Science.gov

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. Synchrotron Radiation Total Reflection X-ray Fluorescence Spectroscopy for Microcontamination Analysis on Silicon Wafer Surfaces

    SciTech Connect

    Takaura, Norikatsu

    1997-10-01

    As dimensions in state-of-the-art CMOS devices shrink to less than 0.1 pm, even low levels of impurities on wafer surfaces can cause device degradation. Conventionally, metal contamination on wafer surfaces is measured using Total Reflection X-Ray Fluorescence Spectroscopy (TXRF). However, commercially available TXRF systems do not have the necessary sensitivity for measuring the lower levels of contamination required to develop new CMOS technologies. In an attempt to improve the sensitivity of TXRF, this research investigates Synchrotron Radiation TXRF (SR TXRF). The advantages of SR TXRF over conventional TXRF are higher incident photon flux, energy tunability, and linear polarization. We made use of these advantages to develop an optimized SR TXRF system at the Stanford Synchrotron Radiation Laboratory (SSRL). The results of measurements show that the Minimum Detection Limits (MDLs) of SR TXRF for 3-d transition metals are typically at a level-of 3x10{sup 8} atoms/cm{sup 2}, which is better than conventional TXRF by about a factor of 20. However, to use our SR TXRF system for practical applications, it was necessary to modify a commercially available Si (Li) detector which generates parasitic fluorescence signals. With the modified detector, we could achieve true MDLs of 3x10{sup 8} atoms/cm{sup 2} for 3-d transition metals. In addition, the analysis of Al on Si wafers is described. Al analysis is difficult because strong Si signals overlap the Al signals. In this work, the Si signals are greatly reduced by tuning the incident beam energy below the Si K edge. The results of our measurements show that the sensitivity for Al is limited by x-ray Raman scattering. Furthermore, we show the results of theoretical modeling of SR TXRF backgrounds consisting of the bremsstrahlung generated by photoelectrons, Compton scattering, and Raman scattering. To model these backgrounds, we extended conventional theoretical models by taking into account several aspects particular

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

    SciTech Connect

    E Mavredaki; A Neville; K Sorbie

    2011-12-31

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

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

    SciTech Connect

    Bu, Wei

    2009-01-01

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

  5. [Synchrotron studies of x-ray reflectivity from surfaces]. Technical progress report

    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.

  6. Larch: X-ray Analysis for Synchrotron Applications using Python

    NASA Astrophysics Data System (ADS)

    Newville, Matthew

    2017-03-01

    Larch is an open-source library and toolkit written in Python for processing and analyzing X-ray spectroscopic data. The primary emphasis is on X-ray spectroscopic and scattering data collected at modern synchrotron sources. Larch provides a wide selection of general-purpose processing, analysis, and visualization tools for processing X-ray data; its related target application areas include X-ray absorption fine structure (XAFS), micro-X-ray fluorescence (XRF) maps, quantitative X-ray fluorescence, X-ray absorption near edge spectroscopy (XANES), and X-ray standing waves and surface scattering. Larch provides a complete set of XAFS Analysis tools and has support for visualizing and analyzing XRF maps and spectra, and additional tools for X-ray spectral analysis, data handling, and general-purpose data modeling.

  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. CHARACTERIZATION OF SALT PARTICLE INDUCED CORROSION PROCESSES BY SYNCHROTRON GENERATED X-RAY FLUORESCENCE AND COMPLEMENTARY SURFACE ANALYSIS TOOLS.

    SciTech Connect

    NEUFELD, A.K.; COLE, I.S.; BOND, A.M.; ISAACS, H.S.; FURMAN, S.A.

    2001-03-25

    The benefits of using synchrotron-generated X-rays and X-ray fluorescence analysis in combination with other surface analysis techniques have been demonstrated. In studies of salt-induced corrosion, for example, the detection of Rb ions in the area of secondary spreading when salt-containing micro-droplets are placed on zinc surfaces, further supports a mechanism involving cation transport during the corrosion and spreading of corrosive salt on exposed metal surfaces. Specifically, the new analytical data shows that: (a) cations are transported radially from a primary drop formed from a salt deposit in a thin film of secondary spreading around the drop; (b) subsequently, micro-pools are formed in the area of secondary spreading, and it is likely that cations transported within the thin film accumulate in these micro-pools until the area is dehydrated; (c) the mechanism of cation transport into the area of secondary spreading does not include transport of the anions; and (d) hydroxide is the counter ion formed from oxygen reduction at the metal surface within the spreading layer. Data relevant to iron corrosion is also presented and the distinct differences relative to the zinc situation are discussed.

  9. 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.

  10. 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.

  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. X-ray reflectivity and surface roughness

    SciTech Connect

    Ocko, B.M.

    1988-01-01

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

  14. Fan-beam monochromatic x-ray CT using fluorescent x rays excited by synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Toyofuku, Fukai; Tokumori, Kenji; Kanda, Shigenobu; Higashida, Yoshiharu; Ohki, Masafumi; Cho, Tetsuji; Nishimura, Katsuyuki; Hyodo, Kazuyuki; Ando, Masami; Uyama, Chikao

    1999-10-01

    Monochromatic x-ray CT has several advantages over conventional CT, which utilizes bremsstrahlung white x-rays from an x-ray tube. Although various types of monochromatic x-ray CT systems using synchrotron radiation have been developed using a parallel x-ray beam for imaging of small samples with a high spatial resolution, imaging of large objects such as the human body have not been developed yet. We have developed a fan-beam monochromatic x-ray CT using fluorescent x-rays generated by irradiating metal targets by synchrotron radiation. A CdTe linear array detector of 512 mm sensitive width was used in the photon counting mode. We made phantom experiments using fluorescent x-rays ranging from 32 to 75 keV. Monochromatic x-ray CT images of a cylindrical lucite phantom filled with several contrast media have been obtained. Measured CT numbers are compared with linear attenuation coefficients, and they showed a good linearity over a wide range of contrast media concentrations.

  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. Application of pixel array detectors at x-ray synchrotrons.

    SciTech Connect

    Miceli, N.; X-Ray Science Division

    2009-03-01

    Pixel array detectors have only recently been seriously used at x-ray synchrotrons. We describe the application of a digital pixel array detector (Pilatus100k) to a variety of synchrotron experiments at the Advanced Photon Source at Argonne National Laboratory. The Pilatus100k was developed at the Paul Scherrer Institut (PSI). It has been commercialized by a PSI spinoff (Dectrics Ltd.) This is the first commercially available pixel array detector for x-ray synchrotron applications. The APS synchrotron provides tunable x-ray pulses with duration of {approx}80 ps and a repetition period of 153 ns (24-bunch mode). The Pilatus100k is a direct detection x-ray detector where each 172 micron pixel counts individual x-ray pulses above a lower threshold. It consists of {approx}100k pixels each of which is capable of single-photon counting (>3 keV) at count rates up to {approx}1 MHz. In addition, the Pilatus100k is an electronically gateable detector. We present data showing that the Pilatus100k is capable of isolating a single x-ray bunch at the APS in 24 bunch mode. We will also present a variety of different experiments exploiting the unique capabilities of the Pilatus100k.

  17. Synchrotron x-ray modification of nanoparticle superlattice formation

    NASA Astrophysics Data System (ADS)

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

    2012-09-01

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

  18. Dynamical diffraction imaging (topography) with X-ray synchrotron radiation

    NASA Technical Reports Server (NTRS)

    Kuriyama, M.; Steiner, B. W.; Dobbyn, R. C.

    1989-01-01

    By contrast to electron microscopy, which yields information on the location of features in small regions of materials, X-ray diffraction imaging can portray minute deviations from perfect crystalline order over larger areas. Synchrotron radiation-based X-ray optics technology uses a highly parallel incident beam to eliminate ambiguities in the interpretation of image details; scattering phenomena previously unobserved are now readily detected. Synchrotron diffraction imaging renders high-resolution, real-time, in situ observations of materials under pertinent environmental conditions possible.

  19. 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

  20. 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.

  1. Radiobiological studies using synchrotron-produced ultrasoft X-rays.

    PubMed

    Gould, M N; Nelms, B E; Hill, C K; Mackay, J F; Lindstrom, M J; Mackie, T R; Deluca, P M

    1999-12-01

    Ultrasoft X-rays have been extensively used to explore radiobiological mechanisms surrounding cell killing. These studies for the most part have been linked to a small number of X-ray energies. Recently, this field of study has been broadened by the availability of synchrotron-produced ultrasoft X-rays which can be produced at any desired energy. We have taken advantage of the University of Wisconsin Synchrotron to reexamine two fundamental radiobiological questions: Dose RBE vary with different ultrasoft X-ray energies? Dose the fraction of the nuclear volume exposed to equal total X-ray energy modify cell cytotoxicity? The first study focuses on the survival of Chinese hamster V79 and mouse C3H10T1/2 cells irradiated with synchrotron-produced 273 eV and 860 eV ultrasoft X-rays. These two energies, which are available by multilayer monochromatization of the synchrotron output spectrum, exhibit equal attenuation within living cells. Such an isoattenuating energy pair allows the direct examination of how biological effectiveness varies with the energy of the ultrasoft X-rays. In comparing survival results, we find similar biological effectiveness of these two energies for both the C3H10T1/2 and the V79 cells. These results are no consistent with previous findings of increasing RBE with decreasing ultrasoft X-ray energies. In addition, after correcting for mean nuclear based on measurements of cell thickness obtained with confocal microscopy, we find no significant differences in survival between the two ultrasoft X-ray energies and 250 kVp X-rays. These results suggest that RBE does not increase with decreasing energy of ultrasoft X-ray between 860 eV and 273 eV. In a second study we introduced an method which allows partial-volume irradiation of live cells using synchrotron-produced ultrasoft X-rays and micro-fabricated irradiation masks. The masks were made by X-ray lithography at the University of Wisconsin Synchrotron Radiation Center, and they consist of 1

  2. X-Ray microanalytical techniques based on synchrotron radiation.

    PubMed

    Snigireva, Irina; Snigirev, Anatoly

    2006-01-01

    The development of 3rd generation synchrotron radiation sources like European Synchrotron Radiation Facility (ESRF) in parallel with recent advances in the technology of X-ray microfocusing elements like Kirkpatrick-Baez (KB) mirrors, diffractive (Fresnel zone plates, FZP) and refractive (compound refractive lenses, CRL) optics, makes it possible to use X-ray microscopy techniques with high energy X-rays (energy superior to 4 keV). Spectroscopy, imaging, tomography and diffraction studies of samples with hard X-rays at micrometre and sub-micrometre spatial resolutions are now possible. The concept of combining these techniques as a high-energy microscopy has been proposed and successfully realized at the ESRF beamlines. Therefore a short summary of X-ray microscopy techniques is presented first. The main emphasis will be put on those methods which aim to produce sub-micron and nanometre resolution. These methods fall into three broad categories: reflective, refractive and diffractive optics. The basic principles and recent achievements will be discussed for all optical devices. Recent applications of synchrotron based microanalytical techniques to characterise radioactive fuel particles (UO(2)) released from the Chernobyl reactor are reported.

  3. Synchrotron X-ray tomographic microscopy of fossil embryos.

    PubMed

    Donoghue, Philip C J; Bengtson, Stefan; Dong, Xi-ping; Gostling, Neil J; Huldtgren, Therese; Cunningham, John A; Yin, Chongyu; Yue, Zhao; Peng, Fan; Stampanoni, Marco

    2006-08-10

    Fossilized embryos from the late Neoproterozoic and earliest Phanerozoic have caused much excitement because they preserve the earliest stages of embryology of animals that represent the initial diversification of metazoans. However, the potential of this material has not been fully realized because of reliance on traditional, non-destructive methods that allow analysis of exposed surfaces only, and destructive methods that preserve only a single two-dimensional view of the interior of the specimen. Here, we have applied synchrotron-radiation X-ray tomographic microscopy (SRXTM), obtaining complete three-dimensional recordings at submicrometre resolution. The embryos are preserved by early diagenetic impregnation and encrustation with calcium phosphate, and differences in X-ray attenuation provide information about the distribution of these two diagenetic phases. Three-dimensional visualization of blastomere arrangement and diagenetic cement in cleavage embryos resolves outstanding questions about their nature, including the identity of the columnar blastomeres. The anterior and posterior anatomy of embryos of the bilaterian worm-like Markuelia confirms its position as a scalidophoran, providing new insights into body-plan assembly among constituent phyla. The structure of the developing germ band in another bilaterian, Pseudooides, indicates a unique mode of germ-band development. SRXTM provides a method of non-invasive analysis that rivals the resolution achieved even by destructive methods, probing the very limits of fossilization and providing insight into embryology during the emergence of metazoan phyla.

  4. 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

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

    PubMed

    Hatsui, Takaki; Graafsma, Heinz

    2015-05-01

    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.

  6. 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.

  7. Hard X-ray Sources for the Mexican Synchrotron Project

    NASA Astrophysics Data System (ADS)

    Reyes-Herrera, Juan

    2016-10-01

    One of the principal tasks for the design of the Mexican synchrotron was to define the storage ring energy. The main criteria for choosing the energy come from studying the electromagnetic spectrum that can be obtained from the synchrotron, because the energy range of the spectrum that can be obtained will determine the applications available to the users of the future light source. Since there is a public demand of hard X-rays for the experiments in the synchrotron community users from Mexico, in this work we studied the emission spectra from some hard X-ray sources which could be the best options for the parameters of the present Mexican synchrotron design. The calculations of the flux and the brightness for one Bending Magnet and four Insertion Devices are presented; specifically, for a Superconducting Bending Magnet (SBM), a Superconducting Wiggler (SCW), an In Vacuum Short Period Undulator (IV-SPU), a Superconducting Undulator (SCU) and for a Cryogenic Permanent Magnet Undulator (CPMU). Two commonly available synchrotron radiation programs were used for the computation (XOP and SRW). From the results, it can be concluded that the particle beam energy from the current design is enough to have one or more sources of hard X-rays. Furthermore, a wide range of hard X-ray region can be covered by the analyzed sources, and the choice of each type should be based on the specific characteristics of the X-ray beam to perform the experiments at the involved beamline. This work was done within the project Fomix Conacyt-Morelos ”Plan Estrategico para la construccion y operación de un Sincrotron en Morelos” (224392).

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

    SciTech Connect

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

    1986-01-01

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

  9. SYNCHROTRON X-RAY BASED CHARACTERIZATION OF CDZNTE CRYSTALS

    SciTech Connect

    Duff, M

    2006-09-28

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

  10. An X-ray microprobe facility using synchrotron radiation.

    PubMed

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

    1990-01-01

    An X-ray microprobe for trace elemental analysis at micrometer spatial resolutions, using synchrotron radiation (SR), is under development. The facility consists of two beamlines, one including a 1:1 focusing mirror and the other an 8:1 ellipsoidal mirror. At present, "white light" is used for excitation of the characteristic X-ray fluorescence lines. Sensitivities in thin biological samples are in the range of 2-20 fg in 100 microns2 areas in 5 min irradiation times. Scanning techniques, as well as microtomography and chemical speciation, are discussed. Application to a specific biomedical study is included.

  11. An x-ray microprobe facility using synchrotron radiation

    SciTech Connect

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

    1989-01-01

    A x-ray microprobe for trace elemental analysis at micrometer spatial resolutions using synchrotron radiation (SR) is under development. The facility consists of two beamlines, one including a 1:1 focusing mirror and the other an 8:1 ellipsoidal mirror. At present ''white light''' is used for excitation of the characteristic x-ray fluorescence lines. Sensitivities in thin biological samples are in the range of 2-20 fg in 100 ..mu..m/sup 2/ areas in 5 min irradiation times. Scanning techniques as well as microtomography and chemical speciation are discussed. Application to a specific biomedical study is included. 13 refs., 2 figs.

  12. 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.

  13. Performance of the undulator based ultraviolet and soft x-ray beamline for catalysis and surface science at National Synchrotron Radiation Laboratory

    NASA Astrophysics Data System (ADS)

    Du, Liangliang; Du, Xuewei; Wei, Shen; Li, Chaoyang; Pan, Congyuan; Ju, Huanxin; Wang, Qiuping; Zhu, Junfa

    2016-12-01

    The undulator based ultraviolet and soft x-ray beamline BL11U for catalysis and surface science at National Synchrotron Radiation Laboratory (NSRL) has been under opteration for months and the present performance is described. This beamline utilizes radiation from an in-vacuum undulator, which has 30 magnetic periods with the period length of 40 mm. A varied-line-spacing plane grating monochromator is employed tto cover the photon energy region of 20-600 eV by two gratings with nominal groove densities of 400 llmm and 1200 l/mm respectively. The energy resolution power E/ΔE is measured with a gas ionization chamber and the photon flux is measured by a photodiode. Results show that the resolution power is better than 10,000 at a photon energy of 29.2 eV. And the flux is higher than 1×1010 phs/s under 300 mA ring beam current for most of the covered photon energy.

  14. 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.

  15. 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.

  16. Applications of Synchrotron X-Rays in Microelectronics Industry Research

    SciTech Connect

    Jordan-Sweet, J.

    2005-01-10

    The high flux and density of x-rays produced at synchrotrons provide the microelectronics industry with a powerful probe of the structure and behavior of a wide array of solid materials that are being developed for use in devices of the future. They also are of great use in determining why currently-used materials and processes sometimes fail. This paper describes the X20 x-ray beamline facility operated by IBM at the National Synchrotron Light Source, and presents a series of three industry challenges and results that illustrate the variety of techniques used and problems addressed. The value of this research ranges from solving short-term, technically-specific problems to increasing our academic understanding of materials in general. Techniques discussed include high-resolution diffraction, time-resolved diffraction, texture measurements, and grazing-incidence diffraction.

  17. 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)

  18. Requirements for X-ray structure analysis with modern synchrotron light sources

    NASA Astrophysics Data System (ADS)

    Laggner, Peter

    2000-11-01

    X-ray diffraction methods, including macromolecular crystallography, small-angle scattering from partly or noncrystalline systems, fiber and surface diffraction, are in the forefront of interest of a broad synchrotron user community from biomedical and technological fields. The main impact comes from the unsurpassed X-ray flux and brilliance of modern third-generation sources, facilitating on the one hand, a dramatic enhancement in sample throughput, and on the other hand, the transformation of X-ray diffraction analysis from a static to a cinematographic technique. In the present article some of the requirements for further development are being discussed.

  19. Synchrotron X-Ray Induced Gold Nanoparticle Formation

    SciTech Connect

    Yang, Y. C.; Wang, C. H.; Yang, T. Y.; Hwu, Y.; Chen, C. H.; Je, J. H.; Margaritondo, G.

    2007-01-19

    We reported a simple approach to generate gold nanoparticles from HAuCl4 containing aqueous solution by synchrotron x-ray irradiation at room temperature. The gold colloidal were investigated by a variety of characterization methods including Transmission Electron Microscope (TEM), Scanning Electron Microscope (SEM), Fourier transformation infrared (FTIR), Ultraviolet and Visible (UV-VIS) spectrometer and the effects of variables including pH value, radiation time were examined.

  20. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2012-02-01

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

  2. Applications of synchrotron X-rays to radiotherapy

    NASA Astrophysics Data System (ADS)

    Blattmann, H.; Gebbers, J.-O.; Bräuer-Krisch, E.; Bravin, A.; Le Duc, G.; Burkard, W.; Di Michiel, M.; Djonov, V.; Slatkin, D. N.; Stepanek, J.; Laissue, J. A.

    2005-08-01

    Radiotherapy is among the most useful treatments of cancer. Penetrating radiation (ionizing particles or bremsstrahlung photons) is aimed toward the tumor-bearing target, gradually delivering as high radiation to it as is usefully suppressive of tumor growth, yet tolerated by normal vital tissues inevitably irradiated with the tumor. The high collimation and dose rate of synchrotron X-ray beams, even when monochromatized, favor radiotherapy. Photon activation therapy, tomotherapy, microbeam radiation therapy, and radiosurgery mediated by synchrotron wigglers are conceptually promising for difficult tumors. Radiotherapy of malignant brain tumors in rats has been encouraging, but suitable beam lines exist at only a few research facilities and much basic work must be done before the promise of synchrotron-based radiotherapy can be realized clinically.

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

    SciTech Connect

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

    2012-05-17

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

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

    SciTech Connect

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

    2008-07-15

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

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

    PubMed

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

    2008-07-01

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

  6. 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.

  7. Pulsars, X-ray synchrotron nebulae, and guest stars

    NASA Technical Reports Server (NTRS)

    Seward, Frederick D.; Wang, Zhen-Ru

    1988-01-01

    X-ray observations of supernova remnants and radio pulsars are used to derive luminosities of neutron stars and synchrotron nebulae. Observations of known isolated pulsars are used to develop an empirical relationship between the X-ray luminosity and the rate of loss of rotational energy. This is used to derive the characteristics of pulsars hidden in remnants which show evidence for a central compact object or associated nebular emission, but no clear pulsed signal from the neutron star itself. Possible periods and period derivatives for the hidden pulsars are discussed. Some might have periods as long as 0.5 s, and period derivatives considerably higher than that of PSR 1509 - 58, currently the pulsar with the highest known period derivative.

  8. Pulsars, X-ray synchrotron nebulae, and guest stars

    NASA Technical Reports Server (NTRS)

    Seward, Frederick D.; Wang, Zhen-Ru

    1988-01-01

    X-ray observations of supernova remnants and radio pulsars are used to derive luminosities of neutron stars and synchrotron nebulae. Observations of known isolated pulsars are used to develop an empirical relationship between the X-ray luminosity and the rate of loss of rotational energy. This is used to derive the characteristics of pulsars hidden in remnants which show evidence for a central compact object or associated nebular emission, but no clear pulsed signal from the neutron star itself. Possible periods and period derivatives for the hidden pulsars are discussed. Some might have periods as long as 0.5 s, and period derivatives considerably higher than that of PSR 1509 - 58, currently the pulsar with the highest known period derivative.

  9. Synchrotron x-ray studies of Austenite and Bainitic ferrite

    SciTech Connect

    Stone, H.; Peet, M.; Bhadeshia, H. K. D. H.; Withers, P.; Babu, Sudarsanam S; Specht, Eliot D

    2008-01-01

    High resolution synchrotron X-ray diffraction has been used to conduct in situ studies of the temporal evolution of phases during the isothermal growth of bainite. Two populations of austenitic material were identified: one corresponding to the initial austenite, the other to the carbon-enriched austenite associated with the bainitic ferrite. The observed lattice parameters and the asymmetry of the peaks from the residual austenite have been interpreted in terms of the carbon partitioning during the transformation. The results are contrasted with an earlier study in which the austenite unit cell appeared to split into two distinct densities prior to the onset of transformation.

  10. Actinide science with soft x-ray synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Shuh, David K.

    2000-07-01

    The primary methods for the experimental investigation of actinide materials in the VUV/soft x-ray region are the complementary photoelectron spectroscopies, near-edge x-ray absorption fine structure (NEXAFS), and x-ray emission spectroscopy (XES) techniques. Resonant photoemission techniques capable of resolving the 5f electron contributions to actinide bonding along with angle-resolving measurements for band structure and surface structure determinations, have clear and immediate applications. Venerable angle-integrating core and valence band photoelectron spectroscopy are valuable for characterization and analytical purposes. Combined with results from NEXAFS measurements, these techniques will provide the information needed to develop improved understandings of the electronic structure of actinide materials and their surface chemistries/physics.

  11. Nuclear Transitions Induced by Synchrotron X-rays

    NASA Astrophysics Data System (ADS)

    Gemmell, Donald S.

    2003-01-01

    We discuss two rare but interesting processes by which synchrotron x-rays with energies up to about 100 keV may be used to induce nuclear transitions. In the NEET (Nuclear Excitation by Electronic Transition) process, an intense x-ray beam is employed to make vacancies, e.g. K-holes, in the atoms of a specific nuclear isotope. When a vacancy is filled by an electronic transition from a higher atomic level, there is some probability that instead of the usual x-ray or Auger emission, the nucleus of the atom itself will be excited. This is then followed by a nuclear decay exhibiting characteristic gamma-rays or other types of radiation, with time delays typical of the nuclear states involved. The probability for NEET increases when the energies of the atomic and the nuclear transitions become close. We address some theoretical aspects of the process and describe experimental efforts to observe it in 189Os and 197Au. The second process to be discussed is the possibility of "triggering" the decay of a nuclear isomer by irradiation with an x-ray beam. We focus on the case of the 31-year, 2.4-MeV, 16+ isomer of 178Hf. There has been speculation that if one could isolate gram quantities, say, of this isomer and then have the capability to accelerate its decay in a controlled way, one would have a powerful triggerable source of enormous energy. This could be used to generate explosions, for rapid irradiations, or for more general energy-storage applications, depending on the rate of energy release. We describe attempts to observe this process.

  12. Nuclear Transitions Induced by Synchrotron X-rays

    SciTech Connect

    Gemmell, Donald S.

    2003-01-24

    We discuss two rare but interesting processes by which synchrotron x-rays with energies up to about 100 keV may be used to induce nuclear transitions. In the NEET (Nuclear Excitation by Electronic Transition) process, an intense x-ray beam is employed to make vacancies, e.g. K-holes, in the atoms of a specific nuclear isotope. When a vacancy is filled by an electronic transition from a higher atomic level, there is some probability that instead of the usual x-ray or Auger emission, the nucleus of the atom itself will be excited. This is then followed by a nuclear decay exhibiting characteristic gamma-rays or other types of radiation, with time delays typical of the nuclear states involved. The probability for NEET increases when the energies of the atomic and the nuclear transitions become close. We address some theoretical aspects of the process and describe experimental efforts to observe it in 189Os and 197Au. The second process to be discussed is the possibility of 'triggering' the decay of a nuclear isomer by irradiation with an x-ray beam. We focus on the case of the 31-year, 2.4-MeV, 16+ isomer of 178Hf. There has been speculation that if one could isolate gram quantities, say, of this isomer and then have the capability to accelerate its decay in a controlled way, one would have a powerful triggerable source of enormous energy. This could be used to generate explosions, for rapid irradiations, or for more general energy-storage applications, depending on the rate of energy release. We describe attempts to observe this process.

  13. Evaluation of sagittal focusing for a spherical quartz crystal x-ray analyzer with synchrotron radiation

    SciTech Connect

    Pereira, Nino R.; Macrander, Albert T.; Hill, Kenneth W.; Baronova, Elena O.; George, Kevin M.; Kotick, Jordan T.

    2015-10-01

    To attain optimum performance in applications such as x-ray imaging and spectroscopy, a spherically bent crystal must diffract well across its entire surface. X-ray topography of sample crystals shows isolated regions where diffraction is problematic, even for a crystal where inspection with visible light does not suggest problems. Covering problem spots may improve the crystal’s focus and decrease the background. We explore the special properties of synchrotron radiation to examine typical spherical crystals from alpha-quartz, in a perpendicular geometry that is especially convenient to examine sagittal focusing.

  14. Picosecond x-ray diagnostics for third and fourth generation synchrotron sources

    SciTech Connect

    DeCamp, Matthew

    2016-03-30

    In the DOE-EPSCoR State/National Laboratory partnership grant ``Picosecond x-ray diagnostics for third and fourth generation synchrotron sources'' Dr. DeCamp set forth a partnership between the University of Delaware and Argonne National Laboratory. This proposal aimed to design and implement a series of experiments utilizing, or improving upon, existing time-domain hard x-ray spectroscopies at a third generation synchrotron source. Specifically, the PI put forth three experimental projects to be explored in the grant cycle: 1) implementing a picosecond ``x-ray Bragg switch'' using a laser excited nano-structured metallic film, 2) designing a robust x-ray optical delay stage for x-ray pump-probe studies at a hard x-ray synchrotron source, and 3) building/installing a laser based x-ray source at the Advanced Photon Source for two-color x-ray pump-probe studies.

  15. 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.

  16. Evaluation of RBC aggregation using synchrotron X-ray speckles

    NASA Astrophysics Data System (ADS)

    Ha, Hojin; Nam, Kwon-Ho; Lee, Sang Joon

    2010-11-01

    When a coherent beam illuminates spatially-disordered particles, speckles are usually generated by the inference of the scattered light waves. The speckle has been known to contain the information of the objects under near-field condition. In this study, we hypothesized that the speckle patterns of the red blood cells are related to the aggregation shape and the size of RBCs in the medium. The speckle patterns of RBCs in static condition were investigated by transmitting the monochromatic synchrotron X-ray beam to the sample with varying hematocrit(10-80 %) and medium type(phosphate buffered saline, autologous plasma and 0.75 % polyvinylpyrrolidone 360 in phosphate buffered saline). The temporal variation of speckle patterns after sudden removal of shear rate was observed by stopping the blood flow in a tube. The size of aggregated RBCs is closely correlated with the characteristic features of the speckle patterns.

  17. Development of an x-ray microprobe using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Thompson, Albert C.; Chapman, Karen L.; Underwood, James H.

    1993-01-01

    An X-ray microprobe is being built that will use a bending magnet port on the new Advanced Light Source (ALS) at the Lawrence Berkeley Laboratory. A pair of elliptical multi-layer mirrors will be used to focus and monochromatize the white radiation beam from the synchrotron. A beam spot size of 1 micrometers X 1 micrometers will be produced with a bandwidth of 1 keV at 10 keV. The energy of the beam will be variable from 3 keV to 12 keV. With a counting time of 30 sec it should be possible to simultaneously measure femtogram amounts of elements from potassium to zinc.

  18. In situ synchrotron x-ray photon beam characterization

    SciTech Connect

    Kyele, Nicholas R.; Silfhout, Roelof G. van; Manolopoulos, Spyros; Nikitenko, S.

    2007-03-15

    We have investigated two in situ methods of measuring x-ray beam parameters such as integrated intensity, position, and intensity distribution. These virtually transparent methods both rely on the collection of scattered radiation from a thin amorphous foil. The scattered radiation is collected by an active pixel sensor placed below the foil, well out of the direction of the beam path. These methods measure a cross-sectional image of the beam as opposed to a profile or beam centroid position provided by existing in situ detection methods. We present the results of measurements taken at a third generation synchrotron radiation source and provide analytical methods of deriving beam profile, position, and absolute intensity.

  19. Synchrotron X-ray diffraction for pyrolytic magnetic carbon

    NASA Astrophysics Data System (ADS)

    Kamishima, K.; Noda, T.; Kadonome, F.; Kakizaki, K.; Hiratsuka, N.

    We have prepared pyrolytic carbon samples from triethylamine and investigated their magnetic and crystallographic properties. The magnetic property depends on pyrolysis temperatures. A ferromagnetic sample with M=5×10-1 emu/g was obtained from the pyrolysis products even at room temperature. The synchrotron X-ray diffraction experiments were performed for the pyrolytic carbon samples in order to see the crystal structure of ferromagnetic samples. Diffraction peaks of iron or iron oxides were not observed for the ferromagnetic samples, whereas the major diffraction peak of the intermediate graphite-diamond (IGD) structure was clearly observed for ferromagnetic and nonmagnetic samples. Therefore, the IGD structure is not the direct cause of ferromagnetism. The ferromagnetism may be related to the graphite-like structure.

