WorldWideScience

Sample records for surface x-ray-scattering measurements

  1. Extreme UV and X-ray scattering measurements from a rough LiF crystal surface characterized by electron micrography

    DEFF Research Database (Denmark)

    Alehyane; Arbaoui; Barchewitz

    1989-01-01

    XUV and X-ray scattering by a LiF crystal is measured. The angular distribution of the scattered radiation (ADSR) reveals characteristic features, side peaks or asymmetry. The surface of the sample is statistically characterized by a microdensitometer analysis of electron micrographs resolving th...

  2. X-ray scattering from surfaces of organic crystals

    DEFF Research Database (Denmark)

    Gidalevitz, D.; Feidenhans'l, R.; Smilgies, D.-M.

    1997-01-01

    X-ray scattering experiments have been performed on the surfaces of organic crystals. The (010) cleavage planes of beta-alanine and alpha-glycine were investigated, and both specular and off-specular crystal truncation rods were measured. This allowed a determination of the molecular layering...

  3. X-Ray-Scattering Measurements Of Strain In PEEK

    Science.gov (United States)

    Cebe, Peggy; Lowry, Lynn E.; Chung, Shirley Y.; Yavrouian, Andre H.; Gupta, Amitava

    1988-01-01

    Internal stress relieved by heating above glass-transition temperature. Report describes wide-angle x-ray scattering and differential scanning calorimetry of specimens of poly(etheretherketone) having undergone various thermal treatments. Wide-angle x-ray scattering particularly useful in determining distances between atoms, crystallinity, and related microstructurally generated phenomena, as thermal expansion and strain. Calorimetric measurements aid interpretation of scattering measurements by enabling correlation with thermal effects.

  4. X-ray scattering studies of surfaces and interfaces

    International Nuclear Information System (INIS)

    Sanyal, M.K.

    1998-01-01

    Here we shall briefly review the basics and some applications of x-ray specular reflectivity and diffuse scattering techniques. These x-ray scattering techniques are uniquely suited to study of the structure of surfaces and interfaces at atomic resolutions as they are nondestructive and can probe even interfaces which are buried. The study of structure of surfaces and interfaces is not only required in understanding physics in reduced dimensions but is also essential in developing technologically important materials

  5. Measurements of x-ray scattering from accelerator vacuum chamber surfaces, and comparison with an analytical model

    Directory of Open Access Journals (Sweden)

    G. F. Dugan

    2015-04-01

    Full Text Available This paper compares measurements and calculations of scattering of photons from technical vacuum chamber surfaces typical of accelerators. Synchrotron radiation generated by a charged particle beam in the accelerator is either absorbed, specularly reflected, or scattered by the vacuum chamber surface. This phenomenon has important implications on the operation of the accelerator. Measurements of photon scattering were made at the BESSY-II synchrotron radiation facility using samples of aluminum vacuum chamber from Cornell electron storage ring (CESR. A description of the analytic model used in the calculation is given, which takes into account the reflectivity of the material, the surface features of the sample, the wavelengths and the incident angles of the photons. The surface properties used in these calculations were obtained from measurements made from an atomic force microscope.

  6. Interference between magnetism and surface roughness in coherent soft X-ray scattering

    International Nuclear Information System (INIS)

    Rahmim, A.; Tixier, S.; Tiedje, T.; Eisebitt, S.; Lorgen, M.; Scherer, R.; Eberhardt, W.; Luning, J.; Scholl, A.

    2002-01-01

    In coherent soft x-ray scattering from magnetically ordered surfaces there are contributions to the scattering from the magnetic domains, from the surface roughness, and from the diffraction associated with the pinhole aperture used as a coherence filter. In the present work, we explore the interplay between these contributions by analyzing speckle patterns in diffusely scattered x rays from the surface of magnetic thin films. Magnetic contrast from the surface of anti ferro magnetically ordered LaFeO3 films is caused by magnetic linear dichroism in resonant x-ray scattering. The samples studied possess two types of domains with their magnetic orientations perpendicular to each other. By tuning the x-ray energy from one of the two Fe-L3 resonant absorption peaks to the other, the relative amplitudes of the x-ray scattering from the two domains is inverted which results in speckle pattern changes. A theoretical expression is derived for the intensity correlation between the speckle patterns with the magnetic contrast inverted and not inverted. The model is found to be in good agreement with the x-ray-scattering observations and independent measurements of the surface roughness. An analytical expression for the correlation function gives an explicit relation between the change in the speckle pattern and the roughness, and magnetic and aperture scattering. Changes in the speckle pattern are shown to arise from beating of magnetic scattering with the roughness scattering and diffraction from the aperture. The largest effect is found when the surface roughness scatter is comparable in intensity to the magnetic scatter

  7. Surface x-ray scattering and scanning tunneling microscopy studies at the Au(111) electrode

    International Nuclear Information System (INIS)

    Ocko, B.M.; Magnussen, O.M.; Wang, J.X.; Adzic, R.R.

    1993-01-01

    This chapter reviews Surface X-ray Scattering and Scanning Tunneling Microscopy results carried out at the Au(111) surface under electrochemical conditions. Results are presented for the reconstructed surface, and for bromide and thallium monolayers. These examples are used to illustrate the complementary nature of the techniques

  8. X-ray scattering at liquid surfaces and interfaces

    International Nuclear Information System (INIS)

    Daillant, Jean

    2000-01-01

    X-ray and neutron reflectivity techniques have become quite popular for the analysis of surfaces and interfaces over the last ten years. In this review, we discuss the specific aspects of both specular and diffuse x-ray reflectivity at liquid interfaces. We start from a model liquid surface for which the scattering cross-section can be calculated in terms of thermally excited capillary and acoustic waves, and we examine in detail the experimental consequences of the large bulk scattering and of the low q divergence of the surface scattering. Deviations from the simple calculated behaviour point to interesting phenomena which can be studied in detail, like the appearance of a bending stiffness. The method is illustrated through the discussion of representative studies of liquid surfaces, of surfactant monolayers, of liquid-liquid interfaces and of microemulsions. (author)

  9. X-ray scattering measurements from thin-foil x-ray mirrors

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; BYRNAK, BP; Hornstrup, Allan

    1992-01-01

    Thin foil X-ray mirrors are to be used as the reflecting elements in the telescopes of the X-ray satellites Spectrum-X-Gamma (SRG) and ASTRO-D. High resolution X-ray scattering measurements from the Au coated and dip-lacquered Al foils are presented. These were obtained from SRG mirrors positioned...... in a test quadrant of the telescope structure and from ASTRO-D foils held in a simple fixture. The X-ray data is compared with laser data and other surface structure data such as STM, atomic force microscopy (AFM), TEM, and electron micrography. The data obtained at Cu K-alpha(1), (8.05 keV) from all...

  10. Progresses in the measurement and evaluation of small-angle x-ray scattering data

    International Nuclear Information System (INIS)

    Bergmann, A.

    2000-08-01

    Scattering methods are a widely used technique for determining size and shape of particles in the mesoscopic size range. This work deals on the one hand with the development of instruments in the field of Small Angle x-ray Scattering (SAXS) and on the other hand with methodical contributions concerning the interpretation of small angle scattering data. After a short introduction about Small Angle Scattering (SAS) and its application in chapter one, follows in chapter two a derivation of the theory of Small Angle x-ray scattering. Thereafter indirect transformations (Generalized Indirect Fourier Transformation [GIFT], Indirect Fourier Transformation [IFT]) are discussed and in this connection the optimization of multidimensional hyper surfaces is described. There are different possibilities for optimizing such multidimensional surfaces. The pros and contras of the different optimization methods with respect to the evaluation of small angle scattering data from interacting systems are discussed in detail. Global optimization methods are mainly used, if the hypersurface, which has to be optimized, shows many local minima. The goal of the optimization is it to find the global minimum. It is essential, that the parameters of the hyper surface are independent of each other, as it is the case in the GIFT. If someone deals with problems in only few dimensions or with many boundary conditions, mostly local optimization routines are sufficient. Therefore a number of starting parameters for the optimization is chosen, which can be obtained systematically or randomly. The best solution obtained represents the result of the optimization procedure. Chapter 3 deals with the description of instruments used in the field of Small Angle x-ray Scattering. After a description of the components (x-ray sources, monochromators, detectors) of these instruments, the different beam geometries are discussed. In chapter 4 improvements of SAXS measurements on Kratky slit systems by Goebel

  11. Measurements of accurate x-ray scattering data of protein solutions using small stationary sample cells

    Science.gov (United States)

    Hong, Xinguo; Hao, Quan

    2009-01-01

    In this paper, we report a method of precise in situ x-ray scattering measurements on protein solutions using small stationary sample cells. Although reduction in the radiation damage induced by intense synchrotron radiation sources is indispensable for the correct interpretation of scattering data, there is still a lack of effective methods to overcome radiation-induced aggregation and extract scattering profiles free from chemical or structural damage. It is found that radiation-induced aggregation mainly begins on the surface of the sample cell and grows along the beam path; the diameter of the damaged region is comparable to the x-ray beam size. Radiation-induced aggregation can be effectively avoided by using a two-dimensional scan (2D mode), with an interval as small as 1.5 times the beam size, at low temperature (e.g., 4 °C). A radiation sensitive protein, bovine hemoglobin, was used to test the method. A standard deviation of less than 5% in the small angle region was observed from a series of nine spectra recorded in 2D mode, in contrast to the intensity variation seen using the conventional stationary technique, which can exceed 100%. Wide-angle x-ray scattering data were collected at a standard macromolecular diffraction station using the same data collection protocol and showed a good signal/noise ratio (better than the reported data on the same protein using a flow cell). The results indicate that this method is an effective approach for obtaining precise measurements of protein solution scattering.

  12. Measurements of accurate x-ray scattering data of protein solutions using small stationary sample cells

    International Nuclear Information System (INIS)

    Hong Xinguo; Hao Quan

    2009-01-01

    In this paper, we report a method of precise in situ x-ray scattering measurements on protein solutions using small stationary sample cells. Although reduction in the radiation damage induced by intense synchrotron radiation sources is indispensable for the correct interpretation of scattering data, there is still a lack of effective methods to overcome radiation-induced aggregation and extract scattering profiles free from chemical or structural damage. It is found that radiation-induced aggregation mainly begins on the surface of the sample cell and grows along the beam path; the diameter of the damaged region is comparable to the x-ray beam size. Radiation-induced aggregation can be effectively avoided by using a two-dimensional scan (2D mode), with an interval as small as 1.5 times the beam size, at low temperature (e.g., 4 deg. C). A radiation sensitive protein, bovine hemoglobin, was used to test the method. A standard deviation of less than 5% in the small angle region was observed from a series of nine spectra recorded in 2D mode, in contrast to the intensity variation seen using the conventional stationary technique, which can exceed 100%. Wide-angle x-ray scattering data were collected at a standard macromolecular diffraction station using the same data collection protocol and showed a good signal/noise ratio (better than the reported data on the same protein using a flow cell). The results indicate that this method is an effective approach for obtaining precise measurements of protein solution scattering.

  13. Bone composition measured by x-ray scattering

    International Nuclear Information System (INIS)

    Newton, M.; Hukins, D.W.L.

    1992-01-01

    Ten composite samples consisting of cortical bone and adipose tissue, in known proportions, were made. The intensity of monochromatic x-rays (energy 8 keV) scattered by these samples was determined as a function of the modulus of the scattering vector, K. The ratio of the heights of peaks at K values of around 134 and 22 nm -1 provided a measure of the ratio of adipose tissue to bone mineral in these samples. This method was then used to determine the ratio of adipose tissue to mineral in samples of trabecular bone from 16 vertebral bodies. The results were correlated with measurements of the bone composition determined by ashing (r = 0.66) and histomorphometry (r = 0.66). Furthermore, the ashing and histomorphometry results were correlated with each other (r = 0.68). The feasibility of using higher energy x-rays (35-80 keV) for obtaining the same information from bone within the body is briefly discussed. (author)

  14. Ion-induced nanopatterns on semiconductor surfaces investigated by grazing incidence x-ray scattering techniques

    Energy Technology Data Exchange (ETDEWEB)

    Carbone, D; Metzger, T H [ID01, ESRF, 6 rue Jules Horowitz, F-38043 Grenoble Cedex (France); Biermanns, A; Pietsch, U [Festkoerperphysik, Universitaet Siegen, D-57068 Siegen (Germany); Ziberi, B; Frost, F [Leibniz-Institut fuer Oberflaechenmodifizierung e.V., D-04318 Leipzig (Germany); Plantevin, O [Universite Paris-Sud, Centre de Spectrometrie Nucleaire et de Spectrometrie de Masse, UMR 8609, F-91405 Orsay (France)], E-mail: gcarbone@esrf.fr

    2009-06-03

    In this review we cover and describe the application of grazing incidence x-ray scattering techniques to study and characterize nanopattern formation on semiconductor surfaces by ion beam erosion under various conditions. It is demonstrated that x-rays under grazing incidence are especially well suited to characterize (sub)surface structures on the nanoscale with high spatial and statistical accuracy. The corresponding theory and data evaluation is described in the distorted wave Born approximation. Both ex situ and in situ studies are presented, performed with the use of a specially designed sputtering chamber which allows us to follow the temporal evolution of the nanostructure formation. Corresponding results show a general stabilization of the ordering wavelength and the extension of the ordering as a function of the ion energy and fluence as predicted by theory. The in situ measurements are especially suited to study the early stages of pattern formation, which in some cases reveal a transition from dot to ripple formation. For the case of medium energy ions crystalline ripples are formed buried under a semi-amorphous thick layer with a ripple structure at the surface being conformal with the crystalline/amorphous interface. Here, the x-ray techniques are especially advantageous since they are non-destructive and bulk-sensitive by their very nature. In addition, the GI x-ray techniques described in this review are a unique tool to study the evolving strain, a topic which remains to be explored both experimentally and theoretically.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Bu, Wei [Iowa State Univ., Ames, IA (United States)

    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.

  17. Study of the grazing-incidence X-ray scattering of strongly disturbed fractal surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Roshchin, B. S., E-mail: ross@crys.ras.ru; Chukhovsky, F. N.; Pavlyuk, M. D.; Opolchentsev, A. M.; Asadchikov, V. E. [Russian Academy of Sciences, Shubnikov Institute of Crystallography, Federal Research Centre “Crystallography and Photonics” (Russian Federation)

    2017-03-15

    The applicability of different approaches to the description of hard X-ray scattering from rough surfaces is generally limited by a maximum surface roughness height of no more than 1 nm. Meanwhile, this value is several times larger for the surfaces of different materials subjected to treatment, especially in the initial treatment stages. To control the roughness parameters in all stages of surface treatment, a new approach has been developed, which is based on a series expansion of wavefield over the plane eigenstate-function waves describing the small-angle scattering of incident X-rays in terms of plane q-waves propagating through the interface between two media with a random function of relief heights. To determine the amplitudes of reflected and transmitted plane q-waves, a system of two linked integral equations was derived. The solutions to these equations correspond (in zero order) to the well-known Fresnel expressions for a smooth plane interface. Based on these solutions, a statistical fractal model of an isotropic rough interface is built in terms of root-mean-square roughness σ, two-point correlation length l, and fractal surface index h. The model is used to interpret X-ray scattering data for polished surfaces of single-crystal cadmium telluride samples.

  18. Measuring helium bubble diameter distributions in tungsten with grazing incidence small angle x-ray scattering (GISAXS)

    Science.gov (United States)

    Thompson, M.; Kluth, P.; Doerner, R. P.; Kirby, N.; Riley, D.; Corr, C. S.

    2016-02-01

    Grazing incidence small angle x-ray scattering was performed on tungsten samples exposed to helium plasma in the MAGPIE and Pisces-A linear plasma devices to measure the size distributions of resulting helium nano-bubbles. Nano-bubbles were fitted assuming spheroidal particles and an exponential diameter distribution. These particles had mean diameters between 0.36 and 0.62 nm. Pisces-A exposed samples showed more complex patterns, which may suggest the formation of faceted nano-bubbles or nano-scale surface structures.

  19. Studies of Actinides Reduction on Iron Surfaces by Means of Resonant Inelastic X-ray Scattering

    International Nuclear Information System (INIS)

    Kvashnina, K.O.; Butorin, S.M.; Shuh, D.K.; Ollila, K.; Soroka, I.; Guo, J.-H.; Werme, L.; Nordgren, J.

    2006-01-01

    The interaction of actinides with corroded iron surfaces was studied using resonant inelastic x-ray scattering (RIXS) spectroscopy at actinide 5d edges. RIXS profiles, corresponding to the f-f excitations are found to be very sensitive to the chemical states of actinides in different systems. Our results clearly indicate that U(VI) (as soluble uranyl ion) was reduced to U(IV) in the form of relatively insoluble uranium species, indicating that the iron presence significantly affects the mobility of actinides, creating reducing conditions. Also Np(V) and Pu (VI) in the ground water solution were getting reduced by the iron surface to Np(IV) and Pu (IV) respectively. Studying the reduction of actinides compounds will have an important process controlling the environmental behavior. Using RIXS we have shown that actinides, formed by radiolysis of water in the disposal canister, are likely to be reduced on the inset corrosion products and prevent release from the canister

  20. Determination of line profiles on nano-structured surfaces using EUV and x-ray scattering

    Science.gov (United States)

    Soltwisch, Victor; Wernecke, Jan; Haase, Anton; Probst, Jürgen; Schoengen, Max; Krumrey, Michael; Scholze, Frank; Pomplun, Jan; Burger, Sven

    2014-09-01

    Non-imaging techniques like X-ray scattering are supposed to play an important role in the further development of CD metrology for the semiconductor industry. Grazing Incidence Small Angle X-ray Scattering (GISAXS) provides directly assessable information on structure roughness and long-range periodic perturbations. The disadvantage of the method is the large footprint of the X-ray beam on the sample due to the extremely shallow angle of incidence. This can be overcome by using wavelengths in the extreme ultraviolet (EUV) spectral range, EUV small angle scattering (EUVSAS), which allows for much steeper angles of incidence but preserves the range of momentum transfer that can be observed. Generally, the potentially higher momentum transfer at shorter wavelengths is counterbalanced by decreasing diffraction efficiency. This results in a practical limit of about 10 nm pitch for which it is possible to observe at least the +/- 1st diffraction orders with reasonable efficiency. At the Physikalisch-Technische Bundesanstalt (PTB), the available photon energy range extends from 50 eV up to 10 keV at two adjacent beamlines. PTB commissioned a new versatile Ellipso-Scatterometer which is capable of measuring 6" square substrates in a clean, hydrocarbon-free environment with full flexibility regarding the direction of the incident light polarization. The reconstruction of line profiles using a geometrical model with six free parameters, based on a finite element method (FEM) Maxwell solver and a particle swarm based least-squares optimization yielded consistent results for EUV-SAS and GISAXS. In this contribution we present scatterometry data for line gratings and consistent reconstruction results of the line geometry for EUV-SAS and GISAXS.

  1. Measurement of x-ray scattering cross sections of hydrogen and helium with synchrotron radiation

    International Nuclear Information System (INIS)

    Ice, G.E.

    1977-01-01

    Total x-ray scattering is a two-electron expectation value. The prominence of the electron correlation effect was demonstrated in recent theoretical work. Only one measurement of x-ray scattering from H 2 has been reported heretofore, nearly fifty years ago. New measurements were carried out using the virtually monochromatic, intense flux of synchrotron radiation in the SSRP EXAFS line. The targets, at 1 atm pressure, were UHP He and ultrapure H 2 that had been passed through a hot Pd--Ag alloy diffusion purifier. The scattered-photon spectra were measured with a Xe-filled proportional counter and fast multichannel analyzer. The incident flux was monitored with a parallel-plate ion chamber, calibrated by direct counting of the absorber-attenuated beam. Measurements were performed at 5, 6, and 7 keV photon energy, as a function of scattering angle (60, 90, and 135 deg) and azimuthal angle (i.e., polarization). The relative total differential photon scattering cross sections for H 2 over the range 3.0 less than or equal to x = 4πsin (theta/2)lambda less than or equal to 5.6 A -1 agree to within approx. 1% with the correlated calculations of Bentley and Stewart. The ratios of measured cross sections for H 2 to those for He at x = 3.0 and 5.6 A -1 agree to within 1% with the ratios of the Bentley--Stewart H 2 cross sections to the correlated wave-function calculations of Brown for He

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-05-15

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

  3. Oxide surfaces and metal/oxide interfaces studied by grazing incidence X-ray scattering

    Science.gov (United States)

    Renaud, Gilles

    Experimental determinations of the atomic structure of insulating oxide surfaces and metal/oxide interfaces are scarce, because surface science techniques are often limited by the insulating character of the substrate. Grazing incidence X-ray scattering (GIXS), which is not subject to charge effects, can provide very precise information on the atomic structure of oxide surfaces: roughness, relaxation and reconstruction. It is also well adapted to analyze the atomic structure, the registry, the misfit relaxation, elastic or plastic, the growth mode and the morphology of metal/oxide interfaces during their growth, performed in situ. GIXS also allows the analysis of thin films and buried interfaces, in a non-destructive way, yielding the epitaxial relationships, and, by variation of the grazing incidence angle, the lattice parameter relaxation along the growth direction. On semi-coherent interfaces, the existence of an ordered network of interfacial misfit dislocations can be demonstrated, its Burger's vector determined, its ordering during in situ annealing cycles followed, and sometimes even its atomic structure can be addressed. Careful analysis during growth allows the modeling of the dislocation nucleation process. This review emphasizes the new information that GIXS can bring to oxide surfaces and metal/oxide interfaces by comparison with other surface science techniques. The principles of X-ray diffraction by surfaces and interfaces are recalled, together with the advantages and properties of grazing angles. The specific experimental requirements are discussed. Recent results are presented on the determination of the atomic structure of relaxed or reconstructed oxide surfaces. A description of results obtained during the in situ growth of metal on oxide surfaces is also given, as well as investigations of thick metal films on oxide surfaces, with lattice parameter misfit relaxed by an array of dislocations. Recent work performed on oxide thin films having

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

    KAUST Repository

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

    2013-01-01

    Drops of exosome dispersions from healthy epithelial colon cell line and colorectal cancer cells were dried on a superhydrophobic PMMA substrate. The residues were studied by small- and wide-angle X-ray scattering using both a synchrotron radiation micrometric beam and a high-flux table-top X-ray source. Structural differences between healthy and cancerous cells were detected in the lamellar lattices of the exosome macro-aggregates. © 2013 The Royal Society of Chemistry.

  5. Dimensions and Global Twist of Single-Layer DNA Origami Measured by Small-Angle X-ray Scattering.

    Science.gov (United States)

    Baker, Matthew A B; Tuckwell, Andrew J; Berengut, Jonathan F; Bath, Jonathan; Benn, Florence; Duff, Anthony P; Whitten, Andrew E; Dunn, Katherine E; Hynson, Robert M; Turberfield, Andrew J; Lee, Lawrence K

    2018-06-04

    The rational design of complementary DNA sequences can be used to create nanostructures that self-assemble with nanometer precision. DNA nanostructures have been imaged by atomic force microscopy and electron microscopy. Small-angle X-ray scattering (SAXS) provides complementary structural information on the ensemble-averaged state of DNA nanostructures in solution. Here we demonstrate that SAXS can distinguish between different single-layer DNA origami tiles that look identical when immobilized on a mica surface and imaged with atomic force microscopy. We use SAXS to quantify the magnitude of global twist of DNA origami tiles with different crossover periodicities: these measurements highlight the extreme structural sensitivity of single-layer origami to the location of strand crossovers. We also use SAXS to quantify the distance between pairs of gold nanoparticles tethered to specific locations on a DNA origami tile and use this method to measure the overall dimensions and geometry of the DNA nanostructure in solution. Finally, we use indirect Fourier methods, which have long been used for the interpretation of SAXS data from biomolecules, to measure the distance between DNA helix pairs in a DNA origami nanotube. Together, these results provide important methodological advances in the use of SAXS to analyze DNA nanostructures in solution and insights into the structures of single-layer DNA origami.

  6. Charge-Orbital Ordering and Verwey Transition in Magnetite Measured by Resonant Soft X-Ray Scattering

    International Nuclear Information System (INIS)

    Huang, D.J.; Lin, H.-J.; Okamoto, J.; Hsu, C.-H.; Huang, C.-M.; Yang, C.S.; Chao, K.S.; Wu, W.B.; Jeng, H.-T.; Guo, G.Y.; Ling, D.C.; Chen, C.T.

    2006-01-01

    We report experimental evidence for the charge-orbital ordering in magnetite below the Verwey transition temperature T V . Measurements of O K-edge resonant x-ray scattering on magnetite reveal that the O 2p states in the vicinity of the Fermi level exhibit a charge-orbital ordering along the c axis with a spatial periodicity of the doubled lattice parameter of the undistorted cubic phase. Such a charge-orbital ordering vanishes abruptly above T V and exhibits a thermal hysteresis, correlating closely with the Verwey transition in magnetite

  7. In situ X-ray scattering studies of protein solution droplets drying on micro- and nanopatterned superhydrophobic PMMA surfaces.

    Science.gov (United States)

    Accardo, Angelo; Gentile, Francesco; Mecarini, Federico; De Angelis, Francesco; Burghammer, Manfred; Di Fabrizio, Enzo; Riekel, Christian

    2010-09-21

    Superhydrophobic poly(methyl methacrylate) surfaces with contact angles of ∼170° and high optical and X-ray transparencies have been fabricated through the use of optical lithography and plasma etching. The surfaces contain either a microscale pattern of micropillars or a random nanofibrillar pattern. Nanoscale asperities on top of the micropillars closely resemble Nelumbo nucifera lotus leaves. The evolution of the contact angle of water and lysozyme solution droplets during evaporation was studied on the micro- and nanopatterned surfaces, showing in particular contact-line pinning for the protein solution droplet on the nanopatterned surface. The microstructural evolution of lysozyme solution droplets was studied on both types of surfaces in situ under nearly contact-free conditions by synchrotron radiation microbeam wide-angle and small-angle X-ray scattering revealing the increasing protein concentration and the onset of precipitation. The solid residuals show hollow sphere morphologies. Rastermicrodiffraction of the detached residuals suggests about a 1/3 volume fraction of ≥17 nm lysozyme nanocrystalline domains and about a 2/3 short-range-order volume fraction. About 5-fold larger nanocrystalline domains were observed at the attachment points of the sphere to the substrates, which is attributed to particle growth in a shear flow. Such surfaces represent nearly contact-free sample supports for studies of inorganic and organic solution droplets, which find applications in biochips.

  8. Technique charts for EC film: direct optical measurements to account for the effects of X-ray scatter

    International Nuclear Information System (INIS)

    Munro, Peter; Jordan, Kevin; Lewis, Craig; Heerema, Tim

    2001-01-01

    Purpose: To develop a method of measuring technique charts for enhanced contrast (EC) film, to demonstrate how X-ray scatter changes the response of EC film, and to generate technique charts for general use. Methods and Materials: We have developed a 'digital cassette' - consisting of a metal plate/phosphor screen, a light guide, a photodiode sensor, and an electrometer - that can be used to measure the light generated in the phosphor screen of the film cassette. In turn, these measurements can be used to generate technique charts for EC film. The digital cassette has been used to measure technique charts for 4-MV and 6-MV X-ray beams for a variety of different phantom thicknesses, field sizes, and phantom-to-cassette air gaps. Results and Discussion: We have observed that the signals generated in an ionization chamber located 9.4 cm behind a 30-cm-thick water-equivalent phantom increase by a factor of 1.9 when the field size is increased from 4x4 cm 2 to 40x40 cm 2 when irradiated by a 6-MV X-ray beam. However, the change in EC film response is a factor of 3.5 under the same conditions. Irradiations to optimally expose the EC film predicted by the digital cassette differ by up to 82% compared to those predicted by ion chamber measurements. Nevertheless, the technique charts measured using the digital cassette predict the response of the EC film to ±0.2 optical density. The overresponse of the EC film is most likely due to low-energy scattered photons, which interact with the high atomic number (Z=64) phosphor screen of the enhanced contrast localization cassette. Therefore, simple solutions, such as placing a high atomic number material above the enhanced contrast localization cassette, can reduce this contribution by scattered photons to the signal generated in the cassettes. Conclusions: We have developed a digital cassette that can make more accurate measurements of the technique charts for EC films. Our measurements show that under some conditions, X-ray

  9. Antiferroelectric surface layers in a liquid crystal as observed by synchrotron x-ray scattering

    DEFF Research Database (Denmark)

    Gramsbergen, E. F.; de Jeu, W. H.; Als-Nielsen, Jens Aage

    1986-01-01

    The X-ray reflectivity form the surface of a liquid crystal with terminally polar (cyano substituted) molecules has been studied using a high-resolution triple-axis X-ray spectrometer in combination with a synchrotron source. It is demonstrated that at the surface of the smectic Al phase a few...... antiferroelectric double layers develop that can be distinguished from the bulk single layer structure. A model is developed that separates the electron density in a contribution from the molecular form factor, and from the structure factor of the mono- and the bilayers, respectively. It shows that (i) the first...

  10. Evaluation of the roughness of a crystal surface by X-ray scattering. Pt. 1

    International Nuclear Information System (INIS)

    Harada, Jimpei

    1992-01-01

    The relationship between the intensity distributions of the crystal truncation rod (CTR) scattering and the surface roughness of a crystal is discussed by developing a kinematic theory for the CTR scattering so as to reflect the two-dimensional aspect of the surface. The intensity of the CTR scattering elongated from a Bragg point is shown to be reduced by a factor vertical strokeΓ(q)vertical stroke 2 for a surface possessing some roughness, where Γ(q) is defined by a simple Fourier summation of γ p , the relative area with the same step height p on a surface, i.e. Γ(q) = Σ ∞ p=o γ p exp (2πipq), with Σ p γ p = 1, q being the distance in reciprocal space from the Bragg point along the CTR scattering. A pair-correlation function between the steps can, therefore, be obtained by a simple Fourier integral of the roughness damping factor vertical strokeΓ(q)vertical stroke 2 . For the case where γ p has a Gaussian distribution around the average step height, vertical strokeΓ(q)vertical stroke 2 is approximated by the well known Debye-Waller-like factor, exp (K- 4π 2 (Δp 2 )q 2 ), where (Δp 2 ) is the mean square deviation of step height in units of the lattice spacing. The intensity formulae proposed so far by several authors are also discussed on the basis of the above factor. (orig.)

  11. Proteins on surfaces investigated by microbeam grazing incidence small angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Gebhardt, Ronald; Riekel, Christian; Burghammer, Manfred [European Synchrotron Radiation Facility, B.P. 220, F-38043 Grenoble Cedex (France); Vendrely, Charlotte [Universite de Cergy-Pontoise, ERRMECE, F-95000, Cergy-Pontoise (France); Mueller-Buschbaum, Peter [TU Muenchen, Physik Department E13, Muenchen (Germany)

    2009-07-01

    Grazing incidence small angle scattering with a 1 micron x-ray beam ({mu}GISAXS) is applied to study structural ordering of casein micelles and fibroin in solution cast films. {mu}GISAXS scans provide the possibility to locate highly ordered areas and to investigate variation in the molecular packing. In the case of the casein micelles, ordered film structures have been generated by decreasing their natural size dispersion. While dynamic light scattering was used to characterize the different size fractions in solution, {mu}GISAXS and roughness are measured on the resulting casein films. GISAXS-Patterns are analyzed by simulations providing the dimension and nearest neighbor distances of casein micelles. In the case of fibroin, ordering of nano-fibers formed during the drying process is investigated. The experimental data are analyzed by simulations and compared to SEM, AFM and Raman scattering experiments.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-11-15

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

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

    Science.gov (United States)

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

    2016-12-22

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

  14. Poisson's ratio of collagen fibrils measured by small angle X-ray scattering of strained bovine pericardium

    Energy Technology Data Exchange (ETDEWEB)

    Wells, Hannah C.; Sizeland, Katie H.; Kayed, Hanan R.; Haverkamp, Richard G., E-mail: r.haverkamp@massey.ac.nz [School of Engineering and Advanced Technology, Massey University, Private Bag 11222, Palmerston North 4442 (New Zealand); Kirby, Nigel; Hawley, Adrian; Mudie, Stephen T. [Australian Synchrotron, 800 Blackburn Road, Clayton, Victoria 3168 (Australia)

    2015-01-28

    Type I collagen is the main structural component of skin, tendons, and skin products, such as leather. Understanding the mechanical performance of collagen fibrils is important for understanding the mechanical performance of the tissues that they make up, while the mechanical properties of bulk tissue are well characterized, less is known about the mechanical behavior of individual collagen fibrils. In this study, bovine pericardium is subjected to strain while small angle X-ray scattering (SAXS) patterns are recorded using synchrotron radiation. The change in d-spacing, which is a measure of fibril extension, and the change in fibril diameter are determined from SAXS. The tissue is strained 0.25 (25%) with a corresponding strain in the collagen fibrils of 0.045 observed. The ratio of collagen fibril width contraction to length extension, or the Poisson's ratio, is 2.1 ± 0.7 for a tissue strain from 0 to 0.25. This Poisson's ratio indicates that the volume of individual collagen fibrils decreases with increasing strain, which is quite unlike most engineering materials. This high Poisson's ratio of individual fibrils may contribute to high Poisson's ratio observed for tissues, contributing to some of the remarkable properties of collagen-based materials.

  15. Recent developments and ASAXS measurements at the ultra small angle X-ray scattering instrument of HASYLAB

    CERN Document Server

    Krosigk, G V; Gehrke, R; Kranold, R

    2001-01-01

    The wiggler beamline BW4 at the synchrotron radiation facility HASYLAB (DESY) is mainly designed for Ultra Small Angle X-ray Scattering (USAXS) and usually operated with detector-sample distances up to 13 m and at photon energies between 4 and 16 keV. With a new optical design the largest observable correlation distances have now been increased up to 9x10 sup 3 A. A grazing incidence set-up [P. Mueller-Buschbaum et al., Europhys. Lett. 42 (5) (1998) 517], vapor chamber, furnace, tensile testing machine and other instruments make the USAXS beamline attractive for a variety of scattering experiments [A. Endres et al., Rev. Sci. Instrum. 11 (1997) 68; A. Karl et al., J. Macromolecular Sci.-Phys. B 38 (5 and 6) (1999) 901; S. Minko et al., J. Macromolecular Sci., Phys. B 38 (5 and 6) (1999) 913]. A fully evacuated beampath allows high quality measurements with very low background signal. A photodiode mounted in the primary beam stop registers the primary beam flux simultaneously to the data acquisition and thus p...

  16. The simultaneous measurement of energy and linear polarization of the scattered radiation in resonant inelastic soft x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Braicovich, L., E-mail: lucio.braicovich@polimi.it; Minola, M.; Dellea, G.; Ghiringhelli, G. [CNR-SPIN and Dipartimento di Fisica, Politecnico di Milano, piazza Leonardo Da Vinci 32, Milano I-20133 (Italy); Le Tacon, M. [Max-Planck-Institut für Festkörperforschung, Heisenbergstrasse 1, D-70569 Stuttgart (Germany); Moretti Sala, M.; Morawe, C.; Peffen, J.-Ch.; Yakhou, F.; Brookes, N. B. [European Synchrotron Radiation Facility, 71 Avenue des Martyrs, Grenoble F-38043 (France); Supruangnet, R. [Synchrotron Light Research Institute, Nakhon Ratchasima (Thailand)

    2014-11-15

    Resonant Inelastic X-ray Scattering (RIXS) in the soft x-ray range is an element-specific energy-loss spectroscopy used to probe the electronic and magnetic excitations in strongly correlated solids. In the recent years, RIXS has been progressing very quickly in terms of energy resolution and understanding of the experimental results, but the interpretation of spectra could further improve, sometimes decisively, from a full knowledge of the polarization of incident and scattered photons. Here we present the first implementation, in a high resolution soft-RIXS spectrometer used to analyze the scattered radiation, of a device allowing the measurement of the degree of linear polarization. The system, based on a graded W/B{sub 4}C multilayer mirror installed in proximity of the CCD detector, has been installed on the AXES spectrometer at the ESRF (European Synchrotron Radiation Facility); it has been fully characterized and it has been used for a demonstration experiment at the Cu L{sub 3} edge on a high-T{sub c} superconducting cuprate. The loss in efficiency suffered by the spectrometer equipped with this test facility was a factor 17.5. We propose also a more advanced version, suitable for a routine use on the next generation of RIXS spectrometers and with an overall efficiency up to 10%.

  17. Two-temperature equilibration in warm dense hydrogen measured with x-ray scattering from the LCLS

    Science.gov (United States)

    Fletcher, Luke; High Energy Density Sciences Collaboration

    2017-10-01

    Understanding the properties of warm dense hydrogen plasmas is critical for modeling stellar and planetary interiors, as well as for inertial confinement fusion (ICF) experiments. Of central importance are the electron-ion collision and equilibration times that determine the microscopic properties in a high energy density state. Spectrally and angularly resolved x-ray scattering measurements from fs-laser heated hydrogen have resolved the picosecond evolution and energy relaxation from a two-temperature plasma towards thermodynamic equilibrium in the warm dense matter regime. The interaction of rapidly heated cryogenic hydrogen irradiated by a 400 nm, 5x1017 W/cm2 , 70 fs-laser is visualized with ultra-bright 5.5 kev x-ray pulses from the Linac Coherent Light (LCLS) source in 1 Hz repetition rate pump-probe setting. We demonstrate that the energy relaxation is faster than many classical binary collision theories that use ad hoc cutoff parameters used in the Landau-Spitzer determination of the Coulomb logarithm. This work was supported by the DOE Office of Science, Fusion Energy Science under contract No. SF00515 and supported under FWP 100182 and DOE Office of Basic Energy Sciences, Materials Sciences and Engineering Division, contract DE-AC02-76SF00515.

  18. Breast tissue classification using x-ray scattering measurements and multivariate data analysis

    Science.gov (United States)

    Ryan, Elaine A.; Farquharson, Michael J.

    2007-11-01

    This study utilized two radiation scatter interactions in order to differentiate malignant from non-malignant breast tissue. These two interactions were Compton scatter, used to measure the electron density of the tissues, and coherent scatter to obtain a measure of structure. Measurements of these parameters were made using a laboratory experimental set-up comprising an x-ray tube and HPGe detector. The breast tissue samples investigated comprise five different tissue classifications: adipose, malignancy, fibroadenoma, normal fibrous tissue and tissue that had undergone fibrocystic change. The coherent scatter spectra were analysed using a peak fitting routine, and a technique involving multivariate analysis was used to combine the peak fitted scatter profile spectra and the electron density values into a tissue classification model. The number of variables used in the model was refined by finding the sensitivity and specificity of each model and concentrating on differentiating between two tissues at a time. The best model that was formulated had a sensitivity of 54% and a specificity of 100%.

  19. Breast tissue classification using x-ray scattering measurements and multivariate data analysis

    Energy Technology Data Exchange (ETDEWEB)

    Ryan, Elaine A; Farquharson, Michael J [School of Allied Health Sciences, City University, Charterhouse Square, London EC1M 6PA (United Kingdom)

    2007-11-21

    This study utilized two radiation scatter interactions in order to differentiate malignant from non-malignant breast tissue. These two interactions were Compton scatter, used to measure the electron density of the tissues, and coherent scatter to obtain a measure of structure. Measurements of these parameters were made using a laboratory experimental set-up comprising an x-ray tube and HPGe detector. The breast tissue samples investigated comprise five different tissue classifications: adipose, malignancy, fibroadenoma, normal fibrous tissue and tissue that had undergone fibrocystic change. The coherent scatter spectra were analysed using a peak fitting routine, and a technique involving multivariate analysis was used to combine the peak fitted scatter profile spectra and the electron density values into a tissue classification model. The number of variables used in the model was refined by finding the sensitivity and specificity of each model and concentrating on differentiating between two tissues at a time. The best model that was formulated had a sensitivity of 54% and a specificity of 100%.

  20. Thermal expansion measurements by x-ray scattering and breakdown of Ehrenfest's relation in alloy liquids

    International Nuclear Information System (INIS)

    Gangopadhyay, A. K.; Blodgett, M. E.; Johnson, M. L.; Vogt, A. J.; Mauro, N. A.; Kelton, K. F.

    2014-01-01

    Measurements of sharp diffraction peaks as a function of temperature are routinely used to obtain precise linear expansion coefficients of crystalline solids. In this case, the relation between temperature dependent changes in peak position in momentum transfer (q 1 ) and volume expansion is straightforward (Ehrenfest's relation: q 1  = K(2π/d), where K is a constant and d is the interatomic spacing) and the data obtained are usually in close agreement with more direct measurements. With high intensity synchrotron x-ray and spallation neutron sources, it is also possible to accurately measure the positions of the much broader peaks for liquids and glasses. This has led to a debate on whether linear expansion coefficients derived from these data are an accurate representation of the volume expansion coefficients. We present here volume thermal expansion and x-ray diffraction data for a large number of glass-forming alloy liquids acquired in a containerless environment using the beamline electrostatic levitation technique. The data show a large difference in the values obtained from the two different techniques. Moreover, the position of the first peak (q 1 ) in the scattered intensity in the structure factor (S(q)) and the atomic volume v for all liquids follow a simple relationship, v∝(q 1 ) −ε . The exponent, ε = 2.28 (±0.11), is much different from the expected value of 3 from Ehrenfest's relation and shows no temperature dependence over the temperature range of the data collected

  1. In situ measurements of soot formation in simple flames using small angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Gardner, C. [Institute of Mathematical and Physical Sciences, University of Wales, Aberystwyth SY23 3BZ (United Kingdom); Greaves, G.N. [Institute of Mathematical and Physical Sciences, University of Wales, Aberystwyth SY23 3BZ (United Kingdom)]. E-mail: gng@aber.ac.uk; Hargrave, G.K. [Wolfson School of Mechanical and Manufacturing Engineering, Loughborough University, Loughborough LE11 3TU (United Kingdom); Jarvis, S. [Wolfson School of Mechanical and Manufacturing Engineering, Loughborough University, Loughborough LE11 3TU (United Kingdom); Wildman, P. [Wolfson School of Mechanical and Manufacturing Engineering, Loughborough University, Loughborough LE11 3TU (United Kingdom); Meneau, F. [Institute of Mathematical and Physical Sciences, University of Wales, Aberystwyth SY23 3BZ (United Kingdom); Netherlands Organisation for Scientific Research (NWO), DUBBLE CRG/ESRF, P.O. Box 220, F38043 Grenoble Cedex (France); Bras, W. [Netherlands Organisation for Scientific Research (NWO), DUBBLE CRG/ESRF, P.O. Box 220, F38043 Grenoble Cedex (France); Thomas, G. [Institute of Mathematical and Physical Sciences, University of Wales, Aberystwyth SY23 3BZ (United Kingdom)

    2005-08-15

    Direct SAXS measurements of soot formation from ethylene have been made using laminar pre-mixed flames for the first time. The slot burner was configured to maximise the signal from particulates. The geometry also enabled the thermal background from the surrounding hot gasses to be accurately removed. With cold flame speeds of 40 cm s{sup -1} we have been able to identify particle sizes and densities from moderately sooty to rich flame conditions. By adjusting the height of the burner in the beam, the development of particles as a function of position above the flame tip and therefore as a function of time from ignition have been obtained. These reveal evidence for bimodal particle nucleation and growth at different stages in the continuous combustion of ethylene.

  2. In situ measurements of soot formation in simple flames using small angle X-ray scattering

    International Nuclear Information System (INIS)

    Gardner, C.; Greaves, G.N.; Hargrave, G.K.; Jarvis, S.; Wildman, P.; Meneau, F.; Bras, W.; Thomas, G.

    2005-01-01

    Direct SAXS measurements of soot formation from ethylene have been made using laminar pre-mixed flames for the first time. The slot burner was configured to maximise the signal from particulates. The geometry also enabled the thermal background from the surrounding hot gasses to be accurately removed. With cold flame speeds of 40 cm s -1 we have been able to identify particle sizes and densities from moderately sooty to rich flame conditions. By adjusting the height of the burner in the beam, the development of particles as a function of position above the flame tip and therefore as a function of time from ignition have been obtained. These reveal evidence for bimodal particle nucleation and growth at different stages in the continuous combustion of ethylene

  3. In situ measurements of soot formation in simple flames using small angle X-ray scattering

    Science.gov (United States)

    Gardner, C.; Greaves, G. N.; Hargrave, G. K.; Jarvis, S.; Wildman, P.; Meneau, F.; Bras, W.; Thomas, G.

    2005-08-01

    Direct SAXS measurements of soot formation from ethylene have been made using laminar pre-mixed flames for the first time. The slot burner was configured to maximise the signal from particulates. The geometry also enabled the thermal background from the surrounding hot gasses to be accurately removed. With cold flame speeds of 40 cm s-1 we have been able to identify particle sizes and densities from moderately sooty to rich flame conditions. By adjusting the height of the burner in the beam, the development of particles as a function of position above the flame tip and therefore as a function of time from ignition have been obtained. These reveal evidence for bimodal particle nucleation and growth at different stages in the continuous combustion of ethylene.

  4. Crystallization behavior of polyethylene on silicon wafers in solution casting processes traced by time-resolved measurements of synchrotron grazing-incidence small-angle and wide-angle X-ray scattering

    International Nuclear Information System (INIS)

    Sasaki, S; Masunaga, H; Takata, M; Itou, K; Tashiro, K; Okuda, H; Takahara, A

    2009-01-01

    Crystallization behavior of polyethylene (PE) on silicon wafers in solution casting processes has been successfully traced by time-resolved grazing-incidence small-angle and wide-angle X-ray scattering (GISWAXS) measurements utilizing synchrotron radiation. A p-xylene solution of PE kept at ca. 343 K was dropped on a silicon wafer at ca. 298 K. While the p-xylene evaporated naturally from the dropped solution sample, PE chains crystallized to be a thin film. Raman spectral measurements were performed simultaneously with the GISWAXS measurements to evaluate quantitatively the p-xylene the dropped solution contained. Grazing-incidence wide-angle X-ray scattering (GIWAXS) patterns indicated nucleation and crystal growth in the dropped solution and the following as-cast film. GIWAXS and Raman spectral data revealed that crystallization of PE was enhanced after complete evaporation of the p-xylene from the dropped solution. The [110] and [200] directions of the orthorhombic PE crystal became relatively parallel to the wafer surface with time, which implied that the flat-on lamellae with respect to the wafer surface were mainly formed in the as-cast film. On the other hand, grazing-incidence small-angle X-ray scattering (GISAXS) patterns implied formation of isolated lamellae in the dropped solution. The lamellae and amorphous might alternatively be stacked in the preferred direction perpendicular to the wafer surface. The synchrotron GISWAXS experimental method could be applied for kinetic study on hierarchical structure of polymer thin films.

  5. Measurement of illite particle thickness using a direct Fourier transform of small-angle X-ray scattering data

    Science.gov (United States)

    Shang, Chao; Rice, James A.; Eberl, Dennis D.; Lin, Jar-Shyong

    2003-01-01

    It has been suggested that interstratified illite-smectite (I-S) minerals are composed of aggregates of fundamental particles. Many attempts have been made to measure the thickness of such fundamental particles, but each of the methods used suffers from its own limitations and uncertainties. Small-angle X-ray scattering (SAXS) can be used to measure the thickness of particles that scatter X-rays coherently. We used SAXS to study suspensions of Na-rectorite and other illites with varying proportions of smectite. The scattering intensity (I) was recorded as a function of the scattering vector, q = (4 /) sin(/2), where  is the X-ray wavelength and  is the scattering angle. The experimental data were treated with a direct Fourier transform to obtain the pair distance distribution function (PDDF) that was then used to determine the thickness of illite particles. The Guinier and Porod extrapolations were used to obtain the scattering intensity beyond the experimental q, and the effects of such extrapolations on the PDDF were examined. The thickness of independent rectorite particles (used as a reference mineral) is 18.3 Å. The SAXS results are compared with those obtained by X-ray diffraction peak broadening methods. It was found that the power-law exponent (α) obtained by fitting the data in the region of q = 0.1-0.6 nm-1 to the power law (I = I0q-α) is a linear function of illite particle thickness. Therefore, illite particle thickness could be predicted by the linear relationship as long as the thickness is within the limit where α <4.0.

  6. Insights into the interactions among Surfactin, betaines, and PAM: surface tension, small-angle neutron scattering, and small-angle X-ray scattering study.

    Science.gov (United States)

    Xiao, Jingwen; Liu, Fang; Garamus, Vasil M; Almásy, László; Handge, Ulrich A; Willumeit, Regine; Mu, Bozhong; Zou, Aihua

    2014-04-01

    The interactions among neutral polymer polyacrylamide (PAM) and the biosurfactant Surfactin and four betaines, N-dodecyl-N,N-dimethyl-3-ammonio-1-propanesulfonate (SDDAB), N-tetradecyl-N,N-dimethyl-3-ammonio-1-propanesulfonate (STDAB), N-hexadecyl-N,N-dimethyl-3-ammonio-1-propanesulfonate (SHDAB), and N-dodecyl-N,N-dimethyl-2-ammonio-acetate (C12BE), in phosphate buffer solution (PBS) have been studied by surface tension measurements, small-angle neutron scattering (SANS), small-angle X-ray scattering (SAXS), and rheological experiments. It has been confirmed that the length of alkyl chain is a key parameter of interaction between betaines and PAM. Differences in scattering contrast between X-ray and neutrons for surfactants and PAM molecules provide the opportunity to separately follow the changes of structure of PAM and surfactant aggregates. At concentrations of betaines higher than CMC (critical micelle concentration) and C2 (CMC of surfactant with the presence of polymer), spherical micelles are formed in betaines and betaines/PAM solutions. Transition from spherical to rod-like aggregates (micelles) has been observed in solutions of Surfactin and Surfactin/SDDAB (αSurfactin = 0.67 (molar fraction)) with addition of 0.8 wt % of PAM. The conformation change of PAM molecules only can be observed for Surfactin/SDDAB/PAM system. Viscosity values follow the structural changes suggested from scattering measurements i.e., gradually increases for mixtures PAM → Surfactin/PAM → Surfactin/SDDAB/PAM in PBS.

  7. Formation process of hierarchical structures in crystalline polymers as analyzed by simultaneous measurements of small-angle X-ray scattering and other techniques

    International Nuclear Information System (INIS)

    Yamamoto, Katsuhiro; Sakurai, Shinichi

    2006-01-01

    Crystalline polymers spontaneously form hierarchical structures, which provide us a potential use as a specialty material. Recently, not only a crystalline homopolymer but also semi-crystalline block copolymers and crystalline polymer blends have been attracting interests for the study of a hierarchical structure. In order to analyze such hierarchical structures in a variety of length scales, a simultaneous measurement of small-(SAXS) and wide-angle (WAXS) X-ray scattering with differential scanning calorimetry (DSC), or with small-angle light scattering (Hv-SALS) are most suitable. In this review, we show some examples of the simultaneous measurements. With DSC, exothermic heat flow can be simultaneously measured with X-ray scattering. On the other hand, with Hv-SALS it is possible to analyze evolution of a spherulitic structure, which is the structure at the highest rank in the hierarchy. For both cases, one can realize that it is impossible to obtain good statistics for SAXS and WAXS measurements without synchrotron radiations. (author)

  8. Healing X-ray scattering images

    Directory of Open Access Journals (Sweden)

    Jiliang Liu

    2017-07-01

    Full Text Available X-ray scattering images contain numerous gaps and defects arising from detector limitations and experimental configuration. We present a method to heal X-ray scattering images, filling gaps in the data and removing defects in a physically meaningful manner. Unlike generic inpainting methods, this method is closely tuned to the expected structure of reciprocal-space data. In particular, we exploit statistical tests and symmetry analysis to identify the structure of an image; we then copy, average and interpolate measured data into gaps in a way that respects the identified structure and symmetry. Importantly, the underlying analysis methods provide useful characterization of structures present in the image, including the identification of diffuse versus sharp features, anisotropy and symmetry. The presented method leverages known characteristics of reciprocal space, enabling physically reasonable reconstruction even with large image gaps. The method will correspondingly fail for images that violate these underlying assumptions. The method assumes point symmetry and is thus applicable to small-angle X-ray scattering (SAXS data, but only to a subset of wide-angle data. Our method succeeds in filling gaps and healing defects in experimental images, including extending data beyond the original detector borders.

  9. Magnetic excitations and phase separation in the underdoped La2-xSrxCuO4 superconductor measured by resonant inelastic X-ray scattering.

    Science.gov (United States)

    Braicovich, L; van den Brink, J; Bisogni, V; Sala, M Moretti; Ament, L J P; Brookes, N B; De Luca, G M; Salluzzo, M; Schmitt, T; Strocov, V N; Ghiringhelli, G

    2010-02-19

    We probe the collective magnetic modes of La2CuO4 and underdoped La2-xSrxCuO4 (LSCO) by momentum resolved resonant inelastic x-ray scattering (RIXS) at the Cu L3 edge. For the undoped antiferromagnetic sample, we show that the single magnon dispersion measured with RIXS coincides with the one determined by inelastic neutron scattering, thus demonstrating that x rays are an alternative to neutrons in this field. In the spin dynamics of LSCO, we find a branch dispersing up to approximately 400 meV coexisting with one at lower energy. The high-energy branch has never been seen before. It indicates that underdoped LSCO is in a dynamic inhomogeneous spin state.

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

    DEFF Research Database (Denmark)

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

    2016-01-01

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

  11. A Mo-anode-based in-house source for small-angle X-ray scattering measurements of biological macromolecules

    Energy Technology Data Exchange (ETDEWEB)

    Bruetzel, Linda K.; Fischer, Stefan; Salditt, Annalena; Sedlak, Steffen M.; Nickel, Bert; Lipfert, Jan, E-mail: Jan.Lipfert@lmu.de [Department of Physics, Nanosystems Initiative Munich, and Center for Nanoscience, Ludwig-Maximilians-University Munich, Amalienstr. 54, 80799 Munich, Germany and Geschwister-Scholl Platz 1, 80539 Munich (Germany)

    2016-02-15

    We demonstrate the use of a molybdenum-anode-based in-house small-angle X-ray scattering (SAXS) setup to study biological macromolecules in solution. Our system consists of a microfocus X-ray tube delivering a highly collimated flux of 2.5 × 10{sup 6} photons/s at a beam size of 1.2 × 1.2 mm{sup 2} at the collimation path exit and a maximum beam divergence of 0.16 mrad. The resulting observable scattering vectors q are in the range of 0.38 Å{sup −1} down to 0.009 Å{sup −1} in SAXS configuration and of 0.26 Å{sup −1} up to 5.7 Å{sup −1} in wide-angle X-ray scattering (WAXS) mode. To determine the capabilities of the instrument, we collected SAXS data on weakly scattering biological macromolecules including proteins and a nucleic acid sample with molecular weights varying from ∼12 to 69 kDa and concentrations of 1.5–24 mg/ml. The measured scattering data display a high signal-to-noise ratio up to q-values of ∼0.2 Å{sup −1} allowing for an accurate structural characterization of the samples. Moreover, the in-house source data are of sufficient quality to perform ab initio 3D structure reconstructions that are in excellent agreement with the available crystallographic structures. In addition, measurements for the detergent decyl-maltoside show that the setup can be used to determine the size, shape, and interactions (as characterized by the second virial coefficient) of detergent micelles. This demonstrates that the use of a Mo-anode based in-house source is sufficient to determine basic geometric parameters and 3D shapes of biomolecules and presents a viable alternative to valuable beam time at third generation synchrotron sources.

  12. Determination of structural changes of dispersed clay platelets in a polymer blend during solid-state rheological property measurement by small-angle X-ray scattering

    CSIR Research Space (South Africa)

    Bandyopadhyay, J

    2011-05-01

    Full Text Available -angle X-ray scattering studies showed that the degree of anisotropy and mean orientation angles of clay platelets in blend matrix were altered significantly after frequency and temperature sweep tests....

  13. Noninvasive in-process thickness measurement of an organic layer on steel using x-ray scattering

    International Nuclear Information System (INIS)

    Moskowitz, J.

    1992-01-01

    The motivation for this work was the need for a non-contacting composition-independent in-process technique for rapidly measuring the mass per unit area (open-quotes surface densityclose quotes) of a continuous slab of organic material prepared on a stainless steel base. It was essential that the technique be adaptable to eventual implementation for on-line process control

  14. Insights into Surface Interactions between Metal Organic Frameworks and Gases during Transient Adsorption and Diffusion by In-Situ Small Angle X-ray Scattering

    Directory of Open Access Journals (Sweden)

    Ludovic F. Dumée

    2016-09-01

    Full Text Available The fabrication of molecular gas sieving materials with specific affinities for a single gas species and able to store large quantities of materials at a low or atmospheric pressure is desperately required to reduce the adverse effects of coal and oil usage in carbon capture. Fundamental understanding of the dynamic adsorption of gas, the diffusion mechanisms across thin film membranes, and the impact of interfaces play a vital role in developing these materials. In this work, single gas permeation tests across micro-porous membrane materials, based on metal organic framework crystals grown on the surface of carbon nanotubes (ZiF-8@CNT, were performed for the first time in-situ at the Australian Synchrotron on the small angle X-ray scattering beamline in order to reveal molecular sieving mechanisms and gas adsorption within the material. The results show that specific chemi-sorption of CO2 across the ZiF-8 crystal lattices affected the morphology and unit cell parameters, while the sieving of other noble or noble like gases across the ZiF-8@CNT membranes was found to largely follow Knudsen diffusion. This work demonstrates for the first time a novel and effective technique to assess molecular diffusion at the nano-scale across sub-nano-porous materials by probing molecular flexibility across crystal lattice and single cell units.

  15. Moments of the Bethe surface and total inelastic x-ray scattering cross sections for H2

    International Nuclear Information System (INIS)

    Sharma, B.S.; Thakkar, A.J.

    1987-01-01

    Moments, S(j,K), of the generalized oscillator strength distribution are global properties of the Bethe surface. Apart from S(-1,K) which is related to the Waller-Hartree incoherent scattering factor, little is known about these moments for nonzero K. This paper describes high-accuracy calculations of S(1,K) and S(2,K) for molecular hydrogen. Comparison with experiment is made, and the utility of simple asymptotic approximations is confirmed. The moments are used to calculate differential cross sections for the inelastic scattering of x rays using the constant-momentum-transfer and constant-angle theories of Bonham. These cross sections differ from the Waller-Hartree cross sections at large angles thus demonstrating the importance of making corrections to the Waller-Hartree theory if the incoherent scattering factor S(K) is to be extracted from experimental inelastic cross sections. Total cross sections for scattering of 6- and 7-keV photons from H 2 are compared with synchrotron radiation scattering experiments. The calculations suggest that the Bonham constant-angle cross sections agree best with experiment. However, further experimental and theoretical work is needed to obtain firm conclusions about the limitations of Waller-Hartree theory

  16. An apparatus for high speed measurements of small-angle x-ray scattering profiles with a linear position sensitive detector

    International Nuclear Information System (INIS)

    Hashimoto, Takeji; Suehiro, Shoji; Shibayama, Mitsuhiro; Saijo, Kenji; Kawai, Hiromichi

    1981-01-01

    An apparatus for high speed measurements of small-angle X-ray scattering (SAXS) is described. This apparatus utilizes a 12 kW rotating anode X-ray generator, a linear position sensitive proportional counter (multicathode delay line PSPC), and a two-parameter multichannel pulse height analyzer (MCA) with 12 kwords (16 bits/word) memory area available for SAXA intensity data as a function of position (scattering angles) and time slice. The two-parameter MCA is constructed within a microcomputer system, by utilizing its R/W memory for data storage, and the memory incrementing and real-time CRT display is implemented by using two direct memory access (DMA) controllers. The cycle time of the access is about 10 μs. The measuring time for SAXS profiles with this apparatus can be shortened approximately by three orders of magnitude in comparison with the measuring time with SAXS apparatuses utilizing a conventional step-scanning goniometer and a conventional X-ray tube, thus permitting time-resolved analyses of SAXS profiles. Some applications of the apparatus to dynamic SAXS measurements are presented for polymeric systems, the preliminary results of which seem to indicate the possibility of obtaining a new class of data on dynamics in structural transformation, deformation, formation and annihilation in the scale of a few tens to several hundred Angstroms. (author)

  17. Small Angle X-Ray Scattering Detector

    Energy Technology Data Exchange (ETDEWEB)

    Hessler, Jan P.

    2004-06-15

    A detector for time-resolved small-angle x-ray scattering includes a nearly constant diameter, evacuated linear tube having an end plate detector with a first fluorescent screen and concentric rings of first fiber optic bundles for low angle scattering detection and an annular detector having a second fluorescent screen and second fiber optic bundles concentrically disposed about the tube for higher angle scattering detection. With the scattering source, i.e., the specimen under investigation, located outside of the evacuated tube on the tube's longitudinal axis, scattered x-rays are detected by the fiber optic bundles, to each of which is coupled a respective photodetector, to provide a measurement resolution, i.e., dq/q, where q is the momentum transferred from an incident x-ray to an x-ray scattering specimen, of 2% over two (2) orders of magnitude in reciprocal space, i.e., qmax/qmin approx=lO0.

  18. Constrained Maximum Likelihood Estimation of Relative Abundances of Protein Conformation in a Heterogeneous Mixture from Small Angle X-Ray Scattering Intensity Measurements

    Science.gov (United States)

    Onuk, A. Emre; Akcakaya, Murat; Bardhan, Jaydeep P.; Erdogmus, Deniz; Brooks, Dana H.; Makowski, Lee

    2015-01-01

    In this paper, we describe a model for maximum likelihood estimation (MLE) of the relative abundances of different conformations of a protein in a heterogeneous mixture from small angle X-ray scattering (SAXS) intensities. To consider cases where the solution includes intermediate or unknown conformations, we develop a subset selection method based on k-means clustering and the Cramér-Rao bound on the mixture coefficient estimation error to find a sparse basis set that represents the space spanned by the measured SAXS intensities of the known conformations of a protein. Then, using the selected basis set and the assumptions on the model for the intensity measurements, we show that the MLE model can be expressed as a constrained convex optimization problem. Employing the adenylate kinase (ADK) protein and its known conformations as an example, and using Monte Carlo simulations, we demonstrate the performance of the proposed estimation scheme. Here, although we use 45 crystallographically determined experimental structures and we could generate many more using, for instance, molecular dynamics calculations, the clustering technique indicates that the data cannot support the determination of relative abundances for more than 5 conformations. The estimation of this maximum number of conformations is intrinsic to the methodology we have used here. PMID:26924916

  19. Measuring the molecular dimensions of wine tannins: comparison of small-angle X-ray scattering, gel-permeation chromatography and mean degree of polymerization.

    Science.gov (United States)

    McRae, Jacqui M; Kirby, Nigel; Mertens, Haydyn D T; Kassara, Stella; Smith, Paul A

    2014-07-23

    The molecular size of wine tannins can influence astringency, and yet it has been unclear as to whether the standard methods for determining average tannin molecular weight (MW), including gel-permeation chromatography (GPC) and depolymerization reactions, are actually related to the size of the tannin in wine-like conditions. Small-angle X-ray scattering (SAXS) was therefore used to determine the molecular sizes and corresponding MWs of wine tannin samples from 3 and 7 year old Cabernet Sauvignon wine in a variety of wine-like matrixes: 5-15% and 100% ethanol; 0-200 mM NaCl and pH 3.0-4.0, and compared to those measured using the standard methods. The SAXS results indicated that the tannin samples from the older wine were larger than those of the younger wine and that wine composition did not greatly impact on tannin molecular size. The average tannin MWs as determined by GPC correlated strongly with the SAXS results, suggesting that this method does give a good indication of tannin molecular size in wine-like conditions. The MW as determined from the depolymerization reactions did not correlate as strongly with the SAXS results. To our knowledge, SAXS measurements have not previously been attempted for wine tannins.

  20. Small-angle x-ray scattering and density measurements of liquid Se50-Te50 mixture at high temperatures and high pressures using synchrotron radiation

    International Nuclear Information System (INIS)

    Kajihara, Y; Inui, M; Matsuda, K; Tomioka, Y

    2010-01-01

    We have carried out small-angle x-ray scattering and x-ray transmission measurements of liquid Se 50 -Te 50 mixture at SPring-8 in Japan and obtained the structure factor S(Q) at small-Q region (0.6 -1 ) and the density at high temperatures and high pressures up to 1000 0 C and 180 MPa. We report preliminary results in this paper. With increasing temperature, the density shows a minimum at around 500 0 C and a maximum at around 700 0 C. On the other hand, S(0) becomes maximum and S(Q) strongly depends on Q at around 600 0 C, which is about the middle temperature where the density shows the minimum and maximum. The temperatures shift to lower side when the pressure increases. These results prove that, with increasing temperature, the sample exhibits gradual transition from low-density structure to high-density structure, which causes mesoscopic density fluctuations in the intermediate temperature region.

  1. Dzyaloshinskii-Moriya interaction in α -Fe2O3 measured by magnetic circular dichroism in resonant inelastic soft x-ray scattering

    Science.gov (United States)

    Miyawaki, Jun; Suga, Shigemasa; Fujiwara, Hidenori; Urasaki, Masato; Ikeno, Hidekazu; Niwa, Hideharu; Kiuchi, Hisao; Harada, Yoshihisa

    2017-12-01

    Fe L2 ,3-edge x-ray absorption spectra (XAS) and magnetic circular dichroism (MCD) in resonant inelastic x-ray scattering (RIXS) of α -Fe2O3 were measured to identify the electronic structure responsible for its weak ferromagnetism caused by the Dzyaloshinskii-Moriya interaction (DMI) at room temperature. In contrast to negligible MCD in XAS, MCD in RIXS (RIXS-MCD) was clearly observed in the d d excitation at 1.8 eV via excitation to charge-transfer states. Furthermore, RIXS-MCD showed a crystal orientation dependence, indicating that the observed RIXS-MCD originated from DMI. The observed RIXS-MCD is well described by ab initio charge-transfer multiplet calculations, revealing that the RIXS-MCD derives from spin flip excitations at delocalized eg orbitals. By the combination of the experiments and calculations, RIXS-MCD has unraveled that the origin of DMI in α -Fe2O3 is the eg orbitals, which are strongly hybridized with the 2 p orbitals of oxygen atoms. The results demonstrate the importance of RIXS-MCD for identifying the electronic structure related to DMI.

