Chow, P.

    2012-12-01

    The Advanced Photon Source (APS) at Argonne National Laboratory was used to obtain real-time, high-resolution x-ray diffraction measurements to determine the microscopic response of shock-compressed single crystals. Disk shaped samples were subjected to plane shock wave compression by impacting them with half-inch diameter, flat-faced projectiles. The projectiles were accelerated to velocities ranging between 300 and 1200 m/s using a compact powder gun designed specifically for use at a synchrotron facility. The experiments were designed to keep the sample probed volume under uniaxial strain and constant stress for a duration longer than the 153.4 ns spacing between x-ray bunches. X-rays from a single pulse (<100 ps duration) out of the periodic x-ray pulses emitted by the synchrotron were used for the diffraction measurements. A synchronization and x-ray detection technique was developed to ensure that the measured signal was obtained unambiguously from the desired x-ray pulse incident on the sample while the sample was in a constant uniaxial strain state. The synchronization and x-ray detection techniques described can be used for a variety of x-ray measurements on shock compressed solids and liquids at the APS. Detailed procedures for applying the Bragg-Brentano parafocusing approach to single crystals at the APS are presented. Analytic developments to determine the effects of crystal substructure and non-ideal geometry on the diffraction pattern position and shape are presented. Representative real-time x-ray diffraction data, indicating shock-induced microstructural changes, are presented for a shock-compressed Al(111) sample. The experimental developments presented here provided, in part, the impetus for the Dynamic Compression Sector (DCS) currently under development at the APS. Both the synchronization/x-ray detection methods and the analysis equations for high-resolution single crystal x-ray diffraction can be used at the DCS.

  1. Development of a Linear Stitching Interferometric System for Evaluation of Very Large X-ray Synchrotron Radiation Substrates and Mirrors

    SciTech Connect

    Assoufid, Lahsen; Shu Deming; Bray, Michael

    2004-05-12

    Stitching interferometry, using small-aperture, high-resolution, phase-measuring interferometric systems has been investigated for quite some time now as a metrology technique to obtain surface profiles of oversized optical components and substrates. The technique offers the potential for providing 3D measurements of mirror surfaces with nanometer resolution. The aim of this work is to apply this technique to the specific case of large, flat, grazing-incidence x-ray mirrors, such as those used in beamlines at synchrotron radiation facilities around the world. In the case of x-ray mirrors, obtaining a 3D surface profile can be particularly useful in many instances, for example, in selecting the best reflecting stripe on a mirror surface to be used for undulator beams. The measurement data can be used for simulating and predicting mirror performance under realistic conditions, etc. A fully automated stitching system is currently being developed at the metrology laboratory of the Advanced Photon Source at Argonne National Laboratory. Preliminary tests performed on a 460-mm-long flat float-glass substrate and on a 300-mm-long superpolished silicon substrate, were encouraging. The stitched profiles showed no obvious overlap errors, and the results agree well with those obtained using other techniques.

  2. Pulsed synchrotron x-ray as a tool for providing molecular movies at 100-picosecond temporal and sub-nanometer spatial resolution

    NASA Astrophysics Data System (ADS)

    Adachi, S.; Nozawa, S.; Ichiyanagi, K.; Ichikawa, H.; Chollet, M.; Guérin, L.; Tazaki, R.; Sato, T.; Tomita, A.; Sawa, H.; Arima, T.; Kawata, H.; Koshihara, S.

    2009-02-01

    Time-resolved X-ray techniques utilizing pulsed nature of synchrotron radiation are becoming general and powerful tools to explore structural dynamics in materials and biological systems. The time-resolved technique enables to produce structural movies at 100-picosecond temporal and sub-nanometer spatial resolution. It will be fascinating to apply such capabilities to capture ultrafast cooperative phenomena in strongly-correlated electron systems, photochemical catalytic reaction dynamics in liquid or on solid surface, light-induced response of photosensitive protein molecules, etc. The time-resolved X-ray studies conducted at NW14, PF-AR, KEK will be presented.

  3. Polarized synchrotron emission in quiescent black hole X-ray transients

    NASA Astrophysics Data System (ADS)

    Russell, David M.; Shahbaz, Tariq; Lewis, Fraser; Gallo, Elena

    2016-08-01

    We present near-infrared polarimetric observations of the black hole X-ray binaries Swift J1357.2-0933 and A0620-00. In both sources, recent studies have demonstrated the presence of variable infrared synchrotron emission in quiescence, most likely from weak compact jets. For Swift J1357.2-0933 we find that the synchrotron emission is polarized at a level of 8.0 ± 2.5 per cent (a 3.2 σ detection of intrinsic polarization). The mean magnitude and rms variability of the flux (fractional rms of 19-24 per cent in KS-band) agree with previous observations. These properties imply a continuously launched (stable on long timescales), highly variable (on short timescales) jet in the Swift J1357.2-0933 system in quiescence, which has a moderately tangled magnetic field close to the base of the jet. We find that for A0620-00, there are likely to be three components to the optical-infrared polarization; interstellar dust along the line of sight, scattering within the system, and an additional source that changes the polarization position angle in the reddest (H and KS) wave-bands. We interpret this as a stronger contribution of synchrotron emission, and by subtracting the line-of-sight polarization, we measure an excess of ˜1.25 ± 0.28 per cent polarization and a position angle of the magnetic field vector that is consistent with being parallel with the axis of the resolved radio jet. These results imply that weak jets in low luminosity accreting systems have magnetic fields which possess similarly tangled fields compared to the more luminous, hard state jets in X-ray binaries.

  4. Relativistic klystron driven compact high gradient accelerator as an injector to an X-ray synchrotron radiation ring

    DOEpatents

    Yu, David U. L.

    1990-01-01

    A compact high gradient accelerator driven by a relativistic klystron is utilized to inject high energy electrons into an X-ray synchrotron radiation ring. The high gradients provided by the relativistic klystron enables accelerator structure to be much shorter (typically 3 meters) than conventional injectors. This in turn enables manufacturers which utilize high energy, high intensity X-rays to produce various devices, such as computer chips, to do so on a cost effective basis.

  5. Scatter of X-rays on polished surfaces

    NASA Technical Reports Server (NTRS)

    Hasinger, G.

    1981-01-01

    In investigating the dispersion properties of telescope mirrors used in X-ray astronomy, the slight scattering characteristics of X-ray radiation by statistically rough surfaces were examined. The mathematics and geometry of scattering theory are described. The measurement test assembly is described and results of measurements on samples of plane mirrors are given. Measurement results are evaluated. The direct beam, the convolution of the direct beam and the scattering halo, curve fitting by the method of least squares, various autocorrelation functions, results of the fitting procedure for small scattering, and deviations in the kernel of the scattering distribution are presented. A procedure for quality testing of mirror systems through diagnosis of rough surfaces is described.

  6. The Application of Monochromatic Energies to Investigate Multiphase Porous Media Systems using Synchrotron X-ray Tomography

    SciTech Connect

    Ham, Kyungmin; Willson, Clinton S.

    2006-01-31

    X-ray computed tomography (CT) is becoming a useful tool for nondestructive imaging of many geoenvironmental and geotechnical systems. Conventional X-ray CT systems typically utilize a polychromatic X-ray beam. While providing a high throughput of photons, the use of polychromatic energy can make quantifying material concentrations, densities or composition very difficult or impossible without appropriate standards. Synchrotron X-rays have an extremely small angular divergence, thus permitting spatial resolution that is only limited by the optical components of the system. In addition, the ability to tune to a monochromatic X-ray energy allows better phase contrast by reducing beam hardening and allowing for elemental discrimination. In this work we will show how monochromatic energy can be used to provide high-quality images allowing for phase separation several different porous media systems thus improving our ability to quantify a range of processes and phenomena.

  7. Phase transitions in freeze-dried systems - quantification using in situ synchrotron X-ray diffractometry

    SciTech Connect

    Varshney, Dushyant B.; Sundaramurthi, Prakash; Kumar, Satyendra; Shalaev, Evgenyi Y.; Kang, Shin-Woong; Gatlin, Larry A.; Suryanarayanan, Raj

    2009-09-02

    The purpose is: (1) To develop a synchrotron X-ray diffraction (SXRD) method to monitor phase transitions during the entire freeze-drying cycle. Aqueous sodium phosphate buffered glycine solutions with initial glycine to buffer molar ratios of 1:3 (17:50 mM), 1:1 (50 mM) and 3:1 were utilized as model systems. (2) To investigate the effect of initial solute concentration on the crystallization of glycine and phosphate buffer salt during lyophilization. Phosphate buffered glycine solutions were placed in a custom-designed sample cell for freeze-drying. The sample cell, covered with a stainless steel dome with a beryllium window, was placed on a stage capable of controlled cooling and vacuum drying. The samples were cooled to -50 C and annealed at -20 C. They underwent primary drying at -25 C under vacuum until ice sublimation was complete and secondary drying from 0 to 25 C. At different stages of the freeze-drying cycle, the samples were periodically exposed to synchrotron X-ray radiation. An image plate detector was used to obtain time-resolved two-dimensional SXRD patterns. The ice, {beta}-glycine and DHPD phases were identified based on their unique X-ray peaks. When the solutions were cooled and annealed, ice formation was followed by crystallization of disodium hydrogen phosphate dodecahydrate (DHPD). In the primary drying stage, a significant increase in DHPD crystallization followed by incomplete dehydration to amorphous disodium hydrogen phosphate was evident. Complete dehydration of DHPD occurred during secondary drying. Glycine crystallization was inhibited throughout freeze-drying when the initial buffer concentration (1:3 glycine to buffer) was higher than that of glycine. A high-intensity X-ray diffraction method was developed to monitor the phase transitions during the entire freeze-drying cycle. The high sensitivity of SXRD allowed us to monitor all the crystalline phases simultaneously. While DHPD crystallizes in frozen solution, it dehydrates

  8. Synchrotron X-ray microfluorescence measurement of metal distributions in Phragmites australis root system in the Yangtze River intertidal zone.

    PubMed

    Feng, Huan; Zhang, Weiguo; Qian, Yu; Liu, Wenliang; Yu, Lizhong; Yoo, Shinjae; Wang, Jun; Wang, Jia Jun; Eng, Christopher; Liu, Chang Jun; Tappero, Ryan

    2016-07-01

    This study investigates the distributions of Br, Ca, Cl, Cr, Cu, K, Fe, Mn, Pb, Ti, V and Zn in Phragmites australis root system and the function of Fe nanoparticles in scavenging metals in the root epidermis using synchrotron X-ray microfluorescence, synchrotron transmission X-ray microscope measurement and synchrotron X-ray absorption near-edge structure techniques. The purpose of this study is to understand the mobility of metals in wetland plant root systems after their uptake from rhizosphere soils. Phragmites australis samples were collected in the Yangtze River intertidal zone in July 2013. The results indicate that Fe nanoparticles are present in the root epidermis and that other metals correlate significantly with Fe, suggesting that Fe nanoparticles play an important role in metal scavenging in the epidermis. PMID:27359142

  9. Macromolecular structures probed by combining single-shot free-electron laser diffraction with synchrotron coherent X-ray imaging.

    PubMed

    Gallagher-Jones, Marcus; Bessho, Yoshitaka; Kim, Sunam; Park, Jaehyun; Kim, Sangsoo; Nam, Daewoong; Kim, Chan; Kim, Yoonhee; Noh, Do Young; Miyashita, Osamu; Tama, Florence; Joti, Yasumasa; Kameshima, Takashi; Hatsui, Takaki; Tono, Kensuke; Kohmura, Yoshiki; Yabashi, Makina; Hasnain, S Samar; Ishikawa, Tetsuya; Song, Changyong

    2014-01-01

    Nanostructures formed from biological macromolecular complexes utilizing the self-assembly properties of smaller building blocks such as DNA and RNA hold promise for many applications, including sensing and drug delivery. New tools are required for their structural characterization. Intense, femtosecond X-ray pulses from X-ray free-electron lasers enable single-shot imaging allowing for instantaneous views of nanostructures at ambient temperatures. When combined judiciously with synchrotron X-rays of a complimentary nature, suitable for observing steady-state features, it is possible to perform ab initio structural investigation. Here we demonstrate a successful combination of femtosecond X-ray single-shot diffraction with an X-ray free-electron laser and coherent diffraction imaging with synchrotron X-rays to provide an insight into the nanostructure formation of a biological macromolecular complex: RNA interference microsponges. This newly introduced multimodal analysis with coherent X-rays can be applied to unveil nano-scale structural motifs from functional nanomaterials or biological nanocomplexes, without requiring a priori knowledge. PMID:24786694

  10. Devices Materials and Processes for Nanoelectronics: Characterization with Advanced X-Ray Techniques Using Lab-Based and Synchrotron Radiation Sources

    SciTech Connect

    E Zschech; C Wyon; C Murray; G Schneider

    2011-12-31

    Future nanoelectronics manufacturing at extraordinary length scales, new device structures, and advanced materials will provide challenges to process development and engineering but also to process control and physical failure analysis. Advanced X-ray techniques, using lab systems and synchrotron radiation sources, will play a key role for the characterization of thin films, nanostructures, surfaces, and interfaces. The development of advanced X-ray techniques and tools will reduce risk and time for the introduction of new technologies. Eventually, time-to-market for new products will be reduced by the timely implementation of the best techniques for process development and process control. The development and use of advanced methods at synchrotron radiation sources will be increasingly important, particularly for research and development in the field of advanced processes and new materials but also for the development of new X-ray components and procedures. The application of advanced X-ray techniques, in-line, in out-of-fab analytical labs and at synchrotron radiation sources, for research, development, and manufacturing in the nanoelectronics industry is reviewed. The focus of this paper is on the study of nanoscale device and on-chip interconnect materials, and materials for 3D IC integration as well.

  11. High resolution three-dimensional visualization and characterization of coronary atherosclerosis in vitro by synchrotron radiation x-ray microtomography and highly localized x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Jin, Hua; Ham, Kyungmin; Chan, Julia Y.; Butler, Leslie G.; Kurtz, Richard L.; Thiam, Serigne; Robinson, James W.; Agbaria, Rezik A.; Warner, Isiah M.; Tracy, Richard E.

    2002-12-01

    Human atherosclerotic plaques in both native and bypass arteries have been visualized using microtomography to provide additional information on the nature of coronary artery disease. Plaques contained within arteries removed from three white males aged 51, 55 and 70 are imaged in three-dimensions with monochromatic synchrotron x-ray radiation. Fields of view are 658 × 658 × 517 voxels, with cubic voxels ranging from 12 to 13 µm on a side. X-ray energies range from 11 to 15 keV (bandpass approximately 10 eV). At lower energies, high local absorption tends to generate reconstruction artefacts, while at higher energies the arterial wall is scarcely visible. At all energies, calcifications are clearly visible and differences are observed between plaques in native arteries (lifetime accumulations) versus bypass arteries (plaques developing in the interval between the heart bypass operation and the autopsy). In order to characterize coronary calcification, a micro-focused, 50 µm2, 25 keV x-ray beam was used to acquire powder diffraction data from selected calcifications. Also, large calcifications were removed from the native arteries and imaged with 25 keV x-ray energy. Calcifications are composed of hydroxyapatite crystallites and an amorphous phase. In summary, native calcifications are larger and have a higher fraction of hydroxyapatite than calcifications from the bypass arteries.

  12. Extracting material parameters from x-ray attenuation: a CT feasibility study using kilovoltage synchrotron x-rays incident upon low atomic number absorbers.

    PubMed

    Kirby, B J; Davis, J R; Grant, J A; Morgan, M J

    2003-10-21

    The work reported here is a feasibility study of the extraction of material parameters from measurements of the linear x-ray attenuation coefficient of low atomic number absorbers. Computed tomography (CT) scans of small samples containing several liquids and solids were carried out with synchrotron radiation at the Australian National Beamline Facility (BL 20B) in Japan. Average values of the x-ray linear attenuation coefficient were extracted for each material for x-ray energies ranging from 11 keV to 20.5 keV. The electron density was estimated by applying results derived from a parametrization of the x-ray linear attenuation coefficient first developed by Jackson and Hawkes and extended for this work. Average estimates for the electron density of triethanolamine and acetic acid were made to within +5.3% of the actual value. Other materials examined included furfuraldehyde, perspex and teflon, for which average estimates of the electron density were less than 10% in excess of the calculated value. PMID:14620065

  13. Extracting material parameters from x-ray attenuation: a CT feasibility study using kilovoltage synchrotron x-rays incident upon low atomic number absorbers

    NASA Astrophysics Data System (ADS)

    Kirby, B. J.; Davis, J. R.; Grant, J. A.; Morgan, M. J.

    2003-10-01

    The work reported here is a feasibility study of the extraction of material parameters from measurements of the linear x-ray attenuation coefficient of low atomic number absorbers. Computed tomography (CT) scans of small samples containing several liquids and solids were carried out with synchrotron radiation at the Australian National Beamline Facility (BL 20B) in Japan. Average values of the x-ray linear attenuation coefficient were extracted for each material for x-ray energies ranging from 11 keV to 20.5 keV. The electron density was estimated by applying results derived from a parametrization of the x-ray linear attenuation coefficient first developed by Jackson and Hawkes and extended for this work. Average estimates for the electron density of triethanolamine and acetic acid were made to within +5.3% of the actual value. Other materials examined included furfuraldehyde, perspex and teflon, for which average estimates of the electron density were less than 10% in excess of the calculated value.

  14. Coupled U-Pb isotopic studies and synchrotron x-ray microbeam analysis of geologic systems

    NASA Astrophysics Data System (ADS)

    Lanzirotti, A.; Sutton, S.; Rasbury, T.; Becker, M.; Hanson, G. N.

    2001-12-01

    Analytical advances in thermal ionization mass spectrometry now allow for precise measurement of U and Pb abundance and Pb isotopic composition in minerals where U and Pb may only amount to a few picograms by weight. High precision analysis at such low levels means that a much wider variety of mineral species can be considered as potentially useful U-Pb geochronometers. However, evaluating the potential use of these minerals for high-precision dating requires understanding the environmental and crystal chemistry of the U and Pb being analyzed in these minerals. Advances in the production of microfocused synchrotron x-ray beams allow more unambiguous evaluation of uranium partitioning and speciation in these geochemical systems. The microbeam capabilities of these instruments, such as the X26A beamline at the NSLS, allow for near simultaneous evaluation of major and trace elements using synchrotron XRF, elemental speciation and coordination using x-ray absorption spectroscopy (XANES and EXAFS), and mineralogy using micro-XRD at resolutions of 10 microns or less. Additionally, the synchrotron hard x-ray microprobe allows for non-destructive analysis of the same hand specimens or thin sections from which samples are separated for isotopic analysis with a detection sensitivity often of 1 ppm or better. Some examples illustrate how these combined studies can help characterize the U and Pb geochemistry of the host environments in which these minerals formed. Andradite garnets from the Grand Canyon Supergroup (1178+/-26 Ma) are shown to be compositionally homogeneous in U abundance (10-25 ppm), with U as a 4+ species. Fossilized Jurassic fish coprolites from the Shuttle Meadow Fm. (ca. 200 Ma) show that although they are dominated by apatite the highest U abundance is consistent with adsorption onto organic C at the time of sedimentation. Examples of U analyzed from a number of terrestrial carbonates shows that U can be incorporated as both 4+ and 6+ species and may also

  15. Unraveling wetting transition through surface textures with X-rays: Liquid meniscus penetration phenomena

    PubMed Central

    Antonini, C.; Lee, J. B.; Maitra, T.; Irvine, S.; Derome, D.; Tiwari, Manish K.; Carmeliet, J.; Poulikakos, D.

    2014-01-01

    In this report we show that synchrotron X-ray radiography is a powerful method to study liquid-air interface penetration through opaque microtextured surface roughness, leading to wetting transition. We investigate this wetting phenomenon in the context of sessile drop evaporation, and establish that liquid interface sinking into the surface texture is indeed dictated by the balance of capillary and Laplace pressures, where the intrinsically three-dimensional nature of the meniscus must be accounted for. Air bubble entrapment in the texture underneath impacting water drops is also visualized and the mechanisms of post-impact drop evaporation are discussed. PMID:24514762

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

    NASA Astrophysics Data System (ADS)

    Newby, David, Jr.

    surface evolution of these films is discussed, and the effects of different gas environments on oxygen vacancy concentration are elucidated. LSMO is commonly used in commercial fuel cell devices. Here the resonant soft x-ray emission (RIXS) spectrum of LSMO is examined, and it is shown that the inelastic x-ray emission structure of LSMO arises from local atomic multiplet effects.

  17. BioCARS: a synchrotron resource for time-resolved X-ray science

    PubMed Central

    Graber, T.; Anderson, S.; Brewer, H.; Chen, Y.-S.; Cho, H. S.; Dashdorj, N.; Henning, R. W.; Kosheleva, I.; Macha, G.; Meron, M.; Pahl, R.; Ren, Z.; Ruan, S.; Schotte, F.; Šrajer, V.; Viccaro, P. J.; Westferro, F.; Anfinrud, P.; Moffat, K.

    2011-01-01

    BioCARS, a NIH-supported national user facility for macromolecular time-resolved X-ray crystallography at the Advanced Photon Source (APS), has recently completed commissioning of an upgraded undulator-based beamline optimized for single-shot laser-pump X-ray-probe measurements with time resolution as short as 100 ps. The source consists of two in-line undulators with periods of 23 and 27 mm that together provide high-flux pink-beam capability at 12 keV as well as first-harmonic coverage from 6.8 to 19 keV. A high-heat-load chopper reduces the average power load on downstream components, thereby preserving the surface figure of a Kirkpatrick–Baez mirror system capable of focusing the X-ray beam to a spot size of 90 µm horizontal by 20 µm vertical. A high-speed chopper isolates single X-ray pulses at 1 kHz in both hybrid and 24-bunch modes of the APS storage ring. In hybrid mode each isolated X-ray pulse delivers up to ∼4 × 1010 photons to the sample, thereby achieving a time-averaged flux approaching that of fourth-generation X-FEL sources. A new high-power picosecond laser system delivers pulses tunable over the wavelength range 450–2000 nm. These pulses are synchronized to the storage-ring RF clock with long-term stability better than 10 ps RMS. Monochromatic experimental capability with Biosafety Level 3 certification has been retained. PMID:21685684

  18. BioCARS: a synchrotron resource for time-resolved X-ray science

    SciTech Connect

    Graber, T.; Anderson, S.; Brewer, H.; Chen, Y.-S.; Cho, H.; Dashdorj, N.; Henning, R.W.; Kosheleva, I.; Macha, G.; Meron, M.; Pahl, R.; Ren, Z.; Ruan, S.; Schotte, F.; Srajer, V.; Viccaro, P.J.; Westferro, F.; Anfinrud, P.; Moffat, K.

    2011-08-16

    BioCARS, a NIH-supported national user facility for macromolecular time-resolved X-ray crystallography at the Advanced Photon Source (APS), has recently completed commissioning of an upgraded undulator-based beamline optimized for single-shot laser-pump X-ray-probe measurements with time resolution as short as 100 ps. The source consists of two in-line undulators with periods of 23 and 27 mm that together provide high-flux pink-beam capability at 12 keV as well as first-harmonic coverage from 6.8 to 19 keV. A high-heat-load chopper reduces the average power load on downstream components, thereby preserving the surface figure of a Kirkpatrick-Baez mirror system capable of focusing the X-ray beam to a spot size of 90 {micro}m horizontal by 20 {micro}m vertical. A high-speed chopper isolates single X-ray pulses at 1 kHz in both hybrid and 24-bunch modes of the APS storage ring. In hybrid mode each isolated X-ray pulse delivers up to {approx}4 x 10{sup 10} photons to the sample, thereby achieving a time-averaged flux approaching that of fourth-generation X-FEL sources. A new high-power picosecond laser system delivers pulses tunable over the wavelength range 450-2000 nm. These pulses are synchronized to the storage-ring RF clock with long-term stability better than 10 ps RMS. Monochromatic experimental capability with Biosafety Level 3 certification has been retained.

  19. BioCARS: a synchrotron resource for time-resolved X-ray science.

    PubMed

    Graber, T; Anderson, S; Brewer, H; Chen, Y S; Cho, H S; Dashdorj, N; Henning, R W; Kosheleva, I; Macha, G; Meron, M; Pahl, R; Ren, Z; Ruan, S; Schotte, F; Srajer, V; Viccaro, P J; Westferro, F; Anfinrud, P; Moffat, K

    2011-07-01

    BioCARS, a NIH-supported national user facility for macromolecular time-resolved X-ray crystallography at the Advanced Photon Source (APS), has recently completed commissioning of an upgraded undulator-based beamline optimized for single-shot laser-pump X-ray-probe measurements with time resolution as short as 100 ps. The source consists of two in-line undulators with periods of 23 and 27 mm that together provide high-flux pink-beam capability at 12 keV as well as first-harmonic coverage from 6.8 to 19 keV. A high-heat-load chopper reduces the average power load on downstream components, thereby preserving the surface figure of a Kirkpatrick-Baez mirror system capable of focusing the X-ray beam to a spot size of 90 µm horizontal by 20 µm vertical. A high-speed chopper isolates single X-ray pulses at 1 kHz in both hybrid and 24-bunch modes of the APS storage ring. In hybrid mode each isolated X-ray pulse delivers up to ~4 × 10(10) photons to the sample, thereby achieving a time-averaged flux approaching that of fourth-generation X-FEL sources. A new high-power picosecond laser system delivers pulses tunable over the wavelength range 450-2000 nm. These pulses are synchronized to the storage-ring RF clock with long-term stability better than 10 ps RMS. Monochromatic experimental capability with Biosafety Level 3 certification has been retained. PMID:21685684

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

    NASA Astrophysics Data System (ADS)

    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

  1. Surface x-ray diffraction of complex metal oxide surfaces and interfaces--a new era

    SciTech Connect

    Schlepuetz, C. M.; Willmott, P. R.; Pauli, S. A.; Herger, R.; Martoccia, D.; Bjoerck, M.; Kumah, D.; Clarke, R.; Yacoby, Y.

    2009-01-29

    The availability of high-brilliance hard x-ray synchrotron radiation and the advent of novel photon counting area detectors have brought surface x-ray diffraction (SXRD) into a new era. It is now possible to record large numbers of structure factors with much improved reliability within reasonable beamtime durations. As a result, structural determination of the surfaces and interfaces of complex crystallographic systems and heterostructures has now become feasible, especially in conjunction with phase-retrieval methods. It is thereby hoped that detailed structural information will shed light on the unusual physical properties of these systems. Complex metal oxide systems investigated at the Materials Science beamline of the Swiss Light Source, including the surface of SrTiO{sub 3}, the interface between LaAlO{sub 3} and SrTiO{sub 3}, and the structure of YBa{sub 2}Cu{sub 3}O{sub 7} grown on NdGaO{sub 3}, SrTiO{sub 3}, and (LaSr)(AlTa)O{sub 3} will be presented as examples of what is now possible using SXRD.

  2. MOSFET dosimetry with high spatial resolution in intense synchrotron-generated x-ray microbeams

    SciTech Connect

    Siegbahn, E. A.; Braeuer-Krisch, E.; Bravin, A.; Nettelbeck, H.; Lerch, M. L. F.; Rosenfeld, A. B.

    2009-04-15

    Various dosimeters have been tested for assessing absorbed doses with microscopic spatial resolution in targets irradiated by high-flux, synchrotron-generated, low-energy ({approx}30-300 keV) x-ray microbeams. A MOSFET detector has been used for this study since its radio sensitive element, which is extraordinarily narrow ({approx}1 {mu}m), suits the main applications of interest, microbeam radiation biology and microbeam radiation therapy (MRT). In MRT, micrometer-wide, centimeter-high, and vertically oriented swaths of tissue are irradiated by arrays of rectangular x-ray microbeams produced by a multislit collimator (MSC). We used MOSFETs to measure the dose distribution, produced by arrays of x-ray microbeams shaped by two different MSCs, in a tissue-equivalent phantom. Doses were measured near the center of the arrays and maximum/minimum (peak/valley) dose ratios (PVDRs) were calculated to determine how variations in heights and in widths of the microbeams influenced this for the therapy, potentially important parameter. Monte Carlo (MC) simulations of the absorbed dose distribution in the phantom were also performed. The results show that when the heights of the irradiated swaths were below those applicable to clinical therapy (<1 mm) the MC simulations produce estimates of PVDRs that are up to a factor of 3 higher than the measured values. For arrays of higher microbeams (i.e., 25 {mu}mx1 cm instead of 25x500 {mu}m{sup 2}), this difference between measured and simulated PVDRs becomes less than 50%. Closer agreement was observed between the measured and simulated PVDRs for the Tecomet MSC (current collimator design) than for the Archer MSC. Sources of discrepancies between measured and simulated doses are discussed, of which the energy dependent response of the MOSFET was shown to be among the most important.

  3. Comparison between x-ray tube-based and synchrotron radiation-based μCT

    NASA Astrophysics Data System (ADS)

    Brunke, Oliver; Brockdorf, Kathleen; Drews, Susanne; Müller, Bert; Donath, Tilman; Herzen, Julia; Beckmann, Felix

    2008-08-01

    Nowadays, X-ray tube-based high-resolution CT systems are widely used in scientific research and industrial applications. But the potential, convenience and economy of these lab systems is often underestimated. The present paper shows the comparison of sophisticated conventional μCT with synchrotron radiation-based μCT (SRμCT). The different aspects and characteristics of both approaches like spatial and density resolution, penetration depth, scanning time or sample size is described in detail. The tube-based μCT measurements were performed with a granite-based nanotom®-CT system (phoenix|x-ray, Wunstorf, Germany) equipped with a 180 kV - 15 W high-power nanofocus® tube with tungsten or molybdenum targets. The tube offers a wide range of applications from scanning low absorbing samples in nanofocus® mode with voxel sizes below 500 nm and highly absorbing objects in the high power mode with focal spot and voxel sizes of a few microns. The SRμCT measurements were carried out with the absorption contrast set-up at the beamlines W 2 and BW 2 at HASYLAB/DESY, operated by the GKSS Research Center. The range of samples examined covers materials of very different absorption levels and related photon energies for the CT scans. Both quantitative and qualitative comparisons of CT scans using biomedical specimens with rather low X-ray absorption such as parts of the human spine as well as using composites from the field of materials science are shown.

  4. Protein folding and protein metallocluster studies using synchrotron small angler X-ray scattering

    SciTech Connect

    Eliezer, D.

    1994-06-01

    Proteins, biological macromolecules composed of amino-acid building blocks, possess unique three dimensional shapes or conformations which are intimately related to their biological function. All of the information necessary to determine this conformation is stored in a protein`s amino acid sequence. The problem of understanding the process by which nature maps protein amino-acid sequences to three-dimensional conformations is known as the protein folding problem, and is one of the central unsolved problems in biophysics today. The possible applications of a solution are broad, ranging from the elucidation of thousands of protein structures to the rational modification and design of protein-based drugs. The scattering of X-rays by matter has long been useful as a tool for the characterization of physical properties of materials, including biological samples. The high photon flux available at synchrotron X-ray sources allows for the measurement of scattering cross-sections of dilute and/or disordered samples. Such measurements do not yield the detailed geometrical information available from crystalline samples, but do allow for lower resolution studies of dynamical processes not observable in the crystalline state. The main focus of the work described here has been the study of the protein folding process using time-resolved small-angle x-ray scattering measurements. The original intention was to observe the decrease in overall size which must accompany the folding of a protein from an extended conformation to its compact native state. Although this process proved too fast for the current time-resolution of the technique, upper bounds were set on the probable compaction times of several small proteins. In addition, an interesting and unexpected process was detected, in which the folding protein passes through an intermediate state which shows a tendency to associate. This state is proposed to be a kinetic molten globule folding intermediate.

  5. MOSFET dosimetry with high spatial resolution in intense synchrotron-generated x-ray microbeams.

    PubMed

    Siegbahn, E A; Bräuer-Krisch, E; Bravin, A; Nettelbeck, H; Lerch, M L F; Rosenfeld, A B

    2009-04-01

    Various dosimeters have been tested for assessing absorbed doses with microscopic spatial resolution in targets irradiated by high-flux, synchrotron-generated, low-energy (approximately 30-300 keV) x-ray microbeams. A MOSFET detector has been used for this study since its radio sensitive element, which is extraordinarily narrow (approximately 1 microm), suits the main applications of interest, microbeam radiation biology and microbeam radiation therapy (MRT). In MRT, micrometer-wide, centimeter-high, and vertically oriented swaths of tissue are irradiated by arrays of rectangular x-ray microbeams produced by a multislit collimator (MSC). We used MOSFETs to measure the dose distribution, produced by arrays of x-ray microbeams shaped by two different MSCs, in a tissue-equivalent phantom. Doses were measured near the center of the arrays and maximum/minimum (peak/valley) dose ratios (PVDRs) were calculated to determine how variations in heights and in widths of the microbeams influenced this for the therapy, potentially important parameter. Monte Carlo (MC) simulations of the absorbed dose distribution in the phantom were also performed. The results show that when the heights of the irradiated swaths were below those applicable to clinical therapy (< 1 mm) the MC simulations produce estimates of PVDRs that are up to a factor of 3 higher than the measured values. For arrays of higher microbeams (i.e., 25 microm x 1 cm instead of 25 x 500 microm2), this difference between measured and simulated PVDRs becomes less than 50%. Closer agreement was observed between the measured and simulated PVDRs for the Tecomet MSC (current collimator design) than for the Archer MSC. Sources of discrepancies between measured and simulated doses are discussed, of which the energy dependent response of the MOSFET was shown to be among the most important. PMID:19472618

  6. Design and fabrication of soft x-ray photolithography experimental beam line at Beijing National Synchrotron Radiation Laboratory

    NASA Astrophysics Data System (ADS)

    Zhou, Changxin

    1991-08-01

    The synchrotron radiation (SR) soft x-ray photolithography experimental beam line (3B1 beam line) at Beijing National Synchrotron Radiation Laboratory, was completed and tested in June 1990. A soft x-ray photolithography experiment was successfully completed, and the width of linear etch on a silicon chip by the device with a 3B1 beam line is up to 0.5 micrometers . This SR soft x-ray photolithography experiment was done successfully for the first time in China. This paper describes the design of the beam line and the fabrication of the most important optical element--the cylindrical scanning mirror in the beam line. The 3B1 beam line consists of the shielding light plate with water-cooling, laser simulation light source system, 3-D adjustable scanning mirror, high pass-band filer (beryllium window), acoustic sensor, helium gas chamber, and vacuum system. The main specifications of the 3B1 beam line are as follows: spectral range 0.4-2 nm; horizontal acceptance angle 7.5 mrad; vertical acceptance angle 0.4 mrad; grazing incidence angle 1.5 deg; light spot size 35 nm X 12 nm; vacuum degree of the mirror box 5 X 10-10 torr (static). The cylindrical scanning mirror in grazing incidence is used in the beam line for photolithography to obtain uniform distributed intensity of illumination of the SR source in the vertical direction (Gaussian distribution) and sufficiently concentrated energy. It is made of aluminum alloy LD2 with a supersmooth optical surface. The curvature radius of the cylindrical surface is 527.5 mm; surface figure error is less than (lambda) /10; surface roughness is better than 1 nm RMS, and fold coating on the surface of the mirror under UHV of 109 torr. The laser simulation light source system is used for adjusting the optical system in the beam line instead of the SR source. The cylindrical mirror was polished supersmoothly using Al2O3 ultra micropower grinding material made in TOMAS in Japan on modified traditional machine tools, and surface

  7. Study of liquid gallium as a function of pressure and temperature using synchrotron x-ray microtomography and x-ray diffraction

    SciTech Connect

    Li, Renfeng; Li, Liangliang; Chen, Jiaxuan; Yu, Tony; Wang, Yanbin; Rivers, Mark L.; Wang, Luhong E-mail: haozhe@hit.edu.cn; Cai, Zhonghou; Chen, Jiuhua; Liu, Haozhe E-mail: haozhe@hit.edu.cn

    2014-07-28

    The volume change of liquid and solid gallium has been studied as a function of pressure and temperature up to 3.02 GPa at 300 K and up to 3.63 GPa at 330 K using synchrotron x-ray microtomography combined with energy dispersive x-ray diffraction techniques. Two sets of directly measured P-V data at 300 K and 330 K were obtained from 3D tomography reconstruction data, and the corresponding isothermal bulk moduli were determined as 23.6 (0.5) GPa and 24.6 (0.4) GPa, respectively. The existence of a liquid-liquid phase transition region is proposed based on the abnormal compressibility of Ga melt at about 2.44 GPa and 330 K conditions.

