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Sample records for surfaces synchrotron x-ray

  1. (Synchrotron studies of x-ray reflectivity from surfaces)

    SciTech Connect

    Pershan, P.S.

    1992-03-03

    Following a long period of theoretical interest, but only limited measurements, there has recently been an increased number of attempts to expand the relative paucity of experimental information on the structure of liquid surfaces using techniques as diverse as ellipsometry, micro-force balances, non-linear optics, Auger and photoelectron spectroscopy, and x-ray scattering. Our group has played a leading role in the currently expanding application of scattering techniques to the general problem of characterizing the microscopic structure of liquid surfaces and we propose here that this work be extended specifically to liquid metals. In the following sections we will briefly describe the salient features of x-ray scattering that are relevant to the current project, the progress that we have made in the current grant period and the work that we propose to carry out in the forthcoming grant period.

  2. 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.

  3. 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.

  4. Semiconductor surface and interface dynamics studied in real time by synchrotron x-ray diffraction

    SciTech Connect

    Braun, Wolfgang; Ploog, Klaus H.

    2007-06-14

    We present an overview of in-situ experiments to study molecular beam epitaxial growth by x-ray diffraction and high-energy electron diffraction. The applicability of kinematic theory allows a quantitative evaluation of the surface kinetics on compound semiconductor surfaces; GaAs(001), InAs(001) and GaSb(001) are presented as examples. Both the growth in the layer-by-layer mode and the recovery can be analyzed in considerable detail. As an example of heteroepitaxy, the nucleation and relaxation of hexagonal MnAs on GaAs(001) is presented. We find an extremely anisotropic interface structure with a periodic array of misfit dislocations that can be quantitatively analyzed.

  5. 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.

  6. 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.

  7. 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

  8. 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.

  9. 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.

  10. Substrate surface effect on the structure of cubic BN thin films from synchrotron-based X-ray diffraction and reflection

    NASA Astrophysics Data System (ADS)

    Zhang, X. M.; Wen, W.; Li, X. L.; He, Q.; Zhou, X. T.

    2013-02-01

    Cubic BN (cBN) thin films prepared by mass-selected ion beam deposition technique (MSIBD) on Si substrates with different surface roughness were studied by synchrotron-based grazing incidence X-ray diffraction (GI-XRD) and X-ray reflectivity (XRR) measurements. The BN films are mostly composed of two phases. One is cBN phase, the other is hexagonal BN (hBN) phase. The cubic phase content of the thin films is dependent on the roughness of their corresponding substrates. The smooth substrate surface is helpful for the nucleation of the cBN phase. cBN phase is mostly grown in the near surface region of the films and there is a hBN interlayer at the film-substrate interface. GIXRD and XRR are proved to be powerful tools for analyzing the structure of the cBN thin films.

  11. Observation of ultralow-level Al impurities on a silicon surface by high-resolution grazing emission x-ray fluorescence excited by synchrotron radiation

    SciTech Connect

    Kubala-Kukus, A.; Banas, D.; Pajek, M.; Cao, W.; Dousse, J.-Cl.; Hoszowska, J.; Kayser, Y.; Szlachetko, M.; Salome, M.; Susini, J.; Szlachetko, J.

    2009-09-15

    We demonstrate that ultralow-level Al impurities on a silicon surface can be measured by using the high-resolution grazing emission x-ray fluorescence (GEXRF) technique combined with synchrotron-radiation excitation. An Al-impurity level of about 10{sup 12} atoms/cm{sup 2} was reached by observing the Al K{alpha} x-ray fluorescence in the resonant Raman-scattering background-''free'' regime by choosing an appropriate beam energy below the Si K absorption edge. Present results show that by combining the GEXRF method with the vapor phase decomposition technique the 10{sup 7} atoms/cm{sup 2} level can be reached for Al detection on silicon. Finally, we found that the high-resolution GEXRF technique is a sensitive tool to study the morphology of surface nanostructures.

  12. Synchrotron x-ray fluorescence and extended x-ray absorption fine structure analysis

    SciTech Connect

    Chen, J.R.; Gordon, B.M.; Hanson, A.L.; Jones, K.W.; Kraner, H.W.; Chao, E.C.T.; Minkin, J.A.

    1984-01-01

    The advent of dedicated synchrotron radiation sources has led to a significant increase in activity in many areas of science dealing with the interaction of x-rays with matter. Synchrotron radiation provides intense, linearly polarized, naturally collimated, continuously tunable photon beams, which are used to determine not only the elemental composition of a complex, polyatomic, dilute material but also the chemical form of the elements with improved accuracy. Examples of the application of synchrotron radiation include experiments in synchrotron x-ray fluorescence (SXRF) analysis and extended x-ray absorption fine structure (EXAFS) analysis. New synchrotron radiation x-ray microprobes for elemental analysis in the parts per billion range are under construction at several laboratories. 76 references, 24 figures.

  13. 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.

  14. Fabrication of X-ray mirrors for synchrotron applications

    NASA Astrophysics Data System (ADS)

    Thiess, H.; Lasser, H.; Siewert, F.

    2010-05-01

    Application of conic section geometries play an important role for soft X-ray synchrotron beams. Mirror design for collimation or focusing under stringent boundary conditions may end up with very aspheric geometries. In particular, the aspheric departure of these surfaces from "base geometries" in combination with high-quality requirements for slope and roughness is challenging. Mirror manufacturing of very aspheric mirrors at Carl Zeiss Laser Optics will be illustrated by recent examples. Fabrication issues of ellipsoids and 2D-parabolas are discussed. In addition, the close interaction of metrology and polishing will be highlighted.

  15. 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

  16. 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.

  17. 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

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

    PubMed

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

    2014-07-01

    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.

  19. 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.

  20. 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

  1. SYNCHROTRON X - RAY OBSERVATIONS OF A MONOLAYER TEMPLATE FOR MINERALIZATION.

    SciTech Connect

    DIMASI,E.; GOWER,L.B.

    2000-11-27

    Mineral nucleation at a Langmuir film interface has been studied by synchrotron x-ray scattering. Diluted calcium bicarbonate solutions were used as subphases for arachidic and stearic acid monolayers, compressed in a Langmuir trough. Self-assembly of the monolayer template is observed directly, and subsequent crystal growth monitored in-situ.

  2. X-ray microscopy using collimated and focussed synchrotron radiation

    SciTech Connect

    Jones, K.W.; Kwiatek, W.M.; Gordon, B.M.; Hanson, A.L.; Pounds, J.G.; Rivers, M.L.; Sutton, S.R.; Thompson, A.C.; Underwood, J.H.; Giauque, R.D.

    1987-01-01

    X-ray microscopy is a field that has developed rapidly in recent years. Two different approaches have been used. Zone plates have been employed to produce focused beams with sizes as low as 0.07 ..mu..m for x-ray energies below 1 keV. Images of biological materials and elemental maps for major and minor low Z have been produced using above and below absorption edge differences. At higher energies collimators and focusing mirrors have been used to make small diameter beams for excitation of characteristic K- or L-x rays of all elements in the periodic table. The practicality of a single instrument combining all the features of these two approaches is unclear. The use of high-energy x rays for x-ray microscopy has intrinsic value for characterization of thick samples and determination of trace amounts of most elements. A summary of work done on the X-26 beam line at the National Synchrotron Light Source (NSLS) with collimated and focused x rays with energies above 4 keV is given here. 6 refs., 5 figs., 1 tab.

  3. Rapid combinatorial screening by synchrotron X-ray imaging

    NASA Astrophysics Data System (ADS)

    Eba, Hiromi; Sakurai, Kenji

    2006-01-01

    An X-ray imaging system, which does not require any scans of the sample or an X-ray beam and which, therefore, dramatically reduces the amount of time required, was employed to evaluate combinatorial libraries efficiently. Two-dimensional X-ray fluorescence (XRF) images of an 8 mm × 8 mm area were observed for combinatorial substrates of manganese-cobalt spinel MnCo 2O 4 and lithium ferrite LiFeO 2 via an exposure time of 1-3 s using synchrotron X-rays. Thus, XRF signals from a whole substrate could be observed at once in a short space of time. In order to observe the chemical environment simultaneously for all materials arranged on the substrate, the fluorescent X-ray absorption fine structure (XAFS) was measured by repeating the imaging during the monochromator scans across the absorption edge for metals. This is extremely efficient because XAFS spectra for all materials placed on the common substrate are obtained from only a single energy scan. One can determine the valence numbers, as well as other aspects of the chemical environment of the metal included in each material, from the differences in spectral features and the energy shifts. Hence, combinatorial libraries can be screened very rapidly, and therefore efficiently, using the X-ray imaging system.

  4. CCD sensors in synchrotron X-ray detectors

    NASA Astrophysics Data System (ADS)

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

    1988-04-01

    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 2 can be imaged on a 2 cm 2 CCD. With a conversion efficiency of ˜ 1 CCD electron/X-ray photon, a peak saturation capacity of > 10 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 × 10 6 pixels/s and the shift rate in the parallel registers is 10 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 a rate of ˜ 1 frame/s or a complete 3-dimensional data set from a single crystal in ˜ 2 min. In electron energy-loss spectroscopy (EELS), the CCD was used in a parallel detection mode which is similar to the mode array detectors are used in dispersive EXAFS. With a beam current corresponding to 3 × 10 9 electron/s on the detector, a series of 64 spectra were recorded on the CCD in a continuous sequence without interruption due to readout. The frame-to-frame pixel signal fluctuations had σ = 0.4% from which DQE = 0.4 was obtained, where the detector conversion efficiency was 2.6 CCD electrons/X-ray photon. These multiple frame series also showed the time-resolved modulation of the electron microscope optics by stray magnetic fields.

  5. 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.

  6. 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.

  7. 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)

  8. 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.

  9. 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.

  10. 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.

  11. Synchrotron X-ray Microbeam Diffraction from Abalone Shell

    NASA Astrophysics Data System (ADS)

    Dimasi, Elaine; Sarikaya, Mehmet

    2004-03-01

    Microstructured biomaterials such as mollusk shells receive much attention, due to the promise that advanced materials can be designed and synthesized with biomimetic techniques that take advantage of self-assembly and aqueous, ambient processing conditions. A satisfactory understanding of this process requires characterization of the microstructure at the growth fronts where control over crystal orientation and morphology is enacted. We present synchrotron x-ray microbeam observations near the nacre-prismatic interface of red abalone shell (Haliotis rufescens). The relative orientations of calcite and aragonite grains exhibit differences from the idealizations reported previously. Long calcite grains impinge the boundary at 45^rc angles, suggestive of nucleation on (104) planes followed by c-axis growth. Within 100 μm of the boundary, crystals lose their bulk orientational order. The calcite crystal mosaic measured by x-ray diffraction rocking curves is resolution limited, comparable to geological calcite.

  12. 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.

  13. 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.

  14. 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.

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

    NASA Astrophysics Data System (ADS)

    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.

  16. In situ synchrotron based x-ray techniques as monitoring tools for atomic layer deposition

    SciTech Connect

    Devloo-Casier, Kilian Detavernier, Christophe; Dendooven, Jolien

    2014-01-15

    Atomic layer deposition (ALD) is a thin film deposition technique that has been studied with a variety of in situ techniques. By exploiting the high photon flux and energy tunability of synchrotron based x-rays, a variety of new in situ techniques become available. X-ray reflectivity, grazing incidence small angle x-ray scattering, x-ray diffraction, x-ray fluorescence, x-ray absorption spectroscopy, and x-ray photoelectron spectroscopy are reviewed as possible in situ techniques during ALD. All these techniques are especially sensitive to changes on the (sub-)nanometer scale, allowing a unique insight into different aspects of the ALD growth mechanisms.

  17. Synchrotron energy-dispersive X-ray diffraction tomography

    NASA Astrophysics Data System (ADS)

    Hall, C.; Barnes, P.; Cockcroft, J. K.; Colston, S. L.; Häusermann, D.; Jacques, S. D. M.; Jupe, A. C.; Kunz, M.

    1998-04-01

    Energy-dispersive diffraction tomography using white-beam synchrotron X-rays with energies up to 140 keV yields images of the interior features of solid objects up to 50 mm thick. The volume sampled is determined by the geometry of the diffracting lozenge defined by the incident beam, the detector system collimation and the Bragg angle. Using conventional beam slits to form a highly collimated 50 μm × 50 μm incident beam and a 40 μm collimator aperture, we demonstrate on a PEEK phantom that a lateral resolution (transverse to the beam direction) of a few microns can be achieved. The resolution in the direction of the incident beam is necessarily poorer than this since the diffracting lozenge is elongated in this direction, with length increasing rapidly at small angles. There is no evidence of significant contamination of the diffracted intensity by the effects of multiple scattering from outside the primary lozenge.

  18. 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.

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

    NASA Astrophysics Data System (ADS)

    Koval'chuk, M. V.; Yatsishina, E. B.; Blagov, A. E.; Tereshchenko, E. Yu.; Prosekov, P. A.; Dyakova, Yu. A.

    2016-09-01

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

  20. 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.

  1. 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).

  2. 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.

  3. 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

  4. 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.

  5. Characterization of a next-generation piezo bimorph X-ray mirror for synchrotron beamlines

    PubMed Central

    Alcock, Simon G.; Nistea, Ioana; Sutter, John P.; Sawhney, Kawal; Fermé, Jean-Jacques; Thellièr, Christophe; Peverini, Luca

    2015-01-01

    Piezo bimorph mirrors are versatile active optics used on many synchrotron beamlines. However, many bimorphs suffer from the ‘junction effect’: a periodic deformation of the optical surface which causes major aberrations to the reflected X-ray beam. This effect is linked to the construction of such mirrors, where piezo ceramics are glued directly below the thin optical substrate. In order to address this problem, a next-generation bimorph with piezos bonded to the side faces of a monolithic substrate was developed at Thales-SESO and optimized at Diamond Light Source. Using metrology feedback from the Diamond-NOM, the optical slope error was reduced to ∼0.5 µrad r.m.s. for a range of ellipses. To maximize usability, a novel holder was built to accommodate the substrate in any orientation. When replacing a first-generation bimorph on a synchrotron beamline, the new mirror significantly improved the size and shape of the reflected X-ray beam. Most importantly, there was no evidence of the junction effect even after eight months of continuous beamline usage. It is hoped that this new design will reinvigorate the use of active bimorph optics at synchrotron and free-electron laser facilities to manipulate and correct X-ray wavefronts. PMID:25537582

  6. Characterization of a next-generation piezo bimorph X-ray mirror for synchrotron beamlines.

    PubMed

    Alcock, Simon G; Nistea, Ioana; Sutter, John P; Sawhney, Kawal; Fermé, Jean Jacques; Thellièr, Christophe; Peverini, Luca

    2015-01-01

    Piezo bimorph mirrors are versatile active optics used on many synchrotron beamlines. However, many bimorphs suffer from the `junction effect': a periodic deformation of the optical surface which causes major aberrations to the reflected X-ray beam. This effect is linked to the construction of such mirrors, where piezo ceramics are glued directly below the thin optical substrate. In order to address this problem, a next-generation bimorph with piezos bonded to the side faces of a monolithic substrate was developed at Thales-SESO and optimized at Diamond Light Source. Using metrology feedback from the Diamond-NOM, the optical slope error was reduced to ∼ 0.5 µrad r.m.s. for a range of ellipses. To maximize usability, a novel holder was built to accommodate the substrate in any orientation. When replacing a first-generation bimorph on a synchrotron beamline, the new mirror significantly improved the size and shape of the reflected X-ray beam. Most importantly, there was no evidence of the junction effect even after eight months of continuous beamline usage. It is hoped that this new design will reinvigorate the use of active bimorph optics at synchrotron and free-electron laser facilities to manipulate and correct X-ray wavefronts.

  7. 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

  8. CT imaging of small animals using monochromatized synchrotron x rays

    SciTech Connect

    Dilmanian, F.A.; Rarback, H.; Nachaliel, E.; Rivers, M.; Thomlinson, W.C.; Chapman, L.D.; Oversluizen, T.; Slatkin, D.N.; Spanne, P.; Spector, S. ); Garrett, R.F. ); Luke, P.N.; Pehl, R.; Thompson, A.C. ); Appel, R.; Miller, M.H. (A

    1992-01-01

    Rats and chicken embryos were imaged in vivo with a prototype Multiple Energy Computed Tomography (MECT) system using monochromatized x rays from the X17 superconducting wiggler at the National Synchrotron Light Source. The CT configuration coated of a horizontal low-divergence, fan-shaped beam, 70 mm wide and 0.5 mm high, and a subject rotating about a vertical aids. A linear-array high-purity Ge detector with 140 elements, each 0.5 mm wide and 6 mm thick, was used with a data acquisition system that provides a linear response over almost six orders of magnitude of detector current. The dual photon absorptiometry (DPA) algorithm was applied to images of the rat head acquired at 20 and 45 keV to obtain two new images, one representing the low-Z, and the other the intermediate-Z clement group. The results indicate that the contrast resolution and the quantification accuracy of the images improve stepwise; first, with the monochromatic beam and, second, the DPA method. The system is a prototype for a brain scanner.

  9. 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.

  10. 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.

  11. 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.

  12. 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

  13. 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.

  14. Surface recombination effects in soft X-ray efficiencies

    NASA Astrophysics Data System (ADS)

    Benitez, E. L.; Husk, D. E.; Tarrio, C.; Schnatterly, S. E.

    1991-07-01

    The soft X-ray efficiencies of a silicon p-i-n photodiode and an La2O2S:Tm phosphor were measured over a broad energy range. Also, the inelastic electron scattering spectra of the constituent materials were measured and values of optical absorption coefficients versus energy were obtained. The energy dependence of the efficiencies is well explained by a model based on surface recombination of electron hole pairs, and the quality of data which can now be obtained from synchrotrons makes possible quantitative fits from which diffusion length, surface recombination velocity, and bulk quantum efficiency are obtained.

  15. X-ray and synchrotron investigations of heterogeneous systems based on multiwalled carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Sivkov, V. N.; Ob"edkov, A. M.; Petrova, O. V.; Nekipelov, S. V.; Kremlev, K. V.; Kaverin, B. S.; Semenov, N. M.; Gusev, S. A.

    2015-01-01

    This paper presents the results of a complex investigation of heterogeneous systems based on multiwalled carbon nanotubes with the outer surfaces covered by iron oxide (Fe3O4) nanocoatings deposited using iron pentacarbonyl as a precursor. Investigations were performed by the methods of electron microscopy, X-ray diffractometry, and ultrasoft X-ray spectroscopy with synchrotron radiation. It was established that the formed thin coatings are continuous and nonuniform in thickness. It was shown that good adhesion of iron oxide on the multiwalled carbon nanotube surface is provided by the formation of epoxy and double carbon-oxygen bonds; in this case, the outer graphene layer of nanotubes is not destroyed and retains the hexagonal structure.

  16. The X-ray Fluorescence Microscopy Beamline at the Australian Synchrotron

    SciTech Connect

    Paterson, D.; Jonge, M. D. de; Howard, D. L.; Lewis, W.; McKinlay, J.; Starritt, A.; Kusel, M.; Ryan, C. G.; Kirkham, R.; Moorhead, G.; Siddons, D. P.

    2011-09-09

    A hard x-ray micro-nanoprobe has commenced operation at the Australian Synchrotron providing versatile x-ray fluorescence microscopy across an incident energy range from 4 to 25 keV. Two x-ray probes are used to collect {mu}-XRF and {mu}-XANES for elemental and chemical microanalysis: a Kirkpatrick-Baez mirror microprobe for micron resolution studies and a Fresnel zone plate nanoprobe capable of 60-nm resolution. Some unique aspects of the beamline design and operation are discussed. An advanced energy dispersive x-ray fluorescence detection scheme named Maia has been developed for the beamline, which enables ultrafast x-ray fluorescence microscopy.

  17. 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.

  18. 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.

  19. 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.

  20. X-ray Magnetic Scattering From Surfaces^*

    NASA Astrophysics Data System (ADS)

    Gibbs, Doon

    1997-03-01

    In the last several years, there have been continuing efforts to probe long-ranged magnetic order at surfaces by x-ray and neutron diffraction, following many earlier studies by low energy electron diffraction. The main motivation has been to discover how bulk magnetic structures are modified near a surface, where the crystal symmetry is broken. In this talk, we describe x-ray scattering studies of the magnetic structure observed near the (001) surface of the antiferromagnet uranium dioxide.(G. M. Watson, Doon Gibbs, G. H. Lander, B. D. Gaulin, L.E. Berman, Hj. Matzke and W. Ellis, Phys. Rev. Lett. 77), 751 (1996). Within about 50 Åof the surface, the intensity of the magnetic scattering decreases continuously as the bulk Neel temperature is approached from below. This contrasts with the bulk magnetic ordering transition which is discontinuous. Recent measurements of the specular magnetic reflectivity suggest that the width of the magnetic interface diverges as a power-law in reduced temperature reminiscent of surface induced disorder. Related experiments concerned with magnetic crystallography of Co_3-Pt(111) surfaces(S. Ferrer, P. Fajardo, F. de Bergevin, J. Alvarez, X. Torrelles, H. A. van der Vegt and V. H. Etgens, Phys. Rev. Lett. 77), 747 (1996). and interfacial magnetic roughness of Co/Cu multilayers(J. F. MacKay, C. Teichert, D.E. Savage and M.G. Lagally, Phys. Rev. Lett. 77), 3925 (1996). will also be discussed. ^* Work at Brookhaven National Laboratory is supported by the U.S. DOE under Contract No. DE-AC02-CH7600016.

  1. 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.

  2. 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.

  3. XPAD3-S: A fast hybrid pixel readout chip for X-ray synchrotron facilities

    NASA Astrophysics Data System (ADS)

    Pangaud, Patrick; Basolo, Stephanie; Boudet, Nathalie; Berar, Jean-François; Chantepie, Benoît; Clemens, Jean-Claude; Delpierre, Pierre; Dinkespiler, Bernard; Medjoubi, Kadda; Hustache, Stephanie; Menouni, Mohsine; Morel, Christian

    2008-06-01

    At X-ray synchrotron facilities, scattering experiments require detectors with a large sensitive surface, an high count rate capability, a large counter dynamics, a fast readout system and an adjustable energy threshold. X-ray pixel chip with adaptable dynamics (XPAD3) is a new pixellized photon detector based on hybrid pixel technology, which provides low noise data readout at high speed. It is designed in 0.25 μm IBM technology and contains 9600 pixels (130 μm×130 μm) distributed into 80 columns of 120 elements each. Its features have been optimized to fulfill a count rate capability up to 10 +6 photons/pixel/s, an high dynamic range over 35 keV, a very low noise of 130e -, and a threshold adjustment well below 4 keV. Fast data readout below 2 ms/frame is expected. To meet these requirements, an innovative architecture has been designed that makes possible the readout the circuit during acquisition while preserving the precise setting of the thresholds all over the pixel array. The XPAD3 circuit can be bump-bonded with Si, CdTe, or GaAs sensors to optimize its detection efficiency at high X-ray energies. XPAD3 detector modules will be tiled together to form the XPIX detector with a 8 cm×12 cm sensitive area. We present first results obtained using a single-chip prototype of the XPAD3 detector.

  4. Synchrotron Radiation and X-ray FEL Projects in Korea

    NASA Astrophysics Data System (ADS)

    Cho, M. H.

    2012-03-01

    There are two on-going major projects in Pohang Accelerator Laboratory (PAL), the PLS-II light source upgrade and the construction of PAL-XFEL facility. PLS-II is a new light source upgraded from PLS(Pohang Light Source) which had been operated for 16 years from 1995 and shut down in Dec. 2010. The performance will be improved from ``18.9 nm-rad, 2.5 GeV, and 200 mA'' to ``5.8 nm-rad, 3 GeV, and 400 mA'' using three superconducting RF cavities. The old storage ring has been completely dismantled and new DBA ring has been re-installed in the same tunnel within 6 months, and is under commissioning now. The unique feature of PLS-II is the compact employment of 20 insertion-devices including 14 in-vacuum undulators. The PALXFEL is a 0.1-nm hard X-ray FEL construction project started in 2011 and to compete in 2014 with a total budget of 400 M. The PAL-XFEL is designed to have hard X-ray undulator lines at the end of 10-GeV linac, and a dog-leg branch line at 2.65 GeV point for a soft X-ray undulator line simultaneously and independently from hard X-ray FEL undulator line. The overview of two projects with current status is presented.

  5. 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.

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

    NASA Astrophysics Data System (ADS)

    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.

  7. 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).