  20. Synchrotron x-ray study of multilayers in Laue geometry

    SciTech Connect

    Kang, H C; Stephenson, G B; Liu, C; Conley, R; Macrander, A T; Maser, J; Bajt, S; Chapman, H N

    2004-07-21

    Zone plates with depth to zone-width ratios as large as 100 are needed for focusing of hard x-rays. Such high aspect ratios are challenging to produce by lithography. We are investigating the fabrication of high-aspect-ratio linear zone plates by multilayer deposition followed by sectioning. As an initial step in this work, we present a synchrotron x-ray study of constant-period multilayers diffracting in Laue (transmission) geometry. Data are presented from two samples: a 200 period W/Si multilayer with d-spacing of 29 nm, and a 2020 period Mo/Si multilayer with d-spacing of 7 nm. By cutting and polishing we have successfully produced thin cross sections with section depths ranging from 2 to 12 {micro}m. Transverse scattering profiles (rocking curves) across the Bragg reflection exhibit well-defined interference fringes originating from the depth of the sample, in agreement with dynamical diffraction theory for a multilayer in Laue geometry.

  1. 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.

  2. 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.

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

    PubMed

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

    2012-07-01

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

  4. Comparison of different surface modification techniques for electrodes by means of electrochemistry and micro synchrotron radiation X-ray fluorescence. dimerization of cobalt(II) tetrasulfonated phthalocyanine and its influence on the electrodeposition on gold surfaces.

    PubMed

    Peeters, Karl; De Wael, Karolien; Vincze, Laszlo; Adriaens, Annemie

    2005-09-01

    This paper compares different electrochemical surface modification techniques with special attention to the immobilization of cobalt(II) tetrasulfonated phthalocyanine tetrasodium salt (Co(II)TSPc) on gold electrodes. Electrochemical and synchrotron radiation X-ray fluorescence (SR-XRF) microbeam analysis were performed in order to compare the amount of adsorbed CoTSPc onto the gold electrode and to determine the level of uniformity of the deposited layer. The nondestructive, quantitative characterization of CoTSPc deposition on gold electrodes by means of scanning SR-XRF on the microscopic scale has never been described before. The described methodology can be in general used for thin-film characterization. Depending on the degree of dimerization of the CoTSPc molecules, different electrochemical behavior is observed.

  5. 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).

  6. 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.

  7. 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.

  8. 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.

  9. Geoscience Applications of Synchrotron X-ray Computed Microtomography

    NASA Astrophysics Data System (ADS)

    Rivers, M. L.

    2009-05-01

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

  10. 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

  11. 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

  12. 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.

  13. 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.

  14. 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.

    1992-12-31

    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.

  15. 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.

  16. Investigating biomineralization using synchrotron based X-ray computed microtomography

    NASA Astrophysics Data System (ADS)

    Armstrong, Ryan; Ajo-Franklin, Jonathan

    2011-04-01

    This work presents the results of a study where synchrotron based x-ray computed microtomography (CMT) was used to investigate changes in pore morphology during calcium carbonate biomineralization. We simultaneously examine changes in pore microstructure and bulk permeability within glass bead columns during biogenic CaCO3 precipitation induced by Sporosarcina pasteurii. We observe a three order of magnitude reduction in permeability over relatively short time-scales (˜60 hrs) during the carbonate precipitation process. The resulting precipitates were a micro-porous composite of spherical and cubic CaCO3 precipitates. CMT images taken during precipitation were analyzed for effective pore radii, effective throat radii, and other pore-scale characteristics using 3DMA-ROCK. The Kozeny-Carman relation provided a poor fit to the raw permeability data, however, once this function was augmented with geometric information extracted from CMT imagery a better fit was provided suggesting that pore geometry should be considered temporally variable when modeling permeability change during biomineralization.

  17. 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.

  18. Investigating biomineralization using synchrotron based X-ray computed microtomography

    SciTech Connect

    Armstrong, Ryan; Ajo-Franklin, Jonathan

    2011-01-01

    This work presents the results of a study where synchrotron based x-ray computed microtomography (CMT) was used to investigate changes in pore morphology during calcium carbonate biomineralization. We simultaneously examine changes in pore microstructure and bulk permeability within glass bead columns during biogenic CaCO₃ precipitation induced by Sporosarcina pasteurii. We observe a three order of magnitude reduction in permeability over relatively short time-scales (~60 hrs) during the carbonate precipitation process. The resulting precipitates were a micro-porous composite of spherical and cubic CaCO₃ precipitates. CMT images taken during precipitation were analyzed for effective pore radii, effective throat radii, and other pore-scale characteristics using 3DMA-ROCK. The Kozeny-Carman relation provided a poor fit to the raw permeability data, however, once this function was augmented with geometric information extracted from CMT imagery a better fit was provided suggesting that pore geometry should be considered temporally variable when modeling permeability change during biomineralization.

  19. Fluorescent scanning x-ray tomography with synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Takeda, Tohoru; Maeda, Toshikazu; Yuasa, Tetsuya; Akatsuka, Takao; Ito, Tatsuo; Kishi, Kenichi; Wu, Jin; Kazama, Masahiro; Hyodo, Kazuyuki; Itai, Yuji

    1995-02-01

    Fluorescent scanning (FS) x-ray tomography was developed to detect nonradioactive tracer materials (iodine and gadolinium) in a living object. FS x-ray tomography consists of a silicon (111) channel cut monochromator, an x-ray shutter, an x-ray slit system and a collimator for detection, a scanning table for the target organ, and an x-ray detector with pure germanium. The minimal detectable dose of iodine in this experiment was 100 ng in a volume of 2 mm3 and a linear relationship was shown between the photon counts of a fluorescent x ray and the concentration of iodine contrast material. A FS x-ray tomographic image was clearly obtained with a phantom.

  20. SOLEIL shining on the solution-state structure of biomacromolecules by synchrotron X-ray footprinting at the Metrology beamline.

    PubMed

    Baud, A; Aymé, L; Gonnet, F; Salard, I; Gohon, Y; Jolivet, P; Brodolin, K; Da Silva, P; Giuliani, A; Sclavi, B; Chardot, T; Mercère, P; Roblin, P; Daniel, R

    2017-05-01

    Synchrotron X-ray footprinting complements the techniques commonly used to define the structure of molecules such as crystallography, small-angle X-ray scattering and nuclear magnetic resonance. It is remarkably useful in probing the structure and interactions of proteins with lipids, nucleic acids or with other proteins in solution, often better reflecting the in vivo state dynamics. To date, most X-ray footprinting studies have been carried out at the National Synchrotron Light Source, USA, and at the European Synchrotron Radiation Facility in Grenoble, France. This work presents X-ray footprinting of biomolecules performed for the first time at the X-ray Metrology beamline at the SOLEIL synchrotron radiation source. The installation at this beamline of a stopped-flow apparatus for sample delivery, an irradiation capillary and an automatic sample collector enabled the X-ray footprinting study of the structure of the soluble protein factor H (FH) from the human complement system as well as of the lipid-associated hydrophobic protein S3 oleosin from plant seed. Mass spectrometry analysis showed that the structural integrity of both proteins was not affected by the short exposition to the oxygen radicals produced during the irradiation. Irradiated molecules were subsequently analysed using high-resolution mass spectrometry to identify and locate oxidized amino acids. Moreover, the analyses of FH in its free state and in complex with complement C3b protein have allowed us to create a map of reactive solvent-exposed residues on the surface of FH and to observe the changes in oxidation of FH residues upon C3b binding. Studies of the solvent accessibility of the S3 oleosin show that X-ray footprinting offers also a unique approach to studying the structure of proteins embedded within membranes or lipid bodies. All the biomolecular applications reported herein demonstrate that the Metrology beamline at SOLEIL can be successfully used for synchrotron X-ray footprinting of

  1. Real time observation of mouse fetal skeleton using a high resolution X-ray synchrotron

    PubMed Central

    Chang, Dong Woo; Kim, Bora; Shin, Jae Hoon; Yun, Young Min; Je, Jung Ho; Hwu, Yeu kuang; Yoon, Jung Hee

    2011-01-01

    The X-ray synchrotron is quite different from conventional radiation sources. This technique may expand the capabilities of conventional radiology and be applied in novel manners for special cases. To evaluate the usefulness of X-ray synchrotron radiation systems for real time observations, mouse fetal skeleton development was monitored with a high resolution X-ray synchrotron. A non-monochromatized X-ray synchrotron (white beam, 5C1 beamline) was employed to observe the skeleton of mice under anesthesia at embryonic day (E)12, E14, E15, and E18. At the same time, conventional radiography and mammography were used to compare with X-ray synchrotron. After synchrotron radiation, each mouse was sacrificed and stained with Alizarin red S and Alcian blue to observe bony structures. Synchrotron radiation enabled us to view the mouse fetal skeleton beginning at gestation. Synchrotron radiation systems facilitate real time observations of the fetal skeleton with greater accuracy and magnification compared to mammography and conventional radiography. Our results show that X-ray synchrotron systems can be used to observe the fine structures of internal organs at high magnification. PMID:21586868

  2. In situ Monitoring of Synchrotron X-Ray-Induced Radiolysis Effects on Chromium Species Using X-Ray Absorption Spectroscopy

    NASA Astrophysics Data System (ADS)

    Men, S.; Anderson, A. J.; Mayanovic, R. A.

    2017-05-01

    Synchrotron X-ray radiolysis-induced redox in a chromium aqueous solution was monitored using in situ X-ray absorption spectroscopy. The radiolysis in the fluid sample within a specifically designed hydrothermal diamond anvil cell caused the oxidation of Cr(III) to Cr(VI) upon heating from room temperature to 400°C, and reduction of Cr(VI) to Cr(III) at 500°C. The two fitted components of the pre-edge features of the Cr K-edge spectra were used to identify the presence of Cr(VI) in the solution.

  3. Reaction of Water Vapor with alpha-Al203 and alpha-Fe203(0001) Surfaces: Synchrotron X-ray Photoemission Studies and Thermodynamic Calculations

    SciTech Connect

    Liu, Ping N.; Kendelewicz, Thomas; Brown, Gordon E.; Nelson, Eric J.; Chambers, Scott A. )

    1998-11-08

    X-ray photoemission experiments were carried out to study the reaction of water vapor with clean (0001) surfaces of single-crystal corundum (alpha-Al2O3) and single-crystal, thin-film hematite (alpha-Fe2O3) at constant reaction time (3 min) as a function of water vapor pressure[p(H2O)] and, in separate experiments, at longer reactions times(=30 min, with total exposure ranging from 1.8 L to 1.8 x 10 (10) L at constant p(H2)). A two-stage reaction was observed for each oxide surface, with dissociative chemisorption of water occurring mainly at defect sites below threshold pressures of {approx}1 Torr and {approx}10 (-4) Torr for the corundum and hematite (0001) surfaces, respectively. Extensive hydroxylation of these surfaces was found to occur above the respective threshold pressures. Longer exposures to water vapor below these threshold pressures did not result in increased hydroxylation; however, longer exposures above these threshold pressures resulted in increased hydroxylation, as expected. Th e threshold pressure of alpha-Al2O3 was accurately predicted using a simple equilibrium thermodynamic model for the conversion of corundum to gibbsite (Al(OH)3). In contrast, the measured threshold pressure for hematite is more than five orders of magnitude lower than the predicted threshold pressure for the conversion of hematite to FeOOH or Fe(OH)3. This difference between observation and prediction of hematite (0001) is not completely understood, but may be due to the presence of a passivating layer of Fe-hydroxide that reduces the surface energy of the hydroxylated hematite (0001).

  4. An x-ray microprobe using focussing optics with a synchrotron radiation source

    SciTech Connect

    Thompson, A.C.; Underwood, J.H.; Wu, Y.; Giauque, R.D.

    1989-01-01

    An x-ray microprobe can be used to produce maps of the concentration of elements in a sample. Synchrotron radiation provides x-ray beams with enough intensity and collimation to make possible elemental images with femtogram sensitivity. The use of focussing x-ray mirrors made from synthetic multilayers with a synchrotron x-ray beam allows beam spot sizes of less than 10 /mu/m /times/ 10 /mu/m to be produced. Since minimal sample preparation is required and a vacuum environment is not necessary, there will be a wide variety of applications for such microprobes. 8 refs., 6 figs.

  5. Synchrotron X-Ray Synthesized Gold Nanoparticles for Tumor Therapy

    SciTech Connect

    Chien, C. C.; Wang, C. H.; Tseng, P. Y.; Yang, T. Y.; Hua, T. E.; Hwu, Y.; Chen, Y. J.; Chung, K. H.; Je, J. H.; Margaritondo, G.

    2007-01-19

    Highly concentrated gold nanoparticles (20 {+-} 5 nm) were produced by an x-ray irradiation method. The particles were then examined for the interactions between gold and tumor cells under x-ray radiation conditions. The biological effects of gold nanoparticles were investigated in terms of the internalization, cytotoxicity and capability to enhance x-ray radiotherapy. The results of this investigation indicated that x-ray derived gold nanoparticles were nontoxic to CT-26 cell line and immobilized within cytoplasm. The irradiation experiments provided further evidence that gold nanoparticles were capable of enhancing the efficiency of radiotherapy.

  6. 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.

  7. 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.

  8. Total external reflection of X-rays from solid surfaces

    NASA Astrophysics Data System (ADS)

    Stozharov, V. M.

    2017-01-01

    The reflection of X-rays from solid surfaces is comprehensively studied using the measurements of patterns of total external reflection and X-ray diffraction with the aid of a parabolic mirror. Principles for theoretical processing of X-ray patterns are developed. An inverse dependence of the refractive index of X-ray radiation on the interplanar distances in crystallites is obtained.

  9. Synchrotron X-ray scattering studies of nanostructure-formation at interfaces

    NASA Astrophysics Data System (ADS)

    Sanyal, Milan K.

    2013-02-01

    We shall discuss results of a series of synchrotron x-ray scattering studies to understand the ordering of nanostructured materials formed at interfaces. In particular we shall discuss formation of germanium quantum-dots at the MBE grown silicon-germanium super-lattice structure and reversible crystallization of monolayer of Polyhedral Oligomeric SilSesquioxane (POSS) on water surface. The consistent analysis of the x-ray reflectivity and diffraction data collected in the Indian Beamline at Photon Factory Synchrotron, KEK, Japan have allowed determination of electron density and strain profile as a function of depth. The electron density profile obtained from the reflectivity and elemental profile obtained from SIMS measurements were effectively used to calculate diffraction data that provided strain and compositional profiles. The behaviour of amphiphilic Silsesquioxane POSS molecules under in-plane pressure in a Langmuir trough was studied at the ChemMatCARS, Sector 15, Advanced Photon Source, USA. We observe clear evidence of reversible crystallization of the POSS monolayers at the air-water interface - at higher pressure sharp diffraction spots are observed and as the pressure is withdrawn typical monolayer scattering comes back. Results of AFM studies of the lifted films in these two extreme phases were found to be consistent with the x-ray data.

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

    NASA Astrophysics Data System (ADS)

    Yamaguchi, A.; Okada, I.; Fukuoka, T.; Ishihara, M.; Sakurai, I.; Utsumi, Y.

    2016-09-01

    The synthesis and deposition of nanoparticles consisting of Cu and Au in a CuSO4 solution with some kinds of alcohol and electroplating solution containing gold (I) trisodium disulphite under synchrotron X-ray radiation was investigated. The functional group of alcohol plays an important in nucleation, growth and aggregation process of copper and cupric oxide particles. We found that the laboratory X-ray source also enables us to synthesize the NPs from the metallic solution. As increasing X-ray exposure time, the full length at half width of particle size distribution is broader and higher-order nanostructure containing NPs clusters is formed. The surface-enhanced Raman scattering (SERS) of 4, 4'-bipyridine (4bpy) in aqueous solution was measured using higher-order nanostructure immobilized on silicon substrates under systematically-varied X-ray exposure. This demonstration provide a clue to develop a three-dimensional printing and sensor for environmental analyses and molecular detection through simple SERS measurements.

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

    PubMed

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

    2016-01-01

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

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

    PubMed

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

    2013-06-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2013-06-01

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

  14. Silicon loss metrology using synchrotron x-ray reflectance and Bragg diffraction

    SciTech Connect

    Bhargava, Mansi; Wolfe, John C.; Donner, Wolfgang; Srivastava, Aseem

    2007-09-26

    We use synchrotron x-ray reflectometry and Bragg diffraction to study silicon loss in the low temperature plasma oxidation of silicon-on-insulator (SOI) wafers. We show that Laue oscillations associated with the Si (004) Bragg peak give the number of Si (004) planes in the device layer to within an experimental error of 0.07 nm and that X-ray reflectometry gives the total thickness of the device layer and the surface oxide to within 0.05 nm. We find that silicon loss in samples processed in two different plasma systems correspond to an increase in total thickness that is consistent with the formation of SiO{sub 2}.

  15. Synchrotron radiation-based x-ray reflection and scattering techniques for dimensional nanometrology

    NASA Astrophysics Data System (ADS)

    Krumrey, Michael; Gleber, Gudrun; Scholze, Frank; Wernecke, Jan

    2011-09-01

    Nanoobjects have at least one dimension in the range from 1 to 100 nm. Thus, if radiation is used for dimensional metrology, it should preferably have a wavelength in or below this range. For example, x-ray reflectometry (XRR) using x-ray tubes with Cu Kα radiation is widely used for layer thickness measurements with relative uncertainties of about 1%. By using different monochromator beamlines in the laboratory of PTB at the synchrotron radiation facility BESSY II, any x-ray wavelength from several nanometers down to about 0.1 nm can be selected for dimensional measurements in the nanometer range. Here, XRR is performed at wavelengths in the vicinity of an absorption edge of the chemical elements involved in order to enhance the contrast for layer systems like SiO2/Si which are difficult to resolve with Cu Kα radiation. By using longer wavelengths of around 2 nm, even an oxide layer and a thin carbonaceous contamination layer on a strongly curved spherical surface were separated, as required for measurements at 95 mm diameter silicon spheres within the international Avogadro project for the new definition of the kilogram. For nanoparticles in suspension, small angle x-ray scattering (SAXS) is the method of choice for dimensional metrology. This ensemble technique requires intense, monochromatic x-rays of low divergence. From the scattering pattern, the particle diameter and the size distribution are obtained. Moreover, the dimensional properties of nanostructured surfaces and nanoparticles on surfaces have been studied by grazing incidence SAXS (GISAXS), combining small angle scattering with the reflection geometry known from XRR. The diameters of gold nanoparticles obtained by SAXS and GISAXS are in very good agreement.

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

    NASA Astrophysics Data System (ADS)

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

    2013-02-01

    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 ˜50 ps x-ray pulse width convoluted with the ˜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.

  17. 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.

  18. Detecting element specific electrons from a single cobalt nanocluster with synchrotron x-ray scanning tunneling microscopy

    NASA Astrophysics Data System (ADS)

    Kersell, Heath; Shirato, Nozomi; Cummings, Marvin; Chang, Hao; Miller, Dean; Rosenmann, Daniel; Hla, Saw-Wai; Rose, Volker

    2017-09-01

    We use a nanofabricated scanning tunneling microscope tip as a detector to investigate local X-ray induced tunneling and electron emission from a single cobalt nanocluster on a Au(111) surface. The tip-detector is positioned a few angstroms above the nanocluster, and ramping the incident X-ray energy across the Co photoabsorption K-edge enables the detection of element specific electrons. Atomic-scale spatial dependent changes in the X-ray absorption cross section are directly measured by taking the X-ray induced current as a function of X-ray energy. From the measured sample and tip currents, element specific X-ray induced current components can be separated and thereby the corresponding yields for the X-ray induced processes of the single cobalt nanocluster can be determined. The detection of element specific synchrotron X-ray induced electrons of a single nanocluster opens an avenue for materials characterization on a one particle at-a-time basis.

  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 microtomography at Shanghai Synchrotron Radiation facility

    NASA Astrophysics Data System (ADS)

    Chen, Rongchang; Xie, Honglan; Deng, Biao; Du, Guohao; Ren, Yuqi; Wang, Yudan; Zhou, Guangzhao; Tan, Hai; Yang, Yiming; Xu, Liang; Hu, Tao; Li, Qiao; Feng, Binggang; Wang, Feixiang; Xiao, Tiqiao

    2016-10-01

    BL13W, an X-ray imaging beamline has been built and opened to users since May 6, 2009. More than 70 user proposals per year are granted and implemented at the beamline, with about 500 user visits/year. Up to now, X-ray microtomography (XMCT) is the dominated method for BL13W user operation, more than 70% user experiments were carried out with XMCT, covering the research fields in material science, biomedicine, physics, environmental science, archaeology and paleontology. To meet the user requirements, micro-CT imaging methods based on a variety of contrast mechanisms, including absorption, phase contrast, X-ray fluorescence, have been developed. Algorithms and related software have been developed achieve the low dose and fast data collection. Quantitative analysis to the three dimensional CT images is highly emphasized and related software for 3D information extraction with high precision and high efficiency, has been developed. Three-dimensional structure evolution has been attracting more and more attention in many scientific research fields. Two-Hertz dynamic phase contrast CT based on monochromatic SR beam was established at SSRF. The limitation of fluorescence X-ray CT from practical applications is the data-collection efficiency. The ordered-subsets expectation maximization algorithm was inducted to improve practicability of X-ray fluorescence computed tomography (XFCT), greatly. A scheme for full field XFCT was also proposed.

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

    PubMed

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

    2015-05-05

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

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

    PubMed Central

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

    2015-01-01

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

  3. First in-flight synchrotron X-ray absorption and photoemission study of carbon soot nanoparticles

    NASA Astrophysics Data System (ADS)

    Ouf, F.-X.; Parent, P.; Laffon, C.; Marhaba, I.; Ferry, D.; Marcillaud, B.; Antonsson, E.; Benkoula, S.; Liu, X.-J.; Nicolas, C.; Robert, E.; Patanen, M.; Barreda, F.-A.; Sublemontier, O.; Coppalle, A.; Yon, J.; Miserque, F.; Mostefaoui, T.; Regier, T. Z.; Mitchell, J.-B. A.; Miron, C.

    2016-11-01

    Many studies have been conducted on the environmental impacts of combustion generated aerosols. Due to their complex composition and morphology, their chemical reactivity is not well understood and new developments of analysis methods are needed. We report the first demonstration of in-flight X-ray based characterizations of freshly emitted soot particles, which is of paramount importance for understanding the role of one of the main anthropogenic particulate contributors to global climate change. Soot particles, produced by a burner for several air-to-fuel ratios, were injected through an aerodynamic lens, focusing them to a region where they interacted with synchrotron radiation. X-ray photoelectron spectroscopy and carbon K-edge near-edge X-ray absorption spectroscopy were performed and compared to those obtained for supported samples. A good agreement is found between these samples, although slight oxidation is observed for supported samples. Our experiments demonstrate that NEXAFS characterization of supported samples provides relevant information on soot composition, with limited effects of contamination or ageing under ambient storage conditions. The highly surface sensitive XPS experiments of airborne soot indicate that the oxidation is different at the surface as compared to the bulk probed by NEXAFS. We also report changes in soot’s work function obtained at different combustion conditions.

  4. First in-flight synchrotron X-ray absorption and photoemission study of carbon soot nanoparticles.

    PubMed

    Ouf, F-X; Parent, P; Laffon, C; Marhaba, I; Ferry, D; Marcillaud, B; Antonsson, E; Benkoula, S; Liu, X-J; Nicolas, C; Robert, E; Patanen, M; Barreda, F-A; Sublemontier, O; Coppalle, A; Yon, J; Miserque, F; Mostefaoui, T; Regier, T Z; Mitchell, J-B A; Miron, C

    2016-11-24

    Many studies have been conducted on the environmental impacts of combustion generated aerosols. Due to their complex composition and morphology, their chemical reactivity is not well understood and new developments of analysis methods are needed. We report the first demonstration of in-flight X-ray based characterizations of freshly emitted soot particles, which is of paramount importance for understanding the role of one of the main anthropogenic particulate contributors to global climate change. Soot particles, produced by a burner for several air-to-fuel ratios, were injected through an aerodynamic lens, focusing them to a region where they interacted with synchrotron radiation. X-ray photoelectron spectroscopy and carbon K-edge near-edge X-ray absorption spectroscopy were performed and compared to those obtained for supported samples. A good agreement is found between these samples, although slight oxidation is observed for supported samples. Our experiments demonstrate that NEXAFS characterization of supported samples provides relevant information on soot composition, with limited effects of contamination or ageing under ambient storage conditions. The highly surface sensitive XPS experiments of airborne soot indicate that the oxidation is different at the surface as compared to the bulk probed by NEXAFS. We also report changes in soot's work function obtained at different combustion conditions.

  5. First in-flight synchrotron X-ray absorption and photoemission study of carbon soot nanoparticles

    PubMed Central

    Ouf, F.-X.; Parent, P.; Laffon, C.; Marhaba, I.; Ferry, D.; Marcillaud, B.; Antonsson, E.; Benkoula, S.; Liu, X.-J.; Nicolas, C.; Robert, E.; Patanen, M.; Barreda, F.-A.; Sublemontier, O.; Coppalle, A.; Yon, J.; Miserque, F.; Mostefaoui, T.; Regier, T. Z.; Mitchell, J.-B. A.; Miron, C.

    2016-01-01

    Many studies have been conducted on the environmental impacts of combustion generated aerosols. Due to their complex composition and morphology, their chemical reactivity is not well understood and new developments of analysis methods are needed. We report the first demonstration of in-flight X-ray based characterizations of freshly emitted soot particles, which is of paramount importance for understanding the role of one of the main anthropogenic particulate contributors to global climate change. Soot particles, produced by a burner for several air-to-fuel ratios, were injected through an aerodynamic lens, focusing them to a region where they interacted with synchrotron radiation. X-ray photoelectron spectroscopy and carbon K-edge near-edge X-ray absorption spectroscopy were performed and compared to those obtained for supported samples. A good agreement is found between these samples, although slight oxidation is observed for supported samples. Our experiments demonstrate that NEXAFS characterization of supported samples provides relevant information on soot composition, with limited effects of contamination or ageing under ambient storage conditions. The highly surface sensitive XPS experiments of airborne soot indicate that the oxidation is different at the surface as compared to the bulk probed by NEXAFS. We also report changes in soot’s work function obtained at different combustion conditions. PMID:27883014

  6. 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.

  7. X-ray synchrotron dual energy imaging for material specific study

    NASA Astrophysics Data System (ADS)

    Singh, B.; Agrawal, A. K.; Kashyap, Y. S.; Gadkari, S. C.

    2017-05-01

    X-ray imaging techniques, in general, are used to study the internal structures of an object non-destructively such as anatomy, imperfections, cracks and voids whereas insensitive to spatial distribution of different element or elemental compositions of the object. With the development of advance bright X-ray synchrotron sources and accurate energy tunability using high resolution crystal monochromator, detection of elemental distribution in an object became possible. Quantitative small concentrations with enhance contrast can be detected fast in X-ray synchrotron based dual energy imaging, in comparison to conventional X-ray lab based techniques. We report here the experimental setup, image acquisition and image processing for the dual energy X-ray imaging (DEI) technique to retrieve the spatial distribution of different elements in the object.

  8. 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.

  9. 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.

  10. A tunable X-ray microprobe using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Wu, Y.; Thompson, A. C.; Underwood, J. H.; Giauque, R. D.; Chapman, K.; Rivers, M. L.; Jones, K. W.

    1990-05-01

    We describe an X-ray microprobe using multilayer mirrors. Previously, we have demonstrated a Kirkpatrick-Baez type focusing system working at both 8 and 10 keV and successfully applied it to a variety of applications, including the determination of elemental contents in fluid inclusions. In this paper, we show that the usable excitation energy for this microprobe is not restricted to between 8 and 10 keV, and furthermore that it can be simply tuned in operation. A 10 keV X-ray fluorescence microprobe can be used to measure the concentration of the elements from K ( Z = 19) to Zn ( Z = 30) using K X-ray lines, and from Cd ( Z = 48) to Er ( Z = 68) using L X-ray lines. There are a number of geologically important elements in the gap between Ga ( Z = 31) and Ag ( Z = 47) and with Z > 68. In order to cover this range, a higher excitation energy is required. On the other hand, for samples that contain major elements with absorption edges lower than the excitation energy, it would be hard to detect other minor elements because of the strong signal from the major elements and the background they produce. In this case, a tunable X-ray source can be used to avoid the excitation of the major elements. We demonstrate that, with the existing setup, it is possible to tune the excitation energy from 6 to 14 keV. In this range, the intensity does not decrease by more than one order of magnitude. As an illustrative example, a geological sample was examined using two different excitation energies to show the advantage of a tunable source. Finally, we discuss the possibility of further extension of the excitation energy range as well as the possibility of improving the intensity.

  11. A tunable x ray microprobe using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Wu, Y.; Thompson, A. C.; Underwood, J. H.; Giauque, R. D.; Chapman, K.; Rivers, M. L.; Jones, K. W.

    1989-08-01

    We describe an x ray microprobe using multilayer mirrors. Previously, we had demonstrated a Kirkpatrick-Baez type focusing system working at both 8 and 10 keV and successfully applied it to a variety of applications, including the determination of elemental contents in fluid inclusions. In this paper, we show that the usable excitation energy for this microprobe is not restricted to between 8 and 10 keV, and furthermore, it can be simply tuned in operation. A 10-keV x ray fluorescence microprobe can be used to measure the concentration of the elements from potassium (Z = 19) to zinc (Z = 30) using K x ray lines, and from cadmium (Z = 48) to erbium (Z = 68) using L x-ray lines. There are a number of geologically important elements in the gap between gallium (Z = 31) and silver (Z = 47) and also with Z greater than 68. In order to cover this range, a higher excitation energy is required. On the other hand, for samples that contain major elements with absorption edges lower than the excitation energy, it would be hard to detect other mirror elements because of the strong signal from the major elements and the background they produce. In this case, a tunable x ray source can be used to avoid the excitation of the major elements. We demonstrate that, with the existing setup, it is possible to tune the excitation energy from 6 keV to 14 keV, in this range, the intensity does not decrease by more than one order of magnitude. As an illustration, a geological sample was examined by using two different excitation energies to show the advantage of a tunable source. Finally, we discuss the possibility of further extension of the excitation energy range as well as the possibility of improving the intensity.