  8. Visualization of ultrasound induced cavitation bubbles using the synchrotron x-ray Analyzer Based Imaging technique

    NASA Astrophysics Data System (ADS)

    Izadifar, Zahra; Belev, George; Izadifar, Mohammad; Izadifar, Zohreh; Chapman, Dean

    2014-12-01

    Observing cavitation bubbles deep within tissue is very difficult. The development of a method for probing cavitation, irrespective of its location in tissues, would improve the efficiency and application of ultrasound in the clinic. A synchrotron x-ray imaging technique, which is capable of detecting cavitation bubbles induced in water by a sonochemistry system, is reported here; this could possibly be extended to the study of therapeutic ultrasound in tissues. The two different x-ray imaging techniques of Analyzer Based Imaging (ABI) and phase contrast imaging (PCI) were examined in order to detect ultrasound induced cavitation bubbles. Cavitation was not observed by PCI, however it was detectable with ABI. Acoustic cavitation was imaged at six different acoustic power levels and six different locations through the acoustic beam in water at a fixed power level. The results indicate the potential utility of this technique for cavitation studies in tissues, but it is time consuming. This may be improved by optimizing the imaging method.

  9. Application of small angle X-ray scattering synchrotron technology for measuring ovine meat quality.

    PubMed

    Hoban, J M; Hopkins, D L; Kirby, N; Collins, D; Dunshea, F R; Kerr, M G; Bailes, K; Cottrell, J J; Holman, B W B; Brown, W; Ponnampalam, E N

    2016-07-01

    A small angle X-ray scattering (SAXS) synchrotron was used to evaluate 100 ovine m. longissimus lumborum, representing lamb (n=50) and sheep (n=50). The diffraction of X-rays gives information on muscle myofibril structure and fat content. The linear relationships between SAXS measures with measures such as, shear force, intramuscular fat content (IMF) and collagen content/solubility, were investigated. A relationship was found between the d-spacing of the actin/myosin fibril spacing (SAX1 and SAX2) and the cross sectional area of the rhombohedral unit cell (Cell area) and shear force after 1 and 5day ageing. There was a positive relationship between IMF and a SAXS Fat area measure. There was a muscle site effect on SAX1, SAX2 and Cell area, with the cranial site having a larger distance between myofibrils. The potential of SAXS as a powerful research tool to determine not only the structural components of ovine tenderness, but also the fat content related to IMF is evident. PMID:26971308

  10. Synchronizing femtosecond laser with x-ray synchrotron operating at arbitrarily different frequencies.

    PubMed

    Jo, Wonhyuk; Lee, Sooheyong; Eom, Intae; Landahl, Eric C

    2014-12-01

    The ability to synchronize a femtosecond laser to x-ray pulses is crucial for performing ultrafast time-resolved x-ray scattering experiments at synchrotrons. Conventionally, the task has been achieved by locking a harmonic frequency of the laser oscillator to the storage ring master radio-frequency (RF). However, when the frequency mismatch between the two sources cannot be compensated by small adjustments to the laser cavity length, synchronization to a harmonic frequency requires modifying the optical components of the laser system. We demonstrate a novel synchronization scheme, which is a flexible alternative for synchronizing these two sources operating at arbitrarily different frequencies. First, we find the greatest common divisor (GCD) of the two frequencies that is still within the limited tuning range of the laser cavity length. The GCD is generated by dividing down from the storage ring RF, and is separately multiplied up to provide a feedback signal for synchronizing the laser cavity. Unique to our scheme, the GCD also serves as a harmonic RF source for the laser amplifier such that only laser oscillator pulses at fixed integer multiples of the storage ring RF are selected for amplification and delivery to experiments. Our method is implemented at the Photon Test Facility beamline of Pohang Light Source where timing-jitter less than 4 ps (r.m.s.) is measured using a new shot-to-shot method. PMID:25554331

  11. Optical and x-ray imaging of electron beams using synchrotron emission

    SciTech Connect

    Wilke, M.D.

    1994-12-01

    In the case of very low eniittance electron and positron storage ring beams, it is impossible to make intrusive measurements of beam properties without increasing the emittance and possibly disrupting the beam. In cases where electron or positron beams have high average power densities (such as free electron laser linacs), intrusive probes such as wires and optical transition radiation screens or Cherenkov emitting screens can be easily damaged or destroyed. The optical and x-ray emissions from the bends in the storage rings and often from linac bending magnets can be used to image the beam profile to obtain emittance information about the beam. The techniques, advantages and limitations of using both optical and x-ray synchrotron emission to measure beam properties are discussed and the possibility of single bunch imaging is considered. The properties of suitable imagers and converters such as phosphors are described. Examples of previous, existing and planned applications are given where available, including a pinhole imaging system currently being designed for the Advanced Photon Source at Argonne National Laboratory.

  12. Optical and x-ray imaging of electron beams using synchrotron emission

    SciTech Connect

    Wilke, M.

    1995-01-01

    In the case of very low emittance electron and positron storage ring beams, it is impossible to make intrusive measurements of beam properties without increasing the emittance and possibly disrupting the beam. In cases where electron or positron beams have high average power densities (such as free electron laser linacs), intrusive probes such as wires and optical transition radiation screens or Cherenkov emitting screens can be easily damaged or destroyed. The optical and x-ray emissions from the bends in the storage rings and often from linac bending magnets can be used to image the beam profile to obtain emittance information about the beam. The techniques, advantages and limitations of using both optical and x-ray synchrotron emission to measure beam properties are discussed and the possibility of single bunch imaging is considered. The properties of suitable imagers and converters such as phosphors are described. Examples of previous, existing and planned applications are given where available, including a pinhole imaging system currently being designed for the Advanced Photon Source at Argonne National Laboratory.

  13. Study of liquid gallium at high pressure using synchrotron x-ray

    SciTech Connect

    Yu, Tony; Guo Quanzhong; Parise, John; Chen Jiuhua; Ehm, Lars; Huang Shu; Luo Shengnian

    2012-06-01

    Liquid gallium has been studied at high pressure up to 2 GPa and ambient temperature in a diamond anvil cell using high energy synchrotron x-ray beam. The total x-ray scattering data of liquid gallium were collected up to Q = 12 A{sup -1} and analyzed using pair distribution functions (PDF). The results indicate that the first nearest neighbor peak and second nearest neighbor (shoulder) peak of PDF in liquid gallium does not change with pressure, whereas the higher order (i.e., third and fourth) nearest neighbor peaks shift towards shorter distance with increasing pressure. Reverse Monte Carlo modeling based on the observed data shows that the coordination number in the liquid gallium increases with pressure from 10.5 at 0.3 GPa to 11.6 at 2 GPa. An atomic arrangement similar to the crystalline phase of Ga(II) with coordination number of 12 is proposed for the locally dense-packed rigid unit in liquid gallium. The volume compression data derived from the structure modeling yield a bulk modulus of 12.1(6) GPa for liquid gallium.

  14. Synchrotron-based X-ray fluorescence imaging and elemental mapping from biological samples

    SciTech Connect

    D Rao; M Swapna; R Cesareo; A Brunetti; T Akatsuka; T Yuasa; T Takeda; G Gigante

    2011-12-31

    The present study utilized the new hard X-ray microspectroscopy beamline facility, X27A, available at NSLS, BNL, USA, for elemental mapping. This facility provided the primary beam in a small spot of the order of {approx}10 {mu}m, for focussing. With this spatial resolution and high flux throughput, the synchrotron-based X-ray fluorescent intensities for Mn, Fe, Zn, Cr, Ti and Cu were measured using a liquid-nitrogen-cooled 13-element energy-dispersive high-purity germanium detector. The sample is scanned in a 'step-and-repeat' mode for fast elemental mapping measurements and generated elemental maps at 8, 10 and 12 keV, from a small animal shell (snail). The accumulated trace elements, from these biological samples, in small areas have been identified. Analysis of the small areas will be better suited to establish the physiology of metals in specific structures like small animal shell and the distribution of other elements.

  15. Synchrotron X-ray Scattering Studies of Poly(lactide) Electrospun Fibers Containing Carbon Nanotubes

    NASA Astrophysics Data System (ADS)

    Zhu, Yazhe; Cebe, Peggy

    2014-03-01

    Carbon nanotubes(CNTs) often serve as an effective nucleating agent that facilitates the crystallization of semicrystalline polymers. Here we study the influence of CNTs on thermal and structural properties of Poly-lactide (PLA), which is well-known as a biodegradable and biocompatible thermoplastic polymer. The effect of CNTs on the crystallization and melting behavior of electrospun fibers of poly (L-lactide) (PLLA, with 100% L-isomer) and poly (D-lactide) (PDLA, containing 4% D-isomer) was systemically studied by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), Fourier transform spectroscopy(FT-IR) and real time synchrotron wide-angle X-ray scattering (WAXS) . Multi-walled CNTs were co-electrospun with the poly(lactides) in weight ratios ranging from 0.1 to 4.0 wt% MW-CNT. PLA/carbon nanotubes composite electrospun fibers were successfully produced by appropriate choice of processing conditions and solution concentration. The morphologies of neat and CNT-filled electrospun nanofibers were observed by scanning electron microscopy. WAXS and DSC results show that lower content of CNTs contributes to higher speed of crystallization. However the results also showed that at the highest concentration of CNTs the ultimate crystallinity was reduced. FTIR and X-ray results show that PLA fibers have different crystal forms at high and low crystallization temperature. DSC results also show that D-lactide has reduced crystallinity compared to L-lactide.

  16. Synchrotron X-Ray Microdiffraction Studies of Electromigration in Interconnect lines at the Advanced Light Source

    SciTech Connect

    Tamura, Nobumichi; Chen, Kai; Kunz, Martin

    2009-05-01

    Synchrotron polychromatic X-ray microdiffraction is a particularly suitable technique to study in situ the effect of electromigration in metal interconnects as add spatial resolution to grain orientation and strain sensitivity. This technique has been extensively used at the Advanced Light Source to monitor changes in aluminum and copper interconnect test structures while high-density current is passed into them during accelerated tests at elevated temperature. One of the principal findings is the observation of electromigration-induced plasticity in the metal lines that appear during the very early stages of electromigration. In some of the lines, high density of geometrically necessary dislocation are formed leading to additional diffusion paths causing an enhancement of electromigration effect at test temperature. This paper presents an overview of the principal results obtained from X-ray microdiffraction studies of electromigration effects on aluminum and copper interconnects at the ALS throughout continuous efforts that spanned over a decade (1998-2008) from approximately 40 weeks of combined beamtime.

  17. Synchronizing femtosecond laser with x-ray synchrotron operating at arbitrarily different frequencies

    SciTech Connect

    Jo, Wonhyuk; Lee, Sooheyong; Eom, Intae; Landahl, Eric C.

    2014-12-15

    The ability to synchronize a femtosecond laser to x-ray pulses is crucial for performing ultrafast time-resolved x-ray scattering experiments at synchrotrons. Conventionally, the task has been achieved by locking a harmonic frequency of the laser oscillator to the storage ring master radio-frequency (RF). However, when the frequency mismatch between the two sources cannot be compensated by small adjustments to the laser cavity length, synchronization to a harmonic frequency requires modifying the optical components of the laser system. We demonstrate a novel synchronization scheme, which is a flexible alternative for synchronizing these two sources operating at arbitrarily different frequencies. First, we find the greatest common divisor (GCD) of the two frequencies that is still within the limited tuning range of the laser cavity length. The GCD is generated by dividing down from the storage ring RF, and is separately multiplied up to provide a feedback signal for synchronizing the laser cavity. Unique to our scheme, the GCD also serves as a harmonic RF source for the laser amplifier such that only laser oscillator pulses at fixed integer multiples of the storage ring RF are selected for amplification and delivery to experiments. Our method is implemented at the Photon Test Facility beamline of Pohang Light Source where timing-jitter less than 4 ps (r.m.s.) is measured using a new shot-to-shot method.

  18. Synchrotron X-ray Studies of Vulcanized Rubbers and Thermoplastic Elastomers

    SciTech Connect

    Toki,S.; Hsiao, B.; Kohjiya, S.; Tosaka, M.; Tosaka, A.; Tsou, A.; Datta, S.

    2006-01-01

    Synchrotron X-ray diffraction technique has revealed strain-induced crystallization and molecular orientation in vulcanized rubbers and thermoplastic elastomers (TPE) during deformation in real time. The stress-strain curves and wide angle X-ray diffraction (WAXD) patterns in vulcanized rubbers and TPE were measured simultaneously. In-situ WAXD patterns were taken not only at different strains during uniaxial deformation but also at different temperatures at a constant strain. Results lead to several new insights. (i) Strain-induced crystallization is a common phenomenon in vulcanized rubbers, except SBR (styrene-butadiene rubber), and in TPE (with crystalline hard segments). (ii) Strain-induced crystallization decreases the stress and increases the elongation in the strained rubber. (iii) The hybrid structure of chemical networks and strain-induced crystallites is responsible to the tensile strength and elongation at break for both systems. (iiii) Some original crystal fraction (hard segment domain) in TPE is destroyed. During deformation, strain-induced crystallization increases with strain. Upon retraction even to stress zero, the majority of oriented strain-induced crystallites remains in tack with preferred orientation.

  19. Study of gold nanoparticle synthesis by synchrotron x-ray diffraction and fluorescence

    NASA Astrophysics Data System (ADS)

    Yan, Zhongying; Wang, Xiao; Yu, Le; Moeendarbari, Sina; Hao, Yaowu; Cai, Zhonghou; Cheng, Xuemei

    Gold nanoparticles have a wide range of potential applications, including therapeutic agent delivery, catalysis, and electronics. Recently a new process of hollow nanoparticle synthesis was reported, the mechanism of which was hypothesized to involve electroless deposition around electrochemically evolved hydrogen bubbles. However, the growth mechanism still needs experimental evidence. We report investigation of this synthesis process using synchrotron x-ray diffraction and fluorescence measurements performed at beamline 2-ID-D of the Advanced Photon Source (APS). A series of gold nanoparticle samples with different synthesis time (50-1200 seconds) were deposited using a mixture electrolyte solution of Na3Au(SO3)2 and H4N2NiO6S2 on anodic aluminum oxide (AAO) membranes. The 2D mapping of fluorescence intensity and comparison of x-ray diffraction peaks of the samples have provided valuable information on the growth mechanism. Work at Bryn Mawr College and University of Texas at Arlington is supported by NSF Grants (1207085 and 1207377) and use of the APS at Argonne National Laboratory is supported by the U. S. Department of Energy under Contract No. DE-AC02-06CH11357.

  20. Zirconium hydride precipitation kinetics in Zircaloy-4 observed with synchrotron X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Blackmur, M. S.; Robson, J. D.; Preuss, M.; Zanellato, O.; Cernik, R. J.; Shi, S.-Q.; Ribeiro, F.; Andrieux, J.

    2015-09-01

    High-energy synchrotron X-ray diffraction was used to investigate the isothermal precipitation of δ-hydride platelets in Zircaloy-4 at a range of temperatures relevant to reactor conditions, during both normal operation and thermal transients. From an examination of the rate kinetics of the precipitation process, precipitation slows with increasing temperature above 200 °C, due to a reduction in the thermodynamic driving force. A model for nucleation rate as a function of temperature was developed, to interpret the precipitation rates seen experimentally. While the strain energy associated with the misfit between hydrides and the matrix makes a significant contribution to the energy barrier for nucleation, a larger contribution arises from the interfacial energy. Diffusion distance calculations show that hydrogen is highly mobile in the considered thermal range and on the scale of inter-hydride spacing and it is not expected to be significantly rate limiting on the precipitation process that takes place under reactor operating conditions.

  1. High precision thermal stress study on flip chips by synchrotron polychromatic x-ray microdiffraction

    SciTech Connect

    Chen, Kai; Tamura, Nobumichi; Tang, Wei; Kunz, Martin; Chou, Yi-Chia; Tu, King-Ning; Lai, Yi-Shao

    2010-01-01

    The bending and residual stress of flip chips caused by the mismatch of thermal expansion between the chip and the substrate have been measured by polychromatic microfocused synchrotron x-ray beam. Precise orientation information as a function of position on the chip was obtained from Laue diffraction patterns, so that the bending angle with respect to a reference position at the center of the chip can be calculated at each position. This in turn allows deducing the local curvature of the entire flip chip. Local stress distribution was then mapped by applying a modified Stoney's stress-strain equation to the measured curvature. Our study shows that thermal stress on the circuits and the solder joints in a flip chip strongly depend on temperature and the distance from the center of the chip, indicating that interconnects at the corner and edge of a flip chip are of reliability concerns.

  2. Synchrotron X-ray Diffraction Study of Neurofilament Networks Interaction under Osmotic Pressure

    NASA Astrophysics Data System (ADS)

    Beck, R.; Deek, J.; Jones, J. B.; Hesse, H.; Choi, M. C.; Safinya, C. R.

    2008-03-01

    Neurofilaments (NFs) are cytoskeletal proteins, which are found abundantly in nerve cell axons and impart mechanical stability and act as structural scaffolds for microtubules. The filaments assemble from 3 different subunit proteins to form a 10 nm diameter flexible polymers with radiating unstructured sidearms. At high protein concentration, the NFs form a nematic hydrogel network with a well-defined interfilament spacing as measured by synchrotron small angle x-ray scattering (SAXS) [1]. Here, NFs purified from bovine spinal cord are reassembled in vitro. Using analogous SAXS-osmotic pressure techniques [2] we study forces between NFs and directly probe the polyampholyte brush interactions between NF sidearms. We measure the interfilament spacing at different osmotic pressure, salt and sidearm concentrations. The study reveals the non-trivial electrostatic nature of the interfilament interaction within the NF hydrogel. [1] J. Jones, C.R. Safinya (submitted) [2] D. J. Needleman et al., PRL 93, 198104 (2004)

  3. Dynamic imaging of oil shale pyrolysis using synchrotron X-ray microtomography

    NASA Astrophysics Data System (ADS)

    Saif, Tarik; Lin, Qingyang; Singh, Kamaljit; Bijeljic, Branko; Blunt, Martin J.

    2016-07-01

    The structure and connectivity of the pore space during the pyrolysis of oil shales determines hydrocarbon flow behavior and ultimate recovery. We image the time evolution of the pore and microfracture networks during oil shale pyrolysis using synchrotron X-ray microtomography. Immature Green River (Mahogany Zone) shale samples were thermally matured under vacuum conditions at temperatures up to 500°C while being periodically imaged with a 2 µm voxel size. The structural transformation of both organic-rich and organic-lean layers within the shale was quantified. The images reveal a dramatic change in porosity accompanying pyrolysis between 390 and 400°C with the formation of micron-scale heterogeneous pores. With a further increase in temperature, the pores steadily expand resulting in connected microfracture networks that predominantly develop along the kerogen-rich laminations.

  4. Organic-modified and biological silica studied by synchrotron x-ray pair distribution function measurements

    NASA Astrophysics Data System (ADS)

    Dimasi, Elaine; Jeffryes, Clayton; Rorrer, Gregory; Belton, David; Perry, Carole

    2007-03-01

    Biomineralization is a process by which living organisms create composite organic/mineral tissues which have hierarchical structures on micron and submicron scales. Fine control over mineral phase and morphology make biomineralization an important inspiration for materials science. It is often not appreciated that even amorphous minerals such as silica can exhibit hierarchical structure and special properties. One difficulty is that the molecular structures of amorphous phases can be hard to elucidate. We are exploring the use of pair distribution function measurements from synchrotron x-ray scattering to study silica structures, comparing both synthetic organic-modifed silicas and germanium-containing biosilica from diatoms. The raw scattering patterns show clear differences. We will discuss how these data can be scrutinized to determine what differences may be created at the molecular level by different silicification processes.

  5. Local structure in diatom biosilica probed by synchrotron x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Dibiccari, Michael; Kwak, Seo-Young; Hind, Geoffrey; Dimasi, Elaine

    2006-03-01

    Diatoms are single-celled algae that form intricate outer shells, or frustrules, composed of biosilica. They have attracted attention in the context of nanotechnology, since the submicron architectures are genetically determined and thus potentially could be reproduced synthetically, by using organic additives that mimic the proteins responsible for controlling biological silicification. We have compared the local atomic structure of diatom biosilica to that of inorganic silica with synchrotron x-ray diffraction, analyzed as the Pair Distribution Function (PDF). Specimens of Thalassiosira weissflogii (Tw) were cleaned of organic matter using either hydrogen peroxide, commercial bleach, or sodium dodecyl sulfate treatments. Low resolution PDF measurements (qmax 13.6 å-1) were made of wet and dry Tw, pure silica microspheres, and diatomaceous earth containing 15% mineral impurities. All samples have similar PDFs, demonstrating that local structure in diatoms and synthetic silica are equivalent, and that the PDF method is insensitive to biological impurites.

  6. A dynamic synchrotron X-ray imaging study of effective temperature in a vibrated granular medium.

    PubMed

    Cao, Yixin; Zhang, Xiaodan; Kou, Binquan; Li, Xiangting; Xiao, Xianghui; Fezzaa, Kamel; Wang, Yujie

    2014-08-01

    We present a dynamic synchrotron X-ray imaging study of the effective temperature Teff in a vibrated granular medium. By tracking the directed motion and the fluctuation dynamics of the tracers inside, we obtained Teff of the system using the Einstein relationship. We found that as the system unjams with increasing vibration intensities Γ, the structural relaxation time τ increases substantially which can be fitted by an Arrhenius law using Teff. And the characteristic energy scale of structural relaxation yielded by the Arrhenius fitting is E = 0.20 ± 0.02pd(3), where p is the pressure and d is the background particle diameter, which is consistent with those from hard sphere simulations in which the structural relaxation happens via the opening up of free volume against pressure. PMID:24930865

  7. Anomalous high-pressure behavior of amorphous selenium from synchrotron x-ray diffraction and microtomography

    PubMed Central

    Liu, Haozhe; Wang, Luhong; Xiao, Xianghui; De Carlo, Francesco; Feng, Ji; Mao, Ho-kwang; Hemley, Russell J.

    2008-01-01

    The high-pressure behavior of amorphous selenium has been investigated with time-resolved diamond anvil cell synchrotron x-ray diffraction and computed microtomography techniques. A two-step dynamic crystallization process is observed in which the monoclinic phase crystallized from the amorphous selenium and gradually converted to the trigonal phase, thereby explaining previously observed anomalous changes in electrical conductivity of the material under pressure. The crystallization of this elemental system involves local topological fluctuations and results in an unusual pressure-induced volume expansion. The metastability of the phases involved in the transition accounts for this phenomenon. The results demonstrate the use of pressure to control and directly monitor the relative densities and energetics of phases to create new phases from highly metastable states. The microtomographic technique developed here represents a method for determination of the equations of state of amorphous materials at extreme pressures and temperatures. PMID:18768800

  8. Hydride precipitation kinetics in Zircaloy-4 studied using synchrotron X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Courty, Olivier F.; Motta, Arthur T.; Piotrowski, Christopher J.; Almer, Jonathan D.

    2015-06-01

    As a result of in-reactor corrosion during operation in nuclear reactors, hydrogen can enter the zirconium fuel cladding and precipitate as brittle hydride particles, which may reduce cladding ductility. Dissolved hydrogen responds to temperature gradients, resulting in transport and precipitation into cold spots so that the distribution of hydrides in the cladding is inhomogeneous. The hydrogen precipitation kinetics plays a strong role in the spatial distribution of the hydrides in the cladding. The precipitation rate is normally described as proportional to the supersaturation of hydrogen in solid solution. The proportionality constant, α2, for hydride precipitation in Zircaloy-4 is measured directly using in situ synchrotron X-Ray diffraction, at different temperatures and with three different initial hydrogen concentrations. The results validate the linear approximation of the phenomenological model and a near constant value of α2 = 4.5 × 10-4 s-1 was determined for the temperature range studied.

  9. Issues of convection in insect respiration: Insights from synchrotron X-ray imaging and beyond

    SciTech Connect

    Socha, John J.; Förster, Thomas D.; Greenlee, Kendra J.

    2010-11-01

    While it has long been known that in small animals, such as insects, sufficient gas transport could be provided by diffusion, it is now recognized that animals generate and control convective flows to improve oxygen delivery across a range of body sizes and taxa. However, size-based methodological limitations have constrained our understanding of the mechanisms that underlie the production of these convective flows. Recently, new techniques have enabled the elucidation of the anatomical structures and physiological processes that contribute to creating and maintaining bulk flow in small animals. In particular, synchrotron X-ray imaging provides unprecedented spatial and temporal resolution of internal functional morphology and is changing the way we understand gas exchange in insects. This symposium highlights recent efforts towards understanding the relationship between form, function, and control in the insect respiratory system.

  10. Synchrotron radiation x-ray beam profile monitor using chemical vapor deposition diamond film

    SciTech Connect

    Kudo, Togo; Takahashi, Sunao; Nariyama, Nobuteru; Hirono, Toko; Tachibana, Takeshi; Kitamura, Hideo

    2006-12-15

    Photoluminescence (PL) of a Si-doped polycrystalline diamond film fabricated using the chemical vapor deposition technique was employed to measure the profile of a synchrotron radiation pink x-ray beam emitted from an in-vacuum hybrid undulator at the SPring-8 facility. The spectrum of the section of the diamond film penetrated by the emitted visible red light exhibited a peak at 739 nm and a wideband structure extending from 550 to 700 nm. The PL intensity increased with the absorbed dose of the incident beam in the diamond within a dynamic range of 10{sup 3}. A two-dimensional distribution of the PL intensity revealed the undulator beam profile.

  11. Synchrotron X-Ray Microdiffraction Studies of Electromigration in Interconnect lines at the Advanced Light Source

    SciTech Connect

    Tamura, Nobumichi; Chen, Kai; Kunz, Martin

    2009-12-01

    Synchrotron polychromatic X-ray microdiffraction is a particularly suitable technique to study in situ the effect of electromigration in metal interconnects as add spatial resolution to grain orientation and strain sensitivity. This technique has been extensively used at the Advanced Light Source to monitor changes in aluminum and copper interconnect test structures while high-density current is passed into them during accelerated tests at elevated temperature. One of the principal findings is the observation of electromigration-induced plasticity in the metal lines that appear during the very early stages of electromigration. In some of the lines, high density of geometrically necessary dislocation are formed leading to additional diffusion paths causing an enhancement of electromigration effect at test temperature.

  12. SYNCHROTRON X-RAY MICROPROBE AND COMPUTED MICROTOMOGRAPHY FOR CHARACTERIZATION OF NANOCATALYSTS.

    SciTech Connect

    JONES, K.W.; FENG, H.; LANZIROTTI, A.; MAHAJAN, D.

    2004-06-01

    Gas-to-liquids (GTL) is a viable pathway for synthesis of clean fuels from natural gas. One of the attractive synthesis options is the Fischer-Tropsch (F-T) method using an iron catalyst to yield a broad range of hydrocarbons. We collected catalyst samples during three separate F-T runs that utilized nanophase (mean particle diameter (MPD): 3 nm and 20-80 nm) and micrometer-sized (32.5 ? m) Fe{sub 2}O{sub 3} that served as catalyst precursors. The collected samples were characterized with micro x-ray fluorescence and computed Microtomography at the National Synchrotron Light Source (NSLS). Results found with two different measurement techniques indicated that there was heterogeneity on a spatial scale corresponding to volumes of roughly 10{sup 3} {micro}m{sup 3}.

  13. Applied x-ray computed tomography with high resolution in paleontology using laboratory and synchrotron sources

    NASA Astrophysics Data System (ADS)

    Bidola, Pidassa; Pacheco, Mirian L. A. F.; Stockmar, Marco K.; Achterhold, Klaus; Pfeiffer, Franz; Beckmann, Felix; Tafforeau, Paul; Herzen, Julia

    2014-09-01

    X-ray computed tomography (CT) has become an established technique in the biomedical imaging or materials science research. Its ability to non-destructively provide high-resolution images of samples makes it attractive for diverse fields of research especially the paleontology. Exceptionally, the Precambrian is a geological time of rocks deposition containing several fossilized early animals, which still need to be investigated in order to predict the origin and evolution of early life. Corumbella werneri is one of those fossils skeletonized in Corumbá (Brazil). Here, we present a study on selected specimens of Corumbella werneri using absorption-based contrast imaging at diverse tomographic setups. We investigated the potential of conventional laboratory-based device and synchrotron radiation sources to visualize internal structures of the fossils. The obtained results are discussed as well as the encountered limitations of those setups.

  14. Compressional residual stress in Bastogne boudins revealed by synchrotron X-ray microdiffraction

    NASA Astrophysics Data System (ADS)

    Chen, Kai; Kunz, Martin; Li, Yao; Zepeda-Alarcon, Eloisa; Sintubin, Manuel; Wenk, Hans-Rudolf

    2016-06-01

    Lattice distortions in crystals can be mapped at the micron scale using synchrotron X-ray Laue microdiffraction (μXRD). From lattice distortions the shape and orientation of the elastic strain tensor can be derived and interpreted in terms of residual stress. Here we apply the new method to vein quartz from the original boudinage locality at Bastogne, Belgium. A long-standing debate surrounds the kinematics of the Bastogne boudins. The μXRD measurements reveal a shortening residual elastic strain, perpendicular to the vein wall, corroborating the model that the Bastogne boudins formed by layer-parallel shortening and not by layer-parallel extension, as is in the geological community generally inferred by the process of boudinage.

  15. Hydride precipitation kinetics in Zircaloy-4 studied using synchrotron X-ray diffraction

    SciTech Connect

    Courty, Olivier Fabrice; Motta, Arthur T.; Piotrowski, Christopher J.; Almer, Jonathan D.

    2015-01-01

    As a result of in-reactor corrosion during operation in nuclear reactors, hydrogen can enter the zirconium fuel cladding and precipitate as brittle hydride particles, which may reduce cladding ductility. Dissolved hydrogen responds to temperature gradients, resulting in transport and precipitation into cold spots so that the distribution of hydrides in the cladding is inhomogeneous. The hydrogen precipitation kinetics plays a strong role in the spatial distribution of the hydrides in the cladding. The precipitation rate is normally described as proportional to the supersaturation of hydrogen in solid solution. The proportionality constant, α2, for hydride precipitation in Zircaloy-4 is measured directly using in situ synchrotron X-Ray diffraction, at different temperatures and with three different initial hydrogen concentrations. The results validate the linear approximation of the phenomenological model and a near constant value of α2 = 4.5 × 10-4 s-1 was determined for the temperature range studied.

  16. Issues of convection in insect respiration: insights from synchrotron X-ray imaging and beyond.

    PubMed

    Socha, John J; Förster, Thomas D; Greenlee, Kendra J

    2010-08-31

    While it has long been known that in small animals, such as insects, sufficient gas transport could be provided by diffusion, it is now recognized that animals generate and control convective flows to improve oxygen delivery across a range of body sizes and taxa. However, size-based methodological limitations have constrained our understanding of the mechanisms that underlie the production of these convective flows. Recently, new techniques have enabled the elucidation of the anatomical structures and physiological processes that contribute to creating and maintaining bulk flow in small animals. In particular, synchrotron X-ray imaging provides unprecedented spatial and temporal resolution of internal functional morphology and is changing the way we understand gas exchange in insects. This symposium highlights recent efforts towards understanding the relationship between form, function, and control in the insect respiratory system. PMID:20347054

  17. Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography.

    PubMed

    Harry, Katherine J; Parkinson, Dilworth Y; Balsara, Nitash P

    2015-01-01

    Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent of lithium-ion batteries, researchers have known that the lithium metal anode has the highest theoretical energy density of any anode material. However, rechargeable batteries containing a lithium metal anode are not widely used in consumer products because the growth of lithium dendrites from the anode upon charging of the battery causes premature cell failure by short circuit. Lithium dendrites can also form in commercial lithium-ion batteries with graphite anodes if they are improperly charged. We demonstrate that lithium dendrite growth can be studied using synchrotron-based hard X-ray microtomography. This non-destructive imaging technique allows researchers to study the growth of lithium dendrites, in addition to other morphological changes inside batteries, and subsequently develop methods to extend battery life. PMID:26382323

  18. X-Ray Irradiation of H2O + CO Ice Mixtures with Synchrotron Light

    NASA Astrophysics Data System (ADS)

    Jiménez-Escobar, A.; Chen, Y.-J.; Ciaravella, A.; Huang, C.-H.; Micela, G.; Cecchi-Pestellini, C.

    2016-03-01

    We irradiated a (4:1) mixture of water and carbon monoxide with soft X-rays of energies up to 1.2 keV. The experiments were performed using the spherical grating monochromator beamline at National Synchrotron Radiation Research Center in Taiwan. Both monochromatic (300 and 900 eV) and broader energy fluxes (250-1200 eV) were employed. During the irradiation, the H2O + CO mixture was ionized, excited, and fragmented, producing a number of reactive species. The composition of the ice has been monitored throughout both the irradiation and warm-up phases. We identified several products, which can be related through a plausible chemical reaction scheme. Such chemistry is initiated by the injection of energetic photoelectrons that produce multiple ionization events generating a secondary electron cascade. The results have been discussed in light of a model for protoplanetary disks around young solar-type stars.

  19. Synchrotron-based soft X-ray spectroscopic studies of the electronic structure of organic semiconducting molecules

    NASA Astrophysics Data System (ADS)

    Demasi, Alexander

    Organic molecules have been the subject of many scientific studies due to their potential for use in a new generation of optoelectronic and semiconducting devices, such as organic photovoltaics and organic light emitting diodes. These studies are motivated by the fact that organic semiconductor devices have several advantages over traditional inorganic semiconductor devices. Unlike inorganic semiconductors, where the electronic properties are a result of the deliberate introduction of dopants to the material, the properties of organic semiconductors are often intrinsic to the molecules themselves. As a result, organic semiconductor devices are frequently less susceptible to contamination by impurities than their inorganic counterparts, which results in the relatively lower cost of producing such devices. Accurate experimental determination of the bulk and surface electronic structure of organic semiconductors is a prerequisite in developing a comprehensive understanding of such materials. The organic materials studied in this thesis were N,N-Ethylene-bis(1,1,1trifluoropentane-2,4-dioneiminato)-copper(ii) (abbreviated Cu-TFAC), aluminum tris-8hydroxyquinoline (A1g3), lithium quinolate (Liq), tetracyanoquinodimethane (TCNQ), and tetrafluorotetracyanoquinodimethane (F4TCNQ). The electronic structures of these materials were measured with several synchrotron-based x-ray spectroscopies. X-ray photoemission spectroscopy was used to measure the occupied total density of states and the core-level states of the aforementioned materials. X-ray absorption spectroscopy (XAS) was used to probe the element-specific unoccupied partial density of states (PDOS); its angle-resolved variant was used to measure the orientation of the molecules in a film and, in some circumstances, to gauge the extent of an organic film's crystallinity. Most notably, x-ray emission spectroscopy (XES) measures the element- specific occupied PDOS and, when aided by XAS, resonant XES can additionally be

  20. Synchrotron radiation-based x-ray analysis of bronze artifacts from an Iron Age site in the Judean hills.

    SciTech Connect

    Friedman, E. S.; Brody, A. J.; Young, M. L.; Almer, J. D.; Serge, C. U.; Mini, S. M.; IIT; Pacific School of Religion; Northwestern Univ.; Northern Illinois Univ.

    2008-07-01

    Seven bronze bangles from Tell en-Nasbeh, northern Judah, were investigated to understand the phase composition and manufacturing process of the artifacts, and possibly suggest a provenance for their origin. Synchrotron x-ray radiation diffraction (XRD) and fluorescence (XRF) were used in the analysis to avoid any destructive sampling and at the same time penetrate through the surface into the core metal. These techniques enabled us to determine that the bangles were not just tin bronze, but leaded tin bronze. Based on excavation reports, it is unlikely that the metal objects were manufactured locally at Tell en-Nasbeh; rather, preliminary XRD and XRF data point towards the neighboring region of Edom as their origin. Despite their political enmity during the Iron Age II, the data suggest that Judahite social demands for bronze may have fostered a strong economic relationship between these two polities.

  1. Synchrotron-based X-ray absorption spectroscopy for art conservation: looking back and looking forward.

    PubMed

    Cotte, Marine; Susini, Jean; Dik, Joris; Janssens, Koen

    2010-06-15

    A variety of analytical techniques augmented by the use of synchrotron radiation (SR), such as X-ray fluorescence (SR-XRF) and X-ray diffraction (SR-XRD), are now readily available, and they differ little, conceptually, from their common laboratory counterparts. Because of numerous advantages afforded by SR-based techniques over benchtop versions, however, SR methods have become popular with archaeologists, art historians, curators, and other researchers in the field of cultural heritage (CH). Although the CH community now commonly uses both SR-XRF and SR-XRD, the use of synchrotron-based X-ray absorption spectroscopy (SR-XAS) techniques remains marginal, mostly because CH specialists rarely interact with SR physicists. In this Account, we examine the basic principles and capabilities of XAS techniques in art preservation. XAS techniques offer a combination of features particularly well-suited for the chemical analysis of works of art. The methods are noninvasive, have low detection limits, afford high lateral resolution, and provide exceptional chemical sensitivity. These characteristics are highly desirable for the chemical characterization of precious, heterogeneous, and complex materials. In particular, the chemical mapping capability, with high spatial resolution that provides information about local composition and chemical states, even for trace elements, is a unique asset. The chemistry involved in both the object's history (that is, during fabrication) and future (that is, during preservation and restoration treatments) can be addressed by XAS. On the one hand, many studies seek to explain optical effects occurring in historical glasses or ceramics by probing the molecular environment of relevant chromophores. Hence, XAS can provide insight into craft skills that were mastered years, decades, or centuries ago but were lost over the course of time. On the other hand, XAS can also be used to characterize unwanted reactions, which are then considered

  2. Progress in silicon-to-silicon direct bonding and its application to synchrotron x-ray optics

    SciTech Connect

    Graber, T.; Krasnicki, S.; Fernandez, P.B.