  2. Resonant diffuse X-ray scattering from magnetic multilayers

    International Nuclear Information System (INIS)

    Spezzani, Carlo; Torelli, Piero; Delaunay, Renaud; Hague, C.F.; Petroff, Frederic; Scholl, Andreas; Gullikson, E.M.; Sacchi, Maurizio

    2004-01-01

    We have measured field-dependent resonant diffuse scattering from a magnetoresistive Co/Cu multilayer. We have observed that the magnetic domain size in zero field depends on the magnetic history of the sample. The results of the X-ray scattering analysis have been compared to PEEM images of the magnetic domains

  3. Diffuse X-Ray Scattering from Several Platinum Chain Compounds

    DEFF Research Database (Denmark)

    Braude, A.; Lindegaard-Andersen, Asger; Carneiro, K.

    1980-01-01

    Values of the Fermi wavevector for several platinum based one-dimensional conductors were determined from diffuse X-ray scattering measurements. The values were compared with those expected from the chemical compositions. The importance of conclusive values of this parameter is stressed and the c...

  4. Resonant inelastic x-ray scattering and photoemission measurement of O2: Direct evidence for dependence of Rydberg-valence mixing on vibrational states in O 1s → Rydberg states

    Science.gov (United States)

    Gejo, T.; Oura, M.; Tokushima, T.; Horikawa, Y.; Arai, H.; Shin, S.; Kimberg, V.; Kosugi, N.

    2017-07-01

    High-resolution resonant inelastic x-ray scattering (RIXS) and low-energy photoemission spectra of oxygen molecules have been measured for investigating the electronic structure of Rydberg states in the O 1s → σ* energy region. The electronic characteristics of each Rydberg state have been successfully observed, and new assignments are made for several states. The RIXS spectra clearly show that vibrational excitation is very sensitive to the electronic characteristics because of Rydberg-valence mixing and vibronic coupling in O2. This observation constitutes direct experimental evidence that the Rydberg-valence mixing characteristic depends on the vibrational excitation near the avoided crossing of potential surfaces. We also measured the photoemission spectra of metastable oxygen atoms (O*) from O2 excited to 1s → Rydberg states. The broadening of the 4p Rydberg states of O* has been found with isotropic behavior, implying that excited oxygen molecules undergo dissociation with a lifetime of the order of 10 fs in 1s → Rydberg states.

  5. New insights into nucleation. Pressure trace measurements and the first small angle X-ray scattering experiments in a supersonic laval nozzle

    Energy Technology Data Exchange (ETDEWEB)

    Ghosh, D.

    2007-07-01

    Homogeneous nucleation rates of the n-alcohols and the n-alkanes have been determined by combining information from two sets of supersonic Laval nozzle expansion experiments under identical conditions. The nucleation rates J=N/{delta}t{sub Jmax} for the n-alcohols are in the range of 1.10{sup 17}measurements were conducted for the n-alkanes to determine the condensible partial pressure, temperature, supersaturation, characteristic time, and the expansion rate corresponding to the maximum nucleation rate. Characteristic times in the range of 13{<=}{delta}t{sub Jmax}/{mu}s{<=}34 were found. In the second set of experiments, the first flow rate resolved Small Angle X-ray Scattering experiments are conducted to determine the particle number density for both substance classes. Particle number densities in the range of 1.10{sup 12}

  6. New insights into nucleation. Pressure trace measurements and the first small angle X-ray scattering experiments in a supersonic laval nozzle

    International Nuclear Information System (INIS)

    Ghosh, D.

    2007-01-01

    Homogeneous nucleation rates of the n-alcohols and the n-alkanes have been determined by combining information from two sets of supersonic Laval nozzle expansion experiments under identical conditions. The nucleation rates J=N/Δt Jmax for the n-alcohols are in the range of 1.10 17 -3 s -1 17 for the temperatures 207≤T/K≤249, the nucleation rates for the n-alkanes lie in the range of 5.10 15 -3 s -1 18 for the temperatures 143 ≤T/K≤215. For the first time it is shown that the nucleation rate is not only a function of the supersaturation and temperature but clearly also sensitive to the expansion rate during supersonic nozzle expansion. A good agreement between the experimental results and those available in literature is found by applying Hale's scaling formalism [Hale, B., Phys. Rev. A 33, 4256 (1986); Hale, B., Metall. Trans. A 23, 1863 (1992)]. The scaling parameters from this work are also in good agreement with those shown by Rusyniak et al. [Rusyniak, M., M. S. El-Shall, J. Phys. Chem. B 105, 11873 (2001)] and Brus et al. [Brus, D., V. Zdimal F. Stratmann, J. Chem Phys. 124, 164306 (2006)]. In the first experiment static pressure measurements were conducted for the n-alkanes to determine the condensible partial pressure, temperature, supersaturation, characteristic time, and the expansion rate corresponding to the maximum nucleation rate. Characteristic times in the range of 13≤Δt Jmax /μs≤34 were found. In the second set of experiments, the first flow rate resolved Small Angle X-ray Scattering experiments are conducted to determine the particle number density for both substance classes. Particle number densities in the range of 1.10 12 -3 12 and 1.10 11 -3 12 for the n-alcohols and n-alkanes are found, respectively. Additionally, by analyzing the radially averaged scattering spectrum, information on the mean radius and the width of the size distribution of the aerosols is obtained. Mean radii for the n-alcohols in the range of 4< left angle r

  7. Small-angle X-ray scattering of solutions

    International Nuclear Information System (INIS)

    Koch, M.H.J.; Stuhrmann, H.B.; Vachette, P.; Tardieu, A.

    1982-01-01

    The use of synchrotron radiation in small-angle X-ray scattering (SAXS) techniques in biological structural studies is described. The main features of the monochromatic radiation systems and the white radiation systems are considered. The detectors, data acquisition and experimental procedures are briefly described. Experimental results are presented for 1) measurements on dilute solutions and weak scatterers, 2) measurement of conformational transitions, 3) contrast variation experiments, 4) time-resolved measurements and 5) complex contrast variation. (U.K.)

  8. Workshop report on new directions in x-ray scattering

    International Nuclear Information System (INIS)

    Brown, G.; Del Grande, N.K.; Fuoss, P.; Mallett, J.H.; Pratt, R.; Templeton, D.

    1987-01-01

    This report is a summary of the Workshop on New Directions in X-Ray Scattering held at the Asilomar Conference Center, Pacific Grove, California, April 2-5, 1985. The report primarily consists of the edited transcript of the final review session of the workshop, in which members of a panel summarized the proceedings. It is clear that we are close to achieving an accurate theory of scattering in independent particle approximation, but for edge regions, there is need to go beyond this approach. Much of what is experimentally interesting in scattering is occurring between the photoabsorption edge and the photoelectric threshold. Applications in condensed matter and biological and chemical material studies are expanding, exploiting higher intensity sources and faster time resolution as in magnetic scattering and surface studies. Storage rings are now conventional sources, and new high-intensity beam lines are under development; the free electron laser is one of the more speculative sources. Recent work in x-ray scattering has led to advances in x-ray optics, and conversely, advances in x-ray optics have benefitted our understanding of x-ray scattering

  9. X-ray scattering signatures of β-thalassemia

    International Nuclear Information System (INIS)

    Desouky, Omar S.; Elshemey, Wael M.; Selim, Nabila S.

    2009-01-01

    X-ray scattering from lyophilized proteins or protein-rich samples is characterized by the presence of two characteristic broad peaks at scattering angles equivalent to momentum transfer values of 0.27 and 0.6 nm -1 , respectively. These peaks arise from the interference of coherently scattered photons. Once the conformation of a protein is changed, these two peaks reflect such change with considerable sensitivity. The present work examines the possibility of characterizing the most common cause of hemolytic anaemia in Egypt and many Mediterranean countries; β-thalassemia, from its X-ray scattering profile. This disease emerges from a genetic defect causing reduced rate in the synthesis of one of the globin chains that make up hemoglobin. As a result, structurally abnormal hemoglobin molecules are formed. In order to detect such molecular disorder, hemoglobin samples of β-thalassemia patients are collected, lyophilized and measured using a conventional X-ray diffractometer. Results show significant differences in the X-ray scattering profiles of most of the diseased samples compared to control. The shape of the first scattering peak at 0.27 nm -1 , in addition to the relative intensity of the first to the second scattering peaks, provides the most reliable signs of abnormality in diseased samples. The results are interpreted and confirmed with the aid of Fourier Transform Infrared (FTIR) spectroscopy of normal and thalassemia samples.

  10. X-ray scattering signatures of β-thalassemia

    Science.gov (United States)

    Desouky, Omar S.; Elshemey, Wael M.; Selim, Nabila S.

    2009-08-01

    X-ray scattering from lyophilized proteins or protein-rich samples is characterized by the presence of two characteristic broad peaks at scattering angles equivalent to momentum transfer values of 0.27 and 0.6 nm -1, respectively. These peaks arise from the interference of coherently scattered photons. Once the conformation of a protein is changed, these two peaks reflect such change with considerable sensitivity. The present work examines the possibility of characterizing the most common cause of hemolytic anaemia in Egypt and many Mediterranean countries; β-thalassemia, from its X-ray scattering profile. This disease emerges from a genetic defect causing reduced rate in the synthesis of one of the globin chains that make up hemoglobin. As a result, structurally abnormal hemoglobin molecules are formed. In order to detect such molecular disorder, hemoglobin samples of β-thalassemia patients are collected, lyophilized and measured using a conventional X-ray diffractometer. Results show significant differences in the X-ray scattering profiles of most of the diseased samples compared to control. The shape of the first scattering peak at 0.27 nm -1, in addition to the relative intensity of the first to the second scattering peaks, provides the most reliable signs of abnormality in diseased samples. The results are interpreted and confirmed with the aid of Fourier Transform Infrared (FTIR) spectroscopy of normal and thalassemia samples.

  11. X-ray scattering signatures of {beta}-thalassemia

    Energy Technology Data Exchange (ETDEWEB)

    Desouky, Omar S. [Radiation Physics Department, National Center for Radiation Research and Technology (NCRRT) (Egypt); Elshemey, Wael M. [Biophysics Department, Faculty of Science, Cairo University (Egypt)], E-mail: waelelshemey@yahoo.com; Selim, Nabila S. [Radiation Physics Department, National Center for Radiation Research and Technology (NCRRT) (Egypt)

    2009-08-11

    X-ray scattering from lyophilized proteins or protein-rich samples is characterized by the presence of two characteristic broad peaks at scattering angles equivalent to momentum transfer values of 0.27 and 0.6 nm{sup -1}, respectively. These peaks arise from the interference of coherently scattered photons. Once the conformation of a protein is changed, these two peaks reflect such change with considerable sensitivity. The present work examines the possibility of characterizing the most common cause of hemolytic anaemia in Egypt and many Mediterranean countries; {beta}-thalassemia, from its X-ray scattering profile. This disease emerges from a genetic defect causing reduced rate in the synthesis of one of the globin chains that make up hemoglobin. As a result, structurally abnormal hemoglobin molecules are formed. In order to detect such molecular disorder, hemoglobin samples of {beta}-thalassemia patients are collected, lyophilized and measured using a conventional X-ray diffractometer. Results show significant differences in the X-ray scattering profiles of most of the diseased samples compared to control. The shape of the first scattering peak at 0.27 nm{sup -1}, in addition to the relative intensity of the first to the second scattering peaks, provides the most reliable signs of abnormality in diseased samples. The results are interpreted and confirmed with the aid of Fourier Transform Infrared (FTIR) spectroscopy of normal and thalassemia samples.

  12. X-ray scattering of soft matter

    International Nuclear Information System (INIS)

    Stribeck, N.

    2007-01-01

    This coherently written volume summarizes the analytical power of modern X-ray scattering in the field of soft matter. Applications of X-ray scattering to soft matter have advanced considerably within recent years, both conceptually and technically. There are now mature high-power X-ray sources, synchrotrons and rotating anodes, as well as high-speed detectors, which have become readily available and which make the whole process more viable. High-quality time-resolved experiments on polymer structure can now be performed with ease, a major advancement due to the genuine power of the scattering method. This manual is a detailed description of simple tools that can elucidate the mechanisms of structure evolution in the studied materials. It is also a step-by-step guide to more advanced methods of the latest X-ray scattering techniques, and breaks down these methods. Data analysis based on clear, unequivocal results is rendered simple and straightforward - with a stress on the careful planning of experiments and adequate recording of all required data. This book, then, serves as a useful ready-reference guide. It has been written for the modern scientist who is a generalist and needs a concise reference, and demonstrates typical errors in data evaluation. (orig.)

  13. Small angle X-ray scattering experiments with three-dimensional imaging gas detectors

    International Nuclear Information System (INIS)

    La Monaca, A.; Iannuzzi, M.; Messi, R.

    1985-01-01

    Measurements of small angle X-ray scattering of lupolen - R, dry collagen and dry cornea are presented. The experiments have been performed with synchrotron radiation and a new three-dimensional imaging drif-chamber gas detector

  14. Detection of impaired diastolic relaxation during myocardial ischemia using x-ray scatter fields

    International Nuclear Information System (INIS)

    McInerney, J.J.; Morris, L.; Herr, M.D.; Copenhaver, G.L.

    1986-01-01

    Precise three-dimensional epicardial displacements and velocities are measured nonivasively (no cutdowns or injections) with low-energy x-rays scattered from the closed chest surface of the heart. Surface reconstructions provide direct visualization of p-wave motion of the atrial wall, isovolumic sphericalization of the heart, global thrust of the ventricle during ejection, swelling of the base during refill, and relaxation during diastole. This new imaging technique was applied to canines before and after closed chest coronary embolization. Displacement and velocity displays of ischemic hearts clearly show reduced ejection displacement amplitudes, asynchronous motion patterns during systole, and impaired relaxation patterns during diastole

  15. Monitoring the recrystallisation of amorphous xylitol using Raman spectroscopy and wide-angle X-ray scattering.

    Science.gov (United States)

    Palomäki, Emmi; Ahvenainen, Patrik; Ehlers, Henrik; Svedström, Kirsi; Huotari, Simo; Yliruusi, Jouko

    2016-07-11

    In this paper we present a fast model system for monitoring the recrystallization of quench-cooled amorphous xylitol using Raman spectroscopy and wide-angle X-ray scattering. The use of these two methods enables comparison between surface and bulk crystallization. Non-ordered mesoporous silica micro-particles were added to the system in order to alter the rate of crystallization of the amorphous xylitol. Raman measurements showed that adding silica to the system increased the rate of surface crystallization, while X-ray measurements showed that the rate of bulk crystallization decreased. Using this model system it is possible to measure fast changes, which occur in minutes or within a few hours. Raman-spectroscopy and wide-angle X-ray scattering were found to be complementary techniques when assessing surface and bulk crystallization of amorphous xylitol. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    1980-01-01

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

  17. Nano-crystal growth in cordierite glass ceramics studied with X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Bras, Wim; Clark, Simon M.; Greaves, G. N.; Kunz, Martin; van Beek, W.; Radmilovic, V.

    2009-01-16

    The development of monodisperse crystalline particles in cordierite glass doped with Cr3+ after a two-step heat treatment is elucidated by a combination of time-resolved small and wide angle x-ray scattering (SAXS/WAXS) experiments with electron microscopy. The effects of bulk and surface crystallization can clearly be distinguished, and the crystallization kinetics of the bulk phase is characterized. The internal pressure due to structural differences between the crystalline and amorphous phase is measured but the physical cause of this pressure can not unambiguously be attributed. The combined measurements comprise a nearly full characterization of the crystallization processes and the resulting sample morphology.

  18. Toroidal silicon polarization analyzer for resonant inelastic x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Xuan [Department of Physics, Western Michigan University, Kalamazoo, Michigan 49008-5252 (United States); Key Laboratory of Multi-scale Manufacturing Technology, Chongqing Institute of Green and Intelligent Technology, Chinese Academy of Sciences, Chongqing 400714 (China); Casa, Diego; Kim, Jungho; Gog, Thomas [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Li, Chengyang [Department of Physics, Western Michigan University, Kalamazoo, Michigan 49008-5252 (United States); Department of Physics, South University of Science and Technology of China, Shenzhen 518055 (China); Burns, Clement [Department of Physics, Western Michigan University, Kalamazoo, Michigan 49008-5252 (United States)

    2016-08-15

    Resonant Inelastic X-ray Scattering (RIXS) is a powerful probe for studying electronic excitations in materials. Standard high energy RIXS measurements do not measure the polarization of the scattered x-rays, which is unfortunate since it carries information about the nature and symmetry of the excitations involved in the scattering process. Here we report the fabrication of thin Si-based polarization analyzers with a double-concave toroidal surface, useful for L-edge RIXS studies in heavier atoms such as the 5-d transition metals.

  19. X-ray scattering by interstellar dust

    International Nuclear Information System (INIS)

    Rolf, D.

    1980-10-01

    This thesis reports work carried out to make a first observation of x-rays scattered by interstellar dust grains. Data about the dust, obtained at wavelengths ranging from the infrared to ultra-violet spectral regions, are discussed in order to establish a useful description of the grains themselves. This is then used to estimate the magnitude and form of the expected x-ray scattering effect which is shown to manifest itself as a diffuse halo accompanying the image of a celestial x-ray source. Two x-ray imaging experiments are then discussed. The first, specifically proposed to look for this effect surrounding a point x-ray source, was the Skylark 1611 project, and comprised an imaging proportional counter coupled to an x-ray mirror. This is described up to its final calibration when the basis for a concise model of its point response function was established. The experiment was not carried out but its objective and the experience gained during its testing were transferred to the second of the x-ray imaging experiments, the Einstein Observatory. The new instrumental characteristics are described and a model for its point response function is developed. Using this, image data for the point x-ray source GX339-4 is shown to exhibit the sought after scattering phenomenon. (author)

  20. Resonance magnetic x-ray scattering study of erbium

    DEFF Research Database (Denmark)

    Sanyal, M.K.; Gibbs, D.; Bohr, J.

    1994-01-01

    The magnetic phases of erbium have been studied by resonance x-ray-scattering techniques. When the incident x-ray energy is tuned near the L(III) absorption edge, large resonant enhancements of the magnetic scattering are observed above 18 K. We have measured the energy and polarization dependence...... of this magnetic scattering and analyzed it using a simple model based on electric dipole and quadrupole transitions among atomic orbitals. The line shapes can be fitted to a magnetic structure combining both c-axis-modulated and basal-plane components. Below 18 K, we have observed unusual behavior of the magnetic...

  1. Real-time x-ray scattering study of the initial growth of organic crystals on polymer brushes

    Energy Technology Data Exchange (ETDEWEB)

    An, Sung Yup; Ahn, Kwangseok; Kim, Doris Yangsoo; Lee, Dong Ryeol, E-mail: drlee@ssu.ac.kr [Department of Physics, Soongsil University, Seoul 156-743 (Korea, Republic of); Lee, Hyun-Hwi [Pohang Accelerator Laboratory, Pohang University of Science and Technology, Pohang 790-784 (Korea, Republic of); Cho, Jeong Ho, E-mail: jhcho94@skku.edu [Department of Chemical Engineering, SKKU Advanced Institute of Nanotechnology (SAINT) and Center for Human Interface Nano Technology (HINT), Sungkyunkwan University, Suwon 440-476 (Korea, Republic of)

    2014-04-21

    We studied the early-stage growth structures of pentacene organic crystals grown on polymer brushes using real-time x-ray scattering techniques. In situ x-ray reflectivity and atomic force microscopy analyses revealed that at temperatures close to the glass transition temperature of polymer brush, the pentacene overlayer on a polymer brush film showed incomplete condensation and 3D island structures from the first monolayer. A growth model based on these observations was used to quantitatively analyze the real-time anti-Bragg x-ray scattering intensities measured during pentacene growth to obtain the time-dependent layer coverage of the individual pentacene monolayers. The extracted total coverage confirmed significant desorption and incomplete condensation in the pentacene films deposited on the polymer brushes. These effects are ascribed to the change in the surface viscoelasticity of the polymer brushes around the glass transition temperature.

  2. Development of general X-ray scattering model

    International Nuclear Information System (INIS)

    Gray, Joe; Wendt, Scott

    2015-01-01

    X-ray scattering is a complex process made difficult to describe due to the effects of a complex energy spectrum interacting with a wide range of material types in complex geometry. The scattering is further complicated by the volume of material illuminated and the experimental configuration of the data acquisition. The importance of accounting for the key physics in scattering modeling is critical to the viability of the model. For example, scattering in the detector and the speed of the detector, as measured by the absorbed dose needed to produce a signal, are important in capturing undercut effects. Another example is the noise properties of the detectors are dependent on photon energy. We report on a semi-empirical treatment of x-ray scattering that includes a full energy treatment for a wide range of material types. We also include complex geometry effects that the part shape introduces. The treatment is based on experimental measurements using an energy dispersive germanium detector over energies from treatment is showing good results with experimental measurements of the scattering component agreeing with the model results to the 10% level over the range of x-ray energies and materials typical in industrial applications. Computation times for this model are in the 20 keV to 320 keV. Detector stripping routines for detector artifacts were developed. The computation time is in the range of a few minutes on a typical PC

  3. CHEMICAL APPLICATIONS OF INELASTIC X-RAY SCATTERING

    Energy Technology Data Exchange (ETDEWEB)

    HAYASHI,H.; UDAGAWA,Y.; GILLET,J.M.; CALIEBE,W.A.; KAO,C.C.

    2001-08-01

    Inelastic x-ray scattering (IXS), complementary to other more established inelastic scattering probes, such as light scattering, electron scattering, and neutron scattering, is becoming an important experimental technique in the study of elementary excitations in condensed matters. Over the past decade, IXS with total energy resolution of few meV has been achieved, and is being used routinely in the study of phonon dispersions in solids and liquids as well as dynamics in disordered and biological systems. In the study of electronic excitations, IXS with total energy resolution on the order of 100 meV to 1 eV is gaining wider applications also. For example, IXS has been used to study collective excitations of valence electrons, single electron excitations of valence electrons, as well as core electron excitations. In comparison with the alternative scattering techniques mentioned above, IXS has several advantages. First, IXS probes the full momentum transfer range of the dielectric response of the sample, whereas light scattering is limited to very small momentum transfers, and electron scattering suffers the effects of multiple scattering at large momentum transfers. Second, since IXS measures the bulk properties of the sample it is not surface sensitive, therefore it does not require special preparation of the sample. The greater flexibility in sample conditions and environments makes IXS an ideal probe in the study of liquids and samples under extreme temperature, pressure, and magnetic field. Third, the tunability of synchrotron radiation sources enables IXS to exploit element specificity and resonant enhancement of scattering cross sections. Fourth, IXS is unique in the study of dynamics of liquids and amorphous solids because it can probe the particular region of energy-momentum transfer phase space, which is inaccessible to inelastic neutron scattering. On the other hand, the main disadvantages of IXS are the small cross sections and the strong absorption of

  4. Surface morphology of vacuum-evaporated pentacene film on Si substrate studied by in situ grazing-incidence small-angle X-ray scattering: I. The initial stage of formation of pentacene film

    Science.gov (United States)

    Hirosawa, Ichiro; Watanabe, Takeshi; Koganezawa, Tomoyuki; Kikuchi, Mamoru; Yoshimoto, Noriyuki

    2018-03-01

    The progress of the surface morphology of a growing sub-monolayered pentacene film on a Si substrate was studied by in situ grazing-incidence small angle X-ray scattering (GISAXS). The observed GISAXS profiles did not show sizes of pentacene islands but mainly protuberances on the boundaries around pentacene film. Scattering of X-ray by residual pits in the pentacene film was also detected in the GISAXS profiles of an almost fully covered film. The average radius of pentacene protuberances increased from 13 to 24 nm as the coverage increased to 0.83 monolayer, and the most frequent radius was almost constant at approximately 9 nm. This result suggests that the population of larger protuberances increase with increasing lengths of boundaries of the pentacene film. It can also be considered that the detected protuberances were crystallites of pentacene, since the average size of protuberances was nearly equal to crystallite sizes of pentacene films. The almost constant characteristic distance of 610 nm and amplitudes of pair correlation functions at low coverages suggest that the growth of pentacene films obeyed the diffusion-limited aggregation (DLA) model, as previously reported. It is also considered that the sites of islands show a triangular distribution for small variations of estimated correlation distances.

  5. Formation of carboxy- and amide-terminated alkyl monolayers on silicon(111) investigated by ATR-FTIR, XPS, and X-ray scattering: Construction of photoswitchable surfaces

    DEFF Research Database (Denmark)

    Rück-Braun, Karola; Petersen, Michael Åxman; Michalik, Fabian

    2013-01-01

    -FTIR and XPS studies of the fulgimide samples revealed closely covered amide-terminated SAMs. Reversible photoswitching of the headgroup was read out by applying XPS, ATR-FTIR, and difference absorption spectra in the mid-IR. In XPS, we observed a reversible breathing of the amide/imide C1s and N1s signals......We have prepared high-quality, densely packed, self-assembled monolayers (SAMs) of carboxy-terminated alkyl chains on Si(111). The samples were made by thermal grafting of methyl undec-10-enoate under an inert atmosphere and subsequent cleavage of the ester functionality to disclose the carboxylic...... zigzag-like substitution pattern for the ester- and carboxy-terminated monolayer. Hydrolysis of the remaining H-Si(111) bonds at the surface furnished HO-Si(111) groups according to XPS and attenuated total reflection Fourier-transform infrared spectroscopy (ATR-FTIR) studies. The amide-terminated alkyl...

  6. New developments in the simultaneous measurement system of wide-angle and small-angle x-ray scatterings and vibrational spectra for the static and dynamic analyses of the hierarchical structures of polymer solids

    International Nuclear Information System (INIS)

    Tashiro, Kohji; Yamamoto, Hiroko; Yoshioka, Taiyo; Ninh, Tran Hai; Shimada, Shigeru; Nakatani, Takeshi; Iwamoto, Hiroyuki; Ohta, Noboru; Masunaga, Hiroyasu

    2012-01-01

    A simultaneous measurement system of wide-angle X-ray diffraction (WAXD), small-angle X-ray scattering (SAXS) and Raman or transmission-type infrared spectroscopy was developed by us. Its purposes is to clarify the static and dynamic structural changes of polymer materials subjected to the various external condition changes. Some examples described here include the study of the stretch-induced reorientation phenomenon of a-axially-oriented polyethylene, the study of structural change in photo-induced solid-state polymerization reaction of muconic acid ester monomer crystal, the study of the two-stage high-temperature phase transitions of aliphatic nylons, the study of stress-induced crystalline phase transition of an oriented poly(tetramethylene terephthalate) sample and its relation to the higher-order structural change, and the study of structural regularization process of poly(L-lactic acid) in the isothermal crystallization of the meso phase. These case studies in the clarification of hierarchical structural changes of polymer materials have proven that the simultaneous measurement systems can be useful to examine the structural changes in polymer systems. (author)

  7. A sample cell to study hydrate formation with x-ray scattering

    International Nuclear Information System (INIS)

    Conrad, Heiko; Lehmkuehler, Felix; Sternemann, Christian; Feroughi, Omid; Tolan, Metin; Simonelli, Laura; Huotari, Simo

    2009-01-01

    We present a new sample cell for measuring nonresonant inelastic x-ray scattering spectra of a tetrahydrofuran (THF)-water liquid mixture and THF hydrate. The hydrate is formed inside the cell after nucleation seeds have been offered by a special magnetic stirring mechanism. Hydrate formation was verified by wide angle x-ray scattering and nonresonant x-ray Raman scattering spectra at the oxygen K-edge. A broad range of scattering angles can be studied with this cell which is necessary for momentum transfer dependent inelastic x-ray scattering. This cell is ideal to examine other liquid hydrate formers or other liquid samples, which have to be mixed in situ during the measurements.

  8. Combining Single-Molecule Optical Trapping and Small-Angle X-Ray Scattering Measurements to Compute the Persistence Length of a Protein ER/K alpha-Helix

    DEFF Research Database (Denmark)

    Sivaramakrishnan, S.; Sung, J.; Ali, M.

    2009-01-01

    as a force transducer, rigid spacer, or flexible linker in proteins. In this study, we quantity this flexibility in terms of persistence length, namely the length scale over which it is rigid. We use single-molecule optical trapping and small-angle x-ray scattering, combined with Monte Carlo simulations...

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

    DEFF Research Database (Denmark)

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

    2018-01-01

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

  10. Probing warm dense lithium by inelastic X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Garcia Saiz, E; Riley, D [School of Mathematics and Physics, Queen' s University of Belfast, Belfast (United Kingdom); Gregori, G [Clarendon Laboratory, University of Oxford, Parks Road, Oxford (United Kingdom); Gregori, G; Clarke, R J; Neely, D; Notley, M M; Spindloe, C [Central Laser Facility, Rutherford Appleton Laboratory, Chilton, Didcot, OX (United Kingdom); Gericke, D O; Vorberger, J; Wunsch, K [Centre for Fusion, Space and Astrophysics, Department of Physics, University of Warwick, Coventry (United Kingdom); Barbrel, B; Koenig, M [Laboratoire pour l' Utilisation des Laser Intenses, Ecole Polytechnique - Universite Paris-6, 91 - Palaiseau (France); Freeman, R R; Weber, R L; Van Woerkom, L [Department of Physics, The Ohio State University, Columbus, Ohio (United States); Glenzer, S H; Landen, O L; Neumayer, P; Price, D [Lawrence Livermore National Laboratory, Livermore, California (United States); Khattak, F Y [Department of Physics, Kohat University of Science and Technology, Kohat-26000, NWFP (Pakistan); Pelka, A; Roth, M; Schollmeier, M [Institut fur Kernphysik, Technische Universitat Darmstadt (Germany)

    2008-10-15

    One of the grand challenges of contemporary physics is understanding strongly interacting quantum systems comprising such diverse examples as ultracold atoms in traps, electrons in high-temperature superconductors and nuclear matter. Warm dense matter, defined by temperatures of a few electron volts and densities comparable with solids, is a complex state of such interacting matter. Moreover, the study of warm dense matter states has practical applications for controlled thermonuclear fusion, where it is encountered during the implosion phase, and it also represents laboratory analogues of astrophysical environments found in the core of planets and the crusts of old stars. Here we demonstrate how warm dense matter states can be diagnosed and structural properties can be obtained by inelastic X-ray scattering measurements on a compressed lithium sample. Combining experiments and ab initio simulations enables us to determine its microscopic state and to evaluate more approximate theoretical models for the ionic structure. (authors)

  11. Magnetic X-Ray Scattering with Synchrotron Radiation

    DEFF Research Database (Denmark)

    Moncton, D. E.; Gibbs, D.; Bohr, Jakob

    1986-01-01

    With the availability of high-brilliance synchrotron radiation from multiple wigglers, magnetic X-ray scattering has become a powerful new probe of magnetic structure and phase transitions. Similar to the well-established magnetic neutron scattering technique, magnetic X-ray scattering methods have...... many complementary advantages. A brief review is presented of the history of magnetic X-ray scattering as well as recent results obtained in studies of the rare-earth magnet holmium with emphasis on instrumentational aspects. In particular, the development of a simple polarization analyzer...... to distinguish charge and magnetic scattering is described....

  12. Electron Dynamics by Inelastic X-Ray Scattering

    CERN Document Server

    Schülke, Winfried

    2007-01-01

    The book offers the first comprehensive review of experimental methods, theory, and successful applications of synchrotron radiation based inelastic X-ray scattering (IXS) spectroscopy, which enables the investigation of electron dynamics in condensed matter (correlated motion and excitation).

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

    International Nuclear Information System (INIS)

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

    1995-01-01

    Synchrotron X-ray scattering techniques provide a powerful tool for the in situ study of atomic scale processes occurring at solid-liquid interfaces. We have applied these techniques to characterize and study reactions at mineral-water interfaces. Here we present two examples. The first is the characterization of the calcite (CaCO 3 ) (10 bar 14) cleavage surface, in equilibrium with deionized water, by crystal truncation rod measurements. The second is the in situ study of the heteroepitaxial growth of otavite (CdCO 3 ) on the calcite (10 bar 14) cleavage surface. The results of such studies will lead to significant progress in understanding mineral-water interface geochemistry

  14. Diffuse X-ray scattering near the Bragg reflection of P-doped Czochralski silicon

    International Nuclear Information System (INIS)

    Stojanoff, V.; Pimentel, C.A.F.

    1983-01-01

    Bragg line profile and high resolution diffuse X-ray scattering measurements around the (400) reciprocal lattice point of dislocation-free Czochralski Si single crystals P-doped have shown defects of interstitial nature with typical size about 1000 A. (Author) [pt

  15. Diffuse X-ray scattering and far infrared absorption of barium and lead β" aluminas

    DEFF Research Database (Denmark)

    Hayes, W.; Kjær, Kristian; Pratt, F. L.

    1985-01-01

    The authors have carried out high-momentum-resolution studies in diffuse X-ray scattering of barium and lead B" aluminas in the temperature range 20-700 degrees C. They have also measured the vibrational spectra of these compounds between 2K and 300K in the energy range 10-100 cm-1. The results...

  16. Low angle X-ray scattering in biological tissues

    International Nuclear Information System (INIS)

    Lemos, Carla; Braz, Delson; Pinto, Nivia G.V.; Lima, Joao C.; Castro, Carlos R.F.; Filgueiras, R.A.; Mendonca, Leonardo; Lopes, Ricardo T.; Barroso, Regina C.

    2007-01-01

    Low-angle x-ray scatter (LAXS) for tissue characterization is based on the differences which result from the interference of photons coherently scattered from molecules of each sample. Biological samples (bone, blood and blood components) have been studied in recent years in our laboratory using powder diffractometer. The scattering information was obtained using a Shimadzu DRX 6000 diffractometer at the Nuclear Instrumentation Laboratory, Rio de Janeiro, Brazil. Unpolarized monoenergetic Kα radiation from Cu provided 8.04 keV photons. The measurements were made in reflection mode (θ-2θ geometry), with the sample stationary on a goniometer which rotates the sample and detector about an axis lying in the plane of the top of the sample holder. LAXS profiles from whole blood, plasma and formed elements were measured to investigate the nature of scattering from such lyophilized samples. The statistical analysis shows that the variation found for the characterization parameters is significant for whole blood considering the age. Gender was positively associated with the variation of the second peak position for the profiles obtained for formed elements. The correlation of the measured relative coherent intensity with the mineral content in the bone samples was investigated. These results suggest that the measurement of bone mineral content within trabecular bone can be performed by using quantitative coherent scattering information. (author)

  17. X-ray scattering on liquid-gas interfaces; Roentgenstreuung an Fluessigkeits-Gas Grenzflaechen

    Energy Technology Data Exchange (ETDEWEB)

    Paulus, Michael

    2006-07-01

    In the framework of this thesis two different theme-fields were studied with dhe methods of the elastic, surface sensitive X-ray scattering. In the first part of the thesis the liquid-gas interfaces water-propane and glycerol-isobutane were studied concerning the structure formation on these interfaces. The system water-propane served for the study of the gas hydrate formation on the water-gas interface. Studies on this interface could give no hints on the formation of propane hydrates or propane-hydrate fragments. However the adsorption of molecularly thin propane films on the water surface was observed. The adsorption behaviour of gases on liquid surfaces was studied by further experiments on the glycerol-isobutane interface. In the second part of the thesis the surfaces of aqueous salt solutions and water were studied. The lateralstructure of these liquid-gas interfaces was studied by the method of the diffuse X-ray scattering.

  18. Resonant x-ray scattering in correlated systems

    CERN Document Server

    Ishihara, Sumio

    2017-01-01

    The research and its outcomes presented here is devoted to the use of x-ray scattering to study correlated electron systems and magnetism. Different x-ray based methods are provided to analyze three dimensional electron systems and the structure of transition-metal oxides. Finally the observation of multipole orderings with x-ray diffraction is shown.

  19. Resonant X-ray scattering in correlated systems

    Energy Technology Data Exchange (ETDEWEB)

    Murakami, Youichi [High Energy Accelerator Research Organization, Tsukuba, Ibaraki (Japan). Inst. of Materials Structure Science; Ishihara, Sumio (ed.) [Tohoku Univ., Sendai, Miyagi (Japan). Dept. of Physics

    2017-03-01

    The research and its outcomes presented here is devoted to the use of X-ray scattering to study correlated electron systems and magnetism. Different X-ray based methods are provided to analyze three dimensional electron systems and the structure of transition-metal oxides. Finally the observation of multipole orderings with X-ray diffraction is shown.

  20. Basic X-ray scattering for soft matter

    CERN Document Server

    De Jeu, Wim H

    2016-01-01

    X-ray scattering is a well-established technique in materials science. Several excellent textbooks exist in the field, typically written by physicists who use mathematics to make things clear. Often these books do not reach students and scientists in the field of soft matter (polymers, liquid crystals, colloids, and self-assembled organic systems), who usually have a chemical-oriented background with limited mathematics. Moreover, often these people like to know more about x-ray scattering as a technique to be used, but do not necessarily intend to become an expert. This volume is unique in trying to accommodate both points. The aim of the book is to explain basic principles and applications of x-ray scattering in a simple way. The intention is a paperback of limited size that people will like to have on hand rather than on a shelf. Second, it includes a large variety of examples of x-ray scattering of soft matter with, at the end of each chapter, a more elaborate case study. Third, the book contains a separa...

  1. Resonant inelastic x-ray scattering studies of elementary excitations

    NARCIS (Netherlands)

    Ament, Lucas Johannes Peter (Luuk)

    2010-01-01

    Resonant Inelastic X-ray Scattering (RIXS) is an X-ray in, X-ray out technique that enables one to study the dispersion of excitations in solids. In this thesis, we investigated how various elementary excitations of transition metal oxides show up in RIXS spectra.

  2. Small angle X-ray scattering from protein in solution

    International Nuclear Information System (INIS)

    Souza, C.F. de; Torriani, I.L.

    1988-01-01

    In this work we report experiments performed with giant respiratory proteins from annelids. X-ray scattering data were obtained both by the use of conventional rotating anod source and synchotron radiation. Data from solutions with several protein concentrations were analyzed. (A.C.A.S.) [pt

  3. X-ray scattering from periodic arrays of quantum dots

    International Nuclear Information System (INIS)

    Holy, V; Stangl, J; Lechner, R T; Springholz, G

    2008-01-01

    Three-dimensional periodic arrays of self-organized quantum dots in semiconductor multilayers are investigated by high-resolution x-ray scattering. We demonstrate that the statistical parameters of the dot array can be determined directly from the scattering data without performing a numerical simulation of the scattered intensity.

  4. Small angle X-ray scattering from hydrating tricalcium silicate

    International Nuclear Information System (INIS)

    Vollet, D.

    1983-01-01

    The small-angle X-ray scattering technique was used to study the structural evolution of hydrated tricalcium silicate at room temperature. The changes in specific area of the associated porosity and the evolution of density fluctuations in the solid hydrated phase were deduced from the scattering data. A correlation of these variations with the hydration mechanism is tried. (Author) [pt

  5. X-ray scattering in giant magneto-resistive multilayers

    International Nuclear Information System (INIS)

    Fulthorpe, B.D.

    1999-01-01

    The scattering mechanisms responsible for Giant Magneto-Resistance (GMR) in magnetic multilayers are believed to be related to many aspects of the multilayer structure. X-ray scattering techniques provide a powerful method with which to study the bulk and interface morphology in these systems, and are therefore crucial in developing an understanding of the dominant factors influencing the magnitude of the GMR. Reflectivity measurements performed on a series of Co/Cu multilayers, sputter deposited onto etched silicon, reveal no variation in the interface roughness with etching voltage, the thickness of the individual layers also remaining constant. The observed decrease in the GMR cannot, therefore, be attributed to variations in spacer thickness or interfacial spin-independent scattering. Electron and X-ray Diffraction measurements suggest the reduction in GMR is due to a loss of antiferromagnetic coupling associated with a transformation of the texture from a randomly oriented to well oriented (111) polycrystalline texture, and subsequent reduction in the volume fraction of (100) oriented grains. Interfaces within Co/Cu are found to propagate with a high degree of conformality with increasing bilayer number, with an out-of-plane correlation length well in excess of 300A. In contrast, the Co/Pt system exhibits a limiting out-of-plane correlation length of the order of 350A arising from a columnar growth mode. X-ray Reflectivity and Diffraction measurements provide' no structural interpretation for the 3-fold enhancement in the rate of increase of the saturation conductivity, as a function of spacer thickness, in Fe/Au (100) compared to Fe/Au (111), or why large oscillations in the GMR occur for the (100) orientation only. Such observations are, however, consistent with the existence of a channelling mechanism in Fe/Au (100). Grazing Incidence Fluorescence data indicates that Nb acts as a surfactant in Fe/Au (111) growth on sapphire. The influence of different

  6. Portable mini-chamber for temperature dependent studies using small angle and wide angle x-ray scattering

    Science.gov (United States)

    Dev, Arun Singh; Kumar, Dileep; Potdar, Satish; Pandit, Pallavi; Roth, Stephan V.; Gupta, Ajay

    2018-04-01

    The present work describes the design and performance of a vacuum compatible portable mini chamber for temperature dependent GISAXS and GIWAXS studies of thin films and multilayer structures. The water cooled body of the chamber allows sample annealing up to 900 K using ultra high vacuum compatible (UHV) pyrolytic boron nitride heater, thus making it possible to study the temperature dependent evolution of structure and morphology of two-dimensional nanostructured materials. Due to its light weight and small size, the chamber is portable and can be accommodated at synchrotron facilities worldwide. A systematic illustration of the versatility of the chamber has been demonstrated at beamline P03, PETRA-III, DESY, Hamburg, Germany. Temperature dependent grazing incidence small angle x-ray scattering (GISAXS) and grazing incidence wide angle x-ray scattering (GIWAXS) measurements were performed on oblique angle deposited Co/Ag multilayer structure, which jointly revealed that the surface diffusion in Co columns in Co/Ag multilayer enhances by increasing temperature from RT to ˜573 K. This results in a morphology change from columnar tilted structure to densely packed morphological isotropic multilayer.

  7. Coherent methods in X-ray scattering

    International Nuclear Information System (INIS)

    Gorobtsov, Oleg

    2017-05-01

    X-ray radiation has been used to study structural properties of materials for more than a hundred years. Construction of extremely coherent and bright X-ray radiation sources such as free electron lasers (FELs) and latest generationstorage rings led to rapid development of experimental methods relying on high radiation coherence. These methods allow to perform revolutionary studies in a wide range of fields from solid state physics to biology. In this thesis I focus on several important problems connected with the coherent methods. The first part considers applications of dynamical diffraction theory on crystals to studies with coherent X-ray radiation. It presents the design of a high-resolution spectrometer for free electron lasers that should allow to resolve spectral structure of individual FEL pulses. The spectrometer is based on the principle of dynamical diffraction focusing. The knowledge of individual FEL pulse spectra is necessary for understanding FEL longitudinal coherence. In the same part I present quasi-kinematical approximation to dynamical theory which allows to treat analytically phase effects observed in X-ray coherent imaging on nanocrystals. These effects may play a big role when methods such as ptychography are used to study crystalline samples. The second part deals with measurements of FEL coherence properties using intensity - intensity interferometry. Results of several experiments performed at FELs FLASH and LCLS are revealed in this section. I have developed models and theories to explain the behavior observed in experiments on FLASH. These models allowed to extract information about external positional jitter of FEL pulses and secondary beams present in FEL radiation. In the LCLS experiment the Hanbury Brown and Twiss type interferometry was performed on Bragg peaks from colloidal crystal. This did not require additional measurements without the sample and information was extracted directly from diffraction patterns. Therefore intensity

  8. Coherent methods in X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Gorobtsov, Oleg

    2017-05-15

    X-ray radiation has been used to study structural properties of materials for more than a hundred years. Construction of extremely coherent and bright X-ray radiation sources such as free electron lasers (FELs) and latest generationstorage rings led to rapid development of experimental methods relying on high radiation coherence. These methods allow to perform revolutionary studies in a wide range of fields from solid state physics to biology. In this thesis I focus on several important problems connected with the coherent methods. The first part considers applications of dynamical diffraction theory on crystals to studies with coherent X-ray radiation. It presents the design of a high-resolution spectrometer for free electron lasers that should allow to resolve spectral structure of individual FEL pulses. The spectrometer is based on the principle of dynamical diffraction focusing. The knowledge of individual FEL pulse spectra is necessary for understanding FEL longitudinal coherence. In the same part I present quasi-kinematical approximation to dynamical theory which allows to treat analytically phase effects observed in X-ray coherent imaging on nanocrystals. These effects may play a big role when methods such as ptychography are used to study crystalline samples. The second part deals with measurements of FEL coherence properties using intensity - intensity interferometry. Results of several experiments performed at FELs FLASH and LCLS are revealed in this section. I have developed models and theories to explain the behavior observed in experiments on FLASH. These models allowed to extract information about external positional jitter of FEL pulses and secondary beams present in FEL radiation. In the LCLS experiment the Hanbury Brown and Twiss type interferometry was performed on Bragg peaks from colloidal crystal. This did not require additional measurements without the sample and information was extracted directly from diffraction patterns. Therefore intensity

  9. Scanning small angle X-ray scattering investigations of bone

    International Nuclear Information System (INIS)

    Rinnerthaler, S.

    1998-06-01

    An important characteristic of bone is its strength, which is determined by bone mass, architecture and material quality. From a physical point of view bone is a composite material consisting of an organic matrix (collagen) and of inlets of mineral crystals (hydroxyapatite). These components build up a hierarchical, heterogeneous structure. The size of the mineral crystals lies in the nano-meter range and can be investigated by positionsensitive Small-Angle X-ray Scattering (Scanning-SAXS) in a non-destructive way. The average thickness, the degree and direction of the predominant orientation, as well as some information about shape and arrangement of the mineral crystals were determined in bones of humans, mice, and baboons by Scanning-SAXS with respect to age, bone diseases (osteogenesis imperfecta, pycnodysostosis) or medical treatments (fluoride or alendronate) of osteoporosis. The crystal thickness and the degree of orientation is much smaller in young individuals than in adults and the predominant orientation of the mineral crystals is different in a mixture of bone and mineralized cartilage compared to bone. Further, because position-resolved measurements are now possible, results from Scanning-SAXS measurements could be compared with the results of other position resolved methods. Due to this new feature it was possible, for the first time, to correlate directly 'mottled' bone visible in back-scattered electron imaging with small η-parameters evaluated from SAXS-patterns and the course of the collagen fibers with the predominant orientation of the mineral crystals. Scanning-SAXS proved to be a powerful tool to characterize bone nano-structure. (author)

  10. X-ray scatter removal by deconvolution

    International Nuclear Information System (INIS)

    Seibert, J.A.; Boone, J.M.

    1988-01-01

    The distribution of scattered x rays detected in a two-dimensional projection radiograph at diagnostic x-ray energies is measured as a function of field size and object thickness at a fixed x-ray potential and air gap. An image intensifier-TV based imaging system is used for image acquisition, manipulation, and analysis. A scatter point spread function (PSF) with an assumed linear, spatially invariant response is modeled as a modified Gaussian distribution, and is characterized by two parameters describing the width of the distribution and the fraction of scattered events detected. The PSF parameters are determined from analysis of images obtained with radio-opaque lead disks centrally placed on the source side of a homogeneous phantom. Analytical methods are used to convert the PSF into the frequency domain. Numerical inversion provides an inverse filter that operates on frequency transformed, scatter degraded images. Resultant inverse transformed images demonstrate the nonarbitrary removal of scatter, increased radiographic contrast, and improved quantitative accuracy. The use of the deconvolution method appears to be clinically applicable to a variety of digital projection images

  11. X-ray scattering studies of non-equilibrium ordering processes

    International Nuclear Information System (INIS)

    Nagler, S.E.

    1990-01-01

    We report on the progress of our project entitled ''X-ray Scattering of Non-Equilibrium Ordering Processes.'' During the past year we have made the first synchrotron measurements of ordering in Cu 3 Au have revealed the presence of an intermediate, non-equilibrium ordered state. Preliminary work involving x-ray magnetic scattering has been carried out. Work is continuing in these areas as well as on related problems. 5 refs

  12. Quantitative characterization of fatty liver disease using x-ray scattering

    International Nuclear Information System (INIS)

    Elsharkawy, Wafaa B.; Elshemey, Wael M.

    2013-01-01

    Nonalcoholic fatty liver disease (NAFLD) is a dynamic condition in which fat abnormally accumulates within the hepatocytes. It is believed to be a marker of risk of later chronic liver diseases, such as liver cirrhosis and carcinoma. The fat content in liver biopsies determines its validity for liver transplantation. Transplantation of livers with severe NAFLD is associated with a high risk of primary non-function. Moreover, NAFLD is recognized as a clinically important feature that influences patient morbidity and mortality after hepatic resection. Unfortunately, there is a lack in a precise, reliable and reproducible method for quantification of NAFLD. This work suggests a method for the quantification of NAFLD. The method is based on the fact that fatty liver tissue would have a characteristic x-ray scattering profile with a relatively intense fat peak at a momentum transfer value of 1.1 nm −1 compared to a soft tissue peak at 1.6 nm −1 . The fat content in normal and fatty liver is plotted against three profile characterization parameters (ratio of peak intensities, ratio of area under peaks and ratio of area under fat peak to total profile area) for measured and Monte Carlo simulated x-ray scattering profiles. Results show a high linear dependence (R 2 >0.9) of the characterization parameters on the liver fat content with a reported high correlation coefficient (>0.9) between measured and simulated data. These results indicate that the current method probably offers reliable quantification of fatty liver disease. - Highlights: • A method for the quantification of NAFLD is suggested. • Fatty liver tissue has characteristic x-ray scattering profile. • Profile characterization parameters show differences between normal and fatty liver. • Monte Carlo simulated x-ray scattering profiles are compared to measured

  13. Low-angle X-ray scattering from spices

    International Nuclear Information System (INIS)

    Desouky, O.S.; Ashour, Ahmed H.; Abdullah, Mohamed I.; Elshemey, Wael M.

    2002-01-01

    Low-angle scattering of X-rays is characterized by the presence of one or more peaks in the forward direction of scattering. These peaks are due to the interference of photons coherently scattered from the molecules of the medium. Thus these patterns are closely linked to the molecular structure of the investigated medium. In this work, low-angle X-ray scattering (LAXS) profiles of five spices; pimpinella anisum (anise), coriandrum sativum (coriander), cuminum cyminum (cumin), foenculum vulgare (fennel) and nigella sativa (nigella or black cumin) are presented after extensive measurements. It is found that all spices exhibit one characteristic peak at a scattering angle around 10 deg. This is equivalent to a value x=0.0565 A -1 , where x=sin(θ/2)/λ. The full width at half maximum (FWHM) of this peak is found to be characteristic for each type of the investigated spices. The possibility to detect the irradiation of these spices from their LAXS profiles is also examined after 10, 20, 30 and 40 kGy doses of gamma radiation. Except for anise, coriander and cumin at 40 kGy, there are no detectable deviations from the control samples in the scattering profiles of irradiated samples. These results comply with the recommendations of the FDA (US Food and Drug Administration) which defines 30 kGy as the maximum dose for irradiation of spices. The present technique could be used to detect over-irradiation, which causes damage to the molecular structure of some spices

  14. Inelastic X-ray Scattering Beamline Collaborative Development Team Final Report

    International Nuclear Information System (INIS)

    Burns, Clement

    2008-01-01

    This is the final report for the project to create a beam line for inelastic x-ray scattering at the Advanced Photon Source. The facility is complete and operating well, with spectrometers for both high resolution and medium resolution measurements. With the advent of third generation synchrotron sources, inelastic x-ray scattering (IXS) has become a valuable technique to probe the electronic and vibrational states of a wide variety of systems of interest in physics, chemistry, and biology. IXS is a weak probe, and experimental setups are complex and require well-optimized spectrometers which need a dedicated beamline to function efficiently. This project was the result of a proposal to provide a world-class, user friendly beamline for IXS at the Advanced Photon Source. The IXS Collaborative Development Team (IXS-CDT) was formed from groups at the national laboratories and a number of different universities. The beamline was designed from the front end to the experimental stations. Two different experimental stations were provided, one for medium resolution inelastic x-ray scattering (MERIX) and a spectrometer for high resolution inelastic x-ray scattering (HERIX). Funding for this project came from several sources as well as the DOE. The beamline is complete with both spectrometers operating well. The facility is now open to the general user community and there has been a tremendous demand to take advantage of the beamline's capabilities. A large number of different experiments have already been carried out on the beamline. A detailed description of the beamline has been given in the final design report (FDR) for the beamline from which much of the material in this report came. The first part of this report contains a general overview of the project with more technical details given later.

  15. Quantum effets in nonresonant X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Slowik, Jan Malte

    2015-11-15

    Due to their versatile properties, X rays are a unique tool to investigate the structure and dynamics of matter. X-ray scattering is the fundamental principle of many imaging techniques. Examples are X-ray crystallography, which recently celebrated one hundred years and is currently the leading method in structure determination of proteins, as well as X-ray phase contrast imaging (PCI), which is an imaging technique with countless applications in biology, medicine, etc. The technological development of X-ray free electron lasers (XFEL) has brought X-ray imaging at the edge of a new scientific revolution. XFELs offer ultrashort X-ray pulses with unprecedented high X-ray fluence and excellent spatial coherence properties. These properties make them an outstanding radiation source for X-ray scattering experiments, providing ultrafast temporal resolution as well as atomic spatial resolution. However, the radiation-matter interaction in XFEL experiments also advances into a novel regime. This demands a sound theoretical fundament to describe and explore the new experimental possibilities. This dissertation is dedicated to the theoretical study of nonresonant X-ray scattering. As the first topic, I consider the near-field imaging by propagation based X-ray phase contrast imaging (PCI). I devise a novel theory of PCI, in which radiation and matter are quantized. Remarkably, the crucial interference term automatically excludes contributions from inelastic scattering. This explains the success of the classical description thus far. The second topic of the thesis is the X-ray imaging of coherent electronic motion, where quantum effects become particularly apparent. The electron density of coherent electronic wave packets - important in charge transfer and bond breaking - varies in time, typically on femto- or attosecond time scales. In the near future, XFELs are envisaged to provide attosecond X-ray pulses, opening the possibility for time-resolved ultrafast X-ray scattering

  16. Quantum effets in nonresonant X-ray scattering

    International Nuclear Information System (INIS)

    Slowik, Jan Malte

    2015-11-01

    Due to their versatile properties, X rays are a unique tool to investigate the structure and dynamics of matter. X-ray scattering is the fundamental principle of many imaging techniques. Examples are X-ray crystallography, which recently celebrated one hundred years and is currently the leading method in structure determination of proteins, as well as X-ray phase contrast imaging (PCI), which is an imaging technique with countless applications in biology, medicine, etc. The technological development of X-ray free electron lasers (XFEL) has brought X-ray imaging at the edge of a new scientific revolution. XFELs offer ultrashort X-ray pulses with unprecedented high X-ray fluence and excellent spatial coherence properties. These properties make them an outstanding radiation source for X-ray scattering experiments, providing ultrafast temporal resolution as well as atomic spatial resolution. However, the radiation-matter interaction in XFEL experiments also advances into a novel regime. This demands a sound theoretical fundament to describe and explore the new experimental possibilities. This dissertation is dedicated to the theoretical study of nonresonant X-ray scattering. As the first topic, I consider the near-field imaging by propagation based X-ray phase contrast imaging (PCI). I devise a novel theory of PCI, in which radiation and matter are quantized. Remarkably, the crucial interference term automatically excludes contributions from inelastic scattering. This explains the success of the classical description thus far. The second topic of the thesis is the X-ray imaging of coherent electronic motion, where quantum effects become particularly apparent. The electron density of coherent electronic wave packets - important in charge transfer and bond breaking - varies in time, typically on femto- or attosecond time scales. In the near future, XFELs are envisaged to provide attosecond X-ray pulses, opening the possibility for time-resolved ultrafast X-ray scattering

  17. Ultrafast x-ray scattering on nanoparticle dynamics

    International Nuclear Information System (INIS)

    Plech, A; Ibrahimkutty, S; Issenmann, D; Kotaidis, V; Siems, A

    2013-01-01

    Pulsed X-ray scattering is used for the determination of structural dynamics of laser-irradiated gold particles. By combining several scattering methods such as powder scattering, small angle scattering and diffuse wide angle scattering it is possible to reconstruct the kinetics of structure evolution on several lengths scales and derive complementary information on the particles and their local environment. A generic structural phase diagram for the reaction as function of delay time after laser excitation and laser fluence can be constructed.

  18. X-ray scattering studies of non-equilibrium ordering processes: Progress report, November 1, 1988--October 31, 1989

    International Nuclear Information System (INIS)

    Nagler, S.E.

    1989-01-01

    We report on the progress of our project entitled ''X-ray Scattering Studies of Non-Equilibrium Ordering Processes.'' In-house time-resolved x-ray scattering has been used to investigate ordering kinetics in single crystal thin films of Cu 3 Au. Scaling analysis of the results shows that two dimensional kinetic behavior is observed in 260 /angstrom/ thick films. Significant improvements have been made in the local capabilities for fast time resolved measurements and data analysis. Measurements of microphase separation and ordering kinetics have been made in block-co-polymers, and experiments on Au-Cd martensitic material are continuing. 15 refs., 7 figs

  19. Theoretical approach to direct resonant inelastic X-ray scattering on magnets and superconductors

    Energy Technology Data Exchange (ETDEWEB)

    Marra, Pasquale

    2015-10-26

    The capability to probe the dispersion of elementary spin, charge, orbital, and lattice excitations has positioned resonant inelastic X-ray scattering (RIXS) at the forefront of photon science. In this work, we will investigate how RIXS can contribute to a deeper understanding of the orbital properties and of the pairing mechanism in unconventional high-temperature superconductors. In particular, we show how direct RIXS spectra of magnetic excitations can reveal long-range orbital correlations in transition metal compounds, by discriminating different kind of orbital order in magnetic and antiferromagnetic systems. Moreover, we show how RIXS spectra of quasiparticle excitations in superconductors can measure the superconducting gap magnitude, and reveal the presence of nodal points and phase differences of the superconducting order parameter on the Fermi surface. This can reveal the properties of the underlying pairing mechanism in unconventional superconductors, in particular cuprates and iron pnictides, discriminating between different superconducting order parameter symmetries, such as s,d (singlet pairing) and p wave (triplet pairing).

  20. Small angle x-ray scattering from proteins in solution

    International Nuclear Information System (INIS)

    de Souza, C.F.; Torriani, I.L.; Bonafe, C.F.S.; Merrelles, N.C.; Vachette, P.

    1989-01-01

    In this work the authors report experiments performed with giant respiratory proteins from annelids (erythrocruorins), known to have a molecular weight in the order of four million Daltons. Preliminary x-ray scattering data was obtained using a conventional rotating anode source. High resolution small angle scattering curves were obtained with synchrotron radiation from the DCI storage ring at LURE. Data from solutions with several protein concentrations were analyzed in order to determine low resolution dimensional parameters, using Guinier plots from the smeared scattering curves and the inverse transformation method

  1. Fractal morphology in lignite coal: a small angle x-ray scattering investigation

    International Nuclear Information System (INIS)

    Chitra, R.; Sen, D.; Mazumder, S.; Chandrasekaran, K.S.

    1999-01-01

    Small angle x-ray scattering technique has been used to study the pore morphology in lignite coal from Neyveli lignite mine (Tamilnadu, India). The sample were collected from three different locations of the same mine. SAXS profiles from all the three samples show almost identical functionality, irrespective of the locations from where the samples were collected. SAXS experiment using two different wavelengths also exhibit same functionality indicating the absence of multiple scattering. The analysis indicates the surface fractal nature of the pore morphology. The surface fractal dimension is calculated to be 2.58. (author)

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

    DEFF Research Database (Denmark)

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

    2014-01-01

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

  3. Magnetism in heterogeneous thin film systems: Resonant X-ray scattering studies

    International Nuclear Information System (INIS)

    Kortright, J.B.; Jiang, J.S.; Bader, S.D.; Hellwig, O.; Marguiles, D.T.; Fullerton, E.E.

    2002-01-01

    Magnetic and chemical heterogeneity are common in a broad range of magnetic thin film systems. Emerging resonant soft x-ray scattering techniques are well suited to resolve such heterogeneity at relevant length scales. Resonant x-ray magneto-optical Kerr effect measurements laterally average over heterogeneity but can provide depth resolution in different ways, as illustrated in measurements resolving reversible and irreversible changes in different layers of exchange-spring heterostructures. Resonant small-angle scattering measures in-plane heterogeneity and can resolve magnetic and chemical scattering sources in different ways, as illustrated in measurements of granular alloy recording media

  4. Direct imaging by atomic force microscopy of surface-localized self-assembled monolayers on a cuprate superconductor and surface X-ray scattering analysis of analogous monolayers on the surface of water

    DEFF Research Database (Denmark)

    Schougaard, Steen B.; Reitzel, Niels; Bjørnholm, Thomas

    2007-01-01

    A self-assembled monolayer of CF3(CF2)(3)(CH2)(11)NH2 atop the (001) surface of the high-temperature superconductor YBa2Cu3O7-x was imaged by atomic force microscopy (AFM). The AFM images provide direct 2D-structural evidence for the epitaxial 5.5 angstrom square root 2 x root 2R45 degrees unit...... was studied by grazing-incidence X-ray diffraction and specular X-ray reflectivity. Structural differences and similarities between the water-supported and superconductor-localized monolayers are discussed....

  5. Inelastic X-ray scattering activities in Europe

    International Nuclear Information System (INIS)

    Dorner, B.

    1984-01-01

    Inelastic X-ray scattering requires an energy determination before and after the scattering process together with a technique to vary at least one energy continuously in a controlled way. Sufficiently monochromatic beams can only be produced by Bragg reflection from single crystals. Stationary X-ray monochromators are standard equipment of conventional X-ray generators to select a particular characteristic line. Quite often they are curved to focus on the sample or the detector. Devices with variable Bragg angle have been and are used as analyzers in Compton scattering which is inelastic X-ray scattering with moderate resolution. With the rapidly increasing availability of synchrotron radiation (SR) monochromators and analyzers became more and more sophisticated improving momentum (Q) resolution and only somewhat the energy resolution ΔE which stays in the order of eV. Very high energy resolution can only be obtained with Bragg angles Theta near to 90 0 . This field is the topic of the present paper

  6. Preliminary Examination of X-ray Scattering from Human Tissues

    International Nuclear Information System (INIS)

    Desouky, O.S.; Wilkinson, S.; Hall, C.; Rogers, K.; Round, A.

    2008-01-01

    Small Angle x-ray scattering (SAXS) and wide angle x-ray scattering (WAXS) patterns have been recorded from different human soft tissues using x-ray synchrotron radiation.Pathological breast, normal kidney and lung tissues show SAXS peaks at q-values equal to 0.291 nm -1 and 0.481 nm -1 (d 21.6 nm and d =13. nm) which are the 3 r d and 5 t h order of the well known axial D-spacing of collagen fibrils. The diffraction is particularly intense in the meridional direction indicating some febrile alignment. In contrast, the normal tissue of brain, liver and heart shows diffuse scatter.The wide-angle coherent scattering from normal human tissues of brain, liver, heart, lung, and kidney is typical of that for amorphous materials. The scatter of the healthy adipose breast tissue shows a sharp peak at momentum transfer 1.24 nm -1 (d= 0.417 nm). The data of the other tissues appears to consist of a broad scattering peak. The two scattering regimes succeed in differentiating between the two major components of breast tissue, collagen and adipose tissue. The results of this study suggest that the soft tissues may have scattering patterns that are characteristics for the particular tissue types and tissue disease state. These results indicate that it may be possible use the coherent scattering as a diagnostic tool

  7. The 7th Japan-Taiwan joint meeting on neutron and X-ray scattering. Proceedings

    International Nuclear Information System (INIS)

    2016-03-01

    The 7th Japan-Taiwan joint meeting on neutron and X-ray scattering in Kumatori is held bilaterally in Japan and Taiwan. This meeting provides the recent outstanding results in the fields of fundamental polymer and biological sciences and their applications as well. In the fields of the X-ray and/or neutron scattering, the methodological progress expands the research fields and gives us new scientific insights. This meeting invites the researchers developing new methodologies, such as dynamics measurement utilizing nuclear Bragg resonance, subunit-kinetics measurement with deuteration-assisted small-angle neutron scattering and so on. (J.P.N.)

  8. Electrochemically adsorbed Pb on Ag (111) studied with grazing- incidence x-ray scattering

    International Nuclear Information System (INIS)

    Kortright, J.B.; Ross, P.N.; Melroy, O.R.; Toney, M.F.; Borges, G.L.; Samant, M.G.

    1989-04-01

    Grazing-incidence x-ray scattering studies of the evolution of electrochemically deposited layers of lead on silver (111) as a function of applied electrochemical potential are presented. Measurements were made with the adsorbed layers in contact with solution in a specially designed sample cell. The observed lead structures are a function of the applied potential and range from an incommensurate monolayer, resulting from underpotential deposition, to randomly oriented polycrystalline bulk lead, resulting from lower deposition potentials. These early experiments demonstrate the ability of in situ x-ray diffraction measurements to determine structures associated with electrochemical deposition. 6 refs., 4 figs

  9. Performance of a micro-strip gas chamber in solution X-ray scattering

    CERN Document Server

    Toyokawa, H; Inoko, Y; Nagayoshi, T; Nishi, Y; Nishikawa, Y; Ochi, A; Suzuki, M; Tanimori, T

    2001-01-01

    The performance of a Micro-Strip Gas Chamber in solution X-ray scattering was studied at the RIKEN structural biology beamline I of the SPring-8 facility. The practical dynamic range was confirmed to be approx 1,000,000 : 1 by measuring S sup - sup 4 decay from a polystyrene latex solution. Steep troughs of scattering profile from an apoferritin solution were clearly obtained without smearing. An unfolding process of a pH jump of cytochrome c was measured. A time resolution of 500 mu s was achieved.