  12. Determination of impurities in graphite using synchrotron radiation based X-ray fluorescence spectrometry.

    PubMed

    Ghosh, M; Swain, K K; Remya Devi, P S; Chavan, T A; Singh, A K; Tiwari, M K; Verma, R

    2017-10-01

    Determination of impurities namely Ca, Mn, Fe, Ni, Zn, Sr and Pb in graphite by energy dispersive X-ray fluorescence spectrometry is described using microfocused synchrotron radiation. The internal standard and standard addition methodologies were adopted for quantification and the results were compared with tube-based X-ray fluorescence spectrometry. Analysis of the results by the F and t-tests revealed their statistical equivalence. Synchrotron measurements improved the detection limits by an order of magnitude compared to the tube based technique. Cr and Zr, which were below the quantification limit in tube based technique, were also quantified by synchrotron based technique. Copyright © 2017 Elsevier Ltd. All rights reserved.

  13. Microstructural investigation to the controlled release kinetics of monolith osmotic pump tablets via synchrotron radiation X-ray microtomography.

    PubMed

    Li, Haiyan; Yin, Xianzhen; Ji, Junqiu; Sun, Lixin; Shao, Qun; York, Peter; Xiao, Tiqiao; He, You; Zhang, Jiwen

    2012-05-10

    Tomographic imaging techniques are attractive tools for the visualization of the internal structural characteristics of pharmaceutical solid dosage forms. In this paper, the internal structure of the tablet core for a monolith osmotic drug delivery system, felodipine sustained-release tablet, was visualized via synchrotron radiation X-ray computed microtomography during the drug release process. The surface areas and three dimensional parameters of the tablet core were calculated based on the three dimensional reconstruction of the images. At different stages of the drug release process, the surface morphology, the hydration, the swelling, and the structure changing of the tablet, were visualized from the two dimensional monochrome X-ray images. The three dimensional volumes of the remaining tablet core correlated well with the percentages of felodipine (R=0.9988). Also, the three dimensional surface area almost unchanged during the drug release process, which clearly demonstrated the intrinsic drug release mechanism of the osmotic drug delivery system. In conclusion, the synchrotron radiation X-ray computed microtomography, with rapid acquisition, high intensity and micro-scale spatial resolution, was found to be a useful tool for the quantitative elucidation of the intrinsic drug release kinetics and the three dimensional parameters such as surface areas of the remained core obtained by the synchrotron radiation. Thus, X-ray computed microtomography can be considered as a new and complimentary analytical tool to standard compendial pharmaceutical tests for quality control of osmotic drug delivery systems.

  14. X-Ray Structure determination of the Glycine Cleavage System Protein H of Mycobacterium tuberculosis Using An Inverse Compton Synchrotron X-Ray Source

    PubMed Central

    Abendroth, Jan; McCormick, Michael S.; Edwards, Thomas E.; Staker, Bart; Loewen, Roderick; Gifford, Martin; Rifkin, Jeff; Mayer, Chad; Guo, Wenjin; Zhang, Yang; Myler, Peter; Kelley, Angela; Analau, Erwin; Hewitt, Stephen Nakazawa; Napuli, Alberto J.; Kuhn, Peter; Ruth, Ronald D.; Stewart, Lance J.

    2010-01-01

    Structural genomics discovery projects require ready access to both X-ray and NMR instrumentation which support the collection of experimental data needed to solve large numbers of novel protein structures. The most productive X-ray crystal structure determination laboratories make extensive frequent use of tunable synchrotron X-ray light to solve novel structures by anomalous diffraction methods. This requires that frozen cryo-protected crystals be shipped to large government-run synchrotron facilities for data collection. In an effort to eliminate the need to ship crystals for data collection, we have developed the first laboratory-scale synchrotron light source capable of performing many of the state-of-the-art synchrotron applications in X-ray science. This Compact Light Source is a first-in-class device that uses inverse Compton scattering to generate X-rays of sufficient flux, tunable wavelength and beam size to allow high-resolution X-ray diffraction data collection from protein crystals. We report on benchmarking tests of X-ray diffraction data collection with hen egg white lysozyme, and the successful high-resolution X-ray structure determination of the Glycine cleavage system protein H from Mycobacterium tuberculosis using diffraction data collected with the Compact Light Source X-ray beam. PMID:20364333

  15. 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.

  16. 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.

  17. 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.

  18. 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

  19. 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.

  20. Synchrotron x-ray study of a Fibonacci superlattice

    SciTech Connect

    Todd, J.; Merlin, R.; Clarke, R.; Mohanty, K.M.; Axe, J.D.

    1986-09-01

    Quasiperiodic ordering is studied in a GaAs-AlAs Fibonacci superlattice by high-resolution x-ray scattering. The data are consistent with the predicted dense set of diffraction vectors. Moderately large growth fluctuations in the sequential deposition of GaAs and AlAs layers do not appear to disturb seriously the quasiperiodic order. The effects of randomness are analyzed in a computer simulation.

  1. 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.

  2. 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.

  3. Synchronizing fast electrically driven phenomena with synchrotron x-ray probes

    SciTech Connect

    Grigoriev, Alexei; Do, D.-H.; Evans, Paul G.; Adams, Bernhard; Landahl, Eric; Dufresne, Eric M.

    2007-02-15

    Time scales of long-range physical processes in solids are typically in the range of picoseconds to nanoseconds. These times are commensurate with the time resolution of structural probes based on modern synchrotron x-ray sources. Several processes of technological and scientific interest can be driven by applied electric fields, but synchronizing electrically driven phenomena with an x-ray probe poses a technical challenge. We describe the synchronization of a well-defined number of fast electrical pulses with the time structure of synchrotron x rays to probe the dynamics of thin films and nanostructures. This synchronization technique yields x-ray transient signals with 600 ps transitions in ferroelectric thin films, with a contribution of approximately 320 ps due to timing jitter in the synchronization.

  4. X-ray analog pixel array detector for single synchrotron bunch time-resolved imaging.

    PubMed

    Koerner, Lucas J; Gruner, Sol M

    2011-03-01

    Dynamic X-ray studies can reach temporal resolutions limited by only the X-ray pulse duration if the detector is fast enough to segregate synchrotron pulses. An analog integrating pixel array detector with in-pixel storage and temporal resolution of around 150 ns, sufficient to isolate pulses, is presented. Analog integration minimizes count-rate limitations and in-pixel storage captures successive pulses. Fundamental tests of noise and linearity as well as high-speed laser measurements are shown. The detector resolved individual bunch trains at the Cornell High Energy Synchrotron Source at levels of up to 3.7 × 10(3) X-rays per pixel per train. When applied to turn-by-turn X-ray beam characterization, single-shot intensity measurements were made with a repeatability of 0.4% and horizontal oscillations of the positron cloud were detected.

  5. X-ray analog pixel array detector for single synchrotron bunch time-resolved imaging

    PubMed Central

    Koerner, Lucas J.; Gruner, Sol M.

    2011-01-01

    Dynamic X-ray studies can reach temporal resolutions limited by only the X-ray pulse duration if the detector is fast enough to segregate synchrotron pulses. An analog integrating pixel array detector with in-pixel storage and temporal resolution of around 150 ns, sufficient to isolate pulses, is presented. Analog integration minimizes count-rate limitations and in-pixel storage captures successive pulses. Fundamental tests of noise and linearity as well as high-speed laser measurements are shown. The detector resolved individual bunch trains at the Cornell High Energy Synchrotron Source at levels of up to 3.7 × 103 X-rays per pixel per train. When applied to turn-by-turn X-ray beam characterization, single-shot intensity measurements were made with a repeatability of 0.4% and horizontal oscillations of the positron cloud were detected. PMID:21335901

  6. 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.

  7. Characterization of cadmium accumulation in willow as a woody metal accumulator using synchrotron radiation-based X-ray microanalyses.

    PubMed

    Harada, Emiko; Hokura, Akiko; Takada, Saori; Baba, Kei'ichi; Terada, Yasuko; Nakai, Izumi; Yazaki, Kazufumi

    2010-05-01

    Trees that accumulate metals are important plants for restoring contaminated soil because of their high biomass. We examined the cadmium (Cd) tolerance and growth rate of six willow (Salix) species common in Japan. To characterize in detail the localization of Cd and its ligands, synchrotron radiation-based micro X-ray fluorescence analysis was used. This revealed the accumulation of cadmium at the tips of the serrations in leaves, and the phellogen and/or the phelloderm under the stem surface. micro-X-ray absorption near edge structure spectra of Cd in all the accumulation sites were similar to that of the Cd ion coordinated by O ligands in S. gilgiana.

  8. Model experiment of in vivo synchrotron X-ray diffraction of human kidney stones

    NASA Astrophysics Data System (ADS)

    Ancharov, A. I.; Potapov, S. S.; Moiseenko, T. N.; Feofilov, I. V.; Nizovskii, A. I.

    2007-05-01

    The diffraction of synchrotron radiation (SR) was used to explore the phase composition of kidney stones placed into a specific object phantom, which imitated the human body. As an imitation of the patient breath, the kidney stone was moved vertically and rotated to an angle of 15° during the recording of the X-ray pattern. It was shown that rotation and displacement did not distort the X-ray pattern.

  9. Flowing CO2 in a fractured shale: effect of flow, fluid chemistry, and proppant on the evolution of the surfaces, as monitored by in situ synchrotron X-ray microtomograph

    NASA Astrophysics Data System (ADS)

    Voltolini, M.; Ajo Franklin, J. B.; Yang, L.

    2016-12-01

    A better understanding of the evolution of fractures during the flow of CO2-rich fluids in shales is crucial in many fields. We will focus on two specific situations: a fractured sealing rock in a CO2 capture scenario, and a propped fracture aimed at unconventional oil recovery stimulated with the injection of CO2. We decided to monitor the evolution of a fractured Niobrara oil shale, using in-situ synchrotron X-ray microtomography in order to obtain information of the phenomena at the micron scale, under three different experimental settings, mimicking realistic flow and pressure conditions in the subsurface: 1) Unpropped fracture and slow flow of CO2-saturated water. 2) Propped fracture and flow of liquid CO2 in a water-saturated sample. 3) Propped fracture and fast flow of CO2-saturated water. The three different cases show three markedly different evolutions of the surface of the fracture, with phenomena such as wormholing, generation of leached layer, proppant protecting the surface from dissolution at the contact points (see figure), etc. These observations provide important hints about the evolution of the fractured shales at different conditions, as well as a starting point and a validation dataset for theoretical models.

  10. 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.

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

    SciTech Connect

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

    2016-01-28

    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.

  12. High-speed X-ray phase imaging and X-ray phase tomography with Talbot interferometer and white synchrotron radiation.

    PubMed

    Momose, Atsushi; Yashiro, Wataru; Maikusa, Hirohide; Takeda, Yoshihiro

    2009-07-20

    X-ray Talbot interferometry, which uses two transmission gratings, has the advantage that broad energy bandwidth x-rays can be used. We demonstrate the use of white synchrotron radiation for high-speed X-ray phase imaging and tomography in combination with an X-ray Talbot interferometer. The moiré fringe visibility over 20% was attained, enabling quantitative phase measurement. X-ray phase images with a frame rate of 500 f/s and an X-ray phase tomogram with a scan time of 0.5 s were obtained successfully. This result suggests a breakthrough for time-resolved three-dimensional observation of objects that weakly absorb X-rays, such as soft material and biological objects.

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

    SciTech Connect

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

    1986-01-01

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

  14. Roles of oxidative stress in synchrotron radiation X-ray-induced testicular damage of rodents

    PubMed Central

    Ma, Yingxin; Nie, Hui; Sheng, Caibin; Chen, Heyu; Wang, Ban; Liu, Tengyuan; Shao, Jiaxiang; He, Xin; Zhang, Tingting; Zheng, Chaobo; Xia, Weiliang; Ying, Weihai

    2012-01-01

    Synchrotron radiation (SR) X-ray has characteristic properties such as coherence and high photon flux, which has excellent potential for its applications in medical imaging and cancer treatment. However, there is little information regarding the mechanisms underlying the damaging effects of SR X-ray on biological tissues. Oxidative stress plays an important role in the tissue damage induced by conventional X-ray, while the role of oxidative stress in the tissue injury induced by SR X-ray remains unknown. In this study we used the male gonads of rats as a model to study the roles of oxidative stress in SR X-ray-induced tissue damage. Exposures of the testes to SR X-ray at various radiation doses did not significantly increase the lipid peroxidation of the tissues, assessed at one day after the irradiation. No significant decreases in the levels of GSH or total antioxidation capacity were found in the SR X-ray-irradiated testes. However, the SR X-ray at 40 Gy induced a marked increase in phosphorylated H2AX – a marker of double-strand DNA damage, which was significantly decreased by the antioxidant N-acetyl cysteine (NAC). NAC also attenuated the SR X-ray-induced decreases in the cell layer number of seminiferous tubules. Collectively, our observations have provided the first characterization of SR X-ray-induced oxidative damage of biological tissues: SR X-ray at high doses can induce DNA damage and certain tissue damage during the acute phase of the irradiation, at least partially by generating oxidative stress. However, SR X-ray of various radiation doses did not increase lipid peroxidation. PMID:22837810

  15. Gas scintillation proportional counters for x-ray synchrotron applications

    SciTech Connect

    Smith, A. ); Bavdaz, M. )

    1992-01-01

    Gas scintillation proportional counters (GSPCs) as x-ray detectors provide some advantages and disadvantages compared with proportional counters. In this paper the various configurations of xenon filled GSPC are described including both imaging and nonimaging devices. It is intended that this work be used to configure a GSPC for a particular application and predict its general performance characteristics. The general principles of operation are described and the performance characteristics are then separately considered. A high performance, imaging, driftless GSPC is described in which a single intermediate window is used between the PMT and gas cell.

  16. Developments in gas detectors for synchrotron x-ray radiation

    SciTech Connect

    Fischer, J.; Radeka, V.; Smith, G.C.

    1985-09-01

    New results on the physical limitations to position resolution in gas detectors for x-rays (approx. =3 to 20 keV) due to the range of photoelectrons and Auger electrons are discussed. These results were obtained with a small gap detector in which position readout was accomplished by using a very low noise centroid finding technique. A description is given of position sensitive detectors for medium rates (a few x 10/sup 5/ photons per second), using delay line readout, and for very high rates (approx. =10/sup 8/ photons per second), using fast signal shaping on the output of each anode wire.

  17. 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.

  18. Synchrotron X-ray PIV Technique for Measurement of Blood Flow Velocity

    SciTech Connect

    Kim, Guk Bae; Lee, Sang Joon; Je, Jung Ho

    2007-01-19

    Synchrotron X-ray micro-imaging method has been used to observe internal structures of various organisms, industrial devices, and so on. However, it is not suitable to see internal flows inside a structure because tracers typically employed in conventional optical flow visualization methods cannot be detectable with the X-ray micro-imaging method. On the other hand, a PIV (particle image velocimetry) method which has recently been accepted as a reliable quantitative flow visualization technique can extract lots of flow information by applying digital image processing techniques However, it is not applicable to opaque fluids such as blood. In this study, we combined the PIV method and the synchrotron X-ray micro-imaging technique to compose a new X-ray PIV technique. Using the X-ray PIV technique, we investigated the optical characteristics of blood for a coherent synchrotron X-ray beam and quantitatively visualized real blood flows inside an opaque tube without any contrast media. The velocity field information acquired would be helpful for investigating hemorheologic characteristics of the blood flow.

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

    SciTech Connect

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

    2003-01-16

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

  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. 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.

  2. 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.

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

    PubMed

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

    2014-12-10

    Carbon and silicon materials are two of the most important materials involved in the history of the science and technology development. In the last two decades, C and Si nanoscale materials, e.g., carbon nanotubes, graphene, and silicon nanowires, and quantum dots, have also emerged as the most interesting nanomaterials in nanoscience and nanotechnology for their myriad promising applications such as for electronics, sensors, biotechnology, etc. In particular, carbon and silicon nanostructures are being utilized in energy-related applications such as catalysis, batteries, solar cells, etc., with significant advances. Understanding of the nature of surface and electronic structures of nanostructures plays a key role in the development and improvement of energy conversion and storage nanosystems. Synchrotron soft X-ray absorption spectroscopy (XAS) and related techniques, such as X-ray emission spectroscopy (XES) and scanning transmission X-ray microscopy (STXM), show unique capability in revealing the surface and electronic structures of C and Si nanomaterials. In this review, XAS is demonstrated as a powerful technique for probing chemical bonding, the electronic structure, and the surface chemistry of carbon and silicon nanomaterials, which can greatly enhance the fundamental understanding and also applicability of these nanomaterials in energy applications. The focus is on the unique advantages of XAS as a complementary tool to conventional microscopy and spectroscopy for effectively providing chemical and structural information about carbon and silicon nanostructures. The employment of XAS for in situ, real-time study of property evolution of C and Si nanostructures to elucidate the mechanisms in energy conversion or storage processes is also discussed. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Thermal, structural, and fabrication aspects of diamond windows for high power synchrotron x-ray beamlines

    SciTech Connect

    Khounsary, A.M. ); Phillips, W. )

    1992-01-01

    Recent advances in chemical vapor deposition (CVD) technology have made it possible to produce thin free-standing diamond foils that can be used as the window material in high heat load, synchrotron beamlines. Numerical simulations suggest that these windows can offer an attractive and at times the only altemative to beryllium windows for use in third generation x-ray synchrotron radiation beamlines. Utilization, design, and fabrication aspects of diamond windows for high heat load x-ray beamlines are discussed, as are the microstructure characteristics bearing on diamond's performance in this role. Analytic and numerical results are also presented to provide a basis for the design and testing of such windows.

  5. 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.

  6. 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.

  7. 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.

  8. 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

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

    PubMed

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

    2014-05-01

    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. 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. 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 3.9%. The good agreement of

  10. Crystal spectroscopy of X-ray synchrotron source brightness

    NASA Astrophysics Data System (ADS)

    Als-Nielsen, Jens; Kjaer, Kristian

    1992-12-01

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

  11. 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

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

    PubMed Central

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

    2016-01-01

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

  13. Intermetallic phase detection in lead-free solders using synchrotron x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Jackson, Gavin J.; Lu, Hua; Durairaj, Raj; Hoo, Nick; Bailey, Chris; Ekere, Ndy N.; Wright, Jon

    2004-12-01

    The high-intensity, high-resolution x-ray source at the European Synchrotron Radiation Facility (ESRF) has been used in x-ray diffraction (XRD) experiments to detect intermetallic compounds (IMCs) in lead-free solder bumps. The IMCs found in 95.5Sn3.8Ag0.7Cu solder bumps on Cu pads with electroplated-nickel immersion-gold (ENIG) surface finish are consistent with results based on traditional destructive methods. Moreover, after positive identification of the IMCs from the diffraction data, spatial distribution plots over the entire bump were obtained. These spatial distributions for selected intermetallic phases display the layer thickness and confirm the locations of the IMCs. For isothermally aged solder samples, results have shown that much thicker layers of IMCs have grown from the pad interface into the bulk of the solder. Additionally, the XRD technique has also been used in a temperature-resolved mode to observe the formation of IMCs, in situ, during the solidification of the solder joint. The results demonstrate that the XRD technique is very attractive as it allows for nondestructive investigations to be performed on expensive state-of-the-art electronic components, thereby allowing new, lead-free materials to be fully characterized.

  14. 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.

  15. 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.

  16. Development rate of PMMA exposed to synchrotron x-ray radiation for LIGA applications

    NASA Astrophysics Data System (ADS)

    McNamara, Shamus

    2011-01-01

    This paper investigates the development rate of poly(methyl methacrylate) (PMMA) after it is exposed to synchrotron x-ray radiation. The x-ray exposures were performed at both Synchrotron Radiation Center and Brookhaven National Laboratories. The development rate of PMMA in a variety of developers was measured as a function of absorbed x-ray dose (J cm-3). The development rate of four different types of PMMA was investigated: unexposed 950k PMMA, Cryo GMS PMMA, Goodfellow CQ PMMA, and Crosslinked PMMA. It was found that the development rate is the same for all types of PMMA studied. The temperature dependence of one developer, GG developer, was studied in detail and it is shown that the selectivity of exposed to unexposed PMMA increases as the temperature is reduced. This work was performed in part at the University of Wisconsin.

  17. Recent advances in synchrotron-based hard x-ray phase contrast imaging

    NASA Astrophysics Data System (ADS)

    Liu, Y.; Nelson, J.; Holzner, C.; Andrews, J. C.; Pianetta, P.

    2013-12-01

    Ever since the first demonstration of phase contrast imaging (PCI) in the 1930s by Frits Zernike, people have realized the significant advantage of phase contrast over conventional absorption-based imaging in terms of sensitivity to ‘transparent’ features within specimens. Thus, x-ray phase contrast imaging (XPCI) holds great potential in studies of soft biological tissues, typically containing low Z elements such as C, H, O and N. Particularly when synchrotron hard x-rays are employed, the favourable brightness, energy tunability, monochromatic characteristics and penetration depth have dramatically enhanced the quality and variety of XPCI methods, which permit detection of the phase shift associated with 3D geometry of relatively large samples in a non-destructive manner. In this paper, we review recent advances in several synchrotron-based hard x-ray XPCI methods. Challenges and key factors in methodological development are discussed, and biological and medical applications are presented.

  18. Photosynthesis and structure of electroless Ni-P films by synchrotron x-ray irradiation

    SciTech Connect

    Hsu, P.-C.; Wang, C.-H.; Yang, T.-Y.; Hwu, Y.-K.; Lin, C.-S.; Chen, C.-H.; Chang, L.-W.; Seol, S.-K.; Je, J.-H.; Margaritondo, G.

    2007-05-15

    The authors describe an electroless deposition method for thin films, based on the irradiation by an x-ray beam emitted by a synchrotron source. Specifically, Ni-P films were deposited at room temperature. This synthesis is a unique combination of photochemical and electrochemical processes. The influence of the pH value on the formation and structural properties of the films was examined by various characterization tools including scanning electron microscopy, x-ray diffraction, and x-ray absorption spectroscopy. Real time monitoring of the deposition process by coherent x-ray microscopy reveals that the formation of hydrogen bubbles leads to a self-catalysis effect without a preexisting catalyst. The mechanisms underlying the deposition process are discussed in details.

  19. Progress Towards A Dedicated Synchrotron Radiation Source For Ultrafast X-Ray Science

    NASA Astrophysics Data System (ADS)

    Lidia, Steve

    2002-03-01

    We present progress towards the design 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.

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

    SciTech Connect

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

    2001-10-26

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

  1. Hard X-ray nanofocusing at low-emittance synchrotron radiation sources

    PubMed Central

    Schroer, Christian G.; Falkenberg, Gerald

    2014-01-01

    X-ray scanning microscopy relies on intensive nanobeams generated by imaging a highly brilliant synchrotron radiation source onto the sample with a nanofocusing X-ray optic. Here, using a Gaussian model for the central cone of an undulator source, the nanobeam generated by refractive X-ray lenses is modeled in terms of size, flux and coherence. The beam properties are expressed in terms of the emittances of the storage ring and the lateral sizes of the electron beam. Optimal source parameters are calculated to obtain efficient and diffraction-limited nanofocusing. With decreasing emittance, the usable fraction of the beam for diffraction-limited nanofocusing experiments can be increased by more than two orders of magnitude compared with modern storage ring sources. For a diffraction-limited storage ring, nearly the whole beam can be focused, making these sources highly attractive for X-ray scanning microscopy. PMID:25177988

  2. 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.

  3. 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.

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

    SciTech Connect

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

    1987-01-01

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

  5. 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

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

    PubMed

    Withers, P J

    2015-03-06

    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.

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

    DOE PAGES

    Jach, Terrence; Bakulin, Alex S.; Durbin, Stephen M.; ...

    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).

  8. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2007-02-01

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

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

    PubMed Central

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

    2015-01-01

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

  11. 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.

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

    DOE PAGES

    Mukhopadhyay, D.; Walko, D. A.; Jung, I. W.; ...

    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

  13. 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.

  14. 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.

  15. X-Ray Exposure of Electron-Deposited Photoresist for Conformal Lithography on Corrugated Surfaces

    NASA Technical Reports Server (NTRS)

    Hartley, F.; Malek, C.; Nguyen, S.

    1998-01-01

    Proximity printing using synchrotron X-ray lithography provides high resolution pattern transfer with large depth of field, low diffraction effects and no reflection from the substrate. Electro-plating of photo-resist allows deposition of thin, uniform films over geometrically complex and topographically diverse, electrically conductive surfaces.

  16. 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.

  17. 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.

  18. Pore-scale evaporation-condensation dynamics resolved by synchrotron x-ray tomography

    NASA Astrophysics Data System (ADS)

    Shahraeeni, Ebrahim; Or, Dani

    2012-01-01

    Capillary processes greatly influence vapor mediated transport dynamics and associated changes in liquid phase content of porous media. Rapid x-ray synchrotron tomography measurements were used to resolve liquid-vapor interfacial dynamics during evaporation and condensation within submillimetric pores forming between sintered glass bead samples subjected to controlled ambient temperature and relative humidity. Evolution of gas-liquid interfacial shapes were in agreement with predictions based on our analytical model for interfacial dynamics in confined wedge-shaped pores. We also compared literature experimental data at the nanoscale to illustrate the capability of our model to describe early stages of condensation giving rise to the onset of capillary forces between rough surfaces. The study provides high resolution, synchrotron-based observations of capillary evaporation-condensation dynamics at the pore scale as the confirmation of the pore scale analytical model for capillary condensation in a pore and enables direct links with evolution of macroscopic vapor gradients within a sintered glass bead sample through their effect on configuration and evolution of the local interfaces. Rapid condensation processes play a critical role in the onset of capillary-induced friction affecting mechanical behavior of physical systems and industrial applications.

  19. 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.

  20. Synchrotron x-ray imaging of acoustic cavitation bubbles induced by acoustic excitation

    NASA Astrophysics Data System (ADS)

    Jung, Sung Yong; Park, Han Wook; Park, Sung Ho; Lee, Sang Joon

    2017-04-01

    The cavitation induced by acoustic excitation has been widely applied in various biomedical applications because cavitation bubbles can enhance the exchanges of mass and energy. In order to minimize the hazardous effects of the induced cavitation, it is essential to understand the spatial distribution of cavitation bubbles. The spatial distribution of cavitation bubbles visualized by the synchrotron x-ray imaging technique is compared to that obtained with a conventional x-ray tube. Cavitation bubbles with high density in the region close to the tip of the probe are visualized using the synchrotron x-ray imaging technique, however, the spatial distribution of cavitation bubbles in the whole ultrasound field is not detected. In this study, the effects of the ultrasound power of acoustic excitation and working medium on the shape and density of the induced cavitation bubbles are examined. As a result, the synchrotron x-ray imaging technique is useful for visualizing spatial distributions of cavitation bubbles, and it could be used for optimizing the operation conditions of acoustic cavitation.

  1. 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.

  2. 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.

  3. 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.

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

    DOE PAGES

    Cordes, Nikolaus L.; Henderson, Kevin; Stannard, Tyler; ...

    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.

  5. 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.

  6. 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.

  7. Focusing synchrotron radiation using a polycapillary half-focusing X-ray lens for imaging.

    PubMed

    Sun, Tianxi; Zhang, Meiling; Liu, Zhiguo; Zhang, Zhiguang; Li, Gang; Ma, Yongzhong; Du, Xiaoguang; Jia, Quanjie; Chen, Yu; Yuan, Qingxi; Huang, Wanxia; Zhu, Peiping; Ding, Xunliang

    2009-01-01

    An imaging system based on a polycapillary half-focusing X-ray lens (PHFXRL) and synchrotron radiation source has been designed. The focal spot size and the gain in power density of the PHFXRL were 22 microm (FWHM) and 4648, respectively, at 14.0 keV. The spatial resolution of this new imaging system was better than 5 microm when an X-ray charge coupled device with a pixel size of 10.9 x 10.9 microm was used. A fossil of an ancient biological specimen was imaged using this system.

  8. Diamond anvil cell radial x-ray diffraction program at the National Synchrotron Light Source.

    PubMed

    Hu, J Z; Mao, H K; Shu, J F; Guo, Q Z; Liu, H Z

    2006-06-28

    During the past decade, the radial x-ray diffraction method using a diamond anvil cell (DAC) has been developed at the X17C beamline of the National Synchrotron Light Source. The detailed experimental procedure used with energy dispersive x-ray diffraction is described. The advantages and limitations of using the energy dispersive method for DAC radial diffraction studies are also discussed. The results for FeO at 135 GPa and other radial diffraction experiments performed at X17C are discussed in this report.

  9. 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.

  10. 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.

  11. Spatial resolution of synchrotron x-ray microtomography in high energy range: Effect of x-ray energy and sample-to-detector distance

    NASA Astrophysics Data System (ADS)

    Seo, D.; Tomizato, F.; Toda, H.; Uesugi, K.; Takeuchi, A.; Suzuki, Y.; Kobayashi, M.

    2012-12-01

    Spatial resolution of three-dimensional images obtained by synchrotron X-ray microtomography technique is evaluated using cyclic bar patterns machined on a steel wire. Influences of X-ray energy and the sample-to-detector distance on spatial resolution were investigated. High X-ray energies of 33-78 keV are applied due to the high X-ray absorption of transition metals. Best spatial resolution of about 1.2 μm pitch was observed at the sample-to-detector distance range of 20-110 mm and at the energy range of 68-78 keV. Several factors such as X-ray scattering and diffraction phenomena affecting the degradation of spatial resolution are also discussed.

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

    PubMed Central

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

    2015-01-01

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

  13. X-ray grating interferometer for imaging at a second-generation synchrotron radiation source

    NASA Astrophysics Data System (ADS)

    Herzen, Julia; Beckmann, Felix; Donath, Tilman; Ogurreck, Malte; David, Christian; Pfeiffer, Franz; Mohr, Jürgen; Reznikova, Elena; Riekehr, Stefan; Haibel, Astrid; Schulz, Georg; Müller, Bert; Schreyer, Andreas

    2010-09-01

    X-ray phase-contrast radiography and tomography enables to increase contrast for weakly absorbing materials. Recently, x-ray grating interferometers were developed which extend the possibility of phase-contrast imaging from highly brilliant radiation sources like third-generation synchrotron even to non-coherent sources. Here, we present a setup of an x-ray grating interferometer designed and installed at low-coherence wiggler source at the GKSS beamline W2 (HARWI II) operated at the second-generation synchrotron storage ring DORIS at the Deutsches Elektronen-Synchrotron (DESY, Hamburg, Germany). The beamline is dedicated to imaging in materials science. Equipped with the grating interferometer, it is the first synchrotron radiation beamline with a three-grating setup combining the advantages of phase-contrast imaging with monochromatic radiation with very high flux and a sufficiently large field of view for centimeter sized objects. Examples of radiography on laser-welded aluminum and magnesium joints are presented to demonstrate the high potential of the new gratingbased setup in the field of materials science. In addition, the results of an off-axis phase-contrast tomography of a human urethra with 15 mm in diameter are presented showing internal structures, which cannot be resolved by the conventional tomography in absorption mode.

  14. Synchrotron X-ray Analytical Techniques for Studying Materials Electrochemistry in Rechargeable Batteries

    DOE PAGES

    Lin, Feng; Liu, Yijin; Yu, Xiqian; ...