    1997-02-01

    X-ray optical elements (such as single-crystal silicon monochromators) illuminated with high-power synchrotron-radiation beams produced by insertion devices and, to a lesser extent bending magnets, require cooling, When operating a silicon crystal at room temperature, channels for the coolant are often fabricated directly beneath the diffracting surface. Then a separate silicon distribution manifold/plenum is manufactured, and the components are bonded together using an adhesive or some intermediate material. In many cases, such monochromators suffer from strains induced by the bond. A silicon-to-silicon direct-bonding technique (i.e., without any intermediate material) has been developed that appears to be an attractive method for creating a bond with less strain between two pieces of silicon. This technique is well understood for the case of thin wafers ({approximately}0.5 mm thickness) and is used by the semiconductor industry. Recently, bonding of 16-mm-thick 10-cm-diameter silicon crystals has been successfully performed inducing very little strain. A short review of the silicon-to-silicon crystals has been successfully performed inducing very little strain. A short review of the silicon-to-silicon direct-bonding process will be presented with an emphasis on its application to room temperature high-heat-load x-ray optics with the present status of direct bonding efforts at the APS.

  3. High-resolution non-invasive 3D imaging of paint microstructure by synchrotron-based X-ray laminography

    NASA Astrophysics Data System (ADS)

    Reischig, Péter; Helfen, Lukas; Wallert, Arie; Baumbach, Tilo; Dik, Joris

    2013-06-01

    The characterisation of the microstructure and micromechanical behaviour of paint is key to a range of problems related to the conservation or technical art history of paintings. Synchrotron-based X-ray laminography is demonstrated in this paper to image the local sub-surface microstructure in paintings in a non-invasive and non-destructive way. Based on absorption and phase contrast, the method can provide high-resolution 3D maps of the paint stratigraphy, including the substrate, and visualise small features, such as pigment particles, voids, cracks, wood cells, canvas fibres etc. Reconstructions may be indicative of local density or chemical composition due to increased attenuation of X-rays by elements of higher atomic number. The paint layers and their interfaces can be distinguished via variations in morphology or composition. Results of feasibility tests on a painting mockup (oak panel, chalk ground, vermilion and lead white paint) are shown, where lateral and depth resolution of up to a few micrometres is demonstrated. The method is well adapted to study the temporal evolution of the stratigraphy in test specimens and offers an alternative to destructive sampling of original works of art.

  4. Method for obtaining silver nanoparticle concentrations within a porous medium via synchrotron X-ray computed microtomography.

    PubMed

    Molnar, Ian L; Willson, Clinton S; O'Carroll, Denis M; Rivers, Mark L; Gerhard, Jason I

    2014-01-21

    Attempts at understanding nanoparticle fate and transport in the subsurface environment are currently hindered by an inability to quantify nanoparticle behavior at the pore scale (within and between pores) within realistic pore networks. This paper is the first to present a method for high resolution quantification of silver nanoparticle (nAg) concentrations within porous media under controlled experimental conditions. This method makes it possible to extract silver nanoparticle concentrations within individual pores in static and quasi-dynamic (i.e., transport) systems. Quantification is achieved by employing absorption-edge synchrotron X-ray computed microtomography (SXCMT) and an extension of the Beer-Lambert law. Three-dimensional maps of X-ray mass linear attenuation are converted to SXCMT-determined nAg concentration and are found to closely match the concentrations determined by ICP analysis. In addition, factors affecting the quality of the SXCMT-determined results are investigated: 1) The acquisition of an additional above-edge data set reduced the standard deviation of SXCMT-determined concentrations; 2) X-ray refraction at the grain/water interface artificially depresses the SXCMT-determined concentrations within 18.1 μm of a grain surface; 3) By treating the approximately 20 × 10(6) voxels within each data set statistically (i.e., averaging), a high level of confidence in the SXCMT-determined mean concentrations can be obtained. This novel method provides the means to examine a wide range of properties related to nanoparticle transport in controlled laboratory porous medium experiments. PMID:24354304

  5. Visualisation by high resolution synchrotron X-ray phase contrast micro-tomography of gas films on submerged superhydrophobic leaves.

    PubMed

    Lauridsen, Torsten; Glavina, Kyriaki; Colmer, Timothy David; Winkel, Anders; Irvine, Sarah; Lefmann, Kim; Feidenhans'l, Robert; Pedersen, Ole

    2014-10-01

    Floods can completely submerge terrestrial plants but some wetland species can sustain O2 and CO2 exchange with the environment via gas films forming on superhydrophobic leaf surfaces. We used high resolution synchrotron X-ray phase contrast micro-tomography in a novel approach to visualise gas films on submerged leaves of common cordgrass (Spartina anglica). 3D tomograms enabled a hitherto unmatched level of detail regarding the micro-topography of leaf gas films. Gas films formed only on the superhydrophobic adaxial leaf side (water droplet contact angle, Φ=162°) but not on the abaxial side (Φ=135°). The adaxial side of the leaves of common cordgrass is plicate with a longitudinal system of parallel grooves and ridges and the vast majority of the gas film volume was found in large ∼180μm deep elongated triangular volumes in the grooves and these volumes were connected to each neighbouring groove via a fine network of gas tubules (∼1.7μm diameter) across the ridges. In addition to the gas film retained on the leaf exterior, the X-ray phase contrast micro-tomography also successfully distinguished gas spaces internally in the leaf tissues, and the tissue porosity (gas volume per unit tissue volume) ranged from 6.3% to 20.3% in tip and base leaf segments, respectively. We conclude that X-ray phase contrast micro-tomography is a powerful tool to obtain quantitative data of exterior gas features on biological samples because of the significant difference in electron density between air, biological tissues and water. PMID:25175398

  6. In situ synchrotron x-ray studies of LiMn{sub 2}O{sub 4} cathodes

    SciTech Connect

    McBreen, J.; Mukerjee, S.; Yang, X.Q.

    1997-05-01

    LiCoO{sub 2} cathodes are now used in most commercial lithium ion batteries. LiMn{sub 2}O{sub 4} is an attractive low cost alternative. However, it is difficult to make reproducibly. At Brookhaven National Laboratory two in situ synchrotron x-ray techniques, that are available at the National Synchrotron Light Source (NSLS), have been used to investigate LiMn{sub 2}O{sub 4}. The techniques are x-ray absorption and high resolution x-ray diffraction. With x-ray absorption it is possible to follow the changes in the Mn oxidation state and the changes in the Mn-O and Mn-Mn bond lengths on cycling. Also it is possible to detect amorphous phases. The high energy x-rays at the diffraction Beam Lines at the NSLS (up to 24 KeV) permit in situ x-ray diffraction, in the transmission mode, in thin lithium and lithium ion cells. The evolution of the structural chances that occur on cycling can be followed. These in situ measurements were done on Li/LiMn{sub 2}O{sub 4} cells with a liquid electrolyte (1 M LiPF{sub 6} in a 1:1:3 PC:EC:DMC solvent).

  7. PROFFIT: Analysis of X-ray surface-brightness profiles

    NASA Astrophysics Data System (ADS)

    Eckert, Dominique

    2016-08-01

    PROFFIT analyzes X-ray surface-brightness profiles for data from any X-ray instrument. It can extract surface-brightness profiles in circular or elliptical annuli, using constant or logarithmic bin size, from the image centroid, the surface-brightness peak, or any user-given center, and provides surface-brightness profiles in any circular or elliptical sectors. It offers background map support to extract background profiles, can excise areas using SAO DS9-compatible (ascl:0003.002) region files to exclude point sources, provides fitting with a number of built-in models, including the popular beta model, double beta, cusp beta, power law, and projected broken power law, uses chi-squared or C statistic, and can fit on the surface-brightness or counts data. It has a command-line interface similar to HEASOFT’s XSPEC (ascl:9910.005) package, provides interactive help with a description of all the commands, and results can be saved in FITS, ROOT or TXT format.

  8. X-ray fluorescence surface contaminant analyzer: A feasibility study

    NASA Technical Reports Server (NTRS)

    Eldridge, Hudson B.

    1988-01-01

    The bonding of liner material to the inner metal surfaces of solid rocket booster cases is adversely affected by minute amounts of impurities on the metal surface. Suitable non-destructive methods currently used for detecting these surface contaminants do not provide the means of identifying their elemental composition. The feasibility of using isotopic source excited energy dispersive X-ray fluorescence as a possible technique for elemental analysis of such contaminants is investigated. A survey is made of the elemental compositions of both D-6ac steel, a common construction material for the booster cases, and Conoco HD-2 grease, a common surface contamination. Source and detector choices that maximize signal to noise ratio in a Recessed Source Geometry are made. A Monte Carlo simulation is then made of the optimized device incorporating the latest available X-ray constants at the energy of the chosen source to determine the device's response to a D-6ac steel surface contained with Conoco HD-2 grease.

  9. Synchrotron X-ray footprinting as a method to visualize water in proteins.

    PubMed

    Gupta, Sayan; Feng, Jun; Chan, Leanne Jade G; Petzold, Christopher J; Ralston, Corie Y

    2016-09-01

    The vast majority of biomolecular processes are controlled or facilitated by water interactions. In enzymes, regulatory proteins, membrane-bound receptors and ion-channels, water bound to functionally important residues creates hydrogen-bonding networks that underlie the mechanism of action of the macromolecule. High-resolution X-ray structures are often difficult to obtain with many of these classes of proteins because sample conditions, such as the necessity of detergents, often impede crystallization. Other biophysical techniques such as neutron scattering, nuclear magnetic resonance and Fourier transform infrared spectroscopy are useful for studying internal water, though each has its own advantages and drawbacks, and often a hybrid approach is required to address important biological problems associated with protein-water interactions. One major area requiring more investigation is the study of bound water molecules which reside in cavities and channels and which are often involved in both the structural and functional aspects of receptor, transporter and ion channel proteins. In recent years, significant progress has been made in synchrotron-based radiolytic labeling and mass spectroscopy techniques for both the identification of bound waters and for characterizing the role of water in protein conformational changes at a high degree of spatial and temporal resolution. Here the latest developments and future capabilities of this method for investigating water-protein interactions and its synergy with other synchrotron-based methods are discussed. PMID:27577756

  10. Chemical Mapping of Paleontological and Archeological Artifacts with Synchrotron X-Rays

    NASA Astrophysics Data System (ADS)

    Bergmann, Uwe; Manning, Phillip L.; Wogelius, Roy A.

    2012-07-01

    The application of the recently developed synchrotron rapid scanning X-ray fluorescence (SRS-XRF) technique to the mapping of large objects is the focus of this review. We discuss the advantages of SRS-XRF over traditional systems and the use of other synchrotron radiation (SR) techniques to provide corroborating spectroscopic and diffraction analyses during the same analytical session. After reviewing routine techniques used to analyze precious specimens, we present several case studies that show how SR-based methods have been successfully applied in archeology and paleontology. For example, SRS-XRF imaging of a seventh-century Qur'ān palimpsest and an overpainted original opera score from Luigi Cherubini is described. We also review the recent discovery of soft-tissue residue in fossils of Archaeopteryx and an ancient reptile, as well as work that has successfully resolved the remnants of pigment in Confuciusornis sanctus, a 120-million-year-old fossil of the oldest documented bird with a fully derived avian beak.

  11. Performance of Multilayer Monochromators for Hard X-Ray Imaging with Coherent Synchrotron Radiation

    SciTech Connect

    Dietsch, R.; Holz, T.; Kraemer, M.; Weissbach, D.; Rack, A.; Weitkamp, T.; Morawe, Ch.; Cloetens, P.; Ziegler, E.; Riotte, M.; Rack, T.; Siewert, F.

    2011-09-09

    We present a study in which multilayers of different periodicity (from 2.5 to 5.5 nm), composition (W/Si, Mo/Si, Pd/B{sub 4}C, Ru/B{sub 4}C), and numbers of layers have been compared. Particularly, we chose mirrors with similar intrinsic quality (roughness and reflectivity) to study their performance (flatness and coherence of the outgoing beam) as monochromators in synchrotron radiography. The results indicate that material composition is the dominating factor for the performance. This is important to consider for future developments in synchrotron-based hard x-ray imaging methods. In these techniques, multilayer monochromators are popular because of their good tradeoff between spectral bandwidth and photon flux density of the outgoing beam, but sufficient homogeneity and preservation of the coherent properties of the reflected beam are major concerns. The experimental results we collected may help scientists and engineers specify multilayer monochromators and can contribute to better exploitation of the advantages of multilayer monochromators in microtomography and other full-field imaging techniques.

  12. Using synchrotron X-ray fluorescence microprobes in the study of metal homeostasis in plants

    PubMed Central

    Punshon, Tracy; Guerinot, Mary Lou; Lanzirotti, Antonio

    2009-01-01

    Background and Aims This Botanical Briefing reviews the application of synchrotron X-ray fluorescence (SXRF) microprobes to the plant sciences; how the technique has expanded our knowledge of metal(loid) homeostasis, and how it can be used in the future. Scope The use of SXRF microspectroscopy and microtomography in research on metal homeostasis in plants is reviewed. The potential use of SXRF as part of the ionomics toolbox, where it is able to provide fundamental information on the way that plants control metal homeostasis, is recommended. Conclusions SXRF is one of the few techniques capable of providing spatially resolved in-vivo metal abundance data on a sub-micrometre scale, without the need for chemical fixation, coating, drying or even sectioning of samples. This gives researchers the ability to uncover mechanisms of plant metal homeostasis that can potentially be obscured by the artefacts of sample preparation. Further, new generation synchrotrons with smaller beam sizes and more sensitive detection systems will allow for the imaging of metal distribution within single living plant cells. Even greater advances in our understanding of metal homeostasis in plants can be gained by overcoming some of the practical boundaries that exist in the use of SXRF analysis. PMID:19182222

  13. Using Synchrotron X-ray Fluorescence Microprobes in the Study of Metal Homeostasis in Plants

    SciTech Connect

    Punshon, T.; Guerinot, M; Lanzirotti, A

    2009-01-01

    Background and Aims: This Botanical Briefing reviews the application of synchrotron X-ray fluorescence (SXRF) microprobes to the plant sciences; how the technique has expanded our knowledge of metal(loid) homeostasis, and how it can be used in the future. Scope: The use of SXRF microspectroscopy and microtomography in research on metal homeostasis in plants is reviewed. The potential use of SXRF as part of the ionomics toolbox, where it is able to provide fundamental information on the way that plants control metal homeostasis, is recommended. Conclusions: SXRF is one of the few techniques capable of providing spatially resolved in-vivo metal abundance data on a sub-micrometre scale, without the need for chemical fixation, coating, drying or even sectioning of samples. This gives researchers the ability to uncover mechanisms of plant metal homeostasis that can potentially be obscured by the artefacts of sample preparation. Further, new generation synchrotrons with smaller beam sizes and more sensitive detection systems will allow for the imaging of metal distribution within single living plant cells. Even greater advances in our understanding of metal homeostasis in plants can be gained by overcoming some of the practical boundaries that exist in the use of SXRF analysis.

  14. X-ray microfluorescence with synchrotron radiation applied in the analysis of pigments from ancient Egypt

    NASA Astrophysics Data System (ADS)

    Calza, C.; Anjos, M. J.; Mendonça de Souza, S. M. F.; Brancaglion, A., Jr.; Lopes, R. T.

    2008-01-01

    In this work, X-ray microfluorescence with the synchrotron radiation technique was applied in the analysis of pigments found in decorative paintings in the sarcophagus of an Egyptian mummy. This female mummy, from the Roman Period, which was embalmed with the arms and legs swathed separately is considered one of the most important pieces of the Egyptian Collection from the National Museum (Rio de Janeiro, Brazil). The measurements were performed at the XRF beamline D09B of the Brazilian Synchrotron Light Laboratory (LNLS), using the white beam and a Si(Li) detector with resolution of 165 eV at 5.9 keV. The possible pigments found in the samples were: Egyptian blue, Egyptian green frit, green earth, verdigris, malachite, ochre, realgar, chalk, gypsum, bone white, ivory black and magnetite. Hierarchical cluster analysis (HCA) and principal component analysis (PCA) were applied to the results in order to verify if the samples belong to the same period of a linen wrapping fragment, whose provenance was well established.

  15. Synchrotron X-ray bio-imaging of natural and synthetic bone-graft materials in an aqueous environment

    NASA Astrophysics Data System (ADS)

    Kim, Yong-Gun; Bark, Chung Wung

    2014-11-01

    Bone-graft materials in dentistry have osteoinductive and osteoconductive abilities, which depend on their microstructural characteristics, such as their porosity, particle size, micro channels, and absorption. These characteristics have been observed using various imaging techniques, such as optical microscopy and scanning electron microscopy (SEM). However, most techniques cannot provide images in water, even though graft materials in vivo are invariably in contact with different water-based fluids. Synchrotron X-ray imaging allows sample microenvironments to be controlled as X-ray beams easily penetrate air and water. In this report, we used the synchrotron X-ray imaging technique to provide in-situ images of various bone-graft materials in aqueous environments. We observed internal microstructural images of bone-graft materials in real-time in 0.9% saline solution and interactions between bone-graft materials and saline, that is, hydration patterns and bone-graft expansion.

  16. Development of Si-APD Timing Detectors for Nuclear Resonant Scattering using High-energy Synchrotron X-rays

    SciTech Connect

    Kishimoto, Shunji; Zhang Xiaowei

    2007-01-19

    A timing detector with silicon avalanche photodiodes (Si-APDs) has been developed for nuclear resonant scattering using synchrotron x-rays. The detector had four pairs of a germanium plate 0.1mm thick and a Si-APD (3 mm in dia., a depletion layer of 30-{mu}m thickness). Using synchrotron x-rays of 67.4 keV, the efficiency increased to 1.5% for the incident beam, while the efficiency was 0.76 % without the germanium converters. A measurement of SR-PAC on Ni-61 was executed by using the detector. Some other types of timing detectors are planned for x-rays of E>20 keV.

  17. Time-Resolved Synchrotron X-ray Diffraction on Pulse Laser Heated Iron in Diamond Anvil Cell

    SciTech Connect

    Yoo, C S; Wei, H; Dias, R; Shen, G; Smith, J; Chen, J Y; Evans, W

    2011-09-21

    The authors present time-resolved synchrotron x-ray diffraction to probe the {var_epsilon}-{delta} phase transition of iron during pulse-laser heating in a diamond anvil cell. The system utilizes a monochromatic synchrotron x-ray beam, a two-dimensional pixel array x-ray detector and a dual beam, double side laser-heating system. Multiple frames of the diffraction images are obtained in real-time every 22 ms over 500 ms of the entire pulse heating period. The results show the structural evolution of iron phases at 17 GPa, resulting in thermal expansion coefficient 1/V({Delta}V/{Delta}T){sub p} = 7.1 * 10{sup -6}/K for {var_epsilon}-Fe and 2.4 * 10{sup -5}/K for {gamma}-Fe, as well as the evidence for metastability of {gamma}-Fe at low temperatures below the {var_epsilon}-{gamma} phase boundary.

  18. Synchrotron X-ray powder diffraction data of LASSBio-1515: A new N-acylhydrazone derivative compound

    NASA Astrophysics Data System (ADS)

    Costa, F. N.; Braz, D.; Ferreira, F. F.; da Silva, T. F.; Barreiro, E. J.; Lima, L. M.; Colaço, M. V.; Kuplich, L.; Barroso, R. C.

    2014-02-01

    In this work, synchrotron X-ray powder diffraction data allowed for a successful indexing of LASSBio-1515 compound, candidate to analgesic and anti-inflammatory activity. X-ray powder diffraction data collected in transmission and high-throughput geometries were used to analyze this compound. The X-ray wavelength of the synchrotron radiation used in this study was determined to be λ=1.55054 Å. LASSBio-1515 was found to be monoclinic with space group P21/c and unit cell parameters a=11.26255(16) Å, b=12.59785(16) Å, c=8.8540(1) Å, β=90.5972(7)° and V=1256.17(3) Å3.

  19. Time-resolved structural studies at synchrotrons and X-ray free electron lasers: opportunities and challenges

    PubMed Central

    Neutze, Richard; Moffat, Keith

    2012-01-01

    X-ray free electron lasers (XFELs) are potentially revolutionary X-ray sources because of their very short pulse duration, extreme peak brilliance and high spatial coherence, features that distinguish them from today’s synchrotron sources. We review recent time-resolved Laue diffraction and time-resolved wide angle X-ray scattering (WAXS) studies at synchrotron sources, and initial static studies at XFELs. XFELs have the potential to transform the field of time-resolved structural biology, yet many challenges arise in devising and adapting hardware, experimental design and data analysis strategies to exploit their unusual properties. Despite these challenges, we are confident that XFEL sources are poised to shed new light on ultrafast protein reaction dynamics. PMID:23021004

  20. High-speed X-ray microscopy by use of high-resolution zone plates and synchrotron radiation.

    PubMed

    Hou, Qiyue; Wang, Zhili; Gao, Kun; Pan, Zhiyun; Wang, Dajiang; Ge, Xin; Zhang, Kai; Hong, Youli; Zhu, Peiping; Wu, Ziyu

    2012-09-01

    X-ray microscopy based on synchrotron radiation has become a fundamental tool in biology and life sciences to visualize the morphology of a specimen. These studies have particular requirements in terms of radiation damage and the image exposure time, which directly determines the total acquisition speed. To monitor and improve these key parameters, we present a novel X-ray microscopy method using a high-resolution zone plate as the objective and the matching condenser. Numerical simulations based on the scalar wave field theory validate the feasibility of the method and also indicate the performance of X-ray microscopy is optimized most with sub-10-nm-resolution zone plates. The proposed method is compatible with conventional X-ray microscopy techniques, such as computed tomography, and will find wide applications in time-resolved and/or dose-sensitive studies such as living cell imaging. PMID:22763718

  1. Quantifying X-Ray Pleochroism Effects in Synchrotron Micro-XANES Microanalyses of Elemental Oxidation States: Feldspar and Biotite

    NASA Technical Reports Server (NTRS)

    Delaney, J. S.; Dyar, M. D.; Sutton, S. R.

    2001-01-01

    X-ray pleochroism is a predictable source of scatter in synchrotron microXANES analyses of elemental oxidation states. The magnitude of the effect is illustrated and a procedure to compensate for it has been implemented, reducing errors significantly. Additional information is contained in the original extended abstract.

  2. Studies of protein structure in solution and protein folding using synchrotron small-angle x-ray scattering

    SciTech Connect

    Chen, Lingling

    1996-04-01

    Synchrotron small angle x-ray scattering (SAXS) has been applied to the structural study of several biological systems, including the nitrogenase complex, the heat shock cognate protein (hsc70), and lysozyme folding. The structural information revealed from the SAXS experiments is complementary to information obtained by other physical and biochemical methods, and adds to our knowledge and understanding of these systems.

  3. An Efficient Referencing And Sample Positioning System To Investigate Heterogeneous Substances With Combined Microfocused Synchrotron X-ray Techniques

    SciTech Connect

    Spangenberg, Thomas; Goettlicher, Joerg; Steininger, Ralph

    2009-01-29

    A referencing and sample positioning system has been developed to transfer object positions measured with an offline microscope to a synchrotron experimental station. The accuracy should be sufficient to deal with heterogeneous samples on micrometer scale. Together with an online fluorescence mapping visualisation the optical alignment helps to optimize measuring procedures for combined microfocused X-ray techniques.

  4. Theoretical analysis of the background intensity distribution in X-ray Birefringence Imaging using synchrotron bending-magnet radiation

    NASA Astrophysics Data System (ADS)

    Sutter, John P.; Dolbnya, Igor P.; Collins, Stephen P.; Harris, Kenneth D. M.; Edwards-Gau, Gregory R.; Palmer, Benjamin A.

    2015-04-01

    In the recently developed technique of X-ray Birefringence Imaging, molecular orientational order in anisotropic materials is studied by exploiting the birefringence of linearly polarized X-rays with energy close to an absorption edge of an element in the material. In the experimental setup, a vertically deflecting high-resolution double-crystal monochromator is used upstream from the sample to select the appropriate photon energy, and a horizontally deflecting X-ray polarization analyzer, consisting of a perfect single crystal with a Bragg reflection at Bragg angle of approximately 45°, is placed downstream from the sample to measure the resulting rotation of the X-ray polarization. However, if the experiment is performed on a synchrotron bending-magnet beamline, then the elliptical polarization of the X-rays out of the electron orbit plane affects the shape of the output beam. Also, because the monochromator introduces a correlation between vertical position and photon energy to the X-ray beam, the polarization analyzer does not select the entire beam, but instead selects a diagonal stripe, the slope of which depends on the Bragg angles of the monochromator and the polarization analyzer. In the present work, the final background intensity distribution is calculated analytically because the phase space sampling methods normally used in ray traces are too inefficient for this setup. X-ray Birefringence Imaging data measured at the Diamond Light Source beamline B16 agree well with the theory developed here.

  5. Theoretical analysis of the background intensity distribution in X-ray Birefringence Imaging using synchrotron bending-magnet radiation

    SciTech Connect

    Sutter, John P. Dolbnya, Igor P.; Collins, Stephen P.; Harris, Kenneth D. M.; Edwards-Gau, Gregory R.; Palmer, Benjamin A.

    2015-04-28

    In the recently developed technique of X-ray Birefringence Imaging, molecular orientational order in anisotropic materials is studied by exploiting the birefringence of linearly polarized X-rays with energy close to an absorption edge of an element in the material. In the experimental setup, a vertically deflecting high-resolution double-crystal monochromator is used upstream from the sample to select the appropriate photon energy, and a horizontally deflecting X-ray polarization analyzer, consisting of a perfect single crystal with a Bragg reflection at Bragg angle of approximately 45°, is placed downstream from the sample to measure the resulting rotation of the X-ray polarization. However, if the experiment is performed on a synchrotron bending-magnet beamline, then the elliptical polarization of the X-rays out of the electron orbit plane affects the shape of the output beam. Also, because the monochromator introduces a correlation between vertical position and photon energy to the X-ray beam, the polarization analyzer does not select the entire beam, but instead selects a diagonal stripe, the slope of which depends on the Bragg angles of the monochromator and the polarization analyzer. In the present work, the final background intensity distribution is calculated analytically because the phase space sampling methods normally used in ray traces are too inefficient for this setup. X-ray Birefringence Imaging data measured at the Diamond Light Source beamline B16 agree well with the theory developed here.

  6. Wetting state on hydrophilic and hydrophobic micro-textured surfaces: Thermodynamic analysis and X-ray visualization

    SciTech Connect

    Yu, Dong In; Kwak, Ho Jae; Doh, Seung Woo; Park, Hyun Sun Kiyofumi, Moriyama; Kang, Hie Chan; Ahn, Ho Seon; Kim, Moo Hwan

    2015-04-27

    In this study, the wetting state on hydrophobic and hydrophilic micro-textured surfaces was investigated. High spatial resolution synchrotron X-ray radiography was used to overcome the limitations in visualization in previous research and clearly visualize the wetting state for each droplet under quantified surface conditions. Based on thermodynamic characteristics, a theoretical model for wetting state depending on the chemical composition (intrinsic contact angle) and geometrical morphology (roughness ratio) of the surfaces was developed.

  7. Rare earth element concentrations in geological and synthetic samples using synchrotron X-ray fluorescence analysis

    USGS Publications Warehouse

    Chen, J.R.; Chao, E.C.T.; Back, J.M.; Minkin, J.A.; Rivers, M.L.; Sutton, S.R.; Cygan, G.L.; Grossman, J.N.; Reed, M.J.

    1993-01-01

    The concentrations of rare earth elements (REEs) in specific mineral grains from the Bayan Obo ore deposit and synthetic high-silica glass samples have been measured by synchrotron X-ray fluorescence (SXRF) analysis using excitation of the REE K lines between 33 and 63 keV. Because SXRF, a nondestructive analytical technique, has much lower minimum detection limits (MDLs) for REEs, it is an important device that extends the in situ analytical capability of electron probe microanalysis (EPMA). The distribution of trace amounts of REEs in common rock-forming minerals, as well as in REE minerals and minerals having minor quantities of REEs, can be analyzed with SXRF. Synchrotron radiation from a bending magnet and a wiggler source at the National Synchrotron Light Source, Brookhaven National Laboratory, was used to excite the REEs. MDLs of 6 ppm (La) to 26 ppm (Lu) for 3600 s in 60-??m-thick standard samples were obtained with a 25-??m diameter wiggler beam. The MDLs for the light REEs were a factor of 10-20 lower than the MDLs obtained with a bending magnet beam. The SXRF REE concentrations in mineral grains greater than 25 ??m compared favorably with measurements using EPMA. Because EPMA offered REE MDLs as low as several hundred ppm, the comparison was limited to the abundant light REEs (La, Ce, Pr, Nd). For trace values of medium and heavy REEs, the SXRF concentrations were in good agreement with measurements using instrumental neutron activation analysis (INAA), a bulk analysis technique. ?? 1993.

  8. Transmission X-ray scattering as a probe for complex liquid-surface structures

    DOE PAGESBeta

    Fukuto, Masafumi; Yang, Lin; Nykypanchuk, Dmytro; Kuzmenko, Ivan

    2016-01-28

    The need for functional materials calls for increasing complexity in self-assembly systems. As a result, the ability to probe both local structure and heterogeneities, such as phase-coexistence and domain morphologies, has become increasingly important to controlling self-assembly processes, including those at liquid surfaces. The traditional X-ray scattering methods for liquid surfaces, such as specular reflectivity and grazing-incidence diffraction, are not well suited to spatially resolving lateral heterogeneities due to large illuminated footprint. A possible alternative approach is to use scanning transmission X-ray scattering to simultaneously probe local intermolecular structures and heterogeneous domain morphologies on liquid surfaces. To test the feasibilitymore » of this approach, transmission small- and wide-angle X-ray scattering (TSAXS/TWAXS) studies of Langmuir films formed on water meniscus against a vertically immersed hydrophilic Si substrate were recently carried out. First-order diffraction rings were observed in TSAXS patterns from a monolayer of hexagonally packed gold nanoparticles and in TWAXS patterns from a monolayer of fluorinated fatty acids, both as a Langmuir monolayer on water meniscus and as a Langmuir–Blodgett monolayer on the substrate. The patterns taken at multiple spots have been analyzed to extract the shape of the meniscus surface and the ordered-monolayer coverage as a function of spot position. These results, together with continual improvement in the brightness and spot size of X-ray beams available at synchrotron facilities, support the possibility of using scanning-probe TSAXS/TWAXS to characterize heterogeneous structures at liquid surfaces.« less

  9. Transmission X-ray scattering as a probe for complex liquid-surface structures.

    PubMed

    Fukuto, Masafumi; Yang, Lin; Nykypanchuk, Dmytro; Kuzmenko, Ivan

    2016-03-01

    The need for functional materials calls for increasing complexity in self-assembly systems. As a result, the ability to probe both local structure and heterogeneities, such as phase-coexistence and domain morphologies, has become increasingly important to controlling self-assembly processes, including those at liquid surfaces. The traditional X-ray scattering methods for liquid surfaces, such as specular reflectivity and grazing-incidence diffraction, are not well suited to spatially resolving lateral heterogeneities due to large illuminated footprint. A possible alternative approach is to use scanning transmission X-ray scattering to simultaneously probe local intermolecular structures and heterogeneous domain morphologies on liquid surfaces. To test the feasibility of this approach, transmission small- and wide-angle X-ray scattering (TSAXS/TWAXS) studies of Langmuir films formed on water meniscus against a vertically immersed hydrophilic Si substrate were recently carried out. First-order diffraction rings were observed in TSAXS patterns from a monolayer of hexagonally packed gold nanoparticles and in TWAXS patterns from a monolayer of fluorinated fatty acids, both as a Langmuir monolayer on water meniscus and as a Langmuir-Blodgett monolayer on the substrate. The patterns taken at multiple spots have been analyzed to extract the shape of the meniscus surface and the ordered-monolayer coverage as a function of spot position. These results, together with continual improvement in the brightness and spot size of X-ray beams available at synchrotron facilities, support the possibility of using scanning-probe TSAXS/TWAXS to characterize heterogeneous structures at liquid surfaces. PMID:26917140

  10. Development of an in situ temperature stage for synchrotron X-ray spectromicroscopy

    NASA Astrophysics Data System (ADS)

    Chakraborty, R.; Serdy, J.; West, B.; Stuckelberger, M.; Lai, B.; Maser, J.; Bertoni, M. I.; Culpepper, M. L.; Buonassisi, T.

    2015-11-01

    In situ characterization of micro- and nanoscale defects in polycrystalline thin-film materials is required to elucidate the physics governing defect formation and evolution during photovoltaic device fabrication and operation. X-ray fluorescence spectromicroscopy is particularly well-suited to study defects in compound semiconductors, as it has a large information depth appropriate to study thick and complex materials, is sensitive to trace amounts of atomic species, and provides quantitative elemental information, non-destructively. Current in situ methods using this technique typically require extensive sample preparation. In this work, we design and build an in situ temperature stage to study defect kinetics in thin-film solar cells under actual processing conditions, requiring minimal sample preparation. Careful selection of construction materials also enables controlled non-oxidizing atmospheres inside the sample chamber such as H2Se and H2S. Temperature ramp rates of up to 300 °C/min are achieved, with a maximum sample temperature of 600 °C. As a case study, we use the stage for synchrotron X-ray fluorescence spectromicroscopy of CuInxGa1-xSe2 (CIGS) thin-films and demonstrate predictable sample thermal drift for temperatures 25-400 °C, allowing features on the order of the resolution of the measurement technique (125 nm) to be tracked while heating. The stage enables previously unattainable in situ studies of nanoscale defect kinetics under industrially relevant processing conditions, allowing a deeper understanding of the relationship between material processing parameters, materials properties, and device performance.

  11. Subacute Neuropathological Effects of Microplanar Beams of X-Rays from a Synchrotron Wiggler

    NASA Astrophysics Data System (ADS)

    Slatkin, D. N.; Spanne, P.; Dilmanian, F. A.; Gebbers, J.-O.; Laissue, J. A.

    1995-09-01

    Microplanar beam radiation therapy has been proposed to treat brain tumors by using a series of rapid exposures to an array of parallel x-ray beams, each beam having uniform microscopic thickness and macroscopic breadth (i.e., microplanar). Thirty-six rats were exposed head-on either to an upright 4-mm-high, 20- or 37-μ m-wide beam or to a horizontal 7-mm-wide, 42-μ m-high beam of mostly 32- to 126-keV, minimally divergent x-rays from the X17 wiggler at the National Synchrotron Light Source at Brookhaven National Laboratory. Parallel slices of the head, separated at either 75 or 200 μ m on center, were exposed sequentially at 310-650 grays (Gy) per second until each skin-entrance absorbed dose reached 312, 625, 1250, 2500, 5000, or 10,000 Gy. The rats were euthanized 2 weeks or 1 month later. Two rats with 10,000-Gy-entrance slices developed brain tissue necrosis. All the other 10,000- and 5000-Gy-entrance slices and some of the 2500- and 1250-Gy-entrance slices showed loss of neuronal and astrocytic nuclei and their perikarya. No other kind of brain damage was evident histologically in any rat with entrance absorbed doses <=5000 Gy. Brain tissues in and between all the 312- and 625-Gy-entrance slices appeared normal. This unusual resistance to necrosis is central to the rationale of microplanar beam radiation therapy for brain tumors.

  12. Development of an in situ temperature stage for synchrotron X-ray spectromicroscopy

    SciTech Connect

    Chakraborty, R. E-mail: buonassisi@mit.edu; Serdy, J.; Culpepper, M. L.; Buonassisi, T. E-mail: buonassisi@mit.edu; West, B.; Stuckelberger, M.; Bertoni, M. I.; Lai, B.; Maser, J.