  8. 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

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

    NASA Astrophysics Data System (ADS)

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

    2006-05-01

    Sepiolite is a hydrous Mg-silicate clay mineral with fibrous morphology that typically occurs as fine-grained, poorly crystalline masses. It occurs in a wide variety of geological environments and has been mined for centuries because of its many uses, e.g. in the pharmaceutical, fertilizer, and pesticide industries. Its versatile functionality derives from the large surface area and microporosity that are characteristic of the material. In recent years, sepiolite has received considerable attention with regard to the adsorption of organics, for use as a support for catalysts, as a molecular sieve, and as an inorganic membrane for ultrafiltration. Because of its fine-grained and poorly crystalline nature, it has not been possible to study sepiolite's crystal structure using single-crystal X-ray diffraction methods, and consequently many details of the structure are still not well known. In this study, Rietveld refinements using synchrotron powder X-ray diffraction data were used to investigate 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 water site. The RT structure under vacuum retained only ~1/8 of the zeolitic water and the volume decreased 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 water is lost by ~390 K, accompanied by a decrease in the a and c unit-cell parameters. Above ~600 K the sepiolite structure folds as one-half of the crystallographically bound water is lost. Rietveld refinements of the "anhydrous" sepiolite structure reveal that, in general, unit-cell parameters a, b, â and volume steadily decrease with increasing temperature; there is an obvious change in slope at ~820 K suggesting a phase

  10. 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.

  11. 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.

  12. 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.

  13. 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

  14. 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.

  15. Evanescent X-Rays Probing Surface-Dominated Phase Transitions

    NASA Astrophysics Data System (ADS)

    Dosch, H.

    This articl rviws th scattring of vanscnt x-ray wavs as thy occur insid a solid in th rgim of total xtrnal rflction. Th thortical and xprimntal dtails of glancing angl scattring and th us of synchrotron radiation ar discussd. It is shown how strong surfac disordr and surfac roughnss affct th Bragg scattring of ths xponntially dampd wavs and how ths scattring signals can b intrprtd in a straightforward way within th distortd wav Born approximation (DWBA). Th application of this novl surfac tchniqu to bulk phas transitions allows th obsrvation of surfac-dominatd bhaviour. This is illustratd via two xampls: 1. Th discontinuous ordr-disordr transition in Cu3Au has bn studid nar th (001) and (111) surfac by vanscnt x-rays. It turns out that th ordr paramtr clos to th fr surfac of th alloy dcays in a vry pronouncd way upon approaching th transition tmpratur. Th quantitativ analysis of th vanscnt suprlattic intnsity is compatibl with a wtting phnomnon. 2. Th critical phnomna associatd with th continuous ordr-disordr transition in F3Al bcom distinctly modifid du to th prsnc of a fr surfac. By applying th vanscnt wav mthod thr nw univrsal surfac xponnts β1, γ11 and η‖ could b dtrmind. This allows for th first tim a critical xprimntal tst of surfac scaling rlations which turn out to b in good agrmnt with th xprimntal findings. At th surfac of binary alloys surfac sgrgation phnomna occur which complicat th xprimntal obsrvation of nar-surfac ordring and disordring phnomna as wll as th thortical modls which hav to account for ths ffcts. Som implications of ths surfac ffcts is brifly prsntd.

  16. 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.

  17. 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.

  18. 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.

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

    NASA Astrophysics Data System (ADS)

    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.

  20. 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.

  1. 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.

  2. 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.

  3. Synchrotron X-ray scattering studies at mineral-water interfaces

    SciTech Connect

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

    1995-03-01

    Synchrotron X-ray scattering techniques provide a powerful tool for the in situ study of atomic scale processes occurring at solid-liquid interfaces. We have applied these techniques to characterize and study reactions at mineral-water interfaces. Here we present two examples. The first is the characterization of the calcite (CaCO{sub 3}) (10{bar 1}4) cleavage surface, in equilibrium with deionized water, by crystal truncation rod measurements. The second is the in situ study of the heteroepitaxial growth of otavite (CdCO{sub 3}) on the calcite (10{bar 1}4) cleavage surface. The results of such studies will lead to significant progress in understanding mineral-water interface geochemistry.

  4. 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.

  5. 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.

  6. Compton scattering imaging of a working battery using synchrotron high-energy X-rays.

    PubMed

    Itou, Masayoshi; Orikasa, Yuki; Gogyo, Yuma; Suzuki, Kosuke; Sakurai, Hiroshi; Uchimoto, Yoshiharu; Sakurai, Yoshiharu

    2015-01-01

    Results of studies on Compton scattering imaging using synchrotron high-energy X-rays are reported. The technique is applied to a discharging coin cell, and the intensity of Compton scattered X-rays from the inside of the cell has been measured as a function of position and time. The position-time intensity map captures the migration of lithium ions in the positive electrode and reveals the structural change due to the volume expansion of the electrode. This experiment is a critical step in developing synchrotron-based Compton scattering imaging for electrochemical cells at a product level.

  7. 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.

  8. Minimally Invasive Coronary Angiography with Monochromatic X-Rays Developmental Studies Utilizing Synchrotron Radiation.

    NASA Astrophysics Data System (ADS)

    Otis, John Noel

    Iodine-containing compounds are used as contrast agents in obtaining X-ray images of blood vessels for medical diagnosis. If the X-ray contrast produced by iodine can be enhanced sufficiently relative to that produced by the intervening body tissues, it becomes possible to obtain images of arteries by introducing the contrast agent into the venous circulation rather than through an arterial catheter directly into the vessel under examination. This prospect is attractive because invasion of the arterial system is the chief cause of the medical complications that are encountered in the application of current angiographic procedures. An imaging system that shows promise of accomplishing this goal for examination of the coronary arteries has been developed for operation in an X-ray beam at the Stanford Synchrotron Radiation Laboratory. Iodine-selective contrast enhancement is achieved by logarithmic subtraction of two images of the same field. One of these images is formed by monochromatic X-rays of energy just above the characteristic iodine K-absorption edge at 33.17 keV, the other by X-rays of energy just below the edge. The computer-controlled imaging system acquires digitized images line by line while scanning the subject through a stationary X-ray beam of linear profile. At present, only synchrotron radiation can provide monochromatic X-ray beams of intensity sufficient to image the small and rapidly moving coronary arteries. Preliminary studies of static phantoms and in vivo studies of dogs establish the feasibility of using synchrotron radiation as the X-ray source for iodine-selective imaging with sensitivity and speed adequate for providing sharp images of coronary arteries after intravenous introduction of contrast agent. Application of the method to human subjects began with imaging studies of three patients in May, 1986.

  9. 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

  10. 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

  11. 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.

  12. Synchrotron Radiation X-Ray Spectroscopy for Investigations of Intracellular Metallointercalators: X-Ray Fluorescence Imaging and X-Ray Absorption Spectroscopy

    NASA Astrophysics Data System (ADS)

    Dillon, Carolyn T.

    In an effort to determine the therapeutic feasibility of DNA metallointercalators as potential anticancer drugs it is important to confirm that they are capable of targeting DNA in cancer cells or tumours - as is the intended purpose of their design. Microprobe synchrotron radiation X-ray fluorescence (micro-SRXRF) spectroscopy is an ideal technique for investigating the cellular uptake and distribution of metallointercalators. The technique is capable of submicron elemental imaging so that samples as small as individual cells (~10 μm diameter), and the features within them, can be resolved. Consequently, the technique can ascertain whether intracellular metallointercalators colocalise with DNA; namely, in the nucleus during interphase or at the chromosomes during middle prophase to late anaphase. Metals, such as those commonly incorporated into metallointercalators (e.g., Cr, Ni, Co, Pd, Pt, Ru, Rh), are often naturally present in negligible quantities in cancer cells. This fact, together with their higher atomic number, Z, makes them ideal for direct probing using hard X-ray microprobes (as discussed in Sect. 11.2). There is no need for the incorporation of fluorescent tracker dyes or radioactive labels into their chemical structure. This is advantageous since it is unknown whether such chemical modifications alter the uptake kinetics of the metallointercalator [1, 2].

  13. 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

  14. X-ray fluorescence spectrometry for high throughput analysis of atmospheric aerosol samples: The benefits of synchrotron X-rays

    NASA Astrophysics Data System (ADS)

    Bukowiecki, Nicolas; Lienemann, Peter; Zwicky, Christoph N.; Furger, Markus; Richard, Agnes; Falkenberg, Gerald; Rickers, Karen; Grolimund, Daniel; Borca, Camelia; Hill, Matthias; Gehrig, Robert; Baltensperger, Urs

    2008-09-01

    The determination of trace element mass concentrations in ambient air with a time resolution higher than one day represents an urgent need in atmospheric research. It involves the application of a specific technique both for the aerosol sampling and the subsequent analysis of the collected particles. Beside the intrinsic sensitivity of the analytical method, the sampling interval and thus the quantity of collected material that is available for subsequent analysis is a major factor driving the overall trace element detection power. This is demonstrated for synchrotron radiation X-ray fluorescence spectrometry (SR-XRF) of aerosol samples collected with a rotating drum impactor (RDI) in hourly intervals and three particle size ranges. The total aerosol mass on the 1-h samples is in the range of 10 µg. An experimental detection of the nanogram amounts of trace elements with the help of synchrotron X-rays was only achievable by the design of a fit-for-purpose sample holder system, which considered the boundary conditions both from particle sampling and analysis. A 6-µm polypropylene substrate film has evolved as substrate of choice, due to its practical applicability during sampling and its suitable spectroscopic behavior. In contrast to monochromatic excitation conditions, the application of a 'white' beam led to a better spectral signal-to-background ratio. Despite the low sample mass, a counting time of less than 30 s per 1-h aerosol sample led to sufficient counting statistics. Therefore the RDI-SR-XRF method represents a high-throughput analysis procedure without the need for any sample preparation. The analysis of a multielemental mass standard film by SR-XRF, laboratory-based wavelength-dispersive XRF spectrometry and laboratory-based micro XRF spectrometry showed that the laboratory-based methods were no alternatives to the SR-XRF method with respect to sensitivity and efficiency of analysis.

  15. 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.

  16. 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.

  17. 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.

  18. High-energy synchrotron X-ray radiography of shock-compressed materials

    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 presentation will discuss the development and application of a high-energy (50 to 250 keV) synchrotron X-ray imaging method to study shock-compressed, high-Z samples at Beamline I12 at the Diamond Light Source synchrotron (Rutherford-Appleton Laboratory, UK). Shock waves are driven into materials using a portable, single-stage gas gun designed by the Institute of Shock Physics. Following plate impact, material deformation is probed in-situ by white-beam X-ray radiography and complimentary velocimetry diagnostics. The high energies, large beam size (13 x 13 mm), and appreciable sample volumes (~ 1 cm3) viable for study at Beamline I12 compliment existing in-house pulsed X-ray capabilities and studies at the Dynamic Compression Sector. The authors gratefully acknowledge the ongoing support of Imperial College London, EPSRC, STFC and the Diamond Light Source, and AWE Plc.

  19. On diamond windows for high power synchrotron x-ray beams

    SciTech Connect

    Khounsary, A.M.; Kuzay, T.M.

    1991-01-01

    Recent advances in chemical vapor deposition (CVD) technology has made available thin, free-standing polycrystalline diamond foils that can be used as the window material on high heat load synchrotron x-ray beamlines. Diamond windows have many advantages that stem from the exceptionally attractive thermal, structural, and physical properties of diamond. Numerical simulations indicate that diamond windows can offer an attractive and at times the only alternative to beryllium windows for use on the third generation x-ray synchrotron radiation beamlines. Utilization, design, and fabrication aspects of diamond windows for high heat load x-ray beamlines are discussed, and analytical and numerical results are presented to provide a basis for the design and testing of such windows.

  20. On diamond windows for high power synchrotron x-ray beams

    SciTech Connect

    Khounsary, A.M.; Kuzay, T.M.

    1991-12-31

    Recent advances in chemical vapor deposition (CVD) technology has made available thin, free-standing polycrystalline diamond foils that can be used as the window material on high heat load synchrotron x-ray beamlines. Diamond windows have many advantages that stem from the exceptionally attractive thermal, structural, and physical properties of diamond. Numerical simulations indicate that diamond windows can offer an attractive and at times the only alternative to beryllium windows for use on the third generation x-ray synchrotron radiation beamlines. Utilization, design, and fabrication aspects of diamond windows for high heat load x-ray beamlines are discussed, and analytical and numerical results are presented to provide a basis for the design and testing of such windows.

  1. 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.

  2. 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.

  3. 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

  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. A new miniature microchannel plate X-ray detector for synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Rosemeier, Ronald G.; Green, Robert E.

    A state-of-the-art microchannel plate detector has been developed which allows real time X-ray imagin of X-ray diffraction as well as a radiographic phenomenon. Advantages of the device include a 50 mm X-ray input, length less than 4″, and a weight of less than 1 lb. Since the use of synchrotron radiation is greatly facilitated by the capability of remote viewing of X-ray diffraction or radiographic images in real time, a prototype electro-optical system has been designed which couples the X-ray microchannel plate detector with a solid state television camera. Advantages of the miniature, lightweight, X-ray synchroton camera include a large 50 mm X-ray input window, an output signal that is available in both analog format for display on a television monitor and in digital format for computer processing, and a completely modular design which allows all the components to be exchanged for other components optimally suited for the desired applications.

  6. 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

  7. 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

  8. 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.

  9. 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.

  10. 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.

  11. 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

  12. Evaluation of a photon-counting hybrid pixel detector array with a synchrotron X-ray source

    NASA Astrophysics Data System (ADS)

    Ponchut, C.; Visschers, J. L.; Fornaini, A.; Graafsma, H.; Maiorino, M.; Mettivier, G.; Calvet, D.

    2002-05-01

    A photon-counting hybrid pixel detector (Medipix-1) has been characterized using a synchrotron X-ray source. The detector consists of a readout ASIC with 64×64 independent photon-counting cells of 170×170 μm 2 pitch, bump-bonded to a 300 μm thick silicon sensor, read out by a PCIbus-based electronics, and a graphical user interface (GUI) software. The intensity and the energy tunability of the X-ray source allow characterization of the detector in the time, space, and energy domains. The system can be read out on external trigger at a frame rate of 100 Hz with 3 ms exposure time per frame. The detector response is tested up to more than 7×10 5 detected events/pixel/s. The point-spread response shows <2% crosstalk between neighboring pixels. Fine scanning of the detector surface with a 10 μm beam reveals no loss in sensitivity between adjacent pixels as could result from charge sharing in the silicon sensor. Photons down to 6 keV can be detected after equalization of the thresholds of individual pixels. The obtained results demonstrate the advantages of photon-counting hybrid pixel detectors and particularly of the Medipix-1 chip for a wide range of X-ray imaging applications, including those using synchrotron X-ray beams.

  13. 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.

  14. Fabrication of an 8:1 ellipsoidal mirror for a synchrotron x-ray microprobe

    SciTech Connect

    Jones, K.W.; Takacs, P.Z.; Hastings, J.B.; Casstevens, J.M.; Pionke, C.D.

    1987-01-11

    The fabrication of an 8:1 demagnifying ellipsoidal mirror to be used for an x-ray microprobe at the National Synchrotron Light Source X-26 beam port is described. The design aim was to produce a mirror that could be used over the photon energy range from about 3 to 17 keV. The 300-mm long mirror was required to operate at a grazing angle of 5 mr. The semimajor axis was 4500 mm and the semiminor axis 14.142 mm. Surface roughness of 1 nm or less and slope errors of 1 arc second parallel to the long axis and 200 arc seconds parallel to the short direction were specified. Production of the first electroless nickel-coated aluminum mirror using a diamond-turning technique has been completed. The mirror meets the 1 arc sec surface figure specification except for areas near the ends of the mirror. The reasons for these deviations arise from subtle details of the diamond-turning process which have not been fully incorporated in to the computer program that controls the diamond-turning machines. Further work in computer correction of repeatable errors of the diamond-turning machine can eliminate the waviness at the ends of the mirror. The diamond-turned mirror surface was not fully polished under this effort and therefore does not meet the roughness specification; however, surface smoothness of a fully polished cylindrical mirror manufactured using the same techniques does not meet the specification. It can be concluded that it is now technically feasible to meet the required specifications for the mirror and that the x-ray microprobe based on its use can be achieved.

  15. 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.

  16. 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.

  17. Microscopic x-ray imaging system for biomedical applications using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Umetani, Keiji; Kobatake, Makito; Yamamoto, Akira; Yamashita, Takenori; Imai, Shigeki

    2007-02-01

    An X-ray direct-conversion type detector with a spatial resolution of 10-11 μm was developed for real-time biomedical imaging. The detector incorporates the X-ray SATICON pickup tube with a photoconductive target layer of amorphous selenium. For high-resolution imaging, the X-ray image is directly converted into an electric signal in the photoconductive layer without image blur. Microangiography experiments were carried out for depicting angiogenic vessels in a rabbit model of cancer using the direct-conversion detector and a third generation synchrotron radiation source at SPring-8. In synchrotron radiation radiography, a long source-to-object distance and a small source spot can produce high-resolution images. After transplantation of cancer cells into the rabbit auricle, small tumor blood vessels with diameters of 20-30 μm in an immature vascular network produced by angiogenesis were visualized by contrast material injection into the auricular artery at a monochromatic X-ray energy of 33.2 keV just above the iodine K-edge energy. The synchrotron radiation system is a useful tool to evaluate the micro-angioarchitecture of malignant tumors in animal models of cancer for in vivo preclinical studies.

  18. 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.

  19. Energy Dependence of Synchrotron X-Ray Rims in Tycho's Supernova Remnant

    NASA Technical Reports Server (NTRS)

    Tran, Aaron; Williams, Brian J.; Petre, Robert; Ressler, Sean M.; Reynolds, Stephen P.

    2015-01-01

    Several young supernova remnants exhibit thin X-ray bright rims of synchrotron radiation at their forward shocks. Thin rims require strong magnetic field amplification beyond simple shock compression if rim widths are only limited by electron energy losses. But, magnetic field damping behind the shock could produce similarly thin rims with less extreme field amplification. Variation of rim width with energy may thus discriminate between competing influences on rim widths. We measured rim widths around Tycho's supernova remnant in 5 energy bands using an archival 750 ks Chandra observation. Rims narrow with increasing energy and are well described by either loss-limited or damped scenarios, so X-ray rim width-energy dependence does not uniquely specify a model. But, radio counterparts to thin rims are not loss-limited and better reflect magnetic field structure. Joint radio and X-ray modeling favors magnetic damping in Tycho's SNR with damping lengths approximately 1-5% of remnant radius and magnetic field strengths approximately 50-400 micron G assuming Bohm diffusion. X-ray rim widths are approximately 1% of remnant radius, somewhat smaller than inferred damping lengths. Electron energy losses are important in all models of X-ray rims, suggesting that the distinction between loss-limited and damped models is blurred in soft X-rays. All loss-limited and damping models require magnetic fields approximately greater than 20 micron G, arming the necessity of magnetic field amplification beyond simple compression.

  20. ENERGY DEPENDENCE OF SYNCHROTRON X-RAY RIMS IN TYCHO’S SUPERNOVA REMNANT

    SciTech Connect

    Tran, Aaron; Williams, Brian J.; Petre, Robert; Reynolds, Stephen P.

    2015-10-20

    Several young supernova remnants (SNRs) exhibit thin X-ray bright rims of synchrotron radiation at their forward shocks. Thin rims require strong magnetic field amplification beyond simple shock compression if rim widths are only limited by electron energy losses. But, magnetic field damping behind the shock could produce similarly thin rims with less extreme field amplification. Variation of rim width with energy may thus discriminate between competing influences on rim widths. We measured rim widths around Tycho's SNR in five energy bands using an archival 750 ks Chandra observation. Rims narrow with increasing energy and are well described by either loss-limited or damped scenarios, so X-ray rim width-energy dependence does not uniquely specify a model. But, radio counterparts to thin rims are not loss-limited and better reflect magnetic field structure. Joint radio and X-ray modeling favors magnetic damping in Tycho's SNR with damping lengths ∼1%–5% of remnant radius and magnetic field strengths ∼50–400 μG assuming Bohm diffusion. X-ray rim widths are ∼1% of remnant radius, somewhat smaller than inferred damping lengths. Electron energy losses are important in all models of X-ray rims, suggesting that the distinction between loss-limited and damped models is blurred in soft X-rays. All loss-limited and damping models require magnetic fields ≳20 μG, affirming the necessity of magnetic field amplification beyond simple compression.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. Synchrotron X-ray Fluorescence Microtomography in Geo-, Cosmo-, and Bio- chemistry

    NASA Astrophysics Data System (ADS)

    Lanzirotti, A.; Sutton, S. R.; Rivers, M.; Tappero, R.

    2009-05-01

    Synchrotron-based X-ray fluorescence computed microtomography (xrfCMT) is a unique method for imaging major and trace element distributions within natural materials nondestructively and with high spatial resolution. The technique is particularly useful in imaging and quantifying elemental abundance in small objects that may be too precious or too difficult to section, or in the analysis of materials in which sectioning may potentially alter elemental distributions. This presentation will highlight how this technique is being applied at beamlines X26A and X27A at the National Synchrotron Light Source (Brookhaven National Laboratory) and at 13-ID at the Advanced Photon Source (Argonne National Laboratory). These instruments utilize 1-10 μm diameter focused, monochromatic X-ray beams to non- destructively measure x-ray fluorescence from a sample as it is translated and rotated within the beam. The resultant fluorescence intensities are then reconstructed as either two-dimensional cross sectional or three- dimensional elemental distribution using a fast fourier transform based computational reconstruction algorithm. Reconstruction of multi-elemental distributions at concentrations down to approximately 1 μg g-1 (element dependent) can be obtained. By collecting and storing full energy dispersive spectra from a multi-channel analyzer for every pixel (rather than regions of interest), it is possible to evaluate a reconstructed spectrum within the object for more robust elemental analysis. For high density matrices in particular, corrections are necessary to account for x-ray absorption by the object of both incoming X-rays and outgoing fluorescent X-rays. These effects limit the size of objects and elements that can be imaged; however reasonable corrections can be made if an estimate of linear absorption coefficient through the material is made. It is also possible to couple fluorescence tomography with microbeam x-ray absorption and diffraction analysis. When coupled

  6. 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.

  7. 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.

  8. 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.

  9. Vertical synchrotron radiation beamline for proximity X-ray lithography: Theoretical analysis

    NASA Astrophysics Data System (ADS)

    Bukreeva, Inna N.; Kozhevnikov, Igor V.

    1997-02-01

    The general physical principles of operation of the vertical beamline of synchrotron radiation (SR) intended for proximity X-ray lithography are considered. An optical system provides a deflection of the SR beam to the vertical plane, a cutoff of the hard X-rays, a uniform illumination of a wafer, a normal incidence of X-ray beam onto a mask, and a small enough divergency of the radiation. A vertical SR beamline makes it possible to circumvent the expensive development of vertical-plane displacement steppers and to use the conventional horizontal ones, to exclude the scanning of the SR beam across the mask and to reduce the requirements imposed on the accuracy of alignment of a gap between the mask and the wafer.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. Probing platinum degradation in polymer electrolyte membrane fuel cells by synchrotron X-ray microscopy.

    PubMed

    Berejnov, Viatcheslav; Martin, Zulima; West, Marcia; Kundu, Sumit; Bessarabov, Dmitri; Stumper, Jürgen; Susac, Darija; Hitchcock, Adam P

    2012-04-14

    Synchrotron-based scanning transmission X-ray spectromicroscopy (STXM) was used to characterize the local chemical environment at and around the platinum particles in the membrane (PTIM) which form in operationally tested (end-of-life, EOL) catalyst coated membranes (CCMs) of polymer electrolyte membrane fuel cells (PEM-FC). The band of metallic Pt particles in operationally tested CCM membranes was imaged using transmission electron microscopy (TEM). The cathode catalyst layer in the beginning-of-life (BOL) CCMs was fabricated using commercially available catalysts created from Pt precursors with and without nitrogen containing ligands. The surface composition of these catalyst powders was measured by X-ray Photoelectron Spectroscopy (XPS). The local chemical environment of the PTIM in EOL CCMs was found to be directly related to the Pt precursor used in CCM fabrication. STXM chemical mapping at the N 1s edge revealed a characteristic spectrum at and around the dendritic Pt particles in CCMs fabricated with nitrogen containing Pt-precursors. This N 1s spectrum was identical to that of the cathode and different from the membrane. For CCM samples fabricated without nitrogen containing Pt-precursors the N 1s spectrum at the Pt particles was indistinguishable from that of the adjacent membrane. We interpret these observations to indicate that nitrogenous ligands in the nitrogen containing precursors, or decomposition product(s) from that source, are transported together with the dissolved Pt from the cathode into the membrane as a result of the catalyst degradation process. This places constraints on possible mechanisms for the PTIM band formation process.

  15. 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

  16. 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.

  17. 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

  18. 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.

  19. Development of Ta-based STJ X-ray Detector Arrays for Synchrotron Science

    NASA Astrophysics Data System (ADS)

    Carpenter, M. H.; Friedrich, S.; Hall, J. A.; Harris, J.; Cantor, R.