    2017-08-30

    Rechargeable battery technologies have ignited major breakthroughs in contemporary society, including but not limited to revolutions in transportation, electronics, and grid energy storage. The remarkable development of rechargeable batteries is largely attributed to in-depth efforts to improve battery electrode and electrolyte materials. There are, however, still intimidating challenges of lower cost, longer cycle and calendar life, higher energy density, and better safety for large scale energy storage and vehicular applications. Further progress with rechargeable batteries may require new chemistries (lithium ion batteries and beyond) and better understanding of materials electrochemistry in the various battery technologies. In the past decade, advancementmore » of battery materials has been complemented by new analytical techniques that are capable of probing battery chemistries at various length and time scales. Synchrotron X-ray techniques stand out as one of the most effective methods that allows for nearly nondestructive probing of materials characteristics such as electronic and geometric structures with various depth sensitivities through spectroscopy, scattering, and imaging capabilities. This article begins with the discussion of various rechargeable batteries and associated important scientific questions in the field, followed by a review of synchrotron X-ray based analytical tools (scattering, spectroscopy and imaging) and their successful applications (ex situ, in situ, and in operando) in gaining fundamental insights into these scientific questions. Furthermore, electron microscopy and spectroscopy complement the detection length scales of synchrotron X-ray tools, and are also discussed towards the end. We highlight the importance of studying battery materials by combining analytical techniques with complementary length sensitivities, such as the combination of X-ray absorption spectroscopy and electron spectroscopy with spatial resolution

  15. Verneuil corundum: an integrated PBC and white beam synchrotron radiation X-ray topography analysis

    NASA Astrophysics Data System (ADS)

    Rinaudo, C.; Orione, P.; Causà, M.

    2002-09-01

    In order to give a deeper insight into the cracking of the Verneuil corundum boules, several samples of different colors and from different industrial sources have been analyzed by means of white beam synchrotron radiation X-ray diffraction topography (WB-SR-XRDT) and PBC analysis (Hartman and Perdock theory). The cracking occurs along an irregular surface containing the elongation axis of boules, and the WB-SR-XRDT analysis shows that this surface is nearly parallel to the { 1 2¯ 0 } crystallographic planes. Following Hartman and Perdock theory, these planes form F-planes with a high density of PBC directions: 3 PBC directions—[2 1 1], [2 1 0] and [ 4¯ 2¯ 1 ]—have been recognized as parallel to the 1 2¯0 plane. The 1¯02 planes that are normal to the cracking surface of boules are F-planes too, but they show a lower bond density per unit area with respect to the 1 2¯0 planes. Ab initio calculations show that these planes have lower surface energies with respect to other hk0 planes, such as {1 0 0} and {0 1 0}.

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

    NASA Technical Reports Server (NTRS)

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

    1985-01-01

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

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

    NASA Technical Reports Server (NTRS)

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

    1985-01-01

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

  18. 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.

  19. 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.

  20. A SYNCHROTRON SELF-COMPTON-DISK REPROCESSING MODEL FOR OPTICAL/X-RAY CORRELATION IN BLACK HOLE X-RAY BINARIES

    SciTech Connect

    Veledina, Alexandra; Poutanen, Juri; Vurm, Indrek E-mail: juri.poutanen@oulu.fi

    2011-08-10

    The physical picture of the emission mechanisms operating in the X-ray binaries was put under question by the simultaneous optical/X-ray observations with high time resolution. The light curves of the two energy bands appeared to be connected and the cross-correlation functions observed in three black hole binaries exhibited a complicated shape. They show a dip of the optical emission a few seconds before the X-ray peak and the optical flare just after the X-ray peak. This behavior could not be explained in terms of standard optical emission candidates (e.g., emission from the cold accretion disk or a jet). We propose a novel model, which explains the broadband optical to the X-ray spectra and the variability properties. We suggest that the optical emission consists of two components: synchrotron radiation from the non-thermal electrons in the hot accretion flow and the emission produced by reprocessing of the X-rays in the outer part of the accretion disk. The first component is anti-correlated with the X-rays, while the second one is correlated, but delayed and smeared relative to the X-rays. The interplay of the components explains the complex shape of the cross-correlation function, the features in the optical power spectral density as well as the time lags.

  1. 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.

  2. 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.

  3. Thermal, structural, and fabrication aspects of diamond windows for high power synchrotron x-ray beamlines

    SciTech Connect

    Khounsary, A.M.; Phillips, W.

    1992-12-01

    Recent advances in chemical vapor deposition (CVD) technology have made it possible to produce thin free-standing diamond foils that can be used as the window material in high heat load, synchrotron beamlines. Numerical simulations suggest that these windows can offer an attractive and at times the only altemative to beryllium windows for use in third generation x-ray synchrotron radiation beamlines. Utilization, design, and fabrication aspects of diamond windows for high heat load x-ray beamlines are discussed, as are the microstructure characteristics bearing on diamond`s performance in this role. Analytic and numerical results are also presented to provide a basis for the design and testing of such windows.

  4. 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

  5. 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.

  6. 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.

  7. Use of multielement detector systems with synchrotron x-ray sources

    SciTech Connect

    Thompson, A.C.

    1981-07-01

    The extremely high intensity and pulsed structure of synchrotron radiation x-ray sources put very demanding requirements on associated x-ray detectors. In current detector systems, trade-offs must be made between the efficiency, energy resolution, counting rate capability and the spatial resolution. Two detector systems are described which illustrate the optimization of these parameters for different applications of synchrotron radiation. One system is a segmented 16 channel multiwire proportional chamber which is used for fluorescent EXAFS measurements. The other is a 30 element Si(Li) linear detector array which is used for digital angiography experiments. The characteristics of these systems are discussed and recent results obtained with them are presented.

  8. 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.

  9. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2010-07-01

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

  11. 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.

  12. A multichannel cryogenic detector system for synchrotron-based x-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Friedrich, S.; Niedermayr, T.; Funk, T.; Drury, O.; van den Berg, M. L.; Cunningham, M. F.; Ullom, J. N.; Loshak, A.; Cramer, S. P.; Frank, M.; Labov, S. E.

    2002-02-01

    Fluorescence-detected x-ray absorption spectroscopy probes the fine structure of electronic energy levels with sub-eV resolution by scanning a monochromatic synchrotron beam through the corresponding absorption edge and measuring the intensity of the resulting x-ray fluorescence. For dilute samples, grating spectrometers lack the detection efficiency and conventional Si(Li) or Ge detectors often lack the energy resolution to separate the weak fluorescence signal from strong nearby emission lines. We have built a high-resolution, high-efficiency cryogenic detector system for synchrotron-based soft x-ray spectroscopy. The sensor is a 3×3 array of 200 μm×200 μm superconducting Nb-Al-AlOx-Al-Nb tunnel junctions with an energy resolution of ~15 eV below 1 keV and a total count rate capability of ~100,000 counts/second. This sensor array is cooled to below 0.4 K by a two-stage adiabatic demagnetization refrigerator while held at the end of a 40-cm-long cold finger that can be inserted into a UHV sample chamber for x-ray fluorescence measurements. We present absorption spectra of dilute compounds (~1000 ppm) and will discuss spectrometer performance with respect to the analysis of metalloproteins. .

  13. X-ray Bragg diffraction from langasite crystal modulated by surface acoustic wave

    NASA Astrophysics Data System (ADS)

    Roshchupkin, D. V.; Irzhak, D. V.; Tucoulou, R.; Buzanov, O. A.

    2003-11-01

    X-ray diffraction on the X cut of a langasite crystal (La3Ga5SiO14) modulated by a Λ=12 μm Rayleigh surface acoustic wave (SAW) has been studied at the ESRF synchrotron radiation source. Due to the sinusoidal modulation of the crystal lattice involved by the SAW diffraction satellites appear on the rocking curve, with their number, angular positions, and intensities depending on the amplitude and wavelength of the ultrasonic superlattice. Full extinction of a specific satellite could be performed by adjusting the acoustic amplitude. It is shown that x-ray diffraction can be used to study surface acoustic wave field distributions in crystals.

  14. 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.

  15. Examination for optimization of synchrotron radiation spectrum for the x ray depth lithography

    NASA Astrophysics Data System (ADS)

    Dany, Raimund

    1992-06-01

    The effect of reducing the vertical distribution of synchrotron radiation on its spectral distribution is examined through resin irradiation. The resulting filter effect is compared to that of absorption filters. Transmission coefficients of titanium, gold, and polyamide were calculated from linear absorption coefficients with the Beer law. The use of a diaphragm in X-ray depth lithography, which is the first step of the LIGA (Lithography Galvanoforming Molding) process, is discussed. A calorimetric device for determining the synchrotron radiation power and distribution was developed and tested. Measurements at the ELSA storage ring show a strong dependence of the vertical emittance on the electron current.

  16. 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.

  17. Understanding the instrumental profile of synchrotron radiation X-ray powder diffraction beamlines.

    PubMed

    Rebuffi, Luca; Sánchez Del Río, Manuel; Busetto, Edoardo; Scardi, Paolo

    2017-05-01

    A Monte Carlo algorithm has been developed to calculate the instrumental profile function of a powder diffraction synchrotron beamline. Realistic models of all optical elements are implemented in a ray-tracing software. The proposed approach and the emerging paradigm have been investigated and verified for several existing X-ray powder diffraction beamlines. The results, which can be extended to further facilities, show a new and general way of assessing the contribution of instrumental broadening to synchrotron radiation data, based on ab initio simulations.

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

    PubMed

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

    2016-11-01

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

  19. 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.

  20. Dosimetry and Radiobiology of Synchrotron-Produced Ultrasoft X-Rays

    NASA Astrophysics Data System (ADS)

    Meger, Carol Mary

    Ultrasoft X-rays provide a unique tool to study the mechanism of radiation damage in biological systems. Experimenters have used X-ray tubes with titanium, copper, silver, magnesium, aluminum and carbon targets to generate characteristic X-rays of these materials to irradiate a variety of mammalian cell lines. Limitations in the photon intensity and the available energies from X-ray tube sources prevent definitive characterization of a relationship between photon energy and biological damage. Synchrotron radiation is a useful alternative source of low energy photons since it is available with high intensity over a continuous spectrum. A system was established including an appropriate dosimetry protocol and a workable system for conducting biology studies. A characterization of the system including spectral and intensity properties of the photon beam is presented. Cell survival curves for C3H/10T1/2 show increased efficiency for cell killing for 1-4 keV photons with respect to 250 kVp X-rays.

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

    SciTech Connect

    Gruner, Sol

    2010-05-01

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

  2. X-Ray-induced Deuterium Enrichment of N-rich Organics in Protoplanetary Disks: An Experimental Investigation Using Synchrotron Light

    NASA Astrophysics Data System (ADS)

    Gavilan, Lisseth; Remusat, Laurent; Roskosz, Mathieu; Popescu, Horia; Jaouen, Nicolas; Sandt, Christophe; Jäger, Cornelia; Henning, Thomas; Simionovici, Alexandre; Lemaire, Jean Louis; Mangin, Denis; Carrasco, Nathalie

    2017-05-01

    The deuterium enrichment of organics in the interstellar medium, protoplanetary disks, and meteorites has been proposed to be the result of ionizing radiation. The goal of this study is to simulate and quantify the effects of soft X-rays (0.1-2 keV), an important component of stellar radiation fields illuminating protoplanetary disks, on the refractory organics present in the disks. We prepared tholins, nitrogen-rich organic analogs to solids found in several astrophysical environments, e.g., Titan’s atmosphere, cometary surfaces, and protoplanetary disks, via plasma deposition. Controlled irradiation experiments with soft X-rays at 0.5 and 1.3 keV were performed at the SEXTANTS beamline of the SOLEIL synchrotron, and were immediately followed by ex-situ infrared, Raman, and isotopic diagnostics. Infrared spectroscopy revealed the preferential loss of singly bonded groups (N-H, C-H, and R-N≡C) and the formation of sp3 carbon defects with signatures at ˜1250-1300 cm-1. Raman analysis revealed that, while the length of polyaromatic units is only slightly modified, the introduction of defects leads to structural amorphization. Finally, tholins were measured via secondary ion mass spectrometry to quantify the D, H, and C elemental abundances in the irradiated versus non-irradiated areas. Isotopic analysis revealed that significant D-enrichment is induced by X-ray irradiation. Our results are compared to previous experimental studies involving the thermal degradation and electron irradiation of organics. The penetration depth of soft X-rays in μm-sized tholins leads to volume rather than surface modifications: lower-energy X-rays (0.5 keV) induce a larger D-enrichment than 1.3 keV X-rays, reaching a plateau for doses larger than 5 × 1027 eV cm-3. Synchrotron fluences fall within the expected soft X-ray fluences in protoplanetary disks, and thus provide evidence of a new non-thermal pathway to deuterium fractionation of organic matter.

  3. Phase contrast X-ray synchrotron imaging: opening access to fossil inclusions in opaque amber.

    PubMed

    Lak, Malvina; Néraudeau, Didier; Nel, André; Cloetens, Peter; Perrichot, Vincent; Tafforeau, Paul

    2008-06-01

    A significant portion of Mesozoic amber is fully opaque. Biological inclusions in such amber are invisible even after polishing, leading to potential bias in paleoecological and phylogenetic studies. Until now, studies using conventional X-ray microtomography focused on translucent or semi-opaque amber. In these cases, organisms of interest were visualized prior to X-ray analyses. It was recently demonstrated that propagation phase contrast X-ray synchrotron imaging techniques are powerful tools to access invisible inclusions in fully opaque amber. Here we describe an optimized synchrotron microradiographic protocol that allowed us to investigate efficiently and rapidly large amounts of opaque amber pieces from Charentes (southwestern France). Amber pieces were imaged with microradiography after immersion in water, which optimizes the visibility of inclusions. Determination is not accurate enough to allow precise phylogenetic studies, but provides preliminary data on biodiversity and ecotypes distribution; phase contrast microtomography remains necessary for precise determination. Because the organisms are generally much smaller than the amber pieces, we optimized local microtomography by using a continuous acquisition mode (sample moving during projection integration). As tomographic investigation of all inclusions is not practical, we suggest the use of a synchrotron for a microradiographic survey of opaque amber, coupled with microtomographic investigations of the most valuable organisms.

  4. Synchrotron X-ray computed microtomography study on gas hydrate decomposition in a sedimentary matrix

    NASA Astrophysics Data System (ADS)

    Yang, Lei; Falenty, Andrzej; Chaouachi, Marwen; Haberthür, David; Kuhs, Werner F.

    2016-09-01

    In-situ synchrotron X-ray computed microtomography with sub-micrometer voxel size was used to study the decomposition of gas hydrates in a sedimentary matrix. Xenon-hydrate was used instead of methane hydrate to enhance the absorption contrast. The microstructural features of the decomposition process were elucidated indicating that the decomposition starts at the hydrate-gas interface; it does not proceed at the contacts with quartz grains. Melt water accumulates at retreating hydrate surface. The decomposition is not homogeneous and the decomposition rates depend on the distance of the hydrate surface to the gas phase indicating a diffusion-limitation of the gas transport through the water phase. Gas is found to be metastably enriched in the water phase with a concentration decreasing away from the hydrate-water interface. The initial decomposition process facilitates redistribution of fluid phases in the pore space and local reformation of gas hydrates. The observations allow also rationalizing earlier conjectures from experiments with low spatial resolutions and suggest that the hydrate-sediment assemblies remain intact until the hydrate spacers between sediment grains finally collapse; possible effects on mechanical stability and permeability are discussed. The resulting time resolved characteristics of gas hydrate decomposition and the influence of melt water on the reaction rate are of importance for a suggested gas recovery from marine sediments by depressurization.

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

    PubMed

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

    2016-05-01

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

  6. 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.

  7. Synchroton X-Ray Studies of Growth Processes on Surfaces

    NASA Astrophysics Data System (ADS)

    Tse, Teddy

    1995-01-01

    We present a series of studies of surface growth processes with the use of synchrotron x-ray diffraction. Submonolayer growth of Pb on Ni(001) at room temperature exhibits self -similar and exponential growth with increasing adsorbate coverage. The results indicate that site degeneracy of the surface structure is not a significant factor in limiting growth before domains come into contact. Repeating the same growth procedure at higher temperatures on Pb on Ni(001) and Pb on Cu(001) results in adsorbate aggregation at pinning sites, followed by phenomena similar to those at low temperature domain growth. Late stage monolayer growth is studied on Pb on Cu(001) in which domains of different sublattices coarsen with constant adsorbate coverage. Domains grow as annealing time to 1/2 power with self-similar diffraction lineshape, consistent with the theory for a doubly degenerate system with a nonconserved order parameter. Multilayer growth of Ag on Ag(111) shows that roughness of the growth front increases with time as a power law, as predicted by the dynamic scaling hypothesis. The value of the growth exponent is found to decrease with increasing substrate temperature. Despite the complex and distinct growth mechanisms of the above systems, the concept of scaling appears to be a powerful tool in describing the non-equilibrium processes.

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

    PubMed

    Liu, Xiaosong; Yang, Wanli; Liu, Zhi

    2014-12-10

    Soft X-ray spectroscopy (SXS) techniques such as photoelectron spectroscopy, soft X-ray absorption spectroscopy and X-ray emission spectroscopy are efficient and direct tools to probe electronic structures of materials. Traditionally, these surface sensitive soft X-ray techniques that detect electrons or photons require high vacuum to operate. Many recent in situ instrument developments of these techniques have overcome this vacuum barrier. One can now study many materials and model devices under near ambient, semi-realistic, and operando conditions. Further developments of integrating the realistic sample environments with efficient and high resolution detection methods, particularly at the high brightness synchrotron light sources, are making SXS an important tool for the energy research community. In this progress report, we briefly describe the basic concept of several SXS techniques and discuss recent development of SXS instruments. We then present several recent studies, mostly in situ SXS experiments, on energy materials and devices. Using these studies, we would like to highlight that the integration of SXS and in situ environments can provide in-depth insight of material's functionality and help researchers in new energy material developments. The remaining challenges and critical research directions are discussed at the end. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Measurement of X-ray mass attenuation coefficient of nickel around the K-edge using synchrotron radiation based X-ray absorption study

    NASA Astrophysics Data System (ADS)

    Roy, Bunty Rani; Rajput, Parasmani; Jha, S. N.; Nageswara Rao, A. S.

    2015-09-01

    The work presents the X-ray absorption fine structure (XAFS) technique for measuring the X-ray mass attenuation coefficient of nickel metal foil in the X-ray energy range of 8271.2-8849.4 eV using scanning XAFS beam line (BL-09) at Indus-2 synchrotron radiation source facility, Raja Ramanna Centre for Advanced Technology (RRCAT) at Indore, India. The result represents the X-ray mass attenuation coefficient data for 0.02 mm thick Ni metal foil in the XAFS region of Ni K-edge. However, the results are compared to theoretical values using X-COM. There is a maximum deviation which is found exactly near the K-edge jump and decreases as we move away from the absorption edge. Oscillatory structure appears just above the observed absorption edge i.e., 8348.7 eV and is confined to around 250 eV above the edge.

  10. 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.

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

    SciTech Connect

    Miao, J.

    2004-06-04

    Recent work is extending the methodology of X-ray crystallography to the structure determination of noncrystalline specimens. The phase problem is solved using the oversampling method, which takes advantage of ''continuous'' diffraction patterns from noncrystalline specimens. Here we review the principle of this newly developed technique and discuss the ongoing experiments of imaging nonperiodic objects, such as cells and cellular structures, using coherent and bright X rays produced by third-generation synchrotron sources. In the longer run, the technique may be applicable to image single biomolecules using anticipated X-ray free electron lasers. Here, computer simulations have so far demonstrated two important steps: (a) by using an extremely intense femtosecond X-ray pulse, a diffraction pattern can be recorded from a macromolecule before radiation damage manifests itself; and (b) the phase information can be retrieved in an ab initio fashion from a set of calculated noisy diffraction patterns of single protein molecules.

  12. 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.

  13. 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.

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

    PubMed

    Toyoshima, Ryo; Kondoh, Hiroshi

    2015-03-04

    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.

  15. A Detailed Spatial and Spectral Study of Synchrotron X-rays from Supernova Remnants with Chandra

    NASA Astrophysics Data System (ADS)

    Bamba, Aya

    2004-01-01

    We present the first results of a systematic spatial and spectral X-ray study of small scale structures on the shock of five supernova remnants (Cas A, Kepler, Tycho, SN 1006, and RCW 86) and a super bubble (30 Dor C), with excellent spatial resolution of the Chandra X-ray observatory. All targets have synchrotron X-ray emission which concentrate on a very narrow region of the outer edge of the shock. The scale length of the region emitting synchrotron X-rays is incredibly small, less than 1% of the radius of the system both in the upstream and the downstream, in which smaller lengths are seen in the upstream than in the downstream. Together with the information of wide band spectra from radio to X-ray, both age-limited and loss-limited assumptions are checked for the acceleration history of all the SNRs. We found a possible magnetic field strength and configuration, and the maximum energy of accelerated electrons have been estimated for each target. The perpendicular magnetic field to the shock normal is accepted in all SNR cases, with highly turbulent magnetic field downstream. Comparing the samples, we found that the scale length of shocks grows as its age increases, in the same rate of Sedov similar solution for upstream (∝ t4/5) and in a faster rate for downstream (∝ t1/2). The energy density of magnetic field and cosmic rays evolve keeping an equipartition with the thermal and kinetic energies of the shock (∝ t-6/5) under the assumption that the system is in the age-limited case, implying that there are strong energy interaction between kinetic, thermal, magnetic field, and cosmic ray energy densities. The magnetic field is always near to perpendicular. These are the first results to estimate observationally the magnetic field and its direction, energy density of magnetic field and cosmic rays, and their evolutions.

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

    PubMed

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

    2016-05-01

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

  17. Combined X-ray fluorescence and absorption computed tomography using a synchrotron beam

    NASA Astrophysics Data System (ADS)

    Hall, C.

    2013-06-01

    X-ray computed tomography (CT) and fluorescence X-ray computed tomography (FXCT) using synchrotron sources are both useful tools in biomedical imaging research. Synchrotron CT (SRCT) in its various forms is considered an important technique for biomedical imaging since the phase coherence of SR beams can be exploited to obtain images with high contrast resolution. Using a synchrotron as the source for FXCT ensures a fluorescence signal that is optimally detectable by exploiting the beam monochromaticity and polarisation. The ability to combine these techniques so that SRCT and FXCT images are collected simultaneously, would bring distinct benefits to certain biomedical experiments. Simultaneous image acquisition would alleviate some of the registration difficulties which comes from collecting separate data, and it would provide increased information about the sample: functional X-ray images from the FXCT, with the morphological information from the SRCT. A method is presented for generating simultaneous SRCT and FXCT images. Proof of principle modelling has been used to show that it is possible to recover a fluorescence image of a point-like source from an SRCT apparatus by suitably modulating the illuminating planar X-ray beam. The projection image can be successfully used for reconstruction by removing the static modulation from the sinogram in the normal flat and dark field processing. Detection of the modulated fluorescence signal using an energy resolving detector allows the position of a fluorescent marker to be obtained using inverse reconstruction techniques. A discussion is made of particular reconstruction methods which might be applied by utilising both the CT and FXCT data.

  18. 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

  19. 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).

  20. Simultaneous scanning tunneling microscopy and synchrotron X-ray measurements in a gas environment.

    PubMed

    Mom, Rik V; Onderwaater, Willem G; Rost, Marcel J; Jankowski, Maciej; Wenzel, Sabine; Jacobse, Leon; Alkemade, Paul F A; Vandalon, Vincent; van Spronsen, Matthijs A; van Weeren, Matthijs; Crama, Bert; van der Tuijn, Peter; Felici, Roberto; Kessels, Wilhelmus M M; Carlà, Francesco; Frenken, Joost W M; Groot, Irene M N

    2017-11-01

    A combined X-ray and scanning tunneling microscopy (STM) instrument is presented that enables the local detection of X-ray absorption on surfaces in a gas environment. To suppress the collection of ion currents generated in the gas phase, coaxially shielded STM tips were used. The conductive outer shield of the coaxial tips can be biased to deflect ions away from the tip core. When tunneling, the X-ray-induced current is separated from the regular, 'topographic' tunneling current using a novel high-speed separation scheme. We demonstrate the capabilities of the instrument by measuring the local X-ray-induced current on Au(1 1 1) in 800 mbar Ar. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Study on Dual-Energy X-ray Computed Tomography using Synchrotron Radiation

    NASA Astrophysics Data System (ADS)

    Tsunoo, T.; Torikoshi, M.; Endo, M.; Natsuhori, M.; Kakizaki, T.; Yamada, N.; Itoh, N.; Uesugi, K.; Yagi, N.

    2004-05-01

    The electron density is one of the most important elements for the treatment planning in the radiotherapy, because this information is used for the range estimation of the heavy-ion beam. In order to measure more precise electron density, we have developed the dual-energy x-ray CT system using synchrotron radiation. The x-ray detector consists of 256 × 96 scintillator-array. It can take more than a hundred projection images per second. The response of the detector to x-rays was proved to be linear up to at least 1013 photon/pixel. The experiments were carried out using two monochromatic x-rays of 40 keV and 70 keV at the beam-line BL20B2 of SPring-8. As the results from samples of water, ethanol and solutions of dipotassium hydrogenphosphate with five concentrations, the electron densities measured in the dual-energy x-ray CT method were in agreement with the theoretical values by about ± 1%. This is almost the same level as that achieved by the one-dimensional CT system we developed previously. In addition, a sample of kidney of a pig fixed by formalin neutral buffer solution was used to distinguish the tissues in the CT images based on the electron density and the effective atomic number that was additionally obtained in the dual-energy x-ray CT. It suggested that renal pelvis was enriched with adipose tissue, and it was difficult to distinguish renal cortex and renal medulla.

  2. Study on Dual-Energy X-ray Computed Tomography using Synchrotron Radiation

    SciTech Connect

    Tsunoo, T.; Torikoshi, M.; Endo, M.; Natsuhori, M.; Kakizaki, T.; Yamada, N.; Itoh, N.; Uesugi, K.; Yagi, N.

    2004-05-12

    The electron density is one of the most important elements for the treatment planning in the radiotherapy, because this information is used for the range estimation of the heavy-ion beam. In order to measure more precise electron density, we have developed the dual-energy x-ray CT system using synchrotron radiation. The x-ray detector consists of 256 x 96 scintillator-array. It can take more than a hundred projection images per second. The response of the detector to x-rays was proved to be linear up to at least 1013 photon/pixel. The experiments were carried out using two monochromatic x-rays of 40 keV and 70 keV at the beam-line BL20B2 of SPring-8. As the results from samples of water, ethanol and solutions of dipotassium hydrogenphosphate with five concentrations, the electron densities measured in the dual-energy x-ray CT method were in agreement with the theoretical values by about {+-} 1%. This is almost the same level as that achieved by the one-dimensional CT system we developed previously. In addition, a sample of kidney of a pig fixed by formalin neutral buffer solution was used to distinguish the tissues in the CT images based on the electron density and the effective atomic number that was additionally obtained in the dual-energy x-ray CT. It suggested that renal pelvis was enriched with adipose tissue, and it was difficult to distinguish renal cortex and renal medulla.

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

    NASA Astrophysics Data System (ADS)

    Singh, Sudhanshu Shekhar

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

  4. Characterization of ion-induced radiation effects in nuclear materials using synchrotron x-ray techniques

    DOE PAGES

    Lang, Maik; Tracy, Cameron L.; Palomares, Raul I.; ...

    2015-05-01

    Recent efforts to characterize the nanoscale structural and chemical modifications induced by energetic ion irradiation in nuclear materials have greatly benefited from the application of synchrotron-based x-ray diffraction (XRD) and x-ray absorption spectroscopy (XAS) techniques. Key to the study of actinide-bearing materials has been the use of small sample volumes, which are particularly advantageous, as the small quantities minimize the level of radiation exposure at the ion-beam and synchrotron user facility. This approach utilizes energetic heavy ions (energy range: 100 MeV–3 GeV) that pass completely through the sample thickness and deposit an almost constant energy per unit length along theirmore » trajectory. High energy x-rays (25–65 keV) from intense synchrotron light sources are then used in transmission geometry to analyze ion-induced structural and chemical modifications throughout the ion tracks. We describe in detail the experimental approach for utilizing synchrotron radiation (SR) to study the radiation response of a range of nuclear materials (e.g., ThO2 and Gd2TixZr2–xO7). Also addressed is the use of high-pressure techniques, such as the heatable diamond anvil cell, as a new means to expose irradiated materials to well-controlled high-temperature (up to 1000 °C) and/or high-pressure (up to 50 GPa) conditions. Furthermore, this is particularly useful for characterizing the annealing kinetics of irradiation-induced material modifications.« less

  5. Characterization of ion-induced radiation effects in nuclear materials using synchrotron x-ray techniques

    SciTech Connect

    Lang, Maik; Tracy, Cameron L.; Palomares, Raul I.; Zhang, Fuxiang; Severin, Daniel; Bender, Markus; Trautmann, Christina; Park, Changyong; Prakapenka, Vitali B.; Skuratov, Vladimir A.; Ewing, Rodney C.

    2015-05-01

    Recent efforts to characterize the nanoscale structural and chemical modifications induced by energetic ion irradiation in nuclear materials have greatly benefited from the application of synchrotron-based x-ray diffraction (XRD) and x-ray absorption spectroscopy (XAS) techniques. Key to the study of actinide-bearing materials has been the use of small sample volumes, which are particularly advantageous, as the small quantities minimize the level of radiation exposure at the ion-beam and synchrotron user facility. This approach utilizes energetic heavy ions (energy range: 100 MeV–3 GeV) that pass completely through the sample thickness and deposit an almost constant energy per unit length along their trajectory. High energy x-rays (25–65 keV) from intense synchrotron light sources are then used in transmission geometry to analyze ion-induced structural and chemical modifications throughout the ion tracks. We describe in detail the experimental approach for utilizing synchrotron radiation (SR) to study the radiation response of a range of nuclear materials (e.g., ThO2 and Gd2TixZr2–xO7). Also addressed is the use of high-pressure techniques, such as the heatable diamond anvil cell, as a new means to expose irradiated materials to well-controlled high-temperature (up to 1000 °C) and/or high-pressure (up to 50 GPa) conditions. Furthermore, this is particularly useful for characterizing the annealing kinetics of irradiation-induced material modifications.