    2015-11-15

    In situ characterization of micro- and nanoscale defects in polycrystalline thin-film materials is required to elucidate the physics governing defect formation and evolution during photovoltaic device fabrication and operation. X-ray fluorescence spectromicroscopy is particularly well-suited to study defects in compound semiconductors, as it has a large information depth appropriate to study thick and complex materials, is sensitive to trace amounts of atomic species, and provides quantitative elemental information, non-destructively. Current in situ methods using this technique typically require extensive sample preparation. In this work, we design and build an in situ temperature stage to study defect kinetics in thin-film solar cells under actual processing conditions, requiring minimal sample preparation. Careful selection of construction materials also enables controlled non-oxidizing atmospheres inside the sample chamber such as H{sub 2}Se and H{sub 2}S. Temperature ramp rates of up to 300 °C/min are achieved, with a maximum sample temperature of 600 °C. As a case study, we use the stage for synchrotron X-ray fluorescence spectromicroscopy of CuIn{sub x}Ga{sub 1−x}Se{sub 2} (CIGS) thin-films and demonstrate predictable sample thermal drift for temperatures 25–400 °C, allowing features on the order of the resolution of the measurement technique (125 nm) to be tracked while heating. The stage enables previously unattainable in situ studies of nanoscale defect kinetics under industrially relevant processing conditions, allowing a deeper understanding of the relationship between material processing parameters, materials properties, and device performance.

  13. Use of Synchrotron X-ray Fluorescence to Measure Trace Metal Distribution in the Brain

    NASA Astrophysics Data System (ADS)

    Linkous, D.; Flinn, J. M.; Lanzirotti, A.; Frederickson, C.; Jones, B. F.; Bertsch, P. M.

    2002-12-01

    X26A, National Synchrotron Light Source, was used to quantitatively evaluate the spatial distribution of trace metals, such as Zn and Cu, in brain tissue. X-ray microprobe techniques offer distinct advantages over other analytical methods by allowing analyses to be done in-situ with little or no chemical pretreatment and low detection limits (about 1 ppm). In the context of neuroscience, SXRF can provide non-destructive measurements of specific metal concentrations and distribution within nerve (brain) tissue. Neuronal tissue from organisms having undergone different normal or experimental conditions may be compared, with analytical capacities not limited by binding states of the metal (i.e., vesicular or enzymatic), as is the case with staining techniques.. Whole regions of tissue may be scanned for detectable trace metals at spatial resolutions of 10um or less using focused monochromatic x-ray beams. Here special attention has been given to zinc because it is the most common trace metal in the brain, and levels have been increasing in the environment. In this investigation, zinc concentrations present within the hilus of a rat hippocampus, and to a lesser extent in the cortex, have been shown to increase following long-term ingestion of zinc-enhanced drinking water that was associated with deficits in spatial memory. Concomitantly, copper concentrations in the internal capsule were comparatively lower. Other first order transition metals, Cr, V, Mn, and Co were not detected. In contrast, elevated levels of Zn, Cu, and Fe have been seen in amyloid plaques associated with Alzheimer's disease.

  14. Neighborite Under High Pressure: In Situ Angle Dispersive X-ray Diffraction Study Using Synchrotron Radiation

    NASA Astrophysics Data System (ADS)

    Liu, H.; Chen, J.; Weidner, D.; Hu, J.; Meng, Y.; Mao, H.

    2003-12-01

    The neighborite (NaMgF3) is an ideal analogue model for silicate perovskite (MgSiO3) due to the similarities between their crystal and electronic structures. The advantage of the analogue study is that the weaker bonding feature of neighborite grants us the opportunity to simulate behavior of silicate perovskite at lower mantlei. e.high pressure and high temperature condition, at relatively lower P-T conditions. The previous high pressure studies for neighborite were reported by Zhao et al [1, 2]. Energy dispersive x-ray diffraction data were achieved within 10GPa and 1000oC, while angle dispersive x-ray diffraction data were obtained only at 4.9GPa and room temperature.More information of atomic position change is required to reveal the role of MgF6 octahedral framework tilting during its phase transition process responding to heating andcompressing. Thus the high-resolution monochromatic x-ray powder diffraction studies on NaMgF3 perovskite at high pressure were carried out using diamond anvil cell at X17C of National Synchrotron Light Source (Brookhaven) and HPCAT of Advance Photon Source (Argonne). The orthorhombic structure keeps stable under pressure up to 30 GPa, and the crystal structure is refined using Rietveld method. The result indicates that tilting angle of the MgF6 octahedral framework increases continually while the octahedral Mg-F bond length decreases slightly with increasing pressure.Difference between the tilting angles derived from macro-structure (lattice parameters) and from micro-structure (atomic positions), as well as the trend of change in the tilting angle with temperature and pressureare discussed. [1]. Zhao YS, Weidner DJ, Ko JD, Leinenweber K, Liu X, Li BS, Meng Y,Pacalo REG, Vaughan MT, Wang YB, Yeganehhaeri A,J.Geophys. Res. Solid Earth, 99 (1994) 2871. [2]. Zhao YS, Parise JB, Wang YB, Kusaba K, Vaughan MT, Weidner DJ, Kikegawa T, Chen J, Shimomura O,Am.Miner., 79 (1994) 615.

  15. Synchrotron x-ray and electron micro-probe study of contaminated dredged sediments.

    NASA Astrophysics Data System (ADS)

    Poitevin, A.; Lerouge, C.; Wille, G.; Bataillard, P.; Hennet, L.

    2012-04-01

    Sediments originating from periodic dredging of waterways were traditionally disposed of in storage sites without any precautions or treatments. There may be some environmental concerns especially when the dredged material comes from historically contaminated areas such as the North French coal basin. This study aims to characterize the metal mobility (mainly Zn and Pb) in deposited dredged sediments by combining chemical and spectroscopic techniques. The sediments consist of a silty fraction (~ 40 %: dominant quartz, minor feldspar), carbonates and a clay fraction (illite dominant, illite-smectite mixed layer, kaolinite). This mineralogical heterogeneity and the observed grain-size distribution (70 to 80 % wt of the total sediment is <50µm) lead to a need to use microbeam techniques to identify Zn and Pb carriers. Electron probe micro-analyse (EPMA) combined with microbeam x-ray fluorescence (µXRF) at Synchrotron sources were used to identify Zn and Pb carriers. In particular Zn and Pb distributions in thin-section samples were determined by µ-XRF elemental mappings. EPMA was used to determine the distribution of light elements for which the energy of the emission lines is below 4 keV (Si, S, P…). The presence of reduced (sulphides) and oxidized (sulphates, oxihydroxides) phases strongly suggests that the redox state is one of the major parameters controlling the metal mobility. Therefore x-ray absorption spectroscopy experiments were also performed to study the oxidation state in both bulk samples and on selected regions of interest in thin section samples. Preliminary chemical analyses In this work, the potential effects of the sample preparation on phase's structure and redox state were also studied and will be presented. In particular measurements using x-ray absorption spectroscopy were carried out on air dried or lyophilised powders and on samples stored in a cryogenic environment after sampling. For the latter, we studied the evolution of the iron

  16. Examining the Microstructural location of Bromide in Arctic and Antarctic Sea Ice Using Synchrotron X-Ray Microfluorescence

    NASA Astrophysics Data System (ADS)

    Lieb-Lappen, R.; Obbard, R. W.

    2013-12-01

    In a changing climate, it is critical to have a full understanding of the different chemical and physical processes governing ice, ocean, and atmosphere interactions. Polar tropospheric ozone depletion events (ODE) are strongly correlated with increased tropospheric concentrations of reactive bromine gases (BrO and Br) (Friess et al. 2004; Simpson et al. 2005), however the mechanism by which Br enters the atmosphere is not well understood. Sea ice plays a critical role in mediating the exchange of heat, gases, and chemical species across the ocean-atmosphere interface. Using synchrotron x-ray fluorescence at Argonne National Laboratory's Advanced Photon Source (APS), we examined the microstructural location of bromide in Arctic and Antarctic sea ice. In particular, we aimed to determine whether Br is found solely in brine channels and at grain boundaries or exists ubiquitously throughout the crystal lattice of ice. Further, we also investigated the spatial distribution of Br in the sea ice column and the presence of Br in both snow lying on and blowing across the sea ice surface. For this first presentation of synchrotron X-ray fluorescence detection of Br in sea ice, we compare results from a single sea ice core retrieved from Barrow, Alaska with data from multiple cores collected from the Ross Sea, Antarctica, including both first-year and multi-year ice. Cores were cut into 0.5 cm-thick slices approximately every ten cm along the length of the core. At APS, a 2 mm x 2 mm region of each sample was scanned by an 18 kV X-ray beam and the resulting fluorescence signal detected using a four-element silicon drift detector. This yielded two-dimensional elemental maps of Br with ten micron resolution. Image processing and analysis techniques for the quantification of the Br distribution are presented. This data will be key as we continue to better understand the full transport of Br from the ocean, through the sea ice, and then into the boundary layer.

  17. A Versatile Hemispherical Great Area X-ray Detector for Synchrotron Radiation

    SciTech Connect

    Figueroa, Rodolfo; Belmar, Felipe

    2009-01-29

    This work presents an X-ray detector with fullerene C60 semi spherical geometry constituted by a set of small cylindrical proportional counter units with needles anodes, which are located in the surface of an hemispherical plastic support. The sample to be analyzed is placed on the center of the hemisphere base. The radiation may enter by one of its flanks or through the hemisphere top. The hemispherical zone that exists between the holder sample base and the proportional counters can be vacuumed, aired or filled with counter gas.

  18. X-ray fluorescence from rough rocky surfaces of asteroids

    NASA Astrophysics Data System (ADS)

    Okada, T.

    2014-07-01

    X-ray fluorescence (XRF) from orbit is a frequently-used technique to determine the elemental composition of atmosphereless planetary bodies. So far, XRF observations have been conducted for asteroids by the Near-Earth Asteroid Rendezvous Shoemaker mission at (433) Eros [1] and the Hayabusa mission at (25143) Itokawa [2]. There has been difficulties to interpret the XRF data to derive the composition quantitatively. One of the reasons is the surface-roughness effect. We have investigated the XRF intensity influenced by a powdery surface as an analogue to fine regolith [3,4]. However, the surfaces of asteroids explored by the spacecraft at, e.g., (25143) Itokawa or (433) Eros, were not always covered with fine regolith but with pebbles or boulders. Thus, we have performed laboratory experiments to study the roughness effect for rocky surfaces to interpret the XRF observations of those asteroids and the observations of future missions. For the powdery surface, we have obtained the following results: 1) the XRF with lower energy is more effective for the same roughness; 2) the XRF intensity decreases for rougher surfaces but converges to a constant value almost 50--60 % of that of a flat surface; and 3) the XRF intensity decreases for larger phase angles, but does not change so for a varying incident angle when when the phase angle remains fixed. We started the experiments for rocky surfaces to investigate the elemental composition of natural unprepared rocks as well as ground rocks for past and future planetary missions. We prepared the basaltic rock samples with different surface roughness. The roughness of the rock surface is measured with a laser microscope to obtain the three-dimensional surface features and characterize the roughness in <10, 30, 60, 100-micron scales by a rectangular function as in our previous studies. We used the X-ray generator (RIGAKU RINT-2000) using an X-ray tube of Cr-target (V-filter) at 20 kV and 10mA, and detected with the Si-PIN diode

  19. Non-invasive airway health measurement using synchrotron x-ray microscopy of high refractive index glass microbeads

    NASA Astrophysics Data System (ADS)

    Donnelley, Martin; Morgan, Kaye; Farrow, Nigel; Siu, Karen; Parsons, David

    2016-01-01

    Cystic fibrosis (CF) is caused by a gene defect that compromises the ability of the mucociliary transit (MCT) system to clear the airways of debris and pathogens. To directly characterise airway health and the effects of treatments we have developed a synchrotron X-ray microscopy method that non-invasively measures the local rate and patterns of MCT behaviour. Although the nasal airways of CF mice exhibit the CF pathophysiology, there is evidence that nasal MCT is not altered in CF mice1. The aim of this experiment was to determine if our non-invasive local airway health assessment method could identify differences in nasal MCT rate between normal and CF mice, information that is potentially lost in bulk MCT measurements. Experiments were performed on the BL20XU beamline at the SPring-8 Synchrotron in Japan. Mice were anaesthetized, a small quantity of micron-sized marker particles were delivered to the nose, and images of the nasal airways were acquired for 15 minutes. The nasal airways were treated with hypertonic saline or mannitol to increase surface hydration and MCT. Custom software was used to locate and track particles and calculate individual and bulk MCT rates. No statistically significant differences in MCT rate were found between normal and CF mouse nasal airways or between treatments. However, we hope that the improved sensitivity provided by this technique will accelerate the ability to identify useful CF lung disease-modifying interventions in small animal models, and enhance the development and efficacy of proposed new therapies.

  20. MeV per nucleon ion irradiation of nuclear materials with high energy synchrotron X-ray characterization

    NASA Astrophysics Data System (ADS)

    Pellin, M. J.; Yacout, Abdellatif M.; Mo, Kun; Almer, Jonathan; Bhattacharya, S.; Mohamed, Walid; Seidman, D.; Ye, Bei; Yun, D.; Xu, Ruqing; Zhu, Shaofei

    2016-04-01

    The combination of MeV/Nucleon ion irradiation (e.g. 133 MeV Xe) and high energy synchrotron x-ray characterization (e.g. at the Argonne Advanced Photon Source, APS) provides a powerful characterization method to understand radiation effects and to rapidly screen materials for the nuclear reactor environment. Ions in this energy range penetrate ∼10 μm into materials. Over this range, the physical interactions vary (electronic stopping, nuclear stopping and added interstitials). Spatially specific x-ray (and TEM and nanoindentation) analysis allow individual quantification of these various effects. Hard x-rays provide the penetration depth needed to analyze even nuclear fuels. Here, this combination of synchrotron x-ray and MeV/Nucleon ion irradiation is demonstrated on U-Mo fuels. A preliminary look at HT-9 steels is also presented. We suggest that a hard x-ray facility with in situ MeV/nucleon irradiation capability would substantially accelerate the rate of discovery for extreme materials.

  1. Synchrotron X-ray Applications Toward an Understanding of Elastic Anisotropy

    NASA Astrophysics Data System (ADS)

    Kanitpanyacharoen, Waruntorn

    The contribution of this dissertation is to expand the current knowledge of factors and mechanisms that influence the development of preferred orientation of minerlas and pores in different materials, ranging from rocks in Earth's crust to minerals in the deep Earth. Preferred orientation--a main contributing component to elastic anisotropy--is however very challenging to quantify. The overall focus of this thesis thus aims to (1) apply the capabilities of synchrotron X-ray techniques to determine preferred orientations of hexagonal metals and shales under different conditions and (2) enhance our understanding of their relationships to the elastic properties. Lattice preferred orientation (LPO) or 'texture' of hexagonal close-packed iron (hcp- Fe) crystals during deformation has been suggested as the cause of the elastic anisotropy observed in Earth's inner core. However, relatively little is known about LPO of other hcp metals. An investigation of a wide range of hcp metals (Cd, Zn, Os, and Hf) as analogs to hcp-Fe was thus undertaken to better understand deformation mechanisms at high pressure and temperature in Chapter 2. Results show that all hcp metals preferentially align their c-axes near the compression axis during deformation but with considerable differences. The gradual texture evolution in Cd and Zn is mainly controlled by basal slip systems while a rapid texture development in Os and Hf at ambient temperature is due to a dominant role of tensile twinning, with some degree of basal slip. At elevated temperature, tensile twinning is suppressed and texturing is governed by combined basal and prismatic slip. Under all conditions, basal slip appears to be the main deformation mechanism in hcp metals at high pressure and temperature. These findings are similar to those of hcp-Fe and useful to better understand the deformation mechanisms of hcp metals and their implications for elastic anisotropy. In Chapter 3, a high-energy synchrotron X-ray diffraction

  2. Synchrotron x-ray high energy PDF and tomography studies for gallium melts under high-pressure conditions

    NASA Astrophysics Data System (ADS)

    Liu, H.; Liu, L. L.; Li, R.; Li, L.

    2015-12-01

    Liquid gallium exhibits unusual and unique physical properties. A rich polymorphism and metastable modifications of solid Ga have been discovered and a number of studies of liquid gallium under high pressure conditions were reported. However, some fundamental properties, such as the equation of state (EoS) of Ga melt under extreme conditions remain unclear. To compare to the previous reports, we performed the pair distribution function (PDF) study using diamond anvil cell, in which synchrotron high-energy x-ray total scattering data, combined with reverse Monte Carlo simulation, was used to study the microstructure and EoS of liquid gallium under high pressure at room temperature conditions. The EoS of Ga melt, which was measured from synchrotron x-ray tomography method at room temperature, was used to avoid the potential relatively big errors for the density estimation from the reverse Monte Carlo simulation with the mathematical fit to the measured structure factor data. The volume change of liquid gallium have been studied as a function of pressure and temperature up to 5 GPa at 370 K using synchrotron x-ray microtomography combined with energy dispersive x-ray diffraction (EDXRD) techniques using Drickamer press. The directly measured P-V-T curves were obtained from 3D tomography reconstruction data. The existence of possible liquid-liquid phase transition regions is proposed based on the abnormal compressibility and local structure change in Ga melts.

  3. Correlating Fischer-Tropsch activity to Ru nanoparticle surface structure as probed by high-energy X-ray diffraction.

    PubMed

    Quek, Xian-Yang; Filot, Ivo A W; Pestman, Robert; van Santen, Rutger A; Petkov, Valeri; Hensen, Emiel J M

    2014-06-01

    Synchrotron X-ray diffraction coupled to atomic pair distribution function analysis and Reverse Monte Carlo simulations is used to determine the atomic-scale structure of Ru nanoparticle catalysts for the Fischer-Tropsch reaction. The rate of CO hydrogenation strongly correlates with the abundance of surface atoms with coordination numbers of 10 and 11. DFT calculations confirm that CO dissociation proceeds with a low barrier on these Ru surface atom ensembles. PMID:24763733

  4. From synchrotron radiation to lab source: advanced speckle-based X-ray imaging using abrasive paper

    PubMed Central

    Wang, Hongchang; Kashyap, Yogesh; Sawhney, Kawal

    2016-01-01

    X-ray phase and dark-field imaging techniques provide complementary and inaccessible information compared to conventional X-ray absorption or visible light imaging. However, such methods typically require sophisticated experimental apparatus or X-ray beams with specific properties. Recently, an X-ray speckle-based technique has shown great potential for X-ray phase and dark-field imaging using a simple experimental arrangement. However, it still suffers from either poor resolution or the time consuming process of collecting a large number of images. To overcome these limitations, in this report we demonstrate that absorption, dark-field, phase contrast, and two orthogonal differential phase contrast images can simultaneously be generated by scanning a piece of abrasive paper in only one direction. We propose a novel theoretical approach to quantitatively extract the above five images by utilising the remarkable properties of speckles. Importantly, the technique has been extended from a synchrotron light source to utilise a lab-based microfocus X-ray source and flat panel detector. Removing the need to raster the optics in two directions significantly reduces the acquisition time and absorbed dose, which can be of vital importance for many biological samples. This new imaging method could potentially provide a breakthrough for numerous practical imaging applications in biomedical research and materials science. PMID:26847921

  5. From synchrotron radiation to lab source: advanced speckle-based X-ray imaging using abrasive paper

    NASA Astrophysics Data System (ADS)

    Wang, Hongchang; Kashyap, Yogesh; Sawhney, Kawal

    2016-02-01

    X-ray phase and dark-field imaging techniques provide complementary and inaccessible information compared to conventional X-ray absorption or visible light imaging. However, such methods typically require sophisticated experimental apparatus or X-ray beams with specific properties. Recently, an X-ray speckle-based technique has shown great potential for X-ray phase and dark-field imaging using a simple experimental arrangement. However, it still suffers from either poor resolution or the time consuming process of collecting a large number of images. To overcome these limitations, in this report we demonstrate that absorption, dark-field, phase contrast, and two orthogonal differential phase contrast images can simultaneously be generated by scanning a piece of abrasive paper in only one direction. We propose a novel theoretical approach to quantitatively extract the above five images by utilising the remarkable properties of speckles. Importantly, the technique has been extended from a synchrotron light source to utilise a lab-based microfocus X-ray source and flat panel detector. Removing the need to raster the optics in two directions significantly reduces the acquisition time and absorbed dose, which can be of vital importance for many biological samples. This new imaging method could potentially provide a breakthrough for numerous practical imaging applications in biomedical research and materials science.

  6. Synchrotron x-ray fluorescence microprobe: Quantification and mapping of mixed valence state samples using micro-XANES

    SciTech Connect

    Sutton, S.R. ); Bajt, S. Department of Applied Science, Brookhaven National Laboratory, Upton, New York 11973 ); Delaney, J. ); Schulze, D. ); Tokunaga, T. )

    1995-02-01

    The synchrotron x-ray fluorescence microprobe is a valuable instrument for quantification and mapping of mixed valence state samples with high spatial resolution and elemental sensitivity. A method has been developed for quantifying the proportions of Fe[sup 2+] and Fe[sup 3+] with 100 [mu]m spatial resolution and better than 100 ppm sensitivity using x-ray absorption near-edge structure (XANES). Applications of valence state mapping have been made to selenium in water-saturated sediments and manganese associated with wheat roots attacked by the take-all fungus.

  7. Multi-Scaled Microstructures in Natural Rubber Characterized by Synchrotron X-ray Scattering and Optical Microscopy

    SciTech Connect

    Toki , S.; Hsiao, B; Amnuaypornsri , S; Sakdapipanich, J; Tanaka, Y

    2008-01-01

    Multi-scaled microstructures induced by natural impurities (i.e., proteins, phospholipids, carbohydrates) in natural rubber (NR) were investigated by synchrotron small-angle X-ray scattering (SAXS), wide-angle X-ray diffraction (WAXD), and optical microscopy using several kinds of untreated and chemically treated un-vulcanized samples. These microstructures include large aggregates (size less than 50 m), well-defined crystals (size less than a few 10 m), and micelles (size much less than 10 m). In un-vulcanized NR samples, even though the concentrations of natural impurities are relatively low, the dispersion of these microstructures significantly affects the mechanical properties

  8. Correlated diffuse x-ray scattering from periodically nanostructured surfaces

    NASA Astrophysics Data System (ADS)

    Soltwisch, V.; Haase, A.; Wernecke, J.; Probst, J.; Schoengen, M.; Burger, S.; Krumrey, M.; Scholze, F.

    2016-07-01

    Laterally periodic nanostructures were investigated with grazing incidence small angle x-ray scattering. To support an improved reconstruction of nanostructured surface geometries, we investigated the origin of the contributions to the diffuse scattering pattern which is correlated to the surface roughness. Resonant diffuse scattering leads to a palmlike structure of intensity sheets. Dynamic scattering generates the so-called Yoneda band caused by a resonant scatter enhancement at the critical angle of total reflection and higher-order Yoneda bands originating from a subsequent diffraction of the Yoneda enhanced scattering at the grating. Our explanations are supported by modeling using a solver for the time-harmonic Maxwell's equations based on the finite-element method.

  9. Synchrotron-based transmission x-ray microscopy for improved extraction in shale during hydraulic fracturing

    NASA Astrophysics Data System (ADS)

    Kiss, Andrew M.; Jew, Adam D.; Joe-Wong, Claresta; Maher, Kate M.; Liu, Yijin; Brown, Gordon E.; Bargar, John

    2015-09-01

    Engineering topics which span a range of length and time scales present a unique challenge to researchers. Hydraulic fracturing (fracking) of oil shales is one of these challenges and provides an opportunity to use multiple research tools to thoroughly investigate a topic. Currently, the extraction efficiency from the shale is low but can be improved by carefully studying the processes at the micro- and nano-scale. Fracking fluid induces chemical changes in the shale which can have significant effects on the microstructure morphology, permeability, and chemical composition. These phenomena occur at different length and time scales which require different instrumentation to properly study. Using synchrotron-based techniques such as fluorescence tomography provide high sensitivity elemental mapping and an in situ micro-tomography system records morphological changes with time. In addition, the transmission X-ray microscope (TXM) at the Stanford Synchrotron Radiation Lightsource (SSRL) beamline 6-2 is utilized to collect a nano-scale three-dimensional representation of the sample morphology with elemental and chemical sensitivity. We present the study of a simplified model system, in which pyrite and quartz particles are mixed and exposed to oxidizing solution, to establish the basic understanding of the more complex geology-relevant oxidation reaction. The spatial distribution of the production of the oxidation reaction, ferrihydrite, is retrieved via full-field XANES tomography showing the reaction pathway. Further correlation between the high resolution TXM data and the high sensitivity micro-probe data provides insight into potential morphology changes which can decrease permeability and limit hydrocarbon recovery.

  10. Human thyroid specimen imaging by fluorescent x-ray computed tomography with synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Takeda, Tohoru; Yu, Quanwen; Yashiro, Toru; Yuasa, Tetsuya; Hasegawa, Yasuo; Itai, Yuji; Akatsuka, Takao

    1999-09-01

    Fluorescent x-ray computed tomography (FXCT) is being developed to detect non-radioactive contrast materials in living specimens. The FXCT system consists of a silicon (111) channel cut monochromator, an x-ray slit and a collimator for fluorescent x ray detection, a scanning table for the target organ and an x-ray detector for fluorescent x-ray and transmission x-ray. To reduce Compton scattering overlapped on the fluorescent K(alpha) line, incident monochromatic x-ray was set at 37 keV. The FXCT clearly imaged a human thyroid gland and iodine content was estimated quantitatively. In a case of hyperthyroidism, the two-dimensional distribution of iodine content was not uniform, and thyroid cancer had a small amount of iodine. FXCT can be used to detect iodine within thyroid gland quantitatively and to delineate its distribution.

  11. Indentation Size Effects in Single Crystal Copper as Revealed by Synchrotron X-ray Microdiffraction

    SciTech Connect

    Feng, G.; Budiman, A. S.; Nix, W. D.; Tamura, N.; Patel, J. R.

    2007-11-19

    The indentation size effect (ISE) has been observed in numerous nanoindentation studies on crystalline materials; it is found that the hardness increases dramatically with decreasing indentation size - a 'smaller is stronger' phenomenon. Some have attributed the ISE to the existence of strain gradients and the geometrically necessary dislocations (GNDs). Since the GND density is directly related to the local lattice curvature, the Scanning X-ray Microdiffraction ({mu}SXRD) technique, which can quantitatively measure relative lattice rotations through the streaking of Laue diffractions, can used to study the strain gradients. The synchrotron {mu}SXRD technique we use - which was developed at the Advanced Light Source (ALS), Berkeley Lab - allows for probing the local plastic behavior of crystals with sub-micrometer resolution. Using this technique, we studied the local plasticity for indentations of different depths in a Cu single crystal. Broadening of Laue diffractions (streaking) was observed, showing local crystal lattice rotation due to the indentation-induced plastic deformation. A quantitative analysis of the streaking allows us to estimate the average GND density in the indentation plastic zones. The size dependence of the hardness, as found by nanoindentation, will be described, and its correlation to the observed lattice rotations will be discussed.

  12. Classification of lead white pigments using synchrotron radiation micro X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Welcomme, E.; Walter, P.; Bleuet, P.; Hodeau, J.-L.; Dooryhee, E.; Martinetto, P.; Menu, M.

    2007-12-01

    Lead white pigment was used and synthesised for cosmetic and artistic purposes since the antiquity. Ancient texts describe the various recipes, and preparation processes as well as locations of production. In this study, we describe the results achieved on several paint samples taken from Matthias Grünewald’s works. Grünewald, who was active between 1503 and 1524, was a major painter at the beginning of the German Renaissance. Thanks to X-ray diffraction analysis using synchrotron radiation, it is possible to associate the composition of the paint samples with the masters ancient recipes. Different approaches were used, in reflection and transmission modes, directly on minute samples or on paint cross-sections embedded in resin. Characterisation of lead white pigments reveals variations in terms of composition, graininess and proportion of mineral phases. The present work enlightens the presence of lead white as differentiable main composition groups, which could be specific of a period, a know-how or a geographical origin. In this way, we aim at understanding the choices and the trading of pigments used to realise paintings during northern European Renaissance.

  13. Applications of pixellated GaAs X-ray detectors in a synchrotron radiation beam

    NASA Astrophysics Data System (ADS)

    Watt, J.; Bates, R.; Campbell, M.; Mathieson, K.; Mikulec, B.; O'Shea, V.; Passmore, M.-S.; Schwarz, C.; Smith, K. M.; Whitehill, C.; XIMAGE Project

    2001-03-01

    Hybrid semiconductor pixel detectors are being investigated as imaging devices for radiography and synchrotron radiation beam applications. Based on previous work in the CERN RD19 and the UK IMPACT collaborations, a photon counting GaAs pixel detector (PCD) has been used in an X-ray powder diffraction experiment. The device consists of a 200 μm thick SI-LEC GaAs detector patterned in a 64×64 array of 170 μm pitch square pixels, bump-bonded to readout electronics operating in single photon counting mode. Intensity peaks in the powder diffraction pattern of KNbO 3 have been resolved and compared with results using the standard scintillator, and a PCD predecessor (the Ω3). The PCD shows improved speed, dynamic range, 2-D information and comparable spatial resolution to the standard scintillator based systems. It also overcomes the severe dead time limitations of the Ω3 by using a shutter based acquisition mode. A brief demonstration of the possibilities of the system for dental radiography and image processing are given, showing a marked reduction in patient dose and dead time compared with film.

  14. Growth dynamics of pentacene thin films: Real-time synchrotron x-ray scattering study

    SciTech Connect

    Mayer, Alex C.; Ruiz, Ricardo; Malliaras, George G.; Zhou, Hua; Headrick, Randall L.; Kazimirov, Alexander

    2006-05-15

    Real-time synchrotron x-ray scattering in the anti-Bragg configuration was used to monitor the dynamics of pentacene film growth on inert substrates. A distributed-growth model, according to which pentacene molecules adsorbed on the nth layer can either nucleate and contribute to the growth of the (n+1)th layer or transfer downward and contribute to the growth of the nth layer, gave a good description of the data. For molecules adsorbed on the first and second layers, the probability of downward transfer was found to be dependent on the substrate, and independent of temperature within the range from 25 to 60 deg. C. For films grown on SiO{sub 2}, an Ehrlich-Schwoebel barrier of the order of 70 meV dominated downward transfer of pentacene molecules in layers away from the substrate. For films grown on an alkylated self-assembled monolayer, significant desorption of pentacene molecules from the substrate at elevated temperatures forced the growth mode toward the three-dimensional limit.

  15. Guiding synchrotron X-ray diffraction by multimodal video-rate protein crystal imaging.

    PubMed

    Newman, Justin A; Zhang, Shijie; Sullivan, Shane Z; Dow, Ximeng Y; Becker, Michael; Sheedlo, Michael J; Stepanov, Sergey; Carlsen, Mark S; Everly, R Michael; Das, Chittaranjan; Fischetti, Robert F; Simpson, Garth J

    2016-07-01

    Synchronous digitization, in which an optical sensor is probed synchronously with the firing of an ultrafast laser, was integrated into an optical imaging station for macromolecular crystal positioning prior to synchrotron X-ray diffraction. Using the synchronous digitization instrument, second-harmonic generation, two-photon-excited fluorescence and bright field by laser transmittance were all acquired simultaneously with perfect image registry at up to video-rate (15 frames s(-1)). A simple change in the incident wavelength enabled simultaneous imaging by two-photon-excited ultraviolet fluorescence, one-photon-excited visible fluorescence and laser transmittance. Development of an analytical model for the signal-to-noise enhancement afforded by synchronous digitization suggests a 15.6-fold improvement over previous photon-counting techniques. This improvement in turn allowed acquisition on nearly an order of magnitude more pixels than the preceding generation of instrumentation and reductions of well over an order of magnitude in image acquisition times. These improvements have allowed detection of protein crystals on the order of 1 µm in thickness under cryogenic conditions in the beamline. These capabilities are well suited to support serial crystallography of crystals approaching 1 µm or less in dimension. PMID:27359145

  16. Thermal equation-of-state of TiC: a synchrotron x-ray diffraction study

    SciTech Connect

    Yu, Xiaohui; Lin, Zhijun; Zhang, Jianzhong; Zhao, Yusheng; Wang, Liping; Ding, Zejun; Jin, Changqing

    2009-01-01

    The pressure (P)-volume (V)-temperature (T) measurements were carried out for titanium carbide at pressures and temperatures up to 8.1 GPa and 1273 K using energy-dispersive synchrotron x-ray diffraction. Thermoelastic parameters were derived for TiC based on a modified high-temperature Birch-Murnaghan equation of state and a thermal-pressure approach. With the pressure derivative of the bulk modulus, K'{sub 0}, fixed at 4.0, we obtain: the ambient bulk modulus K{sub 0} = 268(6) GPa, temperature derivative of bulk modulus at constant pressure ({partial_derivative}K{sub T}/{partial_derivative}T){sub p} = -0.026(9) GPa K{sup -1}, volumetric thermal expansivity a{sub T}(K{sup -1}) = a + bT with a = 1.62(12) x 10{sup -5} K{sup -1} and b = 1.07(17) x 10{sup -8} K{sup -2}, pressure derivative of thermal expansion ({partial_derivative}a/{partial_derivative}P){sub T} = (-3.62 {+-} 1.14) x 10{sup -7} GPa{sup -1} K{sup -1}, and temperature derivative of bulk modulus at constant volume ({partial_derivative}K{sub T}/{partial_derivative}T){sub v} = -0.015 (8) GPa K{sup -1}. These results provide fundamental thermo physical properties for TiC and are important to theoretical and computational modeling of transition metal carbides.

  17. Biomimetic growth of calcium oxalate crystals: synchrotron X-ray studies

    NASA Astrophysics Data System (ADS)

    Uysal, Ahmet; Stripe, Benjamin; Dutta, Pulak

    2010-03-01

    Oriented crystals of calcium oxalate monohydrate (COM) form one of the major constituents of kidney stones in humans, and these crystals are also found in many plants. It is widely accepted that an organic matrix of lipids and proteins is involved in the crystallization of COM, though their role is not well-understood [1]. Langmuir monolayers of lipids on supersaturated aqueous solutions can be used to mimic the lipid-crystal interface during mineralization. We have studied nucleation and growth of COM crystals under heneicosanoic acid monolayers at the air-water interface. We used synchrotron x-rays in the grazing incidence geometry to determine the structure of the organic monolayer and the orientation of COM crystals in-situ during crystallization. We see that the (-101) faces of COM crystals are parallel to the organic matrix. There is a commensurate relationship between the heneicosanoic acid monolayer and the (-101) crystal face that may be responsible from the oriented growth. Evolution of the monolayer structure with time will be described. [1]S. R. Khan, Calcium Oxalate in Biological Systems, CRC Press, Boca Raton, 1995

  18. Solving mercury (Hg) speciation in soil samples by synchrotron X-ray microspectroscopic techniques.

    PubMed

    Terzano, Roberto; Santoro, Anna; Spagnuolo, Matteo; Vekemans, Bart; Medici, Luca; Janssens, Koen; Göttlicher, Jörg; Denecke, Melissa A; Mangold, Stefan; Ruggiero, Pacifico

    2010-08-01

    Direct mercury (Hg) speciation was assessed for soil samples with a Hg concentration ranging from 7 up to 240 mg kg(-1). Hg chemical forms were identified and quantified by sequential extractions and bulk- and micro-analytical techniques exploiting synchrotron generated X-rays. In particular, microspectroscopic techniques such as mu-XRF, mu-XRD and mu-XANES were necessary to solve bulk Hg speciation, in both soil fractions <2 mm and <2 microm. The main Hg-species found in the soil samples were metacinnabar (beta-HgS), cinnabar (alpha-HgS), corderoite (Hg(3)S(2)Cl(2)), and an amorphous phase containing Hg bound to chlorine and sulfur. The amount of metacinnabar and amorphous phases increased in the fraction <2 microm. No interaction among Hg-species and soil components was observed. All the observed Hg-species originated from the slow weathering of an inert Hg-containing waste material (K106, U.S. EPA) dumped in the area several years ago, which is changing into a relatively more dangerous source of pollution. PMID:20605298

  19. In-situ characterization of highly reversible phase transformation by synchrotron X-ray Laue microdiffraction

    NASA Astrophysics Data System (ADS)

    Chen, Xian; Tamura, Nobumichi; MacDowell, Alastair; James, Richard D.

    2016-05-01

    The alloy Cu25Au30Zn45 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.

  20. Rainwater analysis by synchrotron radiation-total reflection X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    López, María L.; Ceppi, Sergio A.; Asar, María L.; Bürgesser, Rodrigo E.; Ávila, Eldo E.

    2015-11-01

    Total reflection X-ray fluorescence analysis excited with synchrotron radiation was used to quantify the elemental concentration of rainwater in Córdoba, Argentina. Standard solutions with gallium as internal standard were prepared for the calibration curves. Rainwater samples of 5 μl were added to an acrylic reflector, allowed to dry, and analyzed for 200 s measuring time. The elemental concentrations of As, Ca, Co, Cr, Cu, Fe, K, Mn, Ni, Pb, S, Sr, V, and Zn were determined. The electrical conductivity, pH, and elemental concentrations were compared to data previously reported for the soluble fraction of rainwater at different sites. A factor analysis was performed in order to determine the sources that contributed to the elemental concentration in rainwater. Anthropogenic sources were identified as traffic pollution, vehicular emissions, and metallurgical factories. The quality of rainwater was analyzed by comparing the concentrations of all the elements in rainwater samples with the WHO guideline values for drinking water. The results show the need to control the atmospheric emissions in order to preserve the quality of rainwater. SR-TXRF analysis of chemical composition of rainwater in Córdoba represents the very first contribution in the region to the knowledge of the concentration of trace metals in the soluble fraction of rainwater. These data are scarce, especially in the Southern Hemisphere.