  10. Observations of non-collective x-ray scattering in warm dense carbon plasma

    International Nuclear Information System (INIS)

    Bao Lihua; Zhang Jiyan; Zhao Yang; Ding Yongkun; Zhang Xiaoding

    2012-01-01

    An experiment for observing the spectrally resolved non-collective x-ray scattering in warm dense carbon plasma is presented in this paper. The experiment used Ta M-band x-rays to heat a foamed carbon cylinder sample isochorically and measured the scattering spectrum with a HOPG crystal spectrometer. The spectrum was compared with the calculation results using a Born-Mermin-approximation model. The best fitting was found at an electron temperature of T e =34 eV and an electron density of n e =1.6×10 23 cm −3 .

  11. Magnetic x-ray scattering studies of holmium using synchro- tron radiation

    International Nuclear Information System (INIS)

    Gibbs, D.; Moncton, D.E.; D'Amico, K.L.; Bohr, J.; Grier, B.H.

    1985-01-01

    We present the results of magnetic x-ray scattering experiments on the rare-earth metal holmium using synchrotron radiation. Direct high-resolution measurements of the nominally incommensurate magnetic satellite reflections reveal new lock-in behavior which we explain within a simple spin-discommensuration model. As a result of magnetoelastic coupling, the spin-discommensuration array produces additional x-ray diffraction satellites. Their observation further substantiates the model and demonstrates additional advantages of synchrotron radiation for magnetic-structure studies

  12. Malnutrition and myelin structure: an X-ray scattering study of rat sciatic and optic nerves

    International Nuclear Information System (INIS)

    Vargas, V.; Vargas, R.; Marquez, G.; Vonasek, E.; Mateu, L.; Luzzati, V.; Borges, J.

    2000-01-01

    Taking advantage of the fast and accurate X-ray scattering techniques recently developed in our laboratory, we tackled the study of the structural alterations induced in myelin by malnutrition. Our work was performed on sciatic and optic nerves dissected from rats fed with either a normal or a low-protein caloric diet, as a function of age (from birth to 60 days). By way of electrophysiological controls we also measured (on the sciatic nerves) the height and velocity of the compound action potential. Malnutrition was found to decrease the amount of myelin and to impair the packing order of the membranes in the sheaths. (orig.)

  13. Theoretical and experimental study of resonant inelastic X-ray scattering for NiO

    International Nuclear Information System (INIS)

    Kotani, A.; Matsubara, M.; Uozumi, T.; Ghiringhelli, G.; Fracassi, F.; Dallera, C.; Tagliaferri, A.; Brookes, N.B.; Braicovich, L.

    2006-01-01

    Resonant inelastic X-ray scattering (RIXS) spectra for Ni 2p to 3d excitation and 3d to 2p de-excitation of NiO are studied both theoretically and experimentally. Theoretical calculations with a single impurity Anderson model (SIAM) describe the charge transfer (CT) and d-d excitations in RIXS, and detailed study is made for the CT energy. High resolution RIXS measurements reveal the precise d-d excitation structure and its polarization dependence, and they are well reproduced by the SIAM calculation

  14. X-ray scattering studies of non-equilibrium ordering processes

    International Nuclear Information System (INIS)

    Nagler, S.E.

    1991-01-01

    We report on the progress of the project entitled ''X-ray Scattering Studies of Non-Equilibrium Ordering Processes.'' The past year has seen continued progress in the study of kinetic effects in metallic binary alloys and polymers. In addition, work has begun on a low dimensional CDW system: blue bronze. A sample chamber has been constructed to perform small angle neutron scattering measurements on a model quantum system with phase separation: solid He3/He4. Work is continuing on magnetic systems. Planned future experiments include an investigation of crystallization in Rubidium

  15. Heavy particle dynamics in liquid Se. Inelastic x-ray scattering

    International Nuclear Information System (INIS)

    Inui, Masanori; Hosokawa, Shinya; Matsuda, Kazuhiro; Tsutsui, Satoshi; Baron, A. Q. R.

    2007-01-01

    The dynamic structure factor of liquid Se was measured at 523 K using high-resolution inelastic X-ray scattering. Anomalous narrowing of the spectrum was observed at 15 nm -1 , where the static structure factor S(Q) exhibits a weak shoulder, but the elastic part of the dynamic structure factor S(Q, E=0) exhibited a strong maximum. The second frequency moment, which is estimated from only the quasielastic peak, is consistent with the motion of rigid six-atom clusters, while a formal agreement with the first-moment sum rule is preserved by the appearance of a weak intramolecular mode at 30 meV. (author)

  16. Small angle neutron and x-ray scattering studies of self-assembled nano structured materials

    International Nuclear Information System (INIS)

    Choi, Sung Min

    2009-01-01

    Full text: Small angle neutron and x-ray scattering are very powerful techniques to investigate nano structured materials. In this presentation, examples of nano structured materials investigated by neutron and x-ray scattering will be presented. Part I: The unique anisotropic physical properties of columnar discotic liquid crystals (DLCs) have attracted considerable interest for their potential applications as electronic devices. For many practical applications, however, it is crucial to obtain uniaxially oriented and highly ordered columnar superstructures of DLC molecules covering macroscopic area. Here, we present a simple and straight-forward approach to fabricate uniaxially oriented and highly ordered columnar superstructures of cobalt octa(n-decylthio) porphyrazine (CoS 1 0), a discotic supra-molecule, in bulk and on substrates [1] over a macroscopic length scale, utilizing an applied magnetic field and the interaction of CoS 1 0 with an OTS-functionalized substrate. The details of the oriented and ordered columnar nano-structures are investigated by SANS and GISAXS. Part II: Self-assembly of one-dimensional (1D) nanoparticles with metallic or semiconducting properties into highly ordered superstructures using various interactions has been of great interest as a route towards materials with new functionalities. Here, we report a new phase diagram of negatively charged 1D nanoparticle (cROD) and cationic liposome (CL) complexes in water which exhibit three different highly ordered phases [2]. Small angle neutron and x-ray scattering measurements show that the cROD-CL complexes exhibit three different highly ordered phases, intercalated lamellar, doubly intercalated lamellar and centered rectangular phases, depending on particle curvature and electrostatic interactions. The new phase diagram can be used to understand and design new highly ordered self-assemblies of 1D nanoparticles in soft matter which provide new functionalities. (author)

  17. X-ray scattering for the characterization of lyophilized breast tissue samples

    International Nuclear Information System (INIS)

    Elshemey, Wael M.; Mohamed, Fayrouz S.; Khater, Ibrahim M.

    2013-01-01

    This work investigates the possibility of characterizing breast cancer by measuring the X-ray scattering profiles of lyophilized excised breast tissue samples. Since X-ray scattering from water-rich tissue is dominated by scattering from water, the removal of water by lyophilization would enhance the characterization process. In the present study, X-ray scattering profiles of 22 normal, 22 malignant and 10 benign breast tissue samples are measured. The cut-offs of scatter diagrams, sensitivity, specificity and diagnostic accuracy of three characterization parameters (full width at half maximum (FWHM) for the peak at 1.1 nm −1 , area under curve (AUC), and ratio of 1st to 2nd scattering peak intensities (I 1 /I 2 %)) are calculated and compared to the data from non-lyophilized samples. Results show increased sensitivity (up to 100%) of the present data on lyophilized breast tissue samples compared to previously reported data for non-lyophilized samples while the specificity (up to 95.4%), diagnostic accuracy (up to 95.4%) and receiver operating characteristic (ROC) curve values (up to 0.9979) for both sets of data are comparable. The present study shows significant differences between normal samples and each of malignant and benign samples. Only subtle differences exist between malignant and benign lyophilized breast tissue samples where FWHM=0.7±0.1 and 0.8±0.3, AUC=1.3±0.2 and 1.4±0.2 and I 1 /I 2 %=44.9±11.0 and 52.4±7.6 for malignant and benign samples respectively. - Highlights: • X-ray scattering profiles of breast tissue samples are acquired. • Three X-ray profile characterization parameters are calculated. • The cut-offs, sensitivity, specificity and diagnostic accuracy are calculated. • They are compared to the data from non-lyophilized samples. • Results show increased sensitivity in case of lyophilized samples

  18. Defect properties from X-ray scattering experiments

    International Nuclear Information System (INIS)

    Peisl, H.

    1976-01-01

    Lattice distortions due to defects in crystals can be studied most directly by elastic X-ray or neutron scattering experiments. The 'size' of the defects can be determined from the shift of the Bragg reflections. Defect induced diffuse scattering intensity close to and between Bragg reflections gives information on the strength and symmetry of the distortion fields and yields the atomic structure of point defects (interstitials, vacancies, small aggregates). Diffuse scattering is a very sensitive method to decide whether defects are present as isolated point defects or have formed aggregates. X-ray scattering has been used to study defects produced in various ionic crystals by γ- and neutron irradiation. After an introduction to the principles of the method the experimental results will be reviewed and discussed in some detail. (orig.) [de

  19. Anomalous x-ray scattering studies of functional disordered materials

    International Nuclear Information System (INIS)

    Kohara, S; Tajiri, H; Song, C H; Ohara, K; Temleitner, L; Sugimito, K; Fujiwara, A; Pusztai, L; Usuki, T; Hosokawa, S; Benino, Y; Kitamura, N; Fukumi, K

    2014-01-01

    We have developed anomalous x-ray scattering (AXS) spectrometers, that employ intrinsic Ge detectors and crystal analyzers, at SPring-8. The use of LiF analyzer crystal provides us with an energy resolution of ∼ 12 eV. Furthermore, it has been established that the use of AXS technique is essential to reveal the relationship between the atomic structure and its function of a fast phase-change material, Ge 2 Sb 2 Te 5 . We were able to address the issue of why the amorphous phase of fast phase change materials is stable at room temperature for a long time despite the fact that it can rapidly transform to the crystalline phase by using a combination of AXS and large scale density functional theory-based molecular dynamics simulations.

  20. Small angle X-ray scattering on concentrated hemoglobin solutions

    International Nuclear Information System (INIS)

    Zinke, M.; Damaschun, G.; Mueller, J.J.; Ruckpaul, K.

    1978-01-01

    The small-angle X-ray scattering technique was used to determine the intermolecular structure and interaction potentials in oxi-and deoxi-hemoglobin solutions. The pair correlation function obtained by the ZERNICKE-PRINS equation characterizes the intermolecular structure of the hemoglobin molecules. The intermolecular structure is concentration dependent. The hemoglobin molecules have a 'short range order structure' with a range of about 4 molecule diameters at 324 g/l. The potential functions of the hemoglobin-hemoglobin interaction have been determined on the basis of fluid theories. Except for the deoxi-hemoglobin solution having the concentration 370 g/l, the pair interaction consists in a short repulsion and a weak short-range attraction against kT. The potential minimum is between 1.2 - 1.5 nm above the greatest hemoglobin diameter. (author)

  1. Inelastic x-ray scattering from polycrystalline materials

    International Nuclear Information System (INIS)

    Fischer, I.

    2008-09-01

    Inelastic X-ray scattering (IXS) is a tool to determine the phonon dispersion along high symmetry directions in single crystals. However, novel materials and crystals under extreme conditions are often only available in form of polycrystalline samples. Thus the investigation is limited to orientation-averaged properties. To overcome these limitations, a methodology to extract the single crystal phonon dispersion from polycrystalline materials was developed. The approach consists of recording IXS spectra over a large momentum transfer region and confront them with a Born - von Karman model calculation. A least-square refinement of the model IXS spectra then provides the single crystal dispersion scheme. In this work the method is developed on the test case Be. Further studies were performed on more and more complex systems, in order to explore the limitations. This novel application of IXS promises to be a valuable tool in cases where single crystalline materials are not available. (author)

  2. Revealing inner shell dynamics with inelastic X-ray scattering

    International Nuclear Information System (INIS)

    Franck, C.

    1990-01-01

    One of the many opportunities provided by the Advanced Photon Source (APS) is to extend the study of intra-atomic dynamics. As a means of testing dynamic response, inelastic x-ray scattering is particularly promising since it allows us to independently vary the period of the exciting field in both space and time. As an example of this type of work, the author presents experiments performed at the Cornell High Energy Synchrotron Source (CHESS) laboratory, a prototype for the APS. This was inner shell inelastic scattering with a twist: in order to explore a new distance scale an x-ray fluorescence trigger was employed. Aside for the atomic insight gained, the experiment taught them the importance of the time structure of the synchrotron beam for coincidence experiments which are dominated by accidental events

  3. Femtosecond X-ray scattering in condensed matter

    Energy Technology Data Exchange (ETDEWEB)

    Korff Schmising, Clemens von

    2008-11-24

    This thesis investigates the manifold couplings between electronic and structural properties in crystalline Perovskite oxides and a polar molecular crystal. Ultrashort optical excitation changes the electronic structure and the dynamics of the connected reversible lattice rearrangement is imaged in real time by femtosecond X-ray scattering experiments. An epitaxially grown superlattice consisting of alternating nanolayers of metallic and ferromagnetic strontium ruthenate (SRO) and dielectric strontium titanate serves as a model system to study optically generated stress. In the ferromagnetic phase, phonon-mediated and magnetostrictive stress in SRO display similar sub-picosecond dynamics, similar strengths but opposite sign and different excitation spectra. The amplitude of the magnetic component follows the temperature dependent magnetization square, whereas the strength of phononic stress is determined by the amount of deposited energy only. The ultrafast, phonon-mediated stress in SRO compresses ferroelectric nanolayers of lead zirconate titanate in a further superlattice system. This change of tetragonal distortion of the ferroelectric layer reaches up to 2 percent within 1.5 picoseconds and couples to the ferroelectric soft mode, or ion displacement within the unit cell. As a result, the macroscopic polarization is reduced by up to 100 percent with a 500 femtosecond delay that is due to final elongation time of the two anharmonically coupled modes. Femtosecond photoexcitation of organic chromophores in a molecular, polar crystal induces strong changes of the electronic dipole moment via intramolecular charge transfer. Ultrafast changes of transmitted X-ray intensity evidence an angular rotation of molecules around excited dipoles following the 10 picosecond kinetics of the charge transfer reaction. Transient X-ray scattering is governed by solvation, masking changes of the chromophore's molecular structure. (orig.)

  4. Femtosecond X-ray scattering in condensed matter

    International Nuclear Information System (INIS)

    Korff Schmising, Clemens von

    2008-01-01

    This thesis investigates the manifold couplings between electronic and structural properties in crystalline Perovskite oxides and a polar molecular crystal. Ultrashort optical excitation changes the electronic structure and the dynamics of the connected reversible lattice rearrangement is imaged in real time by femtosecond X-ray scattering experiments. An epitaxially grown superlattice consisting of alternating nanolayers of metallic and ferromagnetic strontium ruthenate (SRO) and dielectric strontium titanate serves as a model system to study optically generated stress. In the ferromagnetic phase, phonon-mediated and magnetostrictive stress in SRO display similar sub-picosecond dynamics, similar strengths but opposite sign and different excitation spectra. The amplitude of the magnetic component follows the temperature dependent magnetization square, whereas the strength of phononic stress is determined by the amount of deposited energy only. The ultrafast, phonon-mediated stress in SRO compresses ferroelectric nanolayers of lead zirconate titanate in a further superlattice system. This change of tetragonal distortion of the ferroelectric layer reaches up to 2 percent within 1.5 picoseconds and couples to the ferroelectric soft mode, or ion displacement within the unit cell. As a result, the macroscopic polarization is reduced by up to 100 percent with a 500 femtosecond delay that is due to final elongation time of the two anharmonically coupled modes. Femtosecond photoexcitation of organic chromophores in a molecular, polar crystal induces strong changes of the electronic dipole moment via intramolecular charge transfer. Ultrafast changes of transmitted X-ray intensity evidence an angular rotation of molecules around excited dipoles following the 10 picosecond kinetics of the charge transfer reaction. Transient X-ray scattering is governed by solvation, masking changes of the chromophore's molecular structure. (orig.)

  5. X-Ray Scattering Studies of the Liquid-Vapor Interface of Gallium.

    Science.gov (United States)

    Kawamoto, Eric Hitoshi

    A UHV system was developed for performing X-ray scattering studies and in situ analyses of liquid metal surfaces. A nearly ideal choice for this study, gallium has a melting point just above room temperature; is amenable to handling in both air and vacuum; its surface oxides can be removed while its cleanliness is maintained and monitored. Using argon glow-discharge sputtering techniques to remove intervening surface oxides, thin wetting layers of gallium were prepared atop nonreactive substrates, to be used as samples suited for liquid surface scattering experiments. Preliminary measurements of X-ray reflectivity from the liquid-vapor interface of gallium were performed with the X-ray UHV chamber configured for use in conjunction with liquid surface spectrometers at two synchrotron beamlines. A novel technique for carrying out and interpreting scattering measurements from curved liquid surfaces was demonstrated. The energy tunability and intense focused white beam flux from a wiggler source was shown to place within reach the large values of wavevector transfer at which specular reflectivity data yield small length scale information about surface structure. Various theoretical treatments and simulations predict quasi-lamellar ordering of atoms near the free surface of metallic liquids due to energetics particular to metals (electron delocalization, the dependence of system energy on ion and electron densities, surface tension and electrostatic energy). However, the experimental data reported to date is insufficient to distinguish between a monotonic, sigmoidal electron density profile found at the free surfaces of dielectric liquids, and the damped oscillatory layer-like profiles anticipated for metallic liquids. Out to a wavevector transfer of Q = 0.55 A ^{-1}, the reflectivity data measured from a curved Ga surface is not inconsistent with what is expected for a liquid-vapor electron density profile of Gaussian width sigma = 1.3 +/- 0.2 A. Subsequent

  6. An Assessment of Critical Dimension Small Angle X-ray Scattering Metrology for Advanced Semiconductor Manufacturing

    Energy Technology Data Exchange (ETDEWEB)

    Settens, Charles M. [State Univ. of New York (SUNY), Albany, NY (United States)

    2015-01-01

    Simultaneous migration of planar transistors to FinFET architectures, the introduction of a plurality of materials to ensure suitable electrical characteristics, and the establishment of reliable multiple patterning lithography schemes to pattern sub-10 nm feature sizes imposes formidable challenges to current in-line dimensional metrologies. Because the shape of a FinFET channel cross-section immediately influences the electrical characteristics, the evaluation of 3D device structures requires measurement of parameters beyond traditional critical dimension (CD), including their sidewall angles, top corner rounding and footing, roughness, recesses and undercuts at single nanometer dimensions; thus, metrologies require sub-nm and approaching atomic level measurement uncertainty. Synchrotron critical dimension small angle X-ray scattering (CD-SAXS) has unique capabilities to non-destructively monitor the cross-section shape of surface structures with single nanometer uncertainty and can perform overlay metrology to sub-nm uncertainty. In this dissertation, we perform a systematic experimental investigation using CD-SAXS metrology on a hierarchy of semiconductor 3D device architectures including, high-aspect-ratio contact holes, H2 annealed Si fins, and a series of grating type samples at multiple points along a FinFET fabrication process increasing in structural intricacy and ending with fully fabricated FinFET. Comparative studies between CD-SAXS metrology and other relevant semiconductor dimensional metrologies, particularly CDSEM, CD-AFM and TEM are used to determine physical limits of CD-SAXS approach for advanced semiconductor samples. CD-SAXS experimental tradeoffs, advice for model-dependent analysis and thoughts on the compatibility with a semiconductor manufacturing environment are discussed.

  7. Atomic dynamics in fluids studied by inelastic x-ray scattering

    International Nuclear Information System (INIS)

    Inui, Masanori; Kajihara, Yukio; Matsuda, Kazuhiro; Ishikawa, Daisuke; Tsutsui, Satoshi; Baron, Alfred Q.

    2010-01-01

    Studies on atomic dynamics in supercritical fluids at high temperature and high pressure have remarkably been advanced by using an inelastic x-ray scattering technique that achieved a meV-energy resolution in the middle of 1990's. In this article, we describe a brief review of the theoretical background on liquid dynamics, our own high-temperature high-pressure technique and recent results of atomic dynamics in supercritical fluids. In particular, we report the results of inelastic x-ray scattering measurements for expanding fluid Hg at high temperature and high pressure, which were conduced at BL35XU/SPring-8. We found that in the metal-nonmetal transition in fluid Hg, the excitation energy of the acoustic mode disperses three times faster than the adiabatic sound velocity obtained by ultrasonic measurements. This phenomenon must be crucial to understand how a metallic state is formed during atomic condensation accurately. Finally we put a future development of this field in perspective. (author)

  8. Quantitative characterization of fatty liver disease using x-ray scattering

    Science.gov (United States)

    Elsharkawy, Wafaa B.; Elshemey, Wael M.

    2013-11-01

    Nonalcoholic fatty liver disease (NAFLD) is a dynamic condition in which fat abnormally accumulates within the hepatocytes. It is believed to be a marker of risk of later chronic liver diseases, such as liver cirrhosis and carcinoma. The fat content in liver biopsies determines its validity for liver transplantation. Transplantation of livers with severe NAFLD is associated with a high risk of primary non-function. Moreover, NAFLD is recognized as a clinically important feature that influences patient morbidity and mortality after hepatic resection. Unfortunately, there is a lack in a precise, reliable and reproducible method for quantification of NAFLD. This work suggests a method for the quantification of NAFLD. The method is based on the fact that fatty liver tissue would have a characteristic x-ray scattering profile with a relatively intense fat peak at a momentum transfer value of 1.1 nm-1 compared to a soft tissue peak at 1.6 nm-1. The fat content in normal and fatty liver is plotted against three profile characterization parameters (ratio of peak intensities, ratio of area under peaks and ratio of area under fat peak to total profile area) for measured and Monte Carlo simulated x-ray scattering profiles. Results show a high linear dependence (R2>0.9) of the characterization parameters on the liver fat content with a reported high correlation coefficient (>0.9) between measured and simulated data. These results indicate that the current method probably offers reliable quantification of fatty liver disease.

  9. The current status of small-angle x-ray scattering beamline at Diamond Light Source

    International Nuclear Information System (INIS)

    Inoue, Katsuaki; Doutch, James; Terrill, Nick

    2013-01-01

    The small-angle X-ray scattering (SAXS) covers the major disciplines of biology, chemistry and physics delivering structural and dynamic information in nanoscience, mesoscopic architectures, supramolecular structures, and nucleation/growth of crystals. SAXS is also proving to be important in archaeological, environmental, and conservation sciences, and has further indicated its ability to span wide-ranging scientific disciplines. Thus, strong needs for SAXS studies are increasing significantly in a broad range of scientific fields year by year. Based on such a background, the demand for high throughput SAXS experiments is increasing. At the synchrotron facility, Diamond Light Source, one SAXS beamline, Non-crystalline diffraction I22 is now operational and highly automated throughput small-angle X-ray scattering (HATSAXS) beamline B21 is now under construction. I22 is the Undulator beamline and wide varieties of experiments, including time-resolved experiments are attempted. Based on the concept of HATSAXS, the key feature of B21 will focuses on the automation of end-station equipment. A automated sample changer has been purchased for solution SAXS measurements on biomolecules. A robotic-arm-type automated sample changer that is capable of handling several kinds of samples in material science is also being constructed. B21 is expected to successfully provide all users highly automated throughput measurements with the highest possible reliability and accuracy. Construction of this beamline will end in the second half of 2012, and will be open for users in the early summer of 2013 after commissioning. (author)

  10. Evolution of elastic x-ray scattering in laser-shocked warm dense lithium.

    Science.gov (United States)

    Kugland, N L; Gregori, G; Bandyopadhyay, S; Brenner, C M; Brown, C R D; Constantin, C; Glenzer, S H; Khattak, F Y; Kritcher, A L; Niemann, C; Otten, A; Pasley, J; Pelka, A; Roth, M; Spindloe, C; Riley, D

    2009-12-01

    We have studied the dynamics of warm dense Li with near-elastic x-ray scattering. Li foils were heated and compressed using shock waves driven by 4-ns-long laser pulses. Separate 1-ns-long laser pulses were used to generate a bright source of 2.96 keV Cl Ly- alpha photons for x-ray scattering, and the spectrum of scattered photons was recorded at a scattering angle of 120 degrees using a highly oriented pyrolytic graphite crystal operated in the von Hamos geometry. A variable delay between the heater and backlighter laser beams measured the scattering time evolution. Comparison with radiation-hydrodynamics simulations shows that the plasma is highly coupled during the first several nanoseconds, then relaxes to a moderate coupling state at later times. Near-elastic scattering amplitudes have been successfully simulated using the screened one-component plasma model. Our main finding is that the near-elastic scattering amplitudes are quite sensitive to the mean ionization state Z[over ] and by extension to the choice of ionization model in the radiation-hydrodynamics simulations used to predict plasma properties within the shocked Li.

  11. Evolution of elastic x-ray scattering in laser-shocked warm dense lithium

    International Nuclear Information System (INIS)

    Kugland, N. L.; Niemann, C.; Gregori, G.; Bandyopadhyay, S.; Spindloe, C.; Brenner, C. M.; Brown, C. R. D.; Constantin, C.; Glenzer, S. H.; Khattak, F. Y.; Kritcher, A. L.; Otten, A.; Pelka, A.; Roth, M.; Pasley, J.; Riley, D.

    2009-01-01

    We have studied the dynamics of warm dense Li with near-elastic x-ray scattering. Li foils were heated and compressed using shock waves driven by 4-ns-long laser pulses. Separate 1-ns-long laser pulses were used to generate a bright source of 2.96 keV Cl Ly-α photons for x-ray scattering, and the spectrum of scattered photons was recorded at a scattering angle of 120 deg. using a highly oriented pyrolytic graphite crystal operated in the von Hamos geometry. A variable delay between the heater and backlighter laser beams measured the scattering time evolution. Comparison with radiation-hydrodynamics simulations shows that the plasma is highly coupled during the first several nanoseconds, then relaxes to a moderate coupling state at later times. Near-elastic scattering amplitudes have been successfully simulated using the screened one-component plasma model. Our main finding is that the near-elastic scattering amplitudes are quite sensitive to the mean ionization state Z and by extension to the choice of ionization model in the radiation-hydrodynamics simulations used to predict plasma properties within the shocked Li.

  12. Small angle X-ray scattering and transmission electron microscopy study of the Lactobacillus brevis S-layer protein

    Energy Technology Data Exchange (ETDEWEB)

    Jaeaeskelaeinen, Pentti [Department of Biomedical Engineering and Computational Science, PO Box 2200, FI-02015 Aalto University School of Science and Technology (Finland); Engelhardt, Peter [Haartman Institute, Department of Pathology, PO Box 21, FIN-00014 University of Helsinki (Finland); Hynoenen, Ulla; Palva, Airi [Department of Basic Veterinary Sciences, Division of Microbiology, FIN-00014 University of Helsinki (Finland); Torkkeli, Mika; Serimaa, Ritva, E-mail: ritva.serimaa@helsinki.f [Department of Physics, POB 64, 00014 University of Helsinki (Finland)

    2010-10-01

    The structure of self-assembly domain containing recombinant truncation mutants of Lactobacillus brevis surface layer protein SlpA in aqueous solution was studied using small-angle X-ray scattering and transmission electron microscopy. The proteins were found out to interact with each other forming stable globular oligomers of about 10 monomers. The maximum diameter of the oligomers varied between 75 A and 435 A.

  13. Determination of the thermodynamic state of concentrated hemoglobin solutions by means of small angle X-ray scattering

    International Nuclear Information System (INIS)

    Zinke, M.

    1979-01-01

    Exemplified by hemoglobin, the thermodynamic equilibrium properties of the dissolved macromolecular system could be determined solely from the small angle X-ray scattering of concentrated macromolecular solutions via the intermolecular structure of the dissolved macromolecules and their intermolecular potentials. From the scattering experiment on concentrated Hb solutions the concentration dependence of the following properties of the dissolved Hb system were determined: fluctuation, isothermic compressibility, internal energy, surface tension, and osmotic pressure. (author)

  14. Silicon Σ13(5 0 1) grain boundary interface structure determined by bicrystal Bragg rod X-ray scattering

    International Nuclear Information System (INIS)

    Howes, P.B.; Rhead, S.; Roy, M.; Nicklin, C.L.; Rawle, J.L.; Norris, C.A.

    2013-01-01

    The atomic structure of the silicon Σ13(5 0 1) symmetric tilt grain boundary interface has been determined using Bragg rod X-ray scattering. In contrast to conventional structural studies of grain boundary structure using transmission electron microscopy, this approach allows the non-destructive measurement of macroscopic samples. The interface was found to have a single structure that is fully fourfold coordinated. X-ray diffraction data were measured at Beamline I07 at the Diamond Light Source

  15. High-resolution inelastic X-ray scattering to study the high-frequency atomic dynamics of disordered systems

    International Nuclear Information System (INIS)

    Monaco, G.

    2008-01-01

    The use of momentum-resolved inelastic X-ray scattering with meV energy resolution to study the high-frequency atomic dynamics in disordered systems is here reviewed. The typical realization of this experiment is described together with some common models used to interpret the measured spectra and to extract parameters of interest for the investigation of disordered systems. With the help of some selected examples, the present status of the field is discussed. Particular attention is given to those results which are still open for discussion or controversial, and which will require further development of the technique to be fully solved. Such an instrumental development seems nowadays possible at the light of recently proposed schemes for advanced inelastic X-ray scattering spectrometers. (author)

  16. Resonant Inelastic X-ray Scattering of Rare-Earth and Copper Systems

    International Nuclear Information System (INIS)

    Kvashnina, Kristina

    2007-01-01

    Rare earths and copper systems were studied using X-ray absorption spectroscopy (XAS) and resonant inelastic X-ray scattering (RIXS). The use of monochromased synchotron radiation and improved energy resolution for RIXS made possible to obtain valuable information on the electronic structure in 4f, 5f and 3d systems. Experimental results for rare-earths (Ho, Gd, Cm, U, Np, Pu) were analyzed by atomic multiplet theory based on the Hartree-Fock calculations. The inelastic scattering structures in RIXS spectra at 5d edge of actinides found to be sensitive to actinide oxidation states in different systems. Comparison of experimental and calculated Cm 5d RIXS spectra gave direct information about valency of the 248-curium isotope in oxide. Scientific understanding of processes that control chemical changes of radioactive species from spent fuel is improved by studying interactions of actinide ions (U, Np, Pu) with corroded iron surfaces. RIXS measurements at the actinide 5d edge found to be sensitive to actinide oxidation states in different systems. Comparison of experimental and calculated Cm 5d RIXS spectra gave direct information about valency of the 248 curium isotope in oxide. Scientific understanding of processes that control chemical changes of radioactive species from spent fuel is improved by studying interactions of actinide ions (U, Np, Pu) with corroded iron surfaces. RIXS measurements at the actinide 5d edge indicate the reduction of U(VI), NP(V) and Pu(VI) to U(IV), Np(IV) and Pu(IV) by presence of iron ions. This thesis is also addressed to the study of changes in the electronic structure of copper films during interaction with synthetic groundwater solutions. The surface modifications induced by chemical reactions of oxidized 100 Angstrom Cu films with CL - , SO 4 2- and HCO 3 - ions in aqueous solutions with various concentrations were studied in-situ using XAS. It was shown that the pH value, the concentration of Cl - ion and presence of HC 3 - ion in

  17. Resonant Inelastic X-ray Scattering of Rare-Earth and CopperSystems

    Energy Technology Data Exchange (ETDEWEB)

    Kvashnina, Kristina [Uppsala Univ. (Sweden)

    2007-07-11

    Rare earths and copper systems were studied using X-ray absorption spectroscopy (XAS) and resonant inelastic X-ray scattering (RIXS). The use of monochromased synchotron radiation and improved energy resolution for RIXS made possible to obtain valuable information on the electronic structure in 4f, 5f and 3d systems. Experimental results for rare-earths (Ho, Gd, Cm, U, Np, Pu) were analyzed by atomic multiplet theory based on the Hartree-Fock calculations. The inelastic scattering structures in RIXS spectra at 5d edge of actinides found to be sensitive to actinide oxidation states in different systems. Comparison of experimental and calculated Cm 5d RIXS spectra gave direct information about valency of the 248-curium isotope in oxide. Scientific understanding of processes that control chemical changes of radioactive species from spent fuel is improved by studying interactions of actinide ions (U, Np, Pu) with corroded iron surfaces. RIXS measurements at the actinide 5d edge found to be sensitive to actinide oxidation states in different systems. Comparison of experimental and calculated Cm 5d RIXS spectra gave direct information about valency of the 248 curium isotope in oxide. Scientific understanding of processes that control chemical changes of radioactive species from spent fuel is improved by studying interactions of actinide ions (U, Np, Pu) with corroded iron surfaces. RIXS measurements at the actinide 5d edge indicate the reduction of U(VI), NP(V) and Pu(VI) to U(IV), Np(IV) and Pu(IV) by presence of iron ions. This thesis is also addressed to the study of changes in the electronic structure of copper films during interaction with synthetic groundwater solutions. The surface modifications induced by chemical reactions of oxidized 100 Angstrom Cu films with CL-, SO42- and HCO3- ions in aqueous solutions with various concentrations were studied in-situ using XAS. It was shown that the pH value, the

  18. Dichroism in resonant inelastic soft X-ray scattering

    International Nuclear Information System (INIS)

    Braicovich, L.

    2004-01-01

    Full text: The dichroism (and in particular the magnetic dichroism) has emerged in the last decade as a key method in the study of electronic states in solids. This has been largely due to the exploitation of the modern sources of Synchrotron Radiation. This approach has been extensively used in X ray Absorption Spectroscopy i.e. in a first order process giving a straightforward access, trough sum rules, to the ground state properties of the sample. On the other hand the studies of dichroism in second order processes as the photon scattering experiments has been up to now relatively limited probably due to experimental difficulties. This is too bad because, at least in principle, the scattering experiments offer unique opportunities typical of second order processes, beyond the possibilities offered by absorption spectroscopy. This requires specific scattering experiments able to give information that cannot be obtained in the absorption mode. A typical example is the circular magnetic dichroism in resonant inelastic scattering in perpendicular geometry i.e. with the light incident perpendicular to the magnetisation. In this case the circular dichroism in absorption is zero by symmetry while the detection of the scattered photons at an angle breaks the left-right symmetry and allows a dichroism to be observed. The aim of the present talk is to review critically the dichroism in resonant X-ray scattering and to show the potential of this approach. In particular it will be shown how to recover, in magnetic samples, the ground state information up to the moments of order four. In this connection original results will be presented including the demonstration of a new experimental approach. The perspectives of the field will be also discussed

  19. Anomalous small-angle x-ray scattering of a femtosecond irradiated germano silicate fibre preform.

    Energy Technology Data Exchange (ETDEWEB)

    Hindle, F.; Fertein, E.; Seifert, S.; Przygodski, C.S.; Bocquet, R.; Douay, M.; Bychkov, E.; Experimental Facilities Division (APS); LPCA, CNRS; PhLAM; Univ. des Sciences et Tech. de Lille

    2005-01-01

    RADIATION is shown to induce significant mesoscopic structure. The scattering intensity for irradiated glasses is close to two orders of magnitude greater than that of unexposed material. Anomalous small-angle X-ray scattering (ASAXS) around the germanium K-edge for the silica and germanium doped silica regions of a fiber preform is used to demonstrate that identical structures are induced in both glass materials, with germanium displaying a capacity to isomorphically replace silicon in the case of the germanium doped silica. Analysis of measured scattering indicates that photo-inscribed features are produced at two distinct scales with typical radii of R {approx} 20 Angstroms and R{sub min} {approx} 200 Angstroms.

  20. Inelastic X-ray scattering on liquid benzene analyzed using a generalized Langevin equation

    Science.gov (United States)

    Yoshida, Koji; Fukuyama, Nami; Yamaguchi, Toshio; Hosokawa, Shinya; Uchiyama, Hiroshi; Tsutsui, Satoshi; Baron, Alfred Q. R.

    2017-07-01

    The dynamic structure factor, S(Q,ω), of liquid benzene was measured by meV-resolved inelastic X-ray scattering (IXS) and analyzed using a generalized Langevin model with a memory function including fast, μ-relaxation and slow, structural, α-relaxation. The model well reproduced the experimental S(Q,ω) of liquid benzene. The dispersion relation of the collective excitation energy yields the high-frequency sound velocity for liquid benzene as related to the α-relaxation. The ratio of the high-frequency to the adiabatic sound velocity is approximately 1.5, larger to that of carbon tetrachloride and smaller than those of methanol and water, reflecting the nature of intermolecular interactions.

  1. Structural characterization of oxidized allotaxially grown CoSi2 layers by x-ray scattering

    International Nuclear Information System (INIS)

    Kaendler, I. D.; Seeck, O. H.; Schlomka, J.-P.; Tolan, M.; Press, W.; Stettner, J.; Kappius, L.; Dieker, C.; Mantl, S.

    2000-01-01

    A series of buried CoSi 2 layers prepared by a modified molecular beam epitaxy process (allotaxy) and a subsequent wet-oxidation process was investigated by x-ray scattering. The oxidation time which determines the depth in which the CoSi 2 layers are located within the Si substrates has been varied during the preparation. The electron density profiles and the structure of the interfaces were extracted from specular reflectivity and diffuse scattering measurements. Crystal truncation rod investigations yielded the structure on an atomic level (crystalline quality). It turns out that the roughness of the CoSi 2 layers increases drastically with increasing oxidation time, i.e., with increasing depth of the buried layers. Furthermore, the x-ray data reveal that the oxidation growth process is diffusion limited. (c) 2000 American Institute of Physics

  2. Some notes on data analysis for nuclear resonant inelastic x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Michael Y., E-mail: myhu@aps.anl.gov [Argonne National Laboratory (United States)

    2016-12-15

    Nuclear Resonant Inelastic X-ray Scattering (NRIXS) is a spectroscopy method to study atomic vibrations and dynamics, currently done with synchrotron radiation at a few high energy third generation facilities. It finds a wide range of applications in condensed matter physics, materials science, chemistry, biophysics, geosciences, and high-pressure researches. Many atomic dynamics and lattice thermodynamics information can be derived from NRIXS measurements. Phonon Density of States (DOS) characterizes lattice dynamics of a material and can be derived under the quasi-harmonic approximation. Combined with modeling and simulations, results from NRIXS can provide unique and clarifying insights into many fields of research. As for a spectroscopic technique, in order to be able to provide reliable information, close attention should be paid to many issues during experiments and data analysis afterwards. Here we discuss several issues relevant to its data analysis, namely, those of multiple sites, background treatments, and error estimates for some derived quantities.

  3. Seeing real-space dynamics of liquid water through inelastic x-ray scattering.

    Science.gov (United States)

    Iwashita, Takuya; Wu, Bin; Chen, Wei-Ren; Tsutsui, Satoshi; Baron, Alfred Q R; Egami, Takeshi

    2017-12-01

    Water is ubiquitous on earth, but we know little about the real-space motion of molecules in liquid water. We demonstrate that high-resolution inelastic x-ray scattering measurement over a wide range of momentum and energy transfer makes it possible to probe real-space, real-time dynamics of water molecules through the so-called Van Hove function. Water molecules are found to be strongly correlated in space and time with coupling between the first and second nearest-neighbor molecules. The local dynamic correlation of molecules observed here is crucial to a fundamental understanding of the origin of the physical properties of water, including viscosity. The results also suggest that the quantum-mechanical nature of hydrogen bonds could influence its dynamics. The approach used here offers a powerful experimental method for investigating real-space dynamics of liquids.

  4. Resonant inelastic X-ray scattering of liquid water

    International Nuclear Information System (INIS)

    Nilsson, Anders; Tokushima, Takashi; Horikawa, Yuka; Harada, Yoshihisa; Ljungberg, Mathias P.; Shin, Shik; Pettersson, Lars G.M.

    2013-01-01

    Highlights: ► Two peaks are observed in the lone pair region of the XES spectrum of water assigned to tetrahedral and distorted hydrogen bonding configurations. ► The isotope effect observed as different relative peak heights is due to spectral line shape differences. ► The two different hydrogen bonding environments can be related to local structures mimicking either low density water or high density water. -- Abstract: We review recent studies using resonant inelastic X-ray scattering (RIXS) or also here denoted X-ray emission spectroscopy (XES) on liquid water and the assignment of the two sharp peaks in the lone-pair region. Using the excitation energy dependence we connect the two peaks to specific features in the X-ray absorption (XAS) spectrum which have independently been assigned to molecules in tetrahedral or distorted configurations. The polarization dependence shows that both peaks are of 1b 1 origin supporting an interpretation in terms of two structural species, tetrahedral or disordered, which is furthermore consistent with the temperature-dependence of the two peaks. We discuss effects of life-time vibrational interference and how this affects the two components differently and also leads to differences in the relative peak heights for H 2 O and D 2 O. We show furthermore that the inherent structure in molecular dynamics simulations contain the structural bimodality suggested by XES, but this is smeared out in the real structure when temperature is included. We present a discussion around alternative interpretations suggesting that the origin of the two peaks is related to ultrafast dissociation and show evidence that such a model is inconsistent with several experimental observations and theoretical concepts. We conclude that the peaks reflect a temperature-dependent balance in fluctuations between tetrahedral and disordered structures in the liquid. This is well-aligned with theories of water under supercooled conditions and higher pressures

  5. Magnetic nanoparticles studied by small angle X-ray scattering

    International Nuclear Information System (INIS)

    Oliveira, Cristiano Luis Pinto; Antonel, Soledad; Negri, Martin

    2011-01-01

    because they exhibit magnetic (ferromagnetic) and electrical properties in the same material. Then, the nickel nanoparticles could be used for the development of electroelastic materials. In this case, the electrical conductivity of the material can be strongly dependent on the applied magnetic field, for example the case of nickel metal nanoparticles dispersed in a polymer, resulting in an anisotropic material with combined piezomagnetic and piezoelectric properties. In order to investigate the structural characteristics of cobalt-iron oxides and nickel nanoparticles, powder samples of those magnetic materials were studied by Small-Angle X-Ray Scattering. As will be shown, from the analysis and modeling of the scattering data, structural information could be obtained, enabling a detailed description of the structural properties of the studied samples which could be directly correlated to the magnetic properties. (author)

  6. Magnetic nanoparticles studied by small angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Cristiano Luis Pinto [Universidade de Sao Paulo (IF/USP), SP (Brazil). Inst. de Fisica. Grupo de Fluidos Complexos; Antonel, Soledad; Negri, Martin [Universidad de Buenos Aires (UBA) (Argentina). Facultad de Ciencias Exactas y Naturales. Dept. de Quimica Inorganica, Analitica y Quimica Fisica

    2011-07-01

    nanoparticles are very interesting because they exhibit magnetic (ferromagnetic) and electrical properties in the same material. Then, the nickel nanoparticles could be used for the development of electroelastic materials. In this case, the electrical conductivity of the material can be strongly dependent on the applied magnetic field, for example the case of nickel metal nanoparticles dispersed in a polymer, resulting in an anisotropic material with combined piezomagnetic and piezoelectric properties. In order to investigate the structural characteristics of cobalt-iron oxides and nickel nanoparticles, powder samples of those magnetic materials were studied by Small-Angle X-Ray Scattering. As will be shown, from the analysis and modeling of the scattering data, structural information could be obtained, enabling a detailed description of the structural properties of the studied samples which could be directly correlated to the magnetic properties. (author)

  7. Resonant inelastic X-ray scattering of liquid water

    Energy Technology Data Exchange (ETDEWEB)

    Nilsson, Anders, E-mail: nilsson@slac.stanford.edu [SUNCAT Ctr Interface Sci and Catalysis, SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, CA 94025 (United States); Stanford Synchrotron Radiation Lightsource, SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, CA 94025 (United States); Department of Physics, AlbaNova University Center, Stockholm University, SE-10691 (Sweden); Tokushima, Takashi [RIKEN/Spring-8, Sayo-cho, Sayo, Hyogo 679-5148 (Japan); Horikawa, Yuka [RIKEN/Spring-8, Sayo-cho, Sayo, Hyogo 679-5148 (Japan); Institute for Solid State Physics (ISSP), The University of Tokyo, Kashiwanoha, Kashiwa, Chiba 277-8581 (Japan); Harada, Yoshihisa [RIKEN/Spring-8, Sayo-cho, Sayo, Hyogo 679-5148 (Japan); Institute for Solid State Physics (ISSP), The University of Tokyo, Kashiwanoha, Kashiwa, Chiba 277-8581 (Japan); Synchrotron Radiation Research Organization, The University of Tokyo, Sayo-cho, Sayo, Hyogo 679-5165 (Japan); Ljungberg, Mathias P. [Department of Physics, AlbaNova University Center, Stockholm University, SE-10691 (Sweden); Institut de Ciencia de Materials de Barcelona (ICMAB-CSIC), Campus UAB, E-08193 Bellaterra (Spain); Shin, Shik [RIKEN/Spring-8, Sayo-cho, Sayo, Hyogo 679-5148 (Japan); Institute for Solid State Physics (ISSP), The University of Tokyo, Kashiwanoha, Kashiwa, Chiba 277-8581 (Japan); Synchrotron Radiation Research Organization, The University of Tokyo, Sayo-cho, Sayo, Hyogo 679-5165 (Japan); Pettersson, Lars G.M. [Department of Physics, AlbaNova University Center, Stockholm University, SE-10691 (Sweden)

    2013-06-15

    Highlights: ► Two peaks are observed in the lone pair region of the XES spectrum of water assigned to tetrahedral and distorted hydrogen bonding configurations. ► The isotope effect observed as different relative peak heights is due to spectral line shape differences. ► The two different hydrogen bonding environments can be related to local structures mimicking either low density water or high density water. -- Abstract: We review recent studies using resonant inelastic X-ray scattering (RIXS) or also here denoted X-ray emission spectroscopy (XES) on liquid water and the assignment of the two sharp peaks in the lone-pair region. Using the excitation energy dependence we connect the two peaks to specific features in the X-ray absorption (XAS) spectrum which have independently been assigned to molecules in tetrahedral or distorted configurations. The polarization dependence shows that both peaks are of 1b{sub 1} origin supporting an interpretation in terms of two structural species, tetrahedral or disordered, which is furthermore consistent with the temperature-dependence of the two peaks. We discuss effects of life-time vibrational interference and how this affects the two components differently and also leads to differences in the relative peak heights for H{sub 2}O and D{sub 2}O. We show furthermore that the inherent structure in molecular dynamics simulations contain the structural bimodality suggested by XES, but this is smeared out in the real structure when temperature is included. We present a discussion around alternative interpretations suggesting that the origin of the two peaks is related to ultrafast dissociation and show evidence that such a model is inconsistent with several experimental observations and theoretical concepts. We conclude that the peaks reflect a temperature-dependent balance in fluctuations between tetrahedral and disordered structures in the liquid. This is well-aligned with theories of water under supercooled conditions and

  8. Application of small-angle X-ray scattering for differentiation among breast tumors

    International Nuclear Information System (INIS)

    Changizi, V.; Kheradmand, A. Arab; Oghabian, M.A.

    2008-01-01

    Small-angle X-ray scattering (SAXS) is an X-ray diffraction-based technique where a narrow collimated beam of X-rays is focused onto a sample and the scattered X-rays recorded by a detector. The pattern of the scattered X-rays carries information on the molecular structure of the material. As breast cancer is the most widespread cancer in women and differentiation among its tumors is important, this project compared the results of coherent X-ray scattering measurements obtained from benign and malignant breast tissues. The energy-dispersive method with a setup including X-ray tube, primary collimator, sample holder, secondary collimator and high-purity germanium (HpGe) detector was used. One hundred thirty-one breast-tissue samples, including normal, fibrocystic changes and carcinoma, were studied at the 6 deg scattering angle. Diffraction profiles (corrected scattered intensity versus momentum transfer) of normal, fibrocystic changes and carcinoma were obtained. These profiles showed a few peak positions for adipose (1.15 ± 0.06 nm -1 ), mixed normal (1.15 ± 0.06 nm -1 and 1.4 ± 0.04 nm -1 ), fibrocystic changes (1.46 ± 0.05 nm -1 and 1.74 ± 0.04 nm -1 ) and carcinoma (1.55 ± 0.04 nm -1 , 1.73 ± 0.06 nm -1 , 1.85 ± 0.05 nm -1 ). We were able to differentiate between normal, fibrocystic changes (benign) and carcinoma (malignant) breast tissues by SAXS. However, we were unable to differentiate between different types of carcinoma. (author)

  9. Application of small-angle X-ray scattering for differentiation among breast tumors

    Directory of Open Access Journals (Sweden)

    Changizi V

    2008-01-01

    Full Text Available Small-angle X-ray scattering (SAXS is an X-ray diffraction-based technique where a narrow collimated beam of X-rays is focused onto a sample and the scattered X-rays recorded by a detector. The pattern of the scattered X-rays carries information on the molecular structure of the material. As breast cancer is the most widespread cancer in women and differentiation among its tumors is important, this project compared the results of coherent X-ray scattering measurements obtained from benign and malignant breast tissues. The energy-dispersive method with a setup including X-ray tube, primary collimator, sample holder, secondary collimator and high-purity germanium (HpGe detector was used. One hundred thirty-one breast-tissue samples, including normal, fibrocystic changes and carcinoma, were studied at the 6° scattering angle. Diffraction profiles (corrected scattered intensity versus momentum transfer of normal, fibrocystic changes and carcinoma were obtained. These profiles showed a few peak positions for adipose (1.15 ± 0.06 nm -1 , mixed normal (1.15 ± 0.06 nm -1 and 1.4 ± 0.04 nm -1 , fibrocystic changes (1.46 ± 0.05 nm -1 and 1.74 ± 0.04 nm -1 and carcinoma (1.55 ± 0.04 nm -1 , 1.73 ± 0.06 nm -1 , 1.85 ± 0.05 nm -1 . We were able to differentiate between normal, fibrocystic changes (benign and carcinoma (malignant breast tissues by SAXS. However, we were unable to differentiate between different types of carcinoma.

  10. Hierarchical nanoparticle morphology for platinum supported on SrTiO3 (0 0 1): A combined microscopy and X-ray scattering study

    International Nuclear Information System (INIS)

    Christensen, Steven T.; Lee, Byeongdu; Feng Zhenxing; Hersam, Mark C.; Bedzyk, Michael J.

    2009-01-01

    The morphology of metal nanoparticles supported on oxide substrates plays an important role in heterogeneous catalysis and in the nucleation of thin films. For platinum evaporated onto SrTiO 3 (0 0 1) and vacuum annealed we find an unexpected growth formation of Pt nanoparticles that aggregate into clusters without coalescence. This hierarchical nanoparticle morphology with an enhanced surface-to-volume ratio for Pt is analyzed by grazing incidence small-angle X-ray scattering (GISAXS), X-ray fluorescence (XRF), atomic force microscopy (AFM) and high-resolution scanning electron microscopy (SEM). The nanoparticle constituents of the clusters measure 2-4 nm in size and are nearly contiguously spaced where the average edge-to-edge spacing is less than 1 nm. These particles make up the clusters, which are 10-50 nm in diameter and are spaced on the order of 100 nm apart.

  11. Observation of Ortho-III correlations by neutron and hard x-ray scattering in an untwinned YBa2Cu3O6.77 single crystal

    DEFF Research Database (Denmark)

    Schleger, P.; Casalta, H.; Hadfield, R.

    1995-01-01

    We present measurements of Ortho-III phase correlations in an untwinned single crystal of YBa2Cu3O6.77 by neutron scattering and the novel method of hard (95 keV) X-ray scattering. The Ortho-III ordering is essentially two-dimensional, exhibiting Lorentzian peak shapes in the a-b plane. At room...

  12. Self-assembly behavior of discotic liquid crystals studied by neutron and X-ray scattering

    International Nuclear Information System (INIS)

    Kim, Hyo Sik

    2011-02-01

    We investigate both thermotropic and lyotropic phase behaviors in DLC molecules with detailed structural analysis which was performed by scattering methods such as small angle neutron scattering (SANS) and grazing incidence x-ray scattering (GIXS) techniques. First, for the study of thermotropic phase behavior in DLC, uniaxially oriented and well-ordered cobalt octa(n-decylthio)porphyrazine (CoS10) molecules in thin-film was used as a model molecule. Second, the lyotropic phase behavior in DLC was studied using model system, hexa-n-dodecyl-hexa-peri-hexabenzocoronene (HBC-C12) in organic solvent (p-xylene). The method for uniaxially oriented and highly ordered columnar superstructure of CoS10 on a large area of substrate (3 cm x 3 cm) has been developed by using applied magnetic field (ca. 1.0 T) and surface interaction simultaneously. When spin-coated CoS10 thin film on an OTS-functionalized silicon substrate was cooled from its isotropic phase to liquid crystalline phase in the presence of an applied magnetic field, the CoS10 formed uniaxially oriented and 'edge-on' arrangement of columnar superstructures with their columnar directors perpendicular to the applied magnetic field. Grazing incidence x-ray scattering (GIXS) measurements showed that CoS10 columns form rectangular columnar packing with a tilted arrangement against the columnar axis (ca. 40 .deg.) in columns. The effects of film thickness on the columnar packing structure in supported thin-films of CoS10 have been investigated by the GISAXS technique, with magnetically aligned CoS10 films on OTS-functionalized substrates used as model systems. CoS10 columnar superstructures in thin-films with thicknesses ranging from 49 nm to 845 nm were uniaxially oriented with 'edge-on' arrangement using magnetic field and surface interaction. The orientational ordering of the columnar packing in the plane perpendicular to the applied magnetic field is strongly dependent on the film thickness. While it is damped by

  13. High-resolution x-ray scattering studies of charge ordering in highly correlated electron systems

    International Nuclear Information System (INIS)

    Ghazi, M.E.

    2002-01-01

    Many important properties of transition metal oxides such as, copper oxide high-temperature superconductivity and colossal magnetoresistance (CMR) in manganites are due to strong electron-electron interactions, and hence these systems are called highly correlated systems. These materials are characterised by the coexistence of different kinds of order, including charge, orbital, and magnetic moment. This thesis contains high-resolution X-ray scattering studies of charge ordering in such systems namely the high-T C copper oxides isostructural system, La 2-x Sr x NiO 4 with various Sr concentrations (x = 0.33 - 0.2), and the CMR manganite system, Nd 1/2 Sr 1/2 MnO 3 . It also includes a review of charge ordering in a large variety of transition metal oxides, such as ferrates, vanadates, cobaltates, nickelates, manganites, and cuprates systems, which have been reported to date in the scientific literature. Using high-resolution synchrotron X-ray scattering, it has been demonstrated that the charge stripes exist in a series of single crystals of La 2-x Sr x NiO 4 with Sr concentrations (x = 0.33 - 0.2) at low temperatures. Satellite reflections due to the charge ordering were found with the wavevector (2ε, 0, 1) below the charge ordering transition temperature, T CO , where 2ε is the amount of separation from the corresponding Bragg peak. The charge stripes are shown to be two-dimensional in nature both by measurements of their correlation lengths and by measurement of the critical exponents of the charge stripe melting transition with an anomaly at x = 0.25. The results show by decreasing the hole concentration from the x = 0.33 to 0.2, the well-correlated charge stripes change to a glassy state at x = 0.25. The electronic transition into the charge stripe phase is second-order without any corresponding structural transition. Above the second-order transition critical scattering was observed due to fluctuations into the charge stripe phase. In a single-crystal of Nd

  14. Quantification of RNA in bacteriophage MS2-like viruses in solution by small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Kuzmanovic, Deborah A.; Elashvili, Ilya; Wick, Charles; O'Connell, Catherine; Krueger, Susan

    2006-01-01

    Recombinant forms of bacteriophage MS2 virus particles, wild-type MS2 and MS2 capsids have been examined in solution using small-angle X-ray scattering (SAXS). SAXS was used to determine the overall size of the virus particles and to quantify the amount of encapsulated viral RNA. These studies show that analysis of natural and recombinant forms of MS2 virus by SAXS can be used as both a quantitative measure of nucleic acid content in situ and diagnostic indicator of sample integrity

  15. Study of the atomic ordering in the alloys Ni-Ir using diffuse X-ray scattering and pseudopotentials

    International Nuclear Information System (INIS)

    Abbas, T.

    1982-06-01

    Experiments were performed on the Ni-Ir alloys to measure the diffuse X-ray scattering intensity after annealing from high temperatures. It was established that the short-range order exists in these alloys when the samples are quenched from 1200 0 C and 1400 0 C. The ordering potentials for various concentrations of Ir in Ni were calculated using the pseudopotentials of Animalu. The method of incorporating the d electrons in the dielectric screening function was proposed. It was shown that the ordering potential is severely affected by the new type of screening. (author)

  16. RESONANT X-RAY SCATTERING AS A PROBE OF ORBITAL AND CHARGE ORDERING

    International Nuclear Information System (INIS)

    NELSON, C.S.; HILL, J.P.; GIBBS, D.

    2002-01-01

    Resonant x-ray scattering is a powerful experimental technique for probing orbital and charge ordering. It involves tuning the incident photon energy to an absorption edge of the relevant ion and observing scattering at previously 'forbidden' Bragg peaks, and it allows high-resolution, quantitative studies of orbital and charge order--even from small samples. Further, resonant x-ray scattering from orbitally ordered systems exhibits polarization- and azimuthal-dependent properties that provide additional information about the details of the orbital order that is difficult, or impossible, to obtain with any other technique. In the manganites, the sensitivity to charge and orbital ordering is enhanced when the incident photon energy is tuned near the Mn K absorption edge (6.539 keV), which is the lowest energy at which a 1s electron can be excited into an unoccupied state. In this process, the core electron is promoted to an intermediate excited state, which decays with the emission of a photon. The sensitivity to charge ordering is believed to be due to the small difference in K absorption edges of the Mn 3+ and Mn 4+ sites. For orbital ordering, the sensitivity arises from a splitting--or difference in the weight of the density of states [239]--of the orbitals occupied by the excited electron in the intermediate state. In the absence of such a splitting, there is no resonant enhancement of the scattering intensity. In principle, other absorption edges in which the intermediate state is anisotropic could be utilized, but the strong dipole transition to the Mn 4p levels--and their convenient energies for x-ray diffraction--make the K edge well-suited to studies of manganites. The Mn 4p levels are affected by the symmetry of the orbital ordering, which makes the technique sensitive to the orbital degree of freedom. Therefore resonant x-ray scattering can be used to obtain important quantitative information concerning the details of this electronic order. Two

  17. An upgrade beamline for combined wide, small and ultra small-angle x-ray scattering at the ESRF

    Energy Technology Data Exchange (ETDEWEB)

    Van Vaerenbergh, Pierre; Léonardon, Joachim; Sztucki, Michael; Boesecke, Peter; Gorini, Jacques; Claustre, Laurent; Sever, Franc; Morse, John; Narayanan, Theyencheri [ESRF - The European Synchrotron, F-38043 Grenoble (France)

    2016-07-27

    This contribution presents the main design features of the upgraded beamline ID02 (TRUSAXS). The beamline combines different small-angle X-ray scattering techniques in one unique instrument. The key component of this instrument is an evacuated (5×10{sup −3} mbar) stainless steel detector tube of length 34 m and diameter 2 m. Three different detectors (Rayonix MX170, Pilatus 300 K and FReLoN 4M) are housed inside a motorized wagon which travels along a rail system with very low parasitic lateral movements (± 0.3 mm). This system allows automatically changing the sample-to-detector distance from about 1 m to 31 m and selecting the desired detector. In addition, a wide angle detector (Rayonix LX170) is installed just above the entrance cone of the tube for optional wide-angle X-ray scattering measurements. The beamstop system enables monitoring of the X-ray beam intensity in addition to blocking the primary beam, and automated insertion of selected masks behind the primary beamstop. The focusing optics and collimation system permit to cover a scattering vector (q) range of 0.002 nm{sup −1} ≤ q ≤ 50 nm{sup −1} with one unique setting using 0.1 nm X-ray wavelength for moderate flux (5×10{sup 12} photons/sec). However, for higher flux (6x10{sup 13} photons/sec) or higher resolution (minimum q < 0.001 nm{sup −1}), focusing and collimation, respectively need to be varied. For a sample-to-detector distance of 31 m and 0.1 nm wavelength, two dimensional ultra small-angle X-ray scattering patterns can be recorded down to q≈0.001 nm{sup −1} with far superior quality as compared to one dimensional profiles obtained with a Bonse-Hart instrument.

  18. Quasi-particle interference of heavy fermions in resonant x-ray scattering.

    Science.gov (United States)

    Gyenis, András; da Silva Neto, Eduardo H; Sutarto, Ronny; Schierle, Enrico; He, Feizhou; Weschke, Eugen; Kavai, Mariam; Baumbach, Ryan E; Thompson, Joe D; Bauer, Eric D; Fisk, Zachary; Damascelli, Andrea; Yazdani, Ali; Aynajian, Pegor

    2016-10-01

    Resonant x-ray scattering (RXS) has recently become an increasingly important tool for the study of ordering phenomena in correlated electron systems. Yet, the interpretation of RXS experiments remains theoretically challenging because of the complexity of the RXS cross section. Central to this debate is the recent proposal that impurity-induced Friedel oscillations, akin to quasi-particle interference signals observed with a scanning tunneling microscope (STM), can lead to scattering peaks in RXS experiments. The possibility that quasi-particle properties can be probed in RXS measurements opens up a new avenue to study the bulk band structure of materials with the orbital and element selectivity provided by RXS. We test these ideas by combining RXS and STM measurements of the heavy fermion compound Ce M In 5 ( M = Co, Rh). Temperature- and doping-dependent RXS measurements at the Ce- M 4 edge show a broad scattering enhancement that correlates with the appearance of heavy f -electron bands in these compounds. The scattering enhancement is consistent with the measured quasi-particle interference signal in the STM measurements, indicating that the quasi-particle interference can be probed through the momentum distribution of RXS signals. Overall, our experiments demonstrate new opportunities for studies of correlated electronic systems using the RXS technique.

  19. Real time X-ray scattering study of the formation of ZnS nanoparticles using synchrotron radiation

    International Nuclear Information System (INIS)

    Rath, T.; Novák, J.; Amenitsch, H.; Pein, A.; Maier, E.; Haas, W.; Hofer, F.; Trimmel, G.

    2014-01-01

    We investigate the growth of ZnS nanoparticles by a real-time simultaneous small and wide angle X-ray scattering (SAXS, WAXS) study using synchrotron radiation. Zinc chloride and elemental sulfur were dissolved in oleylamine. The formation of nanoparticles was induced by heating to 170 °C and 215 °C. The influence of temperature, reaction time, and sulfur concentration was investigated. After a short phase of rapid growth, saturation in size and a slower growth is observed depending on the temperature. The final size of the nanoparticles ranges between 2 and 6 nm for the investigated growth conditions and increases with the reaction temperature and sulfur concentration. SAXS analysis allows for determination of the size of the nanoparticles and proves also the existence of an organized layer of oleylamine molecules covering the nanoparticles' surfaces, which, however, appears only for diameters of the nanoparticles larger than approximately 2.8 nm. The investigation of the measured structure factor of the nanoparticle assemblies showed that the distance of an attractive interaction is 2.5 nm, which was interpreted as a consequence of the ordered oleylamine surface layer. - Highlights: • ZnS nanoparticle growth is investigated by real-time simultaneous SAXS and WAXS measurements. • Nanoparticle growth can be divided into two growth phases. • Higher reaction temperature or higher surplus of sulfur leads to larger nanoparticles. • Post-growth ex situ XRD and TEM measurements confirm results of the in situ study. • Nanoparticles are surrounded by a 2.6 nm thick ordered shell of oleylamine

  20. Experimental elucidation: microscopic mechanism of resonant X-ray scattering in manganite films

    CERN Document Server

    Ohsumi, H; Kiyama, T

    2003-01-01

    Resonant X-ray scattering experiments have been performed on perovskite manganite La sub 0 sub . sub 5 Sr sub 0 sub . sub 5 MnO sub 3 thin films, which are grown on three distinct perovskite with a coherent epitaxial strain and have a forced ferro-type orbital ordering of Mn 3d orbitals. Using an interference technique, we have successfully observed the resonant X-ray scattering signal from the system having the ferro-type orbital ordering and also revealed the energy scheme of Mn 4p bands. For the forced ferro-type orbital ordering system, the present results evidence that the resonant X-ray scattering signal originates from the band structure effect due to the Jahn-Teller distortion of a MnO sub 6 octahedron, and not from the Coulomb interaction between 3d and 4p electrons. (author)

  1. A preliminary study of breast cancer diagnosis using laboratory based small angle x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Round, A R [Daresbury Laboratories, Warrington, WA4 4AD (United Kingdom); Wilkinson, S J [Daresbury Laboratories, Warrington, WA4 4AD (United Kingdom); Hall, C J [Daresbury Laboratories, Warrington, WA4 4AD (United Kingdom); Rogers, K D [Department of Materials and Medical Sciences, Cranfield University, Swindon, SN6 8LA (United Kingdom); Glatter, O [Department of Chemistry, University of Graz (Austria); Wess, T [School of Optometry and Vision Sciences, Cardiff University, Cardiff CF10 3NB, Wales (United Kingdom); Ellis, I O [Nottingham City Hospital, Nottingham (United Kingdom)

    2005-09-07

    Breast tissue collected from tumour samples and normal tissue from bi-lateral mastectomy procedures were examined using small angle x-ray scattering. Previous work has indicated that breast tissue disease diagnosis could be performed using small angle x-ray scattering (SAXS) from a synchrotron radiation source. The technique would be more useful to health services if it could be made to work using a conventional x-ray source. Consistent and reliable differences in x-ray scatter distributions were observed between samples from normal and tumour tissue samples using the laboratory based 'SAXSess' system. Albeit from a small number of samples, a sensitivity of 100% was obtained. This result encourages us to pursue the implementation of SAXS as a laboratory based diagnosis technique.