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

    NASA Technical Reports Server (NTRS)

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

    1989-01-01

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

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

    PubMed

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

    2013-03-10

    Computed tomography (CT) using synchrotron X-ray radiation was evaluated as a non-destructive structural analysis method for fine granules. Two kinds of granules have been investigated: a bromhexine hydrochloride (BHX)-layered Celphere CP-102 granule coated with pH-sensitive polymer Kollicoat Smartseal 30-D, and a wax-matrix granule constructed from acetaminophen (APAP), dibasic calcium phosphate dehydrate, and aminoalkyl methacrylate copolymer E (AMCE) manufactured by melt granulation. The diameters of both granules were 200-300 μm. CT analysis of CP-102 granule could visualize the laminar structures of BHX and Kollicoat layers, and also visualize the high talc-content regions in the Kollicoat layer that could not be detected by scanning electron microscopy. Moreover, CT analysis using X-ray energies above the absorption edge of Br specifically enhanced the contrast in the BHX layer. As for granules manufactured by melt granulation, CT analysis revealed that they had a small inner void space due to a uniform distribution of APAP and other excipients. The distribution of AMCE revealed by CT analysis was also found to involve in the differences of drug dissolution from the granules as described previously. These observations demonstrate that CT analysis using synchrotron X-ray radiation is a powerful method for the detailed internal structure analysis of fine granules. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. 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.

  9. In vivo microscopic x-ray imaging in rat and mouse using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Umetani, Keiji; Sakurai, Takashi; Kondoh, Takeshi

    2008-02-01

    A preclinical laboratory animal imaging modality similar to microangiography, with spatial resolution as high as 6 μm, has been developed at SPring-8 using an X-ray direct-conversion type detector incorporating an X-ray SATICON pickup tube. The imaging modality is intended to provide a basic understanding of disease mechanisms. In synchrotron radiation radiography, a long source-to-object distance and a small source spot can produce high-resolution images with spatial resolution in the micrometer range. Synchrotron radiation microangiography presents the main advantage of depicting the anatomy of small blood vessels with tens of micrometers' diameter. We performed cerebral microangiography in rats and mice and particularly undertook radiographical evaluation of changes in small arteries located deep in the brain; such vessels had not been observed and studied previously. Moreover, an X-ray direct-conversion type solid-state imager with spatial resolution in the micrometer range is being designed for large field-of-view imaging. This study is also intended to clarify requirements related to specifications of prospective solid-state image sensors.

  10. 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.

  11. Simple method to surface slope error characterization using x-ray optics

    SciTech Connect

    Gavinho, L.; Cusatis, C.; Mazzaro, I.; Tirao, G.

    2005-05-15

    This work shows a method to characterize nearly flat reflective surfaces. Slope error on the mirror surface under the total reflection condition of x rays is measured by perfect crystal rocking curve profile widening. The experiment was performed using a conventional x-ray tube and a simple optical setup. The sensitivity was sufficient to detect at least a slope error of 7 {mu}rad, typical quality for synchrotron mirrors. It is shown that this technique can also be used to characterize roughness and curvature. The method proposed here is an alternative to the traditional techniques for surface characterization and has the advantages of simplicity, versatility and sensitivity, and the synchrotron mirror quality can be evaluated under similar conditions as those for the designed operation.

  12. A new approach to synchrotron energy-dispersive X-ray diffraction computed tomography.

    PubMed

    Lazzari, Olivier; Egan, Christopher K; Jacques, Simon D M; Sochi, Taha; Di Michiel, Marco; Cernik, Robert J; Barnes, Paul

    2012-07-01

    A new data collection strategy for performing synchrotron energy-dispersive X-ray diffraction computed tomography has been devised. This method is analogous to angle-dispersive X-ray diffraction whose diffraction signal originates from a line formed by intersection of the incident X-ray beam and the sample. Energy resolution is preserved by using a collimator which defines a small sampling voxel. This voxel is translated in a series of parallel straight lines covering the whole sample and the operation is repeated at different rotation angles, thus generating one diffraction pattern per translation and rotation step. The method has been tested by imaging a specially designed phantom object, devised to be a demanding validator for X-ray diffraction imaging. The relative strengths and weaknesses of the method have been analysed with respect to the classic angle-dispersive technique. The reconstruction accuracy of the method is good, although an absorption correction is required for lower energy diffraction because of the large path lengths involved. The spatial resolution is only limited to the width of the scanning beam owing to the novel collection strategy. The current temporal resolution is poor, with a scan taking several hours. The method is best suited to studying large objects (e.g. for engineering and materials science applications) because it does not suffer from diffraction peak broadening effects irrespective of the sample size, in contrast to the angle-dispersive case.

  13. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2007-03-01

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

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

    PubMed

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

    2014-10-01

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

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

    PubMed Central

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

    2014-01-01

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

  17. 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.

  18. 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.

  19. Source assemblage types for cratonic diamonds from X-ray synchrotron diffraction

    NASA Astrophysics Data System (ADS)

    Nestola, F.; Alvaro, M.; Casati, M. N.; Wilhelm, H.; Kleppe, A. K.; Jephcoat, A. P.; Domeneghetti, M. C.; Harris, J. W.

    2016-11-01

    Three single crystals of clinopyroxene trapped within three different gem-quality diamonds from the Udachnaya kimberlite (Siberia, Russia) were analysed in situ by single-crystal synchrotron X-ray diffraction in order to obtain information on their chemical composition and infer source assemblage type. A non-destructive approach was used with high-energy (≈ 60 keV; λ ≈ 0.206 Å) at I15, the extreme-conditions beamline at Diamond Light Source. A dedicated protocol was used to center the mineral inclusions located deep inside the diamonds in the X-ray beam. Our results reveal that two of the inclusions can be associated with peridotitic paragenesis whereas the third is eclogitic. This study also demonstrates that this non-destructive experimental approach is extremely efficient in evaluating the origin of minerals trapped in their diamond hosts.

  20. Low energy X-ray grating interferometry at the Brazilian Synchrotron

    NASA Astrophysics Data System (ADS)

    Koch, F. J.; O'Dowd, F. P.; Cardoso, M. B.; Da Silva, R. R.; Cavicchioli, M.; Ribeiro, S. J. L.; Schröter, T. J.; Faisal, A.; Meyer, P.; Kunka, D.; Mohr, J.

    2017-06-01

    Grating based X-ray differential phase contrast imaging has found a large variety of applications in the last decade. Different types of samples call for different imaging energies, and efforts have been made to establish the technique all over the spectrum used for conventional X-ray imaging. Here we present a two-grating interferometer working at 8.3 keV, implemented at the bending magnet source of the IMX beamline of the Brazilian Synchrotron Light Laboratory. The low design energy is made possible by gratings fabricated on polymer substrates, and makes the interferometer mainly suited to the investigation of light and thin samples. We investigate polymer microspheres filled with Fe2O3 nanoparticles, and find that these particles give rise to a significant visibility reduction due to small angle scattering.

  1. High-energy synchrotron x-ray techniques for studying irradiated materials

    DOE PAGES

    Park, Jun-Sang; Zhang, Xuan; Sharma, Hemant; ...

    2015-03-20

    High performance materials that can withstand radiation, heat, multiaxial stresses, and corrosive environment are necessary for the deployment of advanced nuclear energy systems. Nondestructive in situ experimental techniques utilizing high energy x-rays from synchrotron sources can be an attractive set of tools for engineers and scientists to investigate the structure–processing–property relationship systematically at smaller length scales and help build better material models. In this paper, two unique and interconnected experimental techniques, namely, simultaneous small-angle/wide-angle x-ray scattering (SAXS/WAXS) and far-field high-energy diffraction microscopy (FF-HEDM) are presented. Finally, the changes in material state as Fe-based alloys are heated to high temperatures ormore » subject to irradiation are examined using these techniques.« less

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

    SciTech Connect

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

    2016-05-23

    We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantify lattice deformation and fracture; diffraction peak broadening is largely caused by fracture-induced strain inhomogeneity. Finally, our results demonstrate the potential of such multiscale measurements for revealing and understanding high strain-rate phenomena at dynamic extremes.

  3. 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.

  4. High-energy synchrotron x-ray techniques for studying irradiated materials

    SciTech Connect

    Park, Jun-Sang; Zhang, Xuan; Sharma, Hemant; Kenesei, Peter; Hoelzer, David; Li, Meimei; Almer, Jonathan

    2015-03-20

    High performance materials that can withstand radiation, heat, multiaxial stresses, and corrosive environment are necessary for the deployment of advanced nuclear energy systems. Nondestructive in situ experimental techniques utilizing high energy x-rays from synchrotron sources can be an attractive set of tools for engineers and scientists to investigate the structure–processing–property relationship systematically at smaller length scales and help build better material models. In this paper, two unique and interconnected experimental techniques, namely, simultaneous small-angle/wide-angle x-ray scattering (SAXS/WAXS) and far-field high-energy diffraction microscopy (FF-HEDM) are presented. Finally, the changes in material state as Fe-based alloys are heated to high temperatures or subject to irradiation are examined using these techniques.

  5. 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

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

    SciTech Connect

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

    2016-05-15

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

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

    SciTech Connect

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

    2016-05-23

    We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantify lattice deformation and fracture; diffraction peak broadening is largely caused by fracture-induced strain inhomogeneity. Finally, our results demonstrate the potential of such multiscale measurements for revealing and understanding high strain-rate phenomena at dynamic extremes.

  8. High-Resolution X-Ray Scattering Topography Using Synchrotron Radiation Microbeam

    NASA Astrophysics Data System (ADS)

    Chikaura, Yoshinori; Suzuki, Yoshifumi; Kii, Hideki

    1994-02-01

    Although spatial resolution is the most essential factor determining the function of X-ray topography, it has not been improved in 30 years in spite of increasing requirements for highly-resolvable topography in materials science. X-ray scattering topography using a microbeam is a method capable of overcoming this resolution problem. Because the maximum resolution of an apparatus using a sealed-off tube is limited to 20 µ m, we designed and constructed scattering topography equipment using a synchrotron radiation microbeam. In the experiment, the slit system forms the microbeam 7 µ m in diameter. We observed a cellulose distribution in bamboo as a testing material. When the scanning step was 2 µ m, we attained spatial resolution less than 5 µ m.

  9. 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.

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

    DOE PAGES

    Asadchikov, Victor E.; Butashin, Andrey V.; Buzmakov, Alexey V.; ...

    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

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

    SciTech Connect

    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; Alexeev, Pavel; Cecilia, Angelica; Baumbach, Tilo; Bessas, Dimitrios; Danilewsky, Andreas N.; Sergueev, Ilya; Wille, Hans -Christian; Hermann, Raphael P.

    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 density is observed, though growth rate is not the only parameter impacting the quality.

  12. X-ray harmonics rejection on third-generation synchrotron sources using compound refractive lenses.

    PubMed

    Polikarpov, Maxim; Snigireva, Irina; Snigirev, Anatoly

    2014-05-01

    A new method of harmonics rejection based on X-ray refractive optics has been proposed. Taking into account the fact that the focal distance of the refractive lens is energy-dependent, the use of an off-axis illumination of the lens immediately leads to spatial separation of the energy spectrum by focusing the fundamental harmonic at the focal point and suppressing the unfocused high-energy radiation with a screen absorber or slit. The experiment was performed at the ESRF ID06 beamline in the in-line geometry using an X-ray transfocator with compound refractive lenses. Using this technique the presence of the third harmonic has been reduced to 10(-3). In total, our method enabled suppression of all higher-order harmonics to five orders of magnitude using monochromator detuning. The method is well suited to third-generation synchrotron radiation sources and is very promising for the future ultimate storage rings.

  13. 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.

  14. 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

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

    NASA Astrophysics Data System (ADS)

    Pogorelsky, I. V.

    1997-03-01

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

  16. CCD-based detector for protein crystallography with synchrotron X-rays

    NASA Astrophysics Data System (ADS)

    Strauss, M. G.; Westbrook, E. M.; Naday, I.; Coleman, T. A.; Westbrook, M. L.; Travis, D. J.; Sweet, R. M.; Pflugrath, J. W.; Stanton, M.

    1990-11-01

    A detector with a 114 mm aperture, based on a charge-coupled device (CCD), has been designed for X-ray diffraction studies in protein crystallography. The detector was tested at the National Synchrotron Light Source with a beam intensity, through a 0.3 mm collimator, of greater than 109 X-ray photons/s. A fiberoptic taper, an image intensifier, and a lens demagnify, intensify, and focus the image onto a CCD having 512×512 pixels. The statistical uncertainty in the detector output was evaluated as a function of conversion gain. From this, a detective quantum efficiency (DQE) of 0.36 was derived. The dynamic range of a 4×4 pixel resolution element, comparable in size to a diffraction peak, was 104. The point-spread function shows FWHM resolution of approximately 1 pixel, where a pixel is 160 μm on the detector face. A data set collected from a chicken egg-white lysozyme crystal, consisting of 495 0.1° frames, was processed by the MADNES data reduction program. The symmetry R-factors for the data were 3.2-3.5%. In a separate experiment a complete lysozyme data set consisting of 45 1° frames was obtained in just 36 s of X-ray exposure. Diffraction images from crystals of the myosin S1 head (a = 275 Å) were also recorded; the Bragg spots, only 5 pixels apart, were separated but not fully resolved. Changes in the detector design that will improve the DQE and spatial resolution are outlined. The overall performance showed that this type of detector is well suited for X-ray scattering investigations with synchrotron sources.

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

    SciTech Connect

    Pogorelsky, I.V.

    1996-11-01

    A laser interacting with a relativistic electron beam behaves like a virtual wiggler of an extremely short period equal to half of the laser wavelength. This approach opens a route to relatively compact, high-brightness x-ray sources alternative or complementary to conventional synchrotron light sources. Although not new, the laser synchrotron source (LSS) concept is still waiting for a convincing demonstration. Available at the BNL Accelerator Test Facility (ATF), a high-brightness electron beam and the high-power CO{sub 2} laser may be used as prototype LSS brick stones. In a feasible demonstration experiment, 10-GW, 100-ps CO{sub 2} laser beam will be brought to a head-on collision with a 10-ps, 0.5-nC, 50 MeV electron bunch. Flashes of collimated 4.7 keV (2.6 {angstrom}) x-rays of 10-ps pulse duration, with a flux of {approximately} 10{sup 19} photons/sec, will be produced via linear Compton backscattering. The x-ray spectrum is tunable proportionally to the e-beam energy. A rational short-term extension of the proposed experiment would be further enhancement of the x-ray flux to the 10{sup 22} photons/sec level, after the ongoing ATF CO{sub 2} laser upgrade to 5 TW peak power and electron bunch shortening to 3 ps is realized. In the future, exploiting the promising approach of a high-gradient laser wake field accelerator, a compact ``table-top`` LSS of monochromatic gamma radiation may become feasible.

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

    SciTech Connect

    Pogorelsky, I.V.

    1997-01-01

    A laser interacting with a relativistic electron beam behaves like a virtual wiggler of an extremely short period equal to half of the laser wavelength. This approach opens a route to relatively compact, high- brightness x-ray sources alternative or complementary to conventional synchrotron light sources. Although not new, the laser synchrotron source (LSS) concept is still waiting for a convincing demonstration. Available at the BNL Accelerator Test Facility (ATF), a high- brightness electron beam and the high-power C0{sub 2} laser may be used as prototype LSS brick stones. In a feasible demonstration experiment, 10 GW, 100 ps C0{sub 2} laser beam will be brought to a head-on collision with a 10 ps, 0.5 nC, 50 MeV electron bunch. Flashes of collimated 4.7 keV (2.6 A) x-rays of 10-ps pulse duration, with a flux of {approximately}10{sup 19} photons/sec, will be produced via linear Compton backscattering. The x-ray spectra is tunable proportionally to the e- beam energy. A rational short-term extension of the proposed experiment would be further enhancement of the x-ray flux to the 10{sup 22} photon/sec level, after the ongoing ATF C0{sub 2} laser upgrade to 5 TW peak power and electron bunch shortening to 3 ps is realized. In the future, exploiting the promising approach of a high-gradient laser wake field accelerator, a compact ``table- top`` LSS of monochromatic gamma radiation may become feasible.

  19. 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

  20. 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.

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

    PubMed

    Kashyap, Yogesh; Wang, Hongchang; Sawhney, Kawal

    2016-08-08

    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.

  2. 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

  3. Synchrotron-based small-angle X-ray scattering of proteins in solution.

    PubMed

    Skou, Soren; Gillilan, Richard E; Ando, Nozomi

    2014-07-01

    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. 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 use 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 nonspecialist. 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. 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 before the experiment.

  4. Synchrotron X-ray diagnostics of cutoff shape of nonthermal electron spectrum at young supernova remnants

    NASA Astrophysics Data System (ADS)

    Yamazaki, Ryo; Ohira, Yutaka; Sawada, Makoto; Bamba, Aya

    2014-02-01

    Synchrotron X-rays can be a useful tool to investigate electron acceleration at young supernova remnants (SNRs). At present, since the magnetic field configuration around the shocks of SNRs is uncertain, it is not clear whether electron acceleration is limited by SNR age, synchrotron cooling, or even escape from the acceleration region. We study whether the acceleration mechanism can be constrained by the cutoff shape of the electron spectrum around the maximum energy. We derive analytical formulae of the cutoff shape in each case where the maximum electron energy is determined by SNR age, synchrotron cooling and escape from the shock. They are related to the energy dependence of the electron diffusion coefficient. Next, we discuss whether information on the cutoff shape can be provided by observations in the near future which will simply give the photon indices and the flux ratios in the soft and hard X-ray bands. We find that if the power-law index of the electron spectrum is independently determined by other observations, then we can constrain the cutoff shape by comparing theoretical predictions of the photon indices and/or the flux ratios with observed data which will be measured by NuSTAR and/or ASTRO-H. Such study is helpful in understanding the acceleration mechanism. In particular, it will supply another independent constraint on the magnetic field strength around the shocks of SNRs.

  5. 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.

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

    SciTech Connect

    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.

    2016-08-11

    Owing to its extreme sensitivity, quantitative mapping of elemental distributionsviaX-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.

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

    PubMed

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

    2016-04-01

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

  8. Development of optical choppers for time-resolved measurements at soft X-ray synchrotron radiation beamlines.

    PubMed

    Osawa, Hitoshi; Ohkochi, Takuo; Fujisawa, Masami; Kimura, Shigeru; Kinoshita, Toyohiko

    2017-05-01

    Two types of optical choppers for time-resolved measurements at synchrotron radiation soft X-ray beamlines have been developed. One type uses an air-spindle-type rotation mechanism with a two-stage differential pumping system to maintain the ultra-high vacuum of the X-ray beamline, and the other uses a magnetic bearing. Both can be installed at the soft X-ray beamlines at SPring-8, greatly improving the accessibility of pump-and-probe spectroscopy. The combination of X-ray chopper and pump-and-probe photoemission electron microscope at SPring-8 provides drastic improvements in signal-to-noise ratio and resolution compared with techniques using high-voltage gating of channel plate detectors. The choppers have the capability to be used not only at synchrotron radiation facilities but also at other types of soft X-ray and VUV beamlines.

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

    SciTech Connect

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

    1989-06-01

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

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

    PubMed

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

    2010-09-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2004-10-01

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

  12. Place-exchange mechanism of Pt (111) oxidation/reduction as observed by synchrotron X-ray scattering

    SciTech Connect

    You, H.; Nagy, Z.; Zurawski, D.J.; Chiarello, R.P.

    1996-07-01

    Structural changes in the Pt(111) single crystal surface associated with incipient electrochemical oxidation/reduction were studied by {ital in}{ital situ} synchrotron x-ray reflectivity. It was shown that lifting of Pt atoms of the surface layer occurs, substantiating the long-standing hypothesis of a place-exchange mechanism for solution/metal interface oxidation. It was also shown that, for a charge transfer of {approx_lt}1.7 e{sup -}/Pt atom, the initially flat surface structure could be recovered by electrochemical reduction. In constrast, the surface was irreversibly roughened for amounts of charge transfer exceeding {approx}1.7 e{sup -}/Pt, but the roughening involved only the atoms in the top layer of the original flat surface. A detailed mechanism is proposed for the place-exchange mechanism and the subsequent roughening of the electrode surface.

  13. Dynamic crystal rotation resolved by high-speed synchrotron X-ray Laue diffraction

    SciTech Connect

    Huang, J. W.; E, J. C.; Huang, J. Y.; Sun, T.; Fezzaa, K.; Luo, S. N.

    2016-03-30

    Dynamic compression experiments are performed on single-crystal Si under split Hopkinson pressure bar loading, together with simultaneous high-speed (250–350 ns resolution) synchrotron X-ray Laue diffraction and phase-contrast imaging. A methodology is presented which determines crystal rotation parameters,i.e.instantaneous rotation axes and angles, from two unindexed Laue diffraction spots. Two-dimensional translation is obtained from dynamic imaging by a single camera. High-speed motion of crystals, including translation and rotation, can be tracked in real timeviasimultaneous imaging and diffraction.

  14. 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.

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

    SciTech Connect

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

    2007-01-19

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

  16. 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.

  17. 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.}

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

    NASA Astrophysics Data System (ADS)

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

    2014-04-01

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

  19. A portable molecular beam epitaxy system for in situ x-ray investigations at synchrotron beamlines.

    PubMed

    Slobodskyy, T; Schroth, P; Grigoriev, D; Minkevich, A A; Hu, D Z; Schaadt, D M; Baumbach, T

    2012-10-01

    A portable synchrotron molecular beam epitaxy (MBE) system is designed and applied for in situ investigations. The growth chamber is equipped with all the standard MBE components such as effusion cells with shutters, main shutter, cooling shroud, manipulator, reflection high energy electron diffraction setup, and pressure gauges. The characteristic feature of the system is the beryllium windows which are used for in situ x-ray measurements. An UHV sample transfer case allows in vacuo transfer of samples prepared elsewhere. We describe the system design and demonstrate its performance by investigating the annealing process of buried InGaAs self-organized quantum dots.

  20. ShadowOui: a new visual environment for X-ray optics and synchrotron beamline simulations.

    PubMed

    Rebuffi, Luca; Sánchez Del Río, Manuel

    2016-11-01

    A new computer environment to perform simulations on synchrotron experiments has been designed. It performs ray-tracing simulations using the popular ray-tracing code SHADOW. With this new application one can define, in a very easy and elegant way, one or several optical systems (beamlines) and perform calculations of the propagation of the X-ray beam through it. Many complementary tools and supplementary calculations improve and extend the functionality of SHADOW to deal with complex optical system optimization, including compound optical elements, iterative calculations, some sample simulations, and implementing corrections for wave optics via a hybrid model.

  1. A portable molecular beam epitaxy system for in situ x-ray investigations at synchrotron beamlines

    SciTech Connect

    Slobodskyy, T.; Schroth, P.; Grigoriev, D.; Minkevich, A. A.; Baumbach, T.; Hu, D. Z.; Schaadt, D. M.

    2012-10-15

    A portable synchrotron molecular beam epitaxy (MBE) system is designed and applied for in situ investigations. The growth chamber is equipped with all the standard MBE components such as effusion cells with shutters, main shutter, cooling shroud, manipulator, reflection high energy electron diffraction setup, and pressure gauges. The characteristic feature of the system is the beryllium windows which are used for in situ x-ray measurements. An UHV sample transfer case allows in vacuo transfer of samples prepared elsewhere. We describe the system design and demonstrate its performance by investigating the annealing process of buried InGaAs self-organized quantum dots.

  2. 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.

  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. ShadowOui: a new visual environment for X-ray optics and synchrotron beamline simulations

    PubMed Central

    Sánchez del Río, Manuel

    2016-01-01

    A new computer environment to perform simulations on synchrotron experiments has been designed. It performs ray-tracing simulations using the popular ray-tracing code SHADOW. With this new application one can define, in a very easy and elegant way, one or several optical systems (beamlines) and perform calculations of the propagation of the X-ray beam through it. Many complementary tools and supplementary calculations improve and extend the functionality of SHADOW to deal with complex optical system optimization, including compound optical elements, iterative calculations, some sample simulations, and implementing corrections for wave optics via a hybrid model. PMID:27787241

  5. Dynamic crystal rotation resolved by high-speed synchrotron X-ray Laue diffraction

    PubMed Central

    Huang, J. W.; E, J. C.; Huang, J. Y.; Sun, T.; Fezzaa, K.; Luo, S. N.

    2016-01-01

    Dynamic compression experiments are performed on single-crystal Si under split Hopkinson pressure bar loading, together with simultaneous high-speed (250–350 ns resolution) synchrotron X-ray Laue diffraction and phase-contrast imaging. A methodology is presented which determines crystal rotation parameters, i.e. instantaneous rotation axes and angles, from two unindexed Laue diffraction spots. Two-dimensional translation is obtained from dynamic imaging by a single camera. High-speed motion of crystals, including translation and rotation, can be tracked in real time via simultaneous imaging and diffraction. PMID:27140150

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

    NASA Astrophysics Data System (ADS)

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

    2016-03-01

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

  8. 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.

  9. Synchrotron X-ray, photoluminescence, and quantum chemistry studies of bismuth-embedded dehydrated zeolite Y.

    PubMed

    Sun, Hong-Tao; Matsushita, Yoshitaka; Sakka, Yoshio; Shirahata, Naoto; Tanaka, Masahiko; Katsuya, Yoshio; Gao, Hong; Kobayashi, Keisuke

    2012-02-15

    For the first time, direct experimental evidence of the formation of monovalent Bi (i.e., Bi(+)) in zeolite Y is provided based on the analysis of high-resolution synchrotron powder X-ray diffraction data. Photoluminescence results as well as quantum chemistry calculations suggest that the substructures of Bi(+) in the sodalite cages contribute to the ultrabroad near-infrared emission. These results not only enrich the well-established spectrum of optically active zeolites and deepen the understanding of bismuth related photophysical behaviors, but also may raise new possibilities for the design and synthesis of novel hybrid nanoporous photonic materials activated by other heavier p-block elements.

  10. 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

  11. 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

  12. A novel technique combining high-resolution synchrotron x-ray microtomography and x-ray diffraction for characterization of micro particulates

    NASA Astrophysics Data System (ADS)

    Merrifield, David R.; Ramachandran, Vasuki; Roberts, Kevin J.; Armour, Wesley; Axford, Danny; Basham, Mark; Connolley, Thomas; Evans, Gwyndaf; McAuley, Katherine E.; Owen, Robin L.; Sandy, James

    2011-11-01

    The processing of solids, such as crystals, is strongly influenced by the surface properties of the material. In recent years the pharmaceutical industry has shown great interest in identifying, or chemically speciating, the molecular components of crystal faces. Formerly, characterization of the molecular identity of crystal faces was restricted to the study of large single crystals. This would have been primarily for structure determination as part of the drug registration process. Diamond Light Source in Oxfordshire is a new synchrotron facility in the UK, having 18 operational beamlines with 4 more in the construction phase. Beamlines at this medium energy light source enable the study of micron-sized objects in great detail. It is well known that x-ray microtomography (XMT) can be used to investigate the external morphology of a crystal whereas x-ray diffraction (XRD) is used to study the molecular orientation, structure and packing within the crystal. The objective of this research is to assess the feasibility of, and thereby develop a new methodology for, characterizing the molecular identity of a particular face of a crystalline particle at a scale of scrutiny of 20-50 µm by combining these two powerful techniques. This work demonstrates the application of XMT and XRD to investigate respectively the shape and crystalline phase/orientation of relevant test crystals. This research has applications in the pharmaceutical industry in that when the exact molecular nature of a particular face is known, the important physico-pharmaceutical properties stemming from that can be better understood. Some initial data are presented and discussed.

  13. NAD+ administration significantly attenuates synchrotron radiation X-ray-induced DNA damage and structural alterations of rodent testes

    PubMed Central

    Sheng, Caibin; Chen, Heyu; Wang, Ban; Liu, Tengyuan; Hong, Yunyi; Shao, Jiaxiang; He, Xin; Ma, Yingxin; Nie, Hui; Liu, Na; Xia, Weiliang; Ying, Weihai

    2012-01-01

    Synchrotron radiation (SR) X-ray has great potential for its applications in medical imaging and cancer treatment. In order to apply SR X-ray in clinical settings, it is necessary to elucidate the mechanisms underlying the damaging effects of SR X-ray on normal tissues, and to search for the strategies to reduce the detrimental effects of SR X-ray on normal tissues. However, so far there has been little information on these topics. In this study we used the testes of rats as a model to characterize SR X-ray-induced tissue damage, and to test our hypothesis that NAD+ administration can prevent SR X-ray-induced injury of the testes. We first determined the effects of SR X-ray at the doses of 0, 0.5, 1.3, 4 and 40 Gy on the biochemical and structural properties of the testes one day after SR X-ray exposures. We found that 40 Gy of SR X-ray induced a massive increase in double-strand DNA damage, as assessed by both immunostaining and Western blot of phosphorylated H2AX levels, which was significantly decreased by intraperitoneally (i.p.) administered NAD+ at doses of 125 and 625 mg/kg. Forty Gy of SR X-ray can also induce marked increases in abnormal cell nuclei as well as significant decreases in the cell layers of the seminiferous tubules one day after SR X-ray exposures, which were also ameliorated by the NAD+ administration. In summary, our study has shown that SR X-ray can produce both molecular and structural alterations of the testes, which can be significantly attenuated by NAD+ administration. These results have provided not only the first evidence that SR X-ray-induced tissue damage can be ameliorated by certain approaches, but also a valuable basis for elucidating the mechanisms underlying SR X-ray-induced tissue injury. PMID:22518270

  14. A large-area CMOS imager as an X-ray detector for synchrotron radiation experiments.

    PubMed

    Yagi, Naoto; Yamamoto, Masaki; Uesugi, Kentaro; Inoue, Katsuaki

    2004-07-01

    The performance of a CMOS flatpanel imager from Hamamatsu Photonics (C7942) has been tested in various synchrotron radiation experiments. This detector has a detection area of about 120 mm x 120 mm with 0.05 mm pixels, and a frame rate of 2 s(-1). The commercially available product was insensitive to X-rays with an energy lower than 15 keV, but slight modifications solved this problem. Images obtained in small-angle scattering, protein crystallography and medical imaging experiments were all of high quality. The fast readout and the large area are advantageous in real-time imaging. Although its noise level is higher than the area detectors that are currently used in synchrotron radiation experiments, it is particularly useful in experiments where other bulky detectors cannot be used. Its relatively low price (about 30,000 US dollars) makes it a unique option in the choice of detectors.

  15. An inexpensive spectroscopic beam monitor for hard X-ray synchrotron applications

    NASA Astrophysics Data System (ADS)

    Owens, A.; Andersson, S.; den Hartog, R.; Quarati, F.; Webb, A.; Welter, E.

    2007-05-01

    We describe an inexpensive beam monitor for hard X-ray synchrotron applications which has good spectroscopic abilities and can operate without cooling. The device is centred on an inexpensive, commercial off-the-shelf, large area (1.2 × 1.2 mm2) Si photodiode operated in single counting mode. Measurements carried out at the HASYLAB synchrotron research facility have shown that it is fully spectroscopic across the energy range 8 keV to 100 keV with a measured energy resolution of ~ 1.2 keV FWHM at room temperature. The measured resolutions were found to be the same under pencil-beam and full-area illumination, indicating uniform crystallinity and stoichiometry of the bulk. The low cost, simplicity and performance of the detector make it suitable for a wider range of applications, e.g., in undergraduate laboratory experiments.