    2014-08-01

    We are developing a cryogen-free Ta-based superconducting tunnel junction (STJ) detector for soft X-ray spectroscopy at synchrotrons. With an energy resolution 10 times higher than conventional solid-state X-ray detectors and count-rate capabilities above 5 kHz/pixel, STJ detectors offer potentially increased sensitivity for fluorescence-yield X-ray absorption spectroscopy (FY-XAS). We have developed 36-pixel arrays of 208 208 m Ta STJs with an energy resolution of 9 eV FWHM at the 525 eV oxygen K line. Compared to earlier Nb-based STJs, Ta-STJs offer improved energy resolution and absorption efficiency and extend the operating range to several keV. Here we describe the integration of the 36-pixel arrays into a cryogen-free, user-friendly X-ray spectrometer. A computer-controlled adiabatic demagnetization refrigerator coupled to a two-stage pulse tube refrigerator allows operation below 100 mK. The detector chip is located at the end of a 42 cm shielded snout for insertion into the analysis chamber. The system is currently being commissioned at the Advanced Light Source synchrotron.

  20. Fast photoconductor CdTe detectors for synchrotron x-ray studies

    SciTech Connect

    Yoo, Sung Shik; Faurie, J.P.; Wang, Kemei; Montano, P.A. |; Huang Qiang; Rodricks, B.

    1993-09-01

    The Advanced Photon Source will be that brightest source of synchrotron x-rays when it becomes operational in 1996. During normal operation, the ring will be filled with 20 bunches of positrons with an interbunch spacing of 177 ns and a bunch width of 119 ps. To perform experiments with x-rays generated by positrons on these time scales one needs extremely high speed detectors. To achieve the necessary high speed, we are developing MBE-grown CdTe-base photoconductive position sensitive array detectors. The arrays fabricated have 64 pixels with a gap of 100 {mu}m between pixels. The high speed response of the devices was tested using a short pulse laser. X-ray static measurements were performed using an x-ray tube and synchrotron radiation to study the device`s response to flux and wavelength changes. This paper presents the response of the devices to some of these tests and discusses different physics aspects to be considered when designing high speed detectors.

  1. 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.

  2. 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.

  3. 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

  4. 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.

  5. 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.

  6. Synchrotron-based X-ray-sensitive nanoprobes for cellular imaging.

    PubMed

    Zhu, Ying; Earnest, Thomas; Huang, Qing; Cai, Xiaoqing; Wang, Zhili; Wu, Ziyu; Fan, Chunhai

    2014-12-10

    It is one of the ultimate goals in cell biology to understand the complex spatio-temporal interplay of biomolecules in the cellular context. To this end, there have been great efforts on the development of various probes to detect and localize specific biomolecules in cells with a variety of microscopic imaging techniques. In this Research News, we first summarize several types of microscopy for visualizing specific biomolecular targets. Then we focus on recent advances in the design of X-ray sensitive nanoprobes for applications in synchrotron-based cellular imaging. With the availability of advanced synchrotron techniques, there has been rapid progress toward high-resolution and multi-color X-ray imaging in cells with various types of functional nanoprobes.

  7. 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.

  8. Extending synchrotron-based atomic physics experiments into the hard X-ray region

    SciTech Connect

    LeBrun, T.

    1996-12-31

    The high-brightness, hard x-ray beams available from third-generation synchrotron sources are opening new opportunities to study the deepest inner shells of atoms, an area where little work has been done and phenomena not observed in less tightly bound inner-shells are manifested. In addition scattering processes which are weak at lower energies become important, providing another tool to investigate atomic structure as well as an opportunity to study photon/atom interactions beyond photoabsorption. In this contribution the authors discuss some of the issues related to extending synchrotron-based atomic physics experiments into the hard x-ray region from the physical and the experimental point of view. They close with a discussion of a technique, resonant Raman scattering, that may prove invaluable in determining the spectra of the very highly-excited states resulting from the excitation of deep inner shells.

  9. 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

  10. Nanosecond laser pulse heating of a platinum surface studied by pump-probe X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Shayduk, Roman; Vonk, Vedran; Arndt, Björn; Franz, Dirk; Strempfer, Jörg; Francoual, Sonia; Keller, Thomas F.; Spitzbart, Tobias; Stierle, Andreas

    2016-07-01

    We report on the quantitative determination of the transient surface temperature of Pt(110) upon nanosecond laser pulse heating. We find excellent agreement between heat transport theory and the experimentally determined transient surface temperature as obtained from time-resolved X-ray diffraction on timescales from hundred nanoseconds to milliseconds. Exact knowledge of the surface temperature's temporal evolution after laser excitation is crucial for future pump-probe experiments at synchrotron storage rings and X-ray free electron lasers.

  11. 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.

  12. 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.

  13. 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.

  14. Synchrotron radiation X-ray imaging of cavitation bubbles in Al-Cu alloy melt.

    PubMed

    Huang, Haijun; Shu, Da; Fu, Yanan; Wang, Jun; Sun, Baode

    2014-07-01

    Cavitation bubbles in Al-10 wt.%Cu melt has been investigated by adopting synchrotron radiation X-ray imaging technology. In-situ observation reveals that most of bubbles concentrate within an intense cavitation zone nearby the radiation face. The measured near-maximum bubble radii obey a similar truncated Gaussian distribution as in water but increase by nearly the magnitude of one order due to higher ultrasonic intensity applied in aluminum melt.

  15. 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.

  16. Vacuum chamber development for the synchrotron x-ray source at Argonne

    SciTech Connect

    Nielsen, R.; Moenich, J.; Wehrle, R.

    1987-03-01

    A vacuum test chamber 1.6 meters in length for the synchrotron x-ray source has been completed and tested for the evaluation of welding, sealing and ultra high vacuum (UHV) applications. A base pressure of 6.5 x 10/sup -11/ Torr (nitrogen equivalent) has been achieved. The pumping system consists of non-evaporable getter (NeG) strips. The pumpdown procedure, NeG characteristics and results are discussed.

  17. 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.

  18. Characteristics of radiation safety for synchrotron radiation and X-ray free electron laser facilities.

    PubMed

    Asano, Yoshihiro

    2011-07-01

    Radiation safety problems are discussed for typical electron accelerators, synchrotron radiation (SR) facilities and X-ray free electron laser (XFEL) facilities. The radiation sources at the beamline of the facilities are SR, including XFEL, gas bremsstrahlung and high-energy gamma ray and photo-neutrons due to electron beam loss. The radiation safety problems for each source are compared by using 8 GeV class SR and XFEL facilities as an example.

  19. 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

  20. 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.

  1. 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.

  2. Characterization of surface carbon films on weathered Japaneseroof tiles by soft x-ray spectroscopy

    SciTech Connect

    Muramatsu, Y.; Yamashita, M.; Motoyama, M.; Hirose, M.; Denlinger, J.D.; Gullikson, E.M.; Perera, R.C.

    2004-07-15

    The effects of weathering on carbon films deposited onJapanese smoked roof tileswere investigated by soft x-ray absorption andemission spectroscopy using synchrotron radiation. X-ray absorptionmeasurements revealed that weathering oxidizes the carbon films and thatpartial carboxy chemical bonding occurs. Incident angle-dependent x-rayabsorption spectra in the C K region confirmed that the degree of theorientation at the surface of the oxidized carbon films decreases withweathering. However, the take-off angle-dependent C K x-ray emissionspectra showed that the orientation of the layered carbon structure ismaintained in the bulk portion when weathered. Therefore, it is confirmedthat oxidation proceeds from the surface of the carbon films. Weatheringdegrades and oxidizes the surface carbon films, which causes the metallicsilver color to change to darker gray.

  3. Surface profiling of X-ray mirrors for shaping focused beams.

    PubMed

    Laundy, David; Alianelli, Lucia; Sutter, John; Evans, Gwyndaf; Sawhney, Kawal

    2015-01-26

    Grazing incidence mirrors are a standard optic for focusing X-rays. Active mirrors, whose surface profile can be finely adjusted, allow control of beam shape and size at the sample. However, progress towards their routine use for beam shaping has been hampered by the strong striations in reflected beams away from the focal plane. Re-entrant (partly concave and partly convex) surface modifications are proposed for shaping X-ray beams to a top-hat in the focal plane while reducing the striations caused by unavoidable polishing errors. A method for constructing such surfaces with continuous height and slope (but only piecewise continuous curvature) will be provided. Ray tracing and wave propagation calculations confirm its effectiveness. A mirror system is proposed allowing vertical beam sizes in the range 0.5 to 10μm. A prototype will be fabricated and is expected to have applications on many synchrotron X-ray beamlines.

  4. Probing the self-assembled nanostructures of functional polymers with synchrotron grazing incidence X-ray scattering.

    PubMed

    Ree, Moonhor

    2014-05-01

    For advanced functional polymers such as biopolymers, biomimic polymers, brush polymers, star polymers, dendritic polymers, and block copolymers, information about their surface structures, morphologies, and atomic structures is essential for understanding their properties and investigating their potential applications. Grazing incidence X-ray scattering (GIXS) is established for the last 15 years as the most powerful, versatile, and nondestructive tool for determining these structural details when performed with the aid of an advanced third-generation synchrotron radiation source with high flux, high energy resolution, energy tunability, and small beam size. One particular merit of this technique is that GIXS data can be obtained facilely for material specimens of any size, type, or shape. However, GIXS data analysis requires an understanding of GIXS theory and of refraction and reflection effects, and for any given material specimen, the best methods for extracting the form factor and the structure factor from the data need to be established. GIXS theory is reviewed here from the perspective of practical GIXS measurements and quantitative data analysis. In addition, schemes are discussed for the detailed analysis of GIXS data for the various self-assembled nanostructures of functional homopolymers, brush, star, and dendritic polymers, and block copolymers. Moreover, enhancements to the GIXS technique are discussed that can significantly improve its structure analysis by using the new synchrotron radiation sources such as third-generation X-ray sources with picosecond pulses and partial coherence and fourth-generation X-ray laser sources with femtosecond pulses and full coherence.

  5. 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.

  6. 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.

  7. 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.

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

    PubMed

    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.

  9. 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.

  10. 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

  11. 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.

  12. 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).

  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).

  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. 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.

  17. 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.

  18. 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

  19. 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.

  20. Ion beam induced surface graphitization of CVD diamond for x-ray beam position monitor applications

    SciTech Connect

    Liu, Chian; Shu, D.; Kuzay, T.M.; Wen, L.; Melendres, C.A. |

    1996-12-31

    The Advanced Photon Source at ANL is a third-generation synchrotron facility that generates powerful x-ray beams on its undulator beamlines. It is important to know the position and angle of the x- ray beam during experiments. Due to very high heat flux levels, several patented x-ray beam position monitors (XBPM) exploiting chemical vapor deposition (CVD) diamond have been developed. These XBPMs have a thin layer of low-atomic-mass metallic coating so that photoemission from the x rays generate a minute but measurable current for position determination. Graphitization of the CVD diamond surface creates a very thin, intrinsic and conducting layer that can stand much higher temperatures and minimal x-ray transmission losses compared to the coated metallic layers. In this paper, a laboratory sputter ion source was used to transform selected surfaces of a CVD diamond substrate into graphite. The effect of 1-5 keV argon ion bombardment on CVD diamond surfaces at various target temperatures from 200 to 500 C was studied using Auger electron spectroscopy and in-situ electrical resistivity measurements. Graphitization after the ion bombardment has been confirmed and optimum conditions for graphitization studied. Raman spectroscopy was used to identify the overall diamond structure in the bulk of CVD diamond substrate after the ion bombardments. It was found that target temperature plays an important role in stability and electrical conductivity of the irradiated CVD diamonds.

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

    PubMed

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

    2015-01-01

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

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

    PubMed

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

    2015-01-01

    The GALAXIES beamline at the SOLEIL synchrotron is dedicated to inelastic X-ray scattering (IXS) and photoelectron spectroscopy (HAXPES) in the 2.3-12 keV hard X-ray range. These two techniques offer powerful complementary methods of characterization of materials with bulk sensitivity, chemical and orbital selectivity, resonant enhancement and high resolving power. After a description of the beamline components and endstations, the beamline capabilities are demonstrated through a selection of recent works both in the solid and gas phases and using either IXS or HAXPES approaches. Prospects for studies on liquids are discussed. PMID:25537606

  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. 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

  5. In situ synchrotron radiation X-ray microspectroscopy of polymer microcontainers.

    PubMed

    Graf-Zeiler, Birgit; Fink, Rainer H; Tzvetkov, George

    2011-12-23

    Direct, real-time analytical techniques that provide high-resolution information on the chemical composition and submicrometer structure of various polymer micro- and nanoparticles are in high demand in a range of life science disciplines. Synchrotron-based scanning transmission X-ray microspectroscopy (STXM) combines both local-spot chemical information (assessed via near-edge X-ray absorption fine structure spectroscopy) and imaging with resolution of several tens of nanometers, and thus can yield new insights into the nanoscale properties of these materials. Furthermore, this method allows in situ examination of soft-matter samples in aqueous/gaseous environments and under external stimuli, such as temperature, pressure, ultrasound, and light irradiation. This Minireview highlights some recent progress in the application of the STXM technique to study the temperature-dependent behavior of polymer core-shell microcapsules and to characterize the physicochemical properties of the supporting shells of gas-filled microbubbles in their natural hydrated state.

  6. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-09-01

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

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

    PubMed Central

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

    2016-01-01

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

  9. 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

  10. 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.

  11. Algorithms for three-dimensional chemical analysis via multi-energy synchrotron X-ray tomography

    NASA Astrophysics Data System (ADS)

    Ham, Kyungmin; Butler, Leslie G.

    2007-08-01

    The conversion of X-ray tomography images into three-dimensional chemical composition requires accurate mass absorption values, high-quality images, and a robust fitting algorithm. The least-squares fits of the images to a three-dimensional chemical composition can proceed with several different options such as minimal vs. over-determined and/or constrained parameters. This project has investigated the impact of XAFS features and a limited CCD dynamic range. These simulated results are compared to a recent experimental project in which synchrotron X-ray tomography was used to image a polymer blend, and from those images, calculated three-dimensional chemical composition maps of the two-component flame retardant, a brominated phthalimide dimer, Saytex ™ BT-93 and a synergist, antimony(III) oxide (Sb 2O 3).

  12. 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.

  13. Residual strain gradient determination in metal matrix composites by synchrotron X-ray energy dispersive diffraction

    NASA Technical Reports Server (NTRS)

    Kuntz, Todd A.; Wadley, Haydn N. G.; Black, David R.

    1993-01-01

    An X-ray technique for the measurement of internal residual strain gradients near the continuous reinforcements of metal matrix composites has been investigated. The technique utilizes high intensity white X-ray radiation from a synchrotron radiation source to obtain energy spectra from small (0.001 cu mm) volumes deep within composite samples. The viability of the technique was tested using a model system with 800 micron Al203 fibers and a commercial purity titanium matrix. Good agreement was observed between the measured residual radial and hoop strain gradients and those estimated from a simple elastic concentric cylinders model. The technique was then used to assess the strains near (SCS-6) silicon carbide fibers in a Ti-14Al-21Nb matrix after consolidation processing. Reasonable agreement between measured and calculated strains was seen provided the probe volume was located 50 microns or more from the fiber/matrix interface.

  14. 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

  15. 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.

  16. 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

  17. 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

  18. 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

  19. 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.

  20. Investigation of artefact sources in synchrotron microtomography via virtual X-ray imaging

    NASA Astrophysics Data System (ADS)

    Vidal, F. P.; Létang, J. M.; Peix, G.; Cloetens, P.

    2005-06-01

    Qualitative and quantitative use of volumes reconstructed by computed tomography (CT) can be compromised due to artefacts which corrupt the data. This article illustrates a method based on virtual X-ray imaging to investigate sources of artefacts which occur in microtomography using synchrotron radiation. In this phenomenological study, different computer simulation methods based on physical X-ray properties, eventually coupled with experimental data, are used in order to compare artefacts obtained theoretically to those present in a volume acquired experimentally, or to predict them for a particular experimental setup. The article begins with the presentation of a synchrotron microtomographic slice of a reinforced fibre composite acquired at the European Synchrotron Radiation Facility (ESRF) containing streak artefacts. This experimental context is used as the motive throughout the paper to illustrate the investigation of some artefact sources. First, the contribution of direct radiation is compared to the contribution of secondary radiations. Then, the effect of some methodological aspects are detailed, including under-sampling, sample and camera misalignment, sample extending outside of the field of view and photonic noise. The effect of harmonic components present in the experimental spectrum are also simulated. Afterwards, detector properties, such as its impulse response or defective pixels, are taken into account. Finally, the importance of phase contrast effects is evaluated. In the last section, this investigation is discussed by putting emphasis on the experimental context which is used throughout this paper.

  1. Biological X-ray spectroscopy on 3rd generation synchrotron radiation sources

    NASA Astrophysics Data System (ADS)

    Ralston, Corie Y.; Chen, Jie; Peng, Gang; George, Simon J.; van Elp, Jan; Cramer, Stephen P.

    1995-02-01

    Third generation synchrotron radiation sources such as the Advanced Light Source (ALS) at Lawrence Berkeley Laboratory deliver 1-2 orders of magnitude more monochromatic flux (and many orders of magnitude higher brightness) than previously available. This paper describes the ring and existing beamlines of the advanced light source, and plans for crystallography and elliptical wiggler stations are discussed. Using nickel metalloprotein spectra recorded at NSLS and SSRL as examples, this paper describes how the higher monochromatic flux available from the ALS will be used for biological soft X-ray spectroscopy.

  2. Synchrotron X-ray Optics Testing at Beamline 1-BM at the Advanced Photon Source

    NASA Astrophysics Data System (ADS)

    Macrander, Albert; Kujala, Naresh

    2014-03-01

    Beamline 1-BM at the Advanced Photon Source has been reconfigured, in part for testing of synchrotron optics with both monochromatic and white beams. Monochromatic energies between 6 and 30 keV are available. Primary agendas include both white beam and monochromatic beam topography, Talbot grating interferometry for measurement of coherence lengths and wavefronts, and micro-focusing. Recent examples will include topography of sapphire , tests of Kirkpatrick-Baez mirrors, and tests of multilayer Laue lenses. Analyzers for Inelastic X-ray Scattering has also been characterized by two user groups. Supported from U.S. DOE, Office of Science, Contract No. DE-AC-02-06CH11357.

  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. A magnetizing system for dichroism measurements in soft x-ray emission excited by synchrotron radiation

    SciTech Connect

    Dallera, C.; Ghiringhelli, G.; Braicovich, L.

    1996-02-01

    We present the design and performance of a magnetic circuit suitable for magnetizing solid samples in the measurements of soft x-ray emission dichroism excited by synchrotron radiation. The system allows a variety of samples to be magnetized and satisfies the rather stringent geometrical constraints due to the need for minimizing the effect of photon self-absorption by the sample. The magnetic circuit is ultrahigh vacuum compatible, can reach about 2800 G, and allows fine adjustment of sample position. {copyright} {ital 1996 American Institute of Physics.}

  5. 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.

  6. 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.

  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. 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.

  9. 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.

  10. 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.

  11. 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

  12. 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

  13. Total reflection x-ray fluorescence analysis with synchrotron radiation and other sources for trace element determination

    NASA Astrophysics Data System (ADS)

    Wobrauschek, Peter; Streli, Christina

    1997-01-01

    Total reflection x-ray fluorescence analysis (TXRF) is an accepted powerful analytical tool for trace element determination in various kinds of samples. In typical applications like environmental, medical and technical sample analysis as well as for quality control during production processes, ultralow concentrations at the pg/g level, or femtogram masses, have to be determined. The combination of synchrotron radiation (SR) and multilayer monochromators together with TXRF is perfectly suited to meet the requirements. Best results can be expected from SR-TXRF though cost and accessability to SR sources limit the application. In some cases the additional inherent advantage of XRF as a nondestructive method is important. Another approach to reach such low detection limits is to increase the photon flux on the sample by means of high power x-ray tubes and multilayer focusing x-ray optics. With standard laboratory equipment the choice of appropriate anode materials for efficient excitation of specific elements and an optimal design of the energy dispersive spectrometer can also increase sensitivity. Various experimental setups used for EDXRF of the elements from B to U by K-shell excitation will be presented and discussed. The results from ultralow trace element analysis of surface impurities on Si wafers demonstrate the excellent potential of this method. With SR-TXRF the detection limits for medium Z elements can be below 20 femtogram.

  14. 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.

  15. 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.

  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. Synchrotron-based Imaging and tomography with hard X-rays.

    SciTech Connect

    Rau, C.; Crecea, V.; Liu, W.; Richter, C. P.; Peterson, K. M.; Jemian, P. R.; Neuhausler, U.; Schneider, G.; Yu, X.; Braun, P. V.; Chiang, T. C.; Robinson, I. K.; X-Ray Science Division; Univ. of Illinois; Purdue Univ.; Northwestern Univ.; Univ. Bielefeld; Univ. Coll. London; Bessy GmbH; NIST

    2007-03-28

    Hard X-ray imaging with synchrotron radiation is a powerful tool to study opaque materials on the micro- and nano-lengthscales. Different imaging methods are available with an instrument recently built at Sector 34 of the Advanced Photon Source. In-line phase contrast imaging is performed with micrometer resolution. Increased spatial resolution is achieved using cone-beam geometry. The almost parallel beam is focused with a Kirkpatrick-Baez mirror system. The focal spot serves as a diverging secondary source. An X-ray magnified image of the sample is projected on the detector. For imaging and tomography with sub-100 nm resolution, an X-ray full-field microscope has been built. It uses a Kirkpatrick-Baez mirror (KB) as a condenser optic, followed by a micro-Fresnel zone plate (FZP) as an objective lens. The zone plates presently provide 50-85 nm spatial resolution when operating the microscope with photon energy between 6 and 12 keV. Tomography experiments have been performed with this new device.

  19. 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.

  20. 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.

  1. 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

  2. Synchrotron X-Ray Microdiffraction Reveals Intrinsic Structural Features of Amyloid Deposits In Situ

    PubMed Central

    Briki, Fatma; Vérine, Jérôme; Doucet, Jean; Bénas, Philippe; Fayard, Barbara; Delpech, Marc; Grateau, Gilles; Riès-Kautt, Madeleine

    2011-01-01

    Amyloidoses are increasingly recognized as a major public health concern in Western countries. All amyloidoses share common morphological, structural, and tinctorial properties. These consist of staining by specific dyes, a fibrillar aspect in electron microscopy and a typical cross-β folding in x-ray diffraction patterns. Most studies that aim at deciphering the amyloid structure rely on fibers generated in vitro or extracted from tissues using protocols that may modify their intrinsic structure. Therefore, the fine details of the in situ architecture of the deposits remain unknown. Here, we present to our knowledge the first data obtained on ex vivo human renal tissue sections using x-ray microdiffraction. The typical cross-β features from fixed paraffin-embedded samples are similar to those formed in vitro or extracted from tissues. Moreover, the fiber orientation maps obtained across glomerular sections reveal an intrinsic texture that is correlated with the glomerulus morphology. These results are of the highest importance to understanding the formation of amyloid deposits and are thus expected to trigger new incentives for tissue investigation. Moreover, the access to intrinsic structural parameters such as fiber size and orientation using synchrotron x-ray microdiffraction, could provide valuable information concerning in situ mechanisms and deposit formation with potential benefits for diagnostic and therapeutic purposes. PMID:21767502

  3. 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.

  4. 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.

  5. 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.

  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. 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

  8. 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.

  9. 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.

  10. 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.

  11. Solution synchrotron x-ray diffraction reveals structural details of lipid domains in ternary mixtures

    NASA Astrophysics Data System (ADS)

    Yuan, Jing; Kiss, Alexander; Pramudya, Yohanes H.; Nguyen, Lam T.; Hirst, Linda S.

    2009-03-01

    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 lo (liquid ordered) and ld (liquid disordered) phases. The high intensity of synchrotron x rays allows the observation of up to 5 orders of diffraction from the lo phase, whereas only two are clearly visible when the ld phase alone is present. This data can be collected in ˜1min/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 10-12mol% 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 soft X-ray and field-emission electron sources: a comparison.

    PubMed

    Spence, J C H; Howells, M R

    2002-12-01

    The soft X-ray spectral region and the useful range of electron energy-loss spectroscopy are very similar, both including the energy range 100-1000 eV. Moreover, well-developed monochromators and parallel detection devices with comparable resolution exist for both. Despite the differing interactions of electrons and photons, many complementary experiments in imaging, spectroscopy and diffraction have been performed using both techniques. We therefore compare the brightness, degeneracy, monochromaticity, beam size, source size, spatial and temporal coherence of field-emission electron beams and soft X-ray synchrotron radiation from typical undulators. Recent brightness values for nanotip field emitters and undulators, both measured and calculated, are provided with examples from the Advanced Light Source synchrotron-radiation facility at Berkeley USA. The quantum mechanical upper limit on source brightness, as well as relationships among beam brightness, coherence parameters, and degeneracy, are discussed. Factors which limit these parameters and methods of measurement are reviewed, and the implications for diffraction, imaging and spectroscopic experiments as well as radiation damage are briefly commented on.