  1. Synchrotron radiation X-ray micro-fluorescence: Protocol to study mesenchymal stem cells.

    PubMed

    Rezende, Karla Mayra; Bönecker, Marcelo; Perez, Carlos Alberto; Mantesso, Andrea

    2016-03-01

    The micro-X-ray fluorescence by synchrotron radiation (μ-XRF) is a method to determine the composition of tissues without destroying the samples. However, this technique has never been used for the analysis of mesenchymal stem cells (MSC). This study compared different protocols for fixing, storing, preserving, and establishing the correct numbers of dental derived MSC submitted to μ-XRF analysis. Stem cells were obtained from human dental tissue. After cell expansion, and MACS isolation, the samples were fixed and the following quantities of cells 1 × 10(4) to 1 × 10(7) were divided in two groups: G1: fixed in 4% paraformaldehyde diluted in phosphate-buffered saline solution, and G2: fixed in 4% paraformaldehyde diluted in MilliQ water. The G1 cells showed precipitation of chemical components from the solution resulting in the formation of salt crystals while G2 cells were clear and almost transparent in the sample holder. With regards to cells concentration, the best results occurred when four droplets of 1 × 10(7) cells were analyzed. This work shows that to identify and study the distribution of trace elements in MSC by μ-XRF, the best protocol is fixation in 4% paraformaldehyde diluted with MilliQ water at 4°C and a concentration of four incremental droplets of 1 × 10(7) cells. PMID:26749077

  2. Strain evolution during hydride precipitation in Zircaloy-4 observed with synchrotron X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Blackmur, M. S.; Preuss, M.; Robson, J. D.; Zanellato, O.; Cernik, R. J.; Ribeiro, F.; Andrieux, J.

    2016-06-01

    Synchrotron X-ray diffraction was used to evaluate strain evolution observed in Zircaloy-4 undergoing hydride precipitation during a range of thermal operations. During continuous heating, a change in the constraining effect of the matrix was observed at a temperature of 280 °C, thought to be the result of matrix dilatation from interstitial hydrogen. A deconvolution of the thermal, chemical and mechanical sources of strain during quench and dwell operations identified a non-negligible mechanical effect in the matrix. During these dwells, slow strain rate relaxation of elastic strains was seen in the matrix and hydride, suggesting that time dependent relaxation of misfit stresses may be possible at reactor relevant temperatures. Notable anisotropy was observed between the rolling and transverse directions, identified as being the likely product of a similar anisotropy in the relaxation of the hydride misfit between the < 11 2 bar 0>α and < 1 1 bar 00>α matrix directions, owing to the differing coherency of these two interfaces.

  3. Experimental measurement of lattice strain pole figures using synchrotron x rays

    SciTech Connect

    Miller, M.P.; Bernier, J.V.; Park, J.-S.; Kazimirov, A.

    2005-11-15

    This article describes a system for mechanically loading test specimens in situ for the determination of lattice strain pole figures and their evolution in multiphase alloys via powder diffraction. The data from these experiments provide insight into the three-dimensional mechanical response of a polycrystalline aggregate and represent an extremely powerful material model validation tool. Relatively thin (0.5 mm) iron/copper specimens were axially strained using a mechanical loading frame beyond the macroscopic yield strength of the material. The loading was halted at multiple points during the deformation to conduct a diffraction experiment using a 0.5x0.5 mm{sup 2} monochromatic (50 keV) x ray beam. Entire Debye rings of data were collected for multiple lattice planes ({l_brace}hkl{r_brace}'s) in both copper and iron using an online image plate detector. Strain pole figures were constructed by rotating the loading frame about the specimen transverse direction. Ideal powder patterns were superimposed on each image for the purpose of geometric correction. The chosen reference material was cerium (IV) oxide powder, which was spread in a thin layer on the downstream face of the specimen using petroleum jelly to prevent any mechanical coupling. Implementation of the system at the A2 experimental station at the Cornell High Energy Synchrotron Source (CHESS) is described. The diffraction moduli measured at CHESS were shown to compare favorably to in situ data from neutron-diffraction experiments conducted on the same alloys.

  4. Deformation in metallic glasses studied by synchrotron x-ray diffraction

    DOE PAGESBeta

    Dmowski, Wojciech; Egami, Takeshi; Tong, Yang

    2016-01-11

    In this study, high mechanical strength is one of the superior properties of metallic glasses which render them promising as a structural material. However, understanding the process of mechanical deformation in strongly disordered matter, such as metallic glass, is exceedingly difficult because even an effort to describe the structure qualitatively is hampered by the absence of crystalline periodicity. In spite of such challenges, we demonstrate that high-energy synchrotron X-ray diffraction measurement under stress, using a two-dimensional detector coupled with the anisotropic pair-density function (PDF) analysis, has greatly facilitated the effort of unraveling complex atomic rearrangements involved in the elastic, anelastic,more » and plastic deformation of metallic glasses. Even though PDF only provides information on the correlation between two atoms and not on many-body correlations, which are often necessary in elucidating various properties, by using stress as means of exciting the system we can garner rich information on the nature of the atomic structure and local atomic rearrangements during deformation in glasses.« less

  5. Synchrotron X-Ray Diffraction Studies of Olivine from Comet Wild 2

    NASA Technical Reports Server (NTRS)

    2008-01-01

    We have analyzed a collection of the Comet Wild 2 coma grains returned by the NASA Stardust Mission, using micro-area Laue diffraction equipment. The purpose of the diffraction experiment is to permit the structure refinement of olivine including site occupancies. In addition to the intrinsic importance of the olivine structures for revealing the thermal history of Wild 2 materials, we wish to test reports that olivine recovered after hypervelocity capture in silica aerogel has undergone a basic structural change due to capture heating [1]. The diffraction equipment placed at beam line BL- 4B1 of PF, KEK was developed with a micropinhole and an imaging plate (Fuji Co. Ltd.) using the Laue method combined with polychromatic X-ray of synchrotron radiation operated at energy of 2.5 GeV. The incident beam is limited to 1.6 m in diameter by a micropinhole set just upstream of the sample [2, 3]. It is essential to apply a microbeam to obtain diffracted intensities with high signal to noise ratios. This equipment has been successfully applied to various extraterrestrial materials, including meteorites and interplanetary dust particles [4]. The Laue pattern of the sample C2067,1,111,4 (Fig. 1) was successfully taken on an imaging plate after a 120 minute exposure (Fig. 2).

  6. Reconstruction of Elemental Distribution Images from Synchrotron Radiation X-Ray Fluorescence Spectra

    NASA Astrophysics Data System (ADS)

    Toque, Jay Arre; Ide-Ektessabi, Ari

    Synchrotron radiation X-ray fluorescence spectroscopy (SRXRF) is a powerful technique for studying trace elements in biological samples and other materials in general. Its features including capability to perform measurements in air and water, noncontact and nondestructive assay are superior to other elemental analysis techniques. In this study, a technique for reconstructing elemental distribution mapping of trace elements from spectral data was developed. The reconstruction was made possible by using the measured fluorescent signals to obtain local differences in elemental concentrations. The proposed technique features interpolation and background subtraction using matrix transformations of the spectral data to produce an enhanced distribution images. It is achieved by employing polychromatic or monochromatic color assignments proportional to the fluorescence intensities for displaying single-element or multiple-element distributions respectively. Some typical applications (i.e., macrophage and tissue surrounding an implant) were presented and the samples were imaged using the proposed method. The distribution images of the trace elements of the selected samples were used in conjunction with other analytical techniques to draw relevant observations, which cannot be achieved using conventional techniques such as metallic uptake and corresponding cellular response. The elemental distribution images produced from this study were found to have better quality compared to images produced using other analytical techniques (e.g., SIMS, PIXE, XPS, etc).

  7. Synchronizing flash-melting in a diamond cell with synchrotron X ray diffraction (XRD)

    NASA Astrophysics Data System (ADS)

    Karandikar, Amol; Boehler, Reinhard; Meng, Yue; Rod, Eric; Shen, Guoyin

    2013-06-01

    The major challenges in measuring melting temperatures in laser heated diamond cells are sample instability, thermal runaway and chemical reactions. To circumvent these problems, we developed a ``flash heating'' method using a modulated CW fiber laser and fast X ray detection capability at APS (Pilatus 1M detector). As an example, Pt spheres of 5 micron diameter were loaded in a single crystal sapphire encapsulation in the diamond cell at 65 GPa and heated in a single flash heating event for 20 ms to reach a desired temperature. A CCD spectrometer and the Pilatus were synchronized to measure the temperature and the XRD signal, respectively, when the sample reached the thermal steady state. Each successive flash heating was done at a higher temperature. The integrated XRD pattern, collected during and after (300 K) each heating, showed no chemical reaction up to 3639 K, the highest temperature reached in the experiment. Pt111 and 200 peak intensity variation showed gradual recrystalization and complete diminishing at about 3600 K, indicating melting. Thus, synchronized flash heating with novel sample encapsulation circumvents previous notorious problems and enables accurate melting temperature measurement in the diamond cell using synchrotron XRD probe. Affiliation 2: Geowissenschaeften, Goethe-Universitaet, Altenhoeferallee 1, D-60438 Frankfurt a.M., Germany.

  8. X-ray synchrotron diffraction study of natural gas hydrates from African margin

    NASA Astrophysics Data System (ADS)

    Bourry, Christophe; Charlou, Jean-Luc; Donval, Jean-Pierre; Brunelli, Michela; Focsa, Cristian; Chazallon, Bertrand

    2007-11-01

    Natural gas hydrates recovered from the Congo-Angola basin and Nigerian margins are analyzed by synchrotron X-ray powder diffraction. Biogenic methane is the most abundant gas trapped in the samples and others minor components (CO2, H2S) are co-clathrated in a type I cubic lattice structure. The refinement for the type I structure gives lattice parameters of a = 11.8646 (39) Å and a = 11.8619 (23) Å for specimens from Congo-Angola and Nigerian margins respectively at 90 K. These values, intermediate between the lattice constant of less pure methane specimens and pure artificial methane hydrates, indicate that lattice constants can be affected by the presence of encaged CO2, H2S and other gas molecules, even in small amounts. Thermal expansion is also presented for Congo-Angola hydrate in the temperature range 90-200 K. The coefficients are comparable with values reported for synthetic hydrates at low temperature and tend to approach thermal expansion of ice at higher temperature.

  9. Synchrotron radiation x-ray scattering in the early stages of in vitro collagen fibril formation

    SciTech Connect

    Suarez, G.; Oronsky, A.L.; Bordas, J.; Koch, M.H.

    1985-07-01

    The time course of in vitro collagen fibril formation was monitored by synchrotron radiation x-ray scattering. Collagen polymerization was induced by a temperature jump from 4 degrees C to 32 degrees C and the solution scattering pattern was recorded continuously with a time resolution of a few seconds. The scattered intensity increased as soon as the final temperature was attained, without discernible lag phase, when the collagen concentration was about 0.56 mg/ml, whereas turbidimetric measurements revealed a lag phase of ca. 2.5 min at 1.05 mg/ml. A direct correlation was found between the temperature and both the rate of formation and the total amount of early aggregates. The formation of these aggregates was only partially reversed by lowering the temperature, except when the collagen had been prevented from forming Schiff base-mediated intermolecular crosslinks by sodium borohydride reduction. In this case, formation of aggregates was completely reversible. The authors conclude that the aggregates that appear to correspond to the subfibrils proposed on the basis of independent methods are formed and simultaneously crosslinked in the early phases of in vitro collagen self-assembly.

  10. From Surface Down To Bulk X-Ray Channeling

    SciTech Connect

    Dabagov, Sultan B.

    2003-01-24

    The basic point to be considered in this report is that X-ray capillary optics relies on the ability of a tapered and/or bent capillary channel to act as an X-ray waveguide. Recently several coherent phenomena associated with propagation of X-rays in capillary optical elements have been observed. In order to describe coherent phenomena of radiation propagation a quantum-wave theory of X-ray channeling was developed. Simple estimations speak on possibility of X-ray channeling in nano-scale capillaries, but with a significant change in character of channeling. In this connection, discovery of carbon nanotubes opens new opportunities to apply capillary waveguide optics. X-ray propagation in capillary micro- and nanostructures within the frame of wave approach will be discussed.

  11. Surface Slope Metrology on Deformable Soft X-ray Mirrors

    SciTech Connect

    Yuan, Sheng; Yashchuk, Valeriy V.; Goldberg, Kenneth A.; Celestre, Rich; Church, Matthew; McKinney, Wayne R.; Morrison, Greg; Warwick, Tony

    2010-01-31

    We report on the current state of surface slope metrology on deformable mirrors for soft x-rays at the Advanced Light Source (ALS). While we are developing techniques for in situ at-wavelength tuning, we are refining methods of ex situ visible-light optical metrology to achieve sub-100-nrad accuracy. This paper reports on laboratory studies, measurements and tuning of a deformable test-KB mirror prior to its use. The test mirror was bent to a much different optical configuration than its original design, achieving a 0.38 micro-radian residual slope error. Modeling shows that in some cases, by including the image conjugate distance as an additional free parameter in the alignment, along with the two force couples, fourth-order tangential shape errors (the so-called bird shape) can be reduced or eliminated.

  12. Surface Slope Metrology on Deformable Soft X-ray Mirrors

    SciTech Connect

    Yuan, S.; Yashchuk, V.V.; Goldberg, K.A.; Celestre, R.; Church, M.; McKinney, W.R.; Morrison, G.; Warwick, T.

    2009-09-18

    We report on the current state of surface slope metrology on deformable mirrors for soft x-rays at the Advanced Light Source (ALS). While we are developing techniques for in situ at-wavelength tuning, we are refining methods of ex situvisible-light optical metrology to achieve sub-100-nrad accuracy. This paper reports on laboratory studies, measurements and tuning of a deformable test-KB mirror prior to its use. The test mirror was bent to a much different optical configuration than its original design, achieving a 0.38 micro-radian residual slope error. Modeling shows that in some cases, by including the image conjugate distance as an additional free parameter in the alignment, along with the two force couples, fourth-order tangential shape errors (the so-called bird shape) can be reduced or eliminated.

  13. Synchrotron X-ray Scattering from Self-organized Soft Nanostructures in Clays

    NASA Astrophysics Data System (ADS)

    Fossum, J. O.

    2009-04-01

    In the general context of self-organization of nanoparticles (in our case clay particles), and transitions in such structures, we study interconnected universal complex physical phenomena such as: (i) spontaneous gravitationally induced phase separation and nematic self-organization in systems of anisotropic clay nanoparticles in aqueous suspension, including studies of isotropic to nematic transitions [1,2] (ii) transitions from biaxial to uniaxial nematics by application of external magnetic field to self-organized systems of the same anisotropic (diamagnetic) clay nanoparticle systems [3,4] (iii) guided self-organization into chainlike structures of the same anisotropic clay nanoparticles in oil suspension when subjected to external electrical fields (electrorheological structures of polarized nanoparticles), and the stability of, and transitions of, such structures, when subjected to external mechanical stress [5,6] The experimental techniques used by us include synchrotron X-ray scattering, neutron scattering, rheometry. microscopy and magnetic resonance. We have demonstrated that clays may be used as good model systems for studies of universal physical phenomena and transitions in self-organized nanostructured soft and complex matter. Self-organization and related transitions in clay systems in particular, may have practical relevance for nano-patterning, properties of nanocomposites, and macroscopically anisotropic gels, among many other applications [7]. The synchrotron experiments have been performed at LNLS-Brazil, PLS- Korea, BNL-USA and ESRF-France. Acknowledgments: Collaborators, postdocs and students at NTNU-Norway, UiO-Norway, IFE-Norway, BNL-USA, LNLS-Brazil, UFPE-Brazil, UnB-Brazil, Univ. Amsterdam-Netherlands, Univ.Paris 7-France and other places. This research has been supported by the Research Council of Norway (RCN), through the NANOMAT, SUP and FRINAT Programs. References 1. J.O. Fossum, E. Gudding, D.d.M. Fonseca, Y. Meheust, E. DiMasi, T

  14. Advantages of a Synchrotron Bending Magnet as the Sample Illuminator for a Wide-field X-ray Microscope

    SciTech Connect

    Feser, M.; Howells, M. R.; Kirz, J.; Rudati, J.; Yun, W.

    2012-09-01

    In our paper the choice between bending magnets and insertion devices as sample illuminators for a hard X-ray full-field microscope is investigated. An optimized bending-magnet beamline design is presented. Its imaging speed is very competitive with the performance of similar microscopes installed currently at insertion-device beamlines. The fact that imaging X-ray microscopes can accept a large phase space makes them very well suited to the output characteristics of bending magnets which are often a plentiful and paid-for resource. There exist opportunities at all synchrotron light sources to take advantage of this finding to build bending-magnet beamlines that are dedicated to transmission X-ray microscope facilities. We expect that demand for such facilities will increase as three-dimensional tomography becomes routine and advanced techniques such as mosaic tomography and XANES tomography (taking three-dimensional tomograms at different energies to highlight elemental and chemical differences) become more widespread.

  15. Scanning x-ray difference microscopy and microtomography using synchrotron radiation of the storage ring VEPP-4

    NASA Astrophysics Data System (ADS)

    Borodin, Yu. I.; Dementyev, E. N.; Dragun, G. N.; Kulipanov, G. N.; Mezentsev, N. A.; Pindyurin, V. F.; Sheromov, M. A.; Skrinsky, A. N.; Sokolov, A. S.; Ushakov, V. A.

    1986-05-01

    A device designed to be employed for X-ray transmission difference microscopy and microtomography at the X-ray absorption edges of chemical elements using synchrotron radiation is described. The device comprises a double-crystal monochromator, collimator system, object scanning unit and two X-ray detection blocks based on an NaI(Tl) crystal, photomultiplier (FEU-130) and appropriate electronics. As an example of the practical application of this technique, the first results on the diagnostics of the lymph system by lymphography, i.e. the visualization of the lymph nodes previously contrasted by a Th-containing preparation, are presented. These results have been obtained at the Th L III-edge ( Eγ = 16.3 keV using difference microscopy and microtomography.

  16. National Synchrotron Light Source user`s manual: Guide to the VUV and x-ray beamlines. Fifth edition

    SciTech Connect

    Gmuer, N.F.

    1993-04-01

    The success of the National Synchrotron Light Source is based, in large part, on the size of the user community and the diversity of the scientific and technical disciplines represented by these users. As evidence of this success, the VUV Ring has just celebrated its 10th anniversary and the X-ray Ring will do the same in 1995. In order to enhance this success, the NSLS User`s Manual: Guide to the VUV and X-Ray Beamlines - Fifth Edition, is being published. This Manual presents to the scientific community-at-large the current and projected architecture, capabilities and research programs of the various VUV and X-ray beamlines. Also detailed is the research and computer equipment a General User can expect to find and use at each beamline when working at the NSLS. The Manual is updated periodically in order to keep pace with the constant changes on these beamlines.

  17. Two step formation of metal aggregates by surface X-ray radiolysis under Langmuir monolayers: 2D followed by 3D growth.

    PubMed

    Mukherjee, Smita; Fauré, Marie-Claude; Goldmann, Michel; Fontaine, Philippe

    2015-01-01

    In order to form a nanostructured metallic layer below a Langmuir monolayer, radiolysis synthesis was carried out in an adapted geometry that we call surface X-ray radiolysis. In this procedure, an X-ray beam produced by a synchrotron beamline intercepts the surface of an aqueous metal-ion solution covered by a Langmuir monolayer at an angle of incidence below the critical angle for total internal reflection. Underneath the organic layer, the X-ray beam induces the radiolytic synthesis of a nanostructured metal-organic layer whose ultrathin thickness is defined by the vertical X-ray penetration depth. We have shown that increasing the X-ray flux on the surface, which considerably enhances the kinetics of the silver layer formation, results in a second growth regime of silver nanocrystals. Here the formation of the oriented thin layer is followed by the appearance of a 3D powder of silver clusters. PMID:26734531

  18. Two step formation of metal aggregates by surface X-ray radiolysis under Langmuir monolayers: 2D followed by 3D growth

    PubMed Central

    Mukherjee, Smita; Fauré, Marie-Claude; Goldmann, Michel

    2015-01-01

    Summary In order to form a nanostructured metallic layer below a Langmuir monolayer, radiolysis synthesis was carried out in an adapted geometry that we call surface X-ray radiolysis. In this procedure, an X-ray beam produced by a synchrotron beamline intercepts the surface of an aqueous metal-ion solution covered by a Langmuir monolayer at an angle of incidence below the critical angle for total internal reflection. Underneath the organic layer, the X-ray beam induces the radiolytic synthesis of a nanostructured metal–organic layer whose ultrathin thickness is defined by the vertical X-ray penetration depth. We have shown that increasing the X-ray flux on the surface, which considerably enhances the kinetics of the silver layer formation, results in a second growth regime of silver nanocrystals. Here the formation of the oriented thin layer is followed by the appearance of a 3D powder of silver clusters. PMID:26734531

  19. In Situ X-ray Diffraction Studies of Li(sub x)Mn(sub 2)O(sub 4) Cathode Materials by Synchrotron X-ray Radiation

    SciTech Connect

    Yang, X. Q.; Sun, X.; Lee, S. J.; McBreen, J.; Mukerjee, S.; Daroux, M. L.; Xing, X. K.

    1998-11-01

    In Situ x-ray diffraction studies on Li{sub x}Mn{sub 2}O{sub 4} spinel cathode materials during charge-discharge cycles were carried out by using a synchrotron as x-ray source. Lithium rich (x = 1.03-1.06) spinel materials obtained from two different sources were studied. Three cubic phases with different lattice constants were observed during charge-discharge cycles in all the samples when a Sufficiently low charge-discharge rate (C/10) was used. There are two regions of two-phase coexistence between these three phases, indicating that both phase transitions are first order. The separation of the Bragg peaks representing these three phases varies from sample to sample and also depends on the charge-discharge rate. These results show that the de-intercalation of lithium in lithium-rich spinel cathode materials proceeds through a series of phase transitions from a lithium-rich phase to a lithium-poor phase and finally to a {lambda}-MnO{sub 2} like cubic phase, rather than through a continuous lattice constant contraction in a single phase.

  20. X-ray extended-range technique for precision measurement of the X-ray mass attenuation coefficient and Im( f) for copper using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Chantler, C. T.; Tran, C. Q.; Paterson, D.; Cookson, D.; Barnea, Z.

    2001-08-01

    We reconsider the long-standing problem of accurate measurement of atomic form factors for fundamental and applied problems. We discuss the X-ray extended-range technique for accurate measurement of the mass attenuation coefficient and the imaginary component of the atomic form factor. Novelties of this approach include the use of a synchrotron with detector normalisation, the direct calibration of dominant systematics using multiple thicknesses, and measurement over wide energy ranges with a resulting improvement of accuracies by an order of magnitude. This new technique achieves accuracies of 0.27-0.5% and reproducibility of 0.02% for attenuation of copper from 8.84 to 20 keV, compared to accuracies of 10% using atomic vapours. This precision challenges available theoretical calculations. Discrepancies of 10% between current theory and experiments can now be addressed.

  1. Study of metallic components of historical organ pipes using synchrotron radiation X-ray microfluorescence imaging and grazing incidence X-ray diffraction.

    PubMed

    Herrera, L K; Justo, A; Muñoz-Páez, A; Sans, J A; Martínez-Criado, G

    2009-12-01

    A comparative study of the composition and microstructure of two different brass alloys from reed pipes, one from a Spanish baroque organ and the other from a modern one, was carried out. This study allowed us to determine the procedure followed to produce the brass used to make ancient reed pipes. Moreover the distribution and correlation of lead and other trace elements present into the main component of the brass, the copper and zinc phases, of the historical tongues and shallots were established. This chemical composition was compared with that of a tongue from a twentieth-century organ. The whole study was accomplished using a combination of laboratory and synchrotron radiation techniques. X-ray fluorescence was the technique used to obtain elemental and chemical imaging of the main phases and the trace elements at a sub-micrometer scale. PMID:19730830

  2. Element distribution in the brain sections of rats measured by synchrotron radiation X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Liu, N. Q.; Zhang, F.; Wang, X. F.; Zhang, Z. Y.; Chai, Z. F.; Huang, Y. Y.; He, W.; Zhao, X. Q.; Zuo, A. J.; Yang, R.

    2004-02-01

    The concentration of trace elements in brain sections was measured by synchrotron radiation X-ray fluorescence. The relative concentration was calculated by means of the normalization of Compton scattering intensity approximately 22 keV, after the normalization for collecting time of X-ray spectrum and the counting of the ion chamber, and subtracting the contribution of the polycarbonate film for supporting sample. Furthermore, the statistical evaluation of the element distribution in various regions of the brain sections of the 20-day-old rats was tested. For investigating the distribution of elements in the brain of iodine deficient rats, Wistar rats were fed with iodine deficient diet and deionized water (ID group). The rats were fed the same iodine deficient diet, but drank KIO 3 solution as control (CT group). The results showed that the contents of calcium (Ca) in thalamus (TH) and copper (Cu) and iron (Fe) in cerebral cortex (CX) of ID rats were significantly lower than that of control rats, while the contents of phosphor (P), sulfur (S), potassium (K), rubidium (Rb), bromine (Br), chlorine (Cl), zinc (Zn), Ca and Cu of ID in hippocampus (H) and the contents of Br, Cl, Zn and Ca in cerebral cortex of ID rats were significantly higher. Especially, the difference of Br, Cl, Zn and Ca in H between ID and CT was more significant. The contents of all elements measured in H were higher than (or equal to) CX and/or TH for both groups, except low Cl of the control rats. Furthermore Zn and Cu contents along the hippocampal fissure in both groups were 1.5 ( P<0.001) and 0.87( P<0.03) times higher than in hippocampus, respectively. Considering the results of cluster analysis our study shows that the marked alterations in the spatial distribution of Zn and Ca of ID rats brain during brain development stages. In addition, the effect of the perfusion with 0.9% NaCl solution before taking brain on the distribution of elements in the brain sections was observed and

  3. X-ray fluorescence spectrometry using Synchrotron Radiation with applications in unmanned aircraft environmental sensing

    NASA Astrophysics Data System (ADS)

    Barberie, Sean Richard Gopal

    In this thesis I present an analytical optimization of the Synchrotron Radiation X-Ray Fluorescence (SR-XRF) technique for applications in unmanned aircraft aerosol studies. In environmental and atmospheric science, there is a pressing need for aerosol measurements at various altitudes in the atmosphere and spanning large regions. This need is currently either ignored, or met to a limited degree by studies that employ manned aircraft. There is, however, a great deal of opportunity to improve and expand on these studies using the emerging technology of unmanned aircraft systems. A newly developed aerosol sampler makes this opportunity a near-reality by its ability to collect aerosol samples in-situ from unmanned aircraft platforms. The challenge lies in analyzing these samples for elemental composition. In airborne aerosol studies, the ability to resolve where a sample was collected both spatially and temporally is limited by the sensitivity of the analysis technique. In aircraft-based aerosol collection, the length of the aerosol sample spot corresponds to distance. Thus the spatial resolution of an airborne study is limited by the amount of mass that must be collected for analysis. The SR-XRF optimizations outlined in this thesis decrease the amount of sample mass required for detectable elemental concentrations, allowing aerosol samples to be analyzed in smaller areas corresponding to smaller time steps. Since, in a flight path, time steps are directly correlated with distance, analysis of smaller time steps results in the ability to measure aerosols at higher spatial resolution. Four SR-XRF analysis configurations were experimentally tested: monochromatic beam, white beam, filtered white beam, and filtered white beam-filtered detector to determine which configuration gave the highest elemental sensitivity and selectivity. Of these tested methods, the straight polychromatic white beam configuration resulted in the best sensitivity for elements across a large

  4. In situ high-resolution X-ray photoelectron spectroscopy - Fundamental insights in surface reactions

    NASA Astrophysics Data System (ADS)

    Papp, Christian; Steinrück, Hans-Peter

    2013-11-01

    Since the advent of third generation synchrotron light sources optimized for providing soft X-rays up to 2 keV, X-ray photoelectron spectroscopy (XPS) has been developed to be an outstanding tool to study surface properties and surface reactions at an unprecedented level. The high resolution allows identifying various surface species, and for small molecules even the vibrational fine structure can be resolved in the XP spectra. The high photon flux reduces the required measuring time per spectrum to the domain of a few seconds or even less, which enables to follow surface processes in situ. Moreover, it also provides access to very small coverages down to below 0.1% of a monolayer, enabling the investigation of minority species or processes at defect sites. The photon energy can be adjusted according to the requirement of a particular experiment, i.e., to maximize or minimize the surface sensitivity or the photoionization cross-section of the substrate or the adsorbate. For a few instruments worldwide, a next step forward was taken by combining in situ high-resolution spectrometers with supersonic molecular beams. These beams allow to control and vary the kinetic and internal energies of the incident molecules and provide a local pressure of up to ~10-5 mbar, which can be switched on and off in a controllable way, thus offering a well-defined time structure to study adsorption or reaction processes.

  5. In Situ Synchrotron Based X-ray Fluorescence and Scattering Measurements During Atomic Layer Deposition: Initial Growth of HfO2 on Si and Ge Substrates

    SciTech Connect

    K Devloo-Casier; J Dendooven; K Ludwig; G Lekens; J DHaen; C Detavernier

    2011-12-31

    The initial growth of HfO{sub 2} was studied by means of synchrotron based in situ x-ray fluorescence (XRF) and grazing incidence small angle x-ray scattering (GISAXS). HfO{sub 2} was deposited by atomic layer deposition (ALD) using tetrakis(ethylmethylamino)hafnium and H{sub 2}O on both oxidized and H-terminated Si and Ge surfaces. XRF quantifies the amount of deposited material during each ALD cycle and shows an inhibition period on H-terminated substrates. No inhibition period is observed on oxidized substrates. The evolution of film roughness was monitored using GISAXS. A correlation is found between the inhibition period and the onset of surface roughness.

  6. Effect of a synchrotron X-ray microtomography imaging experiment on the amino acid content of a CM chondrite

    NASA Astrophysics Data System (ADS)

    Friedrich, Jon M.; Glavin, Daniel P.; Rivers, Mark L.; Dworkin, Jason P.

    2016-02-01

    X-ray microcomputed tomography and synchrotron X-ray microcomputed tomography (μCT) are becoming popular tools for the reconnaissance imaging of chondrites. However, there are occasional concerns that the use of μCT may be detrimental to organic components of a chondrite. Soluble organic compounds represent ~2-10% of the total solvent extractable carbon in CI and CM carbonaceous chondrites and amino acids are among the most abundant compounds in the soluble organic fraction. We irradiated two samples of the Murchison CM2 carbonaceous chondrite under conditions slightly harsher (increased beam exposure time) than those typically used for x-ray μCT imaging experiments to determine if detectable changes in the amino acid abundance and distribution relative to a nonexposed control sample occurred. After subjecting two meteorite portions to ionizing radiation dosages of 1.1 kiloGray (kGy) and 1.2 kGy with 48.6 and 46.6 keV monochromatic X-rays, respectively, we analyzed the amino acid content of each sample. Within analytical errors, we found no differences in the amino acid abundances or enantiomeric ratios when comparing the control samples (nonexposed Murchison) and the irradiated samples. We show with calculations that any sample heating due to x-ray exposure is negligible. We conclude that a monochromatic synchrotron X-ray μCT experiment at beamline 13-BM-D of the Advanced Photon Source, which imparts ~1 kGy doses, has no detectable effect on the amino acid content of a carbonaceous chondrite. These results are important for the initial reconnaissance of returned samples from the OSIRIS-REx and Hayabusa 2 asteroid sample return missions.

  7. Investigation of Essential Element Distribution in the Equine Metacarpophalangeal Joint using a Synchrotron Radiation Micro X-Ray Fluorescence Technique

    SciTech Connect

    Kaabar, Wejdan; Gundogdu, O.; Attenburrow, D.; Bradley, D. A.; Tzaphlidou, M.; Janousch, M.

    2008-05-20

    In articular cartilage, Ca, P, K and S are among some of the well known co-factors of the metalloproteinases enzymatic family, the latter playing a pivotal role in the growth and degeneration of the collagenous bone-cartilage interface of articulating joints. Current study forms part of a larger investigation concerning the distribution of these and other key elements in such media. For the purpose of evaluating these low atomic number elements (Z{<=}20), use was made of the capabilities of the LUCIA Station, located at the synchrotron facility of the Paul Scherrer Institute (PSI). Using an incident radiation energy of 4.06 keV, a synchrotron radiation micro x-ray fluorescence (SR-{mu}XRF) technique was applied in examining the distribution of the essential elements Ca, P, K and S in the bone-cartilage interface of both healthy and diseased (osteoarthritic) areas of an equine metacarpophalangeal joint. The SR-{mu}XRF mappings and line profile patterns have revealed remarkable changes in both the pattern and absolute distributions of these elements, agreeing with the findings of others. The elemental presence shown in the individual area scans encompassing the lesion each reflect the visibly abraded outer surface of the cartilage and change in shape of the bone surface. One of the area scans for the bone-cartilage interface shows a marked change in both the pattern and absolute elemental presence for all three elements compared to that observed at two other scan sites. The observation of change in bone cartilage composition around the surface of the articulating joint is thought to be novel, the variation being almost certainly due to the differing weight-bearing role of the subchondral bone at each locati0008.

  8. Investigation of Essential Element Distribution in the Equine Metacarpophalangeal Joint using a Synchrotron Radiation Micro X-Ray Fluorescence Technique

    NASA Astrophysics Data System (ADS)

    Kaabar, Wejdan; Gundogdu, O.; Tzaphlidou, M.; Janousch, M.; Attenburrow, D.; Bradley, D. A.

    2008-05-01

    In articular cartilage, Ca, P, K and S are among some of the well known co-factors of the metalloproteinases enzymatic family, the latter playing a pivotal role in the growth and degeneration of the collagenous bone-cartilage interface of articulating joints. Current study forms part of a larger investigation concerning the distribution of these and other key elements in such media. For the purpose of evaluating these low atomic number elements (Z⩽20), use was made of the capabilities of the LUCIA Station, located at the synchrotron facility of the Paul Scherrer Institute (PSI). Using an incident radiation energy of 4.06 keV, a synchrotron radiation micro x-ray fluorescence (SR-μXRF) technique was applied in examining the distribution of the essential elements Ca, P, K and S in the bone-cartilage interface of both healthy and diseased (osteoarthritic) areas of an equine metacarpophalangeal joint. The SR-μXRF mappings and line profile patterns have revealed remarkable changes in both the pattern and absolute distributions of these elements, agreeing with the findings of others. The elemental presence shown in the individual area scans encompassing the lesion each reflect the visibly abraded outer surface of the cartilage and change in shape of the bone surface. One of the area scans for the bone-cartilage interface shows a marked change in both the pattern and absolute elemental presence for all three elements compared to that observed at two other scan sites. The observation of change in bone cartilage composition around the surface of the articulating joint is thought to be novel, the variation being almost certainly due to the differing weight-bearing role of the subchondral bone at each location.

  9. Synchrotron radiation sources and condensers for projection x-ray lithography

    SciTech Connect

    Murphy, J.B.; MacDowell, A.A. ); White, D.L. ); Wood, O.R. II )

    1992-01-01

    The design requirements for a compact electron storage ring that could be used as a soft x-ray source for projection lithography are discussed. The design concepts of the x-ray optics that are required to collect and condition the radiation in divergence, uniformity and direction to properly illuminate the mask and the particular x-ray projection camera used are discussed. Preliminary designs for an entire soft x-ray projection lithography system using an electron storage ring as a soft X-ray source are presented. It is shown that by combining the existing technology of storage rings with large collection angle condensers, a powerful and reliable source of 130[Angstrom] photons for production line projection x-ray lithography is possible.

  10. Synchrotron radiation sources and condensers for projection x-ray lithography

    SciTech Connect

    Murphy, J.B.; MacDowell, A.A.; White, D.L.; Wood, O.R. II

    1992-11-01

    The design requirements for a compact electron storage ring that could be used as a soft x-ray source for projection lithography are discussed. The design concepts of the x-ray optics that are required to collect and condition the radiation in divergence, uniformity and direction to properly illuminate the mask and the particular x-ray projection camera used are discussed. Preliminary designs for an entire soft x-ray projection lithography system using an electron storage ring as a soft X-ray source are presented. It is shown that by combining the existing technology of storage rings with large collection angle condensers, a powerful and reliable source of 130{Angstrom} photons for production line projection x-ray lithography is possible.