  16. 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.

  17. 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.

  18. Coherence properties of focused X-ray beams at high-brilliance synchrotron sources

    PubMed Central

    Singer, Andrej; Vartanyants, Ivan A.

    2014-01-01

    An analytical approach describing properties of focused partially coherent X-ray beams is presented. The method is based on the results of statistical optics and gives both the beam size and transverse coherence length at any distance behind an optical element. In particular, here Gaussian Schell-model beams and thin optical elements are considered. Limiting cases of incoherent and fully coherent illumination of the focusing element are discussed. The effect of the beam-defining aperture, typically used in combination with focusing elements at synchrotron sources to improve transverse coherence, is also analyzed in detail. As an example, the coherence properties in the focal region of compound refractive lenses at the PETRA III synchrotron source are analyzed. PMID:24365911

  19. 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.

  20. Dose-rate plays a significant role in synchrotron radiation X-ray-induced damage of rodent testes

    PubMed Central

    Chen, Heyu; Wang, Ban; Wang, Caixia; Cao, Wei; Zhang, Jie; Ma, Yingxin; Hong, Yunyi; Fu, Shen; Wu, Fan; Ying, Weihai

    2016-01-01

    Synchrotron radiation (SR) X-ray has significant potential for applications in medical imaging and cancer treatment. However, the mechanisms underlying SR X-ray-induced tissue damage remain unclear. Previous studies on regular X-ray-induced tissue damage have suggested that dose-rate could affect radiation damage. Because SR X-ray has exceedingly high dose-rate compared to regular X-ray, it remains to be determined if dose-rate may affect SR X-ray-induced tissue damage. We used rodent testes as a model to investigate the role of dose-rate in SR X-ray-induced tissue damage. One day after SR X-ray irradiation, we determined the effects of the irradiation of the same dosage at two different dose-rates, 0.11 Gy/s and 1.1 Gy/s, on TUNEL signals, caspase-3 activation and DNA double-strand breaks (DSBs) of the testes. Compared to those produced by the irradiation at 0.11 Gy/s, irradiation at 1.1 Gy/s produced higher levels of DSBs, TUNEL signals, and caspase-3 activation in the testes. Our study has provided the first evidence suggesting that dose-rate could be a significant factor in SR X-ray-induced tissue damage, which may establish a valuable base for utilizing this factor to manipulate the tissue damage in SR X-ray-based medical applications. PMID:28078052

  1. Dose-rate plays a significant role in synchrotron radiation X-ray-induced damage of rodent testes.

    PubMed

    Chen, Heyu; Wang, Ban; Wang, Caixia; Cao, Wei; Zhang, Jie; Ma, Yingxin; Hong, Yunyi; Fu, Shen; Wu, Fan; Ying, Weihai

    2016-01-01

    Synchrotron radiation (SR) X-ray has significant potential for applications in medical imaging and cancer treatment. However, the mechanisms underlying SR X-ray-induced tissue damage remain unclear. Previous studies on regular X-ray-induced tissue damage have suggested that dose-rate could affect radiation damage. Because SR X-ray has exceedingly high dose-rate compared to regular X-ray, it remains to be determined if dose-rate may affect SR X-ray-induced tissue damage. We used rodent testes as a model to investigate the role of dose-rate in SR X-ray-induced tissue damage. One day after SR X-ray irradiation, we determined the effects of the irradiation of the same dosage at two different dose-rates, 0.11 Gy/s and 1.1 Gy/s, on TUNEL signals, caspase-3 activation and DNA double-strand breaks (DSBs) of the testes. Compared to those produced by the irradiation at 0.11 Gy/s, irradiation at 1.1 Gy/s produced higher levels of DSBs, TUNEL signals, and caspase-3 activation in the testes. Our study has provided the first evidence suggesting that dose-rate could be a significant factor in SR X-ray-induced tissue damage, which may establish a valuable base for utilizing this factor to manipulate the tissue damage in SR X-ray-based medical applications.

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

    PubMed

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

    2015-10-01

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

  3. Steep Decay of GRB X-Ray Flares: The Results of Anisotropic Synchrotron Radiation

    NASA Astrophysics Data System (ADS)

    Geng, Jin-Jun; Huang, Yong-Feng; Dai, Zi-Gao

    2017-05-01

    When an emitting spherical shell with a constant Lorentz factor turns off emission abruptly at some radii, its high-latitude emission would obey the relation of \\hat{α } (the temporal index) = 2+\\hat{β } (the spectral index). However, this relation is violated by the X-ray fares in some gamma-ray bursts (GRBs), whose \\hat{α } is much more steeper. We show that the synchrotron radiation should be anisotropic when the angular distribution of accelerated electrons has a preferable orientation, and this anisotropy would naturally lead to a steeper decay for the high-latitude emission if the intrinsic emission is limb-brightened. We use this simple toy model to reproduce the temporal and spectral evolution of X-ray flares. We show that our model can well interpret the steep decay of the X-ray flares in the three GRBs selected as an example. Recent simulations on particle acceleration may support the specific anisotropic distribution of the electrons adopted in our work. Reversely, confirmation of the anisotropy in the radiation would provide meaningful clues to the details of electron acceleration in the emitting region.

  4. 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.

  5. Correlative organelle fluorescence microscopy and synchrotron X-ray chemical element imaging in single cells.

    PubMed

    Roudeau, Stéphane; Carmona, Asuncion; Perrin, Laura; Ortega, Richard

    2014-11-01

    X-ray chemical element imaging has the potential to enable fundamental breakthroughs in the understanding of biological systems because chemical element interactions with organelles can be studied at the sub-cellular level. What is the distribution of trace metals in cells? Do some elements accumulate within sub-cellular organelles? What are the chemical species of the elements in these organelles? These are some of the fundamental questions that can be addressed by use of X-ray chemical element imaging with synchrotron radiation beams. For precise location of the distribution of the elements, identification of cellular organelles is required; this can be achieved, after appropriate labelling, by use of fluorescence microscopy. As will be discussed, this approach imposes some limitations on sample preparation. For example, standard immunolabelling procedures strongly modify the distribution of the elements in cells as a result of the chemical fixation and permeabilization steps. Organelle location can, however, be performed, by use of a variety of specific fluorescent dyes or fluorescent proteins, on living cells before cryogenic fixation, enabling preservation of element distribution. This article reviews the methods used for fluorescent organelle labelling and X-ray chemical element imaging and speciation of single cells. Selected cases from our work and from other research groups are presented to illustrate the potential of the combination of the two techniques.

  6. Basic principles of Synchrotron Radiation-Induced X-Ray Fluorescence (SRXRF)

    SciTech Connect

    Gigante, G.E. . Dipt. di Fisica); Hanson, A.L. )

    1990-05-01

    The characteristic x rays can be used as powerful analytical tools for qualitative and quantitative determination of the major, minor and trace composition of materials. X Ray Fluorescence (XRF) techniques used for almost four decade to solve many problems in basic, applied science, and in industry. The XRF techniques that were developed initially used crystal spectrometers, and are referred to in literature as Wavelength Dispersive (WD) techniques. These WD techniques are still used in many fields and have the merit of a excellent energy resolution that allows for the analysis of many elements while avoiding the overlapping of some fluorescence peaks. They are also particularly useful in a matrix that produces copious quantities of a particular radiation. The principal disadvantages of a WD system are the low efficiency of crystal and the reduced energy region in which crystal spectrometer can be used. In the 1960's, Solid State Detectors (SSD) were developed with energy resolution such that the Energy Dispersive XRF techniques could be developed. These SSD's overcame some of the limitations of the WD techniques. The most attractive characteristics of the EDXRF techniques are in their intrinsic multielemental and non destructive capabilities. The development of the high intensity, high brilliance Synchrotron Radiation (SR) sources have open the possibility to make microanalyses using the XRF techniques, increasing the interest of the scientific community for these techniques. In this paper the basic concepts of the XRF technique are reviewed taking in account the availability of the new sources of x rays. 32 refs., 7 figs.

  7. 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.

  8. Concentration of synchrotron beams by means of monolithic polycapillary X-ray optics

    NASA Astrophysics Data System (ADS)

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

    1995-02-01

    Capillary optics are valuable tools for concentrating synchrotron radiation [D.J. Tiel, A.E. Stern, D.H. Bilderback and A. Lewis, Physica B 158 (1989) 314]. 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 can achieve very short focal distances for a wide range of energies. The measurements shown here represent first tests performed with polycapillaries with large collection area. The performance with respect to transmission efficiency and spot size was evaluated for a set of four very different prototypes. It is shown that for these prototypes 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.

  9. Synchrotron x-ray microdiffraction reveals intrinsic structural features of amyloid deposits in situ.

    PubMed

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

    2011-07-20

    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. Copyright © 2011 Biophysical Society. Published by Elsevier Inc. All rights reserved.

  10. Advancements and Application of Microsecond Synchrotron X-ray Footprinting at the Advanced Light Source

    SciTech Connect

    Gupta, Sayan; Celestre, Rich; Feng, Jun; Ralston, Corie

    2016-01-02

    The method of synchrotron X-ray protein footprinting (XF-MS) is used to determine protein conformational changes, folding, protein-protein and protein-ligand interactions, providing information which is often difficult to obtain using X-ray crystallography and other common structural biology methods [1 G. Xu and M.R. Chance, Chemical Reviews 107, 3514–3543 (2007). [CrossRef], [PubMed], [Web of Science ®], [Google Scholar] –3 V.N. Bavro, Biochem Soc Trans 43, 983–994 (2015). [CrossRef], [PubMed], [Web of Science ®], [Google Scholar] ]. The technique uses comparative in situ labeling of solvent-accessible side chains by highly reactive hydroxyl radicals (•OH) in buffered aqueous solution under different assay conditions. In regions where a protein is folded or binds a partner, these •OH susceptible sites are inaccessible to solvent, and therefore protected from labeling. The •OH are generated by the ionization of water using high-flux-density X-rays. High-flux density is a key factor for XF-MS labeling because obtaining an adequate steady-state concentration of hydroxyl radical within a short irradiation time is necessary to minimize radiation-induced secondary damage and also to overcome various scavenging reactions that reduce the yield of labeled side chains.

  11. Linear parabolic single-crystal diamond refractive lenses for synchrotron X-ray sources.

    PubMed

    Terentyev, Sergey; Polikarpov, Maxim; Snigireva, Irina; Di Michiel, Marco; Zholudev, Sergey; Yunkin, Vyacheslav; Kuznetsov, Sergey; Blank, Vladimir; Snigirev, Anatoly

    2017-01-01

    Linear parabolic diamond refractive lenses are presented, designed to withstand high thermal and radiation loads coming from upgraded accelerator X-ray sources. Lenses were manufactured by picosecond laser treatment of a high-quality single-crystal synthetic diamond. Twelve lenses with radius of curvature at parabola apex R = 200 µm, geometrical aperture A = 900 µm and length L = 1.5 mm were stacked as a compound refractive lens and tested at the ESRF ID06 beamline. A focal spot of size 2.2 µm and a gain of 20 were measured at 8 keV. The lens profile and surface quality were estimated by grating interferometry and X-ray radiography. In addition, the influence of X-ray glitches on the focusing properties of the compound refractive lens were studied.

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

    PubMed

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

    2011-12-01

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

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

    SciTech Connect

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

    2011-12-15

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

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

    NASA Astrophysics Data System (ADS)

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

    2011-12-01

    Here, we report on a novel experimental apparatus for performing time-resolved soft x-ray absorption spectroscopy in the sub-ns time scale using non-hybrid multi-bunch mode synchrotron radiation. The present setup is based on a variable repetition rate Ti:sapphire laser (pump pulse) synchronized with the ˜500 MHz x-ray synchrotron radiation bunches and on a detection system that discriminates and singles out the significant x-ray photon pulses by means of a custom made photon counting unit. The whole setup has been validated by measuring the time evolution of the L3 absorption edge during the melting and the solidification of a Ge single crystal irradiated by an intense ultrafast laser pulse. These results pave the way for performing synchrotron time-resolved experiments in the sub-ns time domain with variable repetition rate exploiting the full flux of the synchrotron radiation.

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

    NASA Astrophysics Data System (ADS)

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

    2009-12-01

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

  16. 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. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

  17. 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.

  18. [Mapping metal elements of Shuangbai dinosaur fossil by synchrotron X-ray fluorescence microprobe].

    PubMed

    Wang, Yi-Lin; Yang, Qun; Ablett, J M

    2008-05-01

    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 ture 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.

  19. 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.

  20. SYNCHROTRON BLOB MODEL OF INFRARED AND X-RAY FLARES FROM SAGITTARIUS A*

    SciTech Connect

    Kusunose, Masaaki; Takahara, Fumio E-mail: takahara@vega.ess.sci.osaka-u.ac.jp

    2011-01-01

    Sagittarius A* in the Galactic center harbors a supermassive black hole and exhibits various active phenomena. Besides quiescent emission in radio and submillimeter radiation, flares in the near-infrared (NIR) and X-ray bands are observed to occur frequently. We study a time-dependent model of the flares, assuming that the emission is from a blob ejected from the central object. Electrons obeying a power law with the exponential cutoff are assumed to be injected in the blob for a limited time interval. The flare data of 2007 April 4 were used to determine the values of model parameters. The spectral energy distribution of flare emission is explained by nonthermal synchrotron radiation in the NIR and X-ray bands. The model light curves suggest that electron acceleration is still underway during the rising phase of the flares. GeV {gamma}-rays are also emitted by synchrotron self-Compton scattering, although their luminosity is not strictly constrained by the current model. If the GeV emission is faint, the plasma blob is dominated by the magnetic energy density over the electron kinetic energy density. Observations in the GeV band will clarify the origin of the blob.

  1. 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.

  2. 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

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

    NASA Astrophysics Data System (ADS)

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

    2002-05-01

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

  4. X-ray beam/biomaterial thermal interactions in third-generation synchrotron sources.

    PubMed

    Kuzay, T M; Kazmierczak, M; Hsieh, B J

    2001-01-01

    Third-generation synchrotron sources generate strong X-ray beams. The beam's interaction with biomaterials gives rise to concerns related to thermal damage and radiation damage. Of the two issues, the thermal interaction is conducive to rigorous analysis from first principles, although this has not been performed to date in a comprehensive manner. In this study, the interaction of the X-ray beam emanating from a third-generation synchrotron with a typical frozen biocrystal is theoretically studied, focusing specifically on the resulting unsteady (time-dependent) and steady heat-transfer phenomena. A unique regime map is developed to explain and to identify, on the basis of Fourier and Biot numbers as governing parameters, the applicable mathematical models that predict the subsequent thermal behavior. Depending on the values of these parameters, some simplified but realistic 'generic' solutions are generated that are suitable for that particular domain of applicability. Classical heat-transfer theory was used to describe the third-generation X-ray beam and biomaterial thermal interaction. Besides the generalized approach presented, numerous illustrative cases were solved and the resulting temperature levels are explicitly presented. Overall, the resulting thermal behavior of the system, i.e. peak and local temperature distribution, during both early transient development and for sustained long-time steady-state conditions, depends on a number of factors including the amount of energy absorbed, convective heat-transfer film coefficient and gas temperature, the sample size and shape, and the thermophysical properties of the sample and cooling gas. Results of the analysis revealed the strong influence that convection has on the transient and final steady-state temperature of the sample and the impact of internal heat conduction. The characteristic timescales of the important and dominant thermal processes with respect to the two types of thermal models are clearly

  5. Evaluation of microstructural properties of coffee beans by synchrotron X-ray microtomography: a methodological approach.

    PubMed

    Pittia, Paola; Sacchetti, Giampiero; Mancini, Lucia; Voltolini, Marco; Sodini, Nicola; Tromba, Giuliana; Zanini, Franco

    2011-03-01

    Synchrotron radiation microtomography was used as a nondestructive imaging technique to investigate the microstructural properties of green and roasted coffee beans. After image acquisition, 2D images have been reconstructed and 3D images of the beans have been then obtained. Qualitative and quantitative analysis of the images allow to fully characterize the morphological and structural features of the coffee beans. Roasting causes meaningful changes in the microstructure of the coffee bean tissue with the development in the entire bean of a porous structure with pores of different shape and size depending on the zone of the bean and cracks occurring mainly in the more external regions and between parenchyma and mucilage. The highly contrasted X-ray images have been analyzed to determine the pore size and its distribution in different regions of the coffee beans by selecting Volume-of-Interest (VoI). The use of phase-contrast hard X-rays imaging techniques represents an interesting tool of investigation of the internal structure, morphology, as well as the quality of whole coffee beans. Moreover, the high potentiality of 3D X-ray imaging and the approach used in this study could be applied in understanding the effects of roasting process conditions on the evolution of microstructural properties of the bean that may affect the stability as well the grinding and brewing performances. Synchrotron radiation microtomography is an elegant nondestructive imaging technique to investigate the microstructural properties of porous cellular matrices like the green and roasted coffee beans. The quantitative analysis of the resulting 2D and 3D images allows a more comprehensive and objective characterization of the sample under investigation as a whole or of extracted Volumes-of-Interest in the bean. This imaging technique could have a major role in understanding the effects of roasting process conditions on the microstructural properties of the bean.

  6. Energy dispersive detector for white beam synchrotron x-ray fluorescence imaging

    SciTech Connect

    Wilson, Matthew D. Seller, Paul; Veale, Matthew C.; Connolley, Thomas; Dolbnya, Igor P.; Malandain, Andrew; Sawhney, Kawal; Grant, Patrick S.; Liotti, Enzo; Lui, Andrew

    2016-07-27

    A novel, “single-shot” fluorescence imaging technique has been demonstrated on the B16 beamline at the Diamond Light Source synchrotron using the HEXITEC energy dispersive imaging detector. A custom made furnace with 200µm thick metal alloy samples was positioned in a white X-ray beam with a hole made in the furnace walls to allow the transmitted beam to be imaged with a conventional X-ray imaging camera consisting of a 500 µm thick single crystal LYSO scintillator, mirror and lens coupled to an AVT Manta G125B CCD sensor. The samples were positioned 45° to the incident beam to enable simultaneous transmission and fluorescence imaging. The HEXITEC detector was positioned at 90° to the sample with a 50 µm pinhole 13 cm from the sample and the detector positioned 2.3m from pinhole. The geometric magnification provided a field of view of 1.1×1.1mm{sup 2} with one of the 80×80 pixels imaging an area equivalent to 13µm{sup 2}. Al-Cu alloys doped with Zr, Ag and Mo were imaged in transmission and fluorescence mode. The fluorescence images showed that the dopant metals could be simultaneously imaged with sufficient counts on all 80x80 pixels within 60 s, with the X-ray flux limiting the fluorescence imaging rate. This technique demonstrated that it is possible to simultaneously image and identify multiple elements on a spatial resolution scale ~10µm or higher without the time consuming need to scan monochromatic energies or raster scan a focused beam of X-rays. Moving to high flux beamlines and using an array of detectors could improve the imaging speed of the technique with element specific imaging estimated to be on a 1 s timescale.

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

    SciTech Connect

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

    1996-03-01

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

  8. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2012-12-01

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

  10. Observation of sagittal X-ray diffraction by surface acoustic waves in Bragg geometry.

    PubMed

    Vadilonga, Simone; Zizak, Ivo; Roshchupkin, Dmitry; Evgenii, Emelin; Petsiuk, Andrei; Leitenberger, Wolfram; Erko, Alexei

    2017-04-01

    X-ray Bragg diffraction in sagittal geometry on a Y-cut langasite crystal (La3Ga5SiO14) modulated by Λ = 3 µm Rayleigh surface acoustic waves was studied at the BESSY II synchrotron radiation facility. Owing to the crystal lattice modulation by the surface acoustic wave diffraction, satellites appear. Their intensity and angular separation depend on the amplitude and wavelength of the ultrasonic superlattice. Experimental results are compared with the corresponding theoretical model that exploits the kinematical diffraction theory. This experiment shows that the propagation of the surface acoustic waves creates a dynamical diffraction grating on the crystal surface, and this can be used for space-time modulation of an X-ray beam.

  11. Observation of sagittal X-ray diffraction by surface acoustic waves in Bragg geometry1

    PubMed Central

    Vadilonga, Simone; Zizak, Ivo; Roshchupkin, Dmitry; Evgenii, Emelin; Petsiuk, Andrei; Leitenberger, Wolfram; Erko, Alexei

    2017-01-01

    X-ray Bragg diffraction in sagittal geometry on a Y-cut langasite crystal (La3Ga5SiO14) modulated by Λ = 3 µm Rayleigh surface acoustic waves was studied at the BESSY II synchrotron radiation facility. Owing to the crystal lattice modulation by the surface acoustic wave diffraction, satellites appear. Their intensity and angular separation depend on the amplitude and wavelength of the ultrasonic superlattice. Experimental results are compared with the corresponding theoretical model that exploits the kinematical diffraction theory. This experiment shows that the propagation of the surface acoustic waves creates a dynamical diffraction grating on the crystal surface, and this can be used for space–time modulation of an X-ray beam. PMID:28381976

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

    NASA Astrophysics Data System (ADS)

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

    2016-12-01

    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 3.2σ 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 time-scales), highly variable (on short time-scales) 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) wavebands. 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.

  13. Optical systems for synchrotron radiation: lecture 4. Soft x-ray imaging systems

    SciTech Connect

    Howells, M.R.

    1986-04-01

    The history and present techniques of soft x-ray imaging are reviewed briefly. The physics of x-ray imaging is described, including the temporal and spatial coherence of x-ray sources. Particular technologies described are: contact x-ray microscopy, zone plate imaging, scanned image zone plate microscopy, scanned image reflection microscopy, and soft x-ray holography and diffraction. (LEW)

  14. Aqueous Nucleation and Growth of Titanium Oxides Using Time-Resolved Synchrotron X- ray Diffraction

    NASA Astrophysics Data System (ADS)

    Hummer, D. R.; Heaney, P. J.; Post, J. E.

    2006-05-01

    The inorganic precipitation of oxide minerals in soil environments has profound effects on a variety of geochemical processes. These include the removal of metals from the aqueous phase, the production of coatings that reduce the reactive surface area of pre-existing mineral grains, and the generation of feedstocks for microbial metabolic reactions. Recent observations of transient, metastable phases during the growth of oxide crystallites has raised questions about their role in crystallization mechanisms, and created a need for more detailed structural measurements. To better understand the process of nucleation and growth, we investigated the crystallization of Ti oxides from aqueous 0.5 M TiCl4 solutions using synchrotron X-ray diffraction at temperatures of 100 and 150 °C. Solutions were heated in a 1.0 mm internal diameter quartz glass capillary sealed with epoxy. Powder diffraction patterns of the growing crystallites were collected using image plate technology with a time step of ~ 4 minutes, providing high resolution in situ measurements of structural changes during the crystallization process. The data indicate a co-precipitation of the two crystalline phases anatase and rutile within the first 30 minutes of heating, followed by a gradual phase transition from anatase to rutile during particle coarsening throughout the 10 hour duration of an experiment. The co-existence of anatase and rutile at the onset of crystallization lends additional support to the assertion of nearly identical free energies for anatase and rutile at the nanoscale, believed to be due to the prominence of surface energy effects (Ranade et al., 2001). Whole pattern analyses using the Rietveld refinement method also documented previously unobserved changes in lattice parameters of both phases during growth, on the order of 0.2-0.3 % expansion for each axis. The trends in lattice parameters are observed to be temperature dependent, generally having lower values at higher

  15. 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.

  16. 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

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

    SciTech Connect

    Ham, Kyungmin; Willson, Clinton S.

    2006-01-31

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

  18. 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.

  19. Ptychographic coherent x-ray surface scattering imaging

    NASA Astrophysics Data System (ADS)

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

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

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

    DOE PAGES

    Feng, Huan; Zhang, Weiguo; Qian, Yu; ...

    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

  1. 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.

  2. Synchrotron radiation micro X-ray fluorescence spectroscopy of thin structures in bone samples: comparison of confocal and color X-ray camera setups.

    PubMed

    Rauwolf, M; Turyanskaya, A; Roschger, A; Prost, J; Simon, R; Scharf, O; Radtke, M; Schoonjans, T; Guilherme Buzanich, A; Klaushofer, K; Wobrauschek, P; Hofstaetter, J G; Roschger, P; Streli, C

    2017-01-01

    In the quest for finding the ideal synchrotron-radiation-induced imaging method for the investigation of trace element distributions in human bone samples, experiments were performed using both a scanning confocal synchrotron radiation micro X-ray fluorescence (SR-µXRF) (FLUO beamline at ANKA) setup and a full-field color X-ray camera (BAMline at BESSY-II) setup. As zinc is a trace element of special interest in bone, the setups were optimized for its detection. The setups were compared with respect to count rate, required measurement time and spatial resolution. It was demonstrated that the ideal method depends on the element of interest. Although for Ca (a major constituent of the bone with a low energy of 3.69 keV for its Kα XRF line) the color X-ray camera provided a higher resolution in the plane, for Zn (a trace element in bone) only the confocal SR-µXRF setup was able to sufficiently image the distribution.

  3. Synchrotron radiation micro X-ray fluorescence spectroscopy of thin structures in bone samples: comparison of confocal and color X-ray camera setups

    PubMed Central

    Rauwolf, M.; Turyanskaya, A.; Roschger, A.; Prost, J.; Simon, R.; Scharf, O.; Radtke, M.; Schoonjans, T.; Guilherme Buzanich, A.; Klaushofer, K.; Wobrauschek, P.; Hofstaetter, J. G.; Roschger, P.; Streli, C.

    2017-01-01

    In the quest for finding the ideal synchrotron-radiation-induced imaging method for the investigation of trace element distributions in human bone samples, experiments were performed using both a scanning confocal synchrotron radiation micro X-ray fluorescence (SR-µXRF) (FLUO beamline at ANKA) setup and a full-field color X-ray camera (BAMline at BESSY-II) setup. As zinc is a trace element of special interest in bone, the setups were optimized for its detection. The setups were compared with respect to count rate, required measurement time and spatial resolution. It was demonstrated that the ideal method depends on the element of interest. Although for Ca (a major constituent of the bone with a low energy of 3.69 keV for its Kα XRF line) the color X-ray camera provided a higher resolution in the plane, for Zn (a trace element in bone) only the confocal SR-µXRF setup was able to sufficiently image the distribution. PMID:28009572

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

    NASA Astrophysics Data System (ADS)

    Takeo, Yoko; Saito, Takahiro; Mimura, Hidekazu

    2015-08-01

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

  5. A compact dispersive refocusing Rowland circle X-ray emission spectrometer for laboratory, synchrotron, and XFEL applications

    NASA Astrophysics Data System (ADS)

    Holden, William M.; Hoidn, Oliver R.; Ditter, Alexander S.; Seidler, Gerald T.; Kas, Joshua; Stein, Jennifer L.; Cossairt, Brandi M.; Kozimor, Stosh A.; Guo, Jinghua; Ye, Yifan; Marcus, Matthew A.; Fakra, Sirine

    2017-07-01

    X-ray emission spectroscopy is emerging as an important complement to x-ray absorption fine structure spectroscopy, providing a characterization of the occupied electronic density of states local to the species of interest. Here, we present details of the design and performance of a compact x-ray emission spectrometer that uses a dispersive refocusing Rowland (DRR) circle geometry to achieve excellent performance for the 2-2.5 keV range, i.e., especially for the K-edge emission from sulfur and phosphorous. The DRR approach allows high energy resolution even for unfocused x-ray sources. This property enables high count rates in laboratory studies, approaching those of insertion-device beamlines at third-generation synchrotrons, despite use of only a low-powered, conventional x-ray tube. The spectrometer, whose overall scale is set by use of a 10-cm diameter Rowland circle and a new small-pixel complementary metal-oxide-semiconductor x-ray camera, is easily portable to synchrotron or x-ray free electron laser beamlines. Photometrics from measurements at the Advanced Light Source show excellent overall instrumental efficiency. In addition, the compact size of this instrument lends itself to future multiplexing to gain large factors in net collection efficiency or its implementation in controlled gas gloveboxes either in the lab or in an endstation.

  6. 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

    2014-05-02

    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.

  7. A compact dispersive refocusing Rowland circle X-ray emission spectrometer for laboratory, synchrotron, and XFEL applications

    DOE PAGES

    Holden, William M.; Hoidn, Oliver R.; Ditter, Alexander S.; ...

    2017-07-27

    X-ray emission spectroscopy is emerging as an important complement to x-ray absorption fine structure spectroscopy, providing a characterization of the occupied electronic density of states local to the species of interest. Here, we present details of the design and performance of a compact x-ray emission spectrometer that uses a dispersive refocusing Rowland (DRR) circle geometry to achieve excellent performance for the 2-2.5 keV range, i.e., especially for the K-edge emission from sulfur and phosphorous. The DRR approach allows high energy resolution even for unfocused x-ray sources. This property enables high count rates in laboratory studies, approaching those of insertion-device beamlinesmore » at third-generation synchrotrons, despite use of only a low-powered, conventional x-ray tube. The spectrometer, whose overall scale is set by use of a 10-cm diameter Rowland circle and a new small-pixel complementary metal-oxide-semiconductor x-ray camera, is easily portable to synchrotron or x-ray free electron laser beamlines. Photometrics from measurements at the Advanced Light Source show excellent overall instrumental efficiency. In addition, the compact size of this instrument lends itself to future multiplexing to gain large factors in net collection efficiency or its implementation in controlled gas gloveboxes either in the lab or in an endstation.« less

  8. A structural study of bone changes in knee osteoarthritis by synchrotron-based X-ray fluorescence and X-ray absorption spectroscopy techniques

    NASA Astrophysics Data System (ADS)

    Sindhupakorn, Bura; Thienpratharn, Suwittaya; Kidkhunthod, Pinit

    2017-10-01

    Osteoarthritis (OA) is characterized by degeneration of articular cartilage and thickening of subchondral bone. The present study investigated the changing of biochemical components of cartilage and bone compared between normal and OA people. Using Synchrotron-based X-ray fluorescence (SR-XRF) and X-ray absorption spectroscopy (XAS) techniquesincluding X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) were employed for the bone changes in kneeosteoarthritisstudies. The bone samples were collected from various osteoarthritis patients with both male and female in the ages range between 20 and 74 years old. SR-XRF results excited at 4240 eV for Ca elements show a majority three main groups, based on their XRF intensities, 20-36 years, 40-60 years and over 70 years, respectively. By employing XAS techniques, XANES features can be used to clearly explain in term of electronic transitions occurring in bone samples which are affected from osteoarthritis symptoms. Moreover, a structural change around Ca ions in bone samples is obviously obtained by EXAFS results indicating an increase of Ca-amorphous phase when the ages increase.

  9. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2002-12-01

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

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

    SciTech Connect

    E Zschech; C Wyon; C Murray; G Schneider

    2011-12-31

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

  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. 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

  15. 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.