  2. A preliminary study of breast cancer diagnosis using laboratory based small angle x-ray scattering

    International Nuclear Information System (INIS)

    Round, A R; Wilkinson, S J; Hall, C J; Rogers, K D; Glatter, O; Wess, T; Ellis, I O

    2005-01-01

    Breast tissue collected from tumour samples and normal tissue from bi-lateral mastectomy procedures were examined using small angle x-ray scattering. Previous work has indicated that breast tissue disease diagnosis could be performed using small angle x-ray scattering (SAXS) from a synchrotron radiation source. The technique would be more useful to health services if it could be made to work using a conventional x-ray source. Consistent and reliable differences in x-ray scatter distributions were observed between samples from normal and tumour tissue samples using the laboratory based 'SAXSess' system. Albeit from a small number of samples, a sensitivity of 100% was obtained. This result encourages us to pursue the implementation of SAXS as a laboratory based diagnosis technique

  3. A preliminary study of breast cancer diagnosis using laboratory based small angle x-ray scattering

    Science.gov (United States)

    Round, A. R.; Wilkinson, S. J.; Hall, C. J.; Rogers, K. D.; Glatter, O.; Wess, T.; Ellis, I. O.

    2005-09-01

    Breast tissue collected from tumour samples and normal tissue from bi-lateral mastectomy procedures were examined using small angle x-ray scattering. Previous work has indicated that breast tissue disease diagnosis could be performed using small angle x-ray scattering (SAXS) from a synchrotron radiation source. The technique would be more useful to health services if it could be made to work using a conventional x-ray source. Consistent and reliable differences in x-ray scatter distributions were observed between samples from normal and tumour tissue samples using the laboratory based 'SAXSess' system. Albeit from a small number of samples, a sensitivity of 100% was obtained. This result encourages us to pursue the implementation of SAXS as a laboratory based diagnosis technique.

  4. Study on the influences of X Ray Scattering on radioscopic inspection

    Energy Technology Data Exchange (ETDEWEB)

    Wozniak, M.; Torrent, J.; Bancelin, A. [SNECMA NDE Dept. Laboratory, France, Evry Corbeil, 91 - Evry (France)

    2007-07-01

    This study issued from European project 'Verdict' (Virtual Evaluation and Robust Detection for engine Components non destructive Testing), aimed at developing and evaluating X Ray Non Destructive Method simulation. An qualitative appreciation and quantification for X Ray scattering for modelling (SINDBAD software) was identified. The effect of such radiation on radiogram results in a disturbing blur for interpretation of indications. The method and the results described are innovative in the analysis of X Ray scattering because for aeronautic field, the configurations used with this energy range are breakthrough. The approach followed consists in an experimental and practical method for evaluating scattered radiation on final image issued from the inspection. Experimental tests results confirmed that the influence of scattering radiation are linked to density variation, geometry of parts in the axis of direct radiation and spatial area. This study performed in industrial configurations contributed to improve X Ray scattering understanding. (authors)

  5. Alzheimer's disease imaging biomarkers using small-angle x-ray scattering

    Science.gov (United States)

    Choi, Mina; Alam, Nadia; Dahal, Eshan; Ghammraoui, Bahaa; Badano, Aldo

    2016-03-01

    There is a need for novel imaging techniques for the earlier detection of Alzheimer's disease (AD). Two hallmarks of AD are amyloid beta (Aβ) plaques and tau tangles that are formed in the brain. Well-characterized x-ray cross sections of Aβ and tau proteins in a variety of structural states could potentially be used as AD biomarkers for small-angle x-ray scattering (SAXS) imaging without the need for injectable probes or contrast agents. First, however, the protein structures must be controlled and measured to determine accurate biomarkers for SAXS imaging. Here we report SAXS measurements of Aβ42 and tau352 in a 50% dimethyl sulfoxide (DMSO) solution in which these proteins are believed to remain monomeric because of the stabilizing interaction of DMSO solution. Our SAXS analysis showed the aggregation of both proteins. In particular, we found that the aggregation of Aβ42 slowly progresses with time in comparison to tau352 that aggregates at a faster rate and reaches a steady-state. Furthermore, the measured signals were compared to the theoretical SAXS profiles of Aβ42 monomer, Aβ42 fibril, and tau352 that were computed from their respective protein data bank structures. We have begun the work to systematically control the structural states of these proteins in vitro using various solvent conditions. Our future work is to utilize the distinct SAXS profiles of various structural states of Aβ and tau to build a library of signals of interest for SAXS imaging in brain tissue.

  6. Small-angle X-ray scattering (SAXS) for metrological size determination of nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Gleber, Gudrun; Krumrey, Michael; Cibik, Levent; Marggraf, Stefanie; Mueller, Peter [Physikalisch-Technische Bundesanstalt, Abbestr. 2-12, 10587 Berlin (Germany); Hoell, Armin [Helmholtz-Zentrum Berlin, Albert-Einstein-Str. 15, 12489 Berlin (Germany)

    2011-07-01

    To measure the size of nanoparticles, different measurement methods are available but their results are often not compatible. In the framework of an European metrology project we use Small-Angle X-ray Scattering (SAXS) to determine the size and size distribution of nanoparticles in aqueous solution, where the special challange is the traceability of the results. The experiments were performed at the Four-Crystal Monochromator (FCM) beamline in the laboratory of Physikalisch-Technische Bundesanstalt (PTB) at BESSY II using the SAXS setup of the Helmholtz-Zentrum Berlin (HZB). We measured different particles made of PMMA and gold in a diameter range of 200 nm down to about 10 nm. The aspects of traceability can be classified in two parts: the first is the experimental part with the uncertainties of distances, angles, and wavelength, the second is the part of analysis, with the uncertainty of the choice of the model used for fitting the data. In this talk we want to show the degree of uncertainty, which we reached in this work yet.

  7. Collective chain dynamics in lipid bilayers by inelastic x-ray scattering

    International Nuclear Information System (INIS)

    Weiss, T.M.; Chen, P.-J.; Sinn, H.; Alp, E.E.; Chen, S.-H.; Hwang, H.W.

    2003-01-01

    We investigated the application of inelastic x-ray scattering (IXS) to lipid bilayers. This technique directly measures the dynamic structure factor S(q,ω) which is the space-time Fourier transform of the electron density correlation function of the measured system. For a multiatomic system, the analysis of S(q,ω) is usually complicated. But for multiple bilayers of lipid, S(q,ω) is dominated by chain-chain correlations within individual bilayers. Thus IXS provides a unique probe for the collective dynamics of lipid chains in a bilayer that cannot be obtained by any other method. IXS of dimyristoyl phosphatidylcholine and dimyristoyl phosphatidylcholine + cholesterol at two different concentrations were measured. S(q,ω) was analyzed by three-mode hydrodynamic equations, including a thermal diffusive mode and two propagating acoustic modes. We obtained the dispersion curves for the phonons that represent the collective in-plane excitations of lipid chains. The effect of cholesterol on chain dynamics was detected. Our analysis shows the importance of having a high instrument resolution as well as the requirement of sufficient signal-to-noise ratio to obtain meaningful results from such an IXS experiment. The requirement on signal-to-noise also applies to molecular dynamics simulations.

  8. Topological investigation of electronic silicon nanoparticulate aggregates using ultra-small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Jonah, E. O.; Britton, D. T.; Beaucage, P.; Rai, D. K.; Beaucage, G.; Magunje, B.; Ilavsky, J.; Scriba, M. R.; Härting, M.

    2012-01-01

    The network topology of two types of silicon nanoparticles, produced by high energy milling and pyrolysis of silane, in layers deposited from inks on permeable and impermeable substrates has been quantitatively characterized using ultra-small-angle X-ray scattering, supported by scanning electron microscopy observations. The milled particles with a highly polydisperse size distribution form agglomerates, which in turn cluster to form larger aggregates with a very high degree of aggregation. Smaller nanoparticles with less polydisperse size distribution synthesized by thermal catalytic pyrolysis of silane form small open clusters. The Sauter mean diameters of the primary particles of the two types of nanoparticles were obtained from USAXS particle volume to surface ratio, with values of ∼41 and ∼21 nm obtained for the high energy milled and pyrolysis samples, respectively. Assuming a log-normal distribution of the particles, the geometric standard deviation of the particles was calculated to be ∼1.48 for all the samples, using parameters derived from the unified fit to the USAXS data. The flow properties of the inks and substrate combination lead to quantitative changes in the mean particle separation, with slowly curing systems with good capillary flow resulting in denser networks with smaller aggregates and better contact between particles.

  9. Small-angle x-ray scattering in amorphous silicon: A computational study

    Science.gov (United States)

    Paudel, Durga; Atta-Fynn, Raymond; Drabold, David A.; Elliott, Stephen R.; Biswas, Parthapratim

    2018-05-01

    We present a computational study of small-angle x-ray scattering (SAXS) in amorphous silicon (a -Si) with particular emphasis on the morphology and microstructure of voids. The relationship between the scattering intensity in SAXS and the three-dimensional structure of nanoscale inhomogeneities or voids is addressed by generating large high-quality a -Si networks with 0.1%-0.3% volume concentration of voids, as observed in experiments using SAXS and positron annihilation spectroscopy. A systematic study of the variation of the scattering intensity in the small-angle scattering region with the size, shape, number density, and the spatial distribution of the voids in the networks is presented. Our results suggest that the scattering intensity in the small-angle region is particularly sensitive to the size and the total volume fraction of the voids, but the effect of the geometry or shape of the voids is less pronounced in the intensity profiles. A comparison of the average size of the voids obtained from the simulated values of the intensity, using the Guinier approximation and Kratky plots, with that of the same from the spatial distribution of the atoms in the vicinity of void surfaces is presented.

  10. High energy resolution inelastic x-ray scattering at the SRI-CAT

    International Nuclear Information System (INIS)

    Macrander, A.T.

    1996-08-01

    This report is a combination of vugraphs and two papers. The vugraphs give information on the beamline at the APS for IXS and the science addressable by IXS. They also cover the 10 milli-eV resolution spectrometer and the 200 milli-eV resolution spectrometer. The first paper covers the performance of the focusing Ge(444) backscattering analyzers for the inelastic x-ray scattering. The second paper discusses inelastic x-ray scattering from TiC and Ti single crystals

  11. High energy x-ray scattering studies of strongly correlated oxides

    International Nuclear Information System (INIS)

    Hatton, Peter D; Wilkins, S B; Spencer, P D; Zimmermann, M v; D'Almeida, T

    2003-01-01

    Many transition metal oxides display strongly correlated charge, spin, or orbital ordering resulting in varied phenomena such as colossal magnetoresistance, high temperature superconductivity, metal-insulator transitions etc. X-ray scattering is one of the principle techniques for probing the structural response to such effects. In this paper, we discuss and review the use of synchrotron radiation high energy x-rays (50-200 keV) for the study of transition metal oxides such as nickelates (La 2-x Sr x NiO 4 ) and manganites (La 2-2x Sr 1+2x Mn 2 O 7 ). High energy x-rays have sufficient penetration to allow us to study large flux-grown single crystals. The huge increase in sample scattering volume means that extremely weak peaks can be observed. This allows us to study very weak charge ordering. Measurements of the intensity, width and position of the charge ordering satellites as a function of temperature provide us with quantitative measures of the charge amplitude, inverse correlation length and wavevector of the charge ordering

  12. Automated acquisition and analysis of small angle X-ray scattering data

    International Nuclear Information System (INIS)

    Franke, Daniel; Kikhney, Alexey G.; Svergun, Dmitri I.

    2012-01-01

    Small Angle X-ray Scattering (SAXS) is a powerful tool in the study of biological macromolecules providing information about the shape, conformation, assembly and folding states in solution. Recent advances in robotic fluid handling make it possible to perform automated high throughput experiments including fast screening of solution conditions, measurement of structural responses to ligand binding, changes in temperature or chemical modifications. Here, an approach to full automation of SAXS data acquisition and data analysis is presented, which advances automated experiments to the level of a routine tool suitable for large scale structural studies. The approach links automated sample loading, primary data reduction and further processing, facilitating queuing of multiple samples for subsequent measurement and analysis and providing means of remote experiment control. The system was implemented and comprehensively tested in user operation at the BioSAXS beamlines X33 and P12 of EMBL at the DORIS and PETRA storage rings of DESY, Hamburg, respectively, but is also easily applicable to other SAXS stations due to its modular design.

  13. Molecular Packing of Amphiphilic Nanosheets Resolved by X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Harutyunyan, Boris; Dannenhoffer, Adam; Kewalramani, Sumit; Aytun, Taner; Fairfield, Daniel J.; Stupp, Samuel I.; Bedzyk, Michael J. (NWU)

    2016-12-29

    Molecular packing in light harvesting 2D assemblies of photocatalytic materials is a critical factor for solar-to-fuel conversion efficiency. However, structure–function correlations have yet to be fully established. This is partly due to the difficulties in extracting the molecular arrangements from the complex 3D powder averaged diffraction patterns of 2D lattices, obtained via in situ wide-angle X-ray scattering. Here, we develop a scattering theory formalism and couple it with a simple geometrical model for the molecular shape of chromophore 9-methoxy-N-(sodium hexanoate)perylene-3,4-dicarboximide (MeO-PMI) used in our study. This generally applicable method fully reproduces the measured diffraction pattern including the asymmetric line shapes for the Bragg reflections and yields the molecular packing arrangement within a 2D crystal structure with a remarkable degree of detail. We find an approximate edge-centered herringbone structure for the PMI fused aromatic rings and ordering of the carboxypentyl chains above and below the nanosheets. Such a packing arrangement differs from the more symmetric face-to-face orientation of the unsubstituted PMI rings. This structural difference is correlated to our measurement of the reduced catalytic performance of MeO-PMI nanosheets as compared to the mesoscopically similar unsubstituted PMI assemblies.

  14. Traceable size determination of PMMA nanoparticles based on Small Angle X-ray Scattering (SAXS)

    Energy Technology Data Exchange (ETDEWEB)

    Gleber, G; Cibik, L; Mueller, P; Krumrey, M [Physikalisch-Technische Bundesanstalt (PTB), Abbestrasse 2-12, 10587 Berlin (Germany); Haas, S; Hoell, A, E-mail: gudrun.gleber@ptb.d [Helmholtz-Zentrum-Berlin fuer Materialien und Energie (HZB), Albert-Einstein-Strasse 15, 12489 Berlin (Germany)

    2010-10-01

    The size and size distribution of PMMA nanoparticles has been investigated with SAXS (small angle X-ray scattering) using monochromatized synchrotron radiation. The uncertainty has contributions from the wavelength or photon energy of the radiation, the scattering angle and the fit procedure for the obtained scattering curves. The wavelength can be traced back to the lattice constant of silicon, and the scattering angle is traceable via geometric measurements of the detector pixel size and the distance between the sample and the detector. SAXS measurements and data evaluations have been performed at different distances and photon energies for two PMMA nanoparticle suspensions with low polydispersity and nominal diameters of 108 nm and 192 nm, respectively, as well as for a mixture of both. The relative variation of the diameters obtained for different experimental conditions was below {+-} 0.3 %. The determined number-weighted mean diameters of (109.0 {+-} 0.7) nm and (188.0 {+-} 1.3) nm, respectively, are close to the nominal values.

  15. Traceable size determination of PMMA nanoparticles based on Small Angle X-ray Scattering (SAXS)

    Science.gov (United States)

    Gleber, G.; Cibik, L.; Haas, S.; Hoell, A.; Müller, P.; Krumrey, M.

    2010-10-01

    The size and size distribution of PMMA nanoparticles has been investigated with SAXS (small angle X-ray scattering) using monochromatized synchrotron radiation. The uncertainty has contributions from the wavelength or photon energy of the radiation, the scattering angle and the fit procedure for the obtained scattering curves. The wavelength can be traced back to the lattice constant of silicon, and the scattering angle is traceable via geometric measurements of the detector pixel size and the distance between the sample and the detector. SAXS measurements and data evaluations have been performed at different distances and photon energies for two PMMA nanoparticle suspensions with low polydispersity and nominal diameters of 108 nm and 192 nm, respectively, as well as for a mixture of both. The relative variation of the diameters obtained for different experimental conditions was below ± 0.3 %. The determined number-weighted mean diameters of (109.0 ± 0.7) nm and (188.0 ± 1.3) nm, respectively, are close to the nominal values.

  16. Traceable size determination of PMMA nanoparticles based on Small Angle X-ray Scattering (SAXS)

    International Nuclear Information System (INIS)

    Gleber, G; Cibik, L; Mueller, P; Krumrey, M; Haas, S; Hoell, A

    2010-01-01

    The size and size distribution of PMMA nanoparticles has been investigated with SAXS (small angle X-ray scattering) using monochromatized synchrotron radiation. The uncertainty has contributions from the wavelength or photon energy of the radiation, the scattering angle and the fit procedure for the obtained scattering curves. The wavelength can be traced back to the lattice constant of silicon, and the scattering angle is traceable via geometric measurements of the detector pixel size and the distance between the sample and the detector. SAXS measurements and data evaluations have been performed at different distances and photon energies for two PMMA nanoparticle suspensions with low polydispersity and nominal diameters of 108 nm and 192 nm, respectively, as well as for a mixture of both. The relative variation of the diameters obtained for different experimental conditions was below ± 0.3 %. The determined number-weighted mean diameters of (109.0 ± 0.7) nm and (188.0 ± 1.3) nm, respectively, are close to the nominal values.

  17. An x ray scatter approach for non-destructive chemical analysis of low atomic numbered elements

    Science.gov (United States)

    Ross, H. Richard

    1993-01-01

    A non-destructive x-ray scatter (XRS) approach has been developed, along with a rapid atomic scatter algorithm for the detection and analysis of low atomic-numbered elements in solids, powders, and liquids. The present method of energy dispersive x-ray fluorescence spectroscopy (EDXRF) makes the analysis of light elements (i.e., less than sodium; less than 11) extremely difficult. Detection and measurement become progressively worse as atomic numbers become smaller, due to a competing process called 'Auger Emission', which reduces fluorescent intensity, coupled with the high mass absorption coefficients exhibited by low energy x-rays, the detection and determination of low atomic-numbered elements by x-ray spectrometry is limited. However, an indirect approach based on the intensity ratio of Compton and Rayleigh scattered has been used to define light element components in alloys, plastics and other materials. This XRS technique provides qualitative and quantitative information about the overall constituents of a variety of samples.

  18. Characterizing morphology in organic systems with resonant soft X-ray scattering

    International Nuclear Information System (INIS)

    Carpenter, Joshua H.; Hunt, Adrian; Ade, Harald

    2015-01-01

    Highlights: • A brief history of the development of R-SoXS for studying soft matter systems. • A theoretical background and an overview of analysis methodology. • Applications to block copolymers, organic electronics, and biological systems. • A discussion of emerging applications and an outlook on the future of R-SoXS. - Abstract: Resonant soft X-ray scattering (R-SoXS) has proven to be a highly useful technique for studying the morphology of soft matter thin films due to the large intrinsic contrast between organic materials and the anisotropic nature of the resonant electronic state transitions from which the contrast originates. This allows R-SoXS users to measure spatial composition correlations from crystalline and amorphous phases in heterogeneous organic samples, infer relative domain purity, and determine average local molecular ordering correlations. R-SoXS has been used to study the morphology of organic photovoltaics, organic thin film transistors, biological systems, and block copolymer engineering applications. The mesoscopic morphological information compliments molecular packing information determined with hard X-rays, so that complex structure–property relationships can be elucidated over a large range of length scales. Extensions of R-SoXS have also emerged that make use of more advanced sample setups or different experimental geometries than normal transmission, such as θ–2θ reflectivity or grazing incidence.

  19. Structural and dynamical properties of chlorinated hydrocarbons studied with resonant inelastic x-ray scattering

    Science.gov (United States)

    Bohinc, R.; Žitnik, M.; Bučar, K.; Kavčič, M.; Carniato, S.; Journel, L.; Guillemin, R.; Marchenko, T.; Kawerk, E.; Simon, M.; Cao, W.

    2016-04-01

    We present a theoretical and experimental study of resonant inelastic x-ray scattering on a large group of chlorinated hydrocarbons: CH3Cl, CH2Cl2, CHCl3, CCl4, CH3CH2Cl, ClCH2CH2Cl, CH3CHCl2, CH3CCl3, C2H2Cl2-iso, C2H2Cl2-cis, C2H2Cl2-trans, and C6H5Cl. Differences in structural and dynamical properties of the molecules generated by diverse chemical environments are observed in the measured Cl(Kα) spectral maps as well as in the Cl(K) total fluorescence yield spectra. The energy position, relative intensity, and the width of the Franck-Condon distribution of low-lying σ∗ and π∗ resonances are extracted by a fitting procedure taking into account the experimental broadening. The theoretical values obtained with the transition potential and Δ Kohn-Sham methods are in good agreement with the experimental parameters indicating subtle differences due to variations in the molecular structure.

  20. Understanding nucleic acid structural changes by comparing wide-angle x-ray scattering (WAXS) experiments to molecular dynamics simulations

    Energy Technology Data Exchange (ETDEWEB)

    Pabit, Suzette A.; Katz, Andrea M.; Pollack, Lois [School of Applied and Engineering Physics, Cornell University, Ithaca, New York 14853 (United States); Tolokh, Igor S. [Department of Computer Science, Virginia Tech, Blacksburg, Virginia 24061 (United States); Drozdetski, Aleksander [Department of Physics, Virginia Tech, Blacksburg, Virginia 24061 (United States); Baker, Nathan [Pacific Northwest National Laboratory, Richland, Washington 99352 (United States); Onufriev, Alexey V. [Department of Computer Science, Virginia Tech, Blacksburg, Virginia 24061 (United States); Department of Physics, Virginia Tech, Blacksburg, Virginia 24061 (United States)

    2016-05-28

    Wide-angle x-ray scattering (WAXS) is emerging as a powerful tool for increasing the resolution of solution structure measurements of biomolecules. Compared to its better known complement, small angle x-ray scattering (SAXS), WAXS targets higher scattering angles and can enhance structural studies of molecules by accessing finer details of solution structures. Although the extension from SAXS to WAXS is easy to implement experimentally, the computational tools required to fully harness the power of WAXS are still under development. Currently, WAXS is employed to study structural changes and ligand binding in proteins; however, the methods are not as fully developed for nucleic acids. Here, we show how WAXS can qualitatively characterize nucleic acid structures as well as the small but significant structural changes driven by the addition of multivalent ions. We show the potential of WAXS to test all-atom molecular dynamics (MD) simulations and to provide insight into understanding how the trivalent ion cobalt(III) hexammine (CoHex) affects the structure of RNA and DNA helices. We find that MD simulations capture the RNA structural change that occurs due to addition of CoHex.

  1. Analysis of Order Formation in Block Copolymer Thin Films UsingResonant Soft X-Ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Virgili, Justin M.; Tao, Yuefei; Kortright, Jeffrey B.; Balsara,Nitash P.; Segalman, Rachel A.

    2006-11-27

    The lateral order of poly(styrene-block-isoprene) copolymer(PS-b-PI) thin films is characterized by the emerging technique ofresonant soft X-ray scattering (RSOXS) at the carbon K edge and comparedto ordering in bulk samples of the same materials measured usingconventional small-angle X-ray scattering. We show resonance using theoryand experiment that the loss of scattering intensity expected with adecrease in sample volume in the case of thin films can be overcome bytuning X-rays to the pi* resonance of PS or PI. Using RSOXS, we study themicrophase ordering of cylinder- and phere-forming PS-b-PI thin films andcompare these results to position space data obtained by atomic forcemicroscopy. Our ability to examine large sample areas (~;9000 mu m2) byRSOXS enables unambiguous identification of the lateral lattice structurein the thin films. In the case of the sphere-forming copolymer thin film,where the spheres are hexagonally arranged, the average sphere-to-spherespacing is between the bulk (body-centered cubic) nearest neighbor andbulk unit cell spacings. In the case of the cylinder-forming copolymerthin film, the cylinder-to-cylinder spacing is within experimental errorof that obtained in the bulk.

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  3. Grazing Incidence X-ray Scattering and Diffraction

    Indian Academy of Sciences (India)

    IAS Admin

    several materials as a function of angle of incidence, αi with X-rays of wavelength ..... are several advantages of using this formulation for the description of surface ..... print of the surface (as shown at the botton of Figure. 5). A Soller collimator ...

  4. Resonant soft x-ray scattering and charge density waves in correlated systems

    NARCIS (Netherlands)

    Rusydi, Andrivo

    2006-01-01

    Summary This work describes results obtained on the study of charge density waves (CDW) in strongly correlated systems with a new experimental method: resonant soft x-ray scattering (RSXS). The basic motivation is the 1986 discovery by Bednorz and Müler of a new type of superconductor, based on Cu

  5. Investigation of nanoscale structures by small-angle X-ray scattering in a radiochromic dosimeter

    DEFF Research Database (Denmark)

    Skyt, Peter Sandegaard; Jensen, Grethe Vestergaard; Wahlstedt, Isak Hannes

    2014-01-01

    This study examines the nanoscale structures in a radiochromic dosimeter that was based on leuco-malachite-green dye and the surfactant sodium dodecyl sulfate (SDS) suspended in a gelatin matrix. Small-angle X-ray scattering was used to investigate the structures of a range of compositions...

  6. Small angle neutron scattering and small angle X-ray scattering ...

    Indian Academy of Sciences (India)

    Abstract. The morphology of carbon nanofoam samples comprising platinum nanopar- ticles dispersed in the matrix was characterized by small angle neutron scattering (SANS) and small angle X-ray scattering (SAXS) techniques. Results show that the structure of pores of carbon matrix exhibits a mass (pore) fractal nature ...

  7. Anomalous X-ray scattering studies of short-, intermediate- and extended-range order in glasses

    International Nuclear Information System (INIS)

    Price, D.L.; Saboungi, M.L.; Armand, P.; Cox, D.E.

    1998-01-01

    The authors present the formalism of anomalous x-ray scattering as applied to partial structure analysis of disordered materials, and give an example of how the technique has been applied, together with that of neutron diffraction, to investigate short-, intermediate- and extended-range order in vitreous germania and rubidium germanate

  8. On the calculation of x-ray scattering signals from pairwise radial distribution functions

    DEFF Research Database (Denmark)

    Dohn, Asmus Ougaard; Biasin, Elisa; Haldrup, Kristoffer

    2015-01-01

    We derive a formulation for evaluating (time-resolved) x-ray scattering signals of solvated chemical systems, based on pairwise radial distribution functions, with the aim of this formulation to accompany molecular dynamics simulations. The derivation is described in detail to eliminate any possi...

  9. RESONANT MAGNETIC-X-RAY SCATTERING FROM MIXED-VALENCE TMSE

    NARCIS (Netherlands)

    MCWHAN, DB; ISAACS, ED; CARRA, P; SHAPIRO, SM; THOLE, BT; HOSHINO, S

    1993-01-01

    The mixed-valent compound TmSe has been studied in its antiferromagnetic state (T x-ray scattering. The (003) magnetic reflection shows two peaks as a function of incident energy corresponding to the L(III) absorption edges of its Tm2+ and Tm2+ configurations. This

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

    International Nuclear Information System (INIS)

    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

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

    DEFF Research Database (Denmark)

    Brandt van Driel, Tim

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

  12. X-ray scatter data for diagnostic radiology

    International Nuclear Information System (INIS)

    Dick, C.E.; Soares, C.G.; Motz, J.W.

    1978-01-01

    The ratio of the scattered to the total X-ray fluence (scatter fraction) at the centre of the image plane for X-rays transmitted through polystyrene phantoms has been measured for X-ray energies of 32 and 69 keV, X-ray beam diameters from 4 to 40 cm, phantom thicknesses from 5 to 30 cm and phantom-to-image-plane separations from 0.3 to 40 cm. The experimental values for this ratio have less than a 10% variation for these two X-ray energies and the experimental data show good agreement with Monte Carlo calculations and available experimental results for low atomic number materials. Based on these results, simple curves are generated which give estimates (+ - 10%) of the scatter fraction for all combinations of the geometric parameters encountered in diagnostic radiology. (author)

  13. Study of human blood and hemocomponents irradiated by low angle x ray scattering (LAXS)

    Energy Technology Data Exchange (ETDEWEB)

    Pinto, Nivia G. Villela; Barroso, Regina C. [Universidade do Estado do Rio de Janeiro (UERJ), RJ (Brazil). Inst. de Fisica. Dept. de Fisica Aplicada e Termodinamica], e-mail: nitatag@gmail.com; Mota, Carla L.S.; Almeida, Andre P.; Azeredo, Soraia R.; Braz, Delson [Coordenacao dos Programas de Pos-graduacao em Engenharia (COPPE/UFRJ), RJ (Brazil). Lab. de Instrumentacao Nuclear], e-mail: delson@lin.ufrj.br

    2009-07-01

    Irradiation of blood and blood components is currently practiced in developed and in a few developing countries. The main purpose of this process is the prevention of graft versus host disease in immunodeficient patients. The Food and Drug Administration recommends a dose range of 15 Gy to 25 Gy for these blood components. When x-ray photons are scattered from biological samples, their angular distribution shows one or more peaks in the forward direction of scattering. These peaks are characteristic for the investigated samples. Due to its wide range of biological and medical applications, low-angle x-ray scattering has attracted the attention of many authors. Thus in this present work was studied the possible variations in scattering profiles due to the irradiation when the gender of patients was considered. Fresh blood specimens were obtained from volunteers using vacutainer tubes containing EDTA, at the Dr. Eliel Figueiredo Laboratory, Rio de Janeiro. All the samples were lyophilized for 48 hours in a freeze drier in order to remove the water. The scattering measurements were carried out in e-2e reflection geometry using a powder diffractometer Shimadzu XRD- 6000. The measured characterization parameters for LAXS were associated with epidemiological data (gender). The mean values of the different parameters were compared using the Students's t-test for each characterization parameters. The scattering profiles from plasma and formed elements are characterized by the presence of two peaks in the forward direction of scattering. For epidemiological data (gender) analyzed was not found significant changes in the mostly of characterization parameters (p>0.05). (author)

  14. Study of human blood and hemocomponents irradiated by low angle x ray scattering (LAXS)

    International Nuclear Information System (INIS)

    Pinto, Nivia G. Villela; Barroso, Regina C.; Mota, Carla L.S.; Almeida, Andre P.; Azeredo, Soraia R.; Braz, Delson

    2009-01-01

    Irradiation of blood and blood components is currently practiced in developed and in a few developing countries. The main purpose of this process is the prevention of graft versus host disease in immunodeficient patients. The Food and Drug Administration recommends a dose range of 15 Gy to 25 Gy for these blood components. When x-ray photons are scattered from biological samples, their angular distribution shows one or more peaks in the forward direction of scattering. These peaks are characteristic for the investigated samples. Due to its wide range of biological and medical applications, low-angle x-ray scattering has attracted the attention of many authors. Thus in this present work was studied the possible variations in scattering profiles due to the irradiation when the gender of patients was considered. Fresh blood specimens were obtained from volunteers using vacutainer tubes containing EDTA, at the Dr. Eliel Figueiredo Laboratory, Rio de Janeiro. All the samples were lyophilized for 48 hours in a freeze drier in order to remove the water. The scattering measurements were carried out in e-2e reflection geometry using a powder diffractometer Shimadzu XRD- 6000. The measured characterization parameters for LAXS were associated with epidemiological data (gender). The mean values of the different parameters were compared using the Students's t-test for each characterization parameters. The scattering profiles from plasma and formed elements are characterized by the presence of two peaks in the forward direction of scattering. For epidemiological data (gender) analyzed was not found significant changes in the mostly of characterization parameters (p>0.05). (author)

  15. X-ray scatter signatures for enhanced breast imaging

    Energy Technology Data Exchange (ETDEWEB)

    Kidane, Ghirmay; Speller, Robert; Royle, Gary [Medical Physics and Bioengineering Department, University College Landon, 11-20 Capper Street, London WC1E 6JA (United Kingdom)

    1999-12-31

    Conventional mammographic imaging suffers from a low specificity. The main cause is the small difference in the x-ray attenuation properties of healthy and diseased tissue leading to poor contrast in the image. It has been observed that additional information on breast tissue type can be obtained from x-ray diffraction effects. A study of excised normal and neoplastic breast tissue samples using x-ray diffraction apparatus has been observed that significant differences exist in the measured spectra between carcinoma and healthy tissue adjacent to the carcinoma. Such a difference allows tissue type to be characterised according to is diseased state. Furthermore the information can be applied to improve diagnosis. It is proposed that collection and analysis of the scattered x-rays present during a mammographic procedure can supply the additional information and be used to improve the image contrast. The ultimate aim of the project is to improve the specificity of x-ray mammography. (authors) 10 refs., 3 figs.

  16. Structural characterization of the human cerebral myelin sheath by small angle x-ray scattering

    International Nuclear Information System (INIS)

    De Felici, M; Felici, R; Ferrero, C; Tartari, A; Gambaccini, M; Finet, S

    2008-01-01

    Myelin is a multi-lamellar membrane surrounding neuronal axons and increasing their conduction velocity. When investigated by small-angle x-ray scattering (SAXS), the lamellar quasi-periodical arrangement of the myelin sheath gives rise to distinct peaks, which allow the determination of its molecular organization and the dimensions of its substructures. In this study we report on the myelin sheath structural determination carried out on a set of human brain tissue samples coming from surgical biopsies of two patients: a man around 60 and a woman nearly 90 years old. The samples were extracted either from white or grey cerebral matter and did not undergo any manipulation or chemical-physical treatment, which could possibly have altered their structure, except dipping them into a formalin solution for their conservation. Analysis of the scattered intensity from white matter of intact human cerebral tissue allowed the evaluation not only of the myelin sheath periodicity but also of its electronic charge density profile. In particular, the thicknesses of the cytoplasm and extracellular regions were established, as well as those of the hydrophilic polar heads and hydrophobic tails of the lipid bilayer. SAXS patterns were measured at several locations on each sample in order to establish the statistical variations of the structural parameters within a single sample and among different samples. This work demonstrates that a detailed structural analysis of the myelin sheath can also be carried out in randomly oriented samples of intact human white matter, which is of importance for studying the aetiology and evolution of the central nervous system pathologies inducing myelin degeneration.

  17. Beyond simple small-angle X-ray scattering: developments in online complementary techniques and sample environments

    Directory of Open Access Journals (Sweden)

    Wim Bras

    2014-11-01

    Full Text Available Small- and wide-angle X-ray scattering (SAXS, WAXS are standard tools in materials research. The simultaneous measurement of SAXS and WAXS data in time-resolved studies has gained popularity due to the complementary information obtained. Furthermore, the combination of these data with non X-ray based techniques, via either simultaneous or independent measurements, has advanced understanding of the driving forces that lead to the structures and morphologies of materials, which in turn give rise to their properties. The simultaneous measurement of different data regimes and types, using either X-rays or neutrons, and the desire to control parameters that initiate and control structural changes have led to greater demands on sample environments. Examples of developments in technique combinations and sample environment design are discussed, together with a brief speculation about promising future developments.

  18. Beyond simple small-angle X-ray scattering: developments in online complementary techniques and sample environments.

    Science.gov (United States)

    Bras, Wim; Koizumi, Satoshi; Terrill, Nicholas J

    2014-11-01

    Small- and wide-angle X-ray scattering (SAXS, WAXS) are standard tools in materials research. The simultaneous measurement of SAXS and WAXS data in time-resolved studies has gained popularity due to the complementary information obtained. Furthermore, the combination of these data with non X-ray based techniques, via either simultaneous or independent measurements, has advanced understanding of the driving forces that lead to the structures and morphologies of materials, which in turn give rise to their properties. The simultaneous measurement of different data regimes and types, using either X-rays or neutrons, and the desire to control parameters that initiate and control structural changes have led to greater demands on sample environments. Examples of developments in technique combinations and sample environment design are discussed, together with a brief speculation about promising future developments.

  19. Study on the structure of Fe sub 2 O sub 3 xerogels by small angle X-ray scattering

    CERN Document Server

    Liu Yi; Zhao Xin; Yang Tong Hua; Zhao Hui; Rong Li Xia; Zhang Jing; Wang Jun; Dong Bao Zhong

    2002-01-01

    Small angle X-ray scattering (SAXS) with synchrotron radiation as X-ray source is used to study the pore structure of Fe sub 2 O sub 3 xerogels prepared by sol-gel procedure and then heat-treated at different temperatures. By analysing the distribution of diameters of the pores, specific surfaces and fractal behaviors in samples, the characters and mechanisms of pores growing are discussed. The results show that the pores in Fe sub 2 O sub 3 xerogels are polydisperse and the structure of the pores is mass fractal. With increase in heat-treatment temperature, the average size of diameters of the pores and the dimension of fractal of Fe sub 2 O sub 3 xerogels are increased, whereas the scale range possessing fractal behavior become narrow

  20. Small-angle x-ray scattering from the early growth stages of zeolite A

    International Nuclear Information System (INIS)

    Singh, P.; White, J.

    1999-01-01

    Full text: The work presented here with the use of SAXS (Small-Angle X-ray Scattering) is in attempt to identify a different paradigm to the organic template induced crystallization of zeolites, in particular zeolite 'A'. The reactions have been followed by small angle X-ray scattering from the time of first mixing of the constituents until the final separation of zeolite A crystals. The processes happening during the growth are expected to follow successive transformation of intermediate metastable phases until the formation of thermodynamically most stable phase and scattering signatures from these developments may be useful for extracting interesting information about the processes in situ. The scattering functions from a synthesis system of zeolite 'A' at the initial and final stage of reaction are presented.The different growth processes of zeolite 'A' from different silicate and aluminium sources are found. The differences are attributed to different rate limiting steps in the syntheses

  1. Nonspherical atomic ground-state densities and chemical deformation densities from x-ray scattering

    International Nuclear Information System (INIS)

    Ruedenberg, K.; Schwarz, W.H.E.

    1990-01-01

    Presuming that chemical insight can be gained from the difference between the molecular electron density and the superposition of the ground-state densities of the atoms in a molecule, it is pointed out that, for atoms with degenerate ground states, an unpromoted ''atom in a molecule'' is represented by a specific ensemble of the degenerate atomic ground-state wave functions and that this ensemble is determined by the anisotropic local surroundings. The resulting atomic density contributions are termed oriented ground state densities, and the corresponding density difference is called the chemical deformation density. The constraints implied by this conceptual approach for the atomic density contributions are formulated and a method is developed for determining them from x-ray scattering data. The electron density of the appropriate promolecule and its x-ray scattering are derived, the determination of the parameters of the promolecule is outlined, and the chemical deformation density is formulated

  2. Precise tests of x-ray scattering theories in the Compton regime

    International Nuclear Information System (INIS)

    Dunford, R. W.; Gemmell, D. S.; Kanter, E. P.; Kraessig, B.; Southworth, S. H.; Young, L.

    1999-01-01

    The authors report two experiments intended to test the accuracy of state-of-the-art theoretical predictions for x-ray scattering from low-Z atoms. The first one deals with the differential x-ray scattering cross sections in Ne and He from 11-22 keV and the Ne Compton-to-Rayleigh scattering ratio in this energy range. It was found that, in order to be consistent with the experimental results, an accurate description at low Z must include nonlocal exchange, electron correlation, and dynamic effects. The second experiment concerns the ratio of helium double-to-single ionization for Compton scattering in the 8-28 keV energy range where published experimental and theoretical results so far fail to give a consistent picture. The progress of the experiment and the data analysis is reported

  3. Structure of liposome encapsulating proteins characterized by X-ray scattering and shell-modeling

    International Nuclear Information System (INIS)

    Hirai, Mitsuhiro; Kimura, Ryota; Takeuchi, Kazuki; Hagiwara, Yoshihiko; Kawai-Hirai, Rika; Ohta, Noboru; Igarashi, Noriyuki; Shimuzu, Nobutaka

    2013-01-01

    Wide-angle X-ray scattering data using a third-generation synchrotron radiation source are presented. Lipid liposomes are promising drug delivery systems because they have superior curative effects owing to their high adaptability to a living body. Lipid liposomes encapsulating proteins were constructed and the structures examined using synchrotron radiation small- and wide-angle X-ray scattering (SR-SWAXS). The liposomes were prepared by a sequential combination of natural swelling, ultrasonic dispersion, freeze-throw, extrusion and spin-filtration. The liposomes were composed of acidic glycosphingolipid (ganglioside), cholesterol and phospholipids. By using shell-modeling methods, the asymmetric bilayer structure of the liposome and the encapsulation efficiency of proteins were determined. As well as other analytical techniques, SR-SWAXS and shell-modeling methods are shown to be a powerful tool for characterizing in situ structures of lipid liposomes as an important candidate of drug delivery systems

  4. Small-angle X-ray scattering studies of thermally-induced globular protein gels

    International Nuclear Information System (INIS)

    Clark, A.H.; Tuffnell, C.D.

    1980-01-01

    Small-angle X-ray scattering has been applied to gels formed by heating globular proteins, in aqueous solution, above their unfolding temperatures. A number of BSA gels, previously characterised by electron microscopy, have been studied, and by setting up theoretical models for the scattering process, the X-ray data have been shown to be consistent with the microscope conclusions regarding network structure. It is concluded that the networks form by a linearly-directed aggregation of unfolded, disc-like, protein molecules, three-dimensional geometry being achieved by occasional branching, and/or cross-linking. Long-range inhomogeneities in network structure, easily observed by electron microscopy, and correlated with variations in pH or ionic strength, have an effect on X-ray scattering, and hence the X-ray method is sensitive not only to different network strand thicknesses, but to different degrees of uniformity as well. (author)

  5. X-ray scattering studies of non-equilibrium ordering processes

    International Nuclear Information System (INIS)

    Nagler, S.E.

    1992-01-01

    This report summarizes the major results obtained under US DOE Grant Number FG05-90ER45280 from the dates November 1, 1989 through October 31, 1992 inclusive. The principal work includes x-ray scattering studies of phase transition kinetics in binary alloy order-disorder transitions, block co-polymer crystallization, and charge density wave solids under applied electric fields, and studies of magnetic excitations in low dimensional quantum systems

  6. Fingerprints of orbital physics in magnetic resonant inelastic X-ray scattering

    Science.gov (United States)

    Marra, Pasquale

    2012-09-01

    Orbital degrees of freedom play a major role in the physics of many strongly correlated transition metal compounds. However, they are still very difficult to access experimentally, in particular by neutron scattering. We propose here how to reveal orbital occupancies of the system ground state by magnetic resonant inelastic x-ray scattering (RIXS). This is possible because, unlike in neutron scattering, the intensity of the magnetic excitations in RIXS depends essentially on the symmetry of the orbitals where the spins are in.

  7. Oil classification using X-ray scattering and principal component analysis

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Danielle S.; Souza, Amanda S.; Lopes, Ricardo T., E-mail: dani.almeida84@gmail.com, E-mail: ricardo@lin.ufrj.br, E-mail: amandass@bioqmed.ufrj.br [Universidade Federal do Rio de Janeiro (UFRJ), Rio de Janeiro, RJ (Brazil); Oliveira, Davi F.; Anjos, Marcelino J., E-mail: davi.oliveira@uerj.br, E-mail: marcelin@uerj.br [Universidade do Estado do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil). Inst. de Fisica Armando Dias Tavares

    2015-07-01

    X-ray scattering techniques have been considered promising for the classification and characterization of many types of samples. This study employed this technique combined with chemical analysis and multivariate analysis to characterize 54 vegetable oil samples (being 25 olive oils)with different properties obtained in commercial establishments in Rio de Janeiro city. The samples were chemically analyzed using the following indexes: iodine, acidity, saponification and peroxide. In order to obtain the X-ray scattering spectrum, an X-ray tube with a silver anode operating at 40kV and 50 μA was used. The results showed that oils cab ne divided in tow large groups: olive oils and non-olive oils. Additionally, in a multivariate analysis (Principal Component Analysis - PCA), two components were obtained and accounted for more than 80% of the variance. One component was associated with chemical parameters and the other with scattering profiles of each sample. Results showed that use of X-ray scattering spectra combined with chemical analysis and PCA can be a fast, cheap and efficient method for vegetable oil characterization. (author)

  8. Oil classification using X-ray scattering and principal component analysis

    International Nuclear Information System (INIS)

    Almeida, Danielle S.; Souza, Amanda S.; Lopes, Ricardo T.; Oliveira, Davi F.; Anjos, Marcelino J.

    2015-01-01

    X-ray scattering techniques have been considered promising for the classification and characterization of many types of samples. This study employed this technique combined with chemical analysis and multivariate analysis to characterize 54 vegetable oil samples (being 25 olive oils)with different properties obtained in commercial establishments in Rio de Janeiro city. The samples were chemically analyzed using the following indexes: iodine, acidity, saponification and peroxide. In order to obtain the X-ray scattering spectrum, an X-ray tube with a silver anode operating at 40kV and 50 μA was used. The results showed that oils cab ne divided in tow large groups: olive oils and non-olive oils. Additionally, in a multivariate analysis (Principal Component Analysis - PCA), two components were obtained and accounted for more than 80% of the variance. One component was associated with chemical parameters and the other with scattering profiles of each sample. Results showed that use of X-ray scattering spectra combined with chemical analysis and PCA can be a fast, cheap and efficient method for vegetable oil characterization. (author)

  9. Resonant Soft X-ray Scattering of Cellulose Microstructure in Plant Primary Cell Walls

    Science.gov (United States)

    Ye, Dan; Kiemle, Sarah N.; Wang, Cheng; Cosgrove, Daniel J.; Gomez, Esther W.; Gomez, Enrique D.

    Cellulosic biomass is the most abundant raw material available for the production of renewable and sustainable biofuels. Breaking down cellulose is the rate-limiting step in economical biofuel production; therefore, a detailed understanding of the microscopic structure of plant cell walls is required to develop efficient biofuel conversion methods. Primary cell walls are key determinants of plant growth and mechanics. Their structure is complex and heterogeneous, making it difficult to elucidate how various components such as pectin, hemicellulose, and cellulose contribute to the overall structure. The electron density of these wall components is similar; such that conventional hard X-ray scattering does not generate enough contrast to resolve the different elements of the polysaccharide network. The chemical specificity of resonant soft X-ray scattering allows contrast to be generated based on differences in chemistry of the different polysaccharides. By varying incident X-ray energies, we have achieved increased scattering contrast between cellulose and other polysaccharides from primary cell walls of onions. By performing scattering at certain energies, features of the network structure of the cell wall are resolved. From the soft X-ray scattering results, we obtained the packing distance of cellulose microfibrils embedded in the polysaccharide network.

  10. Studies of oxide-based thin-layered heterostructures by X-ray scattering methods

    Energy Technology Data Exchange (ETDEWEB)

    Durand, O. [Thales Research and Technology France, Route Departementale 128, F-91767 Palaiseau Cedex (France)]. E-mail: olivier.durand@thalesgroup.com; Rogers, D. [Nanovation SARL, 103 bis rue de Versailles 91400 Orsay (France); Universite de Technologie de Troyes, 10-12 rue Marie Curie, 10010 (France); Teherani, F. Hosseini [Nanovation SARL, 103 bis rue de Versailles 91400 Orsay (France); Andrieux, M. [LEMHE, ICMMOCNRS-UMR 8182, Universite d' Orsay, Batiment 410, 91410 Orsay (France); Modreanu, M. [Tyndall National Institute, Lee Maltings, Prospect Row, Cork (Ireland)

    2007-06-04

    Some X-ray scattering methods (X-ray reflectometry and Diffractometry) dedicated to the study of thin-layered heterostructures are presented with a particular focus, for practical purposes, on the description of fast, accurate and robust techniques. The use of X-ray scattering metrology as a routinely working non-destructive testing method, particularly by using procedures simplifying the data-evaluation, is emphasized. The model-independent Fourier-inversion method applied to a reflectivity curve allows a fast determination of the individual layer thicknesses. We demonstrate the capability of this method by reporting X-ray reflectometry study on multilayered oxide structures, even when the number of the layers constitutive of the stack is not known a-priori. Fast Fourier transform-based procedure has also been employed successfully on high resolution X-ray diffraction profiles. A study of the reliability of the integral-breadth methods in diffraction line-broadening analysis applied to thin layers, in order to determine coherent domain sizes, is also reported. Examples from studies of oxides-based thin-layers heterostructures will illustrate these methods. In particular, X-ray scattering studies performed on high-k HfO{sub 2} and SrZrO{sub 3} thin-layers, a (GaAs/AlOx) waveguide, and a ZnO thin-layer are reported.

  11. High resolution x-ray scattering studies of strain in epitaxial thin films of yttrium silicide grown on silicon (111)

    International Nuclear Information System (INIS)

    Marthinez-Miranda, L.J.; Santiago-Aviles, J.J.; Siegal, M.P.; Graham, W.R.; Heiney, P.A.

    1990-01-01

    The authors have used high resolution grazing incidence x-ray scattering (GIXS) to study the in- plane and out-of-plane structure of epitaxial YSi 2-x films grown on Si(111), with thicknesses ranging from 85 Angstrom to 510 Angstrom. Their results indicate that the films are strained, and that film strain increases as a function of thickness, with lattice parameters varying from a = 3.846 Angstrom/c = 4.142 Angstrom for the 85 Angstrom film to a = 3.877 Angstrom/c = 4.121 Angstrom for the 510 Angstrom film. The authors correlate these results with an increase in pinhole areal coverage as a function of thickness. In addition, the authors' measurements show no evidence for the existence of ordered silicon vacancies in the films

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

    DEFF Research Database (Denmark)

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

    2017-01-01

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

  13. Probing single magnon excitations in Sr₂IrO₄ using O K-edge resonant inelastic x-ray scattering.

    Science.gov (United States)

    Liu, X; Dean, M P M; Liu, J; Chiuzbăian, S G; Jaouen, N; Nicolaou, A; Yin, W G; Rayan Serrao, C; Ramesh, R; Ding, H; Hill, J P

    2015-05-27

    Resonant inelastic x-ray scattering (RIXS) at the L-edge of transition metal elements is now commonly used to probe single magnon excitations. Here we show that single magnon excitations can also be measured with RIXS at the K-edge of the surrounding ligand atoms when the center heavy metal elements have strong spin-orbit coupling. This is demonstrated with oxygen K-edge RIXS experiments on the perovskite Sr2IrO4, where low energy peaks from single magnon excitations were observed. This new application of RIXS has excellent potential to be applied to a wide range of magnetic systems based on heavy elements, for which the L-edge RIXS energy resolution in the hard x-ray region is usually poor.

  14. A simple, direct method for x-ray scatter estimation and correction in digital radiography and cone-beam CT

    International Nuclear Information System (INIS)

    Siewerdsen, J.H.; Daly, M.J.; Bakhtiar, B.

    2006-01-01

    X-ray scatter poses a significant limitation to image quality in cone-beam CT (CBCT), resulting in contrast reduction, image artifacts, and lack of CT number accuracy. We report the performance of a simple scatter correction method in which scatter fluence is estimated directly in each projection from pixel values near the edge of the detector behind the collimator leaves. The algorithm operates on the simple assumption that signal in the collimator shadow is attributable to x-ray scatter, and the 2D scatter fluence is estimated by interpolating between pixel values measured along the top and bottom edges of the detector behind the collimator leaves. The resulting scatter fluence estimate is subtracted from each projection to yield an estimate of the primary-only images for CBCT reconstruction. Performance was investigated in phantom experiments on an experimental CBCT benchtop, and the effect on image quality was demonstrated in patient images (head, abdomen, and pelvis sites) obtained on a preclinical system for CBCT-guided radiation therapy. The algorithm provides significant reduction in scatter artifacts without compromise in contrast-to-noise ratio (CNR). For example, in a head phantom, cupping artifact was essentially eliminated, CT number accuracy was restored to within 3%, and CNR (breast-to-water) was improved by up to 50%. Similarly in a body phantom, cupping artifact was reduced by at least a factor of 2 without loss in CNR. Patient images demonstrate significantly increased uniformity, accuracy, and contrast, with an overall improvement in image quality in all sites investigated. Qualitative evaluation illustrates that soft-tissue structures that are otherwise undetectable are clearly delineated in scatter-corrected reconstructions. Since scatter is estimated directly in each projection, the algorithm is robust with respect to system geometry, patient size and heterogeneity, patient motion, etc. Operating without prior information, analytical modeling

  15. In situ ultra-small-angle X-ray scattering study under uniaxial stretching of colloidal crystals prepared by silica nanoparticles bearing hydrogen-bonding polymer grafts

    Directory of Open Access Journals (Sweden)

    Ryohei Ishige

    2016-05-01

    Full Text Available A molded film of single-component polymer-grafted nanoparticles (SPNP, consisting of a spherical silica core and densely grafted polymer chains bearing hydrogen-bonding side groups capable of physical crosslinking, was investigated by in situ ultra-small-angle X-ray scattering (USAXS measurement during a uniaxial stretching process. Static USAXS revealed that the molded SPNP formed a highly oriented twinned face-centered cubic (f.c.c. lattice structure with the [11−1] plane aligned nearly parallel to the film surface in the initial state. Structural analysis of in situ USAXS using a model of uniaxial deformation induced by rearrangement of the nanoparticles revealed that the f.c.c. lattice was distorted in the stretching direction in proportion to the macroscopic strain until the strain reached 35%, and subsequently changed into other f.c.c. lattices with different orientations. The lattice distortion and structural transition behavior corresponded well to the elastic and plastic deformation regimes, respectively, observed in the stress–strain curve. The attractive interaction of the hydrogen bond is considered to form only at the top surface of the shell and then plays an effective role in cross-linking between nanoparticles. The rearrangement mechanism of the nanoparticles is well accounted for by a strong repulsive interaction between the densely grafted polymer shells of neighboring particles.

  16. Effects of phosphonium-based ionic liquids on phospholipid membranes studied by small-angle X-ray scattering

    Czech Academy of Sciences Publication Activity Database

    Kontro, I.; Svedström, K.; Duša, Filip; Ahvenainen, P.; Ruokonen, S. K.; Witos, J.; Wiedmer, S. K.

    2016-01-01

    Roč. 201, DEC (2016), s. 59-66 ISSN 0009-3084 Institutional support: RVO:68081715 Keywords : phospholipids * x-ray scattering Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.361, year: 2016

  17. Building a Unified Computational Model for the Resonant X-Ray Scattering of Strongly Correlated Materials

    International Nuclear Information System (INIS)

    Bansil, Arun

    2016-01-01

    Basic-Energy Sciences of the Department of Energy (BES/DOE) has made large investments in x-ray sources in the U.S. (NSLS-II, LCLS, NGLS, ALS, APS) as powerful enabling tools for opening up unprecedented new opportunities for exploring properties of matter at various length and time scales. The coming online of the pulsed photon source literally allows us to see and follow the dynamics of processes in materials at their natural timescales. There is an urgent need therefore to develop theoretical methodologies and computational models for understanding how x-rays interact with matter and the related spectroscopies of materials. The present project addressed aspects of this grand challenge of X-ray science. In particular, our Collaborative Research Team (CRT) focused on understanding and modeling of elastic and inelastic resonant X-ray scattering processes. We worked to unify the three different computational approaches currently used for modeling X-ray scattering-density functional theory, dynamical mean-field theory, and small-cluster exact diagonalization-to achieve a more realistic material-specific picture of the interaction between X-rays and complex matter. To achieve a convergence in the interpretation and to maximize complementary aspects of different theoretical methods, we concentrated on the cuprates, where most experiments have been performed. Our team included both US and international researchers, and it fostered new collaborations between researchers currently working with different approaches. In addition, we developed close relationships with experimental groups working in the area at various synchrotron facilities in the US. Our CRT thus helped toward enabling the US to assume a leadership role in the theoretical development of the field, and to create a global network and community of scholars dedicated to X-ray scattering research.

  18. International workshop on resonant X-ray scattering in electrically-ordered systems

    Energy Technology Data Exchange (ETDEWEB)

    Collins, S.P.; Pettifer, R.F.; Laundy, D.; Ishida, K.; Kokubun, J.; Giles, C.; Yokaichiya, F.; Song, C.; Lee, K.B.; Ji, S.; Koo, J.; Park, Y.J.; Kim, J.Y.; Park, J.H.; Shin, H.J.; Rhyee, J.S.; Oh, B.H.; Cho, B.K.; Wilkins Stuart, B.; Paixao, J.A.; Caciuffo, R.; Javorsky, P.; Wastin, F.; Rebizant, J.; Detlefs, C.; Bernheoft, N.; Lander, G.H.; Bombardi, A.; Bergevin, F. de; Matteo, S. di; Paolasini, L.; Rodriguez-Carvajal, J.; Carretta, P.; Millet, P.; Caciuffo, R.; Goff, J.P.; Deen, P.P.; Lee, S.; Stunault, A.; Brown, S.; Mannix, D.; McIntyre, G.J.; Ward, R.C.C.; Wells, M.R.; Lorenzo, J.E.; Joly, Y.; Nazarenko, E.; Staub, U.; Srajer, G.; Haskel, D.; Choi, Y.; Lee, D.R.; Lang, J.C.; Meersschaut, J.; Jiang, J.S.; Bader, S.D.; Bouchenoire, L.; Brown, S.D.; Beesley, A.; Herring, A.; Thomas, M.; Thompson, P.; Langridge, S.; Stirling, W.G.; Mirone, A.; Lander, G.; Wilkins, S.; Ward, R.C.C.; Wells, M.R.; Zochowski, S.W.; Garcia, J.; Subias, G.; Blasco, J.; Sanchez, M.C.; Proietti, M.G.; Lovesey, S.W.; Dmitrienko, V.E.; Ovchinnikova, E.N.; Ishida, K.; Kokubun, J.; Kirfel, A.; Collins, S.P.; Laundy, D.; Oreshko, A.P.; Strange, P.; Horne, M.; Arola, E.; Winter, H.; Szotek, Z.; Temmerman, W.M.; Igarashi, J.; Usuda, M.; Takahashi, M.; Matteo, S. di; Bernhoeft, N.; Hill, J.P.; Lang, J.C.; McWhan, D.; Lee, D.R.; Haskel, D.; Srajer, G.; Hatton Peter, D.; Katsumata, K.; Braithwaite, D

    2004-07-01

    The research field of Resonant X-ray Scattering (RXS) has achieved tremendous progress in the last years. Nowadays RXS is rapidly becoming the crucial technique for investigating the subtleties of microscopic magnetism in systems where the ground state properties reflect a delicate balance between several different correlated processes. The aim of this workshop is to discuss present and future possibilities for RXS investigations of electronic order, including studies of charge, magnetic, and multipolar ordered states. The sessions will cover experimental and theoretical aspects of hard and soft X-ray resonant scattering from single crystals and thin films. This document gathers the summaries of the presentations.

  19. A high-resolution multiwire area detector for X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Faruqi, A R; Andrews, H [Medical Research Council, Cambridge (UK). Lab. of Molecular Biology

    1989-11-10

    A high-resolution multiwire area detector has been developed for recording X-ray scattering from biological specimens. The detector is 100x100 mm{sup 2} and, under the present operating conditions, has a spatial resolution of about 250 {mu}m in both directions. The detector is set up on a double-mirror focusing camera on a rotating anode X-ray generator and has been used in a number of small-angle experiments, two of which are described in this paper. (orig.).

  20. Wide-angle X-ray scattering study of heat-treated PEEK and PEEK composite

    Science.gov (United States)

    Cebe, Peggy; Lowry, Lynn; Chung, Shirley Y.; Yavrouian, Andre; Gupta, Amitava

    1987-01-01

    Samples of poly(etheretherketone) (PEEK) neat resin and APC-2 carbon fiber composite were subjected to various heat treatments, and the effect of quenching and annealing treatments was studied by wide-angle X-ray scattering. It is found that high-temperature treatments may introduce disorder into neat resin and composite PEEK when followed by rapid cooling. The disorder is metastable and can revert to ordered state when the material is heated above its glass transition temperature and then cooled slowly. The disorder may result from residual thermal stresses.

  1. Ion track annealing in quartz investigated by small angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Schauries, D.; Afra, B.; Rodriguez, M.D. [Department of Electronic Materials Engineering, Research School of Physics and Engineering, The Australian National University, Canberra, ACT 2601 (Australia); Trautmann, C. [GSI Helmholtz Centre for Heavy Ion Research, Planckstrasse 1, 64291 Darmstadt (Germany); Technische Universität Darmstadt, 64287 Darmstadt (Germany); Hawley, A. [Australian Synchrotron, 800 Blackburn Road, Clayton, VIC 3168 (Australia); Kluth, P. [Department of Electronic Materials Engineering, Research School of Physics and Engineering, The Australian National University, Canberra, ACT 2601 (Australia)

    2015-12-15

    We report on the reduction of cross-section and length of amorphous ion tracks embedded within crystalline quartz during thermal annealing. The ion tracks were created via Au ion irradiation with an energy of 2.2 GeV. The use of synchrotron-based small angle X-ray scattering (SAXS) allowed characterization of the latent tracks, without the need for chemical etching. Temperatures between 900 and 1000 °C were required to see a notable change in track size. The shrinkage in cross-section and length was found to be comparable for tracks aligned perpendicular and parallel to the c-axis.

  2. Integrative structural modeling with small angle X-ray scattering profiles

    Directory of Open Access Journals (Sweden)

    Schneidman-Duhovny Dina

    2012-07-01

    Full Text Available Abstract Recent technological advances enabled high-throughput collection of Small Angle X-ray Scattering (SAXS profiles of biological macromolecules. Thus, computational methods for integrating SAXS profiles into structural modeling are needed more than ever. Here, we review specifically the use of SAXS profiles for the structural modeling of proteins, nucleic acids, and their complexes. First, the approaches for computing theoretical SAXS profiles from structures are presented. Second, computational methods for predicting protein structures, dynamics of proteins in solution, and assembly structures are covered. Third, we discuss the use of SAXS profiles in integrative structure modeling approaches that depend simultaneously on several data types.

  3. Resonant Inelastic X-ray Scattering: From band mapping to inter-orbital excitations

    International Nuclear Information System (INIS)

    Luning, J.; Hague, C.F.

    2008-01-01

    Resonant inelastic X-ray scattering (also known as resonant X-ray Raman spectroscopy when only valence and conduction states are involved in the final state excitation) has developed into a major tool for understanding the electronic properties of complex materials. Presently it provides access to electron excitations in the few hundred meV range with element and bulk selectivity. Recent progress in X-ray optics and synchrotron radiation engineering have opened up new perspectives for this powerful technique to improve resolving power and efficiency. We briefly present the basics of the method and illustrate its potential with examples chosen from the literature. (authors)

  4. International workshop on resonant X-ray scattering in electrically-ordered systems

    International Nuclear Information System (INIS)

    Collins, S.P.; Pettifer, R.F.; Laundy, D.; Ishida, K.; Kokubun, J.; Giles, C.; Yokaichiya, F.; Song, C.; Lee, K.B.; Ji, S.; Koo, J.; Park, Y.J.; Kim, J.Y.; Park, J.H.; Shin, H.J.; Rhyee, J.S.; Oh, B.H.; Cho, B.K.; Wilkins Stuart, B.; Paixao, J.A.; Caciuffo, R.; Javorsky, P.; Wastin, F.; Rebizant, J.; Detlefs, C.; Bernheoft, N.; Lander, G.H.; Bombardi, A.; Bergevin, F. de; Matteo, S. di; Paolasini, L.; Rodriguez-Carvajal, J.; Carretta, P.; Millet, P.; Caciuffo, R.; Goff, J.P.; Deen, P.P.; Lee, S.; Stunault, A.; Brown, S.; Mannix, D.; McIntyre, G.J.; Ward, R.C.C.; Wells, M.R.; Lorenzo, J.E.; Joly, Y.; Nazarenko, E.; Staub, U.; Srajer, G.; Haskel, D.; Choi, Y.; Lee, D.R.; Lang, J.C.; Meersschaut, J.; Jiang, J.S.; Bader, S.D.; Bouchenoire, L.; Brown, S.D.; Beesley, A.; Herring, A.; Thomas, M.; Thompson, P.; Langridge, S.; Stirling, W.G.; Mirone, A.; Lander, G.; Wilkins, S.; Ward, R.C.C.; Wells, M.R.; Zochowski, S.W.; Garcia, J.; Subias, G.; Blasco, J.; Sanchez, M.C.; Proietti, M.G.; Lovesey, S.W.; Dmitrienko, V.E.; Ovchinnikova, E.N.; Ishida, K.; Kokubun, J.; Kirfel, A.; Collins, S.P.; Laundy, D.; Oreshko, A.P.; Strange, P.; Horne, M.; Arola, E.; Winter, H.; Szotek, Z.; Temmerman, W.M.; Igarashi, J.; Usuda, M.; Takahashi, M.; Matteo, S. di; Bernhoeft, N.; Hill, J.P.; Lang, J.C.; McWhan, D.; Lee, D.R.; Haskel, D.; Srajer, G.; Hatton Peter, D.; Katsumata, K.; Braithwaite, D.

    2004-01-01

    The research field of Resonant X-ray Scattering (RXS) has achieved tremendous progress in the last years. Nowadays RXS is rapidly becoming the crucial technique for investigating the subtleties of microscopic magnetism in systems where the ground state properties reflect a delicate balance between several different correlated processes. The aim of this workshop is to discuss present and future possibilities for RXS investigations of electronic order, including studies of charge, magnetic, and multipolar ordered states. The sessions will cover experimental and theoretical aspects of hard and soft X-ray resonant scattering from single crystals and thin films. This document gathers the summaries of the presentations

  5. Temperature- and density-dependent x-ray scattering in a low-Z plasma

    International Nuclear Information System (INIS)

    Brown, R.T.

    1976-06-01

    A computer program is described which calculates temperature- and density-dependent differential and total coherent and incoherent x-ray scattering cross sections for a low-Z scattering medium. Temperature and density are arbitrary within the limitations of the validity of local thermodynamic equilbrium, since ionic populations are calculated under this assumption. Scattering cross sections are calculated in the form factor approximation. The scattering medium may consist of any mixure of elements with Z less than or equal to 8, with this limitation imposed by the availability of atomic data

  6. Study of pore growth in glassy carbon using small angle x-ray scattering

    International Nuclear Information System (INIS)

    Hoyt, J.