  11. Studies of LSO:Tb radio-luminescence properties using white beam hard X-ray synchrotron irradiation

    NASA Astrophysics Data System (ADS)

    Cecilia, A.; Rack, A.; Pelliccia, D.; Douissard, P.-A.; Martin, T.; Couchaud, M.; Dupré, K.; Baumbach, T.

    A radio-luminescence set-up was installed at the synchrotron light source ANKA to characterise scintillators under the high X-ray photon flux density of white beam synchrotron radiation. The system allows for investigating the radio-luminescence spectrum of the material under study as well as analysing in situ changes of its scintillation behaviour (e.g. under heat load and/or intensive ionising radiation). In this work we applied the radio-luminescence set-up for investigating the radiation damage effects on the luminescence properties of a new kind of thin single crystal scintillator for high resolution X-ray imaging based on a layer of modified Lu2SiO5 grown by liquid phase epitaxy on a dedicated substrate within the framework of an EC project (SCINTAX).

  12. HIGH-PERFORMANCE COMPUTING FOR THE STUDY OF EARTH AND ENVIRONMENTAL SCIENCE MATERIALS USING SYNCHROTRON X-RAY COMPUTED MICROTOMOGRAPHY.

    SciTech Connect

    FENG,H.; JONES,K.W.; MCGUIGAN,M.; SMITH,G.J.; SPILETIC,J.

    2001-10-12

    Synchrotron x-ray computed microtomography (CMT) is a non-destructive method for examination of rock, soil, and other types of samples studied in the earth and environmental sciences. The high x-ray intensities of the synchrotron source make possible the acquisition of tomographic volumes at a high rate that requires the application of high-performance computing techniques for data reconstruction to produce the three-dimensional volumes, for their visualization, and for data analysis. These problems are exacerbated by the need to share information between collaborators at widely separated locations over both local and tide-area networks. A summary of the CMT technique and examples of applications are given here together with a discussion of the applications of high-performance computing methods to improve the experimental techniques and analysis of the data.

  13. Asymmetric Distribution of Metals in the Xenopus Laevis Oocyte: a Synchrotron X-Ray Fluorescence Microprobe Study

    SciTech Connect

    Popescu, B.F.Gh.; Belak, Z.R.; Ignatyev, K.; Ovsenek, N.; Nichol, H.

    2009-06-04

    The asymmetric distribution of many components of the Xenopus oocyte, including RNA, proteins, and pigment, provides a framework for cellular specialization during development. During maturation, Xenopus oocytes also acquire metals needed for development, but apart from zinc, little is known about their distribution. Synchrotron X-ray fluorescence microprobe was used to map iron, copper, and zinc and the metalloid selenium in a whole oocyte. Iron, zinc, and copper were asymmetrically distributed in the cytoplasm, while selenium and copper were more abundant in the nucleus. A zone of high copper and zinc was seen in the animal pole cytoplasm. Iron was also concentrated in the animal pole but did not colocalize with zinc, copper, or pigment accumulations. This asymmetry of metal deposition may be important for normal development. Synchrotron X-ray fluorescence microprobe will be a useful tool to examine how metals accumulate and redistribute during fertilization and embryonic development.

  14. Asymmetri Distribution of Metals in the Xenopus Laevis Oocyte: a Synchrotron X-Ray Fluorescence Microprobe Study

    SciTech Connect

    Popescu, B.F.G.; Belak, Z.R.; Ignatyev, K.; Ovsenek, N.; Nichol, H.; /Saskatchewan U. /SLAC, SSRL

    2009-04-29

    The asymmetric distribution of many components of the Xenopus oocyte, including RNA, proteins, and pigment, provides a framework for cellular specialization during development. During maturation, Xenopus oocytes also acquire metals needed for development, but apart from zinc, little is known about their distribution. Synchrotron X-ray fluorescence microprobe was used to map iron, copper, and zinc and the metalloid selenium in a whole oocyte. Iron, zinc, and copper were asymmetrically distributed in the cytoplasm, while selenium and copper were more abundant in the nucleus. A zone of high copper and zinc was seen in the animal pole cytoplasm. Iron was also concentrated in the animal pole but did not colocalize with zinc, copper, or pigment accumulations. This asymmetry of metal deposition may be important for normal development. Synchrotron X-ray fluorescence microprobe will be a useful tool to examine how metals accumulate and redistribute during fertilization and embryonic development.

  15. High rate, high resolution, two-dimensional gas proportional detectors for x-ray synchrotron radiation experiments

    SciTech Connect

    Smith, G.C.; Yu, B.; Fischer, J.; Radeka, V.; Harder, J.A.

    1992-02-01

    Two-dimensional, gas proportional detectors are being developed for use with X-ray synchrotron radiation. Two new types of interpolating cathode structures have been investigated, both of which can operate with a significantly smaller number of readout nodes along each sensing axis than previous cathodes. Lumped parameter delay lines are used as the position encoders. Timing signals from fast, low noise shaping electronics are fed to a new, dual TDC system developed for this purpose. Operating with a clock frequency of 500 MHz, the TDCs have an intrinsic differential non-linearity of 0.1%. The complete system can handle X-ray fluxes in excess of 10{sup 6} per sec without distortion of the position information. A resolution of approximately 100 {mu}m FWHM and differenfial non-linearity of {plus minus}4% have been achieved. Application of a detector with active area 10 cm {times} 10 cm using synchrotron radiation is described.

  16. A non-destructive synchrotron X-ray study of the metallurgy and manufacturing processes of Eastern and Western astrolabes in the Adler Planetarium collection

    NASA Astrophysics Data System (ADS)

    Newbury, Brian Dale

    The astrolabe collection of the Adler Planetarium and History of Astronomy Museum, Chicago, IL, was examined using non-destructive synchrotron based high-energy X-ray techniques including diffraction, fluorescence, and radiography to determine the metallurgy, microstructure, and metal forming processes used in astrolabe construction. All high-energy X-ray measurements were performed at the Advanced Photon Source (APS) synchrotron of Argonne National Laboratory, Argonne, IL. Astrolabes from the collection were selected to represent all major astrolabe production centers possible and time periods. It was found that all European astrolabes were manufactured of traditional cementation brass by hand worked metal forming processes consistent with technology in the literature. Of the Islamic astrolabes examined, all seven from Lahore in current-day Pakistan exhibited advanced brass alloys not typical of alloys discussed in the literature. It was found that these alloys were selected for their specific hot working properties, allowing the Lahore metalworkers to more efficiently make brass sheet from which to make astrolabe components. In addition, the alloy required a fundamental change in the brass foundry process, indicating advanced Zn metal production techniques. It was found that analysis by high energy X-rays from the APS was essential to produce data on the chemistry and microstructure from the interior of the astrolabe components in a non-destructive manner. Many astrolabe components had undergone surface dezincification due to heavy annealing during manufacturing, causing the Zn composition measured by the surface sensitive fluorescence technique to be lower than the true bulk alloy Zn composition. This would have been impossible to quantify non-destructively without the high-energy diffraction capability of the APS. The results of this study have proven the effectiveness of the synchrotron as a viable non-destructive analysis technique for examining cultural

  17. Genesis Sample Surface Contamination Study using Total-reflection X-Ray Fluorescence (TXRF)

    NASA Astrophysics Data System (ADS)

    Brennan, S.; Luening, K.; Pianetta, P.; Ishii, H. A.; Burnett, D. S.

    2005-12-01

    We have used synchrotron-based Total-reflection X-Ray Fluorescence (TXRF) to measure the surface and near-surface contamination of Genesis flight spare material as well as one piece of sapphire which flew on the mission. Flight spare samples included uncoated, Al-coated and Au-coated sapphire wafers and diamond-like carbon (DLC) on silicon. These studies were performed to determine the suitability of TXRF for the study of Genesis materials. The technique is optimally suited and highly surface sensitive for elements between Na and Br with sensitivities ranging from 1e9 to 1e12 atoms/cm2. By changing the x-ray angle of incidence one can vary the sampling depth from ~ 100 Å to several thousand Å. We found that the level of contamination of the flight-spare material varied widely. For the case of the returned piece of sapphire there were concentrations of Ge on the surface approaching monolayer coverage.

  18. In situ investigation of high humidity stress corrosion cracking of 7075 aluminum alloy by three-dimensional (3D) X-ray synchrotron tomography

    SciTech Connect

    Singh, S. S.; Williams, J. J.; Lin, M. F.; Xiao, X.; De Carlo, F.; Chawla, N.

    2014-05-14

    In situ X-ray synchrotron tomography was used to investigate the stress corrosion cracking behavior of under-aged Al–Zn–Mg–Cu alloy in moisture. The discontinuous surface cracks (crack jumps) mentioned in the literature are actually a single continuous and tortuous crack when observed in three dimension (3D). Contrary to 2D measurements made at the surface which suggest non-uniform crack growth rates, 3D measurements of the crack length led to a much more accurate measurement of crack growth rates.

  19. In situ investigation of high humidity stress corrosion cracking of 7075 aluminum alloy by three-dimensional (3D) X-ray synchrotron tomography

    DOE PAGESBeta

    Singh, S. S.; Williams, J. J.; Lin, M. F.; Xiao, X.; De Carlo, F.; Chawla, N.

    2014-05-14

    In situ X-ray synchrotron tomography was used to investigate the stress corrosion cracking behavior of under-aged Al–Zn–Mg–Cu alloy in moisture. The discontinuous surface cracks (crack jumps) mentioned in the literature are actually a single continuous and tortuous crack when observed in three dimension (3D). Contrary to 2D measurements made at the surface which suggest non-uniform crack growth rates, 3D measurements of the crack length led to a much more accurate measurement of crack growth rates.

  20. Superhydrophobic surfaces allow probing of exosome self organization using X-ray scattering

    NASA Astrophysics Data System (ADS)

    Accardo, Angelo; Tirinato, Luca; Altamura, Davide; Sibillano, Teresa; Giannini, Cinzia; Riekel, Christian; di Fabrizio, Enzo

    2013-02-01

    Drops of exosome dispersions from healthy epithelial colon cell line and colorectal cancer cells were dried on a superhydrophobic PMMA substrate. The residues were studied by small- and wide-angle X-ray scattering using both a synchrotron radiation micrometric beam and a high-flux table-top X-ray source. Structural differences between healthy and cancerous cells were detected in the lamellar lattices of the exosome macro-aggregates.Drops of exosome dispersions from healthy epithelial colon cell line and colorectal cancer cells were dried on a superhydrophobic PMMA substrate. The residues were studied by small- and wide-angle X-ray scattering using both a synchrotron radiation micrometric beam and a high-flux table-top X-ray source. Structural differences between healthy and cancerous cells were detected in the lamellar lattices of the exosome macro-aggregates. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr34032e

  1. Microdiffraction Study of Polycrystalline Copper during UniaxialTension Deformation using a Synchrotron X-ray Source

    SciTech Connect

    Joo, H.D.; Kim, J.S.; Bark, C.W.; Kim, J.Y.; Koo, Y.M.; Tamura, N.

    2004-10-04

    In-situ measurement of local orientation and strain has been carried out for a copper polycrystals under a uniaxial loading using a synchrotron x-ray microdiffraction method at the Advanced Light Source.The heterogeneities of deformation-induced microstructure within single grains were observed. There were differences in the selection of simultaneously acting slip systems among neighboring volume elements within a grain.

  2. Nuclear Bragg x-ray scattering of synchrotron radiation by sup 57 Fe sub 2 O sub 3

    SciTech Connect

    Haustein, P.E.; Berman, L.E.; Faigel, G.; Grover, J.R.; Hastings, J.B.; Siddons, D.P.

    1989-01-01

    A program of studies of nuclear Bragg x-ray scattering with {sup 57}Fe{sub 2}O{sub 3} at the National Synchrotron Light Source at Brookhaven National Laboratory and at the Cornell University CHESS facility is reviewed. Two main areas, instrumentation development and studies of dynamical diffraction processes, are described. The latter area has included: measurements of the temporal behaviour of nuclear collective decay mode and direct observation of polarization mixing. 7 refs., 5 figs.

  3. Demonstration experiment of a laser synchrotron source for tunable, monochromatic x-rays at 500 eV

    SciTech Connect

    Ting, A.; Fischer, R.; Fisher, A.

    1995-12-31

    A Laser Synchrotron Source (LSS) was proposed to generate short-pulsed, tunable x-rays by Thomson scattering of laser photons from a relativistic electron beam. A proof-of-principle experiment was performed to generate x-ray photons of 20 eV. A demonstration experiment is being planned and constructed to generate x-ray photons in the range of {approximately}500 eV. Laser photons of {lambda}=1.06 {mu}m are Thomson backscattered by a 4.5 MeV electron beam which is produced by an S-band RF electron gun. The laser photons are derived from either (i) a 15 Joules, 3 nsec Nd:glass laser, (ii) the uncompressed nsec: pulse of the NRL table-top terawatt (T{sup 3}) laser, or (iii) the compressed sub-picosec pulse of the T{sup 3} laser. The RF electron gun is being constructed with initial operation using a thermionic cathode. It will be upgraded to a photocathode to produce high quality electron beams with high current and low emittance. The x-ray pulse structure consists of {approximately}10 psec within an envelope of a macropulse whose length depends on the laser used. The estimated x-ray photon flux is {approximately}10{sup 18} photons/sec, and the number of photons per macropulse is {approximately}10{sup 8}. Design parameters and progress of the experiment will be presented.

  4. Implementation of ultrafast X-ray diffraction at the 1W2B wiggler beamline of Beijing Synchrotron Radiation Facility.

    PubMed

    Sun, Da Rui; Xu, Guang Lei; Zhang, Bing Bing; Du, Xue Yan; Wang, Hao; Li, Qiu Ju; Zhou, Yang Fan; Li, Zhen Jie; Zhang, Yan; He, Jun; Yue, Jun Hui; Lei, Ge; Tao, Ye

    2016-05-01

    The implementation of a laser pump/X-ray probe scheme for performing picosecond-resolution X-ray diffraction at the 1W2B wiggler beamline at Beijing Synchrotron Radiation Facility is reported. With the hybrid fill pattern in top-up mode, a pixel array X-ray detector was optimized to gate out the signal from the singlet bunch with interval 85 ns from the bunch train. The singlet pulse intensity is ∼2.5 × 10(6) photons pulse(-1) at 10 keV. The laser pulse is synchronized to this singlet bunch at a 1 kHz repetition rate. A polycapillary X-ray lens was used for secondary focusing to obtain a 72 µm (FWHM) X-ray spot. Transient photo-induced strain in BiFeO3 film was observed at a ∼150 ps time resolution for demonstration. PMID:27140165

  5. Synchrotron X-ray Tomographic Quantification of Deformation Induced Strain Localisation in Semi-solid Al- 15wt.%Cu

    NASA Astrophysics Data System (ADS)

    Cai, B.; Karagadde, S.; Marrow, T. J.; Connolley, T.; Lee, P. D.

    2015-06-01

    Uniaxial compression and indentation of a semi-solid Al-15wt.%Cu alloy was investigated by high speed synchrotron X-ray microtomography, quantifying the microstructural response of a solidifying alloy to applied strain. Tomograms were continuously acquired whilst performing deformation using a precision thermal-mechanical rig on a synchrotron beamline. The results illustrate how defects and shear bands can form in response to different loading conditions. Using digital volume correlation, the global and localised strains were measured, providing quantitative datasets for granular flow models of semi-solid deformation.

  6. Elemental concentrations in skin of patients with fibroeptelial polip using synchrotron radiation total reflection x-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Soares, Júlio C. A. C. R.; Anjos, Marcelino J.; Canellas, Catarine G. L.; Lopes, Ricardo T.

    2012-05-01

    In this work, the concentrations of trace elements were measured in acrochordon, a skin lesion also known as skin tag or fibroepithelial polyp, as well as in normal skin from the same patient. The samples were analyzed by Synchrotron Radiation Total Reflection X-ray Fluorescence (SRTXRF) in the Synchrotron Light National Laboratory (LNLS) in Campinas/São Paulo-Brazil. The collection of lesion and healthy skin samples, including papillary dermis and epidermis, has involved 17 patients. It was evaluated the presence of P, S, Cl, K, Ca, Fe, Cu and Zn in the paired samples, which were compared, and significant differences were found in some of them.

  7. Measuring Non-Wetting/Wetting Interfacial Area: Comparing Synchrotron X-ray Microtomography and Interfacial Partitioning Tracer Methods

    NASA Astrophysics Data System (ADS)

    Narter, M. E.; Brusseau, M. L.

    2008-12-01

    Previous studies have shown that non-wetting/wetting interfacial areas measured with synchrotron X-ray microtomography are significantly smaller than those measured using the interfacial tracer test method for natural porous media. Research was conducted to evaluate the source of the disparity between these methods. It has been hypothesized that the disparity is due primarily to resolution constraints associated with microtomography, wherein the interfacial area associated with microscopic surface roughness is not measured. To test this hypothesis, experiments were conducted with glass beads that were shown to have no measureable surface roughness. Tetrachloroethene (PCE) was used as the model non-wetting fluid and sodium dodecylbenzene sulfonate was used as the interfacial tracer. Tracer tests yielded an average interfacial area of 2.8 +/- 5 1/cm while microtomography results produced an interfacial area of 3.4 +/- 2 1/cm. The values are similar for the two methods, indicating that the disparity observed for natural media is likely due to resolution limitations of microtomography.

  8. Determining the Structure of Biomaterials Interfaces using Synchrotron-based X-ray Diffraction

    SciTech Connect

    McBride, M

    2002-01-24

    The purpose of this project is to explore the feasibility of using surface X-ray diffraction (SXRD) to determine the structure of biomineral surfaces in electrolyte solutions and of the adsorbed layer of acidic amino acids that are believed to play a central role in the control of biomineral formation and function. The work is a critical component in the development of an integrated picture of the physical and chemical basis for deposition and dissolution at solid-liquid interfaces in biological systems, and brings a new and very powerful surface-sensitive capability to LLNL. We have chosen as our model systems calcium carbonate and calcium phosphate in aspartic and glutamic acid-bearing solutions. The calcium compounds are ubiquitous among biomineral structures, both those that are beneficial such as bones and teeth, and those that are pathological such as kidney stones, while the two acidic amino acids--both as simple and poly-amino acids--are the dominant constituents of protein mixtures implicated in the control of biomineralization. The goals of the work are: (1) to determine the surface structure of pure calcium phosphate and calcium carbonate surfaces in aqueous solution using SXRD; (2) to determine how those surfaces are modified by the presence of aspartic and glutamic acid, both as the simple amino acids and as poly-aspartate and poly-glutamate and (3) to model the interactions of acidic amino acids with calcite.

  9. Quantifying trace elements in individual aquatic protist cells with a synchrotron X-ray fluorescence microprobe.

    PubMed

    Twining, Benjamin S; Baines, Stephen B; Fisher, Nicholas S; Maser, Jörg; Vogt, Stefan; Jacobsen, Chris; Tovar-Sanchez, Antonio; Sañudo-Wilhelmy, Sergio A

    2003-08-01

    The study of trace metal cycling by aquatic protists is limited by current analytical techniques. Standard "bulk" element analysis techniques that rely on physical separations to concentrate cells for analysis cannot separate cells from co-occurring detrital material or other cells of differing taxonomy or trophic function. Here we demonstrate the ability of a synchrotron-based X-ray fluorescence (SXRF) microprobe to quantify the elements Si, Mn, Fe, Ni, and Zn in individual aquatic protist cells. This technique distinguishes between different types of cells in an assemblage and between cells and other particulate matter. Under typical operating conditions, the minimum detection limits are 7.0 x 10(-16) mol microm(-2) for Si and between 5.0 x 10(-20) and 3.9 x 10(-19) mol microm(-2) for Mn, Fe, Ni, and Zn; this sensitivity is sufficient to detect these elements in cells from even the most pristine waters as demonstrated in phytoplankton cells collected from remote areas of the Southern Ocean. Replicate analyses of single cells produced variations of <5% for Si, Mn, Fe, and Zn and <10% for Ni. Comparative analyses of cultured phytoplankton cells generally show no significant differences in cellular metal concentrations measured with SXRF and standard bulk techniques (spectrophotometry and graphite furnace atomic absorption spectrometry). SXRF also produces two-dimensional maps of element distributions in cells, thereby providing information not available with other analytical approaches. This technique enables the accurate and precise measurement of trace metals in individual aquatic protists collected from natural environments. PMID:14572047

  10. Quantifying trace elements in individual aquatic protist cells with a synchrotron x-ray fluorescence microprobe.

    SciTech Connect

    Twining, B. S.; Baines, S. B.; Fisher, N. S.; Maser, J.; Vogt, S.; Jacobsen, C.; Tovar-Sanchez, A.; Sanudo-Wihelmy, S. A.; Experimental Facilities Division; Stony Brook Univ.

    2003-01-01

    The study of trace metal cycling by aquatic protists is limited by current analytical techniques. Standard 'bulk' element analysis techniques that rely on physical separations to concentrate cells for analysis cannot separate cells from co-occurring detrital material or other cells of differing taxonomy or trophic function. Here we demonstrate the ability of a synchrotron-based X-ray fluorescence (SXRF) microprobe to quantify the elements Si, Mn, Fe, Ni, and Zn in individual aquatic protist cells. This technique distinguishes between different types of cells in an assemblage and between cells and other particulate matter. Under typical operating conditions, the minimum detection limits are 7.0 x 10{sup -16} mol {mu}m{sup -2} for Si and between 5.0 x 10{sup -20} and 3.9 x 10{sup -19} mol {mu}m{sup -2} for Mn, Fe, Ni, and Zn; this sensitivity is sufficient to detect these elements in cells from even the most pristine waters as demonstrated in phytoplankton cells collected from remote areas of the Southern Ocean. Replicate analyses of single cells produced variations of <5% for Si, Mn, Fe, and Zn and <10% for Ni. Comparative analyses of cultured phytoplankton cells generally show no significant differences in cellular metal concentrations measured with SXRF and standard bulk techniques (spectrophotometry and graphite furnace atomic absorption spectrometry). SXRF also produces two-dimensional maps of element distributions in cells, thereby providing information not available with other analytical approaches. This technique enables the accurate and precise measurement of trace metals in individual aquatic protists collected from natural environments.

  11. Visualizing Metal Content and Intracellular Distribution in Primary Hippocampal Neurons with Synchrotron X-Ray Fluorescence

    PubMed Central

    2016-01-01

    Increasing evidence suggests that metal dyshomeostasis plays an important role in human neurodegenerative diseases. Although distinctive metal distributions are described for mature hippocampus and cortex, much less is known about metal levels and intracellular distribution in individual hippocampal neuronal somata. To solve this problem, we conducted quantitative metal analyses utilizing synchrotron radiation X-Ray fluorescence on frozen hydrated primary cultured neurons derived from rat embryonic cortex (CTX) and two regions of the hippocampus: dentate gyrus (DG) and CA1. Comparing average metal contents showed that the most abundant metals were calcium, iron, and zinc, whereas metals such as copper and manganese were less than 10% of zinc. Average metal contents were generally similar when compared across neurons cultured from CTX, DG, and CA1, except for manganese that was larger in CA1. However, each metal showed a characteristic spatial distribution in individual neuronal somata. Zinc was uniformly distributed throughout the cytosol, with no evidence for the existence of previously identified zinc-enriched organelles, zincosomes. Calcium showed a peri-nuclear distribution consistent with accumulation in endoplasmic reticulum and/or mitochondria. Iron showed 2–3 distinct highly concentrated puncta only in peri-nuclear locations. Notwithstanding the small sample size, these analyses demonstrate that primary cultured neurons show characteristic metal signatures. The iron puncta probably represent iron-accumulating organelles, siderosomes. Thus, the metal distributions observed in mature brain structures are likely the result of both intrinsic neuronal factors that control cellular metal content and extrinsic factors related to the synaptic organization, function, and contacts formed and maintained in each region. PMID:27434052

  12. Trace element abundances in single presolar silicon carbide grains by synchrotron X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Kashiv, Yoav

    2004-12-01

    Synchrotron x-ray fluorescence (SXRF) was applied to the study of presolar grains for the first time in this study. 41 single SiC grains of the KJF size fraction (mass-weighted median size of 1.86 μm) from the Murchison (CM2) Meteorite were analyzed. The absolute abundances of the following elements were determined (not every element in every grain): S, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Sr, Y, Zr, Nb, Mo, Ru, Os, Ir and Pt (underlined elements were detected here for the first time in single grains). There is good agreement between the heavier trace element abundances in the grains and s-process nucleosynthesis calculations. It suggests that smaller 13C pocket sizes are needed in the parent stars, a free parameter in the stellar models, than is deduced from isotopic analyses of s-, and s-mainly, elements, such as Zr and Mo. In addition, the data confirms the radiogenic nature of the Nb in the grains, due to the in situ decay of 93Zr (t 1/2 = 1.5 × 106 year). The data suggest that the trace elements condensed into the host SiC grains by a combination of condensation in solid solution and incorporation of subgrains. It seems that many of the trace elements reside mainly in subgrains of two solid solution: (1)a TiC based solid solution, and (2)a Mo-Ru carbide based solid solution. The presence of subgrains of an Fe-Ni alloy solid solution is suggested as well. Subgrains of all 3 solid solutions were observed previously in presolar graphite grains.* *This dissertation is a compound document (contains both a paper copy and a CD as part of the dissertation). The CD requires the following system requirements: Adobe Acrobat.

  13. Bone Implant Interface Investigation by Synchrotron Radiation X-Ray Microfluorescence

    SciTech Connect

    Calasans-Maia, M.; Sales, E.; Lopes, R. T.; Lima, I.

    2010-04-06

    Zinc is known to play a relevant role in growth and development; it has stimulatory effects on in vitro and in vivo bone formation and an inhibitory effect on in vitro osteoclastic bone resorption. The inorganic component of the bone tissue is nonstoichiometric apatite; changes in the composition of hidroxyapatite are subject of studies in order to improve the tissue response after implantation. The objective of this study was to investigate the effect of 0.5% zinc-containing hydroxyapatite in comparison to hydroxyapatite on osseous repair of rabbit's tibia. Cylinders (2x6 mm) of both materials were produced according to the specification of the International Organization for Standardization. Ethics Commission on Teaching and Research in Animals approved this project (HUAP-195/06). Fifteen White New Zealand rabbits were submitted to general anesthesia and two perforations (2 mm) were made in each tibia for implantation of zinc-containing hydroxyapatite cylinders (left tibia) and hydroxyapatite cylinders (right tibia). After 1, 2 and 4 weeks, the animals were killed and one fragment of each tibia with the cylinder was collected and embedded in a methacrylate-based resin and cut into slices (approx200 {mu}m thickness), parallel to the implant's long axis with a precision diamond saw for Synchrotron Radiation X-ray Microfluorescence investigation. The accomplishment of the standard procedures helped the planning, execution and the comparative analysis of the results. The chemical and physical properties of the biomaterials were modified after its implantation and the incorporation of zinc. Both materials are biocompatible and promote osteoconduction and favored bone repair.

  14. Thermal equation of state of TiC: A synchrotron x-ray diffraction study

    SciTech Connect

    Yu Xiaohui; Lin Zhijun; Zhang Jianzhong; Zhao Yusheng; Wang Liping; Ding Zejun; Jin Changqing

    2010-06-15

    The pressure-volume-temperature measurements were carried out for titanium carbide (TiC) at pressures and temperatures up to 8.1 GPa and 1273 K using energy-dispersive synchrotron x-ray diffraction. Thermoelastic parameters were derived for TiC based on a modified high-temperature Birch-Murnaghan equation of state and a thermal pressure approach. With the pressure derivative of the bulk modulus, K{sub 0}{sup '}, fixed at 4.0, we obtain: the ambient bulk modulus K{sub 0}=268(6) GPa, which is comparable to previously reported value; temperature derivative of bulk modulus at constant pressure ({partial_derivative}K{sub T}/{partial_derivative}T){sub P}=-0.026(9) GPa K{sup -1}, volumetric thermal expansivity {alpha}{sub T}(K{sup -1})=a+bT with a=1.62(12)x10{sup -5} K{sup -1} and b=1.07(17)x10{sup -8} K{sup -2}, pressure derivative of thermal expansion ({partial_derivative}{alpha}/{partial_derivative}P){sub T}=(-3.62{+-}1.14)x10{sup -7} GPa{sup -1} K{sup -1}, and temperature derivative of bulk modulus at constant volume ({partial_derivative}K{sub T}/{partial_derivative}T){sub V}=-0.015(8) GPa K{sup -1}. These results provide fundamental thermophysical properties for TiC for the first time and are important to theoretical and computational modeling of transition metal carbides.

  15. Visualizing Metal Content and Intracellular Distribution in Primary Hippocampal Neurons with Synchrotron X-Ray Fluorescence.

    PubMed

    Colvin, Robert A; Jin, Qiaoling; Lai, Barry; Kiedrowski, Lech

    2016-01-01

    Increasing evidence suggests that metal dyshomeostasis plays an important role in human neurodegenerative diseases. Although distinctive metal distributions are described for mature hippocampus and cortex, much less is known about metal levels and intracellular distribution in individual hippocampal neuronal somata. To solve this problem, we conducted quantitative metal analyses utilizing synchrotron radiation X-Ray fluorescence on frozen hydrated primary cultured neurons derived from rat embryonic cortex (CTX) and two regions of the hippocampus: dentate gyrus (DG) and CA1. Comparing average metal contents showed that the most abundant metals were calcium, iron, and zinc, whereas metals such as copper and manganese were less than 10% of zinc. Average metal contents were generally similar when compared across neurons cultured from CTX, DG, and CA1, except for manganese that was larger in CA1. However, each metal showed a characteristic spatial distribution in individual neuronal somata. Zinc was uniformly distributed throughout the cytosol, with no evidence for the existence of previously identified zinc-enriched organelles, zincosomes. Calcium showed a peri-nuclear distribution consistent with accumulation in endoplasmic reticulum and/or mitochondria. Iron showed 2-3 distinct highly concentrated puncta only in peri-nuclear locations. Notwithstanding the small sample size, these analyses demonstrate that primary cultured neurons show characteristic metal signatures. The iron puncta probably represent iron-accumulating organelles, siderosomes. Thus, the metal distributions observed in mature brain structures are likely the result of both intrinsic neuronal factors that control cellular metal content and extrinsic factors related to the synaptic organization, function, and contacts formed and maintained in each region. PMID:27434052

  16. Mapping and load response of overload strain fields: Synchrotron X-ray measurements

    SciTech Connect

    Shukla, V; Jisrawi, N M; Sadangi, R K; Pao, P S; Horvath, K; Sadananda, K; Ignatov, A; Skaritka, J; Tsakalakos, T

    2009-02-05

    High energy synchrotron X-ray diffraction measurements have been performed to provide quantitative microscopic guidance for modeling of fatigue crack growth. Specifically we report local strain mapping, along with in situ loading strain response, results on 4140 steel fatigue specimens exhibiting the crack growth retardation 'overload effect'. Detailed, 2D, {epsilon}{gamma}{gamma}-strain field mapping shows that a single overload (OL) cycle creates a compressive strain field extending millimeters above and below the crack plane. The OL strain field structures are shown to persist after the crack tip has grown well beyond the OL position. The specimen exhibiting the maximal crack growth rate retardation following overload exhibits a tensile residual strain region at the crack tip. Strain field results, on in situ tensile loaded specimens, show a striking critical threshold load, F{sub c}, phenomenon in their strain response. At loads below F{sub c} the strain response is dominated by a rapid suppression of the compressive OL feature with modest response at the crack tip. At loads above F{sub c} the strain response at the OL position terminates and the response at the crack tip becomes large. This threshold load response behavior is shown to exhibit lower F{sub c} values, and dramatically enhanced rates of strain change with load as the crack tip propagates farther beyond the OL position. The OL strain feature behind the crack tip also is shown to be suppressed by removing the opposing crack faces via an electron discharge cut passing through the crack tip. Finally unique 2D strain field mapping (imaging) results, through the depth of the specimen, of the fatigue crack front and the OL feature in the wake are also presented.

  17. Three-dimensional imaging of copper pillars using x-ray tomography within a scanning electron microscope: A simulation study based on synchrotron data

    NASA Astrophysics Data System (ADS)

    Martin, N.; Bertheau, J.; Bleuet, P.; Charbonnier, J.; Hugonnard, P.; Laloum, D.; Lorut, F.; Tabary, J.

    2013-02-01

    While microelectronic devices are frequently characterized with surface-sensitive techniques having nanometer resolution, interconnections used in 3D integration require 3D imaging with high penetration depth and deep sub-micrometer spatial resolution. X-ray tomography is well adapted to this situation. In this context, the purpose of this study is to assess a versatile and turn-key tomographic system allowing for 3D x-ray nanotomography of copper pillars. The tomography tool uses the thin electron beam of a scanning electron microscope (SEM) to provoke x-ray emission from specific metallic targets. Then, radiographs are recorded while the sample rotates in a conventional cone beam tomography scheme that ends up with 3D reconstructions of the pillar. Starting from copper pillars data, collected at the European Synchrotron Radiation Facility, we build a 3D numerical model of a copper pillar, paying particular attention to intermetallics. This model is then used to simulate physical radiographs of the pillar using the geometry of the SEM-hosted x-ray tomography system. Eventually, data are reconstructed and it is shown that the system makes it possible the quantification of 3D intermetallics volume in copper pillars. The paper also includes a prospective discussion about resolution issues.

  18. Three-dimensional imaging of copper pillars using x-ray tomography within a scanning electron microscope: A simulation study based on synchrotron data

    SciTech Connect

    Martin, N.; Bertheau, J.; Charbonnier, J.; Hugonnard, P.; Lorut, F.; Bleuet, P.; Tabary, J.; Laloum, D.

    2013-02-15

    While microelectronic devices are frequently characterized with surface-sensitive techniques having nanometer resolution, interconnections used in 3D integration require 3D imaging with high penetration depth and deep sub-micrometer spatial resolution. X-ray tomography is well adapted to this situation. In this context, the purpose of this study is to assess a versatile and turn-key tomographic system allowing for 3D x-ray nanotomography of copper pillars. The tomography tool uses the thin electron beam of a scanning electron microscope (SEM) to provoke x-ray emission from specific metallic targets. Then, radiographs are recorded while the sample rotates in a conventional cone beam tomography scheme that ends up with 3D reconstructions of the pillar. Starting from copper pillars data, collected at the European Synchrotron Radiation Facility, we build a 3D numerical model of a copper pillar, paying particular attention to intermetallics. This model is then used to simulate physical radiographs of the pillar using the geometry of the SEM-hosted x-ray tomography system. Eventually, data are reconstructed and it is shown that the system makes it possible the quantification of 3D intermetallics volume in copper pillars. The paper also includes a prospective discussion about resolution issues.

  19. Imaging local electric fields produced upon synchrotron X-ray exposure

    PubMed Central

    Dettmar, Christopher M.; Newman, Justin A.; Toth, Scott J.; Becker, Michael; Fischetti, Robert F.; Simpson, Garth J.

    2015-01-01

    Electron–hole separation following hard X-ray absorption during diffraction analysis of soft materials under cryogenic conditions produces substantial local electric fields visualizable by second harmonic generation (SHG) microscopy. Monte Carlo simulations of X-ray photoelectron trajectories suggest the formation of substantial local electric fields in the regions adjacent to those exposed to X-rays, indicating a possible electric-field–induced SHG (EFISH) mechanism for generating the observed signal. In studies of amorphous vitreous solvents, analysis of the SHG spatial profiles following X-ray microbeam exposure was consistent with an EFISH mechanism. Within protein crystals, exposure to 12-keV (1.033-Å) X-rays resulted in increased SHG in the region extending ∼3 μm beyond the borders of the X-ray beam. Moderate X-ray exposures typical of those used for crystal centering by raster scanning through an X-ray beam were sufficient to produce static electric fields easily detectable by SHG. The X-ray–induced SHG activity was observed with no measurable loss for longer than 2 wk while maintained under cryogenic conditions, but disappeared if annealed to room temperature for a few seconds. These results provide direct experimental observables capable of validating simulations of X-ray–induced damage within soft materials. In addition, X-ray–induced local fields may potentially impact diffraction resolution through localized piezoelectric distortions of the lattice. PMID:25552555

  20. The study of X-ray scattering to determine surface topography of smooth surfaces. [X-ray telescope mirrors

    NASA Technical Reports Server (NTRS)

    Williams, A. C.

    1982-01-01

    The scattering of X-rays from state-of-the-art polished mirrors is discussed with reference to the requirements of the Advanced X-ray Astrophysics Facility telescope. An experimental set-up is described which allows information to be obtained with subarcsecond resolution. A sample of the data obtained is presented along with a possible theoretical model for its interpretation.