  16. Probing local structure of pyrochlore lead zinc niobate with synchrotron x-ray absorption spectroscopy technique

    NASA Astrophysics Data System (ADS)

    Kanchiang, Kanokwan; Pramchu, Sittichain; Yimnirun, Rattikorn; Pakawanit, Phakkhananan; Ananta, Supon; Laosiritaworn, Yongyut

    2013-08-01

    Local structure of lead zinc niobate (PZN) ceramic, synthesized via B-site oxide precursor route in atmospheric pressure, was investigated using synchrotron x-ray absorption spectroscopy (XAS) technique. The x-ray absorption near-edge structure (XANES) simulation was first carried out. The XANES simulation results indicate that the PZN ceramic is in pyrochlore phase having Zn2+ substituted on Nb5+ site. Afterwards, the extended x-ray absorption fine structure (EXAFS) analysis was performed to extract the bond length information between Zn2+ and its neighboring atoms. From the EXAFS fitting, the bond length between Zn2+ and Pb2+ in the pyrochlore phase was found to be longer than the previously reported bond length in the perovskite phase. Further, with the radial distribution information of Zn2+'s neighboring atoms, the formation energies along the precursor-to-pyrochlore and precursor-to-perovskite reaction paths were calculated using the density functional theory (DFT). The calculated results show that the formation energy of the perovskite phase is noticeably higher than that of the pyrochlore phase, which is influenced by the presence of energetic Pb2+ lone pair, as the perovskite phase has shorter Zn2+ to Pb2+ bonding. This therefore suggests the steric hindrance of Pb2+ lone pair and the mutual interactions between Pb2+ lone pair and Zn2+ are main causes of the instability of lead zinc niobate in the perovskite structure and confirm the efficacy of XAS and DFT analysis in revealing local structural details of complex pyrochlore materials.

  17. Chemical shifts of K-X-ray absorption edges on copper in different compounds by X-ray absorption spectroscopy (XAS) with Synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Joseph, D.; Basu, S.; Jha, S. N.; Bhattacharyya, D.

    2012-03-01

    Cu K X-ray absorption edges were measured in compounds such as CuO, Cu(CH3CO2)2, Cu(CO3)2, and CuSO4 where Cu is present in oxidation state of 2+, using the energy dispersive EXAFS beamline at INDUS-2 Synchrotron radiation source at RRCAT, Indore. Energy shifts of ˜4-7 eV were observed for Cu K X-ray absorption edge in the above compounds compared to its value in elemental copper. The difference in the Cu K edge energy shifts in the different compounds having same oxidation state of Cu shows the effect of different chemical environments surrounding the cation in the above compounds. The above chemical effect has been quantitatively described by determining the effective charges on Cu cations in the above compounds.

  18. 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.

  19. In situ synchrotron X-ray diffraction study of hydrides in Zircaloy-4 during thermomechanical cycling

    NASA Astrophysics Data System (ADS)

    Cinbiz, Mahmut N.; Koss, Donald A.; Motta, Arthur T.; Park, Jun-Sang; Almer, Jonathan D.

    2017-04-01

    The d-spacing evolution of both in-plane and out-of-plane hydrides has been studied using in situ synchrotron radiation X-ray diffraction during thermo-mechanical cycling of cold-worked stress-relieved Zircaloy-4. The structure of the hydride precipitates is such that the δ{111} d-spacing of the planes aligned with the hydride platelet face is greater than the d-spacing of the 111 planes aligned with the platelet edges. Upon heating from room temperature, the δ{111} planes aligned with hydride plate edges exhibit bi-linear thermally-induced expansion. In contrast, the d-spacing of the (111) plane aligned with the hydride plate face initially contracts upon heating. These experimental results can be understood in terms of a reversal of stress state associated with precipitating or dissolving hydride platelets within the α-zirconium matrix.

  20. Compressional residual stress in Bastogne boudins revealed by synchrotron X-ray microdiffraction

    SciTech Connect

    Chen, Kai; Kunz, Martin; Li, Yao; Zepeda-Alarcon, Eloisa; Sintubin, Manuel; Wenk, Hans-Rudolf

    2016-06-22

    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. We apply the new method to vein quartz from the original boudinage locality at Bastogne, Belgium. Furthermore, 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.

  1. Compressional residual stress in Bastogne boudins revealed by synchrotron X-ray microdiffraction

    DOE PAGES

    Chen, Kai; Kunz, Martin; Li, Yao; ...

    2016-06-22

    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. We apply the new method to vein quartz from the original boudinage locality at Bastogne, Belgium. Furthermore, 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 themore » geological community generally inferred by the process of boudinage.« less

  2. 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.

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

    SciTech Connect

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

    2010-01-01

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

  4. X-RAY IRRADIATION OF H{sub 2}O + CO ICE MIXTURES WITH SYNCHROTRON LIGHT

    SciTech Connect

    Jiménez-Escobar, A.; Ciaravella, A.; Micela, G.; Cecchi-Pestellini, C.; Chen, Y.-J.; Huang, C.-H. E-mail: ciarave@astropa.inaf.it E-mail: cecchi-pestellini@astropa.inaf.it E-mail: 101222023@cc.ncu.edu.tw

    2016-03-20

    We irradiated a (4:1) mixture of water and carbon monoxide with soft X-rays of energies up to 1.2 keV. The experiments were performed using the spherical grating monochromator beamline at National Synchrotron Radiation Research Center in Taiwan. Both monochromatic (300 and 900 eV) and broader energy fluxes (250–1200 eV) were employed. During the irradiation, the H{sub 2}O + CO mixture was ionized, excited, and fragmented, producing a number of reactive species. The composition of the ice has been monitored throughout both the irradiation and warm-up phases. We identified several products, which can be related through a plausible chemical reaction scheme. Such chemistry is initiated by the injection of energetic photoelectrons that produce multiple ionization events generating a secondary electron cascade. The results have been discussed in light of a model for protoplanetary disks around young solar-type stars.

  5. X-Ray Irradiation of H2O + CO Ice Mixtures with Synchrotron Light

    NASA Astrophysics Data System (ADS)

    Jiménez-Escobar, A.; Chen, Y.-J.; Ciaravella, A.; Huang, C.-H.; Micela, G.; Cecchi-Pestellini, C.

    2016-03-01

    We irradiated a (4:1) mixture of water and carbon monoxide with soft X-rays of energies up to 1.2 keV. The experiments were performed using the spherical grating monochromator beamline at National Synchrotron Radiation Research Center in Taiwan. Both monochromatic (300 and 900 eV) and broader energy fluxes (250-1200 eV) were employed. During the irradiation, the H2O + CO mixture was ionized, excited, and fragmented, producing a number of reactive species. The composition of the ice has been monitored throughout both the irradiation and warm-up phases. We identified several products, which can be related through a plausible chemical reaction scheme. Such chemistry is initiated by the injection of energetic photoelectrons that produce multiple ionization events generating a secondary electron cascade. The results have been discussed in light of a model for protoplanetary disks around young solar-type stars.

  6. 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.

  7. Applied x-ray computed tomography with high resolution in paleontology using laboratory and synchrotron sources

    NASA Astrophysics Data System (ADS)

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

    2014-09-01

    X-ray computed tomography (CT) has become an established technique in the biomedical imaging or materials science research. Its ability to non-destructively provide high-resolution images of samples makes it attractive for diverse fields of research especially the paleontology. Exceptionally, the Precambrian is a geological time of rocks deposition containing several fossilized early animals, which still need to be investigated in order to predict the origin and evolution of early life. Corumbella werneri is one of those fossils skeletonized in Corumbá (Brazil). Here, we present a study on selected specimens of Corumbella werneri using absorption-based contrast imaging at diverse tomographic setups. We investigated the potential of conventional laboratory-based device and synchrotron radiation sources to visualize internal structures of the fossils. The obtained results are discussed as well as the encountered limitations of those setups.

  8. 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.

  9. SYNCHROTRON X-RAY MICROPROBE AND COMPUTED MICROTOMOGRAPHY FOR CHARACTERIZATION OF NANOCATALYSTS.

    SciTech Connect

    JONES, K.W.; FENG, H.; LANZIROTTI, A.; MAHAJAN, D.

    2004-06-01

    Gas-to-liquids (GTL) is a viable pathway for synthesis of clean fuels from natural gas. One of the attractive synthesis options is the Fischer-Tropsch (F-T) method using an iron catalyst to yield a broad range of hydrocarbons. We collected catalyst samples during three separate F-T runs that utilized nanophase (mean particle diameter (MPD): 3 nm and 20-80 nm) and micrometer-sized (32.5 ? m) Fe{sub 2}O{sub 3} that served as catalyst precursors. The collected samples were characterized with micro x-ray fluorescence and computed Microtomography at the National Synchrotron Light Source (NSLS). Results found with two different measurement techniques indicated that there was heterogeneity on a spatial scale corresponding to volumes of roughly 10{sup 3} {micro}m{sup 3}.

  10. In situ synchrotron x-ray studies of ferroelectric thin films.

    SciTech Connect

    Fong, D. D.; Eastman, J. A.; Stephenson, G. B.; Fuoss, P. H.; Streiffer, S. K.; Thompson, C.; Auciello, O.; Materials Science Division; Northern Illinois Univ.

    2005-03-01

    In situ synchrotron X-ray scattering was used to observe both the growth of PbTiO{sub 3} films by metal-organic chemical vapor deposition and the behavior of the ferroelectric phase transition as a function of film thickness. The dependences of growth mode and deposition rate on gas flows and substrate temperature were determined by homoepitaxial growth studies on thick films (>50 nm). These studies facilitated the growth of thin coherently strained PbTiO{sub 3} films on SrTiO{sub 3} (001) substrates, with thicknesses ranging from 2 to 42 nm. Experiments on the ferroelectric phase transition as a function of film thickness were carried out in these films under controlled mechanical and electrical boundary conditions.

  11. True-3D Strain Mapping for Assessment of Material Deformation by Synchrotron X-Ray Microtomography

    SciTech Connect

    Ahn, J.J.; Toda, H.; Niinomi, M.; Kobayashi, T.; Akahori, T.; Uesugi, K.

    2005-04-09

    Downsizing of products with complex shapes has been accelerated thanks to the rapid development of electrodevice manufacturing technology. Micro electromechanical systems (MEMS) are one of such typical examples. 3D strain measurement of such miniature products is needed to ensure their reliability. In the present study, as preliminary trial for it 3D tensile deformation behavior of a pure aluminum wire is examined using the synchrotron X-ray microtomography technique at Spring-8, Japan. Multipurpose in-situ tester is used to investigate real-time tensile deformation behavior of the Al wire. Tensile tests are carried out under strokes of 0, 0.005, 0.01 and 0.015mm. It measures 3D local deformation of a region of interest by tracking a relative movement of a pair of particles at each point. Local deformation behavior of the Al wire is identified to be different from macroscopic deformation behavior. It may be closely associated with underlying microstructure.

  12. In situ synchrotron X-ray diffraction study of hydrides in Zircaloy-4 during thermomechanical cycling

    DOE PAGES

    Cinbiz, Mahmut N.; Koss, Donald A.; Motta, Arthur T.; ...

    2017-02-20

    The d-spacing evolution of both in-plane and out-of-plane hydrides has been studied using in situ synchrotron radiation X-ray diffraction during thermo-mechanical cycling of cold-worked stress-relieved Zircaloy-4. The structure of the hydride precipitates is such that the δ{111} d-spacing of the planes aligned with the hydride platelet face is greater than the d-spacing of the 111 planes aligned with the platelet edges. Upon heating from room temperature, the δ{111} planes aligned with hydride plate edges exhibit bi-linear thermally-induced expansion. In contrast, the d-spacing of the (111) plane aligned with the hydride plate face initially contracts upon heating. Furthermore, these experimental resultsmore » can be understood in terms of a reversal of stress state associated with precipitating or dissolving hydride platelets within the α-zirconium matrix.« less

  13. Issues of convection in insect respiration: insights from synchrotron X-ray imaging and beyond.

    PubMed

    Socha, John J; Förster, Thomas D; Greenlee, Kendra J

    2010-08-31

    While it has long been known that in small animals, such as insects, sufficient gas transport could be provided by diffusion, it is now recognized that animals generate and control convective flows to improve oxygen delivery across a range of body sizes and taxa. However, size-based methodological limitations have constrained our understanding of the mechanisms that underlie the production of these convective flows. Recently, new techniques have enabled the elucidation of the anatomical structures and physiological processes that contribute to creating and maintaining bulk flow in small animals. In particular, synchrotron X-ray imaging provides unprecedented spatial and temporal resolution of internal functional morphology and is changing the way we understand gas exchange in insects. This symposium highlights recent efforts towards understanding the relationship between form, function, and control in the insect respiratory system.

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

    PubMed Central

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

    2015-01-01

    Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent of lithium-ion batteries, researchers have known that the lithium metal anode has the highest theoretical energy density of any anode material. However, rechargeable batteries containing a lithium metal anode are not widely used in consumer products because the growth of lithium dendrites from the anode upon charging of the battery causes premature cell failure by short circuit. Lithium dendrites can also form in commercial lithium-ion batteries with graphite anodes if they are improperly charged. We demonstrate that lithium dendrite growth can be studied using synchrotron-based hard X-ray microtomography. This non-destructive imaging technique allows researchers to study the growth of lithium dendrites, in addition to other morphological changes inside batteries, and subsequently develop methods to extend battery life. PMID:26382323

  15. Synchrotron X-ray studies of Ti-doped NaAlH4.

    PubMed

    Canton, Patrizia; Fichtner, Maximilian; Frommen, Christoph; Léon, Aline

    2006-02-23

    Pure and doped NaAlH(4) with 5 mol % Ti on the basis of Ti(13).6THF have been investigated by means of X-ray synchrotron radiation. The Rietveld method has been used to study the possible substitution of Ti inside the NaAlH(4) structure and/or the presence of vacancies. This study indicates that there is no significant variation of the lattice parameter once the Na Alanate is doped with the Ti cluster. From the refinement of the site occupation factors, the substitution of Ti on the Na site can be excluded. A slight improvement was found when Ti was substituted on the Al site, but it is not significant enough to say that Ti definitely substitutes for Al in the Alanate phase. Additionally, there is no evidence for vacancy formation in Ti-colloid-doped sodium Alanate.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. Quantification of phosphorus in single cells using synchrotron X-ray fluorescence.

    PubMed

    Núñez-Milland, Daliángelis R; Baines, Stephen B; Vogt, Stefan; Twining, Benjamin S

    2010-07-01

    Phosphorus is required for numerous cellular compounds and as a result can serve as a useful proxy for total cell biomass in studies of cell elemental composition. Single-cell analysis by synchrotron X-ray fluorescence (SXRF) enables quantitative and qualitative analyses of cell elemental composition with high elemental sensitivity. Element standards are required to convert measured X-ray fluorescence intensities into element concentrations, but few appropriate standards are available, particularly for the biologically important element P. Empirical P conversion factors derived from other elements contained in certified thin-film standards were used to quantify P in the model diatom Thalassiosira pseudonana, and the measured cell quotas were compared with those measured in bulk by spectrophotometry. The mean cellular P quotas quantified with SXRF for cells on Au, Ni and nylon grids using this approach were not significantly different from each other or from those measured spectrophotometrically. Inter-cell variability typical of cell populations was observed. Additionally, the grid substrates were compared for their suitability to P quantification based on the potential for spectral interferences with P. Nylon grids were found to have the lowest background concentrations and limits of detection for P, while background concentrations in Ni and Au grids were 1.8- and 6.3-fold higher. The advantages and disadvantages of each grid type for elemental analysis of individual phytoplankton cells are discussed.

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

    SciTech Connect

    Wilke, M.

    1995-01-01

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

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

    SciTech Connect

    Wilke, M.D.

    1994-12-01

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

  5. 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.

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

    DOE PAGES

    Fan, D.; Huang, J. W.; Zeng, X. L.; ...

    2016-05-23

    We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantifymore » lattice deformation and fracture; diffraction peak broadening is largely caused by fracture-induced strain inhomogeneity. Finally, our results demonstrate the potential of such multiscale measurements for revealing and understanding high strain-rate phenomena at dynamic extremes.« less

  7. 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.

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

    PubMed

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

    2014-12-07

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

  9. High-throughput synchrotron X-ray diffraction for combinatorial phase mapping.

    PubMed

    Gregoire, J M; Van Campen, D G; Miller, C E; Jones, R J R; Suram, S K; Mehta, A

    2014-11-01

    Discovery of new materials drives the deployment of new technologies. Complex technological requirements demand precisely tailored material functionalities, and materials scientists are driven to search for these new materials in compositionally complex and often non-equilibrium spaces containing three, four or more elements. The phase behavior of these high-order composition spaces is mostly unknown and unexplored. High-throughput methods can offer strategies for efficiently searching complex and multi-dimensional material genomes for these much needed new materials and can also suggest a processing pathway for synthesizing them. However, high-throughput structural characterization is still relatively under-developed for rapid material discovery. Here, a synchrotron X-ray diffraction and fluorescence experiment for rapid measurement of both X-ray powder patterns and compositions for an array of samples in a material library is presented. The experiment is capable of measuring more than 5000 samples per day, as demonstrated by the acquisition of high-quality powder patterns in a bismuth-vanadium-iron oxide composition library. A detailed discussion of the scattering geometry and its ability to be tailored for different material systems is provided, with specific attention given to the characterization of fiber textured thin films. The described prototype facility is capable of meeting the structural characterization needs for the first generation of high-throughput material genomic searches.

  10. Design of x-ray diagnostic beam line for a synchrotron radiation source and measurement results

    NASA Astrophysics Data System (ADS)

    Garg, Akash Deep; Karnewar, A. K.; Ojha, A.; Shrivastava, B. B.; Holikatti, A. C.; Puntambekar, T. A.; Navathe, C. P.

    2014-08-01

    Indus-2 is a 2.5 GeV synchrotron radiation source (SRS) operational at the Raja Ramanna Centre for Advanced Technology (RRCAT) in India. We have designed, developed and commissioned x-ray diagnostic beam line (X-DBL) at the Indus-2. It is based on pinhole array imaging (8-18 keV). We have derived new equations for online measurements of source position and emission angle with pinhole array optics. Measured values are compared with the measurements at an independent x-ray beam position monitor (staggered pair blade monitor) installed in the X-DBL. The measured values are close to the theoretical expected values within ±12 μm (or ±1.5 μrad) for sufficiently wide range of the beam movements. So, beside the beam size and the beam emittance, online information for the vertical position and angle is also used in the orbit steering. In this paper, the various design considerations of the X-DBL and online measurement results are presented.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

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

    NASA Astrophysics Data System (ADS)

    Zhu, Yazhe; Cebe, Peggy

    2014-03-01

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

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

    PubMed

    Erdélyi, M; Lajkó, M; Kákonyi, R; Szabó, G

    2009-02-01

    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 microm deep cracks. The surface roughness on the island is typically below 1 microm, 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.

  17. Synchrotron x-ray diffraction studies for zincite and ceria under high pressure conditions

    NASA Astrophysics Data System (ADS)

    Wang, L.; Liu, H.; Sinogeikin, S.; Shu, J.; Mao, H.

    2007-12-01

    Certificated by National Institute of Standards & Technology (NIST), the ZnO and CeO2 powders are intended for use as internal standards for quantitative x-ray diffraction (XRD) analysis, and as external standards for checking the intensity response of x-ray diffraction instruments. For the current high pressure XRD beamlines in synchrotron sources, these oxide powders are normally used as calibration standards at ambient conditions. It is also possible to use these standards as internal standards via their well measured equation of state (EoS). For example, use the wurtzite phase of ZnO to calibrate the wavelength and the distance between sample and detector at ambient conditions. Then use its well-known wurtzite-to-rocksalt type phase transition at 9.3 GPa as fixed point. Its simple rocksalt structure could support such calibrations since we observed its structural stability to high pressure from 10 GPa to at least 215 GPa. A series of synchrotron XRD experimental results will be presented: CeO2 in helium pressure medium up to phase transition pressure; ZnO at high pressure conditions in various pressure media, and the rocksalt phase stability above 200 GPa. High pressure and low temperature down to 15K XRD experiments were also performed for ZnO to fulfill its wurtzite-to-rocksalt type phase transition boundary at low temperature domain. The internal atomic pre-transition distortion effect at low temperature and high pressure will be discussed combine the first-principles calculations results.

  18. Characterization and quantification of cerebral edema induced by synchrotron x-ray microbeam radiation therapy

    NASA Astrophysics Data System (ADS)

    Serduc, Raphaël; van de Looij, Yohan; Francony, Gilles; Verdonck, Olivier; van der Sanden, Boudewijn; Laissue, Jean; Farion, Régine; Bräuer-Krisch, Elke; Siegbahn, Erik Albert; Bravin, Alberto; Prezado, Yolanda; Segebarth, Christoph; Rémy, Chantal; Lahrech, Hana

    2008-03-01

    Cerebral edema is one of the main acute complications arising after irradiation of brain tumors. Microbeam radiation therapy (MRT), an innovative experimental radiotherapy technique using spatially fractionated synchrotron x-rays, has been shown to spare radiosensitive tissues such as mammal brains. The aim of this study was to determine if cerebral edema occurs after MRT using diffusion-weighted MRI and microgravimetry. Prone Swiss nude mice's heads were positioned horizontally in the synchrotron x-ray beam and the upper part of the left hemisphere was irradiated in the antero-posterior direction by an array of 18 planar microbeams (25 mm wide, on-center spacing 211 mm, height 4 mm, entrance dose 312 Gy or 1000 Gy). An apparent diffusion coefficient (ADC) was measured at 7 T 1, 7, 14, 21 and 28 days after irradiation. Eventually, the cerebral water content (CWC) was determined by microgravimetry. The ADC and CWC in the irradiated (312 Gy or 1000 Gy) and in the contralateral non-irradiated hemispheres were not significantly different at all measurement times, with two exceptions: (1) a 9% ADC decrease (p < 0.05) was observed in the irradiated cortex 1 day after exposure to 312 Gy, (2) a 0.7% increase (p < 0.05) in the CWC was measured in the irradiated hemispheres 1 day after exposure to 1000 Gy. The results demonstrate the presence of a minor and transient cellular edema (ADC decrease) at 1 day after a 312 Gy exposure, without a significant CWC increase. One day after a 1000 Gy exposure, the CWC increased, while the ADC remained unchanged and may reflect the simultaneous presence of cellular and vasogenic edema. Both types of edema disappear within a week after microbeam exposure which may confirm the normal tissue sparing effect of MRT. For more information on this article, see medicalphysicsweb.org

  19. 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.

  20. Specifying the surface finish of x-ray mirrors

    SciTech Connect

    Church, E.L.; Takacs, P.Z.

    1993-12-31

    Our measurements of x-ray mirrors at Brookhaven indicate that the power spectral densities of their finish errors have inverse power-law or fractal forms, rather than being flat at low frequencies as is usually assumed. This paper reviews these data and discusses how this apparent divergent behavior leads to finite but unconventional effects in imaging. Results are then used to develop more rational and realistic surface-finish specifications.

  1. 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.

  2. Direct determination of cadmium speciation in municipal solid waste fly ashes by synchrotron radiation induced mu-X-ray fluorescence and mu-X-ray absorption spectroscopy.

    PubMed

    Pinzani, Maria Caterina Camerani; Somogyi, Andrea; Simionovici, Alexandre S; Ansell, Stuart; Steenari, Britt-Marie; Lindqvist, Oliver

    2002-07-15

    Cadmium is a toxic metal that causes environmental concern in connection with utilization and land filling of ash from combustion of municipal solid waste (MSW). Collecting information about the chemical associations of Cd in ash is fundamental since this affects its solubility and leachability from the ash material. In the work presented here, the content, distribution, and chemical forms of toxic metals especially of Cd on/in individual Municipal Solid Waste (MSW) fly ash particles have been investigated in situ by synchrotron radiation induced mu-X-ray fluorescence and absorption spectrometry. The use of an excitation energy of 27 keV made it possible to detect trace metals, such as Cd, present at ppm levels routinely. Changing the excitation energy in the vicinity of the absorption edge of Cd (26.71 keV), the absorption spectra of this element were measured for the first time in this high energy range in micron-sized spots of individual fly ash particles. The measurements indicated Cd to be preferably concentrated in some small areas ("hot-spots") with high concentration (up to 200 ppm) rather than in a homogeneous distribution or as a thin coating on the whole particle surface, making the surface-reaction the most probable mechanism of Cd enrichment during MSW combustion processes. Comparisons of XAS spectra of fly ashes and reference compounds showed that in the particles studied Cd is present in the oxidation state +2. Analyses of linear combinations of standard spectra allowed estimating the Cd presence within fly ash particles as an admixture of primarily CdSO4, CdO, and CdCl2 as well as an unidentified compound not included as a standard.

  3. 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

  4. Unraveling wetting transition through surface textures with X-rays: liquid meniscus penetration phenomena.

    PubMed

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

    2014-02-11

    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.

  5. High-resolution mucociliary transport measurement in live excised large animal trachea using synchrotron X-ray imaging.

    PubMed

    Donnelley, Martin; Morgan, Kaye S; Awadalla, Maged; Farrow, Nigel R; Hall, Chris; Parsons, David W

    2017-05-16

    The Australian Synchrotron Imaging and Medical Beamline (IMBL) was designed as the world's widest synchrotron X-ray beam, enabling both clinical imaging and therapeutic applications for humans as well as the imaging of large animal models. Our group is developing methods for imaging the airways of newly developed CF animal models that display human-like lung disease, such as the CF pig, and we expect that the IMBL can be utilised to image airways in animals of this size. This study utilised samples of excised tracheal tissue to assess the feasibility, logistics and protocols required for airway imaging in large animal models such as pigs and sheep at the IMBL. We designed an image processing algorithm to automatically track and quantify the tracheal mucociliary transport (MCT) behaviour of 103 μm diameter high refractive index (HRI) glass bead marker particles deposited onto the surface of freshly-excised normal sheep and pig tracheae, and assessed the effects of airway rehydrating aerosols. We successfully accessed and used scavenged tracheal tissue, identified the minimum bead size that is visible using our chosen imaging setup, verified that MCT could be visualised, and that our automated tracking algorithm could quantify particle motion. The imaging sequences show particles propelled by cilia, against gravity, up the airway surface, within a well-defined range of clearance speeds and with examples of 'clumping' behaviour that is consistent with the in vivo capture and mucus-driven transport of particles. This study demonstrated that the wide beam at the IMBL is suitable for imaging MCT in ex vivo tissue samples. We are now transitioning to in vivo imaging of MCT in live pigs, utilising higher X-ray energies and shorter exposures to minimise motion blur.

  6. High-resolution non-invasive 3D imaging of paint microstructure by synchrotron-based X-ray laminography

    NASA Astrophysics Data System (ADS)

    Reischig, Péter; Helfen, Lukas; Wallert, Arie; Baumbach, Tilo; Dik, Joris

    2013-06-01

    The characterisation of the microstructure and micromechanical behaviour of paint is key to a range of problems related to the conservation or technical art history of paintings. Synchrotron-based X-ray laminography is demonstrated in this paper to image the local sub-surface microstructure in paintings in a non-invasive and non-destructive way. Based on absorption and phase contrast, the method can provide high-resolution 3D maps of the paint stratigraphy, including the substrate, and visualise small features, such as pigment particles, voids, cracks, wood cells, canvas fibres etc. Reconstructions may be indicative of local density or chemical composition due to increased attenuation of X-rays by elements of higher atomic number. The paint layers and their interfaces can be distinguished via variations in morphology or composition. Results of feasibility tests on a painting mockup (oak panel, chalk ground, vermilion and lead white paint) are shown, where lateral and depth resolution of up to a few micrometres is demonstrated. The method is well adapted to study the temporal evolution of the stratigraphy in test specimens and offers an alternative to destructive sampling of original works of art.

  7. Structural Analysis on Reduced Graphene Oxide Prepared from Old Coconut Shell by Synchrotron X-Ray Scattering

    NASA Astrophysics Data System (ADS)

    Yogi Nugraheni, Ananda; Jayanti, Dwi Noor; Kurniasari; Soontaranon, Siriwat; Giri Rachman Putra, Edy; Darminto

    2017-05-01

    This work is aimed to identify the distribution of size and structure of the reduced graphene oxide (rGO) particles before and after the mechanical exfoliation process from coconut shell. The burnt sample was heated at 400°C in ambient air, followed by sonication and centrifugation method for various concentration. The characterization were performed by using wide angle X-ray scattering (WAXS) and synchrotron small angle X-ray scattering (SAXS). Based on SAXS result, the structure of rGO showed that in low range of momentum transfer (Q), the particle size was too big to be measured using SAXS. In the high Q, the graph shown the apparent absence of change in curvature which indicates that the small particles are typically seen on high Q range, having aggregate with a new shape and big particles. The average fitting slope is -3.3, implying that the particles structure tends to be fractal (rough) surface, where the particles form aggregates to become bigger size and irregular structure. Further, the WAXS characterization shows that the exfoliation step has not affected the rGO phase formed.

  8. Synchrotron x-ray multiple diffraction in the study of Fe+ ion implantation in Si(0 0 1)

    NASA Astrophysics Data System (ADS)

    dos Santos, A. O.; Lang, R.; de Menezes, A. S.; Meneses, E. A.; Amaral, L.; Reboh, S.; Cardoso, L. P.

    2009-10-01

    In this work, x-ray multiple diffraction has been used as a three-dimensional high-resolution probe to study the Fe+ ion implantation process in Si(0 0 1). The semiconducting β-FeSi2 crystallographic phase has been synthesized by Fe ion co-implantation in Si(0 0 1) followed by ion-beam-induced epitaxial crystallization (IBIEC) and thermal treatment. This phase was clearly detected by the conventional techniques, micro-Raman scattering spectroscopy, transmission electron microscopy (TEM) and grazing incidence x-ray diffraction. Synchrotron radiation rocking curves (ω-scans) and mapping of the Bragg surface diffraction (BSD) of the Si matrix, as-implanted, after the IBIEC process and thermally treated, have enabled the detection of co-implanted regions formation that present distinct lattices in comparison with the matrix one clearly observed by TEM. Also, the compressive strain of both regions in depth by rocking curve and in-plane has been determined by using BSD, which is one order of magnitude smaller.

  9. 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.

  10. 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.

  11. 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.

  12. Synchrotron X-ray footprinting as a method to visualize water in proteins

    SciTech Connect

    Gupta, Sayan; Feng, Jun; Chan, Leanne Jade G.; Petzold, Christopher J.; Ralston, Corie Y.

    2016-07-27

    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. Recently, 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. Finally, 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.

  13. Synchrotron X-ray footprinting as a method to visualize water in proteins

    DOE PAGES

    Gupta, Sayan; Feng, Jun; Chan, Leanne Jade G.; ...