  13. Surface X-ray emission from lanthanide metals

    NASA Astrophysics Data System (ADS)

    Hübinger, F.; Shulakov, A. S.; Starke, K.; Grigoriev, A.; Kaindl, G.

    2003-02-01

    O 3 X-ray emission (XE) upon 5p 3/2 electron-impact ionization of La(0 0 0 1) and Sm(0 0 0 1) metal surfaces exhibits up to 30% spectral intensity from the topmost atomic surface layer. The energy separation of surface and bulk XE peaks is explained by the surface core-level shift of La and the surface valence transition of Sm. While the bulk XE spectra are in reasonable agreement with theoretical sd partial density of states (DOS), the experimental access to the partial surface-layer DOS opens new opportunities in studying surface phenomena in lanthanide metals and compounds.

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

    PubMed

    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.

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

    SciTech Connect

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

    2012-12-15

    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.

  16. On the Correlation Between Fatigue Striation Spacing and Crack Growth Rate: A Three-Dimensional (3-D) X-ray Synchrotron Tomography Study

    NASA Astrophysics Data System (ADS)

    Williams, Jason J.; Yazzie, Kyle E.; Connor Phillips, N.; Chawla, Nikhilesh; Xiao, Xinghui; de Carlo, Francesco; Iyyer, Nagaraja; Kittur, Maddan

    2011-12-01

    In situ three-dimensional (3-D) X-ray synchrotron tomography of fatigue crack growth was conducted in a 7075-T6 aluminum alloy. Local measurements of da/ dN were possible with the 3-D data sets obtained from tomography. A comparison with fatigue striation spacings obtained from scanning electron microscopy of the fracture surfaces yielded excellent correlation with da/ dN obtained from tomography. The X-ray tomography technique can be used to obtain a highly accurate and representative measurements of crack growth locally in the microstructure of the material.

  17. 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.

  18. 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.

  19. 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.

  20. 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

  1. Soft x-ray emission spectroscopy using monochromatized synchrotron radiation (invited)

    NASA Astrophysics Data System (ADS)

    Nordgren, J.; Bray, G.; Cramm, S.; Nyholm, R.; Rubensson, J.-E.; Wassdahl, N.

    1989-07-01

    Soft x-ray emission spectroscopy is a common tool for the study of the electronic structure of molecules and solids. However, the interpretation of spectra is sometimes made difficult by overlaying lines due to satellite transitions or close-lying core holes. Also, irrelevant inner core transitions may accidentally fall in the wavelength region under study. These problems, which often arise for spectra excited with electrons or broadband photon sources can be removed by using monochromatized synchrotron radiation. In addition, one achieves other advantages as well, such as the ability to study resonant behavior. Another important aspect is the softness of this excitation agent, which allows chemically fragile compounds to be investigated. In this work we demonstrate the feasibility of using monochromatized synchrotron radiation to excite soft x-ray spectra. We also show new results which have been accomplished as a result of the selectivity of the excitation. The work has been carried out using the Flipper I wiggler beamline at HASYLAB in Hamburg using a new grazing incidence instrument designed specifically for this experiment. The photon flux at the Flipper I station (typically 5×1012 photons per second on the sample with a 1% bandpass) is enough to allow soft x-ray fluorescence spectra to be recorded at relatively high resolution and within reasonable accumulation times (typically, the spectra presented in this work were recorded in 30 min). The spectrometer is based on a new concept which allows the instrument to be quite small, still covering a large wavelength range (10-250 Å). The basic idea involves the use of several fixed mounted gratings and a large two-dimensional detector. The grating arrangement provides simple mounting within a limited space and, in particular, large spectral range. The detector can be moved in a three-axis coordinate system in order to cover the different Rowland curves defined by the different gratings. The arrangement permits

  2. 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.

  3. First Observation of a Wooden Foreign Body in Soft Palate by Means of Synchrotron X-Ray Refraction Contrast

    NASA Astrophysics Data System (ADS)

    Mori, Koichi; Sekine, Norio; Sato, Hitoshi; Shikano, Naoto; Shimao, Daisuke; Shiwaku, Hideaki; Hyodo, Kazuyuki; Ohashi, Kenjirou

    2002-08-01

    A clear image of a wooden chopstick penetrating the soft palate of a pig-head was obtained using highly coherent synchrotron X-ray. The image was recorded on a mammography film with an intensifying screen at an X-ray energy of 35 keV. The tubular tissues as sieve tubes or ducts in the chopsticks appeared as white-black line images by means of X-ray refraction contrast. This method may enable development of an accurate diagnostic method in the field of penetrating trauma by wood.

  4. 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.

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

    DOE PAGESBeta

    Feng, Huan; Zhang, Weiguo; Qian, Yu; Liu, Wenliang; Yu, Lizhong; Yoo, Shinjae; Wang, Jun; Wang, Jia -Jun; Eng, Christopher; Liu, Chang -Jun; et al

    2016-06-15

    This paper 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 themore » root epidermis and that other metals correlate significantly with Fe, suggesting that Fe nanoparticles play an important role in metal scavenging in the epidermis.« less

  6. 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

  7. MESSENGER X-Ray Spectrometer Detection of Electron-induced X-ray Fluorescence from Mercury's Surface

    NASA Astrophysics Data System (ADS)

    Starr, R. D.; Nittler, L. R.; Weider, S. Z.; Rhodes, E. A.; Schriver, D.; Schlemm, C. E., II; Solomon, S. C.

    2011-12-01

    The X-Ray Spectrometer (XRS) onboard the MESSENGER spacecraft measures elemental abundances on the surface of Mercury by detecting fluorescent X-ray emissions induced on the planet's surface by the incident solar X-ray flux. The most prominent fluorescent lines are the Kα lines from the elements Mg, Al, Si, S, Ca, Ti, and Fe (1-10 keV). The XRS began orbital observations on 23 March 2011 and has observed X-ray fluorescence from the surface of the planet during both "quiet" Sun and flaring conditions whenever a sunlit portion of Mercury has been within the XRS field of view. XRS can detect the characteristic X-rays of Mg, Al, and Si during quiet-Sun conditions, but solar flares are required to produce measureable signals from the elements of higher atomic number such as S, Ca, Ti, and Fe. Nevertheless, X-ray fluorescence up to the Ca fluorescent line (3.69 keV) has been detected from Mercury's surface at times when the XRS field of view included only unlit portions of the planet or during quiet-Sun illumination. To date, seven such events have been detected and are identified as electron-induced X-ray emission produced by ~1-10 keV electrons interacting with Mercury's surface. Electrons in this energy range were detected by the XRS during the three Mercury flybys, and since the beginning of orbital operations electrons of this same energy range have been detected by XRS during almost every orbit. These electron events last from minutes to tens of minutes. Electron transport models suggest that a large percentage of these quasi-trapped electrons do not complete even a single orbit about Mercury before impacting the surface. Knowledge of the precipitating electron distribution at the planet's surface makes it possible to infer surface composition from the measured fluorescent spectra, providing additional measurement opportunities for the XRS.

  8. 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.

  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. Accounting for low-frequency synchrotron X-ray beam position fluctuations for dynamic visualizations.

    PubMed

    Hinebaugh, J; Challa, P R; Bazylak, A

    2012-11-01

    Synchrotron X-ray radiography on beamline 05B1-1 at the Canadian Light Source Inc. was employed to study dynamic liquid water transport in the porous electrode materials of polymer electrolyte membrane fuel cells. Dynamic liquid water distributions were quantified for each radiograph in a sequence, and non-physical liquid water measurements were obtained. It was determined that the position of the beam oscillated vertically with an amplitude of ~25 µm at the sample and a frequency of ~50 mHz. In addition, the mean beam position moved linearly in the vertical direction at a rate of 0.74 µm s(-1). No evidence of horizontal oscillations was detected. In this work a technique is presented to account for the temporal and spatial dependence of synchrotron beam intensity, which resulted in a significant reduction in false water thickness. This work provides valuable insight into the treatment of radiographic time-series for capturing dynamic processes from synchrotron radiation.

  11. 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.

  12. 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

  13. 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.

  14. 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.

  15. 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

  16. 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

  17. 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.

  18. Synchrotron X-ray diffraction study of 112-type Ca1-xLaxFeAs2

    NASA Astrophysics Data System (ADS)

    Katayama, N.; Sugawara, K.; Nakano, A.; Kitou, S.; Sugiyama, Y.; Kawaguchi, N.; Ito, H.; Higuchi, T.; Fujii, T.; Sawa, H.

    2015-11-01

    Synchrotron X-ray diffraction studies of Ca1-xLaxFeAs2 with monovalent arsenic zigzag chain layers are presented. While the crystal twins appear in all samples for the nominal composition of x = 0.25, we successfully obtained the samples without crystal twins for the nominal composition of x = 0.17. We present the structural parameters obtained using the synchrotron X-ray diffraction data and physical properties for the samples with x = 0.17. We further discuss the tactics for exploring novel 112-type iron arsenides without arsenic zigzag chains.

  19. 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.

  20. 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.

  1. 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.

  2. Synchrotron Radiation {mu}-X Ray Fluorescence on Multicellular Tumor Spheroids

    SciTech Connect

    Burattini, E.; Cinque, G.; Bellisola, G.; Fracasso, G.; Colombatti, M.; Monti, F.

    2003-01-24

    Synchrotron Radiation micro X-Ray Fluorescence (SR {mu}-XRF) was applied for the first time to map the trace element content on Multicellular Tumor Spheroids (MTS), i.e. human cell clusters used as an in vitro model for testing micrometastases responses to antitumoral drugs. In particular, immunotoxin molecules composed of a carrier protein (Transferrin) bound to a powerful cytotoxin (Ricin A), were here considered as representatives of a class of therapheutic macromolecules used in cancer theraphy. Spheroids included in polyacrylamide gel and placed inside quartz capillaries were studied at the ESRF ID22 beamline using a 15 keV monochromatic photon microbeam. Elemental maps (of Fe, Cu, Zn and Pb) on four groups of spheroids grown under different conditions were studied: untreated, treated only with the carrier molecule or with the toxin alone, and with the complete immunotoxin molecule (carrier+toxin). The results indicate that the distribution of Zn and, to some extent, Cu in the spheroid cells is homogeneous and independent of the treatment type. Total Reflection X-Ray Fluorescence (TR-XRF) was also applied to quantify the average trace element content in the spheroids. Future developments of the technique are finally outlined on the basis of these preliminary results.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. Synchrotron Radiation μ-X Ray Fluorescence on Multicellular Tumor Spheroids

    NASA Astrophysics Data System (ADS)

    Burattini, E.; Cinque, G.; Bellisola, G.; Fracasso, G.; Monti, F.; Colombatti, M.

    2003-01-01

    Synchrotron Radiation micro X-Ray Fluorescence (SR μ-XRF) was applied for the first time to map the trace element content on Multicellular Tumor Spheroids (MTS), i.e. human cell clusters used as an in vitro model for testing micrometastases responses to antitumoral drugs. In particular, immunotoxin molecules composed of a carrier protein (Transferrin) bound to a powerful cytotoxin (Ricin A), were here considered as representatives of a class of therapheutic macromolecules used in cancer theraphy. Spheroids included in polyacrylamide gel and placed inside quartz capillaries were studied at the ESRF ID22 beamline using a 15 keV monochromatic photon microbeam. Elemental maps (of Fe, Cu, Zn and Pb) on four groups of spheroids grown under different conditions were studied: untreated, treated only with the carrier molecule or with the toxin alone, and with the complete immunotoxin molecule (carrier+toxin). The results indicate that the distribution of Zn and, to some extent, Cu in the spheroid cells is homogeneous and independent of the treatment type. Total Reflection X-Ray Fluorescence (TR-XRF) was also applied to quantify the average trace element content in the spheroids. Future developments of the technique are finally outlined on the basis of these preliminary results.

  9. 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.

  10. Investigation of GEM-Micromegas detector on X-ray beam of synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Zhang, Yu-Lian; Qi, Hui-Rong; Hu, Bi-Tao; Fan, Sheng-Nan; Wang, Bo; Liu, Mei; Zhang, Jian; Liu, Rong-Guang; Chang, Guang-Cai; Liu, Peng; Ouyang, Qun; Chen, Yuan-Bo; Yi, Fu-Ting

    2014-04-01

    To reduce the discharge of the standard bulk Micromegas and GEM detectors, a GEM-Micromegas detector was developed at the Institute of High Energy Physics. Taking into account the advantages of the two detectors, one GEM foil was set as a preamplifier on the mesh of Micromegas in the structure and the GEM preamplification decreased the working voltage of Micromegas to significantly reduce the effect of the discharge. At the same gain, the spark probability of the GEM-Micromegas detector can be reduced to a factor 0.01 compared to the standard Micromegas detector, and an even higher gain could be obtained. This paper describes the performance of the X-ray beam detector that was studied at 1W2B Laboratory of Beijing Synchrotron Radiation Facility. Finally, the result of the energy resolution under various X-ray energies was given in different working gases. This indicates that the GEM-Micromegas detector has an energy response capability in an energy range from 6 keV to 20 keV and it could work better than the standard bulk-Micromegas.

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

    NASA Astrophysics Data System (ADS)

    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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. Synchrotron X-ray microprobe and computed microtomography for characterization of nanocatalysts

    NASA Astrophysics Data System (ADS)

    Jones, K. W.; Feng, H.; Lanzirotti, A.; Mahajan, D.

    2005-12-01

    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 μm) Fe2O3 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 103 μm3.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. A novel crystal bender for x-ray synchrotron radiation monochromators

    NASA Astrophysics Data System (ADS)

    Zaeper, Ralf; Richwin, Matthias; Lützenkirchen-Hecht, Dirk; Frahm, Ronald

    2002-03-01

    A new bending mechanism for an indirectly water cooled monochromator crystal has been developed. The main design goals were a lightweight construction, ease of manufacture, and control. The construction consists of a U-shaped first Si(111) crystal, which can be bent by compressed air to compensate the bowing induced by the heat load from the impinging white synchrotron radiation. The performance of the system was tested at the x-ray undulator beamline BW1 at HASYLAB (Hamburg, Germany). For heat loads between ˜100 and 400 W, rebending of the crystal significantly increases the intensity of the monochromatic beam while the rocking curve is narrowed accordingly, typical widths obtained at 8.9 keV photon energy amount to about 10 arc sec.

  3. 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.

  4. Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography.

    PubMed

    Harry, Katherine J; Parkinson, Dilworth Y; Balsara, Nitash P

    2015-08-26

    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.

  5. 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.

  6. 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.

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

    SciTech Connect

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

    1998-07-01

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

  8. 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.

  9. 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

  10. 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

  11. Bio-metals imaging and speciation in cells using proton and synchrotron radiation X-ray microspectroscopy

    PubMed Central

    Ortega, Richard; Devès, Guillaume; Carmona, Asunción

    2009-01-01

    The direct detection of biologically relevant metals in single cells and of their speciation is a challenging task that requires sophisticated analytical developments. The aim of this article is to present the recent achievements in the field of cellular chemical element imaging, and direct speciation analysis, using proton and synchrotron radiation X-ray micro- and nano-analysis. The recent improvements in focusing optics for MeV-accelerated particles and keV X-rays allow application to chemical element analysis in subcellular compartments. The imaging and quantification of trace elements in single cells can be obtained using particle-induced X-ray emission (PIXE). The combination of PIXE with backscattering spectrometry and scanning transmission ion microscopy provides a high accuracy in elemental quantification of cellular organelles. On the other hand, synchrotron radiation X-ray fluorescence provides chemical element imaging with less than 100 nm spatial resolution. Moreover, synchrotron radiation offers the unique capability of spatially resolved chemical speciation using micro-X-ray absorption spectroscopy. The potential of these methods in biomedical investigations will be illustrated with examples of application in the fields of cellular toxicology, and pharmacology, bio-metals and metal-based nano-particles. PMID:19605403

  12. 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.

  13. Sulfur fixation in wood mapped by synchrotron X-ray studies: implications for environmental archives.

    PubMed

    Fairchild, Ian I; Loader, Neil J; Wynn, Peter M; Frisia, Silvia; Thomas, Peter A; Lageard, Jonathan G A; De Momi, Anna; Hartland, Adam; Borsato, Andrea; La Porta, Nicola; Susini, Jean

    2009-03-01

    There is a shortage of archives of sulfur that can be used to investigate industrial orvolcanic pollution in terrestrial catchments, but the role of S as a nutrient, coupled with sparse published evidence, suggests that trees are promising targets. We focused on two conifer species (Picea abies (L.) Karst and Abies alba Miller) from an Alpine site in NE Italy. Bulk analyses of Abies demonstrate that S concentrations were higher in the second half of the 20th century but with some high outliers possibly reflecting particulate impurities. X-ray synchrotron analyses confirmed the observed time trend, which is similar to that of a nearby stalagmite, and reflects an atmospheric pollution record mediated by storage in the soil and ecosystem. S and P were found to be localized in the inner cell wall (ca. 2 microm wide), local thickenings of which probably account for some outlying high values of S in synchrotron studies. S occurs as a mixture of oxidation states (0 to +0.5, +2, +5, and +6) which are consistent in space and time. The results indicate that wood older than a few years contains archive-quality S but that robust conclusions require multiple replicate analyses.

  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 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

  16. 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.

  17. 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.

  18. 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.

  19. Chemical mapping of paleontological and archeological artifacts with synchrotron X-rays.

    PubMed

    Bergmann, Uwe; Manning, Phillip L; Wogelius, Roy A

    2012-01-01

    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. PMID:22524223

  20. 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.

  1. 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.

  2. 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.

  3. Synchrotron X-ray fluorescence studies of a bromine-labelled cyclic RGD peptide interacting with individual tumor cells.

    PubMed

    Sheridan, Erin J; Austin, Christopher J D; Aitken, Jade B; Vogt, Stefan; Jolliffe, Katrina A; Harris, Hugh H; Rendina, Louis M

    2013-03-01

    The first example of synchrotron X-ray fluorescence imaging of cultured mammalian cells in cyclic peptide research is reported. The study reports the first quantitative analysis of the incorporation of a bromine-labelled cyclic RGD peptide and its effects on the biodistribution of endogenous elements (for example, K and Cl) within individual tumor cells.

  4. 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.

  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. 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.

  7. AFM-measured surface roughness of SU-8 structures produced by deep x-ray lithography

    NASA Astrophysics Data System (ADS)

    Vora, K. D.; Lochel, B.; Harvey, E. C.; Hayes, J. P.; Peele, A. G.

    2006-10-01

    Deep x-ray lithography is a well-known technique used to pattern ultra high aspect ratio microstructures. It relies on the fact that higher energy synchrotron x-rays have the ability to penetrate millimeters of resist layers. However, the spectral shape of the beam will vary as a function of penetration depth, sometimes by design, so as to distribute the dose differently for different thickness structures and always as a result of filtering of lower energies. Some studies have shown that in PMMA sidewall roughness can be affected by spectral issues. SU-8 is now the resist of choice for certain high aspect ratio structures due to its high sensitivity and contrast. As sidewall roughness is a key parameter in several potential applications of high aspect ratio structures, we therefore investigated the surface roughness of 500 µm thick SU-8 structures exposed using beam spectra with peak energies between 3 keV and 12 keV. Results indicate that as the x-ray energy increases so too does the surface roughness. The surface roughness also increases as a function of feature depth. We attribute this to the random secondary physical processes of photo and Auger electron scattering both of which are strongly energy dependent.

  8. 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.

  9. 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

  10. 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.

  11. 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.

  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. 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.

  14. YB66 as a new soft x-ray monochromator for synchrotron radiation (abstract)

    NASA Astrophysics Data System (ADS)

    Rek, Z.; Wong, Joe; Tanaka, T.; Shimkaveg, G.; Eckart, M.

    1992-01-01

    YB66, a complex binary semiconducting compound with a cubic crystal structure and a lattice parameter of 23.44 Å, is potentially a very good candidate for monochromatization of soft x-ray synchrotron radiation. The features such as: a large interatomic spacing, lack of absorption edges by the constituent elements in the region 1-2 keV, very narrow intrinsic rocking curves for (400) and (222) reflections and good thermal and mechanical properties make the material very useful. Using the known structure factors for the (400) and (222) reflections, having 2d values of 11.76 and 13.53 Å, respectively, their rocking curves have been calculated and are shown [J. Wang, G. Shimkaveg, W. Goldstein, M. Eckart, T. Tanaka, Z. Rek, H. Tompkins, Nucl. Instrum. Methods A 291, 243 (1990)] to be comparable to or better than that of beryl (101¯0). A novel indirect heating floating zone method for growing large size crystals was used by Tanaka and his coworkers in Japan [T. Tanaka, S. Otani, and Y. Ishizawa, J. Cryst. Growth 73, 31 (1985)]. Numerous modifications of this technique and double-zone passes were applied to reduce sub grain structure and lattice deformations. The crystalline perfection and absence of defects is critical to obtaining high energy resolution and good crystal reflectivity. Crystals large enough to accept 1 mrad of radiation, with growth direction [100] and [110] were grown. Rocking curve measurements, etch pit density, and x-ray white beam topography are used to characterize the quality of these crystals as a function of some critical growth parameters. Most crystals exhibit the existence of sub grain boundaries. Areas perfect enough were observed to give ˜ 0.5 eV energy resolution. Recent experiments in crystal growth, results of crystals characterization, and comparison with theoretical calculations will be discussed.

  15. Subacute neuropathological effects of microplanar beams of x-rays from a synchrotron wiggler.

    PubMed

    Slatkin, D N; Spanne, P; Dilmanian, F A; Gebbers, J O; Laissue, J A

    1995-09-12

    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-microns-wide beam or to a horizontal 7-mm-wide, 42-microns-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 microns 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 < or = 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.

  16. Synchrotron X-ray studies of epitaxial ferroelectric thin films and nanostructures

    NASA Astrophysics Data System (ADS)

    Klug, Jeffrey A.

    The study of ferroelectric thin films is a field of considerable scientific and technological interest. In this dissertation synchrotron x-ray techniques were applied to examine the effects of lateral confinement and epitaxial strain in ferroelectric thin films and nanostructures. Three materials systems were investigated: laterally confined epitaxial BiFeO3 nanostructures on SrTiO3 (001), ultra-thin commensurate SrTiO 3 films on Si (001), and coherently strained films of BaTiO3 on DyScO3 (110). Epitaxial films of BiFeO3 were deposited by radio frequency magnetron sputtering on SrRuO3 coated SrTiO 3 (001) substrates. Laterally confined nanostructures were fabricated using focused ion-beam processing and subsequently characterized with focused beam x-ray nanodiffraction measurements with unprecedented spatial resolution. Results from a series of rectangular nanostructures with lateral dimensions between 500 nm and 1 mum and a comparably-sized region of the unpatterned BiFeO3 film revealed qualitatively similar distributions of local strain and lattice rotation with a 2-3 times larger magnitude of variation observed in those of the nanostructures compared to the unpatterned film. This indicates that lateral confinement leads to enhanced variation in the local strain and lattice rotation fields in epitaxial BiFeO3 nanostructures. A commensurate 2 nm thick film of SrTiO3 on Si was characterized by the x-ray standing wave (XSW) technique to determine the Sr and Ti cation positions in the strained unit cell in order to verify strain-induced ferroelectricity in SrTiO3/Si. A Si (004) XSW measurement at 10°C indicated that the average Ti displacement from the midpoint between Sr planes was consistent in magnitude to that predicted by a density functional theory (DFT) calculated ferroelectric structure. The Ti displacement determined from a 35°C measurement better matched a DFT-predicted nonpolar structure. The thin film extension of the XSW technique was employed to

  17. 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

  18. 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.

  19. 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.

  20. 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.

  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. Measurement of the x-ray tube anodes' surface profile and its effects on the x-ray spectra

    SciTech Connect

    Erdelyi, M.; Lajko, M.; Kakonyi, R.; Szabo, G.

    2009-02-15

    An experimental study--involving measurements with an optical microscope, a profilometer, and a scanning electron microscope--for determination of the surface profile of x-ray tube anodes is presented. The islands on the ''mud-flatting'' surface are separated by approximately 8 {mu}m deep cracks. The surface roughness on the island is typically below 1 {mu}m, and the area ratio of cracks to the total surface is higher on the more extensively used regions (anode aging). A simple model was proposed to calculate the spectrum modification introduced by the rough surface. Loss of x-ray intensity of 4% was predicted using the roughest surface at a small emission angle.

  3. 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.

  4. 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.