  1. Development of synchrotron x-ray micro-spectroscopic techniques and application to problems in low temperature geochemistry. Progress report

    SciTech Connect

    Not Available

    1993-10-01

    The focus of the technical development effort has been the development of apparatus and techniques for the utilization of X-ray Fluorescence (XRF), Extended X-ray Absorption Fine Structure (EXAFS) and X-ray Absorption Near Edge Structure (XANES) spectroscopies in a microprobe mode. The present XRM uses white synchrotron radiation (3 to 30 keV) from a bending magnet for trace element analyses using the x-ray fluorescence technique Two significant improvements to this device have been recently implemented. Focusing Mirror: An 8:1 ellipsoidal mirror was installed in the X26A beamline to focus the incident synchrotron radiation and thereby increase the flux on the sample by about a factor of 30. Incident Beam Monochromator: The monochromator has been successfully installed and commissioned in the X26A beamline upstream of the mirror to permit analyses with focused monochromatic radiation. The monochromator consists of a channel-cut silicon (111) crystal driven by a Klinger stepping motor translator. We have demonstrated the operating range of this instrument is 4 and 20 keV with 0.01 eV steps and produces a beam with a {approximately}10{sup {minus}4} energy bandwidth. The primary purpose of the monochromator is for x-ray absorption spectroscopy (XAS) measurements but it is also used for selective excitation in trace element microanalysis. To date, we have conducted XANES studies on Ti, Cr, Fe, Ce and U, spanning the entire accessible energy range and including both K and L edge spectra. Practical detection limits for microXANES are 10--100 ppM for 100 {mu}m spots.

  2. Synchrotron X-Ray Microtomography and Interfacial Partitioning Tracer Test Measurements of Napl-Water Interfacial Areas

    NASA Astrophysics Data System (ADS)

    Brusseau, M. L.; Janousek, H.; Murao, A.; Schnaar, G.

    2007-12-01

    Interfacial areas between an immiscible organic liquid (NAPL) and water were measured for two natural porous media using two methods, aqueous-phase interfacial partitioning tracer tests and synchrotron X-ray microtomography. The interfacial areas measured with the tracer tests were similar to previously reported values obtained with the method. The values were, however, significantly larger than those obtained from microtomography. Analysis of microtomography data collected before and after introduction of the interfacial tracer solution indicated that the surfactant tracer had minimal impact on fluid-phase configuration and interfacial areas under conditions associated with typical laboratory application. The disparity between the tracer-test and microtomography values is attributed primarily to the inability of the microtomography method to resolve interfacial area associated with microscopic surface heterogeneity. This hypothesis is consistent with results recently reported for a comparison of microtomographic analysis and interfacial tracer tests conducted for an air-water system. The tracer-test method provides a measure of effective, total (capillary and film) interfacial area, whereas microtomography can be used to determine separately both capillary-associated and film-associated interfacial areas. Both methods appear to provide useful information for given applications. A key to their effective use is recognizing the specific nature of the information provided by each, as well as associated limitations.

  3. Synchrotron X-ray diffraction and scanning electron microscopy to understand enamel affected by metabolic disorder mucopolysaccharidosis.

    PubMed

    Khan, Malik Arshman; Addison, Owen; James, Alison; Hendriksz, Christian J; Al-Jawad, Maisoon

    2016-04-01

    Mucopolysaccharidosis (MPS) is an inherited metabolic disorder that can affect the tooth structure leading to defects. Synchrotron X-ray diffraction being a state of the art technique has been used to determine the enamel crystallite orientation in deciduous enamel affected by Mucopolysaccharidosis Type I and Mucopolysaccharidosis Type IVA and comparing these with that of healthy deciduous enamel. Using this technique it was observed that there is a loss of texture in deciduous enamel affected by Mucopolysaccharidosis Type I and Mucopolysaccharidosis Type IVA when compared to the healthy deciduous enamel. Generally it was observed that the incisal surface of the deciduous teeth possessed a higher texture or preferred orientation of enamel crystallites and on progression towards the cervical region there was a decrease in the texture or preferred orientation of enamel crystallites. Scanning electron microscopy showed that the presence of a poorly calcified layer between the enamel and dentine at the enamel-dentine junction (EDJ) in MPS affected samples was likely to be responsible for rendering the tooth structure weak and prone to fracture as is often the case in MPS affected deciduous enamel. PMID:26896739

  4. Non-destructive trace element microanalysis of as-received cometary nucleus samples using synchrotron x ray fluorescence

    NASA Technical Reports Server (NTRS)

    Sutton, S. R.

    1989-01-01

    The Synchrotron X ray Fluorescence (SXRF) microprobe at the National Synchrotron Light Source (NSLS), Brookhaven National Laboratory, will be an excellent instrument for non-destructive trace element analyses of cometary nucleus samples. Trace element analyses of as-received cometary nucleus material will also be possible with this technique. Bulk analysis of relatively volatile elements will be important in establishing comet formation conditions. However, as demonstrated for meteorites, microanalyses of individual phases in their petrographic context are crucial in defining the histories of particular components in unequilibrated specimens. Perhaps most informative in comparing cometary material with meteorites will be the halogens and trace metals. In-situ, high spatial resolution microanalyses will be essential in establishing host phases for these elements and identifying terrestrial (collection/processing) overprints. The present SXRF microprobe is a simple, yet powerful, instrument in which specimens are excited with filtered, continuum synchrotron radiation from a bending magnet on a 2.5 GeV electron storage ring. A refrigerated cell will be constructed to permit analyses at low temperatures. The cell will consist essentially of an air tight housing with a cold stage. Kapton windows will be used to allow the incident synchrotron beam to enter the cell and fluorescent x rays to exit it. The cell will be either under vacuum or continuous purge by ultrapure helium during analyses. Several other improvements of the NSLS microprobe will be made prior to the cometary nucleus sample return mission that will greatly enhance the sensitivity of the technique.

  5. Structure of nanocrystalline calcium silicate hydrates: insights from X-ray diffraction, synchrotron X-ray absorption and nuclear magnetic resonance

    PubMed Central

    Grangeon, Sylvain; Claret, Francis; Roosz, Cédric; Sato, Tsutomu; Gaboreau, Stéphane; Linard, Yannick

    2016-01-01

    The structure of nanocrystalline calcium silicate hydrates (C–S–H) having Ca/Si ratios ranging between 0.57 ± 0.05 and 1.47 ± 0.04 was studied using an electron probe micro-analyser, powder X-ray diffraction, 29Si magic angle spinning NMR, and Fourier-transform infrared and synchrotron X-ray absorption spectroscopies. All samples can be described as nanocrystalline and defective tobermorite. At low Ca/Si ratio, the Si chains are defect free and the Si Q 3 and Q 2 environments account, respectively, for up to 40.2 ± 1.5% and 55.6 ± 3.0% of the total Si, with part of the Q 3 Si being attributable to remnants of the synthesis reactant. As the Ca/Si ratio increases up to 0.87 ± 0.02, the Si Q 3 environment decreases down to 0 and is preferentially replaced by the Q 2 environment, which reaches 87.9 ± 2.0%. At higher ratios, Q 2 decreases down to 32.0 ± 7.6% for Ca/Si = 1.38 ± 0.03 and is replaced by the Q 1 environment, which peaks at 68.1 ± 3.8%. The combination of X-ray diffraction and NMR allowed capturing the depolymerization of Si chains as well as a two-step variation in the layer-to-layer distance. This latter first increases from ∼11.3 Å (for samples having a Ca/Si ratio <∼0.6) up to 12.25 Å at Ca/Si = 0.87 ± 0.02, probably as a result of a weaker layer-to-layer connectivity, and then decreases down to 11 Å when the Ca/Si ratio reaches 1.38 ± 0.03. The decrease in layer-to-layer distance results from the incorporation of interlayer Ca that may form a Ca(OH)2-like structure, nanocrystalline and intermixed with C–S–H layers, at high Ca/Si ratios. PMID:27275135

  6. Understanding Electrocatalytic Pathways in Low and Medium Temperature Fuel Cells: Synchrotron-based In Situ X-Ray Absorption Spectroscopy

    SciTech Connect

    Mukerjee, S.; Ziegelbauer, J; Arruda, T; Ramaker, D; Shyam, B

    2008-01-01

    Over the last few decades, researchers have made significant developments in producing more advanced electrocatalytic materials for power generation applications. For example, traditional fuel cell catalysts often involve high-priced precious metals such as Pt. However, in order for fuel cells to become commercially viable, there is a need to reduce or completely remove precious metal altogether. As a result, a myriad of novel, unconventional materials have been explored such as chalcogenides, porphyrins, and organic-metal-macrocycles for low/medium temperature fuel cells as well as enzymatic and microbial fuel cells. As these materials increasingly become more complex, researchers often find themselves in search of new characterization methods, especially those which are allow in situ and operando measurements with element specificity. One such method that has received much attention for analysis of electrocatalytic materials is X-ray absorption spectroscopy (XAS). XAS is an element specific, core level absorption technique which yields structural and electronic information. As a core electron method, XAS requires an extremely bright source, hence a synchrotron. The resulting intensity of synchrotron radiation allow for experiments to be conducted in situ, under electrochemically relevant conditions. Although a bulk-averaging technique requiring rigorous mathematical manipulation, XAS has the added benefit that it can probe materials which possess no long range order. This makes it ideal to characterize nano-scale electrocatalysts. XAS experiments are conducted by ramping the X-ray photon energy while measuring absorption of the incident beam the sample or by counting fluorescent photons released from a sample due to subsequent relaxation. Absorption mode XAS follows the Beer-Lambert Law, {mu}x = log(I{sub 0}/I{sub t}) (1) where {mu} is the absorption coefficient, x is the sample thickness and I{sub 0} and I{sub t} are the intensities of the incident and

  7. Synchrotron X-ray diffraction studies of phase transitions and mechanical properties of nanocrystalline materials at high pressure

    SciTech Connect

    Prilliman, Gerald Stephen

    2003-09-01

    The behavior of nanocrystals under extreme pressure was investigated using synchrotron x-ray diffraction. A major part of this investigation was the testing of a prototype synchrotron endstation on a bend magnet beamline at the Advanced Light Source for high pressure work using a diamond anvil cell. The experiments conducted and documented here helped to determine issues of efficiency and accuracy that had to be resolved before the construction of a dedicated ''super-bend'' beamline and endstation. The major conclusions were the need for a cryo-cooled monochromator and a fully remote-controllable pressurization system which would decrease the time to change pressure and greatly reduce the error created by the re-placement of the diamond anvil cell after each pressure change. Two very different types of nanocrystal systems were studied, colloidal iron oxide (Fe{sub 2}O{sub 3}) and thin film TiN/BN. Iron oxide nanocrystals were found to have a transition from the {gamma} to the {alpha} structure at a pressure strongly dependent on the size of the nanocrystals, ranging from 26 GPa for 7.2 nm nanocrystals to 37 GPa for 3.6 nm nanocrystals. All nanocrystals were found to remain in the {alpha} structure even after release of pressure. The transition pressure was also found, for a constant size (5.7 nm) to be strongly dependent on the degree of aggregation of the nanocrystals, increasing from 30 GPa for completely dissolved nanocrystals to 45 GPa for strongly aggregated nanocrystals. Furthermore, the x-ray diffraction pattern of the pressure induced {alpha} phase demonstrated a decrease in intensity for certain select peaks. Together, these observations were used to make a complete picture of the phase transition in nanocrystalline systems. The size dependence of the transition was interpreted as resulting from the extremely high surface energy of the {alpha} phase which would increase the thermodynamic offset and thereby increase the kinetic barrier to transition that

  8. Primary radiation damage of protein crystals by an intense synchrotron X-ray beam.

    PubMed

    Teng, T Y; Moffat, K

    2000-09-01

    X-ray radiation damage of a lysozyme single crystal by an intense monochromatic beam from a third-generation radiation source at the Advanced Photon Source has been studied. The results show that primary radiation damage is linearly dependent on the X-ray dose even when the crystal is at cryogenic temperatures. The existence of an upper limit for the primary radiation damage was observed. Above the threshold of approximately 1 x 10(7) Gy, excessive damage of the crystal develops which is interpreted as the onset of secondary and/or tertiary radiation damage. This upper limit of X-ray dose is compared with Henderson's limit [Henderson (1990). Proc. R. Soc. London, B241, 6-8], and its implication for the amount of useful X-ray diffraction data that can be obtained for crystals of a given scattering power is also discussed. PMID:16609214

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

    SciTech Connect

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

    2009-12-01

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

  10. Sapphire hard X-ray Fabry-Perot resonators for synchrotron experiments.

    PubMed

    Tsai, Yi Wei; Wu, Yu Hsin; Chang, Ying Yi; Liu, Wen Chung; Liu, Hong Lin; Chu, Chia Hong; Chen, Pei Chi; Lin, Pao Te; Fu, Chien Chung; Chang, Shih Lin

    2016-05-01

    Hard X-ray Fabry-Perot resonators (FPRs) made from sapphire crystals were constructed and characterized. The FPRs consisted of two crystal plates, part of a monolithic crystal structure of Al2O3, acting as a pair of mirrors, for the backward reflection (0 0 0 30) of hard X-rays at 14.3147 keV. The dimensional accuracy during manufacturing and the defect density in the crystal in relation to the resonance efficiency of sapphire FPRs were analyzed from a theoretical standpoint based on X-ray cavity resonance and measurements using scanning electron microscopic and X-ray topographic techniques for crystal defects. Well defined resonance spectra of sapphire FPRs were successfully obtained, and were comparable with the theoretical predictions. PMID:27140144

  11. Deformation experiment on fayalite using deformation-Cubic Anvil, D-CAP 700, with synchrotron X rays

    NASA Astrophysics Data System (ADS)

    Ohnuma, R. S.; Ohtani, E.; Suzuki, A.; Kubo, T.; Doi, N.; Shimojuku, A.; Kato, T.; Kikegawa, T.

    2009-12-01

    Studies of the rheological properties of rocks and minerals are important for understanding the dynamics and evolution of the Earth’s mantle. A new deformation apparatus had been proposed by Durham et al. (2002) and the new apparatus is capable of deforming samples under confining pressure up to 15GPa. Basically, the new apparatus consists of the cubic-anvil apparatus known as the DIA and two differential rams, which is called the D-DIA. The system has been introduced into synchrotron X-ray beamlines, and a procedure for measuring stress and strain using synchrotron X-rays had been developed. So far, experiments using the deformation DIA with synchrotron X-rays have been conducted at only two beamlines, the GeoSoilEnviro CARS 13-BM-D beamline of the Advanced Photon Source and the X17B2 beamline of the National Synchrotron Light Source. So, we installed a deformation cubic anvil, D-CAP 700 at the 14C2 beamline of the Photon Factory, which is essentially similar to the conventional D-DIA system. The differential rams are driven by micro-discharge pumps, and the deformation cubic anvil component is driven by MAX-III 700ton press installed at the 14C2 beamline. Two differential rams are controlled by an oil pressure controller, and both of the pressure control and the displacement control are available. The displacements of two differential rams are measured by the stroke sensor attached to rams. An incident X-ray beam was monochromatized at energy of 50 keV by a monochromater. Strain is observed from transmitted X-ray imaging of sample using the YAG:Ce single crystal phosphor and the CCD camera. Stress is measured by analyzing the two dimensional diffraction patterns of samples. The two dimensional diffraction patterns are collected by an imaging plate. Using this new deformation apparatus, D-CAP 700 and the measurement system at the 14C2 beamline of the Photon Factory, we have conducted the deformation experiments of fayalite. Samples were deformed at a confining

  12. A seven-crystal Johann-type hard x-ray spectrometer at the Stanford Synchrotron Radiation Lightsource

    PubMed Central

    Sokaras, D.; Weng, T.-C.; Nordlund, D.; Alonso-Mori, R.; Velikov, P.; Wenger, D.; Garachtchenko, A.; George, M.; Borzenets, V.; Johnson, B.; Rabedeau, T.; Bergmann, U.

    2013-01-01

    We present a multicrystal Johann-type hard x-ray spectrometer (∼5–18 keV) recently developed, installed, and operated at the Stanford Synchrotron Radiation Lightsource. The instrument is set at the wiggler beamline 6-2 equipped with two liquid nitrogen cooled monochromators – Si(111) and Si(311) – as well as collimating and focusing optics. The spectrometer consists of seven spherically bent crystal analyzers placed on intersecting vertical Rowland circles of 1 m of diameter. The spectrometer is scanned vertically capturing an extended backscattering Bragg angular range (88°–74°) while maintaining all crystals on the Rowland circle trace. The instrument operates in atmospheric pressure by means of a helium bag and when all the seven crystals are used (100 mm of projected diameter each), has a solid angle of about 0.45% of 4π sr. The typical resolving power is in the order of \\documentclass[12pt]{minimal}\\begin{document}$\\frac{E}{\\Delta E} \\sim 10\\,000$\\end{document}EΔE∼10000. The spectrometer's high detection efficiency combined with the beamline 6-2 characteristics permits routine studies of x-ray emission, high energy resolution fluorescence detected x-ray absorption and resonant inelastic x-ray scattering of very diluted samples as well as implementation of demanding in situ environments. PMID:23742527

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

    NASA Astrophysics Data System (ADS)

    Tanaka, M.; Katsuya, Y.; Matsushita, Y.

    2013-03-01

    The focused-beam flat-sample method (FFM), which is a method for high-resolution and rapid synchrotron X-ray powder diffraction measurements by combination of beam focusing optics, a flat shape sample and an area detector, was applied for diffraction experiments with anomalous scattering effect. The advantages of FFM for anomalous diffraction were absorption correction without approximation, rapid data collection by an area detector and good signal-to-noise ratio data by focusing optics. In the X-ray diffraction experiments of CoFe2O4 and Fe3O4 (By FFM) using X-rays near the Fe K absorption edge, the anomalous scattering effect between Fe/Co or Fe2+/Fe3+ can be clearly detected, due to the change of diffraction intensity. The change of observed diffraction intensity as the incident X-ray energy was consistent with the calculation. The FFM is expected to be a method for anomalous powder diffraction.

  14. Constructing a multi-scan synchrotron X-ray microscope to study the function of osteocyte canaliculi in mouse bone

    SciTech Connect

    Nango, Nobuhito; Kubota, Shogo; Yashiro, Wataru; Momose, Atsushi; Takada, Yasunari; Matsuo, Koichi

    2012-07-31

    Formulating a multi-scan method applied to an X-ray microscope CT with synchrotron radiation, we attempted to analyze the 3D functional structure of osteocyte canaliculi inside the cortical bone of a mouse tibia. We employed a two-method combination to scan the same position of the specimen. To extract the internal bone canalicular structure, we first combined a Talbot interferometer with an X-ray microscope, and applied a differential phase imaging method to measure the absolute value of bone mineral around the canaliculi. Next, we used the X-ray microscope without the Talbot interferometer under a defocus condition, moving the specimen toward the zone plate by 6 mm. This defocus contrast method visualizes the canaliculi by emphasizing the edges of the bone. We performed CT scans by the two configurations and precisely aligned resultant 3D images so that the same position in the specimen is compared. We could extract the osteocyte canaliculi and evaluate the mineral density of their surroundings. The degree of mineralization varied for each osteocyte lacuna and canaliculus. The multi-scan microscopic X-ray CT is a powerful tool for analyzing bone mineralization.

  15. PREFACE: Exploring surfaces and buried interfaces of functional materials by advanced x-ray and neutron techniques Exploring surfaces and buried interfaces of functional materials by advanced x-ray and neutron techniques

    NASA Astrophysics Data System (ADS)

    Sakurai, Kenji

    2010-12-01

    updates on recent progress and global trends in the field. We planned to cover quite a wide area of surface and buried interface science with x-rays and neutrons. Following a great deal of discussion during the editing process, we have decided to change direction. As we intend to publish similar special issues on a frequent basis, we will not insist on editing this issue as systematic and complete collections of research. Many authors decided to write an ordinary research paper rather than an article including systematic accounts. Due to this change in policy, some authors declined to contribute, and the number of papers is now just 12. However, readers will find that the special issue gives an interesting collection of new original research in surface and buried interface studies with x-rays and neutrons. The 12 papers cover the following research topics: (1) polymer analysis by diffuse scattering; (2) discussion of the electrochemical solid--liquid interface by synchrotron x-ray diffraction; (3) analysis of capped nanodots by grazing incidence small-angle x-ray scattering (GISAXS); (4) discussion of the strain distribution in silicon by high-resolution x-ray diffraction; (5) study of mesoporous structures by a combination of x-ray reflectivity and GISAXS; (6) discussion of energy-dispersive x-ray reflectometry and its applications; (7) neutron reflectivity studies on hydrogen terminated silicon interface; (8) the fabrication and performance of a special mirror for water windows; (9) depth selective analysis by total-reflection x-ray diffraction; (10) nanoparticle thin films prepared by a gas deposition technique; (11) discussion of crystal truncation rod (CTR) scattering of semiconductor nanostructures; (12) magnetic structure analysis of thin films by polarized neutron reflectivity. While not discussed in the present special issue, x-ray and neutron techniques have made great progress. The most important steps forward have been in 2D/3D real-space imaging, and realtime

  16. Scanning X-ray fluorescent elemental microanalysis with synchrotron radiation in geochemical research

    NASA Astrophysics Data System (ADS)

    Darin, A.; Kalugin, I.; Zolotarev, K.

    2009-04-01

    The traditional XRF analysis with high limits of detection is limited in application for geochemical researches. Use of synchrotron radiation considerably expands its opportunities [1]. Since 1985 in BINP analytical works with syncrotron radiation from storage ring VEPP-3 are carried out. A plenty of methodical and research works with geochemical samples has been executed. The range of energy excitation 15 - 50 keV is now accessible, that allows to determine the following elements in geological samples weight from 1 mg: P, S, Cl, K, Ca, Ti (LD=50 ppm, St.dev.=5 ppm); V, Cr, Mn, Fe, Co, Ni (LD=5 ppm, St.dev.=0.5 ppm); Cu, Zn, Ga, Ge, As, Se (LD=0.5 ppm, St.dev.=0.05 ppm); Br, Rb, Sr, Y, Zr, Nb, Mo (LD=0.1 ppm, St.dev.=0.03 ppm); Ru, Rh, Pd, Ag (LD=0.05 ppm, St.dev.=0.01 ppm); Cd, In, Sn, Sb, Te, I (LD=0.1 ppm, St.dev.=0.03 ppm); Ba, La, Ce, Nd, Sm (LD=1.0 ppm, St.dev.=0.15 ppm); Pb, Bi, Th, U (LD=1 ppm, St.dev.=0.1 ppm). The analysis is carried out in some stages with use various energy of excitation (usually - 15-18, 22 - 25 and 40-45 keV). The first instrument of scanning X-ray fluorescent elemental microanalysis with synchrotron radiation from storage ring VEPP-3 (scan.XRFA-SR) was founded in BINP SB RAS in the 1988 and applied to study the spatial distribution of elements in geological samples [2]. Scan.XRFA-SR was used in paleoclimate reconstructions based on high-resolution sediments and tree-rings analysis [3, 4, 5]. Unique opportunities of XRF SR allow to carry out scanning microanalysis with spatial resolution ~ 10 micron. The set of analyzed elements and range of concentration are determined by selection of energy of excitation and time of measurement in a point. In recent years, has been studied many different geological samples: diamonds, xenolith, ferromanganese nodules, bottom sediments. Studies have demonstrated the unique ability of scanning XRFA-SR: a simultaneous analysis of more than 30 chemical elements with a spatial resolution of 10-50 microns

  17. High-Pressure X-ray Tomography Microscope: Synchrotron Computed Microtomography at High Pressure and Temperature

    SciTech Connect

    Wang, Y.; Uchida, T.; Westferro, F.; Rivers, M.L.; Gebhardt, J.; Lesher, C.E.; Sutton, S.R.

    2010-07-20

    A new apparatus has been developed for microtomography studies under high pressure. The pressure generation mechanism is based on the concept of the widely used Drickamer anvil apparatus, with two opposed anvils compressed inside a containment ring. Modifications are made with thin aluminum alloy containment rings to allow transmission of x rays. Pressures up to 8 GPa have been generated with a hydraulic load of 25 T. The modified Drickamer cell is supported by thrust bearings so that the entire pressure cell can be rotated under load. Spatial resolution of the high pressure tomography apparatus has been evaluated using a sample containing vitreous carbon spheres embedded in FeS matrix, with diameters ranging from 0.01 to 0.2 mm. Spheres with diameters as small as 0.02 mm were well resolved, with measured surface-to-volume ratios approaching theoretical values. The sample was then subject to a large shear strain field by twisting the top and bottom Drickamer anvils. Imaging analysis showed that detailed microstructure evolution information can be obtained at various steps of the shear deformation, allowing strain partition determination between the matrix and the inclusions. A sample containing a vitreous Mg{sub 2}SiO{sub 4} sphere in FeS matrix was compressed to 5 GPa, in order to evaluate the feasibility of volume measurement by microtomography. The results demonstrated that quantitative inclusion volume information can be obtained, permitting in situ determination of P-V-T equation of state for noncrystalline materials.

  18. Synchrotron X-ray Scattering Studies of Hydration Dynamics in a Synthetic Smectite Clay

    NASA Astrophysics Data System (ADS)

    Fossum, Jon Otto; Dimasi, Elaine; Maaloey, Knut Joergen; da Silva, Geraldo Jose

    2001-03-01

    We present studies of pressed bulk samples of the synthetic smectite clay Na-fluorohectorite[1]. Hydration dynamics was measured by observing mono layer by mono layer water intercalation in between stacked smectite platelets. Using NSLS beam line X22A at Brookhaven Nat. Lab., we have studied interlayer Bragg peaks as a function of temperatures between 0 and 130 deg C, and relative humidities at near 100near 0intercalated. Williamson-Hall analysis[2] suggests near perfectly stacked finite regions consisting of about 100 platelets, i.e about 0.1 micrometers, representing the solid framework for micro porosity in these samples. Transition dynamics in between stable mono layer conditions are characterized by simultaneous water mono layer Bragg as well as Hendricks-Teller random intercalation[3] peaks. Both scattering off surfaces in reflection, and scattering in transmission through the bulk were done, enabling us to distinguish the slow and fast time scales representing water transport in micro and nano pores respectively. Our bulk scattering experiments represent a novel approach within clay materials science X-ray studies. [1]J.O. Fossum in Soft Condensed Matter: Configurations, Dynamics and Functionality, A.T Skjeltorp and S.F. Edwards (eds.) 269-279, Kluwer Academic Publishers (2000) [2]G.K. Williamson and W.H. Hall, Acta Metallurgica 1, 22 (1953) [3]S. Hendricks and E. Teller, J.Chem.Phys. 10, 147 (1942)

  19. Metals distribution and investigation of L'vov platform surface using principal component analysis, multi-way principal component analysis, micro synchrotron radiation X-ray fluorescence spectrometry and scanning electron microscopy after the determination of Al in a milk slurry sample

    NASA Astrophysics Data System (ADS)

    Pereira-Filho, E. R.; Pérez, C. A.; Poppi, R. J.; Arruda, M. A. Z.

    2002-08-01

    This work describes the use of different strategies/techniques, such as scanning electron microscopy (SEM), multivariate analysis (principal component analysis (PCA) and multi-way PCA) and micro synchrotron radiation X-ray fluorescence (μSRXRF), in order to extract information about platform morphology, metals distribution on its surface, and the performance of conventional and permanent modifiers after slurry analyses using electrothermal atomic absorption spectrometry (ET AAS). With multivariate analysis it was possible to select Zr (500 μg for each 50 heating cycles) as a permanent chemical modifier for the determination of Al in milk powder slurry samples. Employing multi-way PCA and SEM, it was possible to note the differences in morphology between platforms permanently treated with Zr and those conventionally treated with Mg(NO 3) 2. The use of PCA and SEM also allowed finding similarities between new platforms, and those with and without Zr treatment. Using the μSRXRF it was possible to establish metals distribution on the L'vov platform and compare the performance of conventional [Mg(NO 3) 2] and permanent (Zr) modifiers.

  20. LPE grown LSO:Tb scintillator films for high-resolution X-ray imaging applications at synchrotron light sources

    NASA Astrophysics Data System (ADS)

    Cecilia, A.; Rack, A.; Douissard, P.-A.; Martin, T.; Dos Santos Rolo, T.; Vagovič, P.; Hamann, E.; van de Kamp, T.; Riedel, A.; Fiederle, M.; Baumbach, T.

    2011-08-01

    Within the project ScinTAX of the 6th framework program (FP6) of the European Commission (SCINTAX—STRP 033 427) we have developed a new thin single crystal scintillator for high-resolution X-ray imaging. The scintillator is based on a Tb-doped Lu2SiO5 (LSO) film epitaxially grown on an adapted substrate. The high density, effective atomic number and light yield of the scintillating LSO significantly improves the efficiency of the X-ray imaging detectors currently used in synchrotron micro-imaging applications. In this work we present the characterization of the scintillating LSO films in terms of their spatial resolution performance and we provide two examples of high spatial and high temporal resolution applications.

  1. Emphysema diagnosis using X-ray dark-field imaging at a laser-driven compact synchrotron light source

    PubMed Central

    Schleede, Simone; Meinel, Felix G.; Bech, Martin; Herzen, Julia; Achterhold, Klaus; Potdevin, Guillaume; Malecki, Andreas; Adam-Neumair, Silvia; Thieme, Sven F.; Bamberg, Fabian; Nikolaou, Konstantin; Bohla, Alexander; Yildirim, Ali Ö.; Loewen, Roderick; Gifford, Martin; Ruth, Ronald; Eickelberg, Oliver; Reiser, Maximilian; Pfeiffer, Franz

    2012-01-01

    In early stages of various pulmonary diseases, such as emphysema and fibrosis, the change in X-ray attenuation is not detectable with absorption-based radiography. To monitor the morphological changes that the alveoli network undergoes in the progression of these diseases, we propose using the dark-field signal, which is related to small-angle scattering in the sample. Combined with the absorption-based image, the dark-field signal enables better discrimination between healthy and emphysematous lung tissue in a mouse model. All measurements have been performed at 36 keV using a monochromatic laser-driven miniature synchrotron X-ray source (Compact Light Source). In this paper we present grating-based dark-field images of emphysematous vs. healthy lung tissue, where the strong dependence of the dark-field signal on mean alveolar size leads to improved diagnosis of emphysema in lung radiographs. PMID:23074250

  2. First Observation of Small Fractures on a Human Dried Proximal Phalanx by Synchrotron X-Ray Interference Radiography

    NASA Astrophysics Data System (ADS)

    Mori, Koichi; Hyodo, Kazuyuki; Shikano, Naoto; Ando, Masami

    1999-11-01

    By taking photographs using wiggler synchrotron radiation (SR),clear images of fine fissures on a human dried proximal phalanx wereobtained. This has never been achieved by the conventional X-raymethod. The 40 mm×40 mm exposure field used to coverthe object was prepared by magnifying the original SR beam crosssection (7 mm×7 mm) with two successive asymmetricreflections of Si crystals. The width of the fissures images wasapproximately 20 µm on medical X-ray film. These images can beexplained by X-ray phase contrast. This new method may enable anaccurate diagnostic method in the field of orthopedics, such as thatfor small fractures associated with a bruise.

  3. Aerosol-induced lung injuries observed by synchrotron radiation X-ray phase-contrast imaging technique

    NASA Astrophysics Data System (ADS)

    Yue, Weisheng; Zhang, Guilin; Liu, Ping; Sun, Jianqi; Hwu, Yeukuang; Je, Jung Ho; Tan, Mingguang; Li, Yan

    2007-09-01

    Adverse health effects are associated with the inhalation of a variety of atmospheric particles. To study the lung injuries caused by aerosol PM2.5, synchrotron radiation (SR) X-ray phase-contrast imaging technique was used. Nude mice were inoculated with PM2.5 samples collected from suburban area (JD), industrial area (BS) and traffic tunnel (DPQ) of Shanghai. From X-ray phase-contrast images of lung tissues, apart from blood vessels and structures of alveoli, even hemorrhage spots of several microns caused by the inflammation were clearly observed. The studies showed that the PM2.5 samples collected from the traffic tunnel (DPQ) produced higher level of lung injury, followed by the aerosol samples collected from industrial area (BS) and suburban area (JD). Our studies also helped us to understand the process of lung injuries caused by aerosol particles.

  4. Emphysema diagnosis using X-ray dark-field imaging at a laser-driven compact synchrotron light source.

    PubMed

    Schleede, Simone; Meinel, Felix G; Bech, Martin; Herzen, Julia; Achterhold, Klaus; Potdevin, Guillaume; Malecki, Andreas; Adam-Neumair, Silvia; Thieme, Sven F; Bamberg, Fabian; Nikolaou, Konstantin; Bohla, Alexander; Yildirim, Ali Ö; Loewen, Roderick; Gifford, Martin; Ruth, Ronald; Eickelberg, Oliver; Reiser, Maximilian; Pfeiffer, Franz

    2012-10-30

    In early stages of various pulmonary diseases, such as emphysema and fibrosis, the change in X-ray attenuation is not detectable with absorption-based radiography. To monitor the morphological changes that the alveoli network undergoes in the progression of these diseases, we propose using the dark-field signal, which is related to small-angle scattering in the sample. Combined with the absorption-based image, the dark-field signal enables better discrimination between healthy and emphysematous lung tissue in a mouse model. All measurements have been performed at 36 keV using a monochromatic laser-driven miniature synchrotron X-ray source (Compact Light Source). In this paper we present grating-based dark-field images of emphysematous vs. healthy lung tissue, where the strong dependence of the dark-field signal on mean alveolar size leads to improved diagnosis of emphysema in lung radiographs. PMID:23074250

  5. Development of synchrotron radiation x-ray intravital microscopy for in vivo imaging of rat heart vascular function.

    PubMed

    Umetani, Keiji; Pearson, James T; Schwenke, Daryl O; Shirai, Mikiyasu

    2011-01-01

    This study elucidates the vascular internal diameter response of coronary arterial circulation in closed-chest rats to evaluate endothelium-dependent and endothelium-independent vasodilatory ability and to investigate disease mechanisms. For this study, we developed an X-ray intravital microscopy system using a microangiography technique and a synchrotron radiation source at SPring-8. An X-ray direct-conversion type detector with 7-μm spatial resolution was used for real-time imaging. Microangiographic images were stored in a digital frame memory system at a maximum rate of 30 frame/s with a 1024 × 1024-pixel, 10-bit format. In imaging experiments, the small coronary arteries were visualized after iodine contrast agent injection into the coronary artery. PMID:22256145

  6. Synchrotron x-ray spectroscopy studies of valence and magnetic state in europium metal to extreme pressures

    SciTech Connect

    Bi, W.; Souza-Neto, N.M.; Haskel, D.; Fabbris, G.; Alp, E.E.; Zhao, J.; Hennig, R.G.; Abd-Elmeguid, M.M.; Meng, Y.; McCallum, Ralph W.; Dennis, Kevin; Schilling, J.S.

    2012-05-22

    In order to probe the changes in the valence state and magnetic properties of Eu metal under extreme pressure, x-ray absorption near-edge spectroscopy, x-ray magnetic circular dichroism, and synchrotron Mössbauer spectroscopy experiments were carried out. The Mössbauer isomer shift exhibits anomalous pressure dependence, passing through a maximum near 20 GPa. Density functional theory has been applied to give insight into the pressure-induced changes in both Eu's electronic structure and Mössbauer isomer shift. Contrary to previous reports, Eu is found to remain nearly divalent to the highest pressures reached (87 GPa) with magnetic order persisting to at least 50 GPa. These results should lead to a better understanding of the nature of the superconducting state found above 75 GPa and of the sequence of structural phase transitions observed to 92 GPa.

  7. On the feasibility of establishing the provenance of Australian Aboriginal artefacts using synchrotron radiation X-ray diffraction and proton-induced X-ray emission

    NASA Astrophysics Data System (ADS)

    Creagh, D. C.; Kubik, M. E.; Sterns, M.

    2007-09-01

    Museums and galleries in Australia have extensive collections of Aboriginal artefacts in their custody. In particular, the National Museum of Australia and the National Gallery of Australia are custodians of works of very considerable significance, in both cultural and financial terms. Art fraud can occur, documentation relating to artefacts can be mislaid, or the artefacts can be incorrectly filed. Because of this, it has become essential to establish protocols for the objective determination of the provenance of artefacts through scientific tests. For the work reported here we are concerned with the comparison of very small quantities of materials, paint scrapings from artefacts. Scrapings from artefacts of unknown provenance are compared with those from artefacts of known provenance, and the database established using an extended set of analytical techniques by Kubik. We describe here our use of synchrotron radiation X-ray diffraction (SR-XRD) to determine the mineral phase compositions of very small amounts of pigment material (<50 μg), and the use of PIXE to give their atomic compositions to a threshold level of 1 ppm for similar masses of material.

  8. Nanophase evolution at semiconductor/electrolyte interface in situ probed by time-resolved high-energy synchrotron x-ray diffraction.