    1982-07-01

    Small-angle x-ray scattering was used to study the average pore size in glass-like carbon as a function of both heat-treatment time and heat-treatment temperature. A pore-growth model based on graphitization processes is presented. The simple mechanism shows that the change in the average radius of gyration with time is related to the total number of pores as a function of time, which in turn depends on the irreversible thermal-expansion phenomenon. The results of this study are inconsistent with a vacancy-migration pore-growth mechanism proposed earlier

  7. On-axis microscopes for the inelastic x-ray scattering beamline at NSLS-II

    Energy Technology Data Exchange (ETDEWEB)

    Gofron, K. J., E-mail: kgofron@bnl.gov; Cai, Y. Q.; Coburn, D. S.; Antonelli, S.; Suvorov, A. [National Synchrotron Light Source II, Brookhaven National Laboratory, Upton, NY 11973 (United States); Flores, J. [Department of Physics and Astronomy, Stony Brook University, NY 11794 (United States)

    2016-07-27

    A novel on-axis X-ray microscope with 3 µm resolution, 3x magnification, and a working distance of 600 mm for in-situ sample alignment and X-ray beam visualization for the Inelastic X-ray Scattering (IXS) beamline at NSLS-II is presented. The microscope uses reflective optics, which minimizes dispersion, and allows imaging from Ultraviolet (UV) to Infrared (IR) with specifically chosen objective components (coatings, etc.). Additionally, a portable high resolution X-ray microscope for KB mirror alignment and X-ray beam characterization was developed.

  8. PREFACE: Structure and dynamics determined by neutron and x-ray scattering Structure and dynamics determined by neutron and x-ray scattering

    Science.gov (United States)

    Müller-Buschbaum, Peter

    2011-06-01

    Neutron and x-ray scattering have emerged as powerful methods for the determination of structure and dynamics. Driven by emerging new, powerful neutron and synchrotron radiation sources, the continuous development of new instrumentation and novel scattering techniques gives rise to exciting possibilities. For example, in situ observations become possible via a high neutron or x-ray flux at the sample and, as a consequence, morphological transitions with small time constants can be detected. This special issue covers a broad range of different materials from soft to hard condensed matter. Hence, different material classes such as colloids, polymers, alloys, oxides and metals are addressed. The issue is dedicated to the 60th birthday of Professor Winfried Petry, scientific director of the Research Neutron Source Heinz Maier-Leibnitz (FRM-II), Germany, advisor at the physics department for the Bayerische Elite-Akademie, chair person of the Arbeitsgemeinschaft Metall- und Materialphysik of the German Physical Society (DPG) and a member of the professional council of the German Science Foundation (Deutsche Forschungsgemeinschaft, DFG). We would like to acknowledge and thank all contributors for their submissions, which made this special issue possible in the first place. Moreover, we would like to thank the staff at IOP Publishing for helping us with the administrative aspects and for coordinating the refereeing process, and Valeria Lauter for the beautiful cover artwork. Finally, to the readers, we hope that you find this special issue a valuable resource that provides insights into the present possibilities of neutron and x-ray scattering as powerful tools for the investigation of structure and dynamics. Structure and dynamics determined by neutron and x-ray scattering contents In situ studies of mass transport in liquid alloys by means of neutron radiography F Kargl, M Engelhardt, F Yang, H Weis, P Schmakat, B Schillinger, A Griesche and A Meyer Magnetic spin

  9. Time- and position-resolved synchrotron x-ray scattering for structure research on biological connective tissue

    International Nuclear Information System (INIS)

    Zizak, I.

    2000-03-01

    ELETTRA in Trieste. The results obtained during this thesis can be summarized in the following way: - If the tendon is stretched fast (0.1 %/second), the collagen fibers are not stretched an equal amount. Interfibrillar connections are responsible for about 50 % of the elongation of the tendon. - If the tendon is slowly stretched, the fibers creep, so they are stretched even less. At stretching speeds of 0.001 %/second the fibers are stretched only 10 % of the total tendon elongation. - There are two different processes in the collagen fiber which occur during the stretching. Stretching of the collagen triple helix is responsible for about 1/4 of the fibril elongation, and the rest can be described with the slippage of the helices, where only the cross-links between the molecules are stretched. There are indications that this process also depends on the velocity, what would include the viscose processes on the molecular level. Scanning small angle x-ray scattering of bone and cartilage Bone and cartilage are composite tissues consisting of an organic matrix (collagen) and small mineral particles (hydroxyapatite). The mineral particles have a typical thickness of about 3 nm and a length of a few hundreds of nanometers. At a higher hierarchical levels (sub-mm), the tissues have a foam like, trabecular structure with the trabeculae oriented along the main tension lines. The mechanical properties of bone depend on the structure at all levels of hierarchical organization. At the nanometer level, they are determined mainly by the size, shape and orientation of the (hard) mineral crystals within the (soft) organic matrix. In the course of this work, the hierarchical structure of the bone and cartilage was investigated using light- and scanning electron microscopy as well as position resolved scattering methods. A great advantage is the use of scanning small angle x-ray scattering (sSAXS) and wide angle scattering (WAXD, also x-ray diffraction, XRD), which provides simultaneous

  10. Automated microfluidic sample-preparation platform for high-throughput structural investigation of proteins by small-angle X-ray scattering

    DEFF Research Database (Denmark)

    Lafleur, Josiane P.; Snakenborg, Detlef; Nielsen, Søren Skou

    2011-01-01

    A new microfluidic sample-preparation system is presented for the structural investigation of proteins using small-angle X-ray scattering (SAXS) at synchrotrons. The system includes hardware and software features for precise fluidic control, sample mixing by diffusion, automated X-ray exposure...... control, UV absorbance measurements and automated data analysis. As little as 15 l of sample is required to perform a complete analysis cycle, including sample mixing, SAXS measurement, continuous UV absorbance measurements, and cleaning of the channels and X-ray cell with buffer. The complete analysis...

  11. Particle-scale structure in frozen colloidal suspensions from small-angle x-ray scattering

    KAUST Repository

    Spannuth, Melissa; Mochrie, S. G. J.; Peppin, S. S. L.; Wettlaufer, J. S.

    2011-01-01

    During directional solidification of the solvent in a colloidal suspension, the colloidal particles segregate from the growing solid, forming high-particle-density regions with structure on a hierarchy of length scales ranging from that of the particle-scale packing to the large-scale spacing between these regions. Previous work has concentrated mostly on the medium- to large-length scale structure, as it is the most accessible and thought to be more technologically relevant. However, the packing of the colloids at the particle scale is an important component not only in theoretical descriptions of the segregation process, but also to the utility of freeze-cast materials for new applications. Here we present the results of experiments in which we investigated this structure across a wide range of length scales using a combination of small-angle x-ray scattering and direct optical imaging. As expected, during freezing the particles were concentrated into regions between ice dendrites forming a microscopic pattern of high- and low-particle-density regions. X-ray scattering indicates that the particles in the high-density regions were so closely packed as to be touching. However, the arrangement of the particles does not conform to that predicted by standard interparticle pair potentials, suggesting that the particle packing induced by freezing differs from that formed during equilibrium densification processes. © 2011 American Physical Society.

  12. X-ray scattering evaluation of ultrastructural changes in human dental tissues with thermal treatment.

    Science.gov (United States)

    Sandholzer, Michael A; Sui, Tan; Korsunsky, Alexander M; Walmsley, Anthony Damien; Lumley, Philip J; Landini, Gabriel

    2014-05-01

    Micro- and ultrastructural analysis of burned skeletal remains is crucial for obtaining a reliable estimation of cremation temperature. Earlier studies mainly focused on heat-induced changes in bone tissue, while this study extends this research to human dental tissues using a novel quantitative analytical approach. Twelve tooth sections were burned at 400-900°C (30-min exposure, increments of 100°C). Subsequent combined small- and wide-angle X-ray scattering (SAXS/WAXS) experiments were performed at the Diamond Light Source synchrotron facility, where 28 scattering patterns were collected within each tooth section. In comparison with the control sample, an increase in mean crystal thickness was found in burned dentine (2.8-fold) and enamel (1.4-fold), however at a smaller rate than reported earlier for bone tissue (5-10.7-fold). The results provide a structural reference for traditional X-ray scattering methods and emphasize the need to investigate bone and dental tissues separately to obtain a reliable estimation of cremation temperature. © 2014 American Academy of Forensic Sciences.

  13. Particle-scale structure in frozen colloidal suspensions from small-angle x-ray scattering

    KAUST Repository

    Spannuth, Melissa

    2011-02-01

    During directional solidification of the solvent in a colloidal suspension, the colloidal particles segregate from the growing solid, forming high-particle-density regions with structure on a hierarchy of length scales ranging from that of the particle-scale packing to the large-scale spacing between these regions. Previous work has concentrated mostly on the medium- to large-length scale structure, as it is the most accessible and thought to be more technologically relevant. However, the packing of the colloids at the particle scale is an important component not only in theoretical descriptions of the segregation process, but also to the utility of freeze-cast materials for new applications. Here we present the results of experiments in which we investigated this structure across a wide range of length scales using a combination of small-angle x-ray scattering and direct optical imaging. As expected, during freezing the particles were concentrated into regions between ice dendrites forming a microscopic pattern of high- and low-particle-density regions. X-ray scattering indicates that the particles in the high-density regions were so closely packed as to be touching. However, the arrangement of the particles does not conform to that predicted by standard interparticle pair potentials, suggesting that the particle packing induced by freezing differs from that formed during equilibrium densification processes. © 2011 American Physical Society.

  14. Effect of Cobalt Fillers on Polyurethane Segmentations Investigated by Synchrotron Small Angle X-Ray Scattering

    Directory of Open Access Journals (Sweden)

    Krit Koyvanich

    2013-01-01

    Full Text Available The segmentation between rigid and rubbery chains in polyurethanes (PUs influences polymeric properties and implementations. Several models have successfully been proposed to visualize the configuration between the hard segment (HS and soft segment (SS. For particulate PU composites, the arrangement of HS and SS is more complicated because the fillers tend to disrupt the chain formation and segmentation. In this work, the effect of ferromagnetic cobalt (Co powders (average diameter 2 μm on PU synthesized from a reaction between polyether polyol (soft segment and diphenylmethane-4,4′-diisocyanate (hard segment was studied with varying loadings (0, 20, 40, and 60 wt.%. The 300 μm thick PU/Co samples were tape-casted and then received heat treatment at 80°C for 180 min. From synchrotron small angle X-ray scattering (SAXS, the plot of the X-ray scattering intensity (I against the scattering vector (q exhibited a typical single peak of PU whose intensity was reduced by the increase in the Co loading. Characteristic SAXS peaks in the case of 0-20 wt.% Co agreed well with the scattering by globular hard segment domains according to Zernike-Prins and Percus-Yevick models. The higher Co loadings led to larger deviations from all theoretical models.

  15. Strongly correlated electrons at high pressure: an approach by inelastic X-Ray scattering

    International Nuclear Information System (INIS)

    Rueff, J.P.

    2007-06-01

    Inelastic X-ray scattering (IXS) and associated methods has turn out to be a powerful alternative for high-pressure physics. It is an all-photon technique fully compatible with high-pressure environments and applicable to a vast range of materials. Standard focalization of X-ray in the range of 100 microns is typical of the sample size in the pressure cell. Our main aim is to provide an overview of experimental results obtained by IXS under high pressure in 2 classes of materials which have been at the origin of the renewal of condensed matter physics: strongly correlated transition metal oxides and rare-earth compounds. Under pressure, d and f-electron materials show behaviors far more complex that what would be expected from a simplistic band picture of electron delocalization. These spectroscopic studies have revealed unusual phenomena in the electronic degrees of freedom, brought up by the increased density, the changes in the charge-carrier concentration, the over-lapping between orbitals, and hybridization under high pressure conditions. Particularly we discuss about pressure induced magnetic collapse and metal-insulator transitions in 3d compounds and valence fluctuations phenomena in 4f and 5f compounds. Thanks to its superior penetration depth, chemical selectivity and resonant enhancement, resonant inelastic X-ray scattering has appeared extremely well suited to high pressure physics in strongly correlated materials. (A.C.)

  16. Use of dynamic light scattering and small-angle X-ray scattering to characterize new surfactants in solution conditions for membrane-protein crystallization

    Science.gov (United States)

    Dahani, Mohamed; Barret, Laurie-Anne; Raynal, Simon; Jungas, Colette; Pernot, Pétra; Polidori, Ange; Bonneté, Françoise

    2015-01-01

    The structural and interactive properties of two novel hemifluorinated surfactants, F2H9-β-M and F4H5-β-M, the syntheses of which were based on the structure and hydrophobicity of the well known dodecyl-β-maltoside (DD-β-M), are described. The shape of their micellar assemblies was characterized by small-angle X-ray scattering and their intermicellar inter­actions in crystallizing conditions were measured by dynamic light scattering. Such information is essential for surfactant phase-diagram determination and membrane-protein crystallization. PMID:26144228

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

    Science.gov (United States)

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

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

  18. More accurate X-ray scattering data of deeply supercooled bulk liquid water

    Energy Technology Data Exchange (ETDEWEB)

    Neuefeind, Joerg C [ORNL; Benmore, Chris J [Argonne National Laboratory (ANL); Weber, Richard [Argonne National Laboratory (ANL); Paschek, Dietmar [Rostock University, Rostock, Germany

    2011-01-01

    Deeply supercooled water droplets held container-less in an acoustic levitator are investigated with high energy X-ray scattering. The temperature dependence X-ray structure function is found to be non-linear. Comparison with two popular computer models reveals that structural changes are predicted too abrupt by the TIP5P model, while the rate of change predicted by TIP4P is in much better agreement with experiment. The abrupt structural changes predicted by the TIP5P model to occur in the temperature range between 260-240K as water approaches the homogeneous nucleation limit are unrealistic. Both models underestimate the distance between neighbouring oxygen atoms and overestimate the sharpness of the OO distance distribution, indicating that the strength of the H-bond is overestimated in these models.

  19. Low-angle polarized neutron and X-ray scattering from magnetic nanolayers and nanostructures

    CERN Document Server

    Paul, Amitesh

    2017-01-01

    This research monograph presents the latest results related to the characterization of low dimensional systems. Low-angle polarized neutron scattering and X-ray scattering at grazing incidence are used as the two main techniques to explore various physical phenomena of these systems. Special focus is put on systems like thin film transition metal and rare-earth layers, oxide heterostructures, hybrid systems, self-assembled nanostructures and self-diffusion.  Readers will gain in-depth knowledge about the usage of specular scattering and off-specular scattering techniques. Investigation of in-plane and out-of-plane structures and magnetism with vector magnetometric information is illustrated comprehensively. The book caters to a wide audience working in the field of nano-dimensional magnetic systems and the neutron and X-ray reflectometry community in particular.

  20. Structure factor of dimyristoylphosphatidylcholine unilamellar vesicles: small-angle x-ray scattering study

    International Nuclear Information System (INIS)

    Kiselev, M.A.; Aksenov, V.L.; Lombardo, D.; Kisselev, A.M.; Lesieur, P.

    2003-01-01

    Small-angle X-ray scattering (SAXS) experiments have been performed on dimyristoylphosphatidylcholine (DMPC) unilamellar vesicles in 40% aqueous sucrose solution. Model of separated form factors was applied for the evaluation of SAXS curves from large unilamellar vesicles. For the first time vesicle structure factor, polydispersity, average radius and membrane thickness were calculated simultaneously from the SAXS curves at T=30 deg C for DMPC concentrations in the range from 15 to 75 mM (1-5% w/w). Structure factor correction to the scattering curve was shown to be negligibly small for the lipid concentration of 15 mM (1% w/w). It was proved to be necessary to introduce structure factor correction to the scattering curves for lipid concentrations ≥ 30 mM (2% w/w)

  1. Theory of X-ray scattering by strongly distorted aging alloys with lamellar distribution of inclusions

    International Nuclear Information System (INIS)

    Barabash, R.I.; Krivoglaz, M.A.; AN Ukrainskoj SSR, Kiev. Inst. Metallofiziki)

    1981-01-01

    The X-ray scattering by strongly distorted heterogeneous alloys containing inclusions of new phase particles is discussed. Two models describing the lamellar structure with various orientation of inclusion axes in different layers are studied. In the first model the dimensions of inclusions are small in comparison with the layer thickness and they are randomly distributed in it, in the second model lamellar inclusions stretch through the whole layer. It is shown that in both models the Debye broadened line intensity distribution consists of overlapping Lorentz curves. A case of inclusions oriented along directions [100] and layers perpendicular to axes [110] is analyzed in detail. The results obtained for this case are compared with experimental results for the Cu-Be alloy

  2. Inelastic X-ray scattering experiments at extreme conditions: high temperatures and high pressures

    Directory of Open Access Journals (Sweden)

    S.Hosokawa

    2008-03-01

    Full Text Available In this article, we review the present status of experimental techniques under extreme conditions of high temperature and high pressure used for inelastic X-ray scattering (IXS experiments of liquid metals, semiconductors, molten salts, molecular liquids, and supercritical water and methanol. For high temperature experiments, some types of single-crystal sapphire cells were designed depending on the temperature of interest and the sample thickness for the X-ray transmission. Single-crystal diamond X-ray windows attached to the externally heated high-pressure vessel were used for the IXS experiment of supercritical water and methanol. Some typical experimental results are also given, and the perspective of IXS technique under extreme conditions is discussed.

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

    Science.gov (United States)

    Kowarik, Stefan

    2017-02-01

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

  4. The modular small-angle X-ray scattering data correction sequence.

    Science.gov (United States)

    Pauw, B R; Smith, A J; Snow, T; Terrill, N J; Thünemann, A F

    2017-12-01

    Data correction is probably the least favourite activity amongst users experimenting with small-angle X-ray scattering: if it is not done sufficiently well, this may become evident only during the data analysis stage, necessitating the repetition of the data corrections from scratch. A recommended comprehensive sequence of elementary data correction steps is presented here to alleviate the difficulties associated with data correction, both in the laboratory and at the synchrotron. When applied in the proposed order to the raw signals, the resulting absolute scattering cross section will provide a high degree of accuracy for a very wide range of samples, with its values accompanied by uncertainty estimates. The method can be applied without modification to any pinhole-collimated instruments with photon-counting direct-detection area detectors.

  5. Structural dissection of human metapneumovirus phosphoprotein using small angle x-ray scattering.

    Science.gov (United States)

    Renner, Max; Paesen, Guido C; Grison, Claire M; Granier, Sébastien; Grimes, Jonathan M; Leyrat, Cédric

    2017-11-01

    The phosphoprotein (P) is the main and essential cofactor of the RNA polymerase (L) of non-segmented, negative-strand RNA viruses. P positions the viral polymerase onto its nucleoprotein-RNA template and acts as a chaperone of the nucleoprotein (N), thereby preventing nonspecific encapsidation of cellular RNAs. The phosphoprotein of human metapneumovirus (HMPV) forms homotetramers composed of a stable oligomerization domain (P core ) flanked by large intrinsically disordered regions (IDRs). Here we combined x-ray crystallography of P core with small angle x-ray scattering (SAXS)-based ensemble modeling of the full-length P protein and several of its fragments to provide a structural description of P that captures its dynamic character, and highlights the presence of varyingly stable structural elements within the IDRs. We discuss the implications of the structural properties of HMPV P for the assembly and functioning of the viral transcription/replication machinery.

  6. Ultrasmall-angle X-ray scattering analysis of photonic crystal structure

    International Nuclear Information System (INIS)

    Abramova, V. V.; Sinitskii, A. S.; Grigor'eva, N. A.; Grigor'ev, S. V.; Belov, D. V.; Petukhov, A. V.; Mistonov, A. A.; Vasil'eva, A. V.; Tret'yakov, Yu. D.

    2009-01-01

    The results of an ultrasmall-angle X-ray scattering study of iron(III) oxide inverse opal thin films are presented. The photonic crystals examined are shown to have fcc structure with amount of stacking faults varying among the samples. The method used in this study makes it possible to easily distinguish between samples with predominantly twinned fcc structure and nearly perfect fcc stacking. The difference observed between samples fabricated under identical conditions is attributed to random layer stacking in the self-assembled colloidal crystals used as templates for fabricating the inverse opals. The present method provides a versatile tool for analyzing photonic crystal structure in studies of inverse opals made of various materials, colloidal crystals, and three-dimensional photonic crystals of other types.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-11-09

    Basic-Energy Sciences of the Department of Energy (BES/DOE) has made large investments in x-ray sources in the U.S. (NSLS-II, LCLS, NGLS, ALS, APS) as powerful enabling tools for opening up unprecedented new opportunities for exploring properties of matter at various length and time scales. The coming online of the pulsed photon source, literally allows us to see and follow the dynamics of processes in materials at their natural timescales. There is an urgent need therefore to develop theoretical methodologies and computational models for understanding how x-rays interact with matter and the related spectroscopies of materials. The present project addressed aspects of this grand challenge of x-ray science. In particular, our Collaborative Research Team (CRT) focused on developing viable computational schemes for modeling x-ray scattering and photoemission spectra of strongly correlated materials in the time-domain. The vast arsenal of formal/numerical techniques and approaches encompassed by the members of our CRT were brought to bear through appropriate generalizations and extensions to model the pumped state and the dynamics of this non-equilibrium state, and how it can be probed via x-ray absorption (XAS), emission (XES), resonant and non-resonant x-ray scattering, and photoemission processes. We explored the conceptual connections between the time-domain problems and other second-order spectroscopies, such as resonant inelastic x-ray scattering (RIXS) because RIXS may be effectively thought of as a pump-probe experiment in which the incoming photon acts as the pump, and the fluorescent decay is the probe. Alternatively, when the core-valence interactions are strong, one can view K-edge RIXS for example, as the dynamic response of the material to the transient presence of a strong core-hole potential. Unlike an actual pump-probe experiment, here there is no mechanism for adjusting the time-delay between the pump and the probe. However, the core hole

  8. Study of thermal degradation of organic light emitting device structures by X-ray scattering

    International Nuclear Information System (INIS)

    Lee, Young-Joo; Lee, Heeju; Byun, Youngsuk; Song, Sanghoon; Kim, Je-Eun; Eom, Daeyong; Cha, Wonsuk; Park, Seong-Sik; Kim, Jinwoo; Kim, Hyunjung

    2007-01-01

    We report the process of thermal degradation of organic light emitting devices (OLEDs) having multilayered structure of [LiF/tris-(8-hydroxyquinoline) aluminum(Alq 3 )/N,N'-Bis(naphthalen-1-yl)-N,N'-bis(phenyl)benzidine (NPB)/copper phthalocyanine (CuPc)/indium tin oxide (ITO)/SiO 2 on a glass] by synchrotron X-ray scattering. The results show that the thermally induced degradation process of OLED multilayers has undergone several evolutions due to thermal expansion of NPB, intermixing between NPB, Alq 3 , and LiF layers, dewetting of NPB on CuPc, and crystallization of NPB and Alq 3 depending on the annealing temperature. The crystallization of NPB appears at 180 deg. C, much higher temperature than the glass transition temperature (T g = 96 deg. C) of NPB. The results are also compared with the findings from the atomic force microscope (AFM) images

  9. Robust, high-throughput solution structural analyses by small angle X-ray scattering (SAXS)

    Energy Technology Data Exchange (ETDEWEB)

    Hura, Greg L.; Menon, Angeli L.; Hammel, Michal; Rambo, Robert P.; Poole II, Farris L.; Tsutakawa, Susan E.; Jenney Jr, Francis E.; Classen, Scott; Frankel, Kenneth A.; Hopkins, Robert C.; Yang, Sungjae; Scott, Joseph W.; Dillard, Bret D.; Adams, Michael W. W.; Tainer, John A.

    2009-07-20

    We present an efficient pipeline enabling high-throughput analysis of protein structure in solution with small angle X-ray scattering (SAXS). Our SAXS pipeline combines automated sample handling of microliter volumes, temperature and anaerobic control, rapid data collection and data analysis, and couples structural analysis with automated archiving. We subjected 50 representative proteins, mostly from Pyrococcus furiosus, to this pipeline and found that 30 were multimeric structures in solution. SAXS analysis allowed us to distinguish aggregated and unfolded proteins, define global structural parameters and oligomeric states for most samples, identify shapes and similar structures for 25 unknown structures, and determine envelopes for 41 proteins. We believe that high-throughput SAXS is an enabling technology that may change the way that structural genomics research is done.

  10. Anomalous X-ray scattering studies on semiconducting and metallic glasses

    International Nuclear Information System (INIS)

    Hosokawa, S.; Pilgrim, W.C.; Berar, J.F.; Kohara, S.

    2012-01-01

    In order to explore local- and intermediate-range atomic structures of several semiconducting and metallic glasses, anomalous X-ray scattering (AXS) experiments were performed using an improved detecting system suitable for third-generation synchrotron radiation facilities, and the obtained data were analyzed using reverse Monte Carlo (RMC) modelling to obtain partial structure factors and to construct three-dimensional atomic configurations of these glasses. Examples of GeSe 2 semiconducting and Pd 40 Ni 40 P 20 metallic glasses are demonstrated to exhibit the feasibility of the combination of AXS and RMC techniques. Importance of an additional combination with neutron scattering is also described for alloys containing light elements. (authors)

  11. Small angle x-ray scattering as a potential tool for cancer diagnosis

    International Nuclear Information System (INIS)

    Kitchen, M.; Siu, K.K.W.; Lewis, R.A.

    2003-01-01

    Full text: The diagnostic potential of Small Angle X-ray Scattering (SAXS) patterns has recently been investigated for malignant breast tissues. The demonstrated systematic differences in the scattering signatures of malignant, benign and normal breast tissue specimens are believed to arise from the changes in the fibrous proteins making up the extracellular matrix (ECM) with the disease progression. The technique may also have the potential to aid in the diagnosis of gliomas, a highly aggressive type of brain tumour. Although complex and difficult to interpret, SAXS data from malignant tissues may prove to be a more effective classification tool than conventional histology techniques. Here we present the methodology of the technique, as applied to breast cancer and brain tumour specimens to date, and some directions for future investigations. We also present a novel analysis method, which employs wavelet decomposition and a naive Bayesian classifier, as a potential semi-automated classification tool

  12. Interpretation and Utility of the Moments of Small-Angle X-Ray Scattering Distributions.

    Science.gov (United States)

    Modregger, Peter; Kagias, Matias; Irvine, Sarah C; Brönnimann, Rolf; Jefimovs, Konstantins; Endrizzi, Marco; Olivo, Alessandro

    2017-06-30

    Small angle x-ray scattering has been proven to be a valuable method for accessing structural information below the spatial resolution limit implied by direct imaging. Here, we theoretically derive the relation that links the subpixel differential phase signal provided by the sample to the moments of scattering distributions accessible by refraction sensitive x-ray imaging techniques. As an important special case we explain the scatter or dark-field contrast in terms of the sample's phase signal. Further, we establish that, for binary phase objects, the nth moment scales with the difference of the refractive index decrement to the power of n. Finally, we experimentally demonstrate the utility of the moments by quantitatively determining the particle sizes of a range of powders with a laboratory-based setup.

  13. Imaging Molecular Motion: Femtosecond X-Ray Scattering of an Electrocyclic Chemical Reaction

    Science.gov (United States)

    Minitti, M. P.; Budarz, J. M.; Kirrander, A.; Robinson, J. S.; Ratner, D.; Lane, T. J.; Zhu, D.; Glownia, J. M.; Kozina, M.; Lemke, H. T.; Sikorski, M.; Feng, Y.; Nelson, S.; Saita, K.; Stankus, B.; Northey, T.; Hastings, J. B.; Weber, P. M.

    2015-06-01

    Structural rearrangements within single molecules occur on ultrafast time scales. Many aspects of molecular dynamics, such as the energy flow through excited states, have been studied using spectroscopic techniques, yet the goal to watch molecules evolve their geometrical structure in real time remains challenging. By mapping nuclear motions using femtosecond x-ray pulses, we have created real-space representations of the evolving dynamics during a well-known chemical reaction and show a series of time-sorted structural snapshots produced by ultrafast time-resolved hard x-ray scattering. A computational analysis optimally matches the series of scattering patterns produced by the x rays to a multitude of potential reaction paths. In so doing, we have made a critical step toward the goal of viewing chemical reactions on femtosecond time scales, opening a new direction in studies of ultrafast chemical reactions in the gas phase.

  14. Structure Factor of Dimyristoylphosphatidylcholine Unilamellar Vesicles Small-Angle X-Ray Scattering Study

    CERN Document Server

    Kiselev, M A; Kisselev, A M; Lesieur, P; Aksenov, V L

    2003-01-01

    Small-angle X-ray scattering (SAXS) experiments have been performed on dimyristoylphosphatidylcholine (DMPC) unilamellar vesicles in 40 % aqueous sucrose solution. Model of separated form factors was applied for the evaluation of SAXS curves from large unilamellar vesicles. For the first time vesicle structure factor, polydispersity, average radius and membrane thickness were calculated simultaneously from the SAXS curves at T=306{\\circ}C for DMPC concentrations in the range from 15 to 75 mM (1-5 % w/w). Structure factor correction to the scattering curve was shown to be negligibly small for the lipid concentration of 15 mM (1 % w/w). It was proved to be necessary to introduce structure factor correction to the scattering curves for lipid concentrations {\\ge}30 mM (2 % w/w).

  15. Structure and dynamics of concentrated dispersions of polystyrene latex spheres in glycerol: Static and dynamic x-ray scattering

    International Nuclear Information System (INIS)

    Lumma, D.; Lurio, L. B.; Borthwick, M. A.; Falus, P.; Mochrie, S. G. J.

    2000-01-01

    X-ray photon correlation spectroscopy and small-angle x-ray scattering measurements are applied to characterize the dynamics and structure of concentrated suspensions of charge-stabilized polystyrene latex spheres dispersed in glycerol, for volume fractions between 2.7% and 52%. The static structures of the suspensions show essentially hard-sphere behavior. The short-time dynamics shows good agreement with predictions for the wave-vector-dependent collective diffusion coefficient, which are based on a hard-sphere model [C. W. J. Beenakker and P. Mazur, Physica A 126, 349 (1984)]. However, the intermediate scattering function is found to violate a scaling behavior found previously for a sterically stabilized hard-sphere suspension [P. N. Segre and P. N. Pusey, Phys. Rev. Lett. 77, 771 (1996)]. Our measurements are parametrized in terms of a viscoelastic model for the intermediate scattering function [W. Hess and R. Klein, Adv. Phys. 32, 173 (1983)]. Within this framework, two relaxation modes are predicted to contribute to the decay of the dynamic structure factor, with mode amplitudes depending on both wave vector and volume fraction. Our measurements indicate that, for particle volume fractions smaller than about 0.30, the intermediate scattering function is well described in terms of single-exponential decays, whereas a double-mode structure becomes apparent for more concentrated systems

  16. Resonant x-ray scattering in manganites: study of the orbital degree of freedom

    International Nuclear Information System (INIS)

    Ishihara, Sumio; Maekawa, Sadamichi

    2002-01-01

    The orbital degree of freedom of electrons and its interplay with spin, charge and lattice degrees of freedom are some of the central issues in colossal magnetoresistive manganites. The orbital degree of freedom has until recently remained hidden, since it does not couple directly to most experimental probes. Development of synchrotron light sources has changed the situation; by the resonant x-ray scattering (RXS) technique the orbital ordering has successfully been observed. In this article, we review progress in the recent studies of RXS in manganites. We start with a detailed review of the RXS experiments applied to the orbital-ordered manganites and other correlated electron systems. We derive the scattering cross section of RXS, where the tensor character of the atomic scattering factor (ASF) with respect to the x-ray polarization is stressed. Microscopic mechanisms of the anisotropic tensor character of the ASF are introduced and numerical results of the ASF and the scattering intensity are presented. The azimuthal angle scan is a unique experimental method to identify RXS from the orbital degree of freedom. A theory of the azimuthal angle and polarization dependence of the RXS intensity is presented. The theoretical results show good agreement with the experiments in manganites. Apart from the microscopic description of the ASF, a theoretical framework of RXS to relate directly to the 3d orbital is presented. The scattering cross section is represented by the correlation function of the pseudo-spin operator for the orbital degree of freedom. A theory is extended to the resonant inelastic x-ray scattering and methods to observe excitations of the orbital degree of freedom are proposed. (author)

  17. Building a Unified Computational Model for the Resonant X-Ray Scattering of Strongly Correlated Materials

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-12-01

    Basic-Energy Sciences of the Department of Energy (BES/DOE) has made large investments in x-ray sources in the U.S. (NSLS-II, LCLS, NGLS, ALS, APS) as powerful enabling tools for opening up unprecedented new opportunities for exploring properties of matter at various length and time scales. The coming online of the pulsed photon source literally allows us to see and follow the dynamics of processes in materials at their natural timescales. There is an urgent need therefore to develop theoretical methodologies and computational models for understanding how x-rays interact with matter and the related spectroscopies of materials. The present project addressed aspects of this grand challenge of X-ray science. In particular, our Collaborative Research Team (CRT) focused on understanding and modeling of elastic and inelastic resonant X-ray scattering processes. We worked to unify the three different computational approaches currently used for modeling X-ray scattering—density functional theory, dynamical mean-field theory, and small-cluster exact diagonalization—to achieve a more realistic material-specific picture of the interaction between X-rays and complex matter. To achieve a convergence in the interpretation and to maximize complementary aspects of different theoretical methods, we concentrated on the cuprates, where most experiments have been performed. Our team included both US and international researchers, and it fostered new collaborations between researchers currently working with different approaches. In addition, we developed close relationships with experimental groups working in the area at various synchrotron facilities in the US. Our CRT thus helped toward enabling the US to assume a leadership role in the theoretical development of the field, and to create a global network and community of scholars dedicated to X-ray scattering research.

  18. ORNL 10-m small-angle X-ray scattering camera

    International Nuclear Information System (INIS)

    Hendricks, R.W.

    1979-12-01

    A new small-angle x-ray scattering camera utilizing a rotating anode x-ray source, crystal monochromatization of the incident beam, pinhole collimation, and a two-dimensional position-sensitive proportional counter was developed. The sample, and the resolution element of the detector are each approximately 1 x 1 mm 2 , the camera was designed so that the focal spot-to-sample and sample-to-detector distances may each be varied in 0.5-m increments up to 5 m to provide a system resolution in the range 0.5 to 4.0 mrad. A large, general-purpose specimen chamber has been provided into which a wide variety of special-purpose specimen holders can be mounted. The detector has an active area of 200 x 200 mm and has up to 200 x 200 resolution elements. The data are recorded in the memory of a minicomputer by a high-speed interface which uses a microprocessor to map the position of an incident photon into an absolute minicomputer memory address. The data recorded in the computer memory can be processed on-line by a variety of programs designed to enhance the user's interaction with the experiment. At the highest angular resolution (0.4 mrad), the flux incident on the specimen is 1.0 x 10 6 photons/s with the x-ray source operating at 45 kV and 100 mA. SAX and its associated programs OVF and MOT are high-priority, pre-queued, nonresident foreground tasks which run under the ModComp II MAX III operating system to provide complete user control of the ORNL 10-m small-angle x-ray scattering camera

  19. A Grazing-Incidence Small-Angle X-Ray Scattering View of Vertically Aligned ZnO Nano wires

    International Nuclear Information System (INIS)

    Lavcevic, M.L.; Silovic, L.; Dubcek, P.; Pavlovic, M.; Bernstorff, S.

    2013-01-01

    We report a grazing-incidence small-angle X-ray scattering study of ZnO films with vertically aligned and randomly distributed nano wires, grown through a hydrothermal growth process on nano structured ZnO seeding coatings and deposited by electron beam evaporation on silicon and glass, respectively. The comparison of the scattering patterns of seeding coatings and nano wires showed that the scattering of vertically aligned nano wires exhibited a specific feature: the dominant characteristic of their scattering patterns is the appearance of fine structure effects around the specular peak. These effects were clarified by the combined reflection and scattering phenomena, suggested for the aligned nano wires-substrate system. Furthermore, they enabled the calculation of the average gyration radius of nano wires in horizontal direction. The calculated value was in good agreement with the radii of nano wires estimated by surface electron microscopy. Therefore, the observed feature in the scattering pattern can serve as evidence of the aligned growth of nano wires.

  20. Dynamical correlation effects in a weakly correlated material: Inelastic x-ray scattering and photoemission spectra of beryllium

    Science.gov (United States)

    Seidu, Azimatu; Marini, Andrea; Gatti, Matteo

    2018-03-01

    Beryllium is a weakly correlated simple metal. Still we find that dynamical correlation effects, beyond the independent-particle picture, are necessary to successfully interpret the electronic spectra measured by inelastic x-ray scattering (IXS) and photoemission spectroscopies (PES). By combining ab initio time-dependent density-functional theory (TDDFT) and many-body Green's function theory in the G W approximation (G W A ), we calculate the dynamic structure factor, the quasiparticle (QP) properties and PES spectra of bulk Be. We show that band-structure effects (i.e., due to interaction with the crystal potential) and QP lifetimes (LT) are both needed in order to explain the origin of the measured double-peak features in the IXS spectra. A quantitative agreement with experiment is obtained only when LT are supplemented to the adiabatic local-density approximation (ALDA) of TDDFT. Besides the valence band, PES spectra display a satellite, a signature of dynamical correlation due to the coupling of QPs and plasmons, which we are able to reproduce thanks to the combination of the G W A for the self-energy with the cumulant expansion of the Green's function.

  1. Small-angle x-ray scattering study on conformation of amorphous polymer chain in the bulk

    International Nuclear Information System (INIS)

    Hayashi, Hisao; Hamada, Fumiyuki; Nakajima, Akio

    1975-01-01

    In a previous paper, the new method for the determination of the conformation of polymer chains in concentrated solution and in bulk by small angle X-ray scattering was reported. The purpose of this paper is to estimate the dimension and conformation of polystyrene chains in bulk by this method. The tagged polymer used was the copolymer of styrene and p-iodostyrene. Excess scattering was obtained by subtracting the intensity of polystyrene matrix from that of a mixture containing polystyrene and a small fraction of the tagged polystyrene. Since the excess scattering originates from the group of iodine atoms in the tagged polystyrene, the radius of gyration of the tagged polystyrene is estimated by Guinier plot. Measurement was made with a Kratky camera, and in order to obtain high scattering intensity, the primary beam with line-shaped cross section was used. The intercepts of two limiting curves in the plotted radius of gyration diagram showed good agreement, and the measured molecular dimension agreed with the unperturbed dimension of this polymer. It was concluded that the molecular chains in bulk are mutually penetrable, and the centers of gravity of the molecules distribute almost randomly. It was suggested from the plot of the excess scattering intensity that the conformation of the tagged molecules is a random coil. The present results did not support the ordered structure revealed by bundle model and meander model. (Kako, I.)

  2. Automation and remote access of EMBL small angle X-ray scattering beamline X33 dedicated to biological macromolecules

    International Nuclear Information System (INIS)

    Weifeng Shang; Roessle, M.; Blanchet, C.; Zozulya, A.; Franke, D.; Petoukhov, M.; Kikhney, A.; Svergun, D.

    2009-01-01

    Full text: The small-angle X-ray scattering beamline X33 of the European Molecular Biology Laboratory (EMBL) at the DORIS III storage ring (HASYLAB/DESY) has been dedicated to structural studies of non-crystalline biological systems for more than two decades. In the last several years, the introduction of new optical systems (monochromator, mirror, slits etc) and detector systems (large area image plate Mar345 and PILATUS 1M) leads to an improvement of photon flux by a factor of 3 and a reduction of the exposure time by a factor of 7. Moreover, an automated sample changer has been constructed and in operation since August 2007. The data analysis pipeline consisting of the program suite yields the radius of gyration and forward scattering intensity using Guinier analysis (AutoRg), pair distance distribution function p(r) using indirect Fourier transform method (AutoGNOM), and bead models using ab initio shape determination (DAMMIN and DAMMIF). The results of these analysis which are immediately available after each measurement provides an invaluable tool for data quality control during the data collection. Furthermore, works on remote control of the integrated data collection and analysis software is ongoing and expected to be operated in late 2009 where users can send their samples and control the measurements at home institutes. (author)

  3. Relationship between electrical properties and crystallization of indium oxide thin films using ex-situ grazing-incidence wide-angle x-ray scattering

    Science.gov (United States)

    González, G. B.; Okasinski, J. S.; Buchholz, D. B.; Boesso, J.; Almer, J. D.; Zeng, L.; Bedzyk, M. J.; Chang, R. P. H.

    2017-05-01

    Grazing-incidence, wide-angle x-ray scattering measurements were conducted on indium oxide thin films grown on silica substrates via pulsed laser deposition. Growth temperatures (TG) in this study ranged from -50 °C to 600 °C, in order to investigate the thermal effects on the film structure and its spatial homogeneity, as well as their relationship to electrical properties. Films grown below room temperature were amorphous, while films prepared at TG = 25 °C and above crystallized in the cubic bixbyite structure, and their crystalline fraction increased with deposition temperature. The electrical conductivity (σ) and electrical mobility (μ) were strongly enhanced at low deposition temperatures. For TG = 25 °C and 50 °C, a strong ⟨100⟩ preferred orientation (texture) occurred, but it decreased as the deposition temperature, and consequential crystallinity, increased. Higher variations in texture coefficients and in lattice parameters were measured at the film surface compared to the interior of the film, indicating strong microstructural gradients. At low crystallinity, the in-plane lattice spacing expanded, while the out-of-plane spacing contracted, and those values merged at TG = 400 °C, where high μ was measured. This directional difference in lattice spacing, or deviatoric strain, was linear as a function of both deposition temperature and the degree of crystallinity. The crystalline sample with TG = 100 °C had the lowest mobility, as well as film diffraction peaks which split into doublets. The deviatoric strains from these doublet peaks differ by a factor of four, supporting the presence of both a microstructure and strain gradient in this film. More isotropic films exhibit larger μ values, indicating that the microstructure directly correlates with electrical properties. These results provide valuable insights that can help to improve the desirable properties of indium oxide, as well as other transparent conducting oxides.

  4. Repeated sorption of water in SBA-15 investigated by means of in situ small-angle x-ray scattering

    International Nuclear Information System (INIS)

    Erko, M; Paris, O; Wallacher, D; Findenegg, G H

    2012-01-01

    The effect of repeated cycles of water adsorption/desorption on the structural stability of ordered mesoporous silica SBA-15 is studied by small-angle x-ray scattering (SAXS). In situ sorption measurements are conducted using a custom-built sorption apparatus in connection with a laboratory SAXS setup. Two striking irreversible changes are observed in the sorption isotherms as derived from the integrated SAXS intensity. First, the capillary condensation pressure shifts progressively to lower relative pressure values with increasing number of sorption cycles. This effect is attributed to chemisorption of water at the silica walls, resulting in a change of the fluid-wall interaction. Second, the sorption cycles do not close completely at vanishing vapour pressure, suggesting that progressively more water remains trapped within the porous material after each cycle. This effect is interpreted to be the result of an irreversible collapse of parts of mesopores, originating from pore wall deformation due to the large Laplace pressure of water acting on the pore walls at capillary condensation and capillary evaporation. (paper)

  5. Ultra-small-angle X-ray scattering characterization of diesel/gasoline soot: sizes and particle-packing conditions

    Energy Technology Data Exchange (ETDEWEB)

    Kameya, Yuki, E-mail: ykameya@anl.gov; Lee, Kyeong O. [Argonne National Laboratory, Center for Transportation Research (United States)

    2013-10-15

    Regulations on particulate emissions from internal combustion engines tend to become more stringent, accordingly the importance of particulate filters in the after-treatment system has been increasing. In this work, the applicability of ultra-small-angle X-ray scattering (USAXS) to diesel soot cake and gasoline soot was investigated. Gasoline-direct-injection engine soot was collected at different fuel injection timings. The unified fits method was applied to analyze the resultant scattering curves. The validity of analysis was supported by comparing with carbon black and taking the sample images using a transmission electron microscope, which revealed that the primary particle size ranged from 20 to 55 nm. In addition, the effects of particle-packing conditions on the USAXS measurement were demonstrated by using samples suspended in acetone. Then, the investigation was extended to characterization of diesel soot cake deposited on a diesel particulate filter (DPF). Diesel soot was trapped on a small piece of DPF at different deposition conditions which were specified using the Peclet number. The dependence of scattering curve on soot-deposition conditions was demonstrated. To support the interpretation of the USAXS results, soot cake samples were observed using a scanning electron microscope and the influence of particle-packing conditions on scattering curve was discussed.

  6. A 5-μm pitch charge-coupled device optimized for resonant inelastic soft X-ray scattering

    Science.gov (United States)

    Andresen, N. C.; Denes, P.; Goldschmidt, A.; Joseph, J.; Karcher, A.; Tindall, C. S.

    2017-08-01

    We have developed a charge-coupled device (CCD) with 5 μm × 45 μm pixels on high-resistivity silicon. The fully depleted 200 μm-thick silicon detector is back-illuminated through a 10 nm-thick in situ doped polysilicon window and is thus highly efficient for soft through >8 keV hard X-rays. The device described here is a 1.5 megapixel CCD with 2496 × 620 pixels. The pixel and camera geometry was optimized for Resonant Inelastic X-ray Scattering (RIXS) and is particularly advantageous for spectrometers with limited arm lengths. In this article, we describe the device architecture, construction and operation, and its performance during tests at the Advance Light Source (ALS) 8.0.1 RIXS beamline. The improved spectroscopic performance, when compared with a current standard commercial camera, is demonstrated with a ˜280 eV (CK) X-ray beam on a graphite sample. Readout noise is typically 3-6 electrons and the point spread function for soft CK X-rays in the 5 μm direction is 4.0 μm ± 0.2 μm. The measured quantum efficiency of the CCD is greater than 75% in the range from 200 eV to 1 keV.

  7. Dynamics of water intercalation fronts in a nano-layered synthetic silicate: A synchrotron X-ray scattering study

    International Nuclear Information System (INIS)

    Lovoll, G.; Sandnes, B.; Meheust, Y.; Maloy, K.J.; Fossum, J.O.; Silva, G.J. da; Mundim, M.S.P.; Droppa, R. Jr.; Fonseca, D.M.

    2005-01-01

    We performed synchrotron X-ray scattering studies of the dynamics of the water intercalation front in a Na-Fluorohectorite clay. Like other smectite clays, fluorohectorite particles can swell due to intercalation of successive water layers. Monitoring the intensities of Bragg peaks of the known 1- and 2-water-layer hydration states at different positions in the sample enabled spatial and temporal measurement of the proportions of the different hydration states. From experiments with controlled temperature and an imposed humidity gradient on a quasi one-dimensional powder sample, we were able to localize the intercalation front and demonstrate that the width of this front was smaller than 2 mm after penetrating 9 mm into the sample. The speed at which the intercalation front advanced through the sample during the diffusion process was shown to decrease with time. The diffraction signature of random water intercalation in the vicinity of the intercalation front also provided information on the changes in the water content of the mesopores around clay particles

  8. Conversion of Natural Tannin to Hydrothermal and Graphene-Like Carbons Studied by Wide-Angle X-ray Scattering.

    Science.gov (United States)

    Jurkiewicz, Karolina; Hawełek, Łukasz; Balin, Katarzyna; Szade, Jacek; Braghiroli, Flavia L; Fierro, Vanessa; Celzard, Alain; Burian, Andrzej

    2015-08-13

    The atomic structure of carbon materials prepared from natural tannin by two different techniques, high-temperature pyrolysis and low-temperature hydrothermal carbonization, was studied by wide-angle X-ray scattering. The obtained diffraction data were converted to the real space representation in the form of pair distribution functions. The X-ray photoelectron spectroscopy measurements provided information about the chemical state of carbon in tannin-based materials that was used to construct final structural models of the investigated samples. The results of the experimental data in both reciprocal and real spaces were compared with computer simulations based on the PM7 semiempirical quantum chemical method. Using the collected detailed information, structural models of the tannin-based carbons were proposed. The characteristics of the investigated materials at the atomic level were discussed in relation to their preparation method. The rearrangement of the tannin molecular structure and its transformation to graphene-like structure was described. The structure of tannin-based carbons pyrolyzed at 900 °C exhibited coherently scattering domains about 20 Å in size, consisting of two defected atomic layers and resembling a graphene-like arrangement.

  9. NiO as a test case for high resolution resonant inelastic soft x-ray scattering

    International Nuclear Information System (INIS)

    Ghiringhelli, G; Matsubara, M; Dallera, C; Fracassi, F; Gusmeroli, R; Piazzalunga, A; Tagliaferri, A; Brookes, N B; Kotani, A; Braicovich, L

    2005-01-01

    Resonant inelastic x-ray scattering (RIXS) at the L 2,3 edges of 3d transition metal compounds has recently become a high resolution spectroscopic technique thanks to improvements in the instrumentation. We have chosen the prototypical case of NiO to explore the various levels of interpretation applicable to L 3 RIXS spectra of strongly correlated electron systems. Starting from a set of experimental data measured across the Ni L 3 absorption edge with 550 meV combined energy resolution, we analyse the rich spectral structure within an atomic framework. The spectra can be separated into dd and charge transfer excitation regions. The dd excitations can be interpreted and well reproduced within a crystal field model. The charge transfer excitations are analysed through the comparison with calculations made in the Anderson impurity model. A series of parameters belonging to the proposed models (crystal field strength, charge transfer energy, hybridization integrals) can thus be extracted in a very direct and unambiguous way

  10. Ultra-small-angle X-ray scattering characterization of diesel/gasoline soot: sizes and particle-packing conditions

    Science.gov (United States)

    Kameya, Yuki; Lee, Kyeong O.

    2013-10-01

    Regulations on particulate emissions from internal combustion engines tend to become more stringent, accordingly the importance of particulate filters in the after-treatment system has been increasing. In this work, the applicability of ultra-small-angle X-ray scattering (USAXS) to diesel soot cake and gasoline soot was investigated. Gasoline-direct-injection engine soot was collected at different fuel injection timings. The unified fits method was applied to analyze the resultant scattering curves. The validity of analysis was supported by comparing with carbon black and taking the sample images using a transmission electron microscope, which revealed that the primary particle size ranged from 20 to 55 nm. In addition, the effects of particle-packing conditions on the USAXS measurement were demonstrated by using samples suspended in acetone. Then, the investigation was extended to characterization of diesel soot cake deposited on a diesel particulate filter (DPF). Diesel soot was trapped on a small piece of DPF at different deposition conditions which were specified using the Peclet number. The dependence of scattering curve on soot-deposition conditions was demonstrated. To support the interpretation of the USAXS results, soot cake samples were observed using a scanning electron microscope and the influence of particle-packing conditions on scattering curve was discussed.

  11. Ultra-small-angle X-ray scattering characterization of diesel/gasoline soot: sizes and particle-packing conditions

    International Nuclear Information System (INIS)

    Kameya, Yuki; Lee, Kyeong O.

    2013-01-01

    Regulations on particulate emissions from internal combustion engines tend to become more stringent, accordingly the importance of particulate filters in the after-treatment system has been increasing. In this work, the applicability of ultra-small-angle X-ray scattering (USAXS) to diesel soot cake and gasoline soot was investigated. Gasoline-direct-injection engine soot was collected at different fuel injection timings. The unified fits method was applied to analyze the resultant scattering curves. The validity of analysis was supported by comparing with carbon black and taking the sample images using a transmission electron microscope, which revealed that the primary particle size ranged from 20 to 55 nm. In addition, the effects of particle-packing conditions on the USAXS measurement were demonstrated by using samples suspended in acetone. Then, the investigation was extended to characterization of diesel soot cake deposited on a diesel particulate filter (DPF). Diesel soot was trapped on a small piece of DPF at different deposition conditions which were specified using the Peclet number. The dependence of scattering curve on soot-deposition conditions was demonstrated. To support the interpretation of the USAXS results, soot cake samples were observed using a scanning electron microscope and the influence of particle-packing conditions on scattering curve was discussed

  12. A 5-μm pitch charge-coupled device optimized for resonant inelastic soft X-ray scattering.

    Science.gov (United States)

    Andresen, N C; Denes, P; Goldschmidt, A; Joseph, J; Karcher, A; Tindall, C S

    2017-08-01

    We have developed a charge-coupled device (CCD) with 5 μm × 45 μm pixels on high-resistivity silicon. The fully depleted 200 μm-thick silicon detector is back-illuminated through a 10 nm-thick in situ doped polysilicon window and is thus highly efficient for soft through >8 keV hard X-rays. The device described here is a 1.5 megapixel CCD with 2496 × 620 pixels. The pixel and camera geometry was optimized for Resonant Inelastic X-ray Scattering (RIXS) and is particularly advantageous for spectrometers with limited arm lengths. In this article, we describe the device architecture, construction and operation, and its performance during tests at the Advance Light Source (ALS) 8.0.1 RIXS beamline. The improved spectroscopic performance, when compared with a current standard commercial camera, is demonstrated with a ∼280 eV (C K ) X-ray beam on a graphite sample. Readout noise is typically 3-6 electrons and the point spread function for soft C K X-rays in the 5 μm direction is 4.0 μm ± 0.2 μm. The measured quantum efficiency of the CCD is greater than 75% in the range from 200 eV to 1 keV.

  13. Quantitative anomalous small-angle X-ray scattering - The determination of chemical concentrations in nano-scale phases

    International Nuclear Information System (INIS)

    Goerigk, G.; Huber, K.; Mattern, N.; Williamson, D.L.

    2012-01-01

    In the last years Anomalous Small-Angle X-ray Scattering became a precise quantitative method resolving scattering contributions two or three orders of magnitude smaller compared to the overall small-angle scattering, which are related to the so-called pure-resonant scattering contribution. Additionally to the structural information precise quantitative information about the different constituents of multi-component systems like the fraction of a chemical component implemented into the materials nano-structures are obtained from these scattering contributions. The application of the Gauss elimination algorithm to the vector equation established by ASAXS measurements at three X-ray energies is demonstrated for three examples from chemistry and solid state physics. All examples deal with the quantitative analysis of the Resonant Invariant (RI-analysis). From the integrals of the pure-resonant scattering contribution the chemical concentrations in nano-scaled phases are determined. In one example the correlated analysis of the Resonant Invariant and the Non-resonant Invariant (NI-analysis) is employed. (authors)

  14. Structural features of various kinds of carbon fibers as determined by small-angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Li, Denghua; Du, Sujun [Shanxi Transportation Research Institute, National and Local Joint Engineering Laboratory of Advanced Road Materials, Taiyuan (China); Lu, Chunxiang; Wu, Gangping; Yang, Yu; Wang, Lina [Chinese Academy of Sciences, National Engineering Laboratory for Carbon Fiber Technology, Institute of Coal Chemistry, Taiyuan (China)

    2016-11-15

    The structural features of polyacrylonitrile and pitch-based carbon fibers were analyzed from a comprehensive point of view by X-ray measurements and related techniques. The results indicated that the undulating graphite ribbon with embedded microvoid was the main structural unit for graphitic fibers. The void's parameters for these fibers could be obtained directly by small-angle X-ray scattering following the classic method deduced based on the typical two-phase system (i.e., Porod's law, Guinier's law and Debye's law). The non-graphitic fibers, however, were composed of two-dimensional turbostratic crystallites in the aggregation of microfibril and thus had a quasi two-phase structure (microfibril, interfibrillar amorphous structure and microvoid embedded within the microfibril). The extended Debye or Beaucage model in this case should be applied in order to obtain the structural parameters. It also revealed that the quasi two-phase system would complete its transformation to two-phase system during high-temperature graphitization. Therefore, the degree of graphitization was speculated to be the essential indicator distinguishing graphitic fibers from non-graphitic ones and would be helpful in understanding the transformation of structural features during the graphitization of carbon fibers. (orig.)

  15. Study on the conformal variations of bovine and human serum albumin in solution using small angle X-ray scattering

    International Nuclear Information System (INIS)

    Olivieri, Johnny Rizzieri.

    1992-01-01

    It is reported a Small Angle X-Ray Scattering (SAXS) study of BSA (Bovine Serum Albumin) and HSA (Human Serum Albumin) on pH between 2.5 and 7.0. The measured scattering intensities, normalized in relation to incident beam, exposition time and scattering due to solvent and capillary, and corrected due to concentration and beam shape effects, have shown a strong dependence of the protein shape with pH for both albumins. It was found that the radius of gyration varies between 26.7 and 35 A, and the analyses of the distance distribution function. P(r), indicated that these proteins undergoes conformational changes with pH. Different theoretical shapes have been proposed and analysed comparing the computed P(r) function generated from the models with the experimental P(r). A large variety of shapes were found in both proteins, indicating that BSA and HSA are very flexibility macromolecules. (author). 60 refs., 49 figs., 7 tabs

  16. X-ray scattering in X-ray fluorescence spectra with X-ray tube excitation - Modelling, experiment, and Monte-Carlo simulation

    International Nuclear Information System (INIS)

    Hodoroaba, V.-D.; Radtke, M.; Vincze, L.; Rackwitz, V.; Reuter, D.

    2010-01-01

    X-ray scattering may contribute significantly to the spectral background of X-ray fluorescence (XRF) spectra. Based on metrological measurements carried out with a scanning electron microscope (SEM) having attached a well characterised X-ray source (polychromatic X-ray tube) and a calibrated energy dispersive X-ray spectrometer (EDS) the accuracy of a physical model for X-ray scattering is systematically evaluated for representative samples. The knowledge of the X-ray spectrometer efficiency, but also of the spectrometer response functions makes it possible to define a physical spectral background of XRF spectra. Background subtraction relying on purely mathematical procedures is state-of-the-art. The results produced by the analytical model are at least as reliable as those obtained by Monte-Carlo simulations, even without considering the very challenging contribution of multiple scattering. Special attention has been paid to Compton broadening. Relevant applications of the implementation of the analytical model presented in this paper are the prediction of the limits of detection for particular cases or the determination of the transmission of X-ray polycapillary lenses.

  17. 1s2p resonant inelastic x-ray scattering in a-Fe2O3

    NARCIS (Netherlands)

    Caliebe, W.A.; Kao, C.-C.; Hastings, J.B.; Taguchi, M.; Kotani, A.; Uozumi, T.; Groot, F.M.F. de

    1998-01-01

    We report experimental and theoretical results on the Fe K edge x-ray absorption spectrum and 1s2p resonant inelastic x-ray scattering (RIXS) spectra in a-Fe2O3 . The results are interpreted using an FeO6^9- cluster model with intra-atomic multiplet coupling and interatomic covalency

  18. Connecting the dots : shedding light on the self-assembly of semiconductor nanocrystals with synchrotron X-ray scattering techniques

    NARCIS (Netherlands)

    Geuchies, J.J.

    2017-01-01

    We studied the formation of two-dimensional crystals from nanocrystals using X-ray scattering techniques. Inside these nanocrystals, with sizes between 5-10 nm, the atoms are ordered in an atomic lattice. We use the nanocrystals as building blocks to create larger lattices in two dimensions. By

  19. Studying nanostructure gradients in injection-molded polypropylene/montmorillonite composites by microbeam small-angle x-ray scattering

    DEFF Research Database (Denmark)

    Stribeck, Norbert; Schneider, Konrad; Zeinolebadi, Ahmad

    2014-01-01

    The core–shell structure in oriented cylindrical rods of polypropylene (PP) and nanoclay composites (NCs) from PP and montmorillonite (MMT) is studied by microbeam small-angle x-ray scattering (SAXS). The structure of neat PP is almost homogeneous across the rod showing regular semicrystalline......-shaped phyllosilicate filler particles....

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

    KAUST Repository

    Smilgies, Detlef-M.

    2014-01-01

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

  1. Studies of protein structure in solution and protein folding using synchrotron small-angle x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Lingling [Stanford Univ., CA (United States)

    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.

  2. A software-based x-ray scatter correction method for breast tomosynthesis

    International Nuclear Information System (INIS)

    Jia Feng, Steve Si; Sechopoulos, Ioannis

    2011-01-01

    Purpose: To develop a software-based scatter correction method for digital breast tomosynthesis (DBT) imaging and investigate its impact on the image quality of tomosynthesis reconstructions of both phantoms and patients. Methods: A Monte Carlo (MC) simulation of x-ray scatter, with geometry matching that of the cranio-caudal (CC) view of a DBT clinical prototype, was developed using the Geant4 toolkit and used to generate maps of the scatter-to-primary ratio (SPR) of a number of homogeneous standard-shaped breasts of varying sizes. Dimension-matched SPR maps were then deformed and registered to DBT acquisition projections, allowing for the estimation of the primary x-ray signal acquired by the imaging system. Noise filtering of the estimated projections was then performed to reduce the impact of the quantum noise of the x-ray scatter. Three dimensional (3D) reconstruction was then performed using the maximum likelihood-expectation maximization (MLEM) method. This process was tested on acquisitions of a heterogeneous 50/50 adipose/glandular tomosynthesis phantom with embedded masses, fibers, and microcalcifications and on acquisitions of patients. The image quality of the reconstructions of the scatter-corrected and uncorrected projections was analyzed by studying the signal-difference-to-noise ratio (SDNR), the integral of the signal in each mass lesion (integrated mass signal, IMS), and the modulation transfer function (MTF). Results: The reconstructions of the scatter-corrected projections demonstrated superior image quality. The SDNR of masses embedded in a 5 cm thick tomosynthesis phantom improved 60%-66%, while the SDNR of the smallest mass in an 8 cm thick phantom improved by 59% (p < 0.01). The IMS of the masses in the 5 cm thick phantom also improved by 15%-29%, while the IMS of the masses in the 8 cm thick phantom improved by 26%-62% (p < 0.01). Some embedded microcalcifications in the tomosynthesis phantoms were visible only in the scatter

  3. Small-angle x-ray scattering investigation of the solution structure of troponin C

    International Nuclear Information System (INIS)

    Hubbard, S.R.; Hodgson, K.O.; Doniach, S.

    1988-01-01

    X-ray crystallographic studies of troponin C have revealed a novel protein structure consisting of two globular domains, each containing two Ca 2+ -binding sites, connected via a nine-turn alpha-helix, three turns of which are fully exposed to solvent. Since the crystals were grown at pH approximately 5, it is of interest to determine whether this structure is applicable to the protein in solution under physiological conditions. We have used small-angle x-ray scattering to examine the solution structure of troponin C at pH 6.8 and the effect of Ca 2+ on the structure. The scattering data are consistent with an elongated structure in solution with a radius of gyration of approximately 23.0 A, which is quite comparable to that computed for the crystal structure. The experimental scattering profile and the scattering profile computed from the crystal structure coordinates do, however, exhibit differences at the 40-A level. A weak Ca 2+ -facilitated dimerization of troponin C was observed. The data rule out large Ca 2+ -induced structural changes, indicating rather that the molecule with Ca 2+ bound is only slightly more compact than the Ca 2+ -free molecule

  4. X-ray Scatter Imaging of Hepatocellular Carcinoma in a Mouse Model Using Nanoparticle Contrast Agents

    Science.gov (United States)

    Rand, Danielle; Derdak, Zoltan; Carlson, Rolf; Wands, Jack R.; Rose-Petruck, Christoph

    2015-10-01

    Hepatocellular carcinoma (HCC) is one of the most common malignant tumors worldwide and is almost uniformly fatal. Current methods of detection include ultrasound examination and imaging by CT scan or MRI; however, these techniques are problematic in terms of sensitivity and specificity, and the detection of early tumors (<1 cm diameter) has proven elusive. Better, more specific, and more sensitive detection methods are therefore urgently needed. Here we discuss the application of a newly developed x-ray imaging technique called Spatial Frequency Heterodyne Imaging (SFHI) for the early detection of HCC. SFHI uses x-rays scattered by an object to form an image and is more sensitive than conventional absorption-based x-radiography. We show that tissues labeled in vivo with gold nanoparticle contrast agents can be detected using SFHI. We also demonstrate that directed targeting and SFHI of HCC tumors in a mouse model is possible through the use of HCC-specific antibodies. The enhanced sensitivity of SFHI relative to currently available techniques enables the x-ray imaging of tumors that are just a few millimeters in diameter and substantially reduces the amount of nanoparticle contrast agent required for intravenous injection relative to absorption-based x-ray imaging.

  5. Dichroism and resonant diffraction in x-ray scattering by complex materials

    International Nuclear Information System (INIS)

    Collins, S P; Lovesey, S W; Balcar, E

    2007-01-01

    We survey universal concepts that influence dichroism and resonant Bragg diffraction, aiming to reach across the range of scientific disciplines that benefit from x-ray techniques, namely, chemistry, physics, life-sciences, and the science of materials. To this end, we adopt a top down discussion of the aspects of symmetry and concomitant selection rules. Starting from selection rules that can be deduced from the global condition that an observable quantity is unchanged on reversing the directions of both space and time separately, to selection rules that flow from bulk symmetry properties of electrons imposed by elements of a point group or crystal class to, finally, atomic selection rules that emerge from the details of the electronic structure. As a motivation for the latter we discuss, with a new calculation of the x-ray scattering length, E 1-M 1 absorption and scattering events that particularly interest scientists studying the chirality of life. In the main text there is modest use of mathematics, with appropriate details relegated to a few appendices. (topical review)

  6. The accurate assessment of small-angle X-ray scattering data.

    Science.gov (United States)

    Grant, Thomas D; Luft, Joseph R; Carter, Lester G; Matsui, Tsutomu; Weiss, Thomas M; Martel, Anne; Snell, Edward H

    2015-01-01

    Small-angle X-ray scattering (SAXS) has grown in popularity in recent times with the advent of bright synchrotron X-ray sources, powerful computational resources and algorithms enabling the calculation of increasingly complex models. However, the lack of standardized data-quality metrics presents difficulties for the growing user community in accurately assessing the quality of experimental SAXS data. Here, a series of metrics to quantitatively describe SAXS data in an objective manner using statistical evaluations are defined. These metrics are applied to identify the effects of radiation damage, concentration dependence and interparticle interactions on SAXS data from a set of 27 previously described targets for which high-resolution structures have been determined via X-ray crystallography or nuclear magnetic resonance (NMR) spectroscopy. The studies show that these metrics are sufficient to characterize SAXS data quality on a small sample set with statistical rigor and sensitivity similar to or better than manual analysis. The development of data-quality analysis strategies such as these initial efforts is needed to enable the accurate and unbiased assessment of SAXS data quality.