  5. 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

  6. Versatile wide angle diffraction setup for simultaneous wide and small angle x-ray scattering measurements with synchrotron radiation

    SciTech Connect

    Rueda, D.R.; Garcia-Gutierrez, M.C.; Nogales, A.; Capitan, M.J.; Ezquerra, T.A.; Labrador, A.; Fraga, E.; Beltran, D.; Juanhuix, J.; Herranz, J.F.; Bordas, J.

    2006-03-15

    Here we present a novel, simple, and versatile experimental setup aimed to perform wide angle x-ray scattering (WAXS) measurements alone or in simultaneous combination with small angle x-ray scattering measurements. The design of the WAXS goniometer allows one to obtain high resolution diffraction patterns in a broad angular range. The setup can incorporate a hot stage in order to evaluate temperature resolved experiments. The performance of the equipment has been verified in the BM16 beam line of the European Synchrotron Radiation Facility with different well known samples such as alumina, isotropic film of high density polyethylene (HDPE), and oriented HPDE fiber.

  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. Chemical Composition and Heterogeneity of Wild 2 Cometary Particles Determined by Synchrotron X-ray Fluorescence

    SciTech Connect

    Lanzirotti,A.; Sutton, S.; Flynn, G.; Newville, M.; Rao, W.

    2008-01-01

    Seven cometary dust particle tracks in Stardust aerogel were studied using synchrotron X-ray fluorescence methods at the National Synchrotron Light Source (NY) and Advanced Photon Source (IL). Elemental maps were produced for each of the tracks and elemental abundances for 156 individual fragments within these tracks were determined. Whole-track elemental abundances were inferred by summing the elemental masses for the fragments in each track and scaling by the ratio of total Fe in the map and total Fe in the fragments. In general, whole-track and terminal-particle abundances are dissimilar. The total Fe masses ranged from 4 to 2200 pg, corresponding to impactors in the size range of 2.7 to 22 {mu}m if Fe abundances are equal to the chondritic value. Systematic variations in element abundance with fragment distance from the aerogel entry point were generally subtle but were pronounced in one track (C2115,19). In this track, Zn/Fe was about three orders of magnitude higher at the top, Cr/Fe was two orders of magnitude higher at the bottom, and S was relatively uniform. Compositional convergence data showed that typically analysis of {approx}10 fragments was needed to reach convergent whole-track abundance. Zinc was an exception, showing nonconvergent profiles and steps due to the presence of rare, high-Zn fragments. The resulting wholetrack elemental abundances show diverse patterns that are generally chondritic (i.e., within a factor of three of CI abundances) with some exceptions, notably depletions in S and enrichments in the moderately volatile elements Cu, Zn, and Ga. Enrichments in large ion lithophile elements relative to Fe were observed in one track. Correlation matrices showed several strong elemental correlations, notably selenium associated with sulfur (sulfides), a ubiquitous correlation of the first-row transition metals Cr, Mn, and Fe attributed to the presence of pyroxene, and enrichments of gallium associated with calcium, likely affiliated with Mg

  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. Imaging local electric fields produced upon synchrotron X-ray exposure.

    PubMed

    Dettmar, Christopher M; Newman, Justin A; Toth, Scott J; Becker, Michael; Fischetti, Robert F; Simpson, Garth J

    2015-01-20

    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

  11. Imaging local electric fields produced upon synchrotron X-ray exposure.

    PubMed

    Dettmar, Christopher M; Newman, Justin A; Toth, Scott J; Becker, Michael; Fischetti, Robert F; Simpson, Garth J

    2015-01-20

    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.

  12. 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.

  13. 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.

  14. 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.

  15. Diagnostic copper imaging of Menkes disease by synchrotron radiation-generated X-ray fluorescence analysis.

    PubMed

    Kinebuchi, Miyuki; Matsuura, Akihiro; Kiyono, Tohru; Nomura, Yumiko; Kimura, Sachiko

    2016-01-01

    Copper (Cu) is an indispensable metal for normal development and function of humans, especially in central nervous system (CNS). However, its redox activity requires accurate Cu transport system. ATP7A, a main Cu(2+) transporting-ATPase, is necessary to efflux Cu across the plasma membrane and synthesize cuproenzymes. Menkes disease (MD) is caused by mutations in ATP7A gene. Clinically, MD is Cu deficiency syndrome and is treated with Cu-histidine injections soon after definite diagnosis. But outcome of the most remains poor. To estimate the standard therapy, Cu distribution in the treated classic MD patients is analyzed by synchrotron-generated X-ray fluorescence technique (SR-XRF), which identifies and quantifies an individual atom up to at subcellular level of resolution with wide detection area. SR-XRF analysis newly reveals that Cu exists in spinal cord parenchyma and flows out via venous and lymph systems. By systemic analysis, excess Cu is detected in the proximal tubular cells of the kidney, the mucosal epithelial cells of the intestine, and the lymph and venous systems. The current study suggests that the standard therapy supply almost enough Cu for patient tissues. But given Cu passes through the tissues to venous and lymph systems, or accumulate in the cells responsible for Cu absorption. PMID:27629586

  16. 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

  17. 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.

  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. 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

  20. Imaging the Transport of Silver Nanoparticles Through Soil With Synchrotron X-ray Microtomography

    NASA Astrophysics Data System (ADS)

    Molnar, I. L.; Gerhard, J.; O'Carroll, D. M.; Willson, C. S.

    2012-12-01

    Synchrotron x-ray computed microtomography (SXCMT) offers the ability to examine the spatial distribution of contaminants within the pore space of a porous medium; examples include the distribution of nonaqueous phase liquids (NAPLs) and micro-sized colloids. Recently presented was a method, based upon the application of the Beer-Lambert law and K-edge imaging, for using SXCMT to accurately determine the distribution of silver nanoparticles in a porous medium (Molnar et al., AGU Fall Meeting, H53B-1418, 2011). By capturing a series of SXCMT images of a single sample evolving over time, this technique can study the changing distribution of nanoparticles throughout the pore-network and even within individual pores. While previous work on this method focused on accuracy, precision and its potential applications, this study will provide an in-depth analysis of the results of multiple silver nanoparticle transport experiments imaged using this new technique. SXCMT images were collected at various stages of silver nanoparticle injection into columns packed with well graded and poorly graded quartz sand, iron oxide sand and glass bead porous media. The collected images were used to explore the influences of grain type, size and shape on the transport of silver nanoparticles through soil. The results of this analysis illustrate how SXCMT can collect hitherto unobtainable data which can yield valuable insights into the factors affecting nanoparticle transport through soil.

  1. Crystal structure of nitarsone determined from synchrotron X-ray powder diffraction data

    NASA Astrophysics Data System (ADS)

    van der Lee, A.; Richez, P.; Tapiero, C.

    2005-05-01

    The crystal structure of nitarsone, 4-nitrophenylarsonic acid, a substitute for nifursol and dimetridazole in the prevention and treatment of turkey histomoniasis desease, has been determined from synchrotron X-ray powder diffraction data. Nitarsone crystallizes in the monoclinic space group P2 1/ n with unit cell parameters a=7.46413(5), b=25.68543(17), c=4.657388(32) Å, β=105.4670(5)°. The structure was solved using simulated annealing techniques by treating the molecule as a rigid body for which the configuration resulting from an energy minimization was used in slightly adapted form. Structure refinement treated the NO 2 and the AsO(OH) 2 groups as free groups, leading to final confidence factors Rp=0.059 and Rwp=0.071. The crystal structure contains 4 molecules per unit cell that are hydrogen bonded to form infinite chains of dimers running along the c-axis. Nitarsone's low toxicity when compared with inorganic sources of arsenic is explained by the existence of a partial double C-As bond (1.866(5) Å) which confers greater stability so that under physiological conditions nitarsone is not converted to mineral-like As V or III.

  2. 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.

  3. 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

  4. In Situ Synchrotron X-ray Study of Ultrasound Cavitation and Its Effect on Solidification Microstructures

    NASA Astrophysics Data System (ADS)

    Mi, Jiawei; Tan, Dongyue; Lee, Tung Lik

    2015-08-01

    Considerable progress has been made in studying the mechanism and effectiveness of using ultrasound waves to manipulate the solidification microstructures of metallic alloys. However, uncertainties remain in both the underlying physics of how microstructures evolve under ultrasonic waves, and the best technological approach to control the final microstructures and properties. We used the ultrafast synchrotron X-ray phase contrast imaging facility housed at the Advanced Photon Source, Argonne National Laboratory, US to study in situ the highly transient and dynamic interactions between the liquid metal and ultrasonic waves/bubbles. The dynamics of ultrasonic bubbles in liquid metal and their interactions with the solidifying phases in a transparent alloy were captured in situ. The experiments were complemented by the simulations of the acoustic pressure field, the pulsing of the bubbles, and the associated forces acting onto the solidifying dendrites. The study provides more quantitative understanding on how ultrasonic waves/bubbles influence the growth of dendritic grains and promote the grain multiplication effect for grain refinement.

  5. Diagnostic copper imaging of Menkes disease by synchrotron radiation-generated X-ray fluorescence analysis

    PubMed Central

    Kinebuchi, Miyuki; Matsuura, Akihiro; Kiyono, Tohru; Nomura, Yumiko; Kimura, Sachiko

    2016-01-01

    Copper (Cu) is an indispensable metal for normal development and function of humans, especially in central nervous system (CNS). However, its redox activity requires accurate Cu transport system. ATP7A, a main Cu2+ transporting-ATPase, is necessary to efflux Cu across the plasma membrane and synthesize cuproenzymes. Menkes disease (MD) is caused by mutations in ATP7A gene. Clinically, MD is Cu deficiency syndrome and is treated with Cu-histidine injections soon after definite diagnosis. But outcome of the most remains poor. To estimate the standard therapy, Cu distribution in the treated classic MD patients is analyzed by synchrotron-generated X-ray fluorescence technique (SR-XRF), which identifies and quantifies an individual atom up to at subcellular level of resolution with wide detection area. SR-XRF analysis newly reveals that Cu exists in spinal cord parenchyma and flows out via venous and lymph systems. By systemic analysis, excess Cu is detected in the proximal tubular cells of the kidney, the mucosal epithelial cells of the intestine, and the lymph and venous systems. The current study suggests that the standard therapy supply almost enough Cu for patient tissues. But given Cu passes through the tissues to venous and lymph systems, or accumulate in the cells responsible for Cu absorption. PMID:27629586

  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. 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.

  10. 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.

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

    PubMed Central

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

    2013-01-01

    The molecular-scale structure of the ionic liquid [C18mim]+[FAP]− near its free surface was studied by complementary methods. X-ray absorption spectroscopy and resonant soft X-ray reflectivity revealed a depth-decaying near-surface layering. Element-specific interfacial profiles were extracted with submolecular resolution from energy-dependent soft X-ray reflectivity data. Temperature-dependent hard X-ray reflectivity, small- and wide-angle X-ray scattering, and infrared spectroscopy uncovered an intriguing melting mechanism for the layered region, where alkyl chain melting drove a negative thermal expansion of the surface layer spacing. PMID:23431181

  12. 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.

  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. 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

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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

  20. 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

  1. 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.

  2. 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

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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).

  10. Feasibility study of high-resolution coherent diffraction microscopy using synchrotron x rays focused by Kirkpatrick-Baez mirrors

    SciTech Connect

    Takahashi, Yukio; Nishino, Yoshinori; Ishikawa, Tetsuya; Mimura, Hidekazu; Tsutsumi, Ryosuke; Kubo, Hideto; Yamauchi, Kazuto

    2009-04-15

    High-flux coherent x rays are necessary for the improvement of the spatial resolution in coherent x-ray diffraction microscopy (CXDM). In this study, high-resolution CXDM using Kirkpatrick-Baez (KB) mirrors is proposed, and the mirrors are designed for experiments of the transmission scheme at SPring-8. Both the photon density and spatial coherence of synchrotron x rays focused by the KB mirrors are investigated by wave optical simulation. The KB mirrors can produce nearly diffraction-limited two-dimensional focusing x rays of approx1 mum in size at 8 keV. When the sample size is less than approx1 mum, the sample can be illuminated with full coherent x rays by adjusting the cross-slit size set between the source and the mirrors. From the estimated photon density at the sample position, the feasibility of CXDM with a sub-1-nm spatial resolution is suggested. The present ultraprecise figuring process enables us to fabricate mirrors for carrying out high-resolution CXDM experiments.

  11. 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.

  12. Synchrotron X-ray Diffraction Study of Microtubules Buckling and Bundling under Osmotic Stress: A Probe of Interprotofilament Interactions

    NASA Astrophysics Data System (ADS)

    Needleman, Daniel J.; Ojeda-Lopez, Miguel A.; Raviv, Uri; Ewert, Kai; Jones, Jayna B.; Miller, Herbert P.; Wilson, Leslie; Safinya, Cyrus R.

    2004-11-01

    Microtubules are hollow cylinders composed of tubulin heterodimers that stack into linear protofilaments that interact laterally to form the microtubule wall. Synchrotron x-ray diffraction of microtubules under increasing osmotic stress shows they transition to rectangular bundles with noncircular buckled cross sections, followed by hexagonally packed bundles. This new technique probes the strength of interprotofilamen bonds, yielding insight into the mechanism by which associated proteins and the chemotherapy drug taxol stabilize microtubules.

  13. 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.

  14. 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.

  15. 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.

  16. 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

  17. 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.

  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. CCD(charge-coupled device)-based synchrotron x-ray detector for protein crystallography: Performance projected from an experiment

    SciTech Connect

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

    1986-01-01

    The intense x radiation from a synchrotron source could, with a suitable detector, provide a complete set of diffraction images from a protein crystal before the crystal is damaged by radiation (2 to 3 min). An area detector consisting of a 40 mm dia. x-ray fluorescing phosphor, coupled with an image intensifier and lens to a CCD image sensor, was developed to determine the effectiveness of such a detector in protein crystallography. The detector was used in an experiment with a rotating anode x-ray generator. Diffraction patterns from a lysozyme crystal obtained with this detector are compared to those obtained with film. The two images appear to be virtually identical. The flux of 10/sup 4/ x-ray photons/s was observed on the detector at the rotating anode generator. At the 6-GeV synchrotron being designed at Argonne, the flux on an 80 x 80 mm/sup 2/ detector is expected to be >10/sup 9/ photons/s. The projected design of such a synchrotron detector shows that a diffraction-peak count >10/sup 6/ could be obtained in approx.0.5 s. With an additional approx.0.5 s readout time of a 512 x 512 pixel CCD, the data acquisition time per frame would be approx.1 s so that ninety 1/sup 0/ diffraction images could be obtained, with approximately 1% precision, in less than 3 min.

  20. 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.

  1. 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.

  2. Bone Implant Interface Investigation by Synchrotron Radiation X-Ray Microfluorescence

    NASA Astrophysics Data System (ADS)

    Calasans-Maia, M.; Sales, E.; Granjeiro, J. M.; Lopes, R. T.; Lima, I.

    2010-04-01

    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 (2×6 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 (˜200 μm 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.

  3. 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.

  4. 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.

  5. 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

  6. 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

  7. 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.

  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. Superhydrophobic surfaces allow probing of exosome self organization using X-ray scattering.

    PubMed

    Accardo, Angelo; Tirinato, Luca; Altamura, Davide; Sibillano, Teresa; Giannini, Cinzia; Riekel, Christian; Di Fabrizio, Enzo

    2013-03-21

    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.

  10. 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.

  11. 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

  12. Synchrotron x-ray-scattering study of the normal-incommensurate phase transition in Rb2ZnCl4

    NASA Astrophysics Data System (ADS)

    Zinkin, M. P.; McMorrow, D. F.; Hill, J. P.; Cowley, R. A.; Lussier, J.-G.; Gibaud, A.; Grübel, G.; Sutter, C.

    1996-08-01

    The results of high-resolution synchrotron x-ray-scattering experiments on the normal-incommensurate phase transition in Rb2ZnCl4 are reported. Measured critical exponents for the intensities of the first three harmonics of the incommensurate modulation wave below Tc agree well with theoretical predictions for the n=2, D=3 (3D-XY) universality class. The scattering observed above Tc corrresponds to critical fluctuations on two distinct length scales: the critical exponents for the short length scale component of the scattering agree with those expected for the 3D-XY universality class. The value found for the exponent of the inverse correlation length of the long length scale component is νs=0.7+/-0.2. A comparison of data taken in Laue and Bragg geometries at different photon energies suggests that the second length scale scattering originates in the near-surface region. Possible explanations of the two length scale behavior are discussed.

  13. μX-ray fluorescence analysis of traces and calcium phosphate phases on tooth tartar interfaces using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Abraham, J. A.; Grenón, M. S.; Sánchez, H. J.; Valentinuzzi, M. C.; Perez, C. A.

    2007-07-01

    Hard dental tissues like dentine and cementum with calcified deposits (dental calculi) were studied in several human dental pieces of adult individuals from the same geographic region. A couple of cross cuts were performed at dental root level resulting in a planar slice with calculus and dental tissue exposed for analysis. The elemental content along a linear path crossing the dentine-cementum-tartar interfaces and also all over a surface was measured by X-ray fluorescence microanalysis using synchrotron radiation (μSRXRF). The concentration of elemental traces like K, V, Cu, Zn, As, Br and Sr showed different features on the analyzed regions. The possible connections with the dynamic of mineralization and biological implications are discussed. The concentrations of major elements Ca and P were also determined and the measured Ca/P molar ratio was used to estimate the average composition of calcium phosphate phases in the measured points. A deeper knowledge of the variations of the elemental compositions and the changes of the different phases will help to a better understanding of the scarcely known mechanism of calculus growing.

  14. 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

  15. Understanding how active volcanoes work: a contribution from synchrotron X-ray computed microtomography

    NASA Astrophysics Data System (ADS)

    Polacci, M.; Baker, D. R.; Mancini, L.

    2009-04-01

    Volcanoes are complex systems that require the integration of many different geoscience disciplines to understand their behaviour and to monitor and forecast their activity. In the last two decades an increasing amount of information on volcanic processes has been obtained by studying the textures and compositions of volcanic rocks. Five years ago we started a continuing collaboration with the SYRMEP beamline of Elettra Sincrotrone, a third generation synchrotron light source near Trieste, Italy, with the goal of performing high-resolution, phase-contrast X-ray tomographic scans and reconstructing 3-D digital volumes of volcanic specimens. These volumes have been then used for the visualization of the internal structure of rocks and for the quantification of rock textures (i.e., vesicle and crystal volume fraction, individual vesicle volumes and shapes, vesicle connectivity, vesicle volume distributions, permeability simulations etc.). We performed tomographic experiments on volcanic products erupted from different hazardous volcanic systems in Italy and around the world: Campi Flegrei, Stromboli, Etna (Southern Italy), Villarrica (Chile), Yasur and Ambrym (Vanuatu Islands). As an example, we used the results of these studies to constrain the dynamics of vesiculation and degassing in basaltic (Polacci et al., 2006; Burton et al., 2007; Colò et al., 2007; Andronico et al., 2008; Polacci et al., 2008a) and trachytic (Piochi et al., 2008) magmas. A better knowledge of how gas is transported and lost from magmas has led us in turn to draw new implications on the eruptive style of these active, hazardous volcanoes (Polacci et al., 2008b). Work in progress consists of optimizing our procedure by establishing a precise protocol that will enable us to quantitatively study the 3-D texture and composition of rocks in a statistically representative way. Future work will concentrate on the study of the spatial relations between phases (crystals, vesicles and glass) in rocks

  16. 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

  17. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2009-11-01

    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.

  19. 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

  20. 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

  1. X-RAY STRIPES IN TYCHO'S SUPERNOVA REMNANT: SYNCHROTRON FOOTPRINTS OF A NONLINEAR COSMIC-RAY-DRIVEN INSTABILITY

    SciTech Connect

    Bykov, Andrei M.; Osipov, Sergei M.; Uvarov, Yury A.; Ellison, Donald C.; Pavlov, George G. E-mail: osm@astro.ioffe.ru E-mail: don_ellison@ncsu.edu

    2011-07-10

    High-resolution Chandra observations of Tycho's supernova remnant (SNR) have revealed several sets of quasi-steady, high-emissivity, nearly parallel X-ray stripes in some localized regions of the SNR. These stripes are most likely the result of cosmic-ray (CR) generated magnetic turbulence at the SNR blast wave. However, for the amazingly regular pattern of these stripes to appear, simultaneous action of a number of shock-plasma phenomena is required, which is not predicted by most models of magnetic field amplification. A consistent explanation of these stripes yields information on the complex nonlinear plasma processes connecting efficient CR acceleration and magnetic field fluctuations in strong collisionless shocks. The nonlinear diffusive shock acceleration (NL-DSA) model described here, which includes magnetic field amplification from a CR-current-driven instability, does predict stripes consistent with the synchrotron observations of Tycho's SNR. We argue that the local ambient mean magnetic field geometry determines the orientation of the stripes and therefore it can be reconstructed with the high-resolution X-ray imaging. The estimated maximum energy of the CR protons responsible for the stripes is {approx}10{sup 15} eV. Furthermore, the model predicts that a specific X-ray polarization pattern, with a polarized fraction {approx}50%, accompanies the stripes, which can be tested with future X-ray polarimeter missions.

  2. Characterization of porosity in a 19th century painting ground by synchrotron radiation X-ray tomography

    NASA Astrophysics Data System (ADS)

    Gervais, Claire; Boon, Jaap J.; Marone, Federica; Ferreira, Ester S. B.

    2013-04-01

    The study of the early oeuvre of the Swiss painter Cuno Amiet (1868-1961) has revealed that, up to 1907, many of his grounds were hand applied and are mainly composed of chalk, bound in protein. These grounds are not only lean and absorbent, but also, as Synchrotron radiation X-ray microtomography has shown, porous. Our approach to the characterization of pore structure and quantity, their connectivity, and homogeneity is based on image segmentation and application of a clustering algorithm to high-resolution X-ray tomographic data. The issues associated with the segmentation of the different components of a ground sample based on X-ray imaging data are discussed. The approach applied to a sample taken from "Portrait of Max Leu" (1899) by Amiet revealed the presence of three sublayers within the ground with distinct porosity features, which had not been observed optically in cross-section. The upper and lower layers are highly porous with important connectivity and thus prone to water uptake/storage. The middle layer however shows low and nonconnected porosity at the resolution level of the X-ray tomography images, so that few direct water absorption paths through the entire sample exist. The potential of the method to characterize porosity and to understand moisture-related issues in paint layer degradation are discussed.

  3. A seven-crystal Johann-type hard x-ray spectrometer at the Stanford Synchrotron Radiation Lightsource

    SciTech Connect

    Sokaras, D.; Weng, T.-C.; Nordlund, D.; Velikov, P.; Wenger, D.; Garachtchenko, A.; George, M.; Borzenets, V.; Johnson, B.; Rabedeau, T.; Alonso-Mori, R.; Bergmann, U.

    2013-05-15

    We present a multicrystal Johann-type hard x-ray spectrometer ({approx}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 Degree-Sign -74 Degree-Sign ) 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 4{pi} sr. The typical resolving power is in the order of (E/{Delta}E){approx}10 000. 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.

  4. 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

  5. Decreased Surface Tension of Water by Hard-X-Ray Irradiation

    SciTech Connect

    Weon, B. M.; Je, J. H.; Hwu, Y.; Margaritondo, G.

    2008-05-30

    We discovered that intense irradiation by hard-x-ray strongly decreases the effects of natural surface tension of water in droplets and capillary tubes. The effect was revealed by direct experimental observations with phase contrast microradiology. A model based on ionization and surface charging explains this so far undetected phenomenon. The effect can impact the results of many experimental techniques based on x rays. This is an example of the largely unexplored effects that can be produced by extreme intense x-ray irradiation--an important issue due to current development of x-ray free-electron-lasers with unprecedented brilliance.

  6. 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

  7. 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)

  8. 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.

  9. Pb distribution in bones from the Franklin expedition: synchrotron X-ray fluorescence and laser ablation/mass spectroscopy

    NASA Astrophysics Data System (ADS)

    Martin, Ronald Richard; Naftel, Steven; Macfie, Sheila; Jones, Keith; Nelson, Andrew

    2013-04-01

    Synchrotron micro-X-ray Fluorescence has been used to map the metal distribution in selected bone fragments representative of remains associated with the Franklin expedition. In addition, laser ablation mass spectroscopy using a 25 μm diameter circular spot was employed to compare the Pb isotope distributions in small regions within the bone fragments. The X-ray Fluorescence mapping shows Pb to be widely distributed in the bone while the Pb isotope ratios obtained by laser ablation within small areas representative of bone with different Pb exchange rates do not show statistically significant differences. These results are inconsistent with the hypothesis that faulty solder seals in tinned meat were the principle source of Pb in the remains of the expedition personnel.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. Synchrotron X-ray fluorescence microscopy of gallium in bladder tissue following gallium maltolate administration during urinary tract infection.