    SciTech Connect

    Sun, Y.; Ren, Y.; Haeffner, D. R.; Almer, J. D.; Wang, L.; Yang, W.; Truong, T. T.

    2010-09-01

    Real-time evolution of nanoparticles grown at the semiconductor/electrolyte interface formed between a single crystalline n-type GaAs wafer and an aqueous solution of AgNO{sub 3} has been studied by using high-energy synchrotron X-ray diffraction. The results reveal the distinct nucleation and growth steps involved in the growth of anisotropic Ag nanoplates on the surface of the GaAs wafer. For the first time, a quick transit stage is observed to be responsible for the structural transformation of the nuclei to form structurally stable seeds that are critical for guiding their anisotropic growth into nanoplates. Reaction between a GaAs wafer and AgNO{sub 3} solution at room temperature primarily produces Ag nanoplates on the surface of the GaAs wafer in the dark and at room temperature. In contrast, X-ray irradiation can induce charge separation in the GaAs wafer to drive the growth of nanoparticles made of silver oxy salt (Ag{sub 7}NO{sub 11}) and silver arsenate (Ag{sub 3}AsO{sub 4}) at the semiconductor/electrolyte interface if the GaAs wafer is illuminated by the X-ray and reaction time is long enough.

  9. Crystallization temperature determination of Itokawa particles by plagioclase thermometry with X-ray diffraction data obtained by a high-resolution synchrotron Gandolfi camera

    NASA Astrophysics Data System (ADS)

    Tanaka, Masahiko; Nakamura, Tomoki; Noguchi, Takaaki; Nakato, Aiko; Ishida, Hatsumi; Yada, Toru; Shirai, Kei; Fujimura, Akio; Ishibashi, Yukihiro; Abe, Masanao; Okada, Tatsuaki; Ueno, Munetaka; Mukai, Toshifumi

    2014-02-01

    The crystallization temperatures of Itokawa surface particles recovered by the space probe Hayabusa were estimated by a plagioclase geothermometer using sodic plagioclase triclinicity. The Δ131-index required for the thermometer, which is the difference in X-ray diffraction peak positions between the 131 and 13¯1 reflections of plagioclase, was obtained by a high-resolution synchrotron Gandolfi camera developed for the third generation synchrotron radiation beamline, BL15XU at SPring-8. Crystallization temperatures were successfully determined from the Δ131-indices for four particles. The observed plagioclase crystallization temperatures were in a range from 655 to 660 °C. The temperatures indicate crystallization temperatures of plagioclases in the process of prograde metamorphism before the peak metamorphic stage.

  10. The effects of synchrotron x-rays on the local structure and the recrystallization of ion-damaged Si

    SciTech Connect

    Kin Man Yu; Lei Wang; Walukiewicz, W.

    1997-04-01

    Ion implantation is used extensively as a routine, controllable and reproducible doping technique for semiconductor processing. In Si, the amorphization by ion beams as well as the subsequent thermally induced solid phase epitaxy (SPE) and the electrical activation of the implanted dopants have been studied extensively. It has been well established that the SPE of amorphous Si ({alpha}-Si) layers created by implantation is initiated by thermal annealing at temperatures {ge} 400{degrees}C and proceeds in a planar fashion. The kinetics of the SPE process was found to follow an Arrhenius equation with an activation energy of 2.7eV. Various models have been proposed to explain the SPE process. In most cases, the mechanism leading to SPE is expected to involve the formation and/or motion of defects at or near the amorphous/crystalline interface. In this work the authors explore the effects of an intense x-ray beam generated by a synchrotron source on the SPE process of ion amorphized Si layers. A layer of amorphous Si was created near the surface of a single crystal Si to a depth of {approximately}2000{Angstrom} by 180keV Zn ion implantation. The sample was then irradiated at beam line 10-3 (microprobe beamline) at the Advance Light Source (ALS) for 5-16 hours. For 5-16 hours irradiation, the total photons absorbed by the {alpha}-Si film was {approximately}0.3-1 photon/Si atom (for 4keV photons). The authors find that in ion amorphized Si layers, although the ion dose is well above the amorphization threshold, small crystallites are still present. The absorption of x-ray by the Si atoms provides enough energy to disperse the small crystallites in the amorphous Si, reducing the number of interfacial defects as well as locally re-arrange the atoms to form a homogeneously amorphous layer with close to four-fold coordinated environment. This rearrangement in local structure of the {alpha}-Si results in nearly a defect-free crystal after SPE.

  11. The X-ray surface brightness of Kepler's supernova remnant

    NASA Technical Reports Server (NTRS)

    White, R. L.; Long, K. S.

    1983-01-01

    The first X-ray images of Kepler's supernova remnant (SN Ophiuchi 1604) are presented, and consequences for SNR models are discussed. Observations made with the Einstein Observatory Imaging Proportional Counter and High Resolution Imager show the remnant to be circular, with a strong shell brighter in the north than in the south. A flux of 1.2 x 10 to the -10th ergs/sq cm per sec was measured in the 0.15-4.5 keV region, which corresponds to an X-ray luminosity of 1.0 x 10 to the 36th ergs/sec at a distance of 5 kpc and an interstellar medium density of 2.8 x 10 to the 21st/sq cm. The X-ray observations do not allow the determination of whether the SNR is in the adiabatic or free expansion phase, but in either case it is shown that the mean ISM density must be greater than about 0.1/cu cm. In addition, the density of the X-ray emitting gas must be high, and its electron temperature must be fairly low. The high ISM densities derived for Kepler's SNR and other SNRs thus suggest an atypical ISM, possibly influenced by mass lost from the pre-supernova star.

  12. Surface structure determination of Pd on W(100) using X-ray photoelectron diffraction

    NASA Astrophysics Data System (ADS)

    Lussani, F. C.; de Siervo, A.; de Figueiredo, J. J. S.; Pancotti, A.; Landers, R.

    2011-11-01

    Ferromagnetic ordering in non-ferromagnetic transition metals induced by structural effects such as lattice expansion and stacking faults have been predicted by several theoretical studies. Different surfaces such as Nb(100), W(100) and C(0001) have been suggested as potential templates which could drive a Pd ultrathin film to a stable ferromagnetic state, depending on growth packing, film thickness and lateral lattice parameter. In this work we present an X-ray photoelectron diffraction (XPD) study of sub-monolayer to a few layers of Pd grown on W(100) and its surface structure determination. XPD patterns of Pd 3d and W 4f peaks were measured using synchrotron radiation with photon energy of 1810 eV provided by the SXS beamline at the Brazilian Synchrotron Light Laboratory. Our results indicate that the first few monolayers of Pd grow on W(100) with bcc packing and lateral lattice parameter dramatically changed in comparison with the Pd(fcc) bulk values. Based on these results we also present a discussion on the magnetic properties of this system derived from spin-polarized DFT calculation.

  13. Gadolinium Deposition in Nephrogenic Systemic Fibrosis: An Examination of Tissue using Synchrotron X-ray Fluorescence Spectroscopy

    SciTech Connect

    High, W.; Ranville, J; Brown, M; Punshon, T; Lanzirotti, A; Jackson, B

    2010-01-01

    Nephrogenic systemic fibrosis is a fibrosing disorder associated with gadolinium (Gd)-based contrast agents dosed during renal insufficiency. In two patients, Gd deposition in tissue affected by nephrogenic systemic fibrosis was quantified using inductively coupled plasma mass spectrometry. The presence of Gd was confirmed and mapped using synchrotron x-ray fluorescence spectroscopy. Affected skin and soft tissue from the lower extremity demonstrated 89 and 209 ppm ({micro}g/g, dry weight, formalin fixed) in cases 1 and 2, respectively. In case 2, the same skin and soft tissue was retested after paraffin embedding, with the fat content removed by xylene washes, and this resulted in a measured value of 189 ppm ({micro}g/g, dry weight, paraffin embedded). Synchrotron x-ray fluorescence spectroscopy confirmed Gd in the affected tissue of both cases, and provided high-sensitivity and high-resolution spatial mapping of Gd deposition. A gradient of Gd deposition in tissue correlated with fibrosis and cellularity. Gd deposited in periadnexal locations within the skin, including hair and eccrine ducts, where it colocalized to areas of high calcium and zinc content. Because of the difficulty in obtaining synchrotron x-ray fluorescence spectroscopy scans, tissue from only two patients were mapped. A single control with kidney disease and gadolinium-based contrast agent exposure did not contain Gd. Gd content on a gravimetric basis was impacted by processing that removed fat and altered the dry weight of the specimens. Gradients of Gd deposition in tissue corresponded to fibrosis and cellularity. Adnexal deposition of Gd correlated with areas of high calcium and zinc content.

  14. X-ray Talbot-Lau interferometer for high-speed phase imaging and tomography using white synchrotron radiation

    SciTech Connect

    Olbinado, Margie P.; Harasse, Sebastien; Yashiro, Wataru; Momose, Atsushi

    2012-07-31

    The Talbot interferometer using white synchrotron radiation has already been demonstrated for high-speed X-ray phase imaging and tomography as well as four-dimensional phase tomography for an observation of a dynamic specimen. In those previous experiments, the grating lines were oriented horizontally because the synchrotron radiation source size is large in the horizontal direction, and only the vertical spatial coherence satisfies the requirement for the operation of the Talbot interferometer given its distance from the source. For non-rigid samples, the horizontal axis of rotation causes unwanted motion of the sample due to gravity which results to artifact in the tomography reconstruction. For fluid samples, a vertical rotation axis is certainly necessary. While it is possible to orient the sample rotation axis perpendicular to the grating lines of the Talbot interferometer, solving the definite integral of the differential phase images to obtain the phase shift for x-ray phase tomography proves to be cumbersome when the sample extends outside the image and there is no null region for which the integration constant is known. In this work we aimed at increasing the spatial coherence of the x-rays along the horizontal so that the grating lines and the sample rotation axis could be oriented vertically. A Talbot-Lau interferometer was constructed by adding an absorption grating which acted as vertical line sources of horizontally spatially coherent white synchrotron radiation to the Talbot interferometer. An average of 20% moire fringe visibility was obtained. The set-up was demonstrated for highspeed phase tomography of a polymer sample.

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

    SciTech Connect

    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. Shortening x-ray pulses for pump-probe experiments at synchrotrons

    SciTech Connect

    Navirian, H. A.; Herzog, M.; Goldshteyn, J.; Shayduk, R.; Leitenberger, W.; Gaal, P.; Vrejoiu, I.; Khakhulin, D.; Wulff, M.; Bargheer, M.

    2011-06-15

    We implemented an experimental scheme for ultrafast x-ray diffraction at storage rings based on a laser-driven Bragg-switch that shortens the x-ray pulses emitted from an undulator. The increased time-resolution is demonstrated by observing changes of intensity, position and width of the diffraction peaks of a La{sub 0.7}Sr{sub 0.3}MnO{sub 3}/SrTiO{sub 3} superlattice sample after optical excitation, i.e., by quantitatively measuring the propagation of an expansion wave through the sample. These experimental transients with timescales of 35 to 60 ps evidence a reduction of the x-ray pulse duration by a factor of two.

  17. A Bayesian Approach to Surface X-ray Diffraction

    SciTech Connect

    Lyman, Paul F.; Saldin, Dilano K.

    2006-11-17

    We report on the development of an iterative method to directly invert surface x-ray diffraction (SXRD) data and thereby provide a map of electron density in the near-surface region of a solid. We have termed this method PARADIGM, which stands for Phase and Amplitude Recovery And Diffraction Image Generation Method. Significant advances in the PARADIGM theory were made during the grant period, and experimental milestones have also been achieved. The two components of the research program worked in concert, each spurring progress in the other. The method works by iteratively recovering the phases of surface scattering factors. Initially, random phases are assigned to the structure factors. After subtracting off the known bulk component, a Fourier transform converts these factors into an estimate of the real-space electron density map. This map is subjected to a support constraint, which holds that the electron density may only be non-zero near the solid surface. The modified electron density is then subjected to an inverse Fourier transform, and the bulk contributions are added back in. This renders an improved estimate of the phases of the surface structure factors. A constraint in reciprocal space is then applied, namely, the amplitudes of the scattering factors are set equal to the experimentally observed ones. This cycle is repeated, transforming between real and reciprocal space and applying constraints in each, until convergence is reached. The result renders a good initial model of the unknown surface structure. Such a direct method is important because conventional structural refinement methods rely on having a guess of the starting structure that sufficiently good that it may be refined into a model with the correct atomic positions. If the starting model has, for example, the wrong number or identity of atoms in the surface unit cell, it can never refine to the correct model. Even in cases where the starting model contains the correct number and identity

  18. X-ray intravital microscopy for functional imaging in rat hearts using synchrotron radiation coronary microangiography

    SciTech Connect

    Umetani, K.; Fukushima, K.

    2013-03-15

    An X-ray intravital microscopy technique was developed to enable in vivo visualization of the coronary, cerebral, and pulmonary arteries in rats without exposure of organs and with spatial resolution in the micrometer range and temporal resolution in the millisecond range. We have refined the system continually in terms of the spatial resolution and exposure time. X-rays transmitted through an object are detected by an X-ray direct-conversion type detector, which incorporates an X-ray SATICON pickup tube. The spatial resolution has been improved to 6 {mu}m, yielding sharp images of small arteries. The exposure time has been shortened to around 2 ms using a new rotating-disk X-ray shutter, enabling imaging of beating rat hearts. Quantitative evaluations of the X-ray intravital microscopy technique were extracted from measurements of the smallest-detectable vessel size and detection of the vessel function. The smallest-diameter vessel viewed for measurements is determined primarily by the concentration of iodinated contrast material. The iodine concentration depends on the injection technique. We used ex vivo rat hearts under Langendorff perfusion for accurate evaluation. After the contrast agent is injected into the origin of the aorta in an isolated perfused rat heart, the contrast agent is delivered directly into the coronary arteries with minimum dilution. The vascular internal diameter response of coronary arterial circulation is analyzed to evaluate the vessel function. Small blood vessels of more than about 50 {mu}m diameters were visualized clearly at heart rates of around 300 beats/min. Vasodilation compared to the control was observed quantitatively using drug manipulation. Furthermore, the apparent increase in the number of small vessels with diameters of less than about 50 {mu}m was observed after the vasoactive agents increased the diameters of invisible small blood vessels to visible sizes. This technique is expected to offer the potential for direct

  19. X-ray intravital microscopy for functional imaging in rat hearts using synchrotron radiation coronary microangiography

    NASA Astrophysics Data System (ADS)

    Umetani, K.; Fukushima, K.

    2013-03-01

    An X-ray intravital microscopy technique was developed to enable in vivo visualization of the coronary, cerebral, and pulmonary arteries in rats without exposure of organs and with spatial resolution in the micrometer range and temporal resolution in the millisecond range. We have refined the system continually in terms of the spatial resolution and exposure time. X-rays transmitted through an object are detected by an X-ray direct-conversion type detector, which incorporates an X-ray SATICON pickup tube. The spatial resolution has been improved to 6 μm, yielding sharp images of small arteries. The exposure time has been shortened to around 2 ms using a new rotating-disk X-ray shutter, enabling imaging of beating rat hearts. Quantitative evaluations of the X-ray intravital microscopy technique were extracted from measurements of the smallest-detectable vessel size and detection of the vessel function. The smallest-diameter vessel viewed for measurements is determined primarily by the concentration of iodinated contrast material. The iodine concentration depends on the injection technique. We used ex vivo rat hearts under Langendorff perfusion for accurate evaluation. After the contrast agent is injected into the origin of the aorta in an isolated perfused rat heart, the contrast agent is delivered directly into the coronary arteries with minimum dilution. The vascular internal diameter response of coronary arterial circulation is analyzed to evaluate the vessel function. Small blood vessels of more than about 50 μm diameters were visualized clearly at heart rates of around 300 beats/min. Vasodilation compared to the control was observed quantitatively using drug manipulation. Furthermore, the apparent increase in the number of small vessels with diameters of less than about 50 μm was observed after the vasoactive agents increased the diameters of invisible small blood vessels to visible sizes. This technique is expected to offer the potential for direct

  20. Using Synchrotron X-Ray Nano-CT to Characterize SOFC Electrode Microstructures in Three-Dimensions at Operating Temperature

    SciTech Connect

    Shearing, P.R.; Bradley, R.S.; Gelb, J.; Lee, S.N.; Atkinson, A.; Withers, P.J.; Brandon, N.P.

    2012-01-20

    In recent years, developments in tomography tools have provided unprecedented insight into the microstructure of electrodes for solid oxide fuel cells, enabling researchers to establish direct links between electrode microstructure and electrochemical performance. Here we present results of high resolution, synchrotron X-ray nano computed tomography experiments, which have enabled microstructural characterisation of a mixed ionic electronic conducting lanthanum strontium cobalt iron oxide (LSCF) cathode with sub-50nm resolution at operating temperature. Using the uniquely non-destructive nano-CT platform, it is possible to characterise microstructural evolution processes associated with heating and operation in-situ.

  1. Design of a humidity controlled sample stage for simultaneous conductivity and synchrotron X-ray scattering measurements

    NASA Astrophysics Data System (ADS)

    Jackson, Andrew; Beers, Keith M.; Chen, X. Chelsea; Hexemer, Alexander; Pople, John A.; Kerr, John B.; Balsara, Nitash P.

    2013-07-01

    We report on the design and operation of a novel sample stage, used to simultaneously measure X-ray scattering profiles and conductivity of a polymer electrolyte membrane (PEM) surrounded by humid air as a function of temperature and relative humidity. We present data obtained at the Advanced Light Source and Stanford Synchrotron Radiation Laboratory. We demonstrate precise humidity control and accurate determination of morphology and conductivity over a wide range of temperatures. The sample stage is used to study structure-property relationships of a semi-crystalline block copolymer PEM, sulfonated polystyrene-block-polyethylene.

  2. The use of X-ray fluorescence analysis with synchrotron radiation to measure elemental composition of phytomass and soils

    NASA Astrophysics Data System (ADS)

    Kutsenogyi, K. P.; Makarikova, R. P.; Milyutin, L. I.; Naumova, N. B.; Tarakanov, V. V.; Chankina, O. V.

    2007-05-01

    The method of X-ray fluorescence analysis with synchrotron radiation was used to estimate soil and phytomass elemental composition in the long-term field experiments with clones and climatypes of Scots pine Pinus sylvestris L. in West Siberia. Overall from 15 to 21 chemical elements (Fe, Ca, K, Ti, Mn, Zr, Sr, Rb, Co, Cr, Zn, V, Y, Sc, Nb, Pb, Ga, Cu, Ni, As, Mo) were detected. The elemental composition of dried needles and needle ash were compared. The influence of genetic variability of Scots pine on some element concentration in the topsoil was revealed. The temporal dynamics of interclonal variability of elemental composition of pine needles was revealed.

  3. A flow cell for in situ synchrotron x-ray diffraction studies of scale formation under Bayer processing conditions.

    PubMed

    Webster, Nathan A S; Madsen, Ian C; Loan, Melissa J; Scarlett, Nicola V Y; Wallwork, Kia S

    2009-08-01

    The design, construction, and commissioning of a stainless steel flow cell for in situ synchrotron x-ray diffraction studies of scale formation under Bayer processing conditions is described. The use of the cell is demonstrated by a study of Al(OH)(3) scale formation on a mild steel substrate from synthetic Bayer liquor at 70 degrees C. The cell design allows for interchangeable parts and substrates and would be suitable for the study of scale formation in other industrial processes. PMID:19725670

  4. In-situ Synchrotron X-ray Microdiffraction Study of Lattice Rotation in Polycrystalline Materials during Uniaxial Deformations

    SciTech Connect

    Joo, H.D.; Bark, C.W.; Koo, Y.M.; Kim, K.H.; Tamura, N.

    2004-05-12

    Recent experiments have shown that formation of dislocation cell structures and rotation of structural elements at the macroscopic level are fundamental to the development of plastic deformation. However, attention should also be focused on micro-volumes because local stress and strain can significantly differ from their averaged values at the macroscale. In-situ orientation measurements in copper polycrystals during uniaxial deformation were performed using synchrotron x-ray microdiffraction at the Advanced Light Source. We observed heterogeneities in deformation-induced microstructure within individual grains. Different slip systems in particular can be simultaneously activated among neighboring volume elements of individual grains.

  5. In-situ synchrotron X-ray microdiffraction study of lattice rotation in polycrystalline materials during uniaxial deformations

    SciTech Connect

    Joo, H.D.; Kim, K.H.; Bark, C.W.; Koo, Y.M.; Tamura, N.

    2004-07-19

    Recent experiments have shown that formation of dislocation cell structures and rotation of structural elements at the macroscopic level are fundamental to the development of plastic deformation. However, attention should also be focused on micro-volumes because local stress and strain can significantly differ from their averaged values at the macroscale. In-situ orientation measurements in copper polycrystals during uniaxial deformation were performed using synchrotron x-ray microdiffraction at the Advanced Light Source. We observed heterogeneities in deformation-induced microstructure within individual grains. Different slip systems in particular can be simultaneously activated among neighboring volume elements of individual grains.

  6. Characterization of dislocations in monoclinic hen egg-white lysozyme crystals by synchrotron monochromatic-beam X-ray topography

    NASA Astrophysics Data System (ADS)

    Sawaura, Takuya; Fujii, Daiki; Shen, Mengyuan; Yamamoto, Yu; Wako, Kei; Kojima, Kenichi; Tachibana, Masaru

    2011-03-01

    Dislocations in monoclinic hen egg-white lysozyme crystals were investigated by means of synchrotron monochromatic-beam X-ray topography. The loop and curved dislocations were observed to be predominant in the crystals. Almost all the dislocations lay in (1 0 1¯) crystallographic plane, which corresponds to that with smallest slicing energy estimated by macrobond approach. One of the Burgers vectors of the dislocations was determined to be [0 1 0], which corresponds to the smallest lattice translational vector on the (1 0 1¯) plane. It is suggested that the loop and curved dislocations are slip ones introduced by a stress concentration during or after the growth.

  7. Thermal equation of state of copper studied by high P-T synchrotron x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Wang, Yuejian; Zhang, Jianzhong; Xu, Hongwu; Lin, Zhijun; Daemen, Luke L.; Zhao, Yusheng; Wang, Liping

    2009-02-01

    The unit-cell volume of copper (Cu) has been measured by synchrotron x-ray at pressures and temperatures of up to 8.1 GPa and 1100 K. From pressure-volume-temperature (P-V-T) measurements, thermoelastic parameters of Cu were derived based on a modified high-T Birch-Murnaghan equation of state and a thermal pressure approach. The ambient bulk modulus derived from this work is comparable to previously reported value, whereas all other thermoelastic parameters of Cu have never been determined before. These results extend our knowledge of the fundamental thermophysical properties on Cu.

  8. Design, development and first experiments on the X-ray imaging beamline at Indus-2 synchrotron source RRCAT, India.

    PubMed

    Agrawal, A K; Singh, B; Kashyap, Y S; Shukla, M; Sarkar, P S; Sinha, Amar

    2015-11-01

    A full-field hard X-ray imaging beamline (BL-4) was designed, developed, installed and commissioned recently at the Indus-2 synchrotron radiation source at RRCAT, Indore, India. The bending-magnet beamline is operated in monochromatic and white beam mode. A variety of imaging techniques are implemented such as high-resolution radiography, propagation- and analyzer-based phase contrast imaging, real-time imaging, absorption and phase contrast tomography etc. First experiments on propagation-based phase contrast imaging and micro-tomography are reported. PMID:26524319

  9. Plastic deformation in Al (Cu) interconnects stressed by electromigration and studied by synchrotron polychromatic X-ray microdiffraction

    SciTech Connect

    Advanced Light Source; UCLA; Chen, Kai; Chen, Kai; Tamura, Nobumichi; Valek, Bryan C.; Tu, King-Ning

    2008-05-14

    We report here an in-depth synchrotron radiation based white beam X-ray microdiffraction study of plasticity in individual grains of an Al (Cu) interconnect during the early stage of electromigration. The study shows a rearrangement of the geometrically necessary dislocations (GND) in bamboo typed grains during that stage. We find that about 90percent of the GNDs are oriented so that their line direction is the closest to the current flow direction. In non-bamboo typed grains, the Laue peak positions shift, indicating that the grains rotate. An analysis in terms of force directions has been carried out and is consistent with observed electromigration induced grain rotation and bending.

  10. Characterization of an x-ray phase contrast imaging system based on the miniature synchrotron MIRRORCLE-6X

    SciTech Connect

    Heekeren, Joop van; Kostenko, Alexander; Hanashima, Takayasu; Yamada, Hironari; Stallinga, Sjoerd; Offerman, S. Erik; Vliet, Lucas J. van

    2011-09-15

    Purpose: The implementation of in-line x-ray phase contrast imaging (PCI) for soft-tissue patient imaging is hampered by the lack of a bright and spatially coherent x-ray source that fits into the hospital environment. This article provides a quantitative characterization of the phase-contrast enhancement of a PCI system based on the miniature synchrotron technology MIRRORCLE-6X. Methods: The phase-contrast effect was measured using an edge response of a plexiglass plate as a function of the incident angle of radiation. We have developed a comprehensive x-ray propagation model based on the system's components, properties, and geometry in order to interpret the measurement data. Monte-Carlo simulations are used to estimate the system's spectral properties and resolution. Results: The measured ratio of the detected phase-contrast to the absorption contrast is currently in the range 100% to 200%. Experiments show that with the current implementation of the MIRRORCLE-6X, a target smaller than 30-40 {mu}m does not lead to a larger phase-contrast. The reason for this is that the fraction of x-rays produced by the material (carbon filament and glue) that is used for mounting the target in the electron beam is more than 25% of the total amount of x-rays produced. This increases the apparent source size. The measured phase-contrast is at maximum two times larger than the absorption contrast with the current set-up. Conclusions: Calculations based on our model of the present imaging system predict that the phase-contrast can be up to an order of magnitude larger than the absorption contrast in case the materials used for mounting the target in the electron beam do not (or hardly) produce x-rays. The methods described in this paper provide vital feedback for guiding future modifications to the design of the x-ray target of MIRRORCLE-type system and configuration of the in-line PCI systems in general.

  11. Soft x-ray emission spectra of lithium fluoride excited by synchrotron radiation

    SciTech Connect

    Tsang, K.L.; Zhang, C.H.; Callcott, T.A.; Arakawa, E.T.; Ederer, D.L.

    1986-01-01

    A core excited Li atom is perhaps the simplest cation defect that can be introduced into LiF. It frequently binds an electron in an electronic state, whose properties dominate both the soft x-ray absorption and soft x-ray emission properties of LiF. This phenomena was examined using a new, very high efficiency, emission spectrometer. Exciton and valence band peaks were observed which decay with time and are replaced by a metallic Li peak at 54 eV.

  12. In Situ Synchrotron X-Ray Techniques for the Study of Lithium Battery Materials

    SciTech Connect

    McBreen, J.; Mukerjee, S.; Yang, X. Q.; Sun, X., Ein-Eli, Y.

    1998-11-01

    The combination of in situ X-ray diffraction (XRD) and x-ray absorption spectroscopy (XAS) is a very powerful technique in the study of lithium battery cathode materials. XRD identifies the phase changes that occur during cycling and XAS gives information on the redox charge compensation processes that occur on the transition metal oxides. Because of its element specific nature XAS can identify the occurrence of redox processes on the various cations in doped oxide cathode materials. Since XAS probes short range order and is particularly useful in the study of amorphous tin based composite oxide anode materials.

  13. Considerations for the use of synchrotron radiation sources to measure sub-keV x-ray photoabsorption cross sections in transmission

    SciTech Connect

    Tirsell, K.G.; Del Grande, N.K.

    1988-02-01

    Sub-keV x-ray photoabsorption cross section measurements in transmission have been made using synchrotron radiation beam lines on the VUV storage ring at the National Synchrotron Light Source (NSLS) and on the SPEAR storage ring at Stanford. The experimental considerations associated with making absolute measurements are reviewed, along with techniques for resolving difficulties. Suggestions for future measurements are included.

  14. [Quantitative structure characteristics and fractal dimension of Chinese medicine granules measured by synchrotron radiation X-ray computed micro tomography].

    PubMed

    Lu, Xiao-long; Zheng, Qin; Yin, Xian-zhen; Xiao, Guang-qing; Liao, Zu-hua; Yang, Ming; Zhang, Ji-wen

    2015-06-01

    The shape and structure of granules are controlled by the granulation process, which is one of the main factors to determine the nature of the solid dosage forms. In this article, three kinds of granules of a traditional Chinese medicine for improving appetite and promoting digestion, namely, Jianwei Granules, were prepared using granulation technologies as pendular granulation, high speed stirring granulation, and fluidized bed granulation and the powder properties of them were investigated. Meanwhile, synchrotron radiation X-ray computed micro tomography (SR-µCT) was applied to quantitatively determine the irregular internal structures of the granules. The three-dimensional (3D) structure models were obtained by 3D reconstruction, which were more accurately to characterize the three-dimensional structures of the particles through the quantitative data. The models were also used to quantitatively compare the structural differences of granules prepared by different granulation processes with the same formula, so as to characterize how the production process plays a role in the pharmaceutical behaviors of the granules. To focus on the irregularity of the particle structure, the box counting method was used to calculate the fractal dimensions of the granules. The results showed that the fractal dimension is more sensitive to reflect the minor differences in the structure features than the conventional parameters, and capable to specifically distinct granules in structure. It is proved that the fractal dimension could quantitatively characterize the structural information of irregular granules. It is the first time suggested by our research that the fractal dimension difference (Df,c) between two fractal dimension parameters, namely, the volume matrix fractal dimension and the surface matrix fractal dimension, is a new index to characterize granules with irregular structures and evaluate the effects of production processes on the structures of granules as a new

  15. Orientation and Mg Incorporation of Calcite Grown on Functionalized Self-Assembled Monolayers: A Synchrotron X-ray Study

    SciTech Connect

    Kwak,S.; DiMasi, E.; Han, Y.; Aizenberg, J.; Kuzmenko, I.

    2005-01-01

    Calcite crystals were nucleated from MgCl2/CaCl2 solutions onto functionalized self-assembled monolayers adsorbed onto E-beam evaporated Au films. Synchrotron X-ray scattering studies of the crystals reveal new information about preferred orientation and Mg incorporation. The Au [111] axis is distributed within 2.6 degrees of the film surface normal, but the oriented crystals may be tilted up to 6 degrees away from this axis. For low Mg{sup 2+} content, SO{sub 3}--functionalized films nucleated primarily near the (106) calcite face, odd-chain-length carboxylic acid terminated alkanethiol films nucleated near the (012) face, and even-chain-length carboxylic acid terminated alkanethiol films nucleated near the (113) face. [Mg{sup 2+}]/[Ca{sup 2+}] concentration ratios (n) of 2 and greater defeated this preferred orientation and created a powder texture. Diffraction patterns within the layer plane from the coarse calcite powders indicated a shift to higher 2 accompanied by peak broadening with increasing n. For 0.5 < n < 3.5, a double set of calcite peaks is observed, showing that two distinct Mg calcite phases form: one of comparatively lower Mg content, derived from the templated crystals, and a Mg-rich phase derived from amorphous precursor particles. According to the refinement of lattice parameters, Mg incorporation of up to 18 mol % occurs for n = 4, independent of film functionality. We discuss the differences between the differently functionalized monolayers and also introduce the hypothesis that two separate routes to Mg calcite formation occur in this system.

  16. Upgraded X-ray topography and microtomography beamline at the Kurchatov synchrotron radiation source

    SciTech Connect

    Senin, R. A. Khlebnikov, A. S.; Vyazovetskova, A. E.; Blinov, I. A.; Golubitskii, A. O.; Kazakov, I. V.; Vorob'ev, A. A.; Buzmakov, A. V.; Asadchikov, V. E.; Shishkov, V. A.; Mukhamedzhanov, E. Kh.; Kovalchuk, M. V.

    2013-05-15

    An upgraded X-ray Topography and Microtomography (XRT-MT) station is described, the parameters of the optical schemes and detectors are given, and the experimental possibilities of the station are analyzed. Examples of tomographic reconstructions are reported which demonstrate spatial resolutions of 2.5 and 10 {mu}m at fields of view of 2.5 and 10 mm, respectively.

  17. High-speed X-ray imaging pixel array detector for synchrotron bunch isolation

    PubMed Central

    Philipp, Hugh T.; Tate, Mark W.; Purohit, Prafull; Shanks, Katherine S.; Weiss, Joel T.; Gruner, Sol M.

    2016-01-01

    A wide-dynamic-range imaging X-ray detector designed for recording successive frames at rates up to 10 MHz is described. X-ray imaging with frame rates of up to 6.5 MHz have been experimentally verified. The pixel design allows for up to 8–12 frames to be stored internally at high speed before readout, which occurs at a 1 kHz frame rate. An additional mode of operation allows the integration capacitors to be re-addressed repeatedly before readout which can enhance the signal-to-noise ratio of cyclical processes. This detector, along with modern storage ring sources which provide short (10–100 ps) and intense X-ray pulses at megahertz rates, opens new avenues for the study of rapid structural changes in materials. The detector consists of hybridized modules, each of which is comprised of a 500 µm-thick silicon X-ray sensor solder bump-bonded, pixel by pixel, to an application-specific integrated circuit. The format of each module is 128 × 128 pixels with a pixel pitch of 150 µm. In the prototype detector described here, the three-side buttable modules are tiled in a 3 × 2 array with a full format of 256 × 384 pixels. The characteristics, operation, testing and application of the detector are detailed. PMID:26917125

  18. High-speed X-ray imaging pixel array detector for synchrotron bunch isolation.

    PubMed

    Philipp, Hugh T; Tate, Mark W; Purohit, Prafull; Shanks, Katherine S; Weiss, Joel T; Gruner, Sol M

    2016-03-01

    A wide-dynamic-range imaging X-ray detector designed for recording successive frames at rates up to 10 MHz is described. X-ray imaging with frame rates of up to 6.5 MHz have been experimentally verified. The pixel design allows for up to 8-12 frames to be stored internally at high speed before readout, which occurs at a 1 kHz frame rate. An additional mode of operation allows the integration capacitors to be re-addressed repeatedly before readout which can enhance the signal-to-noise ratio of cyclical processes. This detector, along with modern storage ring sources which provide short (10-100 ps) and intense X-ray pulses at megahertz rates, opens new avenues for the study of rapid structural changes in materials. The detector consists of hybridized modules, each of which is comprised of a 500 µm-thick silicon X-ray sensor solder bump-bonded, pixel by pixel, to an application-specific integrated circuit. The format of each module is 128 × 128 pixels with a pixel pitch of 150 µm. In the prototype detector described here, the three-side buttable modules are tiled in a 3 × 2 array with a full format of 256 × 384 pixels. The characteristics, operation, testing and application of the detector are detailed. PMID:26917125

  19. The theoretical reflectance of X-rays from optical surfaces

    NASA Technical Reports Server (NTRS)

    Neergaard, J. R.; Reynolds, J. M.; Fields, S. A.

    1976-01-01

    The theoretical reflectance of X-rays from various materials and evaporated films is presented. A computer program was written that computes the reflected intensity as a function of the angle of the incident radiation. The quantities necessary to generate the efficiency and their effect on the data are demonstrated. Five materials were chosen for evaluation: (1) fused silica, (2) chromium, (3) beryllium, (4) gold, and (5) a thin layer contaminant. Fused silica is a versatile and common material; chromium has high reflection efficiency at X-ray wavelengths and is in the middle of the atomic number range; beryllium contains a single atomic shell and has a low range atomic number; gold contains multiple atomic shells and has a high atomic number; the contaminant is treated as a thin film in the calculations and results are given as a function of thickness for selected wavelengths. The theoretical results are compared to experimental data at lambda = 8.34 A.

  20. Repeatability and reproducibility of intracellular molar concentration assessed by synchrotron-based x-ray fluorescence microscopy

    NASA Astrophysics Data System (ADS)

    Merolle, L.; Malucelli, E.; Fratini, M.; Gianoncelli, A.; Notargiacomo, A.; Cappadone, C.; Farruggia, G.; Sargenti, A.; Procopio, A.; Lombardo, M.; Lagomarsino, S.; Iotti, S.

    2016-01-01

    Elemental analysis of biological sample can give information about content and distribution of elements essential for human life or trace elements whose absence is the cause of abnormal biological function or development. However, biological systems contain an ensemble of cells with heterogeneous chemistry and elemental content; therefore, accurate characterization of samples with high cellular heterogeneity may only be achieved by analyzing single cells. Powerful methods in molecular biology are abundant, among them X-Ray microscopy based on synchrotron light source has gaining increasing attention thanks to its extremely sensitivity. However, reproducibility and repeatability of these measurements is one of the major obstacles in achieving a statistical significance in single cells population analysis. In this study, we compared the elemental content of human colon adenocarcinoma cells obtained by three distinct accesses to synchrotron radiation light.