  7. Resonant x-ray scattering study of the antiferroelectric and ferrielectric phases in liquid crystal devices

    International Nuclear Information System (INIS)

    Matkin, L. S.; Watson, S. J.; Gleeson, H. F.; Pindak, R.; Pitney, J.; Johnson, P. M.; Huang, C. C.; Barois, P.; Levelut, A.-M.; Srajer, G.

    2001-01-01

    Resonant x-ray scattering has been used to investigate the interlayer ordering of the antiferroelectric and ferrielectric smectic C * subphases in a device geometry. The liquid crystalline materials studied contain a selenium atom and the experiments were carried out at the selenium K edge allowing x-ray transmission through glass. The resonant scattering peaks associated with the antiferroelectric phase were observed in two devices containing different materials. It was observed that the electric-field-induced antiferroelectric to ferroelectric transition coincides with the chevron to bookshelf transition in one of the devices. Observation of the splitting of the antiferroelectric resonant peaks as a function of applied field also confirmed that no helical unwinding occurs at fields lower than the chevron to bookshelf threshold. Resonant features associated with the four-layer ferrielectric liquid crystal phase were observed in a device geometry. Monitoring the electric field dependence of these ferrielectric resonant peaks showed that the chevron to bookshelf transition occurs at a lower applied field than the ferrielectric to ferroelectric switching transition

  8. Innovative diffraction gratings for high-resolution resonant inelastic soft x-ray scattering spectroscopy

    International Nuclear Information System (INIS)

    Voronov, D.L.; Warwick, T.; Gullikson, E. M.; Salmassi, F.; Padmore, H. A.

    2016-01-01

    High-resolution Resonant Inelastic X-ray Scattering (RIXS) requires diffraction gratings with very exacting characteristics. The gratings should provide both very high dispersion and high efficiency which are conflicting requirements and extremely challenging to satisfy in the soft x-ray region for a traditional grazing incidence geometry. To achieve high dispersion one should increase the groove density of a grating; this however results in a diffraction angle beyond the critical angle range and results in drastic efficiency loss. The problem can be solved by use of multilayer coated blazed gratings (MBG). In this work we have investigated the diffraction characteristics of MBGs via numerical simulations and have developed a procedure for optimization of grating design for a multiplexed high resolution imaging spectrometer for RIXS spectroscopy to be built in sector 6 at the Advanced Light Source (ALS). We found that highest diffraction efficiency can be achieved for gratings optimized for 4"t"h or 5"t"h order operation. Fabrication of such gratings is an extremely challenging technological problem. We present a first experimental prototype of these gratings and report its performance. High order and high line density gratings have the potential to be a revolutionary new optical element that should have great impact in the area of soft x-ray RIXS.

  9. Structure of Nanoporous Biocarbon for Hydrogen Storage as Determined by Small Angle X-Ray Scattering

    Science.gov (United States)

    Wood, Mikael; Burress, J.; Pobst, J.; Carter, S.; Pfeifer, P.; Wexler, C.; Shah, P.; Suppes, G.

    2008-03-01

    As a member of the Alliance for Collaborative Research in Alternative Fuel Technology (ALL-CRAFT) our research group studies the properties of nanoporous biocarbon, produced from waste corn cob, with the goal of achieving the Department of Energy's gravimetric and volumetric standards for both hydrogen and methane gas storage. Small Angle X-Ray Scattering (SAXS) is a valuable tool in our investigation of the geometry of the pore space in our carbon samples. In this talk, we will compare the experimental SAXS data with theoretical results for various pore geometries to determine which pore models are consistent with experiment. Using data from nitrogen adsorption isotherms, along with SAXS, yields significant structural information about the pore space. This analysis should allow us to fully optimize our production process and to achieve the DOE's target storage capacities. This work supported by: 1. National Science Foundation (PFI-0438469) 2. U.S. Department of Education (P200A040038) 3. U.S. Department of Energy (DE-AC02-06CH11357) 4. University of Missouri (RB-06-040) 5. U.S. Department of Defense (N00164-07-P-1306) 6. U.S. Department of Energy (DE-FG02-07ER46411)

  10. Density functional simulation of resonant inelastic X-ray scattering experiments in liquids: acetonitrile.

    Science.gov (United States)

    Niskanen, Johannes; Kooser, Kuno; Koskelo, Jaakko; Käämbre, Tanel; Kunnus, Kristjan; Pietzsch, Annette; Quevedo, Wilson; Hakala, Mikko; Föhlisch, Alexander; Huotari, Simo; Kukk, Edwin

    2016-09-21

    In this paper we report an experimental and computational study of liquid acetonitrile (H 3 C-C[triple bond, length as m-dash]N) by resonant inelastic X-ray scattering (RIXS) at the N K-edge. The experimental spectra exhibit clear signatures of the electronic structure of the valence states at the N site and incident-beam-polarization dependence is observed as well. Moreover, we find fine structure in the quasielastic line that is assigned to finite scattering duration and nuclear relaxation. We present a simple and light-to-evaluate model for the RIXS maps and analyze the experimental data using this model combined with ab initio molecular dynamics simulations. In addition to polarization-dependence and scattering-duration effects, we pinpoint the effects of different types of chemical bonding to the RIXS spectrum and conclude that the H 2 C-C[double bond, length as m-dash]NH isomer, suggested in the literature, does not exist in detectable quantities. We study solution effects on the scattering spectra with simulations in liquid and in vacuum. The presented model for RIXS proved to be light enough to allow phase-space-sampling and still accurate enough for identification of transition lines in physical chemistry research by RIXS.

  11. Structural evaluation of an amyloid fibril model using small-angle x-ray scattering

    Science.gov (United States)

    Dahal, Eshan; Choi, Mina; Alam, Nadia; Bhirde, Ashwinkumar A.; Beaucage, Serge L.; Badano, Aldo

    2017-08-01

    Amyloid fibrils are highly structured protein aggregates associated with a wide range of diseases including Alzheimer’s and Parkinson’s. We report a structural investigation of an amyloid fibril model prepared from a commonly used plasma protein (bovine serum albumin (BSA)) using small-angle x-ray scattering (SAXS) technique. As a reference, the size estimates from SAXS are compared to dynamic light scattering (DLS) data and the presence of amyloid-like fibrils is confirmed using Congo red absorbance assay. Our SAXS results consistently show the structural transformation of BSA from spheroid to rod-like elongated structures during the fibril formation process. We observe the elongation of fibrils over two months with fibril length growing from 35.9  ±  3.0 nm to 51.5  ±  2.1 nm. Structurally metastable fibrils with distinct SAXS profiles have been identified. As proof of concept, we demonstrate the use of such distinct SAXS profiles to detect fibrils in the mixture solutions of two species by estimating their volume fractions. This easily detectable and well-characterized amyloid fibril model from BSA can be readily used as a control or standard reference to further investigate SAXS applications in the detection of structurally diverse amyloid fibrils associated with protein aggregation diseases.

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

    Directory of Open Access Journals (Sweden)

    Athanasios Ch Mitropoulos

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

  13. Theoretical model of x-ray scattering as a dense matter probe.

    Science.gov (United States)

    Gregori, G; Glenzer, S H; Rozmus, W; Lee, R W; Landen, O L

    2003-02-01

    We present analytical expressions for the dynamic structure factor, or form factor S(k,omega), which is the quantity describing the x-ray cross section from a dense plasma or a simple liquid. Our results, based on the random phase approximation for the treatment on the charged particle coupling, can be applied to describe scattering from either weakly coupled classical plasmas or degenerate electron liquids. Our form factor correctly reproduces the Compton energy down-shift and the known Fermi-Dirac electron velocity distribution for S(k,omega) in the case of a cold degenerate plasma. The usual concept of scattering parameter is also reinterpreted for the degenerate case in order to include the effect of the Thomas-Fermi screening. The results shown in this work can be applied to interpreting x-ray scattering in warm dense plasmas occurring in inertial confinement fusion experiments or for the modeling of solid density matter found in the interior of planets.

  14. Morphological and structural characterization of PHBV/organoclay nanocomposites by small angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Carli, Larissa N., E-mail: lncarli@ucs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, Porto Alegre, 91501-970, RS (Brazil); Centro de Ciencias Exatas e Tecnologia, Universidade de Caxias do Sul, Rua Francisco Getulio Vargas, 1130, Caxias do Sul, 95070-560, RS (Brazil); Bianchi, Otavio, E-mail: obianchi@ucs.br [Centro de Ciencias Exatas e Tecnologia, Universidade de Caxias do Sul, Rua Francisco Getulio Vargas, 1130, Caxias do Sul, 95070-560, RS (Brazil); Machado, Giovanna, E-mail: giovannamachado@uol.com.br [Centro de Tecnologias Estrategicas do Nordeste, Av. Prof. Luiz Freire, 01, Cidade Universitaria, Recife, 50740-540, PE (Brazil); Programa de Pos-Graduacao de Materiais, Universidade Federal de Pernambuco, Av. Prof. Moraes Rego, 1235, Recife, 50670-901, PE (Brazil); Crespo, Janaina S., E-mail: jscrespo@ucs.br [Centro de Ciencias Exatas e Tecnologia, Universidade de Caxias do Sul, Rua Francisco Getulio Vargas, 1130, Caxias do Sul, 95070-560, RS (Brazil); Mauler, Raquel S., E-mail: raquel.mauler@ufrgs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, Porto Alegre, 91501-970, RS (Brazil)

    2013-03-01

    In this work, the morphological and structural behaviors of poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV) nanocomposites were investigated using small angle X-ray scattering (SAXS), wide angle X-ray diffraction (WAXD) and transmission electron microscopy (TEM). The nanocomposites with 1, 3 and 5 wt.% of organically modified montmorillonite Cloisite Registered-Sign 30B (OMMT) were prepared by melt processing in a twin screw extruder using two different processing conditions (low and high shear intensity). The lamellar long period of the polymer was lower for the nanocomposites, with high polydispersity values. However, the crystalline thickness increased with the clay content and was independent of the processing conditions. This behavior resulted in a high linear crystallinity of the nanocomposites with 3 and 5 wt.% OMMT. The disruption factor ({beta}) was in agreement with the WAXD and TEM findings, indicating a good dispersion of the nanoparticles in the PHBV matrix with 3 wt.% of OMMT during the high shear intensity of melt processing. Highlights: Black-Right-Pointing-Pointer SAXS was used for morphological and crystalline studies of PHBV/OMMT nanocomposites. Black-Right-Pointing-Pointer The crystalline structure was influenced by the presence of clay. Black-Right-Pointing-Pointer The degree of clay dispersion in a polymer matrix was quantified. Black-Right-Pointing-Pointer The morphology comprised exfoliated particles, nanoscale and microscale clusters. Black-Right-Pointing-Pointer The results obtained by SAXS agreed well with TEM and WAXD results.

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

    Science.gov (United States)

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

    2016-01-01

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

  16. Six-dimensional real and reciprocal space small-angle X-ray scattering tomography.

    Science.gov (United States)

    Schaff, Florian; Bech, Martin; Zaslansky, Paul; Jud, Christoph; Liebi, Marianne; Guizar-Sicairos, Manuel; Pfeiffer, Franz

    2015-11-19

    When used in combination with raster scanning, small-angle X-ray scattering (SAXS) has proven to be a valuable imaging technique of the nanoscale, for example of bone, teeth and brain matter. Although two-dimensional projection imaging has been used to characterize various materials successfully, its three-dimensional extension, SAXS computed tomography, poses substantial challenges, which have yet to be overcome. Previous work using SAXS computed tomography was unable to preserve oriented SAXS signals during reconstruction. Here we present a solution to this problem and obtain a complete SAXS computed tomography, which preserves oriented scattering information. By introducing virtual tomography axes, we take advantage of the two-dimensional SAXS information recorded on an area detector and use it to reconstruct the full three-dimensional scattering distribution in reciprocal space for each voxel of the three-dimensional object in real space. The presented method could be of interest for a combined six-dimensional real and reciprocal space characterization of mesoscopic materials with hierarchically structured features with length scales ranging from a few nanometres to a few millimetres--for example, biomaterials such as bone or teeth, or functional materials such as fuel-cell or battery components.

  17. Collagen Orientation and Crystallite Size in Human Dentin: A Small Angle X-ray Scattering Study

    Energy Technology Data Exchange (ETDEWEB)

    Pople, John A

    2001-03-29

    The mechanical properties of dentin are largely determined by the intertubular dentin matrix, which is a complex composite of type I collagen fibers and a carbonate-rich apatite mineral phase. The authors perform a small angle x-ray scattering (SAXS) study on fully mineralized human dentin to quantify this fiber/mineral composite architecture from the nanoscopic through continuum length scales. The SAXS results were consistent with nucleation and growth of the apatite phase within periodic gaps in the collagen fibers. These mineralized fibers were perpendicular to the dentinal tubules and parallel with the mineralization growth front. Within the plane of the mineralization front, the mineralized collagen fibers were isotropic near the pulp, but became mildly anisotropic in the mid-dentin. Analysis of the data also indicated that near the pulp the mineral crystallites were approximately needle-like, and progressed to a more plate-like shape near the dentino-enamel junction. The thickness of these crystallites, {approx} 5 nm, did not vary significantly with position in the tooth. These results were considered within the context of dentinogenesis and maturation.

  18. The small angle x-ray scattering of globular proteins in solution during heat denaturation

    Science.gov (United States)

    Banuelos, Jose; Urquidi, Jacob

    2008-10-01

    The ability of proteins to change their conformation in response to changes in their environment has consequences in biological processes like metabolism, chemical regulation in cells, and is believed to play a role in the onset of several neurodegenerative diseases. Factors such as a change in temperature, pressure, and the introduction of ions into the aqueous environment of a protein can give rise to the folding/unfolding of a protein. As a protein unfolds, the ratio of nonpolar to polar groups exposed to water changes, affecting a protein's thermodynamic properties. Using small angle x-ray scattering (SAXS), we are currently studying the intermediate protein conformations that arise during the folding/unfolding process as a function of temperature for five globular proteins. Trends in the observed intermediate structures of these globular proteins, along with correlations with data on protein thermodynamics may help elucidate shared characteristics between all proteins in the folding/unfolding process. Experimental design considerations will be discussed and preliminary results for some of these systems will be presented.

  19. Soft X-ray radiation damage in EM-CCDs used for Resonant Inelastic X-ray Scattering

    Science.gov (United States)

    Gopinath, D.; Soman, M.; Holland, A.; Keelan, J.; Hall, D.; Holland, K.; Colebrook, D.

    2018-02-01

    Advancement in synchrotron and free electron laser facilities means that X-ray beams with higher intensity than ever before are being created. The high brilliance of the X-ray beam, as well as the ability to use a range of X-ray energies, means that they can be used in a wide range of applications. One such application is Resonant Inelastic X-ray Scattering (RIXS). RIXS uses the intense and tuneable X-ray beams in order to investigate the electronic structure of materials. The photons are focused onto a sample material and the scattered X-ray beam is diffracted off a high resolution grating to disperse the X-ray energies onto a position sensitive detector. Whilst several factors affect the total system energy resolution, the performance of RIXS experiments can be limited by the spatial resolution of the detector used. Electron-Multiplying CCDs (EM-CCDs) at high gain in combination with centroiding of the photon charge cloud across several detector pixels can lead to sub-pixel spatial resolution of 2-3 μm. X-ray radiation can cause damage to CCDs through ionisation damage resulting in increases in dark current and/or a shift in flat band voltage. Understanding the effect of radiation damage on EM-CCDs is important in order to predict lifetime as well as the change in performance over time. Two CCD-97s were taken to PTB at BESSY II and irradiated with large doses of soft X-rays in order to probe the front and back surfaces of the device. The dark current was shown to decay over time with two different exponential components to it. This paper will discuss the use of EM-CCDs for readout of RIXS spectrometers, and limitations on spatial resolution, together with any limitations on instrument use which may arise from X-ray-induced radiation damage.

  20. Solution small-angle x-ray scattering as a screening and predictive tool in the fabrication of asymmetric block copolymer membranes

    KAUST Repository

    Dorin, Rachel Mika; Marques, Debora S.; Sai, Hiroaki; Vainio, Ulla; Phillip, William A.; Peinemann, Klaus; Nunes, Suzana Pereira; Wiesner, Ulrich B.

    2012-01-01

    Small-angle X-ray scattering (SAXS) analysis of the diblock copolymer poly(styrene-b-(4-vinyl)pyridine) in a ternary solvent system of 1,4-dioxane, tetrahydrofuran, and N,N-dimethylformamide, and the triblock terpolymer poly(isoprene-b-styrene-b-(4-vinyl)-pyridine) in a binary solvent system of 1,4-dioxane and tetrahydrofuran, reveals a concentration-dependent onset of ordered structure formation. Asymmetric membranes fabricated from casting solutions with polymer concentrations at or slightly below this ordering concentration possess selective layers with the desired nanostructure. In addition to rapidly screening possible polymer solution concentrations, solution SAXS analysis also predicts hexagonal and square pore lattices of the final membrane surface structure. These results suggest solution SAXS as a powerful tool for screening casting solution concentrations and predicting surface structure in the fabrication of asymmetric ultrafiltration membranes from self-assembled block copolymers. (Figure presented) © 2012 American Chemical Society.

  1. Solution small-angle x-ray scattering as a screening and predictive tool in the fabrication of asymmetric block copolymer membranes

    KAUST Repository

    Dorin, Rachel Mika

    2012-05-15

    Small-angle X-ray scattering (SAXS) analysis of the diblock copolymer poly(styrene-b-(4-vinyl)pyridine) in a ternary solvent system of 1,4-dioxane, tetrahydrofuran, and N,N-dimethylformamide, and the triblock terpolymer poly(isoprene-b-styrene-b-(4-vinyl)-pyridine) in a binary solvent system of 1,4-dioxane and tetrahydrofuran, reveals a concentration-dependent onset of ordered structure formation. Asymmetric membranes fabricated from casting solutions with polymer concentrations at or slightly below this ordering concentration possess selective layers with the desired nanostructure. In addition to rapidly screening possible polymer solution concentrations, solution SAXS analysis also predicts hexagonal and square pore lattices of the final membrane surface structure. These results suggest solution SAXS as a powerful tool for screening casting solution concentrations and predicting surface structure in the fabrication of asymmetric ultrafiltration membranes from self-assembled block copolymers. (Figure presented) © 2012 American Chemical Society.

  2. Small-angle x-ray scattering study of kinetics of spinodal decomposition in N-isopropylacrylamide gels

    International Nuclear Information System (INIS)

    Liao, G.; Xie, Y.; Ludwig, K.F. Jr.; Bansil, R.; Gallagher, P.; Xie, Y.; Gallagher, P.

    1999-01-01

    We present synchrotron-based time-resolved small-angle x-ray scattering (SAXS) measurements of spinodal decomposition in a covalently cross-linked N-isopropylacrylamide gel. The range of wave numbers examined is well beyond the position of the maximum in the structure factor S(q,t). The equilibrium structure factor is described by the sum of a Lorentzian and a Gaussian. Following a temperature jump into the two phase region, the scattered intensity increases with time and eventually saturates. For early times the linear Cahn-Hilliard-Cook (CHC) theory can be used to describe the time evolution of the scattered intensity. From this analysis we found that the growth rate R(q) is linearly dependent on q 2 , in agreement with mean-field theoretical predictions. However the Onsager transport coefficient Λ(q)∼q -4 , which is stronger than the q dependence predicted by the mean-field theory. We found that the growth rate R(q)>0, even though the wave numbers q probed by SAXS are greater than √ (2) q m where q m is the position of the peak of S(q,t), also in agreement with the mean-field predictions for a deep quench. We have also examined the range of validity of the linear CHC theory, and found that its breakdown occurs earlier at higher wave numbers. At later times, a pinning of the structure was observed. The relaxation to a final, microphase-separated morphology is faster and occurs earlier at the highest wave numbers, which probe length scales comparable to the average distance between crosslinks. copyright 1999 The American Physical Society

  3. Using resonant x-ray scattering to determine how structure controls the charge generation process in PCPDTBT:PC70BM solar cells

    Science.gov (United States)

    Pope, Michael; Waldrip, Matthew; Ferron, Thomas; Collins, Brian

    Increased solar power conversion efficiencies to 12% in bulk heterojunction organic photovoltaics (OPVs) continue to brighten their prospects as an economically viable source of solar energy. It is known that OPV performance can be enhanced through processing additives that change the nanostructure. We track these critical structure-property relationships in the OPV system PCPDTBT:PC70BM while varying the amount of DIO additive. Resonant Soft X-ray Scattering reveals domain purity, domain size, and molecular orientation to highlight the system's complex dependence on DIO concentration. We will show the effect the resulting structure has on charge generation and recombination via in-situ transient and steady state optoelectronic measurements. By measuring structure, excited state dynamics and device performance all on the same sample enables direct relationships to be measured. We show that the appropriate balance of crystallinity, domain size and domain purity are important for optimized excited state dynamics and device performance.

  4. Introducing a New Capability at SSRL: Resonant Soft X-ray Scattering

    Science.gov (United States)

    Lee, Jun-Sik; Jang, Hoyoung; Lu, Donghui; Kao, Chi-Chang

    Stanford Synchrotron Radiation Lightsource (SSRL) at SLAC recently developed a setup for the resonant soft x-ray scattering (RSXS). In general, the RSXS technique uniquely probes not only structural information, but also chemical specific information. This is because this technique can explore the spatial periodicities of charge, orbital, spin, and lattice with spectroscopic aspect. Moreover, the soft x-ray range is particularly relevant for a study of soft materials as it covers the K-edge of C, N, F, and O, as well as the L-edges of transition metals and M-edges of rare-earth elements. Hence, the RSXS capability has been regarded as a very powerful technique for investigating the intrinsic properties of materials such as quantum- and energy-materials. The RSXS capability at the SSRL composes of in-vacuum 4-circle diffractometer. There are also the fully motorized sample-motion manipulations. Also, the sample can be cooled down to 25 K via the liquid helium. This capability has been installed at BL 13-3, where the photon source is from elliptically polarized undulator (EPU). Covering the photon energies is from 230 eV to 1400 eV. Furthermore, this EPU system offers more degree of freedoms for controlling x-ray polarizations (linear and circular). Using the advance of controlling x-ray polarization, we can also investigate a morphology effect of local domain/grain in materials. The detailed introduction of the RSXS end-station and several results will be touched in this poster presentation.

  5. PREFACE: REXS 2013 - Workshop on Resonant Elastic X-ray Scattering in Condensed Matter

    Science.gov (United States)

    Beutier, G.; Mazzoli, C.; Yakhou, F.; Brown, S. D.; Bombardi, A.; Collins, S. P.

    2014-05-01

    The aim of this workshop was to bring together experts in experimental and theoretical aspects of resonant elastic x-ray scattering, along with researchers who are new to the field, to discuss important recent results and the fundamentals of the technique. The meeting was a great success, with the first day dedicated to students and new researchers in the field, who received introductory lectures and tutorials. All conference delegates were invited either to make an oral presentation or to present a poster, accompanied by a short talk. The first two papers selected for the REXS13 proceedings (Grenier & Joly and Helliwell) give a basic background to the theory of REXS and applications across a wide range of scientific areas. The remainder of the papers report on some of the latest scientific results obtained by applying the REXS technique to contemporary problems in condensed matter, materials and x-ray physics. It is hoped that these proceedings provide a snapshot of the current status of a vibrant and diverse scientific technique that will be of value not just to those who attended the workshop but also to any other reader with an interest in the subject. Local Scientific Committee REXS13 International Scientific Advisory Committee M Altarelli, European XFEL, Germany F de Bergevin, European Synchrotron Radiation Facility, France J Garcia-Ruiz, Universidad de Zaragoza, Spain A I Goldman, Iowa State University, USA M Goldmann, Institut Nanosciences, France T Schulli, European Synchrotron Radiation Facility, France C R Natoli, Laboratori Nazionali de Frascati, Italy G Materlik, Diamond Light Source, UK L Paolasini, European Synchrotron Radiation Facility, France U Staub, Paul Scherrer Institut, Switzerland K Finkelstein, Cornell University, USA Y Murakami, Photon Factory, Japan REXS13 Local Scientific Committee G Beutier, CNRS Grenoble, France C Mazzoli, Politecnico di Milano, Italy F Yakhou, European Synchrotron Radiation Facility, France S D Brown, XMaS UK CRG

  6. Calculation of accurate small angle X-ray scattering curves from coarse-grained protein models

    Directory of Open Access Journals (Sweden)

    Stovgaard Kasper

    2010-08-01

    Full Text Available Abstract Background Genome sequencing projects have expanded the gap between the amount of known protein sequences and structures. The limitations of current high resolution structure determination methods make it unlikely that this gap will disappear in the near future. Small angle X-ray scattering (SAXS is an established low resolution method for routinely determining the structure of proteins in solution. The purpose of this study is to develop a method for the efficient calculation of accurate SAXS curves from coarse-grained protein models. Such a method can for example be used to construct a likelihood function, which is paramount for structure determination based on statistical inference. Results We present a method for the efficient calculation of accurate SAXS curves based on the Debye formula and a set of scattering form factors for dummy atom representations of amino acids. Such a method avoids the computationally costly iteration over all atoms. We estimated the form factors using generated data from a set of high quality protein structures. No ad hoc scaling or correction factors are applied in the calculation of the curves. Two coarse-grained representations of protein structure were investigated; two scattering bodies per amino acid led to significantly better results than a single scattering body. Conclusion We show that the obtained point estimates allow the calculation of accurate SAXS curves from coarse-grained protein models. The resulting curves are on par with the current state-of-the-art program CRYSOL, which requires full atomic detail. Our method was also comparable to CRYSOL in recognizing native structures among native-like decoys. As a proof-of-concept, we combined the coarse-grained Debye calculation with a previously described probabilistic model of protein structure, TorusDBN. This resulted in a significant improvement in the decoy recognition performance. In conclusion, the presented method shows great promise for

  7. X-ray scatter correction method for dedicated breast computed tomography: improvements and initial patient testing

    International Nuclear Information System (INIS)

    Ramamurthy, Senthil; D’Orsi, Carl J; Sechopoulos, Ioannis

    2016-01-01

    A previously proposed x-ray scatter correction method for dedicated breast computed tomography was further developed and implemented so as to allow for initial patient testing. The method involves the acquisition of a complete second set of breast CT projections covering 360° with a perforated tungsten plate in the path of the x-ray beam. To make patient testing feasible, a wirelessly controlled electronic positioner for the tungsten plate was designed and added to a breast CT system. Other improvements to the algorithm were implemented, including automated exclusion of non-valid primary estimate points and the use of a different approximation method to estimate the full scatter signal. To evaluate the effectiveness of the algorithm, evaluation of the resulting image quality was performed with a breast phantom and with nine patient images. The improvements in the algorithm resulted in the avoidance of introduction of artifacts, especially at the object borders, which was an issue in the previous implementation in some cases. Both contrast, in terms of signal difference and signal difference-to-noise ratio were improved with the proposed method, as opposed to with the correction algorithm incorporated in the system, which does not recover contrast. Patient image evaluation also showed enhanced contrast, better cupping correction, and more consistent voxel values for the different tissues. The algorithm also reduces artifacts present in reconstructions of non-regularly shaped breasts. With the implemented hardware and software improvements, the proposed method can be reliably used during patient breast CT imaging, resulting in improvement of image quality, no introduction of artifacts, and in some cases reduction of artifacts already present. The impact of the algorithm on actual clinical performance for detection, diagnosis and other clinical tasks in breast imaging remains to be evaluated. (paper)

  8. Alamethicin in lipid bilayers: combined use of X-ray scattering and MD simulations.

    Science.gov (United States)

    Pan, Jianjun; Tieleman, D Peter; Nagle, John F; Kucerka, Norbert; Tristram-Nagle, Stephanie

    2009-06-01

    We study fully hydrated bilayers of two di-monounsaturated phospholipids diC18:1PC (DOPC) and diC22:1PC with varying amounts of alamethicin (Alm). We combine the use of X-ray diffuse scattering and molecular dynamics simulations to determine the orientation of alamethicin in model lipids. Comparison of the experimental and simulated form factors shows that Alm helices are inserted transmembrane at high humidity and high concentrations, in agreement with earlier results. The X-ray scattering data and the MD simulations agree that membrane thickness changes very little up to 1/10 Alm/DOPC. In contrast, the X-ray data indicate that the thicker diC22:1PC membrane thins with added Alm, a total decrease in thickness of 4 A at 1/10 Alm/diC22:1PC. The different effect of Alm on the thickness changes of the two bilayers is consistent with Alm having a hydrophobic thickness close to the hydrophobic thickness of 27 A for DOPC; Alm is then mismatched with the 7 A thicker diC22:1PC bilayer. The X-ray data indicate that Alm decreases the bending modulus (K(C)) by a factor of approximately 2 in DOPC and a factor of approximately 10 in diC22:1PC membranes (P/L approximately 1/10). The van der Waals and fluctuational interactions between bilayers are also evaluated through determination of the anisotropic B compressibility modulus.

  9. Fast electron and X-ray scattering as a tool to study target's structure

    International Nuclear Information System (INIS)

    Amusia, M.Ya.

    2007-01-01

    We concentrate on several relatively new aspects of the study of fast electron and X-ray scattering by atoms and atom-like objects, namely endohedral atoms and fullerenes. However, main attention is given to fast charge particle scattering. We show that the corresponding cross-sections, being expressed via so-called generalized oscillator strengths (GOS), give information on the electronic structure of the target and on the role of electron correlations in it. We consider what sort of information became available when analyzing the dependence of GOS upon their multipolarity, transferred momentum q and energy ω. To obtain theoretical results, we employ both the one-electron Hartree-Fock approximation and account for the multi-electron correlation in the target, using the random phase approximation with exchange. We demonstrate the role of non-dipole corrections in the small-angle fast-electron inelastic scattering. There dipole contribution dominates while non-dipole corrections can be considerably and controllably enhanced as compared to the case of low and medium energy photoionization. We show also that analyses of GOS for discrete level excitations permit to clarify their multipolarity. The results of calculations of Compton excitation and ionization cross-sections are presented. Attention is given to cooperative effects in inelastic fast electron-atom scattering that results in directed motion of the secondary electrons, a phenomenon that is similar to 'drag currents' in photoionization. We demonstrate how one should derive GOS for endohedral atoms, e.g. A-C 60 and what is the additional information that can be obtained from corresponding GOS. Most of discussions are illustrated by the results of concrete calculations

  10. High-energy x-ray scattering quantification of in-situ-loading-related strain gradients spanning the dentinoenamel junction (DEJ) in bovine tooth specimens

    International Nuclear Information System (INIS)

    Almer, J.D.; Stock, S.R.

    2010-01-01

    High energy X-ray scattering (80.7keV photons) at station 1-ID of the Advanced Photon Source quantified internal strains as a function of applied stress in mature bovine tooth. These strains were mapped from dentin through the dentinoenamel junction (DEJ) into enamel as a function of applied compressive stress in two small parallelepiped specimens. One specimen was loaded perpendicular to the DEJ and the second parallel to the DEJ. Internal strains in enamel and dentin increased and, as expected from the relative values of the Young's modulus, the observed strains were much higher in dentin than in enamel. Large strain gradients were observed across the DEJ, and the data suggest that the mantle dentin-DEJ-aprismatic enamel structure may shield the near-surface volume of the enamel from large strains. In the enamel, drops in internal strain for applied stresses above 40MPa also suggest that this structure had cracked.

  11. The atomic scale structure of CXV carbon: wide-angle x-ray scattering and modeling studies.

    Science.gov (United States)

    Hawelek, L; Brodka, A; Dore, J C; Honkimaki, V; Burian, A

    2013-11-13

    The disordered structure of commercially available CXV activated carbon produced from finely powdered wood-based carbon has been studied using the wide-angle x-ray scattering technique, molecular dynamics and density functional theory simulations. The x-ray scattering data has been converted to the real space representation in the form of the pair correlation function via the Fourier transform. Geometry optimizations using classical molecular dynamics based on the reactive empirical bond order potential and density functional theory at the B3LYP/6-31g* level have been performed to generate nanoscale models of CXV carbon consistent with the experimental data. The final model of the structure comprises four chain-like and buckled graphitic layers containing a small percentage of four-fold coordinated atoms (sp(3) defects) in each layer. The presence of non-hexagonal rings in the atomic arrangement has been also considered.

  12. Identifying low and high density amorphous phases during zeolite amorphisation using small and wide angle X-ray scattering

    International Nuclear Information System (INIS)

    Meneau, F.; Greaves, G.N.

    2005-01-01

    In situ experiments following the thermal amorphisation of zeolites reveal massive increases in small angle X-ray scattering (SAXS), persisting well beyond the stage where wide angle X-ray scattering (WAXS) can detect that any crystalline phase is present. This heterogeneity in the amorphised phase is attributed to the transition from a low density amorphous phase (LDA) to a high density amorphous phase (HDA) at the glass transition. The fractions of zeolite, LDA and HDA phases obtained from SAXS analysis are discussed in the context of non-linear changes detected in 29 Si solid state NMR during zeolite amorphisation. Whilst the HDA phase is chemically disordered, the LDA phase exhibits much of the Al-Si ordering present in the starting zeolite. These findings are considered in the context of perfect glasses predicted to occur when super strong liquids are supercooled

  13. Resonant X-Ray Scattering and the jeff=1/2 Electronic Ground State in Iridate Perovskites

    DEFF Research Database (Denmark)

    Sala, M. Moretti; Boseggia, S.; McMorrow, Desmond Francis

    2014-01-01

    The resonant x-ray scattering (magnetic elastic, RXMS, and inelastic, RIXS) of Ir4+ at the L-2,L-3 edges relevant to spin-orbit Mott insulators A(n+1) Ir(n)O3(n+1) (A = Sr, Ba, etc.) are calculated using a single-ion model which treats the spin-orbit and tetragonal crystal-field terms on an equal...

  14. Electron Dynamics in the Core-Excited CS 2 Molecule Revealed through Resonant Inelastic X-Ray Scattering Spectroscopy

    OpenAIRE

    Marchenko , T; Carniato , S; Journel , L; Guillemin , R; Kawerk , E; Žitnik , M; Kavčič , M; Bučar , K; Bohinc , R; Petric , M; Vaz Da Cruz , V; Gel 'mukhanov , F; Simon , Marielle

    2015-01-01

    International audience; We present an experimental and theoretical study of resonant inelastic x-ray scattering (RIXS) in the carbon disulphide CS 2 molecule near the sulfur K-absorption edge. We observe a strong evolution of the RIXS spectral profile with the excitation energy tuned below the lowest unoccupied molecular orbital (LUMO) absorption resonance. The reason for this is twofold. Reducing the photon energy in the vicinity of the LUMO absorption resonance leads to a relative suppressi...

  15. Pepsi-SAXS : an adaptive method for rapid and accurate computation of small-angle X-ray scattering profiles

    OpenAIRE

    Grudinin , Sergei; Garkavenko , Maria; Kazennov , Andrei

    2017-01-01

    International audience; A new method called Pepsi-SAXS is presented that calculates small-angle X-ray scattering profiles from atomistic models. The method is based on the multipole expansion scheme and is significantly faster compared with other tested methods. In particular, using the Nyquist–Shannon–Kotelnikov sampling theorem, the multipole expansion order is adapted to the size of the model and the resolution of the experimental data. It is argued that by using the adaptive expansion ord...

  16. Analysis of the aggregation structure from amphiphilic block copolymers in solutions by small-angle x-ray scattering

    CERN Document Server

    Rong Li Xia; Wang Jun; Wei Liu He; Li Fu Mian; Li Zi Chen

    2002-01-01

    The aggregation structure of polystyrene-p vinyl benzoic amphiphilic block copolymers which were prepared in different conditions was investigated by synchrotron radiation small-angle x-ray scattering (SAXS). The micelle was self-assembled in selective solvents of the block copolymers. Authors' results demonstrate that the structure of the micelle depends on the factors, such as the composition of the copolymers, the nature of the solvent and the concentration of the solution

  17. Diffuse x-ray scattering and transmission electron microscopy study of defects in antimony-implanted silicon

    Science.gov (United States)

    Takamura, Y.; Marshall, A. F.; Mehta, A.; Arthur, J.; Griffin, P. B.; Plummer, J. D.; Patel, J. R.

    2004-04-01

    Ion implantation followed by laser annealing has been used to create supersaturated and electrically active concentrations of antimony in silicon. Upon subsequent thermal annealing, however, these metastable dopants deactivate towards the equilibrium solubility limit. In this work, the formation of inactive antimony structures has been studied with grazing incidence diffuse x-ray scattering, and transmission electron microscopy, and the results are correlated to previous high-resolution x-ray diffraction data. We find that at a concentration of 6.0×1020 cm-3, small, incoherent clusters of radius 3-4 Å form during annealing at 900 °C. At a higher concentration of 2.2×1021 cm-3, deactivation at 600 °C occurs through the formation of small, antimony aggregates and antimony precipitates. The size of these precipitates from diffuse x-ray scattering is roughly 15 Å in radius for anneal times from 15 to 180 seconds. This value is consistent with the features observed in high-resolution and mass contrast transmission electron microscopy images. The coherent nature of the aggregates and precipitates causes the expansion of the surrounding silicon matrix as the deactivation progresses. In addition, the sensitivity of the diffuse x-ray scattering technique has allowed us to detect the presence of small clusters of radius ˜2 Å in unprocessed Czochralski silicon wafers. These defects are not observed in floating zone silicon wafers, and are tentatively attributed to thermal donors.

  18. Difference in x-ray scattering between metallic and non-metallic liquids due to conduction electrons

    International Nuclear Information System (INIS)

    Chihara, Junzo

    1987-01-01

    X-ray scattered intensity from a liquid metal as an electron-ion mixture is described using the structure factors, which are exactly expressed in terms of the static and dynamic direct correlation functions. This intensity for a metal is shown to differ from the usual scattered intensity from a non-metal in two points: the atomic form factor and the incoherent (Compton) scattering factor. It is shown that the valence electron form factor, which constitutes the atomic form factor in a liquid metal, leads to a determination of the electron-electron and electron-ion structure factors by combining the ionic structure factor. It is also shown that a part of the electron structure factor, which appears as the incoherent x-ray scattering, is usually approximated as the electron structure factor of the jellium model in the case of a simple metal. As a by-product, the x-ray scattered intensity from a crystalline metal and the inelastic scattering from a liquid metal are given by taking account of the presence of conduction electrons. In this way, we clarify some confusion which appeared in the proposal by Egelstaff et al for extracting the electron-electron correlation function in a metal from x-ray and neutron scattering experiments. A procedure to extract the electron-electron and electron-ion structure factors in a liquid metal is proposed on the basis of formula for scattered intensity derived here. (author)

  19. High-resolution resonant magnetic x-ray scattering on TbNi2B2C: Determination of the modulation wave vector in the orthorhombic phase

    International Nuclear Information System (INIS)

    Song, C.; Wermeille, D.; Goldman, A. I.; Canfield, P. C.; Rhee, J. Y.; Harmon, B. N.

    2001-01-01

    Resonant magnetic x-ray scattering measurements have been performed on a single crystal of TbNi 2 B 2 C to uniquely determine the modulation wave vector in the low-temperature orthorhombic phase. Below the transition temperature of 14.4(±0.1)K, two magnetic satellite peaks develop, centered on (h00) orth charge reflections. Our study shows that the longitudinal modulation of the magnetic moment is along the longer basal plane axes of the orthorhombic phase. Power law fits to the temperature dependence of the structural distortion, a/b-1, and the magnetic scattering intensity result in the same exponent, β, and transition temperature evidencing explicitly that the structural phase transition is magneto-elastic in origin

  20. Probing single magnon excitations in Sr2IrO4 using O K-edge resonant inelastic x-ray scattering

    International Nuclear Information System (INIS)

    Liu, X; Ding, H; Dean, M P M; Yin, W G; Hill, J P; Liu, J; Ramesh, R; Chiuzbăian, S G; Jaouen, N; Nicolaou, A; Serrao, C Rayan

    2015-01-01

    Resonant inelastic x-ray scattering (RIXS) at the L-edge of transition metal elements is now commonly used to probe single magnon excitations. Here we show that single magnon excitations can also be measured with RIXS at the K-edge of the surrounding ligand atoms when the center heavy metal elements have strong spin–orbit coupling. This is demonstrated with oxygen K-edge RIXS experiments on the perovskite Sr 2 IrO 4 , where low energy peaks from single magnon excitations were observed. This new application of RIXS has excellent potential to be applied to a wide range of magnetic systems based on heavy elements, for which the L-edge RIXS energy resolution in the hard x-ray region is usually poor. (fast track communication)

  1. Core–Shell Structure and Aggregation Number of Micelles Composed of Amphiphilic Block Copolymers and Amphiphilic Heterografted Polymer Brushes Determined by Small-Angle X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Szymusiak, Magdalena; Kalkowski, Joseph; Luo, Hanying; Donovan, Alexander J.; Zhang, Pin; Liu, Chang; Shang, Weifeng; Irving, Thomas; Herrera-Alonso, Margarita; Liu, Ying (JHU); (IIT); (UIC)

    2017-08-31

    A large group of functional nanomaterials employed in biomedical applications, including targeted drug delivery, relies on amphiphilic polymers to encapsulate therapeutic payloads via self-assembly processes. Knowledge of the micelle structures will provide critical insights into design of polymeric drug delivery systems. Core–shell micelles composed of linear diblock copolymers poly(ethylene glycol)-b-poly(caprolactone) (PEG-b-PCL), poly(ethylene oxide)-b-poly(lactic acid) (PEG-b-PLA), as well as a heterografted brush consisting of a poly(glycidyl methacrylate) backbone with PEG and PLA branches (PGMA-g-PEG/PLA) were characterized by dynamic light scattering (DLS) and small-angle X-ray scattering (SAXS) measurements to gain structural information regarding the particle morphology, core–shell size, and aggregation number. The structural information at this quasi-equilibrium state can also be used as a reference when studying the kinetics of polymer micellization.

  2. Core–Shell Structure and Aggregation Number of Micelles Composed of Amphiphilic Block Copolymers and Amphiphilic Heterografted Polymer Brushes Determined by Small-Angle X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Szymusiak, Magdalena [Department; Kalkowski, Joseph [Department; Luo, Hanying [Department; Donovan, Alexander J. [Department; Zhang, Pin [Department; Liu, Chang [Department; Shang, Weifeng [Department; Irving, Thomas [Department; Herrera-Alonso, Margarita [Department; Liu, Ying [Department; Department

    2017-08-16

    A large group of functional nanomaterials employed in biomedical applications, including targeted drug delivery, relies on amphiphilic polymers to encapsulate therapeutic payloads via self-assembly processes. Knowledge of the micelle structures will provide critical insights into design of polymeric drug delivery systems. Core–shell micelles composed of linear diblock copolymers poly(ethylene glycol)-b-poly(caprolactone) (PEG-b-PCL), poly(ethylene oxide)-b-poly(lactic acid) (PEG-b-PLA), as well as a heterografted brush consisting of a poly(glycidyl methacrylate) backbone with PEG and PLA branches (PGMA-g-PEG/PLA) were characterized by dynamic light scattering (DLS) and small-angle X-ray scattering (SAXS) measurements to gain structural information regarding the particle morphology, core–shell size, and aggregation number. The structural information at this quasi-equilibrium state can also be used as a reference when studying the kinetics of polymer micellization.

  3. BioXTAS RAW, a software program for high-throughput automated small-angle X-ray scattering data reduction and preliminary analysis

    DEFF Research Database (Denmark)

    Nielsen, S.S.; Toft, K.N.; Snakenborg, Detlef

    2009-01-01

    A fully open source software program for automated two-dimensional and one-dimensional data reduction and preliminary analysis of isotropic small-angle X-ray scattering (SAXS) data is presented. The program is freely distributed, following the open-source philosophy, and does not rely on any...... commercial software packages. BioXTAS RAW is a fully automated program that, via an online feature, reads raw two-dimensional SAXS detector output files and processes and plots data as the data files are created during measurement sessions. The software handles all steps in the data reduction. This includes...... mask creation, radial averaging, error bar calculation, artifact removal, normalization and q calibration. Further data reduction such as background subtraction and absolute intensity scaling is fast and easy via the graphical user interface. BioXTAS RAW also provides preliminary analysis of one...

  4. Note: Comparison of grazing incidence small angle x-ray scattering of a titania sponge structure at the beamlines BW4 (DORIS III) and P03 (PETRA III)

    International Nuclear Information System (INIS)

    Rawolle, M.; Körstgens, V.; Ruderer, M. A.; Metwalli, E.; Guo, S.; Müller-Buschbaum, P.; Herzog, G.; Benecke, G.; Schwartzkopf, M.; Buffet, A.; Perlich, J.; Roth, S. V.

    2012-01-01

    Grazing incidence small angle x-ray scattering (GISAXS) is a powerful technique for morphology investigation of nanostructured thin films. GISAXS measurements at the newly installed P03 beamline at the storage ring PETRA III in Hamburg, Germany, are compared to the GISAXS data from the beamline BW4 at the storage ring DORIS III, which had been used extensively for GISAXS investigations in the past. As an example, a titania thin film sponge structure is investigated. Compared to BW4, at beamline P03 the resolution of larger structures is slightly improved and a higher incident flux leads to a factor of 750 in scattered intensity. Therefore, the acquisition time in GISAXS geometry is reduced significantly at beamline P03.

  5. Investigation of the topological shape of bovine serum albumin in solution by small-angle x-ray scattering at Beijing synchrotron radiation facility

    International Nuclear Information System (INIS)

    Dong Shuqiang; Chen Ximeng; Li Liqin; Liu Peng; Dong Yuhui

    2008-01-01

    This paper reports that at a newly constructed small-angle x-ray scattering station of Beijing Synchrotron Radiation Facility, the topological shape of ligand-free bovine serum albumin in solution has been investigated. An appropriate scattering curve is obtained and the calculated value of the gyration radius is 31.2ű0.25A (1Å=0.1 nm) which is coincident with other ones' results. It finds that the low-resolution structure models obtained by making use of ab initio reconstruction methods are fitting the crystal structure of human serum albumin very well. All of these results perform the potential of the beamline to apply to structural biology studies. The characteristics, the defects, and the improving measures of the station in future are also discussed. (condensed matter: structure, thermal and mechanical properties)

  6. Small-angle X-ray scattering tensor tomography: model of the three-dimensional reciprocal-space map, reconstruction algorithm and angular sampling requirements.

    Science.gov (United States)

    Liebi, Marianne; Georgiadis, Marios; Kohlbrecher, Joachim; Holler, Mirko; Raabe, Jörg; Usov, Ivan; Menzel, Andreas; Schneider, Philipp; Bunk, Oliver; Guizar-Sicairos, Manuel

    2018-01-01

    Small-angle X-ray scattering tensor tomography, which allows reconstruction of the local three-dimensional reciprocal-space map within a three-dimensional sample as introduced by Liebi et al. [Nature (2015), 527, 349-352], is described in more detail with regard to the mathematical framework and the optimization algorithm. For the case of trabecular bone samples from vertebrae it is shown that the model of the three-dimensional reciprocal-space map using spherical harmonics can adequately describe the measured data. The method enables the determination of nanostructure orientation and degree of orientation as demonstrated previously in a single momentum transfer q range. This article presents a reconstruction of the complete reciprocal-space map for the case of bone over extended ranges of q. In addition, it is shown that uniform angular sampling and advanced regularization strategies help to reduce the amount of data required.

  7. Power spectrum analysis of the x-ray scatter signal in mammography and breast tomosynthesis projections.

    Science.gov (United States)

    Sechopoulos, Ioannis; Bliznakova, Kristina; Fei, Baowei

    2013-10-01

    power spectrum reflected a fast drop-off with increasing spatial frequency, with a reduction of four orders of magnitude by 0.1 lp/mm. The β values for the scatter signal were 6.14 and 6.39 for the 0° and 30° projections, respectively. Although the low-frequency characteristics of scatter in mammography and breast tomosynthesis were known, a quantitative analysis of the frequency domain characteristics of this signal was needed in order to optimize previously proposed software-based x-ray scatter reduction algorithms for these imaging modalities.

  8. Topology and temperature dependence of the diffuse X-ray scattering in Na0.5Bi0.5TiO3 ferroelectric single crystals.

    Science.gov (United States)

    Gorfman, Semën; Keeble, Dean S; Bombardi, Alessandro; Thomas, Pam A

    2015-10-01

    The results of high-resolution measurements of the diffuse X-ray scattering produced by a perovskite-based Na 0.5 Bi 0.5 TiO 3 ferroelectric single crystal between 40 and 620 K are reported. The study was designed as an attempt to resolve numerous controversies regarding the average structure of Na 0.5 Bi 0.5 TiO 3 , such as the mechanism of the phase transitions between the tetragonal, P 4 bm , and rhombohedral | monoclinic, R 3 c  |  Cc , space groups and the correlation between structural changes and macroscopic physical properties. The starting point was to search for any transformations of structural disorder in the temperature range of thermal depoling (420-480 K), where the average structure is known to remain unchanged. The intensity distribution around the {032} pseudocubic reflection was collected using a PILATUS 100K detector at the I16 beamline of the Diamond Light Source (UK). The data revealed previously unknown features of the diffuse scattering, including a system of dual asymmetric L-shaped diffuse scattering streaks. The topology, temperature dependence, and relationship between Bragg and diffuse intensities suggest the presence of complex microstructure in the low-temperature R 3 c  |  Cc phase. This microstructure may be formed by the persistence of the higher-temperature P 4 bm phase, built into a lower-temperature R 3 c  |  Cc matrix, accompanied by the related long-range strain fields. Finally, it is shown that a correlation between the temperature dependence of the X-ray scattering features and the temperature regime of thermal depoling is present.

  9. Calculation of X-ray scattering curves and electron distance distribution functions of biological macromolecules in solution using the PROTEIN DATA BANK

    International Nuclear Information System (INIS)

    Mueller, J.J.; Friedrichowicz, E.; Nothnagel, A.; Wunderlich, T.; Ziehlsdorf, E.; Damaschun, G.

    1983-01-01

    The wide angle X-ray scattering curve, the electron distance distribution function and the solvent excluded volume of a macromolecule in solution are calculated from the atomic coordinates contained in the PROTEIN DATA BANK. The structures and the projections of the excluded volumes are depicted using molecule graphic routines. The described computer programs are used to determine the three-dimensional structure of macromolecules in solution from wide angle X-ray scattering data. (author)

  10. Water structure as a function of temperature from X-ray scattering experiments and ab initio molecular dynamics

    International Nuclear Information System (INIS)

    Hura, Greg; Russo, Daniela; Glaeser, Robert M.; Head-Gordon, Teresa; Krack, Matthias; Parrinello, Michele

    2003-01-01

    We present high-quality X-ray scattering experiments on pure water taken over a temperature range of 2 to 77 C using a synchrotron beam line at the advanced light source (ALS) at Lawrence Berkeley National Laboratory. The ALS X-ray scattering intensities are qualitatively different in trend of maximum intensity over this temperature range compared to older X-ray experiments. While the common procedure is to report both the intensity curve and radial distribution function(s), the proper extraction of the real-space pair correlation functions from the experimental scattering is very difficult due to uncertainty introduced in the experimental corrections, the proper weighting of OO, OH, and HH contributions, and numerical problems of Fourier transforming truncated data in Q-space. Instead, we consider the direct calculation of X-ray scattering spectra using electron densities derived from density functional theory based on real-space configurations generated with classical water models. The simulation of the experimental intensity is therefore definitive for determining radial distribution functions over a smaller Q-range. We find that the TIP4P, TIP5P and polarizable TIP4P-Pol2 water models, with DFT-LDA densities, show very good agreement with the experimental intensities, and TIP4P-Pol2 in particular shows quantitative agreement over the full temperature range. The resulting radial distribution functions from TIP4P-Pol2 provide the current best benchmarks for real-space water structure over the biologically relevant temperature range studied here

  11. Myelin structure is a key difference in the x-ray scattering signature between meningioma, schwannoma and glioblastoma multiforme

    International Nuclear Information System (INIS)

    Falzon, G; Pearson, S; Murison, R; Hall, C; Siu, K; Round, A; Schueltke, E; Kaye, A H; Lewis, R

    2007-01-01

    Small angle x-ray scattering (SAXS) patterns of benign and malignant brain tumour tissue were examined. Independent component analysis was used to find a feature set representing the images collected. A set of coefficients was then used to describe each image, which allowed the use of the statistical technique of flexible discriminant analysis to discover a hidden order in the data set. The key difference was found to be in the intensity and spectral content of the second and fourth order myelin scattering peaks. This has clearly demonstrated that significant differences in the structure of myelin exist in the highly malignant glioblastoma multiforme as opposed to the benign: meningioma and schwannoma

  12. Laser ablation and injection moulding as techniques for producing micro channels compatible with Small Angle X-Ray Scattering

    DEFF Research Database (Denmark)

    Haider, R.; Marmiroli, B.; Gavalas, I.

    2018-01-01

    Microfluidic mixing is an important means for in-situ sample preparation and handling while Small Angle X-Ray Scattering (SAXS) is a proven tool for characterising (macro-)molecular structures. In combination those two techniques enable investigations of fast reactions with high time resolution......, the requirement for low scattering especially limits the techniques suitable for producing the mixer, as the fabrication process can induce molecular orientations and stresses that can adversely influence the scattering signal. Not only is it important to find a production method that results in a device with low...

  13. In situ multi-axial loading frame to probe elastomers using X-ray scattering.

    Science.gov (United States)

    Pannier, Yannick; Proudhon, Henry; Mocuta, Cristian; Thiaudière, Dominique; Cantournet, Sabine

    2011-11-01

    An in situ tensile-shear loading device has been designed to study elastomer crystallization using synchrotron X-ray scattering at the Synchrotron Soleil on the DiffAbs beamline. Elastomer tape specimens of thickness 2 mm can be elongated by up to 500% in the longitudinal direction and sheared by up to 200% in the transverse direction. The device is fully automated and plugged into the TANGO control system of the beamline allowing synchronization between acquisition and loading sequences. Experimental results revealing the evolution of crystallization peaks under load are presented for several tension/shear loading sequences.

  14. High resolution X-ray scattering techniques for studying the sliding CDWS distortions, in NbSe sub 3

    CERN Document Server

    Rideau, D; Currat, R; Requardt, H; Nad, F Y; Lorenzo, J E; Brazovskii, S; Detlefs, C; Grübel, G

    2001-01-01

    The phase gradient in a sliding-charge density wave (CDW), which is observable as a longitudinal shift, q propor to partial deriv phi/partial deriv x, of the CDW satellite peak position, is due to the conversion free-electrons CDW-condensate, at the current electrodes. Using high resolution X-ray scattering techniques and time-resolved techniques, we monitor, on thin NbSe sub 3 whiskers, the shift, q(x), and its relaxation, q(t), upon switching off the current.

  15. Order in poly(di-n-alkyl itaconate)s revealed by X-ray scattering experiments

    International Nuclear Information System (INIS)

    Holmes, P.F.; Arrighi, V.; McEwen, I.J.; Qian, H.; Terrill, N.J.

    2003-01-01

    The effects of both blending and copolymersiation on local ordering in poly(di-n-alkyl itaconate)s is investigated, as a function of side chain length, using small-angle X-ray scattering. Preliminary results show that local ordering is unaffected by blending in these immiscible materials, however copolymerisation leads to different behaviour. For short side chains the characteristic distance varies smoothly with copolymer composition, but with longer side chains the characteristic separations found for the homopolymers are observed, and these remain unchanged with composition

  16. Order in poly(di-n-alkyl itaconate)s revealed by X-ray scattering experiments

    Energy Technology Data Exchange (ETDEWEB)

    Holmes, P.F.; Arrighi, V. E-mail: v.arrighi@hw.ac.uk; McEwen, I.J.; Qian, H.; Terrill, N.J

    2003-01-01

    The effects of both blending and copolymersiation on local ordering in poly(di-n-alkyl itaconate)s is investigated, as a function of side chain length, using small-angle X-ray scattering. Preliminary results show that local ordering is unaffected by blending in these immiscible materials, however copolymerisation leads to different behaviour. For short side chains the characteristic distance varies smoothly with copolymer composition, but with longer side chains the characteristic separations found for the homopolymers are observed, and these remain unchanged with composition.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-03-13

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

  18. Quadrupolar frustration in shastry-sutherland lattice of DyB4 studied by resonant x-ray scattering

    International Nuclear Information System (INIS)

    Okuyama, Daisuke; Matsumura, Takeshi; Nakao, Hironori; Murakami, Youichi

    2005-01-01

    We have observed geometrical frustration of quadrupolar and magnetic moments in dysprosium tetraboride, DyB 4 , where the rare-earth sites form a Shastry-Sutherland lattice. Resonant X-ray scattering at the L III absorption edge of Dy was utilized. Analysis of the energy, polarization, temperature, and azimuthal-angle dependences of the E1 resonance of the (100) forbidden reflection show that the magnetic and quadrupolar components within the frustrated c plane have a short-range correlation, suggesting that the moments are fluctuating. In contrast, the basic antiferromagnetic component along the c-axis has a long-range order. (author)

  19. Antibodies under pressure: A Small-Angle X-ray Scattering study of Immunoglobulin G under high hydrostatic pressure.

    Science.gov (United States)

    König, Nico; Paulus, Michael; Julius, Karin; Schulze, Julian; Voetz, Matthias; Tolan, Metin

    2017-12-01

    In the present work two subclasses of the human antibody Immunoglobulin G (IgG) have been investigated by Small-Angle X-ray Scattering under high hydrostatic pressures up to 5kbar. It is shown that IgG adopts a symmetric T-shape in solution which differs significantly from available crystal structures. Moreover, high-pressure experiments verify the high stability of the IgG molecule. It is not unfolded by hydrostatic pressures of up to 5kbar but a slight increase of the radius of gyration was observed at elevated pressures. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Electron dynamics in the core-excited CS2 molecule revealed through resonant inelastic x-ray scattering spectroscopy

    International Nuclear Information System (INIS)

    Marchenko, T; Carniato, S; Journel, L; Guillemin, R; Kawerk, E; Simon, M; Žitnik, M; Kavčič, M; Bučar, K; Bohinc, R; Petric, M; Da Cruz, V Vaz; Gel'mukhanov, F

    2015-01-01

    We present an experimental and theoretical study of resonant inelastic x-ray scattering (RIXS) in the CS 2 molecule near the S 1s edge. We show that localization of the S 1s core-hole occurs in CS 2 during the RIXS process due to the orientational dephasing of interference between the waves scattering on the two sulfur atoms. Strong evolution of the RIXS profile with the excitation energy far below the first absorption resonance reflects the onset of electron dynamics triggered by a coherent excitation of multiple electronic states. (paper)

  1. Electron dynamics in the core-excited CS 2 molecule revealed through resonant inelastic x-ray scattering spectroscopy

    OpenAIRE

    Marchenko , T; Carniato , S; Journel , L; Guillemin , R; Kawerk , E; Žitnik , M; Kavčič , M; Bučar , K; Bohinc , R; Petric , M; da Cruz , V Vaz; Gel'mukhanov , F; Simon , Marielle

    2015-01-01

    International audience; We present an experimental and theoretical study of resonant inelastic x-ray scattering (RIXS) in the CS2 molecule near the S 1s edge. We show that localization of the S 1s core-hole occurs in CS2 during the RIXS process due to the orientational dephasing of interference between the waves scattering on the two sulfur atoms. Strong evolution of the RIXS profile with the excitation energy far below the first absorption resonance reflects the onset of electron dynamics tr...

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

    Science.gov (United States)

    Nepal, Prakash; Saldin, D. K.

    2018-05-01

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

  3. X-ray crystal structure and small-angle X-ray scattering of sheep liver sorbitol dehydrogenase

    Energy Technology Data Exchange (ETDEWEB)

    Yennawar, Hemant [Pennsylvania State University, 8 Althouse Laboratory, University Park, PA 16802 (United States); Møller, Magda [Cornell High Energy Synchrotron Source, Ithaca, NY 14853 (United States); University of Copenhagen, DK-2100 Copenhagen (Denmark); Gillilan, Richard [Cornell High Energy Synchrotron Source, Ithaca, NY 14853 (United States); Yennawar, Neela, E-mail: nhy1@psu.edu [Pennsylvania State University, 8 Althouse Laboratory, University Park, PA 16802 (United States)

    2011-05-01

    The X-ray crystal structure and a small-angle X-ray scattering solution structure of sheep liver sorbitol dehydrogenase have been determined. The details of the interactions that enable the tetramer scaffold to be the functional biological unit have been analyzed. The X-ray crystal structure of sheep liver sorbitol dehydrogenase (slSDH) has been determined using the crystal structure of human sorbitol dehydrogenase (hSDH) as a molecular-replacement model. slSDH crystallized in space group I222 with one monomer in the asymmetric unit. A conserved tetramer that superposes well with that seen in hSDH (despite belonging to a different space group) and obeying the 222 crystal symmetry is seen in slSDH. An acetate molecule is bound in the active site, coordinating to the active-site zinc through a water molecule. Glycerol, a substrate of slSDH, also occupies the substrate-binding pocket together with the acetate designed by nature to fit large polyol substrates. The substrate-binding pocket is seen to be in close proximity to the tetramer interface, which explains the need for the structural integrity of the tetramer for enzyme activity. Small-angle X-ray scattering was also used to identify the quaternary structure of the tetramer of slSDH in solution.

  4. Mineral crystal alignment in mineralized fracture callus determined by 3D small-angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Liu Yifei; Manjubala, Inderchand; Fratzl, Peter [Department of Biomaterials, Max Planck Institute of Colloids and Interfaces, 14424 Potsdam (Germany); Roschger, Paul [4th Medical Department, Ludwig Boltzmann Institute of Osteology at Hanusch Hospital of WGKK and AUVA Trauma Centre Meidling, 1140 Vienna (Austria); Schell, Hanna; Duda, Georg N, E-mail: fratzl@mpikg.mpg.d [Julius Wolff Institut and Center for Musculoskeletal Surgery, Charite- University Medicine Berlin, Augustenburger Platz 1, 13353 Berlin (Germany)

    2010-10-01

    Callus tissue formed during bone fracture healing is a mixture of different tissue types as revealed by histological analysis. But the structural characteristics of mineral crystals within the healing callus are not well known. Since two-dimensional (2D) scanning small-angle X-ray scattering (sSAXS) patterns showed that the size and orientation of callus crystals vary both spatially and temporally [1] and 2D electron microscopic analysis implies an anisotropic property of the callus morphology, the mineral crystals within the callus are also expected to vary in size and orientation in 3D. Three-dimensional small-angle X-ray scattering (3D SAXS), which combines 2D SAXS patterns collected at different angles of sample tilting, has been previously applied to investigate bone minerals in horse radius [2] and oim/oim mouse femur/tibia [3]. We implement a similar 3D SAXS method but with a different way of data analysis to gather information on the mineral alignment in fracture callus. With the proposed accurate yet fast assessment of 3D SAXS information, it was shown that the plate shaped mineral particles in the healing callus were aligned in groups with their predominant orientations occurring as a fiber texture.

  5. Mineral crystal alignment in mineralized fracture callus determined by 3D small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Liu Yifei; Manjubala, Inderchand; Fratzl, Peter; Roschger, Paul; Schell, Hanna; Duda, Georg N

    2010-01-01

    Callus tissue formed during bone fracture healing is a mixture of different tissue types as revealed by histological analysis. But the structural characteristics of mineral crystals within the healing callus are not well known. Since two-dimensional (2D) scanning small-angle X-ray scattering (sSAXS) patterns showed that the size and orientation of callus crystals vary both spatially and temporally [1] and 2D electron microscopic analysis implies an anisotropic property of the callus morphology, the mineral crystals within the callus are also expected to vary in size and orientation in 3D. Three-dimensional small-angle X-ray scattering (3D SAXS), which combines 2D SAXS patterns collected at different angles of sample tilting, has been previously applied to investigate bone minerals in horse radius [2] and oim/oim mouse femur/tibia [3]. We implement a similar 3D SAXS method but with a different way of data analysis to gather information on the mineral alignment in fracture callus. With the proposed accurate yet fast assessment of 3D SAXS information, it was shown that the plate shaped mineral particles in the healing callus were aligned in groups with their predominant orientations occurring as a fiber texture.

  6. Analysis of liquid structure without construction of any structure models by the X-ray scattering method

    International Nuclear Information System (INIS)

    Katayama, Misaki; Ashiki, Shingo; Ozutsumi, Kazuhiko

    2007-01-01

    A simple approach for determining a liquid structure using X-ray scattering data, in which a liquid structure is uniquely evaluated without construction of any plausible structure models, has been applied to liquid acetonitrile, acetone and cyclohexane. For a pair of molecules, a given point within a molecule is located at the origin with a given molecular orientation. The site of the given point of another molecule is defined by the polar coordinates and the molecular orientation is treated by three Eulerian angles. These parameters are optimized by a non-linear least-squares calculation applied to X-ray scattering data. The reliability of the method was examined by determining the liquid structure of polar acetonitrile and the obtained intermolecular interatomic distances are in good agreement with the previously reported values. The method was then successfully applied to the determination of the liquid structure of acetone cyclohexane. Especially for nonpolar cyclohexane, the construction of a variety of plausible structural models is very difficult. It was revealed that acetone has an ordered liquid arrangement similar to that found in its crystal, although the intermolecular distances in liquid acetone are different from those in the crystal. On the other hand, the liquid structure of cyclohexane is disordered. (author)

  7. Simbol-X Mirror Module Thermal Shields: II-Small Angle X-Ray Scattering Measurements

    Science.gov (United States)

    Barbera, M.; Ayers, T.; Collura, A.; Nasillo, G.; Pareschi, G.; Tagliaferri, G.

    2009-05-01

    The formation flight configuration of the Simbol-X mission implies that the X-ray mirror module will be open to Space on both ends. In order to reduce the power required to maintain the thermal stability and, therefore, the high angular resolution of the shell optics, a thin foil thermal shield will cover the mirror module. Different options are presently being studied for the foil material of these shields. We report results of an experimental investigation conducted to verify that the scattering of X-rays, by interaction with the thin foil material of the thermal shield, will not significantly affect the performances of the telescope.

  8. Simbol-X Mirror Module Thermal Shields: II-Small Angle X-Ray Scattering Measurements

    International Nuclear Information System (INIS)

    Barbera, M.; Ayers, T.; Collura, A.; Nasillo, G.; Pareschi, G.; Tagliaferri, G.

    2009-01-01

    The formation flight configuration of the Simbol-X mission implies that the X-ray mirror module will be open to Space on both ends. In order to reduce the power required to maintain the thermal stability and, therefore, the high angular resolution of the shell optics, a thin foil thermal shield will cover the mirror module. Different options are presently being studied for the foil material of these shields. We report results of an experimental investigation conducted to verify that the scattering of X-rays, by interaction with the thin foil material of the thermal shield, will not significantly affect the performances of the telescope.

  9. Melting of short 1-alcohol monolayers on water: Thermodynamics and x-ray scattering studies

    DEFF Research Database (Denmark)

    Berge, B.; Konovalov, O.; Lajzerowicz, J.

    1994-01-01

    From surface tension measurements we extract the melting entropy Delta S-2D of fatty-alcohol monolayers on water. Delta S-2D is found to be 4(kB)/mol lower than in the bulk. Because of the role of the conformational entropy, the melting transition is discontinuous for long chains, but tends to be...

  10. A customizable software for fast reduction and analysis of large X-ray scattering data sets: applications of the new DPDAK package to small-angle X-ray scattering and grazing-incidence small-angle X-ray scattering.

    Science.gov (United States)

    Benecke, Gunthard; Wagermaier, Wolfgang; Li, Chenghao; Schwartzkopf, Matthias; Flucke, Gero; Hoerth, Rebecca; Zizak, Ivo; Burghammer, Manfred; Metwalli, Ezzeldin; Müller-Buschbaum, Peter; Trebbin, Martin; Förster, Stephan; Paris, Oskar; Roth, Stephan V; Fratzl, Peter

    2014-10-01

    X-ray scattering experiments at synchrotron sources are characterized by large and constantly increasing amounts of data. The great number of files generated during a synchrotron experiment is often a limiting factor in the analysis of the data, since appropriate software is rarely available to perform fast and tailored data processing. Furthermore, it is often necessary to perform online data reduction and analysis during the experiment in order to interactively optimize experimental design. This article presents an open-source software package developed to process large amounts of data from synchrotron scattering experiments. These data reduction processes involve calibration and correction of raw data, one- or two-dimensional integration, as well as fitting and further analysis of the data, including the extraction of certain parameters. The software, DPDAK (directly programmable data analysis kit), is based on a plug-in structure and allows individual extension in accordance with the requirements of the user. The article demonstrates the use of DPDAK for on- and offline analysis of scanning small-angle X-ray scattering (SAXS) data on biological samples and microfluidic systems, as well as for a comprehensive analysis of grazing-incidence SAXS data. In addition to a comparison with existing software packages, the structure of DPDAK and the possibilities and limitations are discussed.

  11. Investigating the origins of nanostructural variations in differential ethnic hair types using X-ray scattering techniques.

    Science.gov (United States)

    Wade, M; Tucker, I; Cunningham, P; Skinner, R; Bell, F; Lyons, T; Patten, K; Gonzalez, L; Wess, T

    2013-10-01

    Human hair is a major determinant of visual ethnic differentiation. Although hair types are celebrated as part of our ethnic diversity, the approach to hair care has made the assumption that hair types are structurally and chemically similar. Although this is clearly not the case at the macroscopic level, the intervention of many hair treatments is at the nanoscopic and molecular levels. The purpose of the work presented here is to identify the main nanoscopic and molecular hierarchical differences across five different ethnic hair types from hair fibres taken exclusively from the scalp. These are Afro (subdivided into elastic 'rubber' and softer non-elastic 'soft'), Chinese, European and Mullato (mixed race). Small angle X-Ray scattering (SAXS) is a technique capable of resolving nanostructural variations in complex materials. Individual hair fibres from different ethnic hair types were used to investigate structural features found in common and also specific to each type. Simultaneous wide angle X-Ray scattering (WAXS) was used to analyse the submolecular level structure of the fibrous keratin present. The data sets from both techniques were analysed with principal component analysis (PCA) to identify underlying variables. Principal component analysis of both SAXS and WAXS data was shown to discriminate the scattering signal between different hair types. The X-ray scattering results show a common underlying keratin intermediate filament (KIF) structure. However, distinct differences were observed in the preferential orientation and intensity signal from the lipid component of the hair. In addition, differences were observed in the intensity distribution of the very low-angle sample-dependent diffuse scatter surrounding the 'beamstop.' The results indicate that the fibrous keratin scaffold remains consistent between ethnic hair types. The hierarchies made by these may be modulated by variation in the content of keratin-associated proteins (KAPs) and lipids that

  12. Structural analysis and characterization of synthesized ordered mesoporous silicate (MCM-41) using small angle X-rays scattering and complementary techniques

    Science.gov (United States)

    Akinlalu, Ademola V.

    Mesoporous silicate have widespread potential applications, such as drug delivery, supports for catalysis, selective adsorption and host to guest molecules. Most important in the area of scientific research and industrial applications is their demand due to its extremely high surface areas (> 800m 2g-1) and larger pores with well defined structures. Mesoporous silicate (MCM-41) samples were prepared by hydrothermal method under various chemo-physical conditions and various experimental methods such as small angle X-rays scattering (SAXS), Nitrogen adsorption-desorption analysis at 77 K, Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) were employed to investigate the changes in the structural morphology and subtle lattice parameter changes. With regards to the subtle changes in the structural characteristics of the synthesized mesoporous silicate, we seek to understand the electron density function changes as the synthesis parameter are varied from low molar concentration of ATAB/Si to higher concentration, the system becoming more acidity due to increase in the hydrolysis time of pH regulator as a result of increased production of ethanol and acetic acid and the changes due to extended reaction time. This Ph.D. research tries to understand the influence of various parameters like surfactant-Si molar ratio, reaction time, and the hydrolysis of the pH regulator on the orderliness/disorderliness of the lattice order, lattice spacing and electron density function. The stages during synthesis are carefully selected to better understand where the greater influence on the overall structural morphology exist so as to be able to ne tune this parameter for any desired specification and application. The SAXS measurement were conducted on a HECUS S3-Micro X-ray system at Rensselaer Polytechnic Institute, Troy, NY. while the data evaluation and visualization were carried in 3DView 4.2 and EasySWAXS software. The electron density functions

  13. Novel micro-reactor flow cell for investigation of model catalysts using in situ grazing-incidence X-ray scattering

    DEFF Research Database (Denmark)

    Kehres, Jan; Pedersen, Thomas; Masini, Federico

    2016-01-01

    at synchrotron facilities are performed utilizing the micro-reactor and a designed transportable gas feed and analysis system. The feasibility of simultaneous in situ GISAXS/GIWAXS experiments in the novel micro-reactor flow cell was confirmed with CO oxidation over mass-selected Ru nanoparticles.......The design, fabrication and performance of a novel and highly sensitive micro-reactor device for performing in situ grazing-incidence X-ray scattering experiments of model catalyst systems is presented. The design of the reaction chamber, etched in silicon on insulator (SIO), permits grazing......-incidence small-angle X-ray scattering (GISAXS) in transmission through 10 µm-thick entrance and exit windows by using micro-focused beams. An additional thinning of the Pyrex glass reactor lid allows simultaneous acquisition of the grazing-incidence wide-angle X-ray scattering (GIWAXS). In situ experiments...

  14. Novel micro-reactor flow cell for investigation of model catalysts using in situ grazing-incidence X-ray scattering

    Science.gov (United States)

    Kehres, Jan; Pedersen, Thomas; Masini, Federico; Andreasen, Jens Wenzel; Nielsen, Martin Meedom; Diaz, Ana; Nielsen, Jane Hvolbæk; Hansen, Ole

    2016-01-01

    The design, fabrication and performance of a novel and highly sensitive micro-reactor device for performing in situ grazing-incidence X-ray scattering experiments of model catalyst systems is presented. The design of the reaction chamber, etched in silicon on insulator (SIO), permits grazing-incidence small-angle X-ray scattering (GISAXS) in transmission through 10 µm-thick entrance and exit windows by using micro-focused beams. An additional thinning of the Pyrex glass reactor lid allows simultaneous acquisition of the grazing-incidence wide-angle X-ray scattering (GIWAXS). In situ experiments at synchrotron facilities are performed utilizing the micro-reactor and a designed transportable gas feed and analysis system. The feasibility of simultaneous in situ GISAXS/GIWAXS experiments in the novel micro-reactor flow cell was confirmed with CO oxidation over mass-selected Ru nanoparticles. PMID:26917133

  15. Novel micro-reactor flow cell for investigation of model catalysts using in situ grazing-incidence X-ray scattering.

    Science.gov (United States)

    Kehres, Jan; Pedersen, Thomas; Masini, Federico; Andreasen, Jens Wenzel; Nielsen, Martin Meedom; Diaz, Ana; Nielsen, Jane Hvolbæk; Hansen, Ole; Chorkendorff, Ib

    2016-03-01

    The design, fabrication and performance of a novel and highly sensitive micro-reactor device for performing in situ grazing-incidence X-ray scattering experiments of model catalyst systems is presented. The design of the reaction chamber, etched in silicon on insulator (SIO), permits grazing-incidence small-angle X-ray scattering (GISAXS) in transmission through 10 µm-thick entrance and exit windows by using micro-focused beams. An additional thinning of the Pyrex glass reactor lid allows simultaneous acquisition of the grazing-incidence wide-angle X-ray scattering (GIWAXS). In situ experiments at synchrotron facilities are performed utilizing the micro-reactor and a designed transportable gas feed and analysis system. The feasibility of simultaneous in situ GISAXS/GIWAXS experiments in the novel micro-reactor flow cell was confirmed with CO oxidation over mass-selected Ru nanoparticles.

  16. Soft x-ray scattering facility at the Advanced Light Source with real-time data processing and analysis.

    Science.gov (United States)

    Gann, E; Young, A T; Collins, B A; Yan, H; Nasiatka, J; Padmore, H A; Ade, H; Hexemer, A; Wang, C

    2012-04-01

    We present the development and characterization of a dedicated resonant soft x-ray scattering facility. Capable of operation over a wide energy range, the beamline and endstation are primarily used for scattering from soft matter systems around the carbon K-edge (∼285 eV). We describe the specialized design of the instrument and characteristics of the beamline. Operational characteristics of immediate interest to users such as polarization control, degree of higher harmonic spectral contamination, and detector noise are delineated. Of special interest is the development of a higher harmonic rejection system that improves the spectral purity of the x-ray beam. Special software and a user-friendly interface have been implemented to allow real-time data processing and preliminary data analysis simultaneous with data acquisition. © 2012 American Institute of Physics

  17. Soft x-ray scattering facility at the Advanced Light Source with real-time data processing and analysis

    Science.gov (United States)

    Gann, E.; Young, A. T.; Collins, B. A.; Yan, H.; Nasiatka, J.; Padmore, H. A.; Ade, H.; Hexemer, A.; Wang, C.

    2012-04-01

    We present the development and characterization of a dedicated resonant soft x-ray scattering facility. Capable of operation over a wide energy range, the beamline and endstation are primarily used for scattering from soft matter systems around the carbon K-edge (˜285 eV). We describe the specialized design of the instrument and characteristics of the beamline. Operational characteristics of immediate interest to users such as polarization control, degree of higher harmonic spectral contamination, and detector noise are delineated. Of special interest is the development of a higher harmonic rejection system that improves the spectral purity of the x-ray beam. Special software and a user-friendly interface have been implemented to allow real-time data processing and preliminary data analysis simultaneous with data acquisition.

  18. Soft x-ray scattering facility at the Advanced Light Source with real-time data processing and analysis

    International Nuclear Information System (INIS)

    Gann, E.; Collins, B. A.; Ade, H.; Young, A. T.; Nasiatka, J.; Padmore, H. A.; Hexemer, A.; Wang, C.; Yan, H.

    2012-01-01

    We present the development and characterization of a dedicated resonant soft x-ray scattering facility. Capable of operation over a wide energy range, the beamline and endstation are primarily used for scattering from soft matter systems around the carbon K-edge (∼285 eV). We describe the specialized design of the instrument and characteristics of the beamline. Operational characteristics of immediate interest to users such as polarization control, degree of higher harmonic spectral contamination, and detector noise are delineated. Of special interest is the development of a higher harmonic rejection system that improves the spectral purity of the x-ray beam. Special software and a user-friendly interface have been implemented to allow real-time data processing and preliminary data analysis simultaneous with data acquisition.

  19. Ordered array of ω particles in β-Ti matrix studied by small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Šmilauerová, J.; Harcuba, P.; Stráský, J.; Stráská, J.; Janeček, M.; Pospíšil, J.; Kužel, R.; Brunátová, T.; Holý, V.; Ilavský, J.

    2014-01-01

    Nanosized particles of ω phase in a β-Ti alloy were investigated by small-angle X-ray scattering using synchrotron radiation. We demonstrated that the particles are spontaneously weakly ordered in a three-dimensional cubic array along the 〈100〉-directions in the β-Ti matrix. The small-angle scattering data fit well to a three-dimensional short-range-order model; from the fit we determined the evolution of the mean particle size and mean distance between particles during ageing. The self-ordering of the particles is explained by elastic interaction between the particles, since the relative positions of the particles coincide with local minima of the interaction energy. We performed numerical Monte Carlo simulation of the particle ordering and we obtained a good agreement with the experimental data

  20. Grazing incidence small angle X-ray scattering study of silver nanoparticles in ion-exchanged glasses

    Energy Technology Data Exchange (ETDEWEB)

    Cheng, Weidong, E-mail: 57399942@qq.com [College of Materials Science and Engineering, Qiqihar University, Qiqihar 161006 (China); Wu, Zhaojun [Department of Practice Teaching and Equipment Management, Qiqihar University, Qiqihar 161006 (China); Gu, Xiaohua [College of Materials Science and Engineering, Qiqihar University, Qiqihar 161006 (China); Xing, Xueqing; Mo, Guang [Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China); Wu, Zhonghua, E-mail: wuzh@ihep.ac.cn [Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China)

    2015-05-15

    The size and distribution of silver nanoparticles in ion-exchanged silicate glass induced by thermal treatments in air at different temperatures were investigated by means of grazing incidence small angle X-ray scattering technique, X-ray diffraction and optical absorption spectra. Silver–sodium ion exchange of soda-lime silicate glasses was done at 350 °C for 240 min, then the samples were treated by thermal annealing in air at different temperatures 400, 500 and 550 °C, respectively, for 1 h. After the annealing treatment above 400 °C for 1 h, smaller Ag nanoparticles occurred, together with bigger ones. Both dissolution of smaller Ag nanoparticles and diffusion of larger ones are discussed in these stages of annealing in this contribution.

  1. Synchrotron X-ray Scattering Analysis of the Interaction Between Corn Starch and an Exogenous Lipid During Hydrothermal Treatment

    Energy Technology Data Exchange (ETDEWEB)

    E Hernandez-Hernandez; C Avila-Orta; B Hsiao; j Castro-Rosas; J Gallegos-Infante; J Morales-Castro; L Ochoa-Martinez; C Gomez-Aldapa

    2011-12-31

    Lipids have an important effect on starch physicochemical properties. There exist few reports about the effect of exogenous lipids on native corn starch structural properties. In this work, a study of the morphological, structural and thermal properties of native corn starch with L-alpha-lysophosphatidylcholine (LPC, the main phospholipid in corn) was performed under an excess of water. Synchrotron radiation, in the form of real-time small and wide-angle X-ray scattering (SAXS/WAXS), was used in order to track structural changes in corn starch, in the presence of LPC during a heating process from 30 to 85 C. When adding LCP, water absorption decreased within starch granule amorphous regions during gelatinization. This is explained by crystallization of the amylose-LPC inclusion complex during gelatinization, which promotes starch granule thermal stability at up to 95 C. Finally, a conceptual model is proposed for explaining the formation mechanism of the starch-LPC complex.

  2. Degradation of periodic multilayers as seen by small-angle x-ray scattering and x-ray diffraction

    CERN Document Server

    Rafaja, D; Simek, D; Zdeborova, L; Valvoda, V

    2002-01-01

    The capabilities of small-angle x-ray scattering (SAXS) and wide-angle x-ray diffraction (XRD) to recognize structural changes in periodic multilayers were compared on Fe/Au multilayers with different degrees of structural degradation. Experimental results have shown that both methods are equally sensitive to the multilayer degradation, i.e., to the occurrence of non-continuous interfaces, to short-circuits in the multilayer structure and to the multilayer precipitation. XRD yielded additional information on the multilayer crystallinity, whilst SAXS could better recognize fragments of a long-range periodicity (remnants of the original multilayer structure). Changes in the multilayer structure were initiated by successive annealing at 200 and 300 deg. C. Experimental data were complemented by numerical simulations performed using a combination of optical theory and the distorted wave Born approximation for SAXS or the kinematical Born approximation for XRD.

  3. Precision mechanical structure of an ultra-high-resolution spectrometer for inelastic X-ray scattering instrument

    Science.gov (United States)

    Shu, Deming; Shvydko, Yuri; Stoupin, Stanislav A.; Khachatryan, Ruben; Goetze, Kurt A.; Roberts, Timothy

    2015-04-14

    A method and an ultrahigh-resolution spectrometer including a precision mechanical structure for positioning inelastic X-ray scattering optics are provided. The spectrometer includes an X-ray monochromator and an X-ray analyzer, each including X-ray optics of a collimating (C) crystal, a pair of dispersing (D) element crystals, anomalous transmission filter (F) and a wavelength (W) selector crystal. A respective precision mechanical structure is provided with the X-ray monochromator and the X-ray analyzer. The precision mechanical structure includes a base plate, such as an aluminum base plate; positioning stages for D-crystal alignment; positioning stages with an incline sensor for C/F/W-crystal alignment, and the positioning stages including flexure-based high-stiffness structure.

  4. Energy and polarization dependence of resonant inelastic X-ray scattering in Nd2CuO4

    International Nuclear Information System (INIS)

    Hill, J.P.; Kao, C.C.; Haemaelaeinen, K.

    1998-01-01

    The authors report the energy and polarization dependence of resonant inelastic x-ray scattering from Nd 2 CuO 4 . An energy loss feature at ∼6 eV is observed in the vicinity of the Cu K-edge. Numerical calculations based on the Anderson impurity model identify this as a charge transfer excitation to the anti-bonding state. The incident polarization is shown to select the intermediate states participating in the resonance process. Resonances are observed at 8,990 eV and 9,000 eV with the incident polarization perpendicular and parallel to the CuO planes, respectively. In contrast to the single-site model calculations, no resonances are observed associated with the 1s3d 10 L intermediate states, suggesting non-local effects play a role

  5. Nonperturbative Series Expansion of Green's Functions: The Anatomy of Resonant Inelastic X-Ray Scattering in the Doped Hubbard Model

    Science.gov (United States)

    Lu, Yi; Haverkort, Maurits W.

    2017-12-01

    We present a nonperturbative, divergence-free series expansion of Green's functions using effective operators. The method is especially suited for computing correlators of complex operators as a series of correlation functions of simpler forms. We apply the method to study low-energy excitations in resonant inelastic x-ray scattering (RIXS) in doped one- and two-dimensional single-band Hubbard models. The RIXS operator is expanded into polynomials of spin, density, and current operators weighted by fundamental x-ray spectral functions. These operators couple to different polarization channels resulting in simple selection rules. The incident photon energy dependent coefficients help to pinpoint main RIXS contributions from different degrees of freedom. We show in particular that, with parameters pertaining to cuprate superconductors, local spin excitation dominates the RIXS spectral weight over a wide doping range in the cross-polarization channel.

  6. Synchrotron X-ray scattering study on stratum corneum of skin. Toward applied research based upon basic research

    International Nuclear Information System (INIS)

    Hatta, Ichiro; Ohta, Noboru; Yagi, Naoto

    2008-01-01

    On considering the applied research on stratum corneum of skin, it is indispensable to know the structure at the molecular level. However, there is even now in a controversy among the researchers who are performing its X-ray scattering study. Here we introduce our solution for the two problems: One is the correlation between the lamellar structures and hydrocarbon-chain packings in intercellular lipid matrix and the other is the existence of water layers in the short lamellar structure. These studies have become possible for the first time by making good use of synchrotron small-angle/wide-angle X-ray diffraction. Based upon the structural evidence, we can further carry out the applied research in stratum corneum. (author)

  7. In situ grazing incidence small-angle X-ray scattering investigation of polystyrene nanoparticle spray deposition onto silicon.

    Science.gov (United States)

    Herzog, Gerd; Benecke, Gunthard; Buffet, Adeline; Heidmann, Berit; Perlich, Jan; Risch, Johannes F H; Santoro, Gonzalo; Schwartzkopf, Matthias; Yu, Shun; Wurth, Wilfried; Roth, Stephan V

    2013-09-10

    We investigated the spray deposition and subsequent self-assembly during drying of a polystyrene nanoparticle dispersion with in situ grazing incidence small-angle X-ray scattering at high time resolution. During the fast deposition of the dispersion and the subsequent evaporation of the solvent, different transient stages of nanoparticle assembly can be identified. In the first stage, the solvent starts to evaporate without ordering of the nanoparticles. During the second stage, large-scale structures imposed by the breakup of the liquid film are observable. In this stage, the solvent evaporates further and nanoparticle ordering starts. In the late third drying stage, the nanoparticles self-assemble into the final layer structure.

  8. The applications of small-angle X-ray scattering in studying nano-scaled polyoxometalate clusters in solutions

    Science.gov (United States)

    Li, Mu; Zhang, Mingxin; Wang, Weiyu; Cheng, Stephen Z. D.; Yin, Panchao

    2018-05-01

    Nano-scaled polyoxometalates (POMs) clusters with sizes ranging from 1 to 10 nm attract tremendous attention and have been extensively studied due to POMs' fascinating structural characteristics and prospects for wide-ranging applications. As a unique class of nanoparticles with well-defined structural topologies and monodispersed masses, the structures and properties of POMs in both bulk state and solutions have been explored with several well-developed protocols. Small-angle X-ray scattering (SAXS) technique, as a powerful tool for studying polymers and nanoparticles, has been recently extended to the investigating of solution behaviors of POMs. In this mini-review, the general principle and typical experimental procedures of SAXS are illustrated first. The applications of SAXS in characterizing POMs' morphology, counterion distribution around POMs, and short-range interactions among POMs in solutions are highlighted. [Figure not available: see fulltext.

  9. Raman and fluorescence contributions to the resonant inelastic soft x-ray scattering on LaAlO3/SrTiO3 heterostructures

    Science.gov (United States)

    Pfaff, F.; Fujiwara, H.; Berner, G.; Yamasaki, A.; Niwa, H.; Kiuchi, H.; Gloskovskii, A.; Drube, W.; Gabel, J.; Kirilmaz, O.; Sekiyama, A.; Miyawaki, J.; Harada, Y.; Suga, S.; Sing, M.; Claessen, R.

    2018-01-01

    We present a detailed study of the Ti 3 d carriers at the interface of LaAlO3/SrTiO3 heterostructures by high-resolution resonant inelastic soft x-ray scattering (RIXS), with special focus on the roles of overlayer thickness and oxygen vacancies. Our measurements show the existence of interfacial Ti 3 d electrons already below the critical thickness for conductivity. The (total) interface charge carrier density increases up to a LaAlO3 overlayer thickness of 6 unit cells before it levels out. Furthermore, we observe strong Ti 3 d charge carrier doping by oxygen vacancies. The RIXS data combined with photoelectron spectroscopy and transport measurements indicate the simultaneous presence of localized and itinerant charge carriers. At variance with previous interpretations, we show that in our excitation energy dependent RIXS measurements the amounts of localized and itinerant Ti 3 d electrons in the ground state do not scale with the intensities of the Raman and fluorescence peaks, respectively. Rather, we attribute the observation of either Raman components or fluorescence signal to the specific nature of the intermediate state reached in the RIXS excitation process.

  10. Lattice dynamics at high pressure: application of inelastic X-ray scattering and ab-initio calculations -MgO at 35 GPa

    International Nuclear Information System (INIS)

    Ghose, Subrata

    2006-01-01

    Full text: Until recently, inelastic neutron scattering (INS) has been extensively used to study the phonon dispersion throughout the Brillouin zone and phonon density of states in crystalline materials. The weak interaction of neutrons with matter and the typical size of the neutron beams require the use of cm-size single crystals that puts an upper limit to the measurement of phonon dispersion at high pressure to about 10-15 Gpa by INS. Inelastic X-ray scattering (IXS) using third generation synchrotron sources now makes it possible to measure the phonon dispersion at high pressures up to 50 GP A in crystals tens of microns in size mounted in a diamond-anvil cell, usually using He as the pressure transmitting medium. We have used this technique to measure the longitudinal acoustic and optic phonon branches of MgO along the Γ-X direction at 35 Gpa. The experimentally observed phonon-branches are in remarkable agreement with ab-initio quantum mechanical calculations using the density-functional perturbation theory. The derived thermodynamic properties, such as specific heat and the entropy are in very good agreement with values obtained from a thermodynamically assessed data set

  11. TU-F-18C-03: X-Ray Scatter Correction in Breast CT: Advances and Patient Testing

    International Nuclear Information System (INIS)

    Ramamurthy, S; Sechopoulos, I

    2014-01-01

    Purpose: To further develop and perform patient testing of an x-ray scatter correction algorithm for dedicated breast computed tomography (BCT). Methods: A previously proposed algorithm for x-ray scatter signal reduction in BCT imaging was modified and tested with a phantom and on patients. A wireless electronic positioner system was designed and added to the BCT system that positions a tungsten plate in and out of the x-ray beam. The interpolation used by the algorithm was replaced with a radial basis function-based algorithm, with automated exclusion of non-valid sampled points due to patient motion or other factors. A 3D adaptive noise reduction filter was also introduced to reduce the impact of scatter quantum noise post-reconstruction. The impact on image quality of the improved algorithm was evaluated using a breast phantom and seven patient breasts, using quantitative metrics such signal difference (SD) and signal difference-to-noise ratios (SDNR) and qualitatively using image profiles. Results: The improvements in the algorithm resulted in a more robust interpolation step, with no introduction of image artifacts, especially at the imaged object boundaries, which was an issue in the previous implementation. Qualitative evaluation of the reconstructed slices and corresponding profiles show excellent homogeneity of both the background and the higher density features throughout the whole imaged object, as well as increased accuracy in the Hounsfield Units (HU) values of the tissues. Profiles also demonstrate substantial increase in both SD and SDNR between glandular and adipose regions compared to both the uncorrected and system-corrected images. Conclusion: The improved scatter correction algorithm can be reliably used during patient BCT acquisitions with no introduction of artifacts, resulting in substantial improvement in image quality. Its impact on actual clinical performance needs to be evaluated in the future. Research Agreement, Koning Corp., Hologic

  12. Estimation of degree of polymerization of poly-acrylonitrile-grafted carbon nanotubes using Guinier plot of small angle x-ray scattering.

    Science.gov (United States)

    Cho, Hyunjung; Jin, Kyeong Sik; Lee, Jaegeun; Lee, Kun-Hong

    2018-07-06

    Small angle x-ray scattering (SAXS) was used to estimate the degree of polymerization of polymer-grafted carbon nanotubes (CNTs) synthesized using a 'grafting from' method. This analysis characterizes the grafted polymer chains without cleaving them from CNTs, and provides reliable data that can complement conventional methods such as thermogravimetric analysis or transmittance electron microscopy. Acrylonitrile was polymerized from the surface of the CNTs by using redox initiation to produce poly-acrylonitrile-grafted CNTs (PAN-CNTs). Polymerization time and the initiation rate were varied to control the degree of polymerization. Radius of gyration (R g ) of PAN-CNTs was determined using the Guinier plot obtained from SAXS solution analysis. The results showed consistent values according to the polymerization condition, up to a maximum R g  = 125.70 Å whereas that of pristine CNTs was 99.23 Å. The dispersibility of PAN-CNTs in N,N-dimethylformamide was tested using ultraviolet-visible-near infrared spectroscopy and was confirmed to increase as the degree of polymerization increased. This analysis will be helpful to estimate the degree of polymerization of any polymer-grafted CNTs synthesized using the 'grafting from' method and to fabricate polymer/CNT composite materials.

  13. Nanoporous active carbons at ambient conditions: a comparative study using X-ray scattering and diffraction, Raman spectroscopy and N2 adsorption

    Science.gov (United States)

    Shiryaev, A. A.; Voloshchuk, A. M.; Volkov, V. V.; Averin, A. A.; Artamonova, S. D.

    2017-05-01

    Furfural-derived sorbents and activated carbonaceous fibers were studied using Small- and Wide-angle X-ray scattering (SWAXS), X-ray diffraction and multiwavelength Raman spectroscopy after storage at ambient conditions. Correlations between structural features with degree of activation and with sorption parameters are observed for samples obtained from a common precursor and differing in duration of activation. However, the correlations are not necessarily applicable to the carbons obtained from different precursors. Using two independent approaches we show that treatment of SWAXS results should be performed with careful analysis of applicability of the Porod law to the sample under study. In general case of a pore with rough/corrugated surface deviations from the Porod law may became significant and reflect structure of the pore-carbon interface. Ignorance of these features may invalidate extraction of closed porosity values. In most cases the pore-matrix interface in the studied samples is not atomically sharp, but is characterized by 1D or 2D fluctuations of electronic density responsible for deviations from the Porod law. Intensity of the pores-related small-angle scattering correlates positively with SBET values obtained from N2 adsorption.

  14. Plasma-assisted atomic layer epitaxial growth of aluminum nitride studied with real time grazing angle small angle x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Anderson, Virginia R.; Nepal, Neeraj; Johnson, Scooter D.; Robinson, Zachary R.; Nath, Anindya; Kozen, Alexander C.; Qadri, Syed B.; DeMasi, Alexander; Hite, Jennifer K.; Ludwig, Karl F.; Eddy, Charles R.

    2017-05-01

    Wide bandgap semiconducting nitrides have found wide-spread application as light emitting and laser diodes and are under investigation for further application in optoelectronics, photovoltaics, and efficient power switching technologies. Alloys of the binary semiconductors allow adjustments of the band gap, an important semiconductor material characteristic, which is 6.2 eV for aluminum nitride (AlN), 3.4 eV for gallium nitride, and 0.7 eV for (InN). Currently, the highest quality III-nitride films are deposited by metalorganic chemical vapor deposition and molecular beam epitaxy. Temperatures of 900 °C and higher are required to deposit high quality AlN. Research into depositing III-nitrides with atomic layer epitaxy (ALEp) is ongoing because it is a fabrication friendly technique allowing lower growth temperatures. Because it is a relatively new technique, there is insufficient understanding of the ALEp growth mechanism which will be essential to development of the process. Here, grazing incidence small angle x-ray scattering is employed to observe the evolving behavior of the surface morphology during growth of AlN by ALEp at temperatures from 360 to 480 °C. Increased temperatures of AlN resulted in lower impurities and relatively fewer features with short range correlations.

  15. Nanoporous active carbons at ambient conditions: a comparative study using X-ray scattering and diffraction, Raman spectroscopy and N2 adsorption

    International Nuclear Information System (INIS)

    Shiryaev, A A; Voloshchuk, A M; Averin, A A; Artamonova, S D.; Volkov, V V

    2017-01-01

    Furfural-derived sorbents and activated carbonaceous fibers were studied using Small- and Wide-angle X-ray scattering (SWAXS), X-ray diffraction and multiwavelength Raman spectroscopy after storage at ambient conditions. Correlations between structural features with degree of activation and with sorption parameters are observed for samples obtained from a common precursor and differing in duration of activation. However, the correlations are not necessarily applicable to the carbons obtained from different precursors. Using two independent approaches we show that treatment of SWAXS results should be performed with careful analysis of applicability of the Porod law to the sample under study. In general case of a pore with rough/corrugated surface deviations from the Porod law may became significant and reflect structure of the pore-carbon interface. Ignorance of these features may invalidate extraction of closed porosity values. In most cases the pore-matrix interface in the studied samples is not atomically sharp, but is characterized by 1D or 2D fluctuations of electronic density responsible for deviations from the Porod law. Intensity of the pores-related small-angle scattering correlates positively with S BET values obtained from N 2 adsorption. (paper)

  16. Dimensional nanometrology with grazing incidence small angle X-ray scattering (GISAXS)

    Energy Technology Data Exchange (ETDEWEB)

    Wernecke, Jan; Krumrey, Michael; Cibik, Levent; Marggraf, Stefanie; Mueller, Peter [Physikalisch-Technische Bundesanstalt (PTB), Berlin (Germany)

    2011-07-01

    Reliable methods for dimensional characterisation of structures in the nanometer range are now a necessity in many fields of industry and science, e.g. for next-generation EUV lithography, new photovoltaic devices or magnetic nanoparticles. The method we have chosen for measurements of statistically averaged structural properties of nanostructured surfaces is GISAXS. This is a versatile technique to probe statistic properties such as mean particle size, spacial distribution and roughness of nanostructured surfaces and nanoparticle assemblies on top of or buried in bulk material. The GISAXS experiments were performed at the Four-Crystal Monochromator (FCM) beamline in the laboratory of PTB at BESSY II using the SAXS setup of the Helmholtz-Zentrum Berlin (HZB). This presentation will give a short overview of the instrumentation and the capabilities of the laboratory to perform dimensional nanometrology with GISAXS and will show first experimental results. Gratings for EUV lithography have been investigated in terms of coating layer thickness, roughness, grating period and blaze angle. Furthermore, dimensional properties of Au nanoparticles on silicon substrate were determined. The obtained particle sizes were in good agreement with SAXS measurements of these particles in liquid suspension.

  17. Time-slicing subsystem of the biology small-angle x-ray scattering station at the National Synchrotron Light Source

    International Nuclear Information System (INIS)

    Stubblefield, F.W.

    1985-11-01

    The time-slicing subsystem of the Biology Small-Angle X-ray Scattering divides the time period during which the data for small-angle x-ray diffraction patterns from biological samples is collected into time slices (or frames). The subsystem, being part of a multiprocessor experiment control and data acquisition system, has its own dedicated processor; it also has special-purpose front-end electronics sufficient to generate the gating and other control signals required to produce a sequence of as many as 256 time slices, measured with a basic time unit of 1 μsec. The electronics also synchronizes with execution of the time slice sequence the application of stimuli to the biological sample, the measurement of voltages generated by the sample, and the application of auxiliary device trigger pulses and routes detector data and auxiliary scaler data into appropriate time-slice-indexed buffers in a large external data memory array. The structure of the entire experiment control and data acquisition system is briefly reviewed. Details of the structure and operation of the time slice subsystem are presented. 7 refs., 5 figs

  18. Precise small-angle X-ray scattering evaluation of the pore structures in track-etched membranes: Comparison with other convenient evaluation methods

    Energy Technology Data Exchange (ETDEWEB)

    Miyazaki, Tsukasa, E-mail: t_miyazaki@cross.or.jp [Neutron Science and Technology Center, Comprehensive Research Organization for Science and Society, 162-1, Shirakata, Tokai-mura, Naka-gun, Ibaraki 319-1106 (Japan); Takenaka, Mikihito [Department of Polymer Chemistry, Gradual School of Engineering, Kyoto University, Kyotodaigaku-katsura, Kyoto 615-8510 (Japan)

    2017-03-01

    Poly(ethylene terephthalate) (PET)-based track-etched membranes (TMs) with pore sizes ranging from few nanometers to approximately 1 μm are used in various applications in the biological field, and their pore structures are determined by small-angle X-ray scattering (SAXS). These TMs with the nanometer-sized cylindrical pores aligned parallel to the film thickness direction are produced by chemical etching of the track in the PET films irradiated by heavy ions with the sodium hydroxide aqueous solution. It is well known that SAXS allows us to precisely and statistically estimate the pore size and the pore size distribution in the TMs by using the form factor of a cylinder with the extremely long pore length relative to the pore diameter. The results obtained were compared with those estimated with scanning electron microscopy and gas permeability measurements. The result showed that the gas permeability measurement is convenient to evaluate the pore size of TMs within a wide length scale, and the SEM observation is also suited to estimate the pore size, although SEM observation is usually limited above approximately 30 nm.

  19. Investigation of the collagen-mineral-relation in bone with special respect to bone diseases with collagen defects by small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Schreiber, S. A.

    1996-06-01

    Small-angle X-ray scattering (SAXS) was used to study the structure of the collagen/mineral composite of bone in the nanometer range. The most important results were: - In horse radius, the angular distribution of mineral crystals as measured by SAXS agreed well with previous measurements of collagen orientation using circularly polarized light microscopy. This shows that the crystals are parallel to the collagen fibrils. - The effect of sodium fluoride, which stimulates bone formation, and bisphosphonates, which reduce bone resorption, were analyzed. A slight increase in the average thickness of the mineral crystals as well as changes in the structure of the mineral/collagen composite were found in the case of fluoride treated animals. No differences were found between alendronate treated animals and controls. The changes with NaF correlate with bone weakening found in an earlier study with the same animals. - In cortical bone from 9 patients with Osteogenesis Imperfecta (brittle bone disease) the mean thickness of the mineral crystals was found approximately constant around 2.4 nm, while in control bones it constantly increased with age up to about 3.5 nm. In addition, the parallel alignment of the mineral crystals was less in OI-bone than in normal controls. Hence, despite the great variability of this genetic collagen defect, smaller and less well aligned mineral crystals seem to characterize the collagen/mineral composite in OI-bone. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-02-15

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

  1. Charge-transfer and Mott-Hubbard Excitations in FeBo3: Fe K-edge resonant Inelastic x-ray scattering study

    International Nuclear Information System (INIS)

    Kim, J.; Shvydko, Y.

    2011-01-01

    Momentum-resolved resonant inelastic x-ray scattering (RIXS) spectroscopy has been carried out successfully at the Fe K-edge for the first time. The RIXS spectra of a FeBO 3 single crystal reveal a wealth of information on ∼ 1-10 eV electronic excitations. The IXS signal resonates when the incident photon energy approaches the pre-edge (1s - -3d) and the main-edge (1s - -4p) of the Fe K-edge absorption spectrum. The RIXS spectra measured at the pre-edge and the main-edge show quantitatively different dependences on the incident photon energy, momentum transfer, photon polarization, and temperature. We present a multielectron analysis of the Mott-Hubbard (MH) and charge transfer (CT) excitations, and calculate their energies. Electronic excitations observed in the pre-edge and main-edge RIXS spectra are interpreted as MH and CT excitations, respectively. We propose the electronic structure around the chemical potential in FeBO 3 based on the experimental data.

  2. Prediction of protein structure with the coarse-grained UNRES force field assisted by small X-ray scattering data and knowledge-based information.

    Science.gov (United States)

    Karczyńska, Agnieszka S; Mozolewska, Magdalena A; Krupa, Paweł; Giełdoń, Artur; Liwo, Adam; Czaplewski, Cezary

    2018-03-01

    A new approach to assisted protein-structure prediction has been proposed, which is based on running multiplexed replica exchange molecular dynamics simulations with the coarse-grained UNRES force field with restraints derived from knowledge-based models and distance distribution from small angle X-ray scattering (SAXS) measurements. The latter restraints are incorporated into the target function as a maximum-likelihood term that guides the shape of the simulated structures towards that defined by SAXS. The approach was first verified with the 1KOY protein, for which the distance distribution was calculated from the experimental structure, and subsequently used to predict the structures of 11 data-assisted targets in the CASP12 experiment. Major improvement of the GDT_TS was obtained for 2 targets, minor improvement for other 2 while, for 6 target GDT_TS deteriorated compared with that calculated for predictions without the SAXS data, partly because of assuming a wrong multimeric state (for Ts866) or because the crystal conformation was more compact than the solution conformation (for Ts942). Particularly good results were obtained for Ts909, in which use of SAXS data resulted in the selection of a correctly packed trimer and, subsequently, increased the GDT_TS of monomer prediction. It was found that running simulations with correct oligomeric state is essential for the success in SAXS-data-assisted prediction. © 2017 Wiley Periodicals, Inc.

  3. Protein crowding in solution, frozen and freeze-dried states: small-angle neutron and X-ray scattering study of lysozyme/sorbitol/water systems

    Science.gov (United States)

    Krueger, Susan; Khodadadi, Sheila; Clark, Nicholas; McAuley, Arnold; Cristiglio, Viviana; Theyencheri, Narayanan; Curtis, Joseph; Shalaev, Evgenyi

    2015-03-01

    For effective preservation, proteins are often stored as frozen solutions or in glassy states using a freeze-drying process. However, aggregation is often observed after freeze-thaw or reconstitution of freeze-dried powder and the stability of the protein is no longer assured. In this study, small-angle neutron and X-ray scattering (SANS and SAXS) have been used to investigate changes in protein-protein interaction distances of a model protein/cryoprotectant system of lysozyme/sorbitol/water, under representative pharmaceutical processing conditions. The results demonstrate the utility of SAXS and SANS methods to monitor protein crowding at different stages of freezing and drying. The SANS measurements of solution samples showed at least one protein interaction peak corresponding to an interaction distance of ~ 90 Å. In the frozen state, two protein interaction peaks were observed by SANS with corresponding interaction distances at 40 Å as well as 90 Å. On the other hand, both SAXS and SANS data for freeze-dried samples showed three peaks, suggesting interaction distances ranging from ~ 15 Å to 170 Å. Possible interpretations of these interaction peaks will be discussed, as well as the role of sorbitol as a cryoprotectant during the freezing and drying process.

  4. Combined in situ small and wide angle X-ray scattering studies of TiO2 nano-particle annealing to 1023 K

    DEFF Research Database (Denmark)

    Kehres, Jan; Andreasen, Jens Wenzel; Krebs, Frederik C

    2010-01-01

    Combined in situ small- and wide-angle X-ray scattering (SAXS/WAXS) studies were performed in a recently developed laboratory setup to investigate the dynamical properties of dry oleic acid-capped titanium dioxide nanorods during annealing in an inert gas stream in a temperature interval of 298-1...

  5. Study of change in dispersion and orientation of clay platelets in a polymer nanocomposite during tensile test by variostage small-angle X-ray scattering

    CSIR Research Space (South Africa)

    Bandyopadhyay, J

    2012-04-01

    Full Text Available To understand the change in dispersion and orientation of clay platelets in three-dimensional space during tensile test, neat polymer and its nanocomposite samples were studied by small- and wide-angle X-ray scattering (SWAXS). The samples after...

  6. Small-angle X-ray scattering studies of metastable intermediates of beta-lactoglobulin isolated after heat-induced aggregation

    DEFF Research Database (Denmark)

    Carrotta, R.; Arleth, L.; Pedersen, J.S.

    2003-01-01

    Small-angle x-ray scattering was used for studying intermediate species, isolated after heat-induced aggregation of the A variant of bovine P-lactoglobulin. The intermediates were separated in two fractions, the heated metastable dimer and heated metastable oligomers larger than the dimer. The pa...

  7. A new small-angle X-ray scattering set-up on the crystallography beamline I711 at MAX-lab

    DEFF Research Database (Denmark)

    Knaapila, M.; Svensson, C.; Barauskas, J.

    2009-01-01

    A small-angle X-ray scattering (SAXS) set-up has recently been developed at beamline I711 at the MAX II storage ring in Lund (Sweden). An overview of the required modifications is presented here together with a number of application examples. The accessible q range in a SAXS experiment is 0.009-0...

  8. X-ray scattering and diffraction from Xe-induced ripples in crystalline silicon

    Energy Technology Data Exchange (ETDEWEB)

    Biermanns, Andreas; Pietsch, Ullrich; Grigorian, Souren [Universitaet Siegen (Germany); Grenzer, Joerg; Facsko, Stefan; Hanisch, Antje [Foschungszentrum Dresden-Rossendorf (Germany); Carbone, Dina; Metzger, Hartmut [ID Beamline, ESRF (France)

    2008-07-01

    The formation of surface-nanostructures with a characteristic size ranging from several nanometer up to microns has attracted significant interest in the last decades in the context of fabrication of novel opto-electronic and storage devices. One kind of those nanostructures are wave-like patterns (ripples) produced by an interplay between a roughening process caused by ion beam erosion (sputtering) of the surface and smoothening processes caused by surface diffusion. In this contribution we report on investigations of patterned Si(001) surfaces after irradiation with Xe{sup +}-ions using ion-energies up to 40 keV. During the sputtering, an amorphous surface-layer is formed followed by a rather sharp interface towards crystalline material, showing the same morphology as the surface. The structures of the amorphous layer and the amorphous-crystalline interface were studied by means of grazing-incidence-small angle scattering (GISAXS) and diffraction (GID) using synchrotron-radiation. We found that the crystal structure at the interface is expanded along the ripples, caused by the creation of defects inside the surface region, whereas this expansion is strongly reduced across the ripples. This different relaxation may play a driving role in pattern formation at the interface.

  9. The Chemically-Specific Structure of an Amorphous Molybdenum Germanium Alloy by Anomalous X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Ishii, H. A.

    2002-06-11

    Since its inception in the late 1970s, anomalous x-ray scattering (AXS) has been employed for chemically-specific structure determination in a wide variety of noncrystalline materials. These studies have successfully produced differential distribution functions (DDFs) which provide information about the compositionally-averaged environment of a specific atomic species in the sample. Despite the wide success in obtaining DDFs, there are very few examples of successful extraction of the fully-chemically-specific partial pair distribution functions (PPDFs), the most detailed description of an amorphous sample possible by x-ray scattering. Extracting the PPDFs is notoriously difficult since the matrix equation involved is ill-conditioned and thus extremely sensitive to errors present in the experimental quantities that enter the equation. Instead of addressing this sensitivity by modifying the data through mathematical methods, sources of error have been removed experimentally: A focusing analyzer crystal was combined with a position-sensitive linear detector to experimentally eliminate unwanted inelastic scattering intensity over most of the reciprocal space range probed. This instrumentation has been used in data collection for the extraction of PPDFs from amorphous (a)-MoGe{sub 3}. This composition arises as a phase separation endpoint in the Ge-rich region of the vapor-deposited Mo-Ge amorphous alloy system but is not present at equilibrium. Since the first Ge-rich compound in the Mo-Ge equilibrium system is MoGe{sub 2}, previous workers have speculated that perhaps a unique MoGe{sub 3} compound exists in the amorphous system. Rather than indicating a distinct MoGe{sub 3} compound with definitive local structure, however, the coordination results are more consistent with a densely-packed alloy having a wide range of solid solubility. Significant improvement in the quality and reliability of experimental PPDFs from a-MoGe{sub 3} by AXS has been achieved solely

  10. Small angle X-ray scattering and cross-linking for data assisted protein structure prediction in CASP 12 with prospects for improved accuracy

    KAUST Repository

    Ogorzalek, Tadeusz L.

    2018-01-04

    Experimental data offers empowering constraints for structure prediction. These constraints can be used to filter equivalently scored models or more powerfully within optimization functions toward prediction. In CASP12, Small Angle X-ray Scattering (SAXS) and Cross-Linking Mass Spectrometry (CLMS) data, measured on an exemplary set of novel fold targets, were provided to the CASP community of protein structure predictors. As HT, solution-based techniques, SAXS and CLMS can efficiently measure states of the full-length sequence in its native solution conformation and assembly. However, this experimental data did not substantially improve prediction accuracy judged by fits to crystallographic models. One issue, beyond intrinsic limitations of the algorithms, was a disconnect between crystal structures and solution-based measurements. Our analyses show that many targets had substantial percentages of disordered regions (up to 40%) or were multimeric or both. Thus, solution measurements of flexibility and assembly support variations that may confound prediction algorithms trained on crystallographic data and expecting globular fully-folded monomeric proteins. Here, we consider the CLMS and SAXS data collected, the information in these solution measurements, and the challenges in incorporating them into computational prediction. As improvement opportunities were only partly realized in CASP12, we provide guidance on how data from the full-length biological unit and the solution state can better aid prediction of the folded monomer or subunit. We furthermore describe strategic integrations of solution measurements with computational prediction programs with the aim of substantially improving foundational knowledge and the accuracy of computational algorithms for biologically-relevant structure predictions for proteins in solution. This article is protected by copyright. All rights reserved.

  11. Small angle X-ray scattering and cross-linking for data assisted protein structure prediction in CASP 12 with prospects for improved accuracy

    KAUST Repository

    Ogorzalek, Tadeusz L.; Hura, Greg L.; Belsom, Adam; Burnett, Kathryn H.; Kryshtafovych, Andriy; Tainer, John A.; Rappsilber, Juri; Tsutakawa, Susan E.; Fidelis, Krzysztof

    2018-01-01

    Experimental data offers empowering constraints for structure prediction. These constraints can be used to filter equivalently scored models or more powerfully within optimization functions toward prediction. In CASP12, Small Angle X-ray Scattering (SAXS) and Cross-Linking Mass Spectrometry (CLMS) data, measured on an exemplary set of novel fold targets, were provided to the CASP community of protein structure predictors. As HT, solution-based techniques, SAXS and CLMS can efficiently measure states of the full-length sequence in its native solution conformation and assembly. However, this experimental data did not substantially improve prediction accuracy judged by fits to crystallographic models. One issue, beyond intrinsic limitations of the algorithms, was a disconnect between crystal structures and solution-based measurements. Our analyses show that many targets had substantial percentages of disordered regions (up to 40%) or were multimeric or both. Thus, solution measurements of flexibility and assembly support variations that may confound prediction algorithms trained on crystallographic data and expecting globular fully-folded monomeric proteins. Here, we consider the CLMS and SAXS data collected, the information in these solution measurements, and the challenges in incorporating them into computational prediction. As improvement opportunities were only partly realized in CASP12, we provide guidance on how data from the full-length biological unit and the solution state can better aid prediction of the folded monomer or subunit. We furthermore describe strategic integrations of solution measurements with computational prediction programs with the aim of substantially improving foundational knowledge and the accuracy of computational algorithms for biologically-relevant structure predictions for proteins in solution. This article is protected by copyright. All rights reserved.

  12. In situ x-ray scattering studies of the Au(111)/electrolyte interface

    International Nuclear Information System (INIS)

    Wang, Jia; Ocko, B.M.; Davenport, A.J.; Isaacs, H.S.

    1991-01-01

    The adsorption of anions at the Au(111) electrode and the subsequent effect on the gold surface structure have been investigated using x-ray specular reflectivity and grazing incident angle diffraction techniques. The top layer of gold atoms undergoes a reversible phase transition between the (1x1) bulk termination and a (23x√ bar 3) reconstructed phase on changing the potential. The shifts of the phase transition potential in NaCland NaBr solutions from the one in NaF can be understood by the anion adsorption induced charge effect. The reconstruction formation rate increases in chloride and bromide solutions due to an increase in the surface mobility with anion adsorption. Adsorbed chloride and bromide monolayers can be monitored during a potential scan by the specular reflectivity

  13. Study of macromolecules of biological interest by x-ray scattering

    International Nuclear Information System (INIS)

    Beltran, J.R.

    1987-08-01

    A brief review of the SAXS theory and experimental is presented. Solutions of crotamine, crotoxine, phospholipase and crotapotine are studied in several concentrations, extrapolated to infinite dilution and the results obtained are presented. The general shape of these proteins were also evaluated taking in consideration the relationships between the respective surface areas and volumes. A model was then devised taking into account the information available relative to aminoacid sequence, predicted secondary structure and spectroscopic data and its P(r) was calculated using the MULTIBODY program (Glatter (1980)). The P(r) curve is this way obtained showed a considerable agreement with the P(r) obtained resing the scattering curve. (author)

  14. Study of particles in solution by small angle x-ray scattering

    International Nuclear Information System (INIS)

    Itri, R.

    1986-01-01

    The implantation of SAXS technique is presented, and mycellas in solution of the dodecyl sodium sulfate SLS/water system are studied. A synthesis of SAXS theory to study parameters such as, volume, radii of gyration and specific surface and distribution function of the distance of homogenous and inhomogeneous particles is also presented. The technique was implanted by the study of a vitreous coal sample with voids in amorphous matrix. Computer programs were used for data treatment. It was concluded that the void configuration must be an oblate ellipsoid with rippled external surface and radii of gyration of ∼20A . The study of mycellas in solution of the SLL/H 2 O binary system showed spherical mycellas with paraffinic radii of 16A and total radii of 25.5 A. Interaction effects start to appear in 15% SLS concentrations. The change in the scattering curve occurs due to the interactions between mycellas. The isotropic-nematic transition in the ternary system by decanol addition was also investigated. (M.C.K.) [pt

  15. Asymptotic form of the reciprocity theorem with applications in x-ray scattering

    International Nuclear Information System (INIS)

    Caticha, Ariel

    2000-01-01

    The emission of electromagnetic waves from a source within or near a nontrivial medium (with or without boundaries, crystalline or amorphous, with inhomogeneities, absorption, and so on) is sometimes studied using the reciprocity principle which is a variation of the method of Green's functions. If one is only interested in the asymptotic radiation fields the generality of these methods may actually be a shortcoming: obtaining expressions valid for the uninteresting near fields is not just a wasted effort but may be prohibitively difficult. In this work we obtain a modified form of the reciprocity principle which gives the asymptotic radiation field directly. The method may also be used to study scattering problems. We give a few pedagogical examples and then, as more challenging applications, we calculate the specular reflection of x rays by a rough surface and by a smoothly graded surface taking polarization effects into account. In conventional treatments of reflection, x rays are treated as scalar waves; polarization effects are neglected. This is a good approximation at grazing incidence but becomes increasingly questionable for soft x rays and UV at higher incidence angles

  16. X-ray scattering study of the interplay between magnetism and structure in CeSb

    DEFF Research Database (Denmark)

    McMorrow, Desmond Francis; Lussier, J.-G.; Lebech, Bente

    1997-01-01

    appeared with commensurate wave vectors q. From their polarization and wave-vector dependence, the peaks are deduced to arise mainly from a periodic lattice distortion. In the resonant regime, when the x-ray energy was tuned to the L absorption edges of Ce, weak, resonantly enhanced magnetic scattering...... was observed at the L(II) edge (E = 6.164 keV), with no scattering found at either L(I) or L(III) Of the six possible zero-field commensurate magnetic structures reported in earlier neutron experiments, we found the phases with q(m) = 2/3 and 4/7 only, with the domain that has moments perpendicular...... to the surface absent. Neutron scattering experiments on the same single crystal confirm that the absence of the other phases is a bulk property of that particular crystal, but the absence of the domain is a feature of the near-surface region. These results are discussed in terms of the currently accepted model...

  17. Determination by Small-angle X-ray Scattering of Pore Size Distribution in Nanoporous Track-etched Polycarbonate Membranes

    Science.gov (United States)

    Jonas, A. M.; Legras, R.; Ferain, E.

    1998-03-01

    Nanoporous track-etched membranes with narrow pore size distributions and average pore size diameters tunable from 100 to 1000 Åare produced by the chemical etching of latent tracks in polymer films after irradiation by a beam of accelerated heavy ions. Nanoporous membranes are used for highly demanding filtration purposes, or as templates to obtain metallic or polymeric nanowires (L. Piraux et al., Nucl. Instr. Meth. Phys. Res. 1997, B131, 357). Such applications call for developments in nanopore size characterization techniques. In this respect, we report on the characterization by small-angle X-ray scattering (SAXS) of nanopore size distribution (nPSD) in polycarbonate track-etched membranes. The obtention of nPSD requires inverting an ill-conditioned inhomogeneous equation. We present different numerical routes to overcome the amplification of experimental errors in the resulting solutions, including a regularization technique allowing to obtain the nPSD without a priori knowledge of its shape. The effect of deviations from cylindrical pore shape on the resulting distributions are analyzed. Finally, SAXS results are compared to results obtained by electron microscopy and conductometry.

  18. Probing Structural Changes in Poly(3-hexylthiophene) (P3HT) During Electrochemical Oxidation with In Situ X-ray Scattering

    Science.gov (United States)

    Thelen, Jacob L.; Patel, Shrayesh N.; Javier, Anna E.; Balsara, Nitash P.

    2014-03-01

    Mixtures of poly(3-hexylthiophene)-b-poly(ethylene oxide) (P3HT-b-PEO) block copolymer and lithium bis(trifluromethanesulfonyl) imide (LiTFSI) salt can microphase separate into electron (P3HT) and ion (PEO/LiTFSI) conducting domains. P3HT is a semicrystalline polymer with intrinsically semiconducting electronic properties. Electrochemical oxidation (doping) of the P3HT block provides the P3HT-b-PEO/LiTFSI mixtures with electronic conductivity suitable for lithium battery operation. Due to the presence of the solid-state electrolyte (PEO/LiTFSI) in intimate contact with the microphase separated P3HT domains, electrochemical oxidation of P3HT can be performed entirely in the solid state; therefore, P3HT-b-PEO/LiTFSI provides a unique opportunity to study the structural changes in P3HT induced by oxidation. We use in situ x-ray scattering techniques to probe structural changes in P3HT during electrochemical oxidation and correlate these changes with previously observed enhancements in electron mobility. Supported by the Joint Center for Energy Storage Research (JCESR).

  19. Conformational Flexibility of Proteins Involved in Ribosome Biogenesis: Investigations via Small Angle X-ray Scattering (SAXS

    Directory of Open Access Journals (Sweden)

    Dritan Siliqi

    2018-02-01

    Full Text Available The dynamism of proteins is central to their function, and several proteins have been described as flexible, as consisting of multiple domains joined by flexible linkers, and even as intrinsically disordered. Several techniques exist to study protein structures, but small angle X-ray scattering (SAXS has proven to be particularly powerful for the quantitative analysis of such flexible systems. In the present report, we have used SAXS in combination with X-ray crystallography to highlight their usefulness at characterizing flexible proteins, using as examples two proteins involved in different steps of ribosome biogenesis. The yeast BRCA2 and CDKN1A-interactig protein, Bcp1, is a chaperone for Rpl23 of unknown structure. We showed that it consists of a rigid, slightly elongated protein, with a secondary structure comprising a mixture of alpha helices and beta sheets. As an example of a flexible molecule, we studied the SBDS (Shwachman-Bodian-Diamond Syndrome protein that is involved in the cytoplasmic maturation of the 60S subunit and constitutes the mutated target in the Shwachman-Diamond Syndrome. In solution, this protein coexists in an ensemble of three main conformations, with the N- and C-terminal ends adopting different orientations with respect to the central domain. The structure observed in the protein crystal corresponds to an average of those predicted by the SAXS flexibility analysis.

  20. Short-range order in Fe-based metallic glasses: Wide-angle X-ray scattering studies

    International Nuclear Information System (INIS)

    Babilas, Rafał; Hawełek, Łukasz; Burian, Andrzej

    2014-01-01

    The local atomic structure of the Fe 80 B 20 , Fe 70 Nb 10 B 20 and Fe 62 Nb 8 B 30 glasses prepared in the form of ribbons has been studied by wide-angle X-ray scattering. Structural information about the amorphous ribbons has been derived from analysis of the radial distribution functions using the least-squares curve-fitting method. The obtained structural parameters indicate that Fe–Fe, Fe–B, Fe–Nb and Nb–B contributions are involved in the near-neighbor coordination spheres. The possible similarities of the local atomic arrangement in the investigated glasses and the crystalline Fe 3 B, Fe 23 B 6 and bcc Fe structures are also discussed. - Graphical abstract: Pair distribution functions (a) and best-fit model and experimental radial distribution functions for Fe 80 B 20 (b), Fe 70 Nb 10 B 20 (c) and Fe 62 Nb 8 B 30 (d) metallic glasses. - Highlights: • The short-range ordering in the Fe-based metallic glasses is presented. • The results of RDF function have been analyzed using the least-squares method. • The Fe–Fe, Fe–B, Fe–Nb or Nb–B contributions are involved in coordination spheres. • The structural unit is distorted triangular prism containing B, Fe or Nb atoms. • Similarities of atomic arrangement in glassy and crystalline structures are discussed

  1. Peculiar atomic dynamics in liquid GeTe with asymmetrical bonding: Observation by inelastic x-ray scattering

    Science.gov (United States)

    Inui, M.; Koura, A.; Kajihara, Y.; Hosokawa, S.; Chiba, A.; Kimura, K.; Shimojo, F.; Tsutsui, S.; Baron, A. Q. R.

    2018-05-01

    Collective dynamics in liquid GeTe was investigated by inelastic x-ray scattering at 2 ≤Q ≤31 nm-1 . The dynamic structure factor shows clear inelastic excitations. The excitation energies at low Q disperse with increasing Q , consistent with the behavior of a longitudinal-acoustic excitation. The dispersion curve has a flat-topped region around the pseudo-Brillouin-zone boundary, similar to what is observed in liquid Bi [Inui et al., Phys. Rev. B 92, 054206 (2015), 10.1103/PhysRevB.92.054206]. The dynamic structure factor shows a low-frequency excitation, and its coupling with the longitudinal-acoustic mode plays an important role for a flat-topped dispersion. From these results, it is inferred that atomic dynamics in liquid GeTe is strongly affected by a Peierls distortion similar to liquid Bi. By comparing the momentum transfer dependence of the excitation energy and quasielastic linewidth to partial structure factors obtained by our own ab initio molecular dynamics simulation for liquid GeTe, the quasielastic and inelastic components were found to be correlated with Te-Te and Ge-(Ge,Te) partial structure factors, respectively.

  2. The Structure of Urease Activation Complexes Examined by Flexibility Analysis, Mutagenesis, and Small-angle X-ray Scattering Approaches

    International Nuclear Information System (INIS)

    Quiroz, Soledad; Sukuru, Sai Chetan K.; Hausinger, Robert P.; Kuhn, Leslie A.; Heller, William T

    2008-01-01

    Conformational changes of Klebsiella aerogenes urease apoprotein (UreABC) 3 induced upon binding of the UreD and UreF accessory proteins were examined by a combination of flexibility analysis, mutagenesis, and small-angle X-ray scattering (SAXS). ProFlex analysis of urease provided evidence that the major domain of UreB can move in a hinge-like motion to account for prior chemical cross-linking results. Rigidification of the UreB hinge region, accomplished through a G11P mutation, reduced the extent of urease activation, in part by decreasing the nickel content of the mutant enzyme, and by sequestering a portion of the urease apoprotein in a novel activation complex that includes all of the accessory proteins. SAXS analyses of urease, (UreABC-UreD) 3 , and (UreABC-UreDF) 3 confirm that UreD and UreF bind near UreB at the periphery of the (UreAC) 3 structure. This study supports an activation model in which a domain-shifted UreB conformation in (UreABC-UreDF) 3 allows CO 2 and nickel ions to gain access to the nascent active site

  3. Synchrotron X-ray scattering characterization of the molecular structures of star polystyrenes with varying numbers of arms.

    Science.gov (United States)

    Jin, Sangwoo; Higashihara, Tomoya; Jin, Kyeong Sik; Yoon, Jinhwan; Rho, Yecheol; Ahn, Byungcheol; Kim, Jehan; Hirao, Akira; Ree, Moonhor

    2010-05-20

    We have synthesized well-defined multiarmed star polystyrenes, with 6, 9, 17, 33, and 57 arms, and studied their molecular shapes and structural characteristics in a good solvent (tetrahydrofuran at 25 degrees C) and in a theta (Theta) solvent (cyclohexane at 35 degrees C) by small-angle X-ray scattering (SAXS) using a synchrotron radiation source. Analysis of the SAXS data provided a detailed characterization of the molecular shapes, including the contributions of the blob morphology of the arms, the radius of gyration, the paired distance distribution, the radial electron density distribution, and the Zimm-Stockmayer and Roovers g-factor, for the multiarmed star polystyrenes. In particular, the molecular shapes of the star polystyrenes were found to change from a fuzzy ellipsoid, for the 6-armed polystyrene, to a fuzzy sphere, for the 57-armed polystyrene, with an increasing number of arms. The ellipsoidal character of the star polystyrenes with fewer arms may originate from the extended anisotropically branched architecture at the center of the molecule. The arms of the star polystyrenes were found to be more extended than those of the linear polystyrenes. Furthermore, the degree of chain extension in the arms increased with the number of arms.

  4. Compact structure of ribosomal protein S4 in solution as revealed by small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Serdyuk, I.N.; Sarkisyan, M.A.; Gogia, Z.V.

    1981-01-01

    The authors report the results of a small-angle X-ray scattering study of ribosomal protein preparations obtained by neutron scattering method. The theoretical resolution of the diffractometer (Kratky camera, the entrance slit 80 μm, the receiving slit 190 μm, the sample-detector distance 20.4 cm) was the same as the resolution of X-ray diffractometers, on which high rsub(g) values for ribosomal proteins were obtained. They used protein S4 adjusted to 20 mg/ml without any essential loss of solubility. The scattering indicatrix obtained in a wide range of angles has demonstrated that the X-ray rsub(g) obtained here coincides with the earlier obtained neutron rsub(g) and the outer part of the scattering curve is similar to that of slightly elongated compact bodies. They conclude that all discrepancies between their data on the study of ribosomal protein structure in solution and other data are not connected with the characteristics of the instruments used but only with the quality of the protein preparations. (Auth.)

  5. Nano-Structural Investigation on Cellulose Highly Dissolved in Ionic Liquid: A Small Angle X-ray Scattering Study

    Directory of Open Access Journals (Sweden)

    Takatsugu Endo

    2017-01-01

    Full Text Available We investigated nano-structural changes of cellulose dissolved in 1-ethyl-3-methylimidazolium acetate—an ionic liquid (IL—using a small angle X-ray scattering (SAXS technique over the entire concentration range (0–100 mol %. Fibril structures of cellulose disappeared at 40 mol % of cellulose, which is a significantly higher concentration than the maximum concentration of dissolution (24–28 mol % previously determined in this IL. This behavior is explained by the presence of the anion bridging, whereby an anion prefers to interact with multiple OH groups of different cellulose molecules at high concentrations, discovered in our recent work. Furthermore, we observed the emergence of two aggregated nano-structures in the concentration range of 30–80 mol %. The diameter of one structure was 12–20 nm, dependent on concentration, which is ascribed to cellulose chain entanglement. In contrast, the other with 4.1 nm diameter exhibited concentration independence and is reminiscent of a cellulose microfibril, reflecting the occurrence of nanofibrillation. These results contribute to an understanding of the dissolution mechanism of cellulose in ILs. Finally, we unexpectedly proposed a novel cellulose/IL composite: the cellulose/IL mixtures of 30–50 mol % that possess liquid crystallinity are sufficiently hard to be moldable.

  6. Review of the fundamental theories behind small angle X-ray scattering, molecular dynamics simulations, and relevant integrated application

    Directory of Open Access Journals (Sweden)

    Lauren Boldon

    2015-02-01

    Full Text Available In this paper, the fundamental concepts and equations necessary for performing small angle X-ray scattering (SAXS experiments, molecular dynamics (MD simulations, and MD-SAXS analyses were reviewed. Furthermore, several key biological and non-biological applications for SAXS, MD, and MD-SAXS are presented in this review; however, this article does not cover all possible applications. SAXS is an experimental technique used for the analysis of a wide variety of biological and non-biological structures. SAXS utilizes spherical averaging to produce one- or two-dimensional intensity profiles, from which structural data may be extracted. MD simulation is a computer simulation technique that is used to model complex biological and non-biological systems at the atomic level. MD simulations apply classical Newtonian mechanics’ equations of motion to perform force calculations and to predict the theoretical physical properties of the system. This review presents several applications that highlight the ability of both SAXS and MD to study protein folding and function in addition to non-biological applications, such as the study of mechanical, electrical, and structural properties of non-biological nanoparticles. Lastly, the potential benefits of combining SAXS and MD simulations for the study of both biological and non-biological systems are demonstrated through the presentation of several examples that combine the two techniques.

  7. Small-angle X-ray scattering on growth of AgCl crystallites in photochromic glasses

    Energy Technology Data Exchange (ETDEWEB)

    Takatohi, U.E. [Inst. Adventista de Ensino, Sao Paulo (Brazil); Bittencourt, D.R.S.; Watanabe, S.

    1997-10-01

    Reversible changes in the optical properties of photochromic glasses are observed owing to the presence of small silver halide crystals inside the glassy matrix. These crystals grow during the glass heat-treatment processing. Samples with molar composition of 40SiO{sub 2}.10Al{sub 2}O{sub 3}.16.1K{sub 2}O.33.9B{sub 2}O{sub 3}, doped with AgCl and CuO, were produced and submitted to different heat treatments: (i) for 0.5 h at temperatures from 753 to 893 K and (ii) at 873 K for periods of time from 0.25 to 1.25 h. Small-angle X-ray scattering (SAXS) was used to characterize the samples. The samples heat treated between 843 and 893 K presented an increasing growth rate of the Guinier radius (R{sub g}). Samples heat treated at a fixed temperature of 873 K and different time t showed a law R{sub g}{sup 3} = kt + c. Variations in the optical absorbance at 280 nm and the additional absorbance spectra of samples exposed to light showed correlation with the SAXS results. (orig.). 16 refs.

  8. Small-angle X-ray scattering on growth of AgCl crystallites in photochromic glasses

    International Nuclear Information System (INIS)

    Takatohi, U.E.; Bittencourt, D.R.S.; Watanabe, S.

    1997-01-01

    Reversible changes in the optical properties of photochromic glasses are observed owing to the presence of small silver halide crystals inside the glassy matrix. These crystals grow during the glass heat-treatment processing. Samples with molar composition of 40SiO 2 .10Al 2 O 3 .16.1K 2 O.33.9B 2 O 3 , doped with AgCl and CuO, were produced and submitted to different heat treatments: (i) for 0.5 h at temperatures from 753 to 893 K and (ii) at 873 K for periods of time from 0.25 to 1.25 h. Small-angle X-ray scattering (SAXS) was used to characterize the samples. The samples heat treated between 843 and 893 K presented an increasing growth rate of the Guinier radius (R g ). Samples heat treated at a fixed temperature of 873 K and different time t showed a law R g 3 = kt + c. Variations in the optical absorbance at 280 nm and the additional absorbance spectra of samples exposed to light showed correlation with the SAXS results. (orig.)

  9. Selective molecular annealing: in situ small angle X-ray scattering study of microwave-assisted annealing of block copolymers.

    Science.gov (United States)

    Toolan, Daniel T W; Adlington, Kevin; Isakova, Anna; Kalamiotis, Alexis; Mokarian-Tabari, Parvaneh; Dimitrakis, Georgios; Dodds, Christopher; Arnold, Thomas; Terrill, Nick J; Bras, Wim; Hermida Merino, Daniel; Topham, Paul D; Irvine, Derek J; Howse, Jonathan R

    2017-08-09

    Microwave annealing has emerged as an alternative to traditional thermal annealing approaches for optimising block copolymer self-assembly. A novel sample environment enabling small angle X-ray scattering to be performed in situ during microwave annealing is demonstrated, which has enabled, for the first time, the direct study of the effects of microwave annealing upon the self-assembly behavior of a model, commercial triblock copolymer system [polystyrene-block-poly(ethylene-co-butylene)-block-polystyrene]. Results show that the block copolymer is a poor microwave absorber, resulting in no change in the block copolymer morphology upon application of microwave energy. The block copolymer species may only indirectly interact with the microwave energy when a small molecule microwave-interactive species [diethylene glycol dibenzoate (DEGDB)] is incorporated directly into the polymer matrix. Then significant morphological development is observed at DEGDB loadings ≥6 wt%. Through spatial localisation of the microwave-interactive species, we demonstrate targeted annealing of specific regions of a multi-component system, opening routes for the development of "smart" manufacturing methodologies.

  10. Spin-Orbital Excitations in Ca2RuO4 Revealed by Resonant Inelastic X-Ray Scattering

    DEFF Research Database (Denmark)

    Das, L.; Forte, F.; Fittipaldi, R.

    2018-01-01

    The strongly correlated insulator Ca2RuO4 is considered as a paradigmatic realization of both spin-orbital physics and a band-Mott insulating phase, characterized by orbitally selective coexistence of a band and a Mott gap. We present a high resolution oxygen K-edge resonant inelastic x-ray scatt......-Mott scenario. The high-energy excitations correspond to intra-atomic singlet-triplet transitions at an energy scale set by Hund's coupling. Our findings give a unifying picture of the spin and orbital excitations in the band-Mott insulator Ca2RuO4.......The strongly correlated insulator Ca2RuO4 is considered as a paradigmatic realization of both spin-orbital physics and a band-Mott insulating phase, characterized by orbitally selective coexistence of a band and a Mott gap. We present a high resolution oxygen K-edge resonant inelastic x......-ray scattering study of the antiferromagnetic Mott insulating state of Ca2RuO4. A set of low-energy (about 80 and 400 meV) and high-energy (about 1.3 and 2.2 eV) excitations are reported, which show strong incident light polarization dependence. Our results strongly support a spin-orbit coupled band...

  11. Spin-Orbital Excitations in Ca_{2}RuO_{4} Revealed by Resonant Inelastic X-Ray Scattering

    Directory of Open Access Journals (Sweden)

    L. Das

    2018-03-01

    Full Text Available The strongly correlated insulator Ca_{2}RuO_{4} is considered as a paradigmatic realization of both spin-orbital physics and a band-Mott insulating phase, characterized by orbitally selective coexistence of a band and a Mott gap. We present a high resolution oxygen K-edge resonant inelastic x-ray scattering study of the antiferromagnetic Mott insulating state of Ca_{2}RuO_{4}. A set of low-energy (about 80 and 400 meV and high-energy (about 1.3 and 2.2 eV excitations are reported, which show strong incident light polarization dependence. Our results strongly support a spin-orbit coupled band-Mott scenario and explore in detail the nature of its exotic excitations. Guided by theoretical modeling, we interpret the low-energy excitations as a result of composite spin-orbital excitations. Their nature unveils the intricate interplay of crystal-field splitting and spin-orbit coupling in the band-Mott scenario. The high-energy excitations correspond to intra-atomic singlet-triplet transitions at an energy scale set by Hund’s coupling. Our findings give a unifying picture of the spin and orbital excitations in the band-Mott insulator Ca_{2}RuO_{4}.

  12. An in situ grazing incidence x-ray scattering study of block copolymer thin films during solvent vapor annealing

    Science.gov (United States)

    Gu, Xiaodan; Gunkel, Ilja; Hexemer, Alexander; Russell, Thomas

    2014-03-01

    Although solvent vapor annealing (SVA) has been widely applied to block copolymer (BCP) thin films to obtain well-ordered microdomains, the mechanism of enhancing lateral order is not well understood. Here, we used real time in situ grazing-incidence small-angle x-ray scattering (in situGISAXS) to study the self-assembly of PS-b-P2VP BCP BCPs with different molecular weights thin films in THF vapor, a near neutral solvent for both blocks. Both swelling and deswelling behavior of BCP thin films were examined. The extent of swellingand the solvent removal rate not only affect the domain spacing of BCPs but also dictate the extent of lateral ordering of the BCP microdomains. Larger grains were observed at higher values of the swelling ratio (close to disordering). To preserve the maximal lateral ordering of the microdomains in the swollen state, the fastest solvent removal rate is required to freeze in the ordered microdomain structure of the swollen BCP film. We thanks support from U.S. Department of Energy BES under contract BES-DE-FG02-96ER45612 and ALS doctoral fellowship.

  13. Quantitative Characterization of Configurational Space Sampled by HIV-1 Nucleocapsid Using Solution NMR, X-ray Scattering and Protein Engineering.

    Science.gov (United States)

    Deshmukh, Lalit; Schwieters, Charles D; Grishaev, Alexander; Clore, G Marius

    2016-06-03

    Nucleic-acid-related events in the HIV-1 replication cycle are mediated by nucleocapsid, a small protein comprising two zinc knuckles connected by a short flexible linker and flanked by disordered termini. Combining experimental NMR residual dipolar couplings, solution X-ray scattering and protein engineering with ensemble simulated annealing, we obtain a quantitative description of the configurational space sampled by the two zinc knuckles, the linker and disordered termini in the absence of nucleic acids. We first compute the conformational ensemble (with an optimal size of three members) of an engineered nucleocapsid construct lacking the N- and C-termini that satisfies the experimental restraints, and then validate this ensemble, as well as characterize the disordered termini, using the experimental data from the full-length nucleocapsid construct. The experimental and computational strategy is generally applicable to multidomain proteins. Differential flexibility within the linker results in asymmetric motion of the zinc knuckles which may explain their functionally distinct roles despite high sequence identity. One of the configurations (populated at a level of ≈40 %) closely resembles that observed in various ligand-bound forms, providing evidence for conformational selection and a mechanistic link between protein dynamics and function. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Electron Dynamics in the Core-Excited CS_{2} Molecule Revealed through Resonant Inelastic X-Ray Scattering Spectroscopy

    Directory of Open Access Journals (Sweden)

    T. Marchenko

    2015-08-01

    Full Text Available We present an experimental and theoretical study of resonant inelastic x-ray scattering (RIXS in the carbon disulphide CS_{2} molecule near the sulfur K-absorption edge. We observe a strong evolution of the RIXS spectral profile with the excitation energy tuned below the lowest unoccupied molecular orbital (LUMO absorption resonance. The reason for this is twofold. Reducing the photon energy in the vicinity of the LUMO absorption resonance leads to a relative suppression of the LUMO contribution with respect to the emission signal from the higher unoccupied molecular orbitals, which results in the modulation of the total RIXS profile. At even larger negative photon-energy detuning from the resonance, the excitation-energy dependence of the RIXS profile is dominated by the onset of electron dynamics triggered by a coherent excitation of multiple electronic states. Furthermore, our study demonstrates that in the hard x-ray regime, localization of the S 1s core hole occurs in CS_{2} during the RIXS process because of the orientational dephasing of interference between the waves scattering on the two sulfur atoms. Core-hole localization leads to violation of the symmetry selection rules for the electron transitions observed in the spectra.

  15. Fluid adsorption in ordered mesoporous solids determined by in situ small-angle X-ray scattering.

    Science.gov (United States)

    Findenegg, Gerhard H; Jähnert, Susanne; Müter, Dirk; Prass, Johannes; Paris, Oskar

    2010-07-14

    The adsorption of two organic fluids (n-pentane and perfluoropentane) in a periodic mesoporous silica material (SBA-15) is investigated by in situ small-angle X-ray scattering (SAXS) using synchrotron radiation. Structural changes are monitored as the ordered and disordered pores in the silica matrix are gradually filled with the fluids. The experiments yield integrated peak intensities from up to ten Bragg reflections from the 2D hexagonal pore lattice, and additionally diffuse scattering contributions arising from disordered (mostly intrawall) porosity. The analysis of the scattering data is based on a separation of these two contributions. Bragg scattering is described by adopting a form factor model for ordered pores of cylindrical symmetry which accounts for the filling of the microporous corona, the formation of a fluid film at the pore walls, and condensation of the fluid in the core. The filling fraction of the disordered intrawall pores is extracted from the diffuse scattering intensity and its dependence on the fluid pressure is analyzed on the basis of a three-phase model. The data analysis introduced here provides an important generalisation of a formalism presented recently (J. Phys. Chem. C, 2009, 13, 15201), which was applicable to contrast-matching fluids only. In this way, the adsorption behaviour of fluids into ordered and disordered pores in periodic mesoporous materials can be analyzed quantitatively irrespective of the fluid density.

  16. Review of the fundamental theories behind small angle X-ray scattering, molecular dynamics simulations, and relevant integrated application.

    Science.gov (United States)

    Boldon, Lauren; Laliberte, Fallon; Liu, Li

    2015-01-01

    In this paper, the fundamental concepts and equations necessary for performing small angle X-ray scattering (SAXS) experiments, molecular dynamics (MD) simulations, and MD-SAXS analyses were reviewed. Furthermore, several key biological and non-biological applications for SAXS, MD, and MD-SAXS are presented in this review; however, this article does not cover all possible applications. SAXS is an experimental technique used for the analysis of a wide variety of biological and non-biological structures. SAXS utilizes spherical averaging to produce one- or two-dimensional intensity profiles, from which structural data may be extracted. MD simulation is a computer simulation technique that is used to model complex biological and non-biological systems at the atomic level. MD simulations apply classical Newtonian mechanics' equations of motion to perform force calculations and to predict the theoretical physical properties of the system. This review presents several applications that highlight the ability of both SAXS and MD to study protein folding and function in addition to non-biological applications, such as the study of mechanical, electrical, and structural properties of non-biological nanoparticles. Lastly, the potential benefits of combining SAXS and MD simulations for the study of both biological and non-biological systems are demonstrated through the presentation of several examples that combine the two techniques.

  17. 1s2p resonant inelastic X-ray scattering combined dipole and quadrupole analysis method

    DEFF Research Database (Denmark)

    Bagger, Alexander; Haarman, Ties; Molina, Anna Puig

    2017-01-01

    , it is shown that only in the case of quadrupole excitations being present is additional information gained by RIXS compared with XAS. Combining this knowledge with methods to calculate the dipole contribution in XAS measurements gives scientists the opportunity to plan more effective experiments....

  18. Background radiation in inelastic X-ray scattering and X-ray emission spectroscopy. A study for Johann-type spectrometers

    Science.gov (United States)

    Paredes Mellone, O. A.; Bianco, L. M.; Ceppi, S. A.; Goncalves Honnicke, M.; Stutz, G. E.

    2018-06-01

    A study of the background radiation in inelastic X-ray scattering (IXS) and X-ray emission spectroscopy (XES) based on an analytical model is presented. The calculation model considers spurious radiation originated from elastic and inelastic scattering processes along the beam paths of a Johann-type spectrometer. The dependence of the background radiation intensity on the medium of the beam paths (air and helium), analysed energy and radius of the Rowland circle was studied. The present study shows that both for IXS and XES experiments the background radiation is dominated by spurious radiation owing to scattering processes along the sample-analyser beam path. For IXS experiments the spectral distribution of the main component of the background radiation shows a weak linear dependence on the energy for the most cases. In the case of XES, a strong non-linear behaviour of the background radiation intensity was predicted for energy analysis very close to the backdiffraction condition, with a rapid increase in intensity as the analyser Bragg angle approaches π / 2. The contribution of the analyser-detector beam path is significantly weaker and resembles the spectral distribution of the measured spectra. Present results show that for usual experimental conditions no appreciable structures are introduced by the background radiation into the measured spectra, both in IXS and XES experiments. The usefulness of properly calculating the background profile is demonstrated in a background subtraction procedure for a real experimental situation. The calculation model was able to simulate with high accuracy the energy dependence of the background radiation intensity measured in a particular XES experiment with air beam paths.

  19. Quantitative analysis of thermal diffuse X-ray scattering on single crystals. Communication 2. FCC metals

    International Nuclear Information System (INIS)

    Najsh, V.E.; Novoselova, T.V.; Sagaradze, I.V.; Kvyatkovskij, B.E.; Fedorov, V.I.; Chernenkov, Yu.P.

    1994-01-01

    With the use of X-ray diffractometer a study was made into the intensity of diffuse scattering in Ni crystals with FCC lattice. Earlier accomplished quantitative analysis for BCC crystals was extended to FCC lattices. Comparative evaluation was made for cooperative thermal oscillation patterns and corresponding diffuse scattering in crystals of various structures. Measurements on FCC crystals were carried out at room temperature using AgK a lpha-radiation in 96 points of Ni crystal. 8 refs., 4 figs

  20. A Microbeam Small-Angle X-ray Scattering Study on Enamel Crystallites in Subsurface Lesion

    Energy Technology Data Exchange (ETDEWEB)

    Yagi, N; Ohta, N; Matsuo, T [Japan Synchrotron Radiation Research Institute, 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan); Tanaka, T; Terada, Y; Kamasaka, H; Kometani, T, E-mail: yagi@spring8.or.j [Ezaki Glico Co. Ltd., 4-6-5 Utajima, Nishiyodogawa-ku, Osaka 555-8502 (Japan)

    2010-10-01

    The early caries lesion in bovine tooth enamel was studied by two different X-ray diffraction systems at the SPring-8 third generation synchrotron radiation facility. Both allowed us simultaneous measurement of the small and large angle regions. The beam size was 6{mu}m at BL40XU and 50{mu}m at BL45XU. The small-angle scattering from voids in the hydroxyapatite crystallites and the wide-angle diffraction from the hydroxyapatite crystals were observed simultaneously. At BL40XU an X-ray image intensifier was used for the small-angle and a CMOS flatpanel detector for the large-angle region. At BL45XU, a large-area CCD detector was used to cover both regions. A linear microbeam scan at BL40XU showed a detailed distribution of voids and crystals and made it possible to examine the structural details in the lesion. The two-dimensional scan at BL45XU showed distribution of voids and crystals in a wider region in the enamel. The simultaneous small- and wide-angle measurement with a microbeam is a powerful tool to elucidate the mechanisms of demineralization and remineralization in the early caries lesion.

  1. A Microbeam Small-Angle X-ray Scattering Study on Enamel Crystallites in Subsurface Lesion

    International Nuclear Information System (INIS)

    Yagi, N; Ohta, N; Matsuo, T; Tanaka, T; Terada, Y; Kamasaka, H; Kometani, T

    2010-01-01

    The early caries lesion in bovine tooth enamel was studied by two different X-ray diffraction systems at the SPring-8 third generation synchrotron radiation facility. Both allowed us simultaneous measurement of the small and large angle regions. The beam size was 6μm at BL40XU and 50μm at BL45XU. The small-angle scattering from voids in the hydroxyapatite crystallites and the wide-angle diffraction from the hydroxyapatite crystals were observed simultaneously. At BL40XU an X-ray image intensifier was used for the small-angle and a CMOS flatpanel detector for the large-angle region. At BL45XU, a large-area CCD detector was used to cover both regions. A linear microbeam scan at BL40XU showed a detailed distribution of voids and crystals and made it possible to examine the structural details in the lesion. The two-dimensional scan at BL45XU showed distribution of voids and crystals in a wider region in the enamel. The simultaneous small- and wide-angle measurement with a microbeam is a powerful tool to elucidate the mechanisms of demineralization and remineralization in the early caries lesion.

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

    International Nuclear Information System (INIS)

    Rodricks, B.

    1994-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Larson, B.C.

    1999-05-23

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

  4. Simulated x-ray scattering of protein solutions using explicit-solvent models

    International Nuclear Information System (INIS)

    Park, Sanghyun; Bardhan, Jaydeep P.; Makowski, Lee; Roux, Benoit

    2009-01-01

    X-ray solution scattering shows new promise for the study of protein structures, complementing crystallography and nuclear magnetic resonance. In order to realize the full potential of solution scattering, it is necessary to not only improve experimental techniques but also develop accurate and efficient computational schemes to relate atomistic models to measurements. Previous computational methods, based on continuum models of water, have been unable to calculate scattering patterns accurately, especially in the wide-angle regime which contains most of the information on the secondary, tertiary, and quaternary structures. Here we present a novel formulation based on the atomistic description of water, in which scattering patterns are calculated from atomic coordinates of protein and water. Without any empirical adjustments, this method produces scattering patterns of unprecedented accuracy in the length scale between 5 and 100 A, as we demonstrate by comparing simulated and observed scattering patterns for myoglobin and lysozyme.

  5. Low-angle X-ray scattering properties of irradiated spices

    International Nuclear Information System (INIS)

    Almeida, A.P.G.; Braz, D.; Barroso, R.C.; Lopes, R.T.

    2007-01-01

    The scattering of X-rays at low angles (LAXS) is a technique dominated by the coherent scattering process. One characteristic observation of low-angle coherent scattering is the so-called molecular interference effect, being characterized by the presence of one or more peaks in the forward direction of scattering. In the present study, LAXS profiles from five different spices are carefully measured in order to establish characteristic scattering signatures. Samples of Ceylon cinnamon, cumin, nutmeg, paprika and black pepper were bought in local market in Rio de Janeiro, Brazil. The LAXS patterns were obtained using a Shimadzu DRX 6000 diffractometer in reflection geometry. Coherent scattering patterns are measured for the samples for θ=5-35 o . The data were collected in 0.05 o increments every 3 s. In order to evaluate the possible molecular structure changes caused to the irradiation procedure, the signatures obtained for control (non-irradiated) spices were compared with spice samples irradiated with different doses varying from 3 to 40 kGy. The LAXS patterns of all samples were obtained after 30, 60, 90, 120 days to evaluate the effect of storage period. Scattering profiles from spices irradiated with different irradiation doses were obtained and the results compared. For each spice, there is no considerable deviation in shape in function of the irradiation dose. It indicates that the molecular structure of each analyzed spices is preserved considering the dose range chosen. The results show that the molecular structure was found to be stable during storage at the ambient temperature for up to 4 months

  6. Structure factor of blends of solvent-free nanoparticle–organic hybrid materials: density-functional theory and small angle X-ray scattering

    KAUST Repository

    Yu, Hsiu-Yu

    2014-09-15

    © the Partner Organisations 2014. We investigate the static structure factor S(q) of solvent-free nanoparticle-organic hybrid materials consisting of silica nanocores and space-filling polyethylene glycol coronas using a density-functional theory and small angle X-ray scattering measurements. The theory considers a bidisperse suspension of hard spheres with different radii and tethered bead-spring oligomers with different grafting densities to approximate the polydispersity effects in experiments. The experimental systems studied include pure samples with different silica core volume fractions and the associated mean corona grafting densities, and blends with different mixing ratios of the pure samples, in order to introduce varying polydispersity of corona grafting density. Our scattering experiments and theory show that, compared to the hard-sphere suspension with the same core volume fraction, S(q) for pure samples exhibit both substantially smaller values at small q and stronger particle correlations corresponding to a larger effective hard core at large q, indicating that the tethered incompressible oligomers enforce a more uniform particle distribution, and the densely grafted brush gives rise to an additional exclusionary effect between the nanoparticles. According to the theory, polydispersity in the oligomer grafting density controls the deviation of S(q) from the monodisperse system at smaller q, and the interplay of the enhanced effective core size and the entropic attraction among the particles is responsible for complex variations in the particle correlations at larger q. The successful comparison between the predictions and the measurements for the blends further suggests that S(q) can be used to assess the uniformity of grafting density in polymer-grafted nanoparticle materials. This journal is

  7. Structure factor of blends of solvent-free nanoparticle-organic hybrid materials: density-functional theory and small angle X-ray scattering.

    Science.gov (United States)

    Yu, Hsiu-Yu; Srivastava, Samanvaya; Archer, Lynden A; Koch, Donald L

    2014-12-07

    We investigate the static structure factor S(q) of solvent-free nanoparticle-organic hybrid materials consisting of silica nanocores and space-filling polyethylene glycol coronas using a density-functional theory and small angle X-ray scattering measurements. The theory considers a bidisperse suspension of hard spheres with different radii and tethered bead-spring oligomers with different grafting densities to approximate the polydispersity effects in experiments. The experimental systems studied include pure samples with different silica core volume fractions and the associated mean corona grafting densities, and blends with different mixing ratios of the pure samples, in order to introduce varying polydispersity of corona grafting density. Our scattering experiments and theory show that, compared to the hard-sphere suspension with the same core volume fraction, S(q) for pure samples exhibit both substantially smaller values at small q and stronger particle correlations corresponding to a larger effective hard core at large q, indicating that the tethered incompressible oligomers enforce a more uniform particle distribution, and the densely grafted brush gives rise to an additional exclusionary effect between the nanoparticles. According to the theory, polydispersity in the oligomer grafting density controls the deviation of S(q) from the monodisperse system at smaller q, and the interplay of the enhanced effective core size and the entropic attraction among the particles is responsible for complex variations in the particle correlations at larger q. The successful comparison between the predictions and the measurements for the blends further suggests that S(q) can be used to assess the uniformity of grafting density in polymer-grafted nanoparticle materials.

  8. Modeling X-Ray Scattering Process and Applications of the Scattering Model

    Science.gov (United States)

    Al-Jundi, Taher Lutfi

    1995-01-01

    Computer modeling of nondestructive inspections with x-rays is proving to be a very useful tool for enhancing the performance of these techniques. Two x-ray based inspection techniques are considered in this study. The first is "Radiographic Inspection", where an existing simulation model has been improved to account for scattered radiation effects. The second technique is "Inspection with Compton backscattering", where a new simulation model has been developed. The effect of scattered radiation on a simulated radiographic image can be insignificant, equally important, or more important than the effect of the uncollided flux. Techniques to account for the scattered radiation effects include Monte Carlo techniques, and solving the particle transport equation for photons. However, these two techniques although accurate, are computationally expensive and hence inappropriate for use in computer simulation of radiography. A less accurate approach but computationally efficient is the principle of buildup factors. Traditionally, buildup factors are defined for monoenergetic photons of energies typical of a nuclear reactor. In this work I have expanded the definition of buildup factors to include a bremsstrahlung spectrum of photons with energies typically used in radiography (keV's instead of MeV's). This expansion of the definition relies on an intensive experimental work to measure buildup factors for a white spectrum of x-rays. I have also developed a monte carlo code to reproduce the measured buildup factors. The code was then converted to a parallel code and distributed on a network of workstations to reduce the execution time. The second inspection technique is based on Compton backscattering, where photons are scattered at large angles, more than 90 degrees. The importance of this technique arises when the inspected object is very large, or when access is limited to only one side of the specimen. The downside of detecting photons from backscattering is the low

  9. Influence of X-ray scatter radiation on image quality in Digital Breast Tomosynthesis (DBT)

    International Nuclear Information System (INIS)

    Rodrigues, M.J.; Di Maria, S.; Baptista, M.; Belchior, A.; Afonso, J.; Venâncio, J.; Vaz, P.

    2017-01-01

    Digital breast tomosynthesis (DBT) is a quasi-three-dimensional imaging technique that was developed to solve the principal limitation of mammography, namely the overlapping tissue effect. This issue in standard mammography (SM) leads to two main problems: low sensitivity (difficulty to detect lesions) and low specificity (non-negligible percentage of false positives). Although DBT is now being introduced in clinical practice the features of this technique have not yet been fully and accurately assessed. Consequently, optimization studies in terms of choosing the most suitable parameters which maximize image quality according to the known limits of breast dosimetry are currently performing. In DBT, scatter radiation can lead to a loss of contrast and to an increase of image noise by reducing the signal-to-difference-noise ratio (SDNR) of a lesion. Moreover the use of an anti-scatter grid is a concern due to the low exposure of the photon flux available per projection. For this reason the main aim of this study was to analyze the influence of the scatter radiation on image quality and the dose delivered to the breast. In particular a detailed analysis of the scatter radiation on the optimal energy that maximizes the SDNR was performed for different monochromatic energies and voltages. To reach this objective the PenEasy Monte Carlo (MC) simulation tool imbedded in the general-purpose main program PENELOPE, was used. After a successful validation of the MC model with measurements, 2D projection images of primary, coherent and incoherent photons were obtained. For that, a homogeneous breast phantom (2, 4, 6, 8 cm) with 25%, 50% and 75% glandular compositions was used, including a 5 mm thick tumor. The images were generated for each monochromatic X-ray energies in the range from 16 keV to 32 keV. For each angular projection considered (25 angular projections covering an arc of 50°) the scatter-to-primary ratio (SPR), the mean glandular dose (MGD) and the signal

  10. Influence of X-ray scatter radiation on image quality in Digital Breast Tomosynthesis (DBT)

    Science.gov (United States)

    Rodrigues, M. J.; Di Maria, S.; Baptista, M.; Belchior, A.; Afonso, J.; Venâncio, J.; Vaz, P.

    2017-11-01

    Digital breast tomosynthesis (DBT) is a quasi-three-dimensional imaging technique that was developed to solve the principal limitation of mammography, namely the overlapping tissue effect. This issue in standard mammography (SM) leads to two main problems: low sensitivity (difficulty to detect lesions) and low specificity (non-negligible percentage of false positives). Although DBT is now being introduced in clinical practice the features of this technique have not yet been fully and accurately assessed. Consequently, optimization studies in terms of choosing the most suitable parameters which maximize image quality according to the known limits of breast dosimetry are currently performing. In DBT, scatter radiation can lead to a loss of contrast and to an increase of image noise by reducing the signal-to-difference-noise ratio (SDNR) of a lesion. Moreover the use of an anti-scatter grid is a concern due to the low exposure of the photon flux available per projection. For this reason the main aim of this study was to analyze the influence of the scatter radiation on image quality and the dose delivered to the breast. In particular a detailed analysis of the scatter radiation on the optimal energy that maximizes the SDNR was performed for different monochromatic energies and voltages. To reach this objective the PenEasy Monte Carlo (MC) simulation tool imbedded in the general-purpose main program PENELOPE, was used. After a successful validation of the MC model with measurements, 2D projection images of primary, coherent and incoherent photons were obtained. For that, a homogeneous breast phantom (2, 4, 6, 8 cm) with 25%, 50% and 75% glandular compositions was used, including a 5 mm thick tumor. The images were generated for each monochromatic X-ray energies in the range from 16 keV to 32 keV. For each angular projection considered (25 angular projections covering an arc of 50°) the scatter-to-primary ratio (SPR), the mean glandular dose (MGD) and the signal

  11. Library based x-ray scatter correction for dedicated cone beam breast CT

    International Nuclear Information System (INIS)

    Shi, Linxi; Zhu, Lei; Vedantham, Srinivasan; Karellas, Andrew

    2016-01-01

    Purpose: The image quality of dedicated cone beam breast CT (CBBCT) is limited by substantial scatter contamination, resulting in cupping artifacts and contrast-loss in reconstructed images. Such effects obscure the visibility of soft-tissue lesions and calcifications, which hinders breast cancer detection and diagnosis. In this work, we propose a library-based software approach to suppress scatter on CBBCT images with high efficiency, accuracy, and reliability. Methods: The authors precompute a scatter library on simplified breast models with different sizes using the GEANT4-based Monte Carlo (MC) toolkit. The breast is approximated as a semiellipsoid with homogeneous glandular/adipose tissue mixture. For scatter correction on real clinical data, the authors estimate the breast size from a first-pass breast CT reconstruction and then select the corresponding scatter distribution from the library. The selected scatter distribution from simplified breast models is spatially translated to match the projection data from the clinical scan and is subtracted from the measured projection for effective scatter correction. The method performance was evaluated using 15 sets of patient data, with a wide range of breast sizes representing about 95% of general population. Spatial nonuniformity (SNU) and contrast to signal deviation ratio (CDR) were used as metrics for evaluation. Results: Since the time-consuming MC simulation for library generation is precomputed, the authors’ method efficiently corrects for scatter with minimal processing time. Furthermore, the authors find that a scatter library on a simple breast model with only one input parameter, i.e., the breast diameter, sufficiently guarantees improvements in SNU and CDR. For the 15 clinical datasets, the authors’ method reduces the average SNU from 7.14% to 2.47% in coronal views and from 10.14% to 3.02% in sagittal views. On average, the CDR is improved by a factor of 1.49 in coronal views and 2.12 in sagittal

  12. Library based x-ray scatter correction for dedicated cone beam breast CT

    Energy Technology Data Exchange (ETDEWEB)

    Shi, Linxi; Zhu, Lei, E-mail: leizhu@gatech.edu [Nuclear and Radiological Engineering and Medical Physics Programs, The George W. Woodruff School of Mechanical Engineering, Georgia Institute of Technology, Atlanta, Georgia 30332 (United States); Vedantham, Srinivasan; Karellas, Andrew [Department of Radiology, University of Massachusetts Medical School, Worcester, Massachusetts 01655 (United States)

    2016-08-15

    Purpose: The image quality of dedicated cone beam breast CT (CBBCT) is limited by substantial scatter contamination, resulting in cupping artifacts and contrast-loss in reconstructed images. Such effects obscure the visibility of soft-tissue lesions and calcifications, which hinders breast cancer detection and diagnosis. In this work, we propose a library-based software approach to suppress scatter on CBBCT images with high efficiency, accuracy, and reliability. Methods: The authors precompute a scatter library on simplified breast models with different sizes using the GEANT4-based Monte Carlo (MC) toolkit. The breast is approximated as a semiellipsoid with homogeneous glandular/adipose tissue mixture. For scatter correction on real clinical data, the authors estimate the breast size from a first-pass breast CT reconstruction and then select the corresponding scatter distribution from the library. The selected scatter distribution from simplified breast models is spatially translated to match the projection data from the clinical scan and is subtracted from the measured projection for effective scatter correction. The method performance was evaluated using 15 sets of patient data, with a wide range of breast sizes representing about 95% of general population. Spatial nonuniformity (SNU) and contrast to signal deviation ratio (CDR) were used as metrics for evaluation. Results: Since the time-consuming MC simulation for library generation is precomputed, the authors’ method efficiently corrects for scatter with minimal processing time. Furthermore, the authors find that a scatter library on a simple breast model with only one input parameter, i.e., the breast diameter, sufficiently guarantees improvements in SNU and CDR. For the 15 clinical datasets, the authors’ method reduces the average SNU from 7.14% to 2.47% in coronal views and from 10.14% to 3.02% in sagittal views. On average, the CDR is improved by a factor of 1.49 in coronal views and 2.12 in sagittal

  13. Structure and optical function of amorphous photonic nanostructures from avian feather barbs: a comparative small angle X-ray scattering (SAXS) analysis of 230 bird species.

    Science.gov (United States)

    Saranathan, Vinodkumar; Forster, Jason D; Noh, Heeso; Liew, Seng-Fatt; Mochrie, Simon G J; Cao, Hui; Dufresne, Eric R; Prum, Richard O

    2012-10-07

    Non-iridescent structural colours of feathers are a diverse and an important part of the phenotype of many birds. These colours are generally produced by three-dimensional, amorphous (or quasi-ordered) spongy β-keratin and air nanostructures found in the medullary cells of feather barbs. Two main classes of three-dimensional barb nanostructures are known, characterized by a tortuous network of air channels or a close packing of spheroidal air cavities. Using synchrotron small angle X-ray scattering (SAXS) and optical spectrophotometry, we characterized the nanostructure and optical function of 297 distinctly coloured feathers from 230 species belonging to 163 genera in 51 avian families. The SAXS data provided quantitative diagnoses of the channel- and sphere-type nanostructures, and confirmed the presence of a predominant, isotropic length scale of variation in refractive index that produces strong reinforcement of a narrow band of scattered wavelengths. The SAXS structural data identified a new class of rudimentary or weakly nanostructured feathers responsible for slate-grey, and blue-grey structural colours. SAXS structural data provided good predictions of the single-scattering peak of the optical reflectance of the feathers. The SAXS structural measurements of channel- and sphere-type nanostructures are also similar to experimental scattering data from synthetic soft matter systems that self-assemble by phase separation. These results further support the hypothesis that colour-producing protein and air nanostructures in feather barbs are probably self-assembled by arrested phase separation of polymerizing β-keratin from the cytoplasm of medullary cells. Such avian amorphous photonic nanostructures with isotropic optical properties may provide biomimetic inspiration for photonic technology.

  14. Liquid Structure of CO 2 –Reactive Aprotic Heterocyclic Anion Ionic Liquids from X-ray Scattering and Molecular Dynamics

    Energy Technology Data Exchange (ETDEWEB)

    Sheridan, Quintin R.; Oh, Seungmin; Morales-Collazo, Oscar; Castner, Jr., Edward W.; Brennecke, Joan F.; Maginn, Edward J. (Rutgers); (Notre)

    2016-11-23

    A combination of X-ray scattering experiments and molecular dynamics simulations were conducted to investigate the structure of ionic liquids (ILs) which chemically bind CO2. The structure functions were measured and computed for four different ILs consisting of two different phosphonium cations, triethyloctylphosphonium ([P2228]+) and trihexyltetradecylphosphonium ([P66614]+), paired with two different aprotic heterocyclic anions which chemically react with CO2, 2-cyanopyrrolide, and 1,2,4-triazolide. Simulations were able to reproduce the experimental structure functions, and by deconstructing the simulated structure functions, further information on the liquid structure was obtained. All structure functions of the ILs studied had three primary features which have been seen before in other ILs: a prepeak near 0.3–0.4 Å–1 corresponding to polar/nonpolar domain alternation, a charge alternation peak near 0.8 Å–1, and a peak near 1.5 Å–1 due to interactions of adjacent molecules. The liquid structure functions were only mildly sensitive to the specific anion and whether or not they were reacted with CO2. Upon reacting with CO2, small changes were observed in the structure functions of the [P2228]+ ILs, whereas virtually no change was observed upon reacting with CO2 in the corresponding [P66614]+ ILs. When the [P2228]+ cation was replaced with the [P66614]+ cation, there was a significant increase in the intensities of the prepeak and adjacency interaction peak. While many of the liquid structure functions are similar, the actual liquid structures differ as demonstrated by computed spatial distribution functions.

  15. In-Situ Monitoring of the Microstructure of TATB-based Explosive Formulations During Temperature Cycling using Ultra-small Angle X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Willey, T M; Hoffman, D M; van Buuren, T; Lauderbach, L; Ilavsky, J; Gee, R H; Maiti, A; Overturf, G; Fried, L

    2008-02-06

    TATB (1,3,5 triamino-2,4,6-trinitrobenzene), an extremely insensitive explosive, is used both in plastic-bonded explosives (PBXs) and as an ultra-fine pressed powder (UFTATB). With both PBXs and UFTATB, an irreversible expansion occurs with temperature cycling known as ratchet growth. In TATB-based explosives using Kel-F 800 as binder (LX-17 and PBX-9502), additional voids, sizes hundreds of nanometers to a few microns account for much of the volume expansion caused by temperature cycling. These voids are in the predicted size regime for hot-spot formation during ignition and detonation, and thus an experimental measure of these voids is important feedback for hot-spot theory and for determining the relationship between void size distributions and detonation properties. Also, understanding the mechanism of ratchet growth allows future choice of explosive/binder mixtures to minimize these types of changes to explosives, further extending PBX shelf life. This paper presents the void size distributions of LX-17, UFTATB, and PBXs using commercially available Cytop M, Cytop A, and Hyflon AD60 binders during temperature cycling between -55 C and 70 C. These void size distributions are derived from ultra-small angle x-ray scattering (USAXS), a technique sensitive to structures from about 10 nm to about 2 mm. Structures with these sizes do not appreciably change in UFTATB, indicating voids or cracks larger than a few microns appear in UFTATB during temperature cycling. Compared to Kel-F 800 binders, Cytop M and Cytop A show relatively small increases in void volume from 0.9% to 1.3% and 0.6% to 1.1%, respectively, while Hyflon fails to prevent irreversible volume expansion (1.2% to 4.6%). Computational mesoscale models of ratchet growth and binder wetting and adhesion properties point to mechanisms of ratchet growth, and are discussed in combination with the experimental results.

  16. Pepsi-SAXS: an adaptive method for rapid and accurate computation of small-angle X-ray scattering profiles.

    Science.gov (United States)

    Grudinin, Sergei; Garkavenko, Maria; Kazennov, Andrei

    2017-05-01

    A new method called Pepsi-SAXS is presented that calculates small-angle X-ray scattering profiles from atomistic models. The method is based on the multipole expansion scheme and is significantly faster compared with other tested methods. In particular, using the Nyquist-Shannon-Kotelnikov sampling theorem, the multipole expansion order is adapted to the size of the model and the resolution of the experimental data. It is argued that by using the adaptive expansion order, this method has the same quadratic dependence on the number of atoms in the model as the Debye-based approach, but with a much smaller prefactor in the computational complexity. The method has been systematically validated on a large set of over 50 models collected from the BioIsis and SASBDB databases. Using a laptop, it was demonstrated that Pepsi-SAXS is about seven, 29 and 36 times faster compared with CRYSOL, FoXS and the three-dimensional Zernike method in SAStbx, respectively, when tested on data from the BioIsis database, and is about five, 21 and 25 times faster compared with CRYSOL, FoXS and SAStbx, respectively, when tested on data from SASBDB. On average, Pepsi-SAXS demonstrates comparable accuracy in terms of χ 2 to CRYSOL and FoXS when tested on BioIsis and SASBDB profiles. Together with a small allowed variation of adjustable parameters, this demonstrates the effectiveness of the method. Pepsi-SAXS is available at http://team.inria.fr/nano-d/software/pepsi-saxs.

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

    Science.gov (United States)

    Shannon, Robert Francis, Jr.

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

  18. Tertiary and quaternary structural differences between two genetic variants of bovine casein by small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Pessen, H.; Kumosinski, T.F.; Farrell, H.M. Jr.; Brumberger, H.

    1991-01-01

    The casein complexes of bovine milk consist of four major protein fractions, alpha s1, alpha s2, beta, and kappa. Colloidal particles of casein (termed micelles) contain inorganic calcium and phosphate; they are very roughly spherical with an average radius of 650 A. Removal of Ca2+ leads to the formation of smaller protein aggregates with an average radius of 94 A. Two genetic variants, A and B, of the predominant fraction, alpha s1-casein, result in milks with markedly different physical properties, such as solubility and heat stability. To investigate the molecular basis for these differences, small-angle X-ray scattering was performed on the respective colloidal micelles and submicelles. Scattering curves for submicelles of both variants showed multiple Gaussian character; data for the B variant were previously interpreted in terms of two concentric regions of different electron density, i.e., a compact core and a relatively loose shell. For the submicelle of A, there was a third Gaussian, reflecting a negative contribution due to interparticle interference. Molecular parameters for submicelles of both A and B are in agreement with hydrodynamic data in the literature. Data for the micelles, for which scattering yields cross-sectional information, were fitted by a sum of three Gaussians for both variants; for these, the corresponding two lower radii of gyration represent the two concentric regions of the submicelles, while the third reflects the average packing of submicelles within the micellar cross section. Most of the molecular parameters obtained showed small but consistent differences between A and B, but for submicelles within the micelle several differences were particularly notable: A has a greater molecular weight for the compact region of the constituent submicelle (82,000 vs 60,000) and a much greater submicellar packing number

  19. Assessment of Escherichia coli selenophosphate synthetase oligomeric states by analytical ultracentrifugation and small angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Silva, I.R.; Faim, F.M.; Oliveira Neto, M.; Thiemann, O.H. [Universidade de Sao Paulo (USP-SC), Sao Carlos, SP (Brazil); Borges, J.C. [Universidade de Sao Paulo (IQSC/USP), Sao Carlos, SP (Brazil). Inst. de Quimica

    2012-07-01

    Full text: Selenium is an essential micronutrient for many organisms and is present in selenium-containing proteins as selenocysteine (Sec) and RNAs as selenouridine. Specific selenium incorporation into selenoproteins and RNAs requires the generation of a biologically active selenium donor compound, selenophosphate, which is produced from the activation of selenide with adenosine 5-triphosphate (ATP) in a reaction catalyzed by Selenophosphate Synthetase (SELD). Therefore, SELD is a key enzyme of the selenium pathway in the cell. The Escherichia coli SELD open reading frame was cloned into pET28a (Novagen) expression vector and the recombinant protein was over expressed in Escherichia coli BL21(DE3) strain. In order to purify the protein, we used metal-chelate affinity chromatography followed by a gel filtration step. Analytical Ultracentrifugation (AUC) and Small Angle X-ray Scattering (SAXS) were employed to study the oligomeric states of the soluble protein. The results of AUC revealed dimer-tetramer and tetramer-octamer equilibrium at low concentrations of protein, with dissociation constants of 70 2 and 560 40 M, respectively. Moreover, the SAXS results pointed the oligomeric state of the protein at higher concentrations as predominantly dimeric and the p(r) and the SAXS envelope revealed the SELD as elongated. We also performed initial crystallization trials with protein samples at 7 mg/ml in 96-well sitting-drop crystallization plates at room temperature using a crystallization robot. Needle crystals appeared after some days. X-ray diffraction for these crystals were tested in the MX2 beamline at the Brazilian Synchrotron Laboratory (LNLS Campinas). We are now working to improve these crystals in order to obtain suitable crystals for structure determination. (author)

  20. Fast electron and X-ray scattering as a tool to study target's structure

    Energy Technology Data Exchange (ETDEWEB)

    Amusia, M.Ya. [Racah Institute of Physics, Hebrew University, Jerusalem 91904 (Israel); A.F. Ioffe Physical-Technical Institute, St. Petersburg 194021 (Russian Federation)], E-mail: amusia@vms.huji.ac.il

    2007-06-15

    We concentrate on several relatively new aspects of the study of fast electron and X-ray scattering by atoms and atom-like objects, namely endohedral atoms and fullerenes. However, main attention is given to fast charge particle scattering. We show that the corresponding cross-sections, being expressed via so-called generalized oscillator strengths (GOS), give information on the electronic structure of the target and on the role of electron correlations in it. We consider what sort of information became available when analyzing the dependence of GOS upon their multipolarity, transferred momentum q and energy {omega}. To obtain theoretical results, we employ both the one-electron Hartree-Fock approximation and account for the multi-electron correlation in the target, using the random phase approximation with exchange. We demonstrate the role of non-dipole corrections in the small-angle fast-electron inelastic scattering. There dipole contribution dominates while non-dipole corrections can be considerably and controllably enhanced as compared to the case of low and medium energy photoionization. We show also that analyses of GOS for discrete level excitations permit to clarify their multipolarity. The results of calculations of Compton excitation and ionization cross-sections are presented. Attention is given to cooperative effects in inelastic fast electron-atom scattering that results in directed motion of the secondary electrons, a phenomenon that is similar to 'drag currents' in photoionization. We demonstrate how one should derive GOS for endohedral atoms, e.g. A-C{sub 60} and what is the additional information that can be obtained from corresponding GOS. Most of discussions are illustrated by the results of concrete calculations.

  1. Quantum theory for the dynamic structure factor in correlated two-component systems in nonequilibrium: Application to x-ray scattering

    Science.gov (United States)

    Vorberger, J.; Chapman, D. A.

    2018-01-01

    We present a quantum theory for the dynamic structure factors in nonequilibrium, correlated, two-component systems such as plasmas or warm dense matter. The polarization function, which is needed as the input for the calculation of the structure factors, is calculated in nonequilibrium based on a perturbation expansion in the interaction strength. To make our theory applicable for x-ray scattering, a generalized Chihara decomposition for the total electron structure factor in nonequilibrium is derived. Examples are given and the influence of correlations and exchange on the structure and the x-ray-scattering spectrum are discussed for a model nonequilibrium distribution, as often encountered during laser heating of materials, as well as for two-temperature systems.

  2. X-ray scattering and electron cryomicroscopy study on the effect of carotenoid biosynthesis to the structure of Chlorobium tepidum chlorosomes

    DEFF Research Database (Denmark)

    Ikonen, T P; Li, H; Psencík, J

    2007-01-01

    effect on chlorosome biogenesis and structure. The results indicate that carotenoids with a sufficiently long conjugated system are important for the biogenesis of the chlorosome baseplate. Defects in the baseplate structure affected the shape of the chlorosomes and were correlated with differences...... studied by means of x-ray scattering and electron cryomicroscopy. The chlorosomes from each mutant strain exhibited a lamellar arrangement of the bacteriochlorophyll c aggregates, which are the major constituents of the chlorosome interior. However, the carotenoid content and composition had a pronounced...... in the arrangement of lamellae and spacing between the lamellar planes of bacteriochlorophyll aggregates. In addition, comparisons among the various mutants enabled refinement of the assignments of the x-ray scattering peaks. While the main scattering peaks come from the lamellar structure of bacteriochlorophyll c...

  3. Quantum theory for the dynamic structure factor in correlated two-component systems in nonequilibrium: Application to x-ray scattering.

    Science.gov (United States)

    Vorberger, J; Chapman, D A

    2018-01-01

    We present a quantum theory for the dynamic structure factors in nonequilibrium, correlated, two-component systems such as plasmas or warm dense matter. The polarization function, which is needed as the input for the calculation of the structure factors, is calculated in nonequilibrium based on a perturbation expansion in the interaction strength. To make our theory applicable for x-ray scattering, a generalized Chihara decomposition for the total electron structure factor in nonequilibrium is derived. Examples are given and the influence of correlations and exchange on the structure and the x-ray-scattering spectrum are discussed for a model nonequilibrium distribution, as often encountered during laser heating of materials, as well as for two-temperature systems.

  4. Small-angle and wide-angle X-ray scattering study on the bilayer structure of synthetic and bovine heart cardiolipins

    Energy Technology Data Exchange (ETDEWEB)

    Takahashi, Hiroshi [Biophysics Laboratory, Department of Chemistry and Chemical Biology, Gunma University, Maebashi, Gunma, 371-8510 (Japan); Hayakawa, Tomohiro [Life Science Laboratory, Advanced Materials Laboratories, Sony Corporation, Yushima, Bunkyo-ku, Tokyo, 113-8510 (Japan); Ito, Kazuki; Takata, Masaki [Structural Materials Science Laboratory, RIKEN SPring-8 Center, Sayo, Hyogo 679-5148 (Japan); Kobayashi, Toshihide, E-mail: htakahas@chem-bio.gunma-u.ac.j [Lipid Biology Laboratory, RIKEN, Wako, Saitama 351-0198 (Japan)

    2010-10-01

    Cardiolipin (CL) is a membrane phospholipid containing four fatty acid chains. CL plays an important role in energy transformation in mitochondria. The disorder of CL biosynthesis is involved in a genetic disease, Barth syndrome. Alteration of fatty acid composition of CLs has been found in Barth syndrome patients, i.e., the decrease of unsaturated fatty acid chains. In this study, we investigated how the degree of saturation alters the structure of CL bilayers by using X-ray scattering. Bovine heart CL and two synthetic CLs were compared. Fatty acid compositions of these three CLs have different saturation. Small-angle X-ray scattering data showed that the decrease of the number of double bonds in the unsaturated fatty acid chains causes to thicken the CL bilayers. In addition, wide-angle X-ray scattering data suggested that the decrease reduces the degree of disorder of the hydrophobic region in a liquid crystalline phase. These results may be related to the dysfunction of mitochondria in Barth syndrome.

  5. Small-angle and wide-angle X-ray scattering study on the bilayer structure of synthetic and bovine heart cardiolipins

    International Nuclear Information System (INIS)

    Takahashi, Hiroshi; Hayakawa, Tomohiro; Ito, Kazuki; Takata, Masaki; Kobayashi, Toshihide

    2010-01-01

    Cardiolipin (CL) is a membrane phospholipid containing four fatty acid chains. CL plays an important role in energy transformation in mitochondria. The disorder of CL biosynthesis is involved in a genetic disease, Barth syndrome. Alteration of fatty acid composition of CLs has been found in Barth syndrome patients, i.e., the decrease of unsaturated fatty acid chains. In this study, we investigated how the degree of saturation alters the structure of CL bilayers by using X-ray scattering. Bovine heart CL and two synthetic CLs were compared. Fatty acid compositions of these three CLs have different saturation. Small-angle X-ray scattering data showed that the decrease of the number of double bonds in the unsaturated fatty acid chains causes to thicken the CL bilayers. In addition, wide-angle X-ray scattering data suggested that the decrease reduces the degree of disorder of the hydrophobic region in a liquid crystalline phase. These results may be related to the dysfunction of mitochondria in Barth syndrome.

  6. A Survey of Students from the National School on Neutron and X-ray Scattering: Communication Habits and Preferences

    Energy Technology Data Exchange (ETDEWEB)

    Bryant, Rebecca [Bryant Research, LLC

    2010-12-01

    Oak Ridge National Laboratory (ORNL) offers the scientific community unique access to two types of world-class neutron sources at a single site - the Spallation Neutron Source (SNS) and the High Flux Isotope Reactor (HFIR). The 85-MW HFIR provides one of the highest steady-state neutron fluxes of any research reactor in the world. And the SNS is one of the world's most intense pulse neutron beams. Management of these resources is the responsibility of the Neutron Sciences Directorate (NScD). NScD started conducting the National School on Neutron and X-ray Scattering (NXS) in conjunction with the Advanced Photon Source (APS) at Argonne National Laboratory in 2007. This survey was conducted to determine the most effective ways to reach students with information about what SNS and HFIR offer the scientific community, including content and communication vehicles. The emphasis is on gaining insights into compelling messages and the most effective channels, e.g., Web sites and social media, for communicating with students about neutron science The survey was conducted in two phases using a classic qualitative investigation to confirm language and content followed by a survey designed to quantify issues, assumptions, and working hypotheses. Phase I consisted of a focus group in late June 2010 with students attending NXS. The primary intent of the group was to inform development of an online survey. Phase two consisted of an online survey that was developed and pre-tested in July 2010 and launched on August 9, 2010 and remained in the field until September 9, 2010. The survey achieved an overall response rate of 48% for a total of 157 completions. The objective of this study is to determine the most effective ways to reach students with information about what SNS and HFIR offer the scientific community, including content and communication vehicles. The emphasis is on gaining insights into compelling messages and the most effective channels, e.g., Web sites, social

  7. Edible oil structures at low and intermediate concentrations. I. Modeling, computer simulation, and predictions for X ray scattering

    Science.gov (United States)

    Pink, David A.; Quinn, Bonnie; Peyronel, Fernanda; Marangoni, Alejandro G.

    2013-12-01

    found that TAGwoods aggregated via DLCA into clusters with fractal dimension D =1.7-1.8. As the simulations were run further, TAGwoods relaxed their positions in order to maximize the attractive interaction making the process look like reaction limited cluster-cluster aggregation with the fractal dimension increasing to D =2.0-2.1. For higher concentrations of CNPs, many TAGwood clusters were formed and, because of their weak interactions, were distributed randomly with D =3.0. We summarize the hierarchy of structures and make predictions for X-ray scattering.

  8. Structure development during isothermal crystallisation of high-density polyethylene: Synchrotron small-angle X-ray scattering study

    International Nuclear Information System (INIS)

    Ślusarczyk, Czesław

    2013-01-01

    Isothermal melt crystallisation in high-density polyethylene (HDPE) was studied using the time-resolved SAXS method with synchrotron radiation over a wide range of crystallisation temperatures. The SAXS profile was analysed by an interface distribution function, g 1 (r), which is a superposition of three contributions associated with the size distributions of crystalline (L C ) and amorphous (L A ) layers and a distribution of long period (LP). The morphological parameters extracted from the g 1 (r) functions show that the lamellar thickness increases with time, obeying a logarithmic time dependence. The time evolution of L C observed for the sample crystallised at 122 °C leads to the conclusion that crystallisation proceeds according to the mechanism of thickening growth. For samples crystallised at lower temperatures (116 °C and 118 °C), the lamellar thickening mechanism has been observed. The rate of lamellar thickening in these cases is much lower than that at 122 °C. At 40 °C, thickening of the crystalline layer does not occur. The interface distribution functions were deconvoluted, and the relative standard deviation σ C /L C obtained in this way is an additional parameter that is varied during crystallisation and can be used for analysis of this process. Time-dependent changes in the σ C /L C at large supercooling (T C =40 °C) indicates that L C presents a broad distribution in which the relative standard deviation increases with time. At lower supercooling (T C =122 °C), L C shows a much sharper distribution. In this case, the relative standard deviation decreases with time. - Highlights: • Isothermal melt crystallisation of high-density polyethylene (HDPE) was studied by time-resolved synchrotron small-angle X-ray scattering (SAXS) over a wide-range of supercoolings. • The SAXS profile was analysed by an interface distribution, g 1 (r), function. • At large supercooling (40 °C) the thickening of the crystalline layer does not occur. At

  9. A Survey of Students from the National School on Neutron and X-ray Scattering: Communication Habits and Preferences

    International Nuclear Information System (INIS)

    Bryant, Rebecca

    2010-01-01

    Oak Ridge National Laboratory (ORNL) offers the scientific community unique access to two types of world-class neutron sources at a single site - the Spallation Neutron Source (SNS) and the High Flux Isotope Reactor (HFIR). The 85-MW HFIR provides one of the highest steady-state neutron fluxes of any research reactor in the world. And the SNS is one of the world's most intense pulse neutron beams. Management of these resources is the responsibility of the Neutron Sciences Directorate (NScD). NScD started conducting the National School on Neutron and X-ray Scattering (NXS) in conjunction with the Advanced Photon Source (APS) at Argonne National Laboratory in 2007. This survey was conducted to determine the most effective ways to reach students with information about what SNS and HFIR offer the scientific community, including content and communication vehicles. The emphasis is on gaining insights into compelling messages and the most effective channels, e.g., Web sites and social media, for communicating with students about neutron science The survey was conducted in two phases using a classic qualitative investigation to confirm language and content followed by a survey designed to quantify issues, assumptions, and working hypotheses. Phase I consisted of a focus group in late June 2010 with students attending NXS. The primary intent of the group was to inform development of an online survey. Phase two consisted of an online survey that was developed and pre-tested in July 2010 and launched on August 9, 2010 and remained in the field until September 9, 2010. The survey achieved an overall response rate of 48% for a total of 157 completions. The objective of this study is to determine the most effective ways to reach students with information about what SNS and HFIR offer the scientific community, including content and communication vehicles. The emphasis is on gaining insights into compelling messages and the most effective channels, e.g., Web sites, social media

  10. Evolution and change of He bubbles in He-containing Ti films upon thermal treatment studied by small-angle X-ray scattering and transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Guangai [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); College of Nuclear Science and Technology, University of Science and Technology of China, Hefei, 230029 (China); Wu, Erdong, E-mail: ewu@imr.ac.cn [National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Huang, Chaoqiang [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); College of Nuclear Science and Technology, University of Science and Technology of China, Hefei, 230029 (China); Cheng, Chun [National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Yan, Guanyun [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); Wang, Xiaolin [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); College of Nuclear Science and Technology, University of Science and Technology of China, Hefei, 230029 (China); Liu, Shi [National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Tian, Qiang; Chen, Bo [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); Wu, Zhonghua [Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China); Liu, Yi; Wang, Jie [Institute of Shanghai Apply Physics, Chinese Academy of Sciences, Shanghai 201800 (China)

    2014-05-02

    Evolution and change of He bubbles in magnetron sputtering prepared He-containing Ti films under thermal treatment are studied by small-angle X-ray scattering (SAXS), transmission electron microscopy (TEM) and X-ray diffraction. Incorporation of He introduces a large number of He-vacancy clusters and some voids in the films, and significantly increases SAXS intensity and causes anisotropic scattering. The change of He induced defects during annealing is affected by thermal diffusion and migration of trapped He to the surface and between interfaces of He induced defects within the films. Annealing at 200 and 400 °C reduces intensity and anisotropy of SAXS, in accord with observed shrinking and disappearance of the voids. The simultaneous growth of non-uniformly distributed He bubbles to the sizes of 1–2 nm and a population level of 10{sup 5}/μm{sup 3} are detected in the temperature range. The changes are explained by migration and coalescence mechanisms, which requires low apparent activation energy. Inconsistence between TEM and SAXS observations is noted and attributed to thinning induced internal stress relaxation of TEM specimen. Remarkable enlargement of He bubbles, associated with increased SAXS intensity and fractal dimension, is observed after 600 °C annealing, indicating involvement of Ostwald Ripening (OR) mechanism. The OR process dominates at 800 °C, where the high temperature provides activation energy for accelerated He dissociation from small bubbles into larger ones, and generating textured microstructure and agglomerated bubble clusters. The inhomogeneous bubble size distribution observed at this temperature covers a broad range of about 10–50 nm and possessing a population density level of 10{sup 3}/μm{sup 3}. - Highlights: • Change of He bubbles in thermally treated Ti–He films is studied by SAXS and TEM. • SAXS reveals size distribution and fractional population of He bubbles in films. • He-vacancy clusters in Ti–He film

  11. Preliminary small-angle X-ray scattering and X-ray diffraction studies of the BTB domain of lola protein from Drosophila melanogaster

    Science.gov (United States)

    Boyko, K. M.; Nikolaeva, A. Yu.; Kachalova, G. S.; Bonchuk, A. N.; Dorovatovskii, P. V.; Popov, V. O.

    2017-11-01

    The Drosophila genome has several dozens of transcription factors (TTK group) containing BTB domains assembled into octamers. The LOLA protein belongs to this family. The purification, crystallization, and preliminary X-ray diffraction and small-angle X-ray scattering (SAXS) studies of the BTB domain of this protein are reported. The crystallization conditions were found by the vapor-diffusion technique. A very low diffraction resolution (8.7 Å resolution) of the crystals was insufficient for the determination of the threedimensional structure of the BTB domain. The SAXS study demonstrated that the BTB domain of the LOLA protein exists as an octamer in solution.

  12. Synchrotron small-angle x-ray scattering investigation on integral membrane protein light-harvesting complex LH2 from photosynthetic bacterium rhodopseudomonas acidophila

    International Nuclear Information System (INIS)

    Du Luchao; Weng Yuxiang; Hong Xinguo; Xian Dingchang; Kobayashi Katsumi

    2006-01-01

    Structures of membrane protein in solution are different from that in crystal phase. We present the primary results of small angle x-ray scattering (SAXS) resolved topological structures of a light harvesting antenna membrane protein complex LH2 from photosynthetic bacteria Rhodopseudomonas acidophila in detergent solution for the first time. Our results show that the elliptical shape of the LH2 complex in solution clearly deviates from its circular structure in crystal phase determined by x-ray diffraction. This result provides an insight into the structure and function interplay in LH2. (authors)

  13. A high count rate one-dimensional position sensitive detector and a data acquisition system for time resolved X-ray scattering studies

    International Nuclear Information System (INIS)

    Pernot, P.

    1982-01-01

    A curved multiwire proportional drift chamber has been built as a general purpose instrument for X-ray scattering and X-ray diffraction experiments with synchrotron radiation. This parallaxe-free one-dimensional linear position sensitive detector has a parallel readout with a double hit logic. The data acquisition system, installed as a part of the D11 camera at LURE-DCI, is designed to perform time slicing and cyclic experiments; it has been used with either the fast multiwire chamber or a standard position sensitive detector with delay line readout [fr

  14. Temperature dependence of the electronic structure of Sr14Cu24O41 studied by resonant inelastic X-ray scattering

    International Nuclear Information System (INIS)

    Yoshida, M.; Ishii, K.; Ikeuchi, K.; Jarrige, I.; Murakami, Y.; Mizuki, J.; Tsutsui, K.; Tohyama, T.; Maekawa, S.; Kudo, K.; Koike, Y.; Endoh, Y.

    2010-01-01

    We report a resonant inelastic X-ray scattering (RIXS) study of charge excitations in the two-leg ladder Sr 14 Cu 24 O 41 . RIXS spectra at 1-5 eV are found to be dependent on temperature. An intraband excitation of the ladder, which appears as a continuum intensity below the Mott gap, decreases in intensity with temperature. Because the intraband excitation is related to the dynamics of doped holes in the ladder, its decrease of the intraband excitation is attributed to the reduction of the mobile holes in the ladder at low temperature.

  15. Using the surface tension to estimate the condensate density of superfluid 4He

    International Nuclear Information System (INIS)

    Campbell, L.J.

    1983-01-01

    Distortion of the condensate wavefunction at the free surface of superfluid 4 He contributes to the surface tension in proportion to the condensate fraction n 0 (T). Using this to resolve the present discrepancy between the measured and predicted temperature dependencies of the surface tension gives n 0 (T) in good agreement with results from neutron and x-ray scattering measurements. This picture is also consistent with the measured 3 He- 4 He interfacial tension

  16. Micellar Surfactant Association in the Presence of a Glucoside-based Amphiphile Detected via High-Throughput Small Angle X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Stanic, Vesna [Brazilian Synchrotron Light Source, Campinas (Brazil); Broadbent, Charlotte [Columbia Univ., New York, NY (United States). Engineering Dept.; DiMasi, Elaine [Brookhaven National Lab. (BNL), Upton, NY (United States). Photon Sciences Division; Galleguillos, Ramiro [Lubrizol Advanced Materials, Cleveland, OH (United States); Woodward, Valerie [Lubrizol Advanced Materials, Cleveland, OH (United States)

    2016-11-14

    The interactions of mixtures of anionic and amphoteric surfactants with sugar amphiphiles were studied via high throughput small angle x-ray scattering (SAXS). The sugar amphiphile was composed of Caprate, Caprylate, and Oleate mixed ester of methyl glucoside, MeGCCO. Optimal surfactant interactions are sought which have desirable physical properties, which must be identified in a cost effective manner that can access the large phase space of possible molecular combinations. X-ray scattering patterns obtained via high throughput SAXS can