    PubMed

    Ball, Katherine R; Sampieri, Francesca; Chirino, Manuel; Hamilton, Don L; Blyth, Robert I R; Sham, Tsun-Kong; Dowling, Patricia M; Thompson, Julie

    2013-11-01

    A mouse model of cystitis caused by uropathogenic Escherichia coli was used to study the distribution of gallium in bladder tissue following oral administration of gallium maltolate during urinary tract infection. The median concentration of gallium in homogenized bladder tissue from infected mice was 1.93 μg/g after daily administration of gallium maltolate for 5 days. Synchrotron X-ray fluorescence imaging and X-ray absorption spectroscopy of bladder sections confirmed that gallium arrived at the transitional epithelium, a potential site of uropathogenic E. coli infection. Gallium and iron were similarly but not identically distributed in the tissues, suggesting that at least some distribution mechanisms are not common between the two elements. The results of this study indicate that gallium maltolate may be a suitable candidate for further development as a novel antimicrobial therapy for urinary tract infections caused by uropathogenic E. coli.

  15. Synchrotron X-Ray Fluorescence Microscopy of Gallium in Bladder Tissue following Gallium Maltolate Administration during Urinary Tract Infection

    PubMed Central

    Sampieri, Francesca; Chirino, Manuel; Hamilton, Don L.; Blyth, Robert I. R.; Sham, Tsun-Kong; Dowling, Patricia M.; Thompson, Julie

    2013-01-01

    A mouse model of cystitis caused by uropathogenic Escherichia coli was used to study the distribution of gallium in bladder tissue following oral administration of gallium maltolate during urinary tract infection. The median concentration of gallium in homogenized bladder tissue from infected mice was 1.93 μg/g after daily administration of gallium maltolate for 5 days. Synchrotron X-ray fluorescence imaging and X-ray absorption spectroscopy of bladder sections confirmed that gallium arrived at the transitional epithelium, a potential site of uropathogenic E. coli infection. Gallium and iron were similarly but not identically distributed in the tissues, suggesting that at least some distribution mechanisms are not common between the two elements. The results of this study indicate that gallium maltolate may be a suitable candidate for further development as a novel antimicrobial therapy for urinary tract infections caused by uropathogenic E. coli. PMID:23877680

  16. 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.

  17. 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.

  18. Nanophase evolution at semiconductor/electrolyte interface in situ probed by time-resolved high-energy synchrotron X-ray diffraction.

    PubMed

    Sun, Yugang; Ren, Yang; Haeffner, Dean R; Almer, Jonathan D; Wang, Lin; Yang, Wenge; Truong, Tu 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(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(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(7)NO(11)) and silver arsenate (Ag(3)AsO(4)) at the semiconductor/electrolyte interface if the GaAs wafer is illuminated by the X-ray and reaction time is long enough.

  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. Phase-contrast imaging with synchrotron hard X-ray of micro lesions of the cartilage of the femoral head in rabbits

    PubMed Central

    Sun, Wei; Zhang, Yong; Gao, Fuqiang; Li, Zirong; Li, Gang; Pan, Lin

    2015-01-01

    Background: To observe micro lesions on the cartilage of the rabbit femoral head using phase-contrast imaging with synchrotron hard X-ray and to prove that this method can be useful in the study of the degeneration of cartilage. Methods: New Zealand white rabbits were used in a micro lesion model of rabbit femoral head cartilage. Bilateral femoral heads were excised from rabbits, and micro lesions were made on one side with a specially made knife with a blade 20 μm in width. The other femur was left intact to serve as the control. Phase-contrast imaging with synchrotron hard X-ray and conventional X-ray imaging were used to observe the cartilage. Histological changes were investigated using modified Golden tri-color staining. Results: Phase-contrast imaging with synchrotron hard X-ray clearly showed the 20 μm lesions on the cartilage on the heads of rabbit femurs. These lesions were not visible with conventional X-ray imaging. Histological observation confirmed the presence of the microscopic lesions. Conclusion: Phase-contrast imaging with synchrotron hard X-ray can detect microscopic lesions on cartilage that cannot be detected by conventional absorption-contrast X-ray. This provides an unequivocal, non-invasive alternative to histological examination in the diagnosis of joint disease. It should be considered a new tool in osteoarthritis and cartilage research. PMID:26884921

  1. 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.

  2. Residual stress profiling in the ferrite and cementite phases of cold-drawn steel rods by synchrotron X-ray and neutron diffraction

    SciTech Connect

    Martinez-Perez, M.L.; Mompean, F.J.; Ruiz-Hervias, J.; Atienza, J.M.; Elices, M.; Peng Rulin; Buslaps, T.

    2004-10-18

    Residual stress profiles have been measured in the ferrite and cementite phases of a cold-drawn eutectoid steel rod by neutron and synchrotron X-ray diffraction in three orientations (axial, radial and hoop). Neutron diffraction was employed to measure the ferrite stresses, whereas synchrotron radiation was used for ferrite and cementite stresses. Experimental results in the ferrite phase showed excellent agreement between both experimental techniques when gauge volume effects were accounted for. Axial cementite stresses were always tensile, with a maximum value close to 1700 MPa at the rod surface. Radial and hoop cementite stresses were compressive along the diameter of the rod, with a minimum of -1900 MPa at the rod center. A 3D-finite element simulation of the macro residual stresses resulting from cold-drawing showed remarkable agreement with those determined from the experimental measurements in the ferrite and cementite phases.

  3. 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.

  4. Preliminary investigation of trace element in Pterygium using Synchrotron radiation micro-beam X-ray fluorescence analysis (-XRF)

    NASA Astrophysics Data System (ADS)

    Xie, Q.; Peng, L.; Cai, F.; Li, Ai G.; Yang, K.

    2013-07-01

    We have assessed the relative content and distribution of Iron and Zinc elements using microbeam synchrotron radiation X-ray fluorescence technique. One such technique is X-ray fluorescence (XRF), which has been used previously to map trace elements distribution in Physical samples. In this article a compromise is suggested in issue Pterygium samples. In this study, a prospective randomized clinical trial was conducted. Serial frozen sections of pterygium tissues and conjunctival tissues of 40 μm thickness were collected from 8 patients £¨10 eyes£©undergoing pterygium excision combine with limbal stem cell transplantation. A synchrotron-based XRF microprobe was used to map the distribution of Fe and Zn in whole frozen pterygium sections. The frozen sections were tested by synchrotron radiation X-ray fluorescence technique. These experiments were performed at BL15U in Shanghai, China. Then, the results have palyed that Iron and Zinc were present in both pterygium tissues and normal conjunctiva tissues (relevance ratio 100%). The contents of Iron and Zinc in normal conjunctiva tissues were significantly lower than in pterygium tissues (P < 0.05). The microelements were mostly clusteredin the pterygium tissues, while sparsely distributed in the normal conjunctiva tissue. Finally, we found that XRF imaging will be useful for mapping elemental distribution in Pterygium tissues. 40 μm frozen section on 6 μm mylar film is good for the test on BL15U. The contents of Iron and Zinc in pterygium tissue were significantly higher than in the control tissues. The results seem to be valuable in that Iron and Zinc may play a role in the development process of Pterygium.

  5. 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.

  6. 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.

  7. The study of oxygen molecules on Pt (111) surface with high resolution x-ray photoemission spectroscopy

    NASA Astrophysics Data System (ADS)

    Kim, Yong Su; Bostwick, Aaron; Rotenberg, Eli; Ross, Philip N.; Hong, Soon Cheol; Mun, Bongjin Simon

    2010-07-01

    By using high resolution x-ray photoelectron spectroscopy, we show that inelastic scattering of photoelectron at low temperature (30-50 K) generates two kinds of oxygen species on Pt (111) surface. Intense synchrotron radiation source dissociates oxygen molecules into chemisorbed atomic oxygen and induces the formation of PtO on the surface. Estimated coverage of dissociated atomic oxygen is 0.5 ML, suggesting possible formation of p(2×1) surface structure, while PtO coverage shows saturation coverage of 0.5 ML. Molecular oxygen dosed at 30 K undergoes thermally activated transition from physisorbed to chemisorbed state at around 40 K.

  8. The study of oxygen molecules on Pt (111) surface with high resolution x-ray photoemission spectroscopy.

    PubMed

    Kim, Yong Su; Bostwick, Aaron; Rotenberg, Eli; Ross, Philip N; Hong, Soon Cheol; Mun, Bongjin Simon

    2010-07-21

    By using high resolution x-ray photoelectron spectroscopy, we show that inelastic scattering of photoelectron at low temperature (30-50 K) generates two kinds of oxygen species on Pt (111) surface. Intense synchrotron radiation source dissociates oxygen molecules into chemisorbed atomic oxygen and induces the formation of PtO on the surface. Estimated coverage of dissociated atomic oxygen is 0.5 ML, suggesting possible formation of p(2 x 1) surface structure, while PtO coverage shows saturation coverage of 0.5 ML. Molecular oxygen dosed at 30 K undergoes thermally activated transition from physisorbed to chemisorbed state at around 40 K. PMID:20649331

  9. 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.

  10. Synchrotron x-ray powder diffraction studies in pulsed magnetic fields

    SciTech Connect

    Frings, P.; Vanacken, J.; Detlefs, C.; Duc, F.; Lorenzo, J. E.; Nardone, M.; Billette, J.; Zitouni, A.; Bras, W.; Rikken, G. L. J. A.

    2006-06-15

    X-ray powder diffraction experiments under pulsed magnetic fields were carried out at the DUBBLE beamline (BM26B) at the ESRF. A mobile generator delivered 110 kJ to the magnet coil, which was sufficient to generate peak fields of 30 T. A liquid He flow cryostat allowed us to vary the sample temperature accurately between 8 and 300 K. Powder diffraction patterns of several samples were recorded using 21 keV monochromatic x-rays and an on-line image plate detector. Here we present the first results on the suppression of the Jahn-Teller structural distortion in TbVO{sub 4} by magnetic field. These data clearly demonstrate the feasibility of x-ray powder diffraction experiments under pulsed magnetic fields with relatively inexpensive instrumentation.

  11. 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.

  12. 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

  13. 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

  14. Texture, residual strain, and plastic deformation around scratches in alloy 600 using synchrotron x-ray Laue micro-diffraction.

    SciTech Connect

    Suominen Fuller, M. L.; Klassen, R. J.; McIntyre, N. S.; Gerson, A. R.; Ramamurthy, S.; King, P. J.; Liu, W.; Univ. of Western Ontario; Univ. of South Australia; Babcock & Wilcox Canada

    2008-01-01

    Deformation around two scratches in Alloy 600 (A600) was studied nondestructively using synchrotron Laue differential aperture X-ray microscopy. The orientation of grains and elastic strain distribution around the scratches were measured. A complex residual deviatoric elastic strain state was found to exist around the scratches. Heavy plastic deformation was observed up to a distance of 20 {micro}m from the scratches. In the region 20-30 {micro}m from the scratches the diffraction spots were heavily streaked and split indicating misoriented dislocation cell structures.

  15. Synchrotron microscopic X-ray fluorescence analysis of the effects of chronic arsenic exposure in rat brain

    NASA Astrophysics Data System (ADS)

    Rubio, Marcelo; Perez, Roberto D.; Perez, Carlos A.; Eynard, Aldo H.; Bongiovanni, Guillermina A.

    2008-01-01

    Synchrotron microscopic X-ray fluorescence (μ-SRXRF) scanning and conventional XRF analysis were applied for studying elemental concentrations in lyophilised brain rat slices. The animals received drinking water—100 ppm of sodium arsenite—ad libitum for 30 and 60 days. Accumulation of arsenic was corroborated and its dependence with arsenic dosage suggests the existence of a protection mechanism which limits the transport of inorganic arsenic to the brain. Chlorine, potassium and iron were reduced changing their spatial distributions while copper and zinc were redistributed.

  16. Internal Electric Field Investigations of a Cadmium Zinc Telluride Detector Using Synchrotron X-ray Mapping and Pockels Effect Measurements

    SciTech Connect

    Yang, G.; Bolotnikov, A; Camarda, G; Cui, Y; Hossain, A; Yao, H; James, R

    2009-01-01

    Cadmium zinc telluride (CZT) has remained a major focus of research due to its promising application as a room-temperature nuclear radiation detector material. Among the several parameters that substantially affect the detectors' performance, an important one is the distribution of the internal electric field. Brookhaven National Laboratory (BNL) employed synchrotron x-ray microscale mapping and measurements of the Pockels effect to investigate the distribution of the internal electric field in a CZT strip detector. Direct evidence that dislocations can distort the internal electric field of the detector was obtained. Furthermore, it was found that 'star' defects in the CZT crystal, possibly ascribed to dislocation loop punching, cause charge trapping.

  17. Microtubule-associated-protein (MAP) Tau Regulates the Number of Protofilaments in Microtubules: A Synchrotron X-ray Scattering Study

    NASA Astrophysics Data System (ADS)

    Choi, Myung Chul; Raviv, Uri; Miller, Herbert; Gaylord, Michelle; Kiris, Erkan; Ventimiglia, Donovan; Needleman, Daniel; Kim, Mahn Won; Wilson, Leslie; Feinstein, Stuart; Safinya, Cyrus

    2009-03-01

    Microtubules (MTs), 25 nm protein nanotubes, are a major filamentous element of the cytoskeleton involved in intracellular trafficking and cell division. MAP tau regulates tubulin assembly and MT stability. Dysfunction of tau has been correlated with numerous neurodegenerative diseases. We describe our recent findings about the effects of six naturally occurring central nervous system (CNS) tau isoforms on the assembly structure of taxol-stabilized MTs, using synchrotron small angle x-ray scattering (SAXS). Most significantly, we found that tau, at low binding density, regulates the distribution of protofilament numbers in MTs. DOE DE-FG02-06ER46314, NSF DMR-0803103, NIHI RO1-NS35010 and NS13560.

  18. 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.

  19. 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.

  20. Design of a humidity controlled sample stage for simultaneous conductivity and synchrotron X-ray scattering measurements.

    PubMed

    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.

  1. A new method to suppress high-order harmonics for a synchrotron radiation soft X-ray beamline

    NASA Astrophysics Data System (ADS)

    Guo, Zhi-Ying; Xing, Hai-Ying; Hong, Cai-Hao; Tang, Kun; Han, Yong; Chen, Dong-Liang; Zhao, Yi-Dong

    2015-04-01

    A feasible and convenient method is proposed to suppress higher-harmonics for a varied-line-spacing plane grating monochromator in the soft X-ray region. Related calculations and experiments demonstrate that decreasing the included angle slightly by changing the parameter of the exit arm length can significantly improve light purity. This method is suitable and has been used for experiments of detector calibration in beamline 4B7B at the Beijing Synchrotron Radiation Facility (BSRF). Supported by National Natural Science Foundation of China (11375227, 61204008)

  2. 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.

  3. 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

  4. 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

  5. Synchrotron X-ray Powder Diffraction Studies in Pulsed Magnetic Fields

    SciTech Connect

    Detlefs, C.; Frings, P.; Duc, F.; Nardone, M.; Billette, J.; Zitouni, A.; Rikken, G. L. J. A.; Vanacken, J.; Lorenzo, J. E.; Bras, W.

    2007-01-19

    X-ray powder diffraction experiments under pulsed magnetic fields were carried out at the DUBBLE beamline (BM26B) at the ESRF. A mobile generator delivered 110kJ to the magnet coil, which was sufficient to generate peak fields of 30T. A liquid He flow cryostat allowed us to vary the sample temperature accurately between 8K and 300K.

  6. 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.

  7. 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.

  8. 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

  9. [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

  10. 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.

  11. [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

  12. 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.

  13. Methodological challenges of optical tweezers-based X-ray fluorescence imaging of biological model organisms at synchrotron facilities.

    PubMed

    Vergucht, Eva; Brans, Toon; Beunis, Filip; Garrevoet, Jan; Bauters, Stephen; De Rijcke, Maarten; Deruytter, David; Janssen, Colin; Riekel, Christian; Burghammer, Manfred; Vincze, Laszlo

    2015-07-01

    Recently, a radically new synchrotron radiation-based elemental imaging approach for the analysis of biological model organisms and single cells in their natural in vivo state was introduced. The methodology combines optical tweezers (OT) technology for non-contact laser-based sample manipulation with synchrotron radiation confocal X-ray fluorescence (XRF) microimaging for the first time at ESRF-ID13. The optical manipulation possibilities and limitations of biological model organisms, the OT setup developments for XRF imaging and the confocal XRF-related challenges are reported. In general, the applicability of the OT-based setup is extended with the aim of introducing the OT XRF methodology in all research fields where highly sensitive in vivo multi-elemental analysis is of relevance at the (sub)micrometre spatial resolution level.

  14. 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.

  15. Synchrotron-induced X-ray fluorescence from rat bone and lumber vertebra of different age groups

    NASA Astrophysics Data System (ADS)

    Rao, Donepudi V.; Swapna, Medasani; Cesareo, Roberto; Brunetti, Antonio; Akatsuka, Tako; Yuasa, Tetsuya; Takeda, Tohoru; Tromba, Giuliana; Gigante, Giovanni E.

    2009-02-01

    The fluorescence spectra from rat bones of different age groups (8, 56 and 78 weeks) and lumber vertebra were measured with 8, 10 and 12 keV synchrotron X-rays. We have utilized the new hard X-ray micro-spectroscopy beamline facility, X27A, available at NSLS with a primary beam spot size of the order of ˜10 μm. With this spatial resolution and high flux throughput, X-ray fluorescent intensities for Ca and other trace elements were measured using a liquid-nitrogen-cooled 13-element energy-dispersive high-purity germanium detector. Regarding the lumber vertebra, we acquired the fluorescence spectra from the left, right and middle portions and calcium accumulation was evaluated and compared with the other samples. We have identified the major trace elements of Ca, Ni, Fe and Zn and minor trace elements of Ti, Cr and Mn in the sample. The percentage of scattered radiation and trace element contributions from these samples were highlighted at different energies.

  16. Advantages of a synchrotron bending magnet as the sample illuminator for a wide-field X-ray microscope.

    PubMed

    Feser, M; Howells, M R; Kirz, J; Rudati, J; Yun, W

    2012-09-01

    In this 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. It is expected 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.

  17. Magnetic field estimates from the synchrotron X-ray shell of 30 Dor C, the first TeV superbubble

    NASA Astrophysics Data System (ADS)

    Kavanagh, P.; Vink, J.; Sasake, M.; Maggi, P.; Haberl, F.; Filipovic, M.

    2016-06-01

    Superbubbles are powered by the stellar winds and subsequent supernovae of a massive stellar population and are often argued as strong candidates for Galactic cosmic-ray acceleration sites. The recent detection of TeV gamma-rays from 30 Dor C in the Large Magellanic Cloud by the High Energy Stereoscopic System (H.E.S.S.) has shown that superbubbles can and do accelerate particles up to very high cosmic-ray energies, and are a new and important source class in TeV astronomy. However, the dominant production mechanism (i.e., hadronic or leptonic) is still unclear. The answer to this question is locked in the unique synchrotron X-ray shell of 30 Dor C. The widths of the synchrotron emission regions are directly related to the magnetic field, which is a crucial parameter assessing dominant gamma-ray emission mechanism. In this talk we will present a study of the synchrotron emission region widths in 30 Dor C using several hundred ks of archival X-ray data from XMM-Newton. We constructed radial emission profiles from various regions of the synchrotron shell, fitted emission models to determine the widths, and derived B-field values in the downstream regions using appropriate models. The resulting low B-field estimates, of the order of a few micro G, favour a leptonic origin for the gamma-ray emission. Hadronic cosmic rays are likely to be accelerated as well, but the low density inside the bubble suppresses their emissivity.

  18. High-resolution spectroscopy of X-rays emitted from electron bombarded surfaces

    NASA Astrophysics Data System (ADS)

    Jabłoński, Ł.; Banaś, D.; Jagodziński, P.; Kubala-Kukuś, A.; Sobota, D.; Pajek, M.

    2015-07-01

    The investigations of a compact 6-crystal Johann/Johansson diffraction X-ray spectrometer, covering a wide range (70 eV-15 keV) of photon energies, applied to observe the X-rays emitted from electron bombarded surfaces are discussed in terms of its focusing properties and achievable energy resolution. In the present study the X-ray spectra of Si-Kα1,2 and Al-Kα1,2 X-ray lines excited by 5 keV electron beam were measured using PET and TAP crystal, respectively, in the "out-of-focus" geometry which will be used to study the electron/ion surface interactions at the electron beam ion source (EBIS) facility. The measured X-ray spectra were interpreted in terms of the performed ray-tracing simulations which demonstrate the key features of the "out-of-focus" geometry. It was demonstrated that in this case the energy resolution in the range 1-3 eV for photon energy 1-2 keV can be achieved with an increased acceptance for the extension of X-ray source, of about 1 mm, which is important feature for practical applications. Additionally, a dependence of the X-ray intensity and energy resolution on slit opening was studied in details. The results are important for investigations of surfaces with electron and ion impact, in particular, for the future high-resolution X-ray spectroscopy experiments at the EBIS facility.

  19. X-ray irradiation of soda-lime glasses studied in situ with surface plasmon resonance spectroscopy

    SciTech Connect

    Serrano, A.; Galvez, F.; Rodriguez de la Fuente, O.; Garcia, M. A.

    2013-03-21

    We present here a study of hard X-ray irradiation of soda-lime glasses performed in situ and in real time. For this purpose, we have used a Au thin film grown on glass and studied the excitation of its surface plasmon resonance (SPR) while irradiating the sample with X-rays, using a recently developed experimental setup at a synchrotron beamline [Serrano et al., Rev. Sci. Instrum. 83, 083101 (2012)]. The extreme sensitivity of the SPR to the features of the glass substrate allows probing the modifications caused by the X-rays. Irradiation induces color centers in the soda-lime glass, modifying its refractive index. Comparison of the experimental results with simulated data shows that both, the real and the imaginary parts of the refractive index of soda-lime glasses, change upon irradiation in time intervals of a few minutes. After X-ray irradiation, the effects are partially reversible. The defects responsible for these modifications are identified as non-bridging oxygen hole centers, which fade by recombination with electrons after irradiation. The kinetics of the defect formation and fading process are also studied in real time.

  20. Methodological approaches for using synchrotron X-ray fluorescence (SXRF) imaging as a tool in ionomics: Examples from Arabidopsis thaliana

    PubMed Central

    Hindt, Maria; Socha, Amanda L.; Zuber, Hélène

    2013-01-01

    Here we present approaches for using multi-elemental imaging (specifically synchrotron X-ray fluorescence microscopy, SXRF) in ionomics, with examples using the model plant Arabidopsis thaliana. The complexity of each approach depends on the amount of a priori information available for the gene and/or phenotype being studied. Three approaches are outlined, which apply to experimental situations where a gene of interest has been identified but has an unknown phenotype (Phenotyping), an unidentified gene is associated with a known phenotype (Gene Cloning) and finally, a Screening approach, where both gene and phenotype are unknown. These approaches make use of open-access, online databases with which plant molecular genetics researchers working in the model plant Arabidopsis will be familiar, in particular the Ionomics Hub and online transcriptomic databases such as the Arabidopsis eFP browser. The approaches and examples we describe are based on the assumption that altering the expression of ion transporters can result in changes in elemental distribution. We provide methodological details on using elemental imaging to aid or accelerate gene functional characterization by narrowing down the search for candidate genes to the tissues in which elemental distributions are altered. We use synchrotron X-ray microprobes as a technique of choice, which can now be used to image all parts of an Arabidopsis plant in a hydrated state. We present elemental images of leaves, stem, root, siliques and germinating hypocotyls. PMID:23912758

  1. A compressed sensing based reconstruction algorithm for synchrotron source propagation-based X-ray phase contrast computed tomography

    NASA Astrophysics Data System (ADS)

    Melli, Seyed Ali; Wahid, Khan A.; Babyn, Paul; Montgomery, James; Snead, Elisabeth; El-Gayed, Ali; Pettitt, Murray; Wolkowski, Bailey; Wesolowski, Michal

    2016-01-01

    Synchrotron source propagation-based X-ray phase contrast computed tomography is increasingly used in pre-clinical imaging. However, it typically requires a large number of projections, and subsequently a large radiation dose, to produce high quality images. To improve the applicability of this imaging technique, reconstruction algorithms that can reduce the radiation dose and acquisition time without degrading image quality are needed. The proposed research focused on using a novel combination of Douglas-Rachford splitting and randomized Kaczmarz algorithms to solve large-scale total variation based optimization in a compressed sensing framework to reconstruct 2D images from a reduced number of projections. Visual assessment and quantitative performance evaluations of a synthetic abdomen phantom and real reconstructed image of an ex-vivo slice of canine prostate tissue demonstrate that the proposed algorithm is competitive in reconstruction process compared with other well-known algorithms. An additional potential benefit of reducing the number of projections would be reduction of time for motion artifact to occur if the sample moves during image acquisition. Use of this reconstruction algorithm to reduce the required number of projections in synchrotron source propagation-based X-ray phase contrast computed tomography is an effective form of dose reduction that may pave the way for imaging of in-vivo samples.

  2. Synchrotron-based crystal structure, associated morphology of snail and bivalve shells by X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Rao, D. V.; Gigante, G. E.; Kumar, Y. Manoj; Cesareo, R.; Brunetti, A.; Schiavon, N.; Akatsuka, T.; Yuasa, T.; Takeda, T.

    2016-10-01

    Synchrotron-based high-resolution X-ray powder diffraction spectra from the body parts of a snail and bivalve (CaCO3), have been recorded with Pilatus area detector. Experiments were performed at Desy, Hamburg, Germany, utilizing the Resonant and Diffraction beamline (P9), with 15 keV X-rays (λ=0.82666 Å). The external shell of these living organisms, is composed of calcium carbonate, which carries strong biological signal. It consists of some light elements, such as, Ca, C and O, which constitute part of the soft tissue and other trace elements. The knowledge of these diffraction patterns and hence the understanding of structures at molecular level are enormous. The application of synchrotron radiation to powder diffraction is well suited for samples of biological nature via changes in their patterns and also to investigate crystallographic phase composition. With the use of Rietveld refinement procedure, to the high-resolution diffraction spectra, we were able to extract the lattice parameters of orthorhombic polymorph of CaCO3, the most abundant mineral produced by these living organisms. The small size of the crystallite is a very important factor related to the biological structure. The natural model presents a combination of organic and inorganic phases with nanometer size. For the present study, we also used the scanning electron microscopy (SEM) to explore the associated morphology of the snail and bivalve.

  3. Gallium melts under high-pressure and temperature conditions: Synchrotron x-ray tomography and diffraction studies

    NASA Astrophysics Data System (ADS)

    Liu, L. L.; Liu, H.

    2014-12-01

    Gallium has a rare water-ice type P-V-T phase diagram in which the density of Ga melt exceeds by about 3 % that of the stable solid Ga phase I at ambient pressure. Liquid gallium, which is easily supercooled, can remain in a metastable liquid state for several months at ambient pressure. A rich polymorphism and metastable modifications of Ga have been discovered in P-T domain. There are a number of studies of liquid gallium under high pressure conditions, but some fundamental properties, such as the equation of state (EoS) of liquid Ga under extreme conditions remain unclear. Very recently, the advanced pair distribution function (PDF) method 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 conditions. However, the application of PDF method for amorphous or liquid samples under pressure conditions normally required a priori knowledge of their EoS. The density estimation from the reverse Monte Carlo simulation with the best mathematical fit to the measured structure factor data could cause big errors if it is calculated without knowing the EoS. In the paper, the volume change of liquid and solid gallium have been studied as a function of pressure and temperature up to 3.63 GPa using synchrotron x-ray microtomography combined with energy dispersive x-ray diffraction (EDXRD) techniques. Two sets of directly measured P-V data at 300 K and 330 K were obtained from 3D tomography reconstruction data. 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.

  4. Nucleation and Grain Growth During Dehydration of Polycrystalline Gypsum Observed in Time-series Synchrotron X-ray Micro-tomography Experiments

    NASA Astrophysics Data System (ADS)

    Leclere, H.; Bedford, J. D.; Fusseis, F.; Wheeler, J.; Faulkner, D.

    2015-12-01

    Nucleation and growth of new minerals in response to disequilibrium is the most fundamental metamorphic process. However, our current understanding of metamorphic reactions is largely based on inference from mineral assemblages brought to the surface by uplift and erosion, rather than from direct observation. The experimental investigation of metamorphism has also been limited, typically to concealed vessels thus restricting the possibility of direct microstructural monitoring. Recent advances in synchrotron-based X-ray micro-tomography allow for new experiments that utilise X-ray transparent setups in order to image these processes on the micron-scale in 4D. We conducted in-situ constant temperature experiments at the Advanced Photon Source (Argonne National Laboratory, USA) to dehydrate confined cylinders of Volterra Gypsum (5mm length x 2mm diameter). The relatively modest temperature of reaction and the apparently simple mineralogy make gypsum an ideal material for investigating processes associated with metamorphic devolatilization. Using a purpose-built X-ray transparent experimental cell (Fusseis et al., 2014, J. Synchrotron Rad. 21, 251-253) to apply an effective pressure of 5MPa, the samples were heated to 388K for approximately 10 hours to acquire three-dimensional time-series tomography datasets comprising forty time steps. Images show grains of the product material (bassanite) growing throughout the sample accompanied by an evolving porous network. These datasets provide new visual insights into the spatiotemporal association between porosity development and the formation of product minerals during devolatilization. The direct observation of reaction also has important implications for general metamorphic theory as we can track the complete history of grain growth from nucleation through to interaction with surrounding grains.

  5. Sagittal focusing of synchrotron radiation X-rays using a winged crystal.

    PubMed

    Nisawa, A; Yoneda, Y; Ueno, G; Murakami, H; Okajima, Y; Yamamoto, K; Senba, Y; Uesugi, K; Tanaka, Y; Yamamoto, M; Goto, S; Ishikawa, T

    2013-03-01

    A Si(111) winged crystal has been designed to minimize anticlastic bending and improve sagittal focusing efficiency. The crystal was thin with wide stiffening wings. The length-to-width ratio of the crystal was optimized by finite element analysis, and the optimal value was larger than the `golden value'. The analysis showed that the slope error owing to anticlastic bending is less than the Darwin width. The X-rays were focused two-dimensionally using the crystal and a tangentially bent mirror. The observed profiles of the focal spot agreed well with the results of a ray-tracing calculation in the energy range from 8 to 17.5 keV. X-ray diffraction measurements with a high signal-to-noise ratio using this focusing system were demonstrated for a small protein crystal.

  6. Synchrotron ultra-fast X-ray imaging of a cavitating flow in a Venturi profile

    NASA Astrophysics Data System (ADS)

    Vabre, A.; Gmar, M.; Lazaro, D.; Legoupil, S.; Coutier, O.; Dazin, A.; Lee, W. K.; Fezzaa, K.

    2009-08-01

    Cavitation consists of successive vaporization and condensation processes in a liquid flow, due to a large pressure decrease usually associated with sudden flow acceleration. This phenomenon occurs typically in pumps and naval propellers, on the blades' suction side and/or in periphery of the rotor. It is associated with performance decrease, blade erosion, vibrations that may lead to damage, and noise due to vapor collapse close to the solid walls. Therefore, a general understanding of the mechanisms that govern flow vaporization and condensation is of the utmost importance to reduce or at least to control these effects. A major issue is to estimate velocity fields in both phases, i.e. liquid and vapor. These combined measurements are missing in the literature. We propose a method of ultra-fast X-ray imaging to cope this lack. This method is based on X-ray absorption and phase-contrast enhancement. This technique can simultaneously measure the flow velocities of both liquid and vapor phases at kHz frequency. For the X-ray measurements, a dedicated Venturi shape canal has been designed for the experiments. The design is based on a known two-phase flows hydraulic set-up. The studied cavitation occurs downstream from the Venturi profile. The experiments were carried out at the Advanced Photon Source (APS) at Argonne National Laboratory. These experiments have confirmed the advantages of ultra-fast X-ray imaging for the visualization of liquid-vapor interfaces. Also, the feasibility of estimating velocity field in the flow is acknowledged.

  7. Simple photoelectron x-ray beam position monitor for synchrotron radiation

    SciTech Connect

    Heald, S.M.

    1985-01-01

    A UHV compatible x-ray beam position monitor is described. The monitor operates by detecting the photoelectrons emitted by two parallel tungsten wires. A key feature of the monitor is the simplicity of its design and construction which allows it to fit on a 2 3/4 in. conflat flange. When combined with a simple log-ratio current amplifier the monitor gives an output linear in the beam position with a sensitivity better than 0.02 mm.

  8. Fast X-Ray Fluorescence Camera Combined with Wide Band Pass Monochromatic Synchrotron Beam

    NASA Astrophysics Data System (ADS)

    Sakurai, Kenji; Mizusawa, Mari

    2004-05-01

    A double W/B4C multilayer monochromator (2d=50.4Å) was commissioned for non-scanning X-ray fluorescence (XRF) imaging experiments. The combination of a brilliant multi-pole wiggler source and the present wide band pass monochromator permits 1.2 × 1013 photons/sec at the sample position for 8.04 keV X-rays. Energy resolution ΔE and ΔE/E are 300˜500 eV and ˜5%, respectively. The exit beam height is constant for X-ray energy ranging from 5.5 to 13.0 keV. Indirect cooling of the 1st multilayer works successfully. In addition, a new fast CCD camera was developed for quick readout and transfer of the image data. It was found that the typical exposure time for one XRF image with 1000 × 1000 pixels is 0.03˜1 sec. This permits in-situ movie recording for the distribution of elements.

  9. Nanoscale Examination of Microdamage in Sheep Cortical Bone Using Synchrotron Radiation Transmission X-Ray Microscopy

    PubMed Central

    Brock, Garry R.; Kim, Grace; Ingraffea, Anthony R.; Andrews, Joy C.; Pianetta, Piero; van der Meulen, Marjolein C. H.

    2013-01-01

    Microdamage occurs in bone through repeated and excessive loading. Accumulation of microdamage weakens bone, leading to a loss of strength, stiffness and energy dissipation in the tissue. Imaging techniques used to examine microdamage have typically been limited to the microscale. In the current study microdamage was examined at the nanoscale using transmission x-ray microscopy with an x-ray negative stain, lead-uranyl acetate. Microdamage was generated in notched and unnotched beams of sheep cortical bone (2×2×20 mm), with monotonic and fatigue loading. Bulk sections were removed from beams and stained with lead-uranyl acetate to identify microdamage. Samples were sectioned to 50 microns and imaged using transmission x-ray microscopy producing projection images of microdamage with nanoscale resolution. Staining indicated microdamage occurred in both the tensile and compressive regions. A comparison between monotonic and fatigue loading indicated a statistically significant greater amount of stain present in fatigue loaded sections. Microdamage occurred in three forms: staining to existing bone structures, cross hatch damage and a single crack extending from the notch tip. Comparison to microcomputed tomography demonstrated differences in damage morphology and total damage between the microscale and nanoscale. This method has future applications for understanding the underlying mechanisms for microdamage formation as well as three-dimensional nanoscale examination of microdamage. PMID:23472121

  10. Solution Phase Molecular Dynamics Probed with Synchrotron Hard X-rays

    NASA Astrophysics Data System (ADS)

    March, Anne; Doumy, Gilles; Kanter, Elliot; Southworth, Stephen; Young, Linda; Nemeth, Zoltan; Vankó, Gyorgy; Assefa, Tadesse; Gawelda, Wojciech

    2013-05-01

    The ability to measure short-lived transient states during a chemical reaction is key to understanding many important processes such as oxygen binding in hemeproteins and electron transport in photosynthesis. Time resolved hard x-ray spectroscopies, which are based on laser-pump/x-ray-probe methods, are a unique tool because unlike UV-VIS techniques they are element specific and can provide electronic and structural information with atomic resolution in the vicinity of a particular atom or ion. These characteristics make them particularly powerful for studying molecules in complex environments such as solutions. Using a MHz, picosecond, high average power laser system implemented at Sector 7ID-D of the Advanced Photon Source we have been developing time resolved x-ray emission techniques to track the evolution of photoexcited molecules in solution. We will present recent studies which include the ligand substitution reaction and hydrated electron formation in the coordination complex ferrocyanide Fe(CN)64-. This work was supported by the Chemical Sciences, Geosciences, and Biosciences Division and the Advanced Photon Source by the Office of Basic Energy Sciences, Office of Science, US Dept of Energy, Contract DE-AC02-06CH11357.

  11. X-ray Topography to Characterize Surface Damage on CdZnTe Crystals

    SciTech Connect

    Black, David; Woicik, Joseph; Duff, Martine C.; Hunter, Douglas B.; Burger, Arnold; Groza, Michael

    2008-12-05

    Synthetic CdZnTe or 'CZT' crystals can be used for room temperature detection of {gamma}-radiation. Structural/morphological heterogeneities within CZT, such as twinning, secondary phases (often referred to as inclusions or precipitates), and poly-crystallinity can affect detector performance. As part of a broader study using synchrotron radiation techniques to correlate detector performance to microstructure, x-ray topography (XRT) has been used to characterize CZT crystals. We have found that CZT crystals almost always have a variety of residual surface damage, which interferes with our ability to observe the underlying microstructure for purposes of crystal quality evaluation. Specific structures are identifiable as resulting from fabrication processes and from handling and shipping of sample crystals. Etching was found to remove this damage; however, our studies have shown that the radiation detector performance of the etched surfaces was inferior to the as-polished surface due to higher surface currents which result in more peak tailing and less energy resolution. We have not fully investigated the effects of the various types of inducible damage on radiation detector performance.

  12. X-ray Topography to Characterize Surface Damage on CdZnTe Crystals

    SciTech Connect

    Black, David; Woicik, Joseph; Duff, Martine C.; Hunter, Douglas B.; Burger, Arnold; Groza, Michael

    2008-07-01

    Synthetic CdZnTe or 'CZT' crystals can be used for room temperature detection of {gamma}-radiation. Structural/morphological heterogeneities within CZT, such as twinning, secondary phases (often referred to as inclusions or precipitates), and poly-crystallinity can affect detector performance. As part of a broader study using synchrotron radiation techniques to correlate detector performance to microstructure, x-ray topography (XRT) has been used to characterize CZT crystals. We have found that CZT crystals almost always have a variety of residual surface damage, which interferes with our ability to observe the underlying microstructure for purposes of crystal quality evaluation. Specific structures are identifiable as resulting from fabrication processes and from handling and shipping of sample crystals. Etching was found to remove this damage; however, our studies have shown that the radiation detector performance of the etched surfaces was inferior to the as-polished surface due to higher surface currents which result in more peak tailing and less energy resolution. We have not fully investigated the effects of the various types of inducible damage on radiation detector performance. (authors)

  13. Synchrotron micro-X-ray fluorescence analysis of natural diamonds: First steps in identification of mineral inclusions in situ

    SciTech Connect

    Sitepu, Husin; Kopylova, Maya G.; Quirt, David H.; Cutler, Jeffrey N.; Kotzer, Thomas G.

    2008-06-09

    Diamond inclusions are of particular research interest in mantle petrology and diamond exploration as they provide direct information about the chemical composition of upper and lower mantle and about the petrogenetic sources of diamonds in a given deposit. The objective of the present work is to develop semi-quantitative analytical tools for non-destructive in situ identification and characterization of mineral inclusions in diamonds using synchrotron micro-X-ray Fluorescence ({mu}SXRF) spectroscopy and micro-X-ray Absorption Near Edge Structure ({mu}XANES) spectroscopy at a focused spot size of 4 to 5 micrometers. The data were collected at the Pacific Northwest Consortium (PNC-CAT) 20-ID microprobe beamline at the Advanced Photon Source, located at the Argonne National Laboratory, and yielded the first high-resolution maps of Ti, Cr, Fe, Ni, Cu, and Zn for natural diamond grains, along with quantitative {mu}SXRF analysis of select chemical elements in exposed kimberlite indicator mineral grains. The distribution of diamond inclusions inside the natural diamond host, both visible and invisible using optical transmitted-light microscopy, can be mapped using synchrotron {mu}XRF analysis. Overall, the relative abundances of chemical elements determined by {mu}SXRF elemental analyses are broadly similar to their expected ratios in the mineral and therefore can be used to identify inclusions in diamonds in situ. Synchrotron {mu}XRF quantitative analysis provides accurate estimates of Cr contents of exposed polished minerals when calibrated using the concentration of Fe as a standard. Corresponding Cr K-edge {mu}XANES analyses on selected inclusions yield unique information regarding the formal oxidation state and local coordination of Cr.

  14. Absorbed dose-to-water protocol applied to synchrotron-generated x-rays at very high dose rates

    NASA Astrophysics Data System (ADS)

    Fournier, P.; Crosbie, J. C.; Cornelius, I.; Berkvens, P.; Donzelli, M.; Clavel, A. H.; Rosenfeld, A. B.; Petasecca, M.; Lerch, M. L. F.; Bräuer-Krisch, E.

    2016-07-01

    Microbeam radiation therapy (MRT) is a new radiation treatment modality in the pre-clinical stage of development at the ID17 Biomedical Beamline of the European synchrotron radiation facility (ESRF) in Grenoble, France. MRT exploits the dose volume effect that is made possible through the spatial fractionation of the high dose rate synchrotron-generated x-ray beam into an array of microbeams. As an important step towards the development of a dosimetry protocol for MRT, we have applied the International Atomic Energy Agency’s TRS 398 absorbed dose-to-water protocol to the synchrotron x-ray beam in the case of the broad beam irradiation geometry (i.e. prior to spatial fractionation into microbeams). The very high dose rates observed here mean the ion recombination correction factor, k s , is the most challenging to quantify of all the necessary corrections to apply for ionization chamber based absolute dosimetry. In the course of this study, we have developed a new method, the so called ‘current ramping’ method, to determine k s for the specific irradiation and filtering conditions typically utilized throughout the development of MRT. Using the new approach we deduced an ion recombination correction factor of 1.047 for the maximum ESRF storage ring current (200 mA) under typical beam spectral filtering conditions in MRT. MRT trials are currently underway with veterinary patients at the ESRF that require additional filtering, and we have estimated a correction factor of 1.025 for these filtration conditions for the same ESRF storage ring current. The protocol described herein provides reference dosimetry data for the associated Treatment Planning System utilized in the current veterinary trials and anticipated future human clinical trials.

  15. Absorbed dose-to-water protocol applied to synchrotron-generated x-rays at very high dose rates.

    PubMed

    Fournier, P; Crosbie, J C; Cornelius, I; Berkvens, P; Donzelli, M; Clavel, A H; Rosenfeld, A B; Petasecca, M; Lerch, M L F; Bräuer-Krisch, E

    2016-07-21

    Microbeam radiation therapy (MRT) is a new radiation treatment modality in the pre-clinical stage of development at the ID17 Biomedical Beamline of the European synchrotron radiation facility (ESRF) in Grenoble, France. MRT exploits the dose volume effect that is made possible through the spatial fractionation of the high dose rate synchrotron-generated x-ray beam into an array of microbeams. As an important step towards the development of a dosimetry protocol for MRT, we have applied the International Atomic Energy Agency's TRS 398 absorbed dose-to-water protocol to the synchrotron x-ray beam in the case of the broad beam irradiation geometry (i.e. prior to spatial fractionation into microbeams). The very high dose rates observed here mean the ion recombination correction factor, k s , is the most challenging to quantify of all the necessary corrections to apply for ionization chamber based absolute dosimetry. In the course of this study, we have developed a new method, the so called 'current ramping' method, to determine k s for the specific irradiation and filtering conditions typically utilized throughout the development of MRT. Using the new approach we deduced an ion recombination correction factor of 1.047 for the maximum ESRF storage ring current (200 mA) under typical beam spectral filtering conditions in MRT. MRT trials are currently underway with veterinary patients at the ESRF that require additional filtering, and we have estimated a correction factor of 1.025 for these filtration conditions for the same ESRF storage ring current. The protocol described herein provides reference dosimetry data for the associated Treatment Planning System utilized in the current veterinary trials and anticipated future human clinical trials. PMID:27366861

  16. X-ray reflectivity measurements of surface roughness using energy dispersive detection

    SciTech Connect

    Chason, E.; Warwick, D.T.

    1990-01-01

    We describe a new technique for measuring x-ray reflectivity using energy dispersive x-ray detection. The benefits of this method are the use of a fixed scattering angle and parallel detection of all energies simultaneously. These advantages make the technique more readily useable with laboratory x-ray sources and more compatible with growth chambers. We find excellent agreement between the calculated Fresnel reflectivity and the reflectivity obtained from a smooth Ge (001) surface. Reflectivities obtained during 500 eV Xe ion bombardment of Ge surfaces demonstrate the sensitivity of the technique to be better than 1 {angstrom}. 9 refs., 4 figs.

  17. Upgrade of surface profiler for x-ray mirror at SPring-8

    NASA Astrophysics Data System (ADS)

    Senba, Y.; Kishimoto, H.; Miura, T.; Ohashi, H.

    2014-09-01

    In beamlines at third-generation synchrotron radiation and X-ray free-electron-laser (XFEL) facilities, various mirrors are used as deflection, focusing, and collimating optics. The required specifications for the mirrors depend on their purpose. In recent years, high-precision aspheric mirrors and flat mirrors, with a figure error less than 10 nm are used as diffraction-limited focusing optics and deflection optics, respectively. The origins of the figure error are fabrication error, gravitational deformation, and clamping deformation. In the case of the bend mirror, figure error is also induced by the bender mechanism. The fabrication error is measured by a long trace profiler (LTP) [1] or by relative-angle determinable stitching interferometry (RADSI) [2] with special high frequency of 0.1-1/mm. Deformation caused by gravity, clamping, and bending should be measured under actual operating conditions because these deformations depend on the direction of the mirror surface and the direction of clamping and bending, respectively. In recent years, in-situ and atwavelength metrology techniques such as the Hartmann sensor, pencil beam, grating base and the speckle-effect-based technique, have been reported [3-6]. These methods are able to investigate the profile of the mirror under real conditions, including the effects of thermal bump; however, these techniques require X-rays and a long optical length to the detector. We attempted to upgrade the LTP at SPring-8 using autocollimators for the precise measurement of height profiles under conditions of both upward and horizontal reflection geometries. A portable Fizeau interferometer was installed for onsite measurement.

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

    NASA Astrophysics Data System (ADS)

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

    2016-11-01

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

  19. X-ray fluorescence studies for the elemental composition and molecular organization of protein films on the surface of the liquid subphase

    SciTech Connect

    Zheludeva, S. I.; Novikova, N. N. Kovalchuk, M. V.; Stepina, N. D.; Konovalov, O. V.; Yurieva, E. A.

    2009-11-15

    This paper reports on the results of the investigation of protein films that are based on alkaline phosphatase and glucose oxidase enzymes and formed on the surface of the liquid subphase. The experimental studies have been performed using total external reflection X-ray fluorescence spectrometry at the European Synchrotron Radiation Facility (Grenoble, France). The self-organization processes that occur in protein systems on the surface of the liquid subphase under the conditions where the protein molecules retain their mobility have been investigated using X-ray fluorescence measurements for the first time.

  20. Torsional oscillator and synchrotron x-ray experiments on solid {sup 4}He in aerogel.

    SciTech Connect

    Mulders, N.; West, J. T.; Chan, M. H. W.; Kodituwakku, C. N.; Burns, C. A.; Lurio, L. B.; Univ. of Delaware; Pennsylvania State Univ.; Western Michigan Univ.; Northern Illinois Univ.

    2008-01-01

    X-ray diffraction experiments show that solid {sup 4}He grown in aerogel is highly polycrystalline, with an hcp crystal structure (as in bulk) and a crystallite size of approximately 100 nm. In contrast to the expectation that the highly disordered solid will have a large supersolid fraction, torsional oscillator measurements show a behavior that is strikingly similar to high purity crystals grown from the superfluid phase. The low temperature supersolid fraction is only {approx}3 x 10{sup -4}, and the onset temperature is {approx}100 mK.

  1. Synchrotron X-ray Microdiffraction Analysis of Proton Irradiated Polycrystalline Diamond Films

    NASA Technical Reports Server (NTRS)

    Newton, R. I.; Davidson, J. L.; Ice, G. E.; Liu, W.

    2004-01-01

    X-ray microdiffraction is a non-destructive technique that allows for depth-resolved, strain measurements with sub-micron spatial resolution. These capabilities make this technique promising for understanding the mechanical properties of MicroElectroMechanical Systems (MEMS). This investigation examined the local strain induced by irradiating a polycrystalline diamond thin film with a dose of 2x10(exp 17) H(+)per square centimeter protons. Preliminary results indicate that a measurable strain, on the order of 10(exp -3), was introduced into the film near the End of Range (EOR) region of the protons.

  2. Electrochemically induced reconstruction of the Au(001) surface: An x-ray scattering study

    SciTech Connect

    Ocko, B.M.; Wang, Jia.

    1991-01-01

    In-situ x-ray specular reflectivity and glancing incident angle x-ray diffraction measurements have been performed in the Au(001) surface in two solutions under potential control in an electrochemical cell. In both the 0.01 M HCl0{sub 4} and 0.01 M KBr solutions a (5 {times} 20)'' reconstruction is formed at sufficient negative potentials. The reconstruction is similar to that obtained for the clean surface in vacuum.

  3. Electrochemically induced reconstruction of the Au(001) surface: An x-ray scattering study

    SciTech Connect

    Ocko, B.M.; Wang, Jia

    1991-12-31

    In-situ x-ray specular reflectivity and glancing incident angle x-ray diffraction measurements have been performed in the Au(001) surface in two solutions under potential control in an electrochemical cell. In both the 0.01 M HCl0{sub 4} and 0.01 M KBr solutions a ``(5 {times} 20)`` reconstruction is formed at sufficient negative potentials. The reconstruction is similar to that obtained for the clean surface in vacuum.

  4. Advanced Techniques for In-Situ Monitoring of Phase Transformations During Welding Using Synchrotron-Based X-Ray Diffraction

    SciTech Connect

    Elmer, J W; Palmer, T A; Zhang, W; DebRoy, T

    2005-06-05

    Understanding the evolution of microstructure in welds is an important goal of welding research because of the strong correlation between weld microstructure and weld properties. To achieve this goal it is important to develop a quantitative measure of phase transformations encountered during welding in order to ultimately develop methods for predicting weld microstructures from the characteristics of the welding process. To aid in this effort, synchrotron radiation methods have been developed at Lawrence Livermore National Laboratory (LLNL) for direct observation of microstructure evolution during welding. Using intense, highly collimated synchrotron radiation, the atomic structure of the weld heat affected and fusion zones can be probed in real time. Two synchrotron-based techniques, known as spatially resolved (SRXRD) and time resolved (TRXRD) x-ray diffraction, have been developed for these investigations. These techniques have now been used to investigate welding induced phase transformations in titanium alloys, low alloy steels, and stainless steel alloys. This paper will provide a brief overview of these methods and will discuss microstructural evolution during the welding of low carbon (AISI 1005) and medium carbon (AISI 1045) steels where the different levels of carbon influence the evolution of microstructures during welding.

  5. Soft X-Ray Microscopy Radiation Damage On Fixed Cells Investigated With Synchrotron Radiation FTIR Microscopy

    PubMed Central

    Gianoncelli, A.; Vaccari, L.; Kourousias, G.; Cassese, D.; Bedolla, D. E.; Kenig, S.; Storici, P.; Lazzarino, M.; Kiskinova, M.

    2015-01-01

    Radiation damage of biological samples remains a limiting factor in high resolution X-ray microscopy (XRM). Several studies have attempted to evaluate the extent and the effects of radiation damage, proposing strategies to minimise or prevent it. The present work aims to assess the impact of soft X-rays on formalin fixed cells on a systematic manner. The novelty of this approach resides on investigating the radiation damage not only with XRM, as often reported in relevant literature on the topic, but by coupling it with two additional independent non-destructive microscopy methods: Atomic Force Microscopy (AFM) and FTIR Microscopy (FTIRM). Human Embryonic Kidney 293 cells were exposed to different radiation doses at 1 keV. In order to reveal possible morphological and biochemical changes, the irradiated cells were systematically analysed with AFM and FTIRM before and after. Results reveal that while cell morphology is not substantially affected, cellular biochemical profile changes significantly and progressively when increasing dose, resulting in a severe breakdown of the covalent bonding network. This information impacts most soft XRM studies on fixed cells and adds an in-depth understanding of the radiation damage for developing better prevention strategies. PMID:25974639

  6. Soft X-Ray Microscopy Radiation Damage On Fixed Cells Investigated With Synchrotron Radiation FTIR Microscopy.

    PubMed

    Gianoncelli, A; Vaccari, L; Kourousias, G; Cassese, D; Bedolla, D E; Kenig, S; Storici, P; Lazzarino, M; Kiskinova, M

    2015-05-14

    Radiation damage of biological samples remains a limiting factor in high resolution X-ray microscopy (XRM). Several studies have attempted to evaluate the extent and the effects of radiation damage, proposing strategies to minimise or prevent it. The present work aims to assess the impact of soft X-rays on formalin fixed cells on a systematic manner. The novelty of this approach resides on investigating the radiation damage not only with XRM, as often reported in relevant literature on the topic, but by coupling it with two additional independent non-destructive microscopy methods: Atomic Force Microscopy (AFM) and FTIR Microscopy (FTIRM). Human Embryonic Kidney 293 cells were exposed to different radiation doses at 1 keV. In order to reveal possible morphological and biochemical changes, the irradiated cells were systematically analysed with AFM and FTIRM before and after. Results reveal that while cell morphology is not substantially affected, cellular biochemical profile changes significantly and progressively when increasing dose, resulting in a severe breakdown of the covalent bonding network. This information impacts most soft XRM studies on fixed cells and adds an in-depth understanding of the radiation damage for developing better prevention strategies.

  7. Synchrotron x-ray photoconductor detector arrays made on MBE grown CdTe

    SciTech Connect

    Yoo, S.S.; Montano, P.A. |; Rodricks, B.; Sivananthan, S.; Faurie, J.P.

    1996-08-01

    We have been fabricating x-ray photoconductor linear array detectors using molecular beam epitaxially (MBE) grown (111)B undoped CdTe layers on (100) Si substrates. A novel technique was developed to remove the Si and to mount the fragile MBE grown CdTe layers onto insulating ceramic substrates. 256 channel linear photoconductor array devices were fabricated on the resulting CdTe layers. The resistivity of MBE (111)B CdTe was high (> 10{sup 8} {Omega}cm) enough to utilize the material for low energy (8 to 25 keV) x-ray detectors. The stability of the detectors are satisfactory, and they were tested at room temperature routinely for over a year. The performance of the photoconductor was greatly improved when the detector was cooled to 230K. Due to its reduced dark current at low temperatures, the dynamic range of the detector response increased to nearly four decades at 230K. 29 refs., 8 figs.

  8. Soft X-Ray Microscopy Radiation Damage On Fixed Cells Investigated With Synchrotron Radiation FTIR Microscopy

    NASA Astrophysics Data System (ADS)

    Gianoncelli, A.; Vaccari, L.; Kourousias, G.; Cassese, D.; Bedolla, D. E.; Kenig, S.; Storici, P.; Lazzarino, M.; Kiskinova, M.

    2015-05-01

    Radiation damage of biological samples remains a limiting factor in high resolution X-ray microscopy (XRM). Several studies have attempted to evaluate the extent and the effects of radiation damage, proposing strategies to minimise or prevent it. The present work aims to assess the impact of soft X-rays on formalin fixed cells on a systematic manner. The novelty of this approach resides on investigating the radiation damage not only with XRM, as often reported in relevant literature on the topic, but by coupling it with two additional independent non-destructive microscopy methods: Atomic Force Microscopy (AFM) and FTIR Microscopy (FTIRM). Human Embryonic Kidney 293 cells were exposed to different radiation doses at 1 keV. In order to reveal possible morphological and biochemical changes, the irradiated cells were systematically analysed with AFM and FTIRM before and after. Results reveal that while cell morphology is not substantially affected, cellular biochemical profile changes significantly and progressively when increasing dose, resulting in a severe breakdown of the covalent bonding network. This information impacts most soft XRM studies on fixed cells and adds an in-depth understanding of the radiation damage for developing better prevention strategies.

  9. In-situ X-ray Synchrotron Microtomography: Real Time Pore Structure Evolution during Olivine Carbonation

    NASA Astrophysics Data System (ADS)

    Zhu, W.; Fusseis, F.; Lisabeth, H. P.; Xiao, X.

    2013-12-01

    Mineral carbonation has been proposed as a promising method for long-term, secure sequestration of carbon dioxide. In porous rocks, fluid-rock interactions can significantly alter the pore space and thus exert important controls over the rate and extent of carbonation. We constructed an x-ray transparent pressure cell [Fusseis et al., 2013] to investigate the real time pore structure evolution during mineral carbonation in porous olivine aggregates. In each experiment, a sintered olivine sample was subjected to a confining pressure of 13 MPa and a pore pressure of 10 MPa, with a sodium bicarbonate solution (NaHCO3 at 1.5 M) as pore fluid. At these pressure conditions, the cell was heated to 473 K. Constant pressure and temperature conditions were maintained during the length of the experiments, lasting 72-120 hours. Using a polychromatic beam in the 2-BM upstream hutch at the Advanced Photon Source, 3-dimensional (3-D) microtomography data were collected in 20 seconds with 30-minute interval. A novel phase retrieval reconstruction algorithm [Paganin et al., 2002] was used to reconstruct microtomographic datasets with a voxel size of ~1.1 micron. The microtomography images at different stages of the carbonation process reveal progressive growth of new crystals in the pore space. Integration of a x-ray transparent pressure vessel with flow through capacity and 3-D microtomography provides a novel research direction of studying the coupled chemo-hydro-thermal-mechanical processes in rocks.

  10. Characterization of Mineral Assemblages in Ancient Roman Maritime Concrete with Synchrotron X-ray Techniques

    NASA Astrophysics Data System (ADS)

    Meral, C.; Jackson, M. D.; Monteiro, P. J.; Wenk, H.

    2012-12-01

    Romans used lime and aluminosilicate-rich volcanic ash to bind tuff aggregates in concrete structures that have remained durable for 2000 years. A major accomplishment of Roman engineers was to construct enduring coastal underwater structures in seawater, which were important to long-distance trade and military endeavors. Two millennia later, the reasons for the extraordinary durability of the maritime structures remain enigmatic. The concretes are highly complex composites composed of relict lime, tuff and pumice clasts and pozzolanic reaction products. Calcium-chloroaluminates and sulfoaluminates occur in certain relict voids. Further understanding of their mineralogical components would provide guidelines in designing future structures. Here, we use synchroton radiation applications to characterize certain phases within a Roman maritime mortar specimen from a breakwater in Pozzuoli Bay, Baianus Sinus, near Naples. We performed X-ray computed micro-tomography (μ-XCT) at beamline 8.3.2 of the Advanced Light Source (ALS) at Lawrence Berkeley Laboratories to segment the complex composite without damaging the specimen. We isolated certain relict sub-spherical voids and illustrated crystal morphologies with 3-D reconstructions. We then used beamline 12.3.2 at the ALS to provide highly accurate identifications of diverse crystal phases in various mortar components - relict lime clasts, tuff or pumice clasts, cementitious matrix and relict voids - in sites previously identified and characterized with petrogaphic techniques. X-ray micro-fluorescence (μ-XRF) mapping provided calcium and iron maps of the sites, which were useful in selecting fine-scale areas for scanning transmission X-ray micro-diffraction (μ-XRD) mapping at high spatial resolution, about 1 micron. The μ-XRD analyses utilized both monochromatic and polychromatic light measurements. Polychromatic light was more appropriate for phases with grain sizes larger than the doubly focused X-ray beam, about 1 x

  11. Experimental results for the scattering of X-rays from smooth surfaces

    NASA Technical Reports Server (NTRS)

    Williams, A. C.; Reily, J. C.

    1984-01-01

    By utilizing the unique X-ray test facility at NASA's Marshall Space Flight Center, high resolution data have been obtained for the scattering of X-rays from smooth optical flats. Using X-rays with energies in the range from 2.99 keV to 8.06 keV, the resulting reflected images from five state-of-the-art polished mirror flats with various substrate and coating materials are presented and analyzed. Evidence for large angle scattering is shown to exist for some energies and is discussed in terms of theoretical models for surface defects.

  12. New insights into globoids of protein storage vacuoles in wheat aleurone using synchrotron soft X-ray microscopy

    PubMed Central

    Regvar, Marjana; Eichert, Diane; Kaulich, Burkhard; Gianoncelli, Alessandra; Pongrac, Paula; Vogel-Mikuš, Katarina; Kreft, Ivan

    2011-01-01

    Mature developed seeds are physiologically and biochemically committed to store nutrients, principally as starch, protein, oils, and minerals. The composition and distribution of elements inside the aleurone cell layer reflect their biogenesis, structural characteristics, and physiological functions. It is therefore of primary importance to understand the mechanisms underlying metal ion accumulation, distribution, storage, and bioavailability in aleurone subcellular organelles for seed fortification purposes. Synchrotron radiation soft X-ray full-field imaging mode (FFIM) and low-energy X-ray fluorescence (LEXRF) spectromicroscopy were applied to characterize major structural features and the subcellular distribution of physiologically important elements (Zn, Fe, Na, Mg, Al, Si, and P). These direct imaging methods reveal the accumulation patterns between the apoplast and symplast, and highlight the importance of globoids with phytic acid mineral salts and walls as preferential storage structures. C, N, and O chemical topographies are directly linked to the structural backbone of plant substructures. Zn, Fe, Na, Mg, Al, and P were linked to globoid structures within protein storage vacuoles with variable levels of co-localization. Si distribution was atypical, being contained in the aleurone apoplast and symplast, supporting a physiological role for Si in addition to its structural function. These results reveal that the immobilization of metals within the observed endomembrane structures presents a structural and functional barrier and affects bioavailability. The combination of high spatial and chemical X-ray microscopy techniques highlights how in situ analysis can yield new insights into the complexity of the wheat aleurone layer, whose precise biochemical composition, morphology, and structural characteristics are still not unequivocally resolved. PMID:21447756

  13. The Advanced Light Source at Lawrence Berkeley Laboratory: A high-brightness soft x-ray synchrotron-radiation facility

    SciTech Connect

    Schlachter, A.S.; Robinson, A.L.

    1990-07-01

    The Advanced Light Source, a third-generation national synchrotron-radiation facility now under construction at the Lawrence Berkeley Laboratory, is scheduled to begin serving qualified users across a broad spectrum of research areas in the spring of 1993. Based on a low-emittance electron storage ring optimized to operate at 1.5 GeV, the ALS will have 10 long straight sections available for insertion devices (undulators and wigglers) and 24 high-quality bend-magnet ports. The short pulse width (30--50 ns) will be ideal for time-resolved measurements. Undulators will generate high-brightness soft x-ray and ultraviolet (XUV) radiation from below 20 eV to above 2 keV. Wigglers and bend magnets will extend the spectrum by generating high fluxes of hard x-rays to photon energies above 10 keV. The ALS will support an extensive research program in which XUV radiation is used to study matter in all its varied gaseous, liquid, and solid forms. The high brightness will open new areas of research in the materials sciences, such as spatially resolved spectroscopy (spectromicroscopy). Biological applications will include x-ray microscopy with element-specific sensitivity in the water window of the spectrum where water is much more transparent than protein. The ALS will be an excellent research tool for atomic physics and chemistry because the high flux will allow measurements to be made with tenuous gas-phase targets. 8 refs., 7 figs., 3 tabs.

  14. New insights into globoids of protein storage vacuoles in wheat aleurone using synchrotron soft X-ray microscopy.

    PubMed

    Regvar, Marjana; Eichert, Diane; Kaulich, Burkhard; Gianoncelli, Alessandra; Pongrac, Paula; Vogel-Mikus, Katarina; Kreft, Ivan

    2011-07-01

    Mature developed seeds are physiologically and biochemically committed to store nutrients, principally as starch, protein, oils, and minerals. The composition and distribution of elements inside the aleurone cell layer reflect their biogenesis, structural characteristics, and physiological functions. It is therefore of primary importance to understand the mechanisms underlying metal ion accumulation, distribution, storage, and bioavailability in aleurone subcellular organelles for seed fortification purposes. Synchrotron radiation soft X-ray full-field imaging mode (FFIM) and low-energy X-ray fluorescence (LEXRF) spectromicroscopy were applied to characterize major structural features and the subcellular distribution of physiologically important elements (Zn, Fe, Na, Mg, Al, Si, and P). These direct imaging methods reveal the accumulation patterns between the apoplast and symplast, and highlight the importance of globoids with phytic acid mineral salts and walls as preferential storage structures. C, N, and O chemical topographies are directly linked to the structural backbone of plant substructures. Zn, Fe, Na, Mg, Al, and P were linked to globoid structures within protein storage vacuoles with variable levels of co-localization. Si distribution was atypical, being contained in the aleurone apoplast and symplast, supporting a physiological role for Si in addition to its structural function. These results reveal that the immobilization of metals within the observed endomembrane structures presents a structural and functional barrier and affects bioavailability. The combination of high spatial and chemical X-ray microscopy techniques highlights how in situ analysis can yield new insights into the complexity of the wheat aleurone layer, whose precise biochemical composition, morphology, and structural characteristics are still not unequivocally resolved.

  15. Synchrotron-based coherent scatter x-ray projection imaging using an array of monoenergetic pencil beams

    NASA Astrophysics Data System (ADS)

    Landheer, Karl; Johns, Paul C.

    2012-09-01

    Traditional projection x-ray imaging utilizes only the information from the primary photons. Low-angle coherent scatter images can be acquired simultaneous to the primary images and provide additional information. In medical applications scatter imaging can improve x-ray contrast or reduce dose using information that is currently discarded in radiological images to augment the transmitted radiation information. Other applications include non-destructive testing and security. A system at the Canadian Light Source synchrotron was configured which utilizes multiple pencil beams (up to five) to create both primary and coherent scatter projection images, simultaneously. The sample was scanned through the beams using an automated step-and-shoot setup. Pixels were acquired in a hexagonal lattice to maximize packing efficiency. The typical pitch was between 1.0 and 1.6 mm. A Maximum Likelihood-Expectation Maximization-based iterative method was used to disentangle the overlapping information from the flat panel digital x-ray detector. The pixel value of the coherent scatter image was generated by integrating the radial profile (scatter intensity versus scattering angle) over an angular range. Different angular ranges maximize the contrast between different materials of interest. A five-beam primary and scatter image set (which had a pixel beam time of 990 ms and total scan time of 56 min) of a porcine phantom is included. For comparison a single-beam coherent scatter image of the same phantom is included. The muscle-fat contrast was 0.10 ± 0.01 and 1.16 ± 0.03 for the five-beam primary and scatter images, respectively. The air kerma was measured free in air using aluminum oxide optically stimulated luminescent dosimeters. The total area-averaged air kerma for the scan was measured to be 7.2 ± 0.4 cGy although due to difficulties in small-beam dosimetry this number could be inaccurate.

  16. Analysis and interpretation of the first monochromatic X-ray tomography data collected at the Australian Synchrotron Imaging and Medical beamline.

    PubMed

    Stevenson, Andrew W; Hall, Christopher J; Mayo, Sheridan C; Häusermann, Daniel; Maksimenko, Anton; Gureyev, Timur E; Nesterets, Yakov I; Wilkins, Stephen W; Lewis, Robert A

    2012-09-01

    The first monochromatic X-ray tomography experiments conducted at the Imaging and Medical beamline of the Australian Synchrotron are reported. The sample was a phantom comprising nylon line, Al wire and finer Cu wire twisted together. Data sets were collected at four different X-ray energies. In order to quantitatively account for the experimental values obtained for the Hounsfield (or CT) number, it was necessary to consider various issues including the point-spread function for the X-ray imaging system and harmonic contamination of the X-ray beam. The analysis and interpretation of the data includes detailed considerations of the resolution and efficiency of the CCD detector, calculations of the X-ray spectrum prior to monochromatization, allowance for the response of the double-crystal Si monochromator used (via X-ray dynamical theory), as well as a thorough assessment of the role of X-ray phase-contrast effects. Computer simulations relating to the tomography experiments also provide valuable insights into these important issues. It was found that a significant discrepancy between theory and experiment for the Cu wire could be largely resolved in terms of the effect of the point-spread function. The findings of this study are important in respect of any attempts to extract quantitative information from X-ray tomography data, across a wide range of disciplines, including materials and life sciences. PMID:22898953

  17. Analysis and interpretation of the first monochromatic X-ray tomography data collected at the Australian Synchrotron Imaging and Medical beamline.

    PubMed

    Stevenson, Andrew W; Hall, Christopher J; Mayo, Sheridan C; Häusermann, Daniel; Maksimenko, Anton; Gureyev, Timur E; Nesterets, Yakov I; Wilkins, Stephen W; Lewis, Robert A

    2012-09-01

    The first monochromatic X-ray tomography experiments conducted at the Imaging and Medical beamline of the Australian Synchrotron are reported. The sample was a phantom comprising nylon line, Al wire and finer Cu wire twisted together. Data sets were collected at four different X-ray energies. In order to quantitatively account for the experimental values obtained for the Hounsfield (or CT) number, it was necessary to consider various issues including the point-spread function for the X-ray imaging system and harmonic contamination of the X-ray beam. The analysis and interpretation of the data includes detailed considerations of the resolution and efficiency of the CCD detector, calculations of the X-ray spectrum prior to monochromatization, allowance for the response of the double-crystal Si monochromator used (via X-ray dynamical theory), as well as a thorough assessment of the role of X-ray phase-contrast effects. Computer simulations relating to the tomography experiments also provide valuable insights into these important issues. It was found that a significant discrepancy between theory and experiment for the Cu wire could be largely resolved in terms of the effect of the point-spread function. The findings of this study are important in respect of any attempts to extract quantitative information from X-ray tomography data, across a wide range of disciplines, including materials and life sciences.

  18. Synchrotron Radiation and Energy Dispersive X-Ray Fluorescence Applications on Elemental Distribution in Human Hair and Bones

    SciTech Connect

    Carvalho, M.L.; Marques, A.F.; Brito, J.

    2003-01-24

    This work is an application of synchrotron microprobe X- Ray fluorescence in order to study elemental distribution along human hair samples of contemporary citizens. Furthermore, X-Ray fluorescence spectrometry is also used to analyse human bones of different historical periods: Neolithic and contemporary subjects. The elemental content in the bones allowed us to conclude about environmental contamination, dietary habits and health status influence in the corresponding citizens. All samples were collected post-mortem. Quantitative analysis was performed for Mn, Fe, Co, Ni, Cu, Zn, Br, Rb, Sr and Pb. Mn and Fe concentration were much higher in bones from pre-historic periods. On the contrary, Pb bone concentrations of contemporary subjects are much higher than in pre-historical ones, reaching 100 {mu}g g-1, in some cases. Very low concentrations for Co, Ni, Br and Rb were found in all the analysed samples. Cu concentrations, allows to distinguish Chalcolithic bones from the Neolithic ones. The distribution of trace elements along human hair was studied for Pb and the obtained pattern was consistent with the theoretical model, based on the diffusion of this element from the root and along the hair. Therefore, the higher concentrations in hair for Pb of contemporary individuals were also observed in the bones of citizens of the same sampling sites. All samples were analysed directly without any chemical treatment.

  19. Spatial Imaging And Speciation of Lead in the Accumulator Plant Sedum Alfredii By Microscopically Focused Synchrotron X-Ray Investigation

    SciTech Connect

    Tian, S.; Lu, L.; Yang, X.; Webb, S.M.; Du, Y.; Brown, P.H.; /SLAC

    2012-08-23

    Sedum alfredii (Crassulaceae), a species native to China, has been characterized as a Zn/Cd cohyperaccumulator and Pb accumulator though the mechanisms of metal tolerance and accumulation are largely unknown. Here, the spatial distribution and speciation of Pb in tissues of the accumulator plant was investigated using synchrotron-based X-ray microfluorescence and powder Extended X-ray absorption fine structure (EXAFS) spectroscopy. Lead was predominantly restricted to the vascular bundles of both leaf and stem of the accumulator. Micro-XRF analysis revealed that Pb distributed predominantly within the areas of vascular bundles, and a positive correlation between the distribution patterns of S and Pb was observed. The dominant chemical form of Pb (>60%) in tissues of both accumulating (AE) and nonaccumulating ecotype (NAE) S. alfredii was similar to prepared Pb-cell wall compounds. However, the percentage of the Pb-cell wall complex is lower in the stem and leaf of AE, and a small amount of Pb appeared to be associated with SH-compounds. These results suggested a very low mobility of Pb out of vascular bundles, and that the metal is largely retained in the cell walls during transportation in plants of S. alfredii.

  20. Synchrotron X-ray micro-tomography imaging and analysis of wood degraded by Physisporinus vitreus and Xylaria longipes.

    PubMed

    Sedighi Gilani, Marjan; Boone, Matthieu N; Mader, Kevin; Schwarze, Francis Willis Mathew Robert

    2014-08-01

    Incubation of Norway spruce with Physisporinus vitreus and sycamore with Xylaria longipes results in reduction in density of these wood species that are traditionally used for the top and bottom plate of a violin, which follows by enhanced acoustic properties. We used Synchrotron X-ray micro-tomography, to study the three-dimensional structure of wood at the micro-scale level and the alterations of the density distribution after incubation with two white-rot fungi. Micro-tomography data from wood treated at different incubation periods are analyzed and compared with untreated (control) specimens to determine the wood density map and changes at the cell-wall level. Differences between the density of early- and latewood, xylem ray and around bordered pits in both Norway spruce and sycamore are studied. Three-dimensional hyphal networks of the P.vitreus and Xylaria longipes hyphae are visualized inside the cell lumina and their significance on the density of the early- and latewood cells after different incubation periods are discussed. The study illustrates the utility of X-ray micro-tomography for both qualitative and quantitative studies of a wide variety of biological systems and due to its high sensitivity, small structural changes can be quantified.