    2016-07-27

    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 approachmore » 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. Recently, 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. Finally, 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.« less

  14. Synchrotron X-ray footprinting as a method to visualize water in proteins

    PubMed Central

    Gupta, Sayan; Feng, Jun; Chan, Leanne Jade G.; Petzold, Christopher J.; Ralston, Corie Y.

    2016-01-01

    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

  15. 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.

  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. 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.

  18. 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.

  19. Time-resolved structural studies at synchrotrons and X-ray free electron lasers: opportunities and challenges

    PubMed Central

    Neutze, Richard; Moffat, Keith

    2012-01-01

    X-ray free electron lasers (XFELs) are potentially revolutionary X-ray sources because of their very short pulse duration, extreme peak brilliance and high spatial coherence, features that distinguish them from today’s synchrotron sources. We review recent time-resolved Laue diffraction and time-resolved wide angle X-ray scattering (WAXS) studies at synchrotron sources, and initial static studies at XFELs. XFELs have the potential to transform the field of time-resolved structural biology, yet many challenges arise in devising and adapting hardware, experimental design and data analysis strategies to exploit their unusual properties. Despite these challenges, we are confident that XFEL sources are poised to shed new light on ultrafast protein reaction dynamics. PMID:23021004

  20. Time-Resolved Synchrotron X-ray Diffraction on Pulse Laser Heated Iron in Diamond Anvil Cell

    SciTech Connect

    Yoo, C S; Wei, H; Dias, R; Shen, G; Smith, J; Chen, J Y; Evans, W

    2011-09-21

    The authors present time-resolved synchrotron x-ray diffraction to probe the {var_epsilon}-{delta} phase transition of iron during pulse-laser heating in a diamond anvil cell. The system utilizes a monochromatic synchrotron x-ray beam, a two-dimensional pixel array x-ray detector and a dual beam, double side laser-heating system. Multiple frames of the diffraction images are obtained in real-time every 22 ms over 500 ms of the entire pulse heating period. The results show the structural evolution of iron phases at 17 GPa, resulting in thermal expansion coefficient 1/V({Delta}V/{Delta}T){sub p} = 7.1 * 10{sup -6}/K for {var_epsilon}-Fe and 2.4 * 10{sup -5}/K for {gamma}-Fe, as well as the evidence for metastability of {gamma}-Fe at low temperatures below the {var_epsilon}-{gamma} phase boundary.

  1. Development of high-repetition-rate X-ray chopper system for time-resolved measurements with synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Osawa, Hitoshi; Kudo, Togo; Kimura, Shigeru

    2017-04-01

    A high-repetition-rate X-ray chopper system has been developed for pump–probe time-resolved measurements with synchrotron radiation. This system has a rotating disc with 108 or 54 grooves (X-ray path on the disc) that provides an opening time of 1.17 or 0.52 µs with a rotating speed of 28,997 rpm. Also, this system could select single-pulse X-rays every 4 or 8 periods of the several-bunch structure operated at SPring-8, corresponding to an X-ray pulse frequency of 52.2 or 26.1 kHz, respectively, and is suitable for pump–probe studies of electronic devices such as next-generation memory devices.

  2. Quantifying X-Ray Pleochroism Effects in Synchrotron Micro-XANES Microanalyses of Elemental Oxidation States: Feldspar and Biotite

    NASA Technical Reports Server (NTRS)

    Delaney, J. S.; Dyar, M. D.; Sutton, S. R.

    2001-01-01

    X-ray pleochroism is a predictable source of scatter in synchrotron microXANES analyses of elemental oxidation states. The magnitude of the effect is illustrated and a procedure to compensate for it has been implemented, reducing errors significantly. Additional information is contained in the original extended abstract.

  3. An Efficient Referencing And Sample Positioning System To Investigate Heterogeneous Substances With Combined Microfocused Synchrotron X-ray Techniques

    SciTech Connect

    Spangenberg, Thomas; Goettlicher, Joerg; Steininger, Ralph

    2009-01-29

    A referencing and sample positioning system has been developed to transfer object positions measured with an offline microscope to a synchrotron experimental station. The accuracy should be sufficient to deal with heterogeneous samples on micrometer scale. Together with an online fluorescence mapping visualisation the optical alignment helps to optimize measuring procedures for combined microfocused X-ray techniques.

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

    PubMed Central

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

    2013-01-01

    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. PMID:23412478

  6. 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.

  7. Multispecies Biofilms Transform Selenium Oxyanions into Elemental Selenium Particles: Studies Using Combined Synchrotron X-ray Fluorescence Imaging and Scanning Transmission X-ray Microscopy

    SciTech Connect

    Yang, Soo In; George, Graham N.; Lawrence, John R.; Kaminskyj, Susan G. W.; Dynes, James J.; Lai, Barry; Pickering, Ingrid J.

    2016-10-04

    Selenium (Se) is an element of growing environmental concern, because low aqueous concentrations can lead to biomagnification through the aquatic food web. Biofilms, naturally occurring microbial consortia, play numerous important roles in the environment, especially in biogeochemical cycling of toxic elements in aquatic systems. The complexity of naturally forming multispecies biofilms presents challenges for characterization because conventional microscopic techniques require chemical and physical modifications of the sample. Here, multispecies biofilms biotransforming selenium oxyanions were characterized using X-ray fluorescence imaging (XFI) and scanning transmission X-ray microscopy (STXM). These complementary synchrotron techniques required minimal sample preparation and were applied correlatively to the same biofilm areas. Sub-micrometer XFI showed distributions of Se and endogenous metals, while Se K-edge X-ray absorption spectroscopy indicated the presence of elemental Se (Se0). Nanoscale carbon K-edge STXM revealed the distributions of microbial cells, extracellular polymeric substances (EPS), and lipids using the protein, saccharide, and lipid signatures, respectively, together with highly localized Se0 using the Se LIII edge. Transmission electron microscopy showed the electron-dense particle diameter to be 50–700 nm, suggesting Se0 nanoparticles. The intimate association of Se0 particles with protein and polysaccharide biofilm components has implications for the bioavailability of selenium in the environment.

  8. 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.

  9. Theoretical analysis of the background intensity distribution in X-ray Birefringence Imaging using synchrotron bending-magnet radiation

    NASA Astrophysics Data System (ADS)

    Sutter, John P.; Dolbnya, Igor P.; Collins, Stephen P.; Harris, Kenneth D. M.; Edwards-Gau, Gregory R.; Palmer, Benjamin A.

    2015-04-01

    In the recently developed technique of X-ray Birefringence Imaging, molecular orientational order in anisotropic materials is studied by exploiting the birefringence of linearly polarized X-rays with energy close to an absorption edge of an element in the material. In the experimental setup, a vertically deflecting high-resolution double-crystal monochromator is used upstream from the sample to select the appropriate photon energy, and a horizontally deflecting X-ray polarization analyzer, consisting of a perfect single crystal with a Bragg reflection at Bragg angle of approximately 45°, is placed downstream from the sample to measure the resulting rotation of the X-ray polarization. However, if the experiment is performed on a synchrotron bending-magnet beamline, then the elliptical polarization of the X-rays out of the electron orbit plane affects the shape of the output beam. Also, because the monochromator introduces a correlation between vertical position and photon energy to the X-ray beam, the polarization analyzer does not select the entire beam, but instead selects a diagonal stripe, the slope of which depends on the Bragg angles of the monochromator and the polarization analyzer. In the present work, the final background intensity distribution is calculated analytically because the phase space sampling methods normally used in ray traces are too inefficient for this setup. X-ray Birefringence Imaging data measured at the Diamond Light Source beamline B16 agree well with the theory developed here.

  10. 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.

  11. Synchrotron X-ray topography analysis of local damage occurring during polishing of 4H-SiC wafers

    NASA Astrophysics Data System (ADS)

    Sasaki, Masayuki; Matsuhata, Hirofumi; Tamura, Kentaro; Sako, Hideki; Kojima, Kazutoshi; Yamaguchi, Hirotaka; Kitabatake, Makoto

    2015-09-01

    Surface defects with a scratch-like appearance are often observed locally on 4H-SiC wafers after epitaxial film (epi-film) growth. Since optical microscopy has only revealed a very flat surface after chemo-mechanical polishing (CMP) and before epi-film growth, the origins of these scratch-like surface defects have remained unknown. Therefore, we investigated the generation mechanism of such surface defects by synchrotron Berg-Barrett X-ray topography. Although only highly flat surfaces are observed by optical microscopy, we found that damaged regions comprising lattice defects are often introduced locally during polishing in the subsurface region. These lattice defects are almost completely removed by hydrogen etching, a pre-process for epi-film growth; however, surface defects associated with step bunching are formed in such damaged areas of the wafer surface. It is clear that local surface defects develop into surface defects with a scratch-like appearance during epi-film growth.

  12. 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.

  13. 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.

  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. Use of Synchrotron X-ray Fluorescence to Measure Trace Metal Distribution in the Brain

    NASA Astrophysics Data System (ADS)

    Linkous, D.; Flinn, J. M.; Lanzirotti, A.; Frederickson, C.; Jones, B. F.; Bertsch, P. M.

    2002-12-01

    X26A, National Synchrotron Light Source, was used to quantitatively evaluate the spatial distribution of trace metals, such as Zn and Cu, in brain tissue. X-ray microprobe techniques offer distinct advantages over other analytical methods by allowing analyses to be done in-situ with little or no chemical pretreatment and low detection limits (about 1 ppm). In the context of neuroscience, SXRF can provide non-destructive measurements of specific metal concentrations and distribution within nerve (brain) tissue. Neuronal tissue from organisms having undergone different normal or experimental conditions may be compared, with analytical capacities not limited by binding states of the metal (i.e., vesicular or enzymatic), as is the case with staining techniques.. Whole regions of tissue may be scanned for detectable trace metals at spatial resolutions of 10um or less using focused monochromatic x-ray beams. Here special attention has been given to zinc because it is the most common trace metal in the brain, and levels have been increasing in the environment. In this investigation, zinc concentrations present within the hilus of a rat hippocampus, and to a lesser extent in the cortex, have been shown to increase following long-term ingestion of zinc-enhanced drinking water that was associated with deficits in spatial memory. Concomitantly, copper concentrations in the internal capsule were comparatively lower. Other first order transition metals, Cr, V, Mn, and Co were not detected. In contrast, elevated levels of Zn, Cu, and Fe have been seen in amyloid plaques associated with Alzheimer's disease.

  16. Development of an in situ temperature stage for synchrotron X-ray spectromicroscopy.

    PubMed

    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 CuIn(x)Ga(1-x)Se2 (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.

  17. In Situ X-ray Synchrotron Tomographic Imaging During the Compression of Hyperelastic Polymeric Materials

    SciTech Connect

    Patterson, Brian M.; Cordes, Nikolaus L.; Henderson, Kevin; Williams, Jason J.; Stannard, Tyler; Singh, Sudhanshu S.; Ovejero, Angel Rodriguez; Xiao, Xianghui; Robinson, Mathew; Chawla, Nikhilesh

    2016-01-01

    Cellular structures are present in many modern and natural materials and their proper utilization is crucial within many industries. Characterizing their structural and mechanical properties is complicated, in that they often have a stochastic cellular structure, and in addition, they often have hyperelastic (i.e., non-linear) mechanical properties. Understanding the 3D structure and the dynamic response of polymer foams to mechanical stress is key to predicting lifetime performance, damage pathways, and stress recovery. Therefore, to gain a more complete picture, experiments which are designed to understand their mechanical properties must simultaneously acquire performance metrics during loading. In situ synchrotron X-ray computed tomography (CT) can image these cellular materials in 3D during uniaxial compression at a 10-2 s-1 strain rate. By utilizing the high X-ray photon flux and high speed camera provided by beamline 2-BM at the Advanced Photon Source (APS), it is possible to collect a full 3D tomogram (900 radiographs as the sample is rotated 180°) within 1 s. Rotating the sample stage in a washing machine motion allows for a 1 s tomogram to be collected every fifth second. In this study, a series of 20 tomograms were collected as the sample was continuously stressed to a nominal 60% compression. Several types of silicone foams with various structures were used to explore this technique. Stress-strain curves, collected simultaneously with the 3D tomograms, can be used to directly correlate the morphology with the mechanical performance and visualize in real-time, the buckling of ligaments. In addition, this method allows for the accurate measurement of the Poisson’s ratio as a function of compression. Coupling this moderate strain rate 3D data with finite element analysis provides a direct comparison between the true mechanical response and the modeled performance and adds a level of robustness that is not possible with other techniques

  18. Corrosion of an alloy studied in situ with synchrotron x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Renner, Frank; Lee, Tien-Lin; Kolb, Dieter M.; Stierle, Andreas; Dosch, Helmut; Zegenhagen, Jorg

    2004-03-01

    Corrosion processes are mostly electrochemical in nature. For the basic understanding of corrosion and similar technical processes, in-situ structural methods capable of atomic resolution, such as scanning probe microscopy or hard X-ray techniques are necessary. We used in-situ X-ray diffraction and in addition ex-situ AFM, to study Cu_3Au(111) single crystal surfaces in 0.1M H_2SO4 electrolyte as a function of electrode potential in the sub-critical regime. This binary metal alloys serves as model systems for more complicated technically utilized metal alloys. During the initial electrochemical corrosion, Cu atoms are dissolved and a passivating layer is formed. The experiments show the formation of an epitaxial and highly strained ultra-thin Cu_xAu_1-x(111) phase on the surface at a potential where Cu dissolution starts. At higher potentials, thicker epitaxial Au islands are growing on the surface. AFM images reveal a surface, densely packed with Au islands of a homogeneous size-distribution. On a prolonged timescale, a percolating, porous morphology of the surface evolves by ripening, even at an electrode potential well below the critical potential.

  19. Characterization of Fatigue Crack Growth Behavior in LENS Fabricated Ti-6Al-4V Using High-Energy Synchrotron X-Ray Microtomography (Postprint)

    DTIC Science & Technology

    2016-03-30

    CHARACTERIZATION OF FATIGUE CRACK GROWTH BEHAVIOR IN LENS FABRICATED TI-6AL-4V USING HIGH- ENERGY SYNCHROTRON X - RAY MICROTOMOGRAPHY (POSTPRINT...20 μm initial crack in LENS fabricated Ti-6Al-4V was captured in-situ, using high-energy synchrotron x - ray microtomography. Fatigue crack growth (FCG...measure long and small crack growth. The observed agreement demonstrates that x - ray microtomography and fractographic analysis using SEM can be

  20. 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

  1. The X-Ray Surface Forces Apparatus: Structure of a Thin Smectic Liquid Crystal Film Under Confinement

    NASA Astrophysics Data System (ADS)

    Idziak, Stefan H. J.; Safinya, Cyrus R.; Hill, Robert S.; Kraiser, Keith E.; Ruths, Marina; Warriner, Heidi E.; Steinberg, Suzi; Liang, Keng S.; Israelachvili, Jacob N.

    1994-06-01

    An x-ray surface forces apparatus for simultaneously measuring forces and structures of confined complex fluids under static and flow conditions is described. This apparatus, combined with an intense synchrotron x-ray source, allows investigation of molecular orientations within a thin liquid crystal film confined between two shearing mica surfaces 3900 angstroms apart. The layer-forming smectic liquid crystal 8CB (4-cyano-4'-octylbiphenyl) adopted a series of distinct planar layer orientations, including the bulk flow-forbidden b orientation.

  2. X-ray fluorescence surface contaminant analyzer: A feasibility study

    NASA Technical Reports Server (NTRS)

    Eldridge, Hudson B.

    1988-01-01

    The bonding of liner material to the inner metal surfaces of solid rocket booster cases is adversely affected by minute amounts of impurities on the metal surface. Suitable non-destructive methods currently used for detecting these surface contaminants do not provide the means of identifying their elemental composition. The feasibility of using isotopic source excited energy dispersive X-ray fluorescence as a possible technique for elemental analysis of such contaminants is investigated. A survey is made of the elemental compositions of both D-6ac steel, a common construction material for the booster cases, and Conoco HD-2 grease, a common surface contamination. Source and detector choices that maximize signal to noise ratio in a Recessed Source Geometry are made. A Monte Carlo simulation is then made of the optimized device incorporating the latest available X-ray constants at the energy of the chosen source to determine the device's response to a D-6ac steel surface contained with Conoco HD-2 grease.

  3. 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.

  4. 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.

  5. MeV per Nucleon Ion Irradiation of Nuclear Materials with High Energy Synchrotron X-ray Characterization

    SciTech Connect

    Pellin, M. J.; Yacout, Abdellatif M.; Mo, Kun; Almer, Jonathan; Bhattacharya, S.; Mohamed, Walid; Seidman, D.; Ye, Bei; Yun, D.; Xu, Ruqing; Zhu, Shaofei

    2016-01-14

    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.

  6. 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

  7. Non-invasive airway health measurement using synchrotron x-ray microscopy of high refractive index glass microbeads

    SciTech Connect

    Donnelley, Martin Farrow, Nigel; Parsons, David; Morgan, Kaye; Siu, Karen

    2016-01-28

    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.

  8. 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.

  9. Single-cell resolution in high-resolution synchrotron X-ray CT imaging with gold nanoparticles.

    PubMed

    Schültke, Elisabeth; Menk, Ralf; Pinzer, Bernd; Astolfo, Alberto; Stampanoni, Marco; Arfelli, Fulvia; Harsan, Laura-Adela; Nikkhah, Guido

    2014-01-01

    Gold nanoparticles are excellent intracellular markers in X-ray imaging. Having shown previously the suitability of gold nanoparticles to detect small groups of cells with the synchrotron-based computed tomography (CT) technique both ex vivo and in vivo, it is now demonstrated that even single-cell resolution can be obtained in the brain at least ex vivo. Working in a small animal model of malignant brain tumour, the image quality obtained with different imaging modalities was compared. To generate the brain tumour, 1 × 10(5) C6 glioma cells were loaded with gold nanoparticles and implanted in the right cerebral hemisphere of an adult rat. Raw data were acquired with absorption X-ray CT followed by a local tomography technique based on synchrotron X-ray absorption yielding single-cell resolution. The reconstructed synchrotron X-ray images were compared with images obtained by small animal magnetic resonance imaging. The presence of gold nanoparticles in the tumour tissue was verified in histological sections.

  10. 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.

  11. Transmission X-ray scattering as a probe for complex liquid-surface structures

    SciTech Connect

    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 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.

  12. Transmission X-ray scattering as a probe for complex liquid-surface structures

    DOE PAGES

    Fukuto, Masafumi; Yang, Lin; Nykypanchuk, Dmytro; ...

    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

  13. Transmission X-ray scattering as a probe for complex liquid-surface structures

    SciTech Connect

    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 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.

  14. 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.

  15. High-resolution visualization of airspace structures in intact mice via synchrotron phase-contrast X-ray imaging (PCXI).

    PubMed

    Parsons, David W; Morgan, Kaye; Donnelley, Martin; Fouras, Andreas; Crosbie, Jeffrey; Williams, Ivan; Boucher, Richard C; Uesugi, Kentaro; Yagi, Naoto; Siu, Karen K W

    2008-08-01

    Anatomical visualization of airspace-containing organs in intact small animals has been limited by the resolution and contrast available from current imaging methods such as X-ray, micro-computed tomography and magnetic resonance imaging. Determining structural relationships and detailed anatomy has therefore relied on suitable fixation, sectioning and histological processing. More complex and informative analyses such as orthogonal views of an organ and three-dimensional structure visualizations have required different animals and image sets, laboriously processed to gather this complementary structural information. Precise three-dimensional anatomical views have always been difficult to achieve in small animals. Here we report the ability of phase-contrast synchrotron X-ray imaging to provide detailed two- and three-dimensional visualization of airspace organ structures in intact animals. Using sub-micrometre square pixel charge-coupled device array detectors, the structure and anatomy of hard and soft tissues, and of airspaces, is readily available using phase-contrast synchrotron X-ray imaging. Moreover, software-controlled volume-reconstructions of tomographic images not only provide unsurpassed image clarity and detail, but also selectable anatomical views that cannot be obtained with established histological techniques. The morphology and structure of nasal and lung airways and the middle ear are illustrated in intact mice, using two- and three-dimensional representations. The utility of phase-contrast synchrotron X-ray imaging for noninvasively localizing objects implanted within airspaces, and the detection of gas bubbles transiting live airways, are other novel features of this visualization methodology. The coupling of phase-contrast synchrotron X-ray imaging technology with software-based reconstruction techniques holds promise for novel and high-resolution non-invasive examination of airspace anatomy in small animal models.

  16. High-resolution visualization of airspace structures in intact mice via synchrotron phase-contrast X-ray imaging (PCXI)

    PubMed Central

    Parsons, David W; Morgan, Kaye; Donnelley, Martin; Fouras, Andreas; Crosbie, Jeffrey; Williams, Ivan; Boucher, Richard C; Uesugi, Kentaro; Yagi, Naoto; Siu, Karen K W

    2008-01-01

    Anatomical visualization of airspace-containing organs in intact small animals has been limited by the resolution and contrast available from current imaging methods such as X-ray, micro-computed tomography and magnetic resonance imaging. Determining structural relationships and detailed anatomy has therefore relied on suitable fixation, sectioning and histological processing. More complex and informative analyses such as orthogonal views of an organ and three-dimensional structure visualizations have required different animals and image sets, laboriously processed to gather this complementary structural information. Precise three-dimensional anatomical views have always been difficult to achieve in small animals. Here we report the ability of phase-contrast synchrotron X-ray imaging to provide detailed two- and three-dimensional visualization of airspace organ structures in intact animals. Using sub-micrometre square pixel charge-coupled device array detectors, the structure and anatomy of hard and soft tissues, and of airspaces, is readily available using phase-contrast synchrotron X-ray imaging. Moreover, software-controlled volume-reconstructions of tomographic images not only provide unsurpassed image clarity and detail, but also selectable anatomical views that cannot be obtained with established histological techniques. The morphology and structure of nasal and lung airways and the middle ear are illustrated in intact mice, using two- and three-dimensional representations. The utility of phase-contrast synchrotron X-ray imaging for non-invasively localizing objects implanted within airspaces, and the detection of gas bubbles transiting live airways, are other novel features of this visualization methodology. The coupling of phase-contrast synchrotron X-ray imaging technology with software-based reconstruction techniques holds promise for novel and high-resolution non-invasive examination of airspace anatomy in small animal models. PMID:19172736

  17. 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.

  18. 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

  19. Site-specific distribution of copper, selenium, and zinc in human kidney by synchrotron radiation induced X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Homma, Shino; Nakai, Izumi; Misawa, Syogo; Shimojo, Nobuhiro

    1995-10-01

    Distribution of trace elements such as Cu, Se, and Zn in human kidney was examined by use of nondestructive synchrotron radiation X-ray fluorescence (SR-XRF) imaging technique. All elements measured were more accumulated in the renal cortex than in the medulla. The renal Cu and Zn distributions obtained by SR-XRF imaging were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES). Furthermore, correlation analysis based on the X-ray intensity data of each analytical point showed a positive correlation of the distribution of these elements.

  20. 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

  1. From synchrotron radiation to lab source: advanced speckle-based X-ray imaging using abrasive paper.

    PubMed

    Wang, Hongchang; Kashyap, Yogesh; Sawhney, Kawal

    2016-02-05

    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.

  2. Lead tolerance and cellular distribution in Elsholtzia splendens using synchrotron radiation micro-X-ray fluorescence.

    PubMed

    Zhang, Jie; Tian, Shengke; Lu, Lingli; Shohag, M J I; Liao, Haibing; Yang, Xiaoe

    2011-12-15

    Hydroponic experiments were conducted to investigate the tolerance and spatial distribution of lead (Pb) in Elsholtzia splendens-a copper (Cu) accumulator plant using synchrotron-based micro-X-ray fluorescence. According to chlorophyll concentration and chlorophyll fluorescence parameters, E. splendens displayed certain tolerance at 100 μM Pb treatment. Lead concentration in roots, stems and leaves of E. splendens reached 45,183.6, 1657.6, and 380.9 mg kg(-1), respectively. Pb was mostly accumulated in the roots, and there were also high concentrations of Pb been transported into stems and leaves. Micro-XRF analysis of the stem and leaf cross section revealed that Pb was mostly restricted in the vascular bundles and epidermis tissues of both stem and leaf of E. splendens. The correlation between distribution of K, Ca, Zn and Pb were analyzed. There were significant positive correlations (P<0.01) among Pb and Ca, K, Zn distribution both in stem and leaf of E. splendens. However, among the three elements, Ca shared the most similar distribution pattern and the highest correlation coefficients with Pb in both stem and leaf cross section of E. splendens. This suggests that Ca may play an important role in Pb accumulation in stem and leaf of E. splendens.

  3. Synchrotron X-ray fluorescence spectroscopy of salts in natural sea ice

    NASA Astrophysics Data System (ADS)

    Obbard, Rachel W.; Lieb-Lappen, Ross M.; Nordick, Katherine V.; Golden, Ellyn J.; Leonard, Jeremiah R.; Lanzirotti, Antonio; Newville, Mathew G.

    2016-11-01

    We describe the use of synchrotron-based X-ray fluorescence spectroscopy to examine the microstructural location of specific elements, primarily salts, in sea ice. This work was part of an investigation of the location of bromine in the sea ice-snowpack-blowing snow system, where it plays a part in the heterogeneous chemistry that contributes to tropospheric ozone depletion episodes. We analyzed samples at beamline 13-ID-E of the Advanced Photon Source at Argonne National Laboratory. Using an 18 keV incident energy beam, we produced elemental maps of salts for sea ice samples from the Ross Sea, Antarctica. The distribution of salts in sea ice depends on ice type. In our columnar ice samples, Br was located in parallel lines spaced roughly 0.5 mm apart, corresponding to the spacing of lamellae in the skeletal region during initial ice growth. The maps revealed concentrations of Br in linear features in samples from all but the topmost and bottommost depths. For those samples, the maps revealed rounded features. Calibration of the Br elemental maps showed bulk concentrations to be 5-10 g/m3, with concentrations ten times larger in the linear features. Through comparison with horizontal thin sections, we could verify that these linear features were brine sheets or layers.

  4. Guiding synchrotron X-ray diffraction by multimodal video-rate protein crystal imaging

    SciTech Connect

    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.

    2016-05-16

    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. Lastly, these capabilities are well suited to support serial crystallography of crystals approaching 1 µm or less in dimension.

  5. 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.

  6. 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.

  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

    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.

  8. Synchrotron X-Ray Diffraction Studies of Olivine from Comet Wild 2

    NASA Technical Reports Server (NTRS)

    2008-01-01

    We have analyzed a collection of the Comet Wild 2 coma grains returned by the NASA Stardust Mission, using micro-area Laue diffraction equipment. The purpose of the diffraction experiment is to permit the structure refinement of olivine including site occupancies. In addition to the intrinsic importance of the olivine structures for revealing the thermal history of Wild 2 materials, we wish to test reports that olivine recovered after hypervelocity capture in silica aerogel has undergone a basic structural change due to capture heating [1]. The diffraction equipment placed at beam line BL- 4B1 of PF, KEK was developed with a micropinhole and an imaging plate (Fuji Co. Ltd.) using the Laue method combined with polychromatic X-ray of synchrotron radiation operated at energy of 2.5 GeV. The incident beam is limited to 1.6 m in diameter by a micropinhole set just upstream of the sample [2, 3]. It is essential to apply a microbeam to obtain diffracted intensities with high signal to noise ratios. This equipment has been successfully applied to various extraterrestrial materials, including meteorites and interplanetary dust particles [4]. The Laue pattern of the sample C2067,1,111,4 (Fig. 1) was successfully taken on an imaging plate after a 120 minute exposure (Fig. 2).

  9. Strains in Thermally Growing Alumina Films Measured in-situ usingSynchrotron X-rays

    SciTech Connect

    Hou, P.Y.; Paulikas, A.P.; Veal, B.W.

    2006-01-02

    Strains in thermally grown oxides have been measured in-situ, as the oxides develop and evolve. Extensive data have been acquired from oxides grown in air at elevated temperatures on different model alloys that form Al{sub 2}O{sub 3}. Using synchrotron x-rays at the Advanced Photon Source (Beamline 12BM, Argonne National Laboratory), Debye-Scherrer diffraction patterns from the oxidizing specimen were recorded every 5 minutes during oxidation and subsequent cooling. The diffraction patterns were analyzed to determine strains in the oxides, as well as phase changes and the degree of texture. To study a specimen's response to stress perturbation, the oxidizing temperature was quickly cooled from 1100 to 950 C to impose a compressive thermal stress in the scale. This paper describes this new experimental approach and gives examples from oxidized {beta}-NiAl, Fe-20Cr-10Al, Fe-28Al-5Cr and H{sub 2}-annealed Fe-28Al-5Cr (all at. %) alloys to illustrate some current understanding of the development and relaxation of growth stresses in Al{sub 2}O{sub 3}.

  10. Deformation in metallic glasses studied by synchrotron x-ray diffraction

    DOE PAGES

    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

  11. Deformation in metallic glasses studied by synchrotron x-ray diffraction

    SciTech Connect

    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, 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.

  12. Guiding synchrotron X-ray diffraction by multimodal video-rate protein crystal imaging

    SciTech Connect

    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.

    2016-05-16

    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. Lastly, these capabilities are well suited to support serial crystallography of crystals approaching 1 µm or less in dimension.

  13. Growth dynamics of pentacene thin films: Real-time synchrotron x-ray scattering study

    SciTech Connect

    Mayer, Alex C.; Ruiz, Ricardo; Malliaras, George G.; Zhou, Hua; Headrick, Randall L.; Kazimirov, Alexander

    2006-05-15

    Real-time synchrotron x-ray scattering in the anti-Bragg configuration was used to monitor the dynamics of pentacene film growth on inert substrates. A distributed-growth model, according to which pentacene molecules adsorbed on the nth layer can either nucleate and contribute to the growth of the (n+1)th layer or transfer downward and contribute to the growth of the nth layer, gave a good description of the data. For molecules adsorbed on the first and second layers, the probability of downward transfer was found to be dependent on the substrate, and independent of temperature within the range from 25 to 60 deg. C. For films grown on SiO{sub 2}, an Ehrlich-Schwoebel barrier of the order of 70 meV dominated downward transfer of pentacene molecules in layers away from the substrate. For films grown on an alkylated self-assembled monolayer, significant desorption of pentacene molecules from the substrate at elevated temperatures forced the growth mode toward the three-dimensional limit.

  14. Experimental measurement of lattice strain pole figures using synchrotron x rays

    NASA Astrophysics Data System (ADS)

    Miller, M. P.; Bernier, J. V.; Park, J.-S.; Kazimirov, A.

    2005-11-01

    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 (0.5mm) 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 0.5×0.5mm2 monochromatic (50keV) x ray beam. Entire Debye rings of data were collected for multiple lattice planes ({hkl}'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.

  15. 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

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

    SciTech Connect

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

    2014-12-11

    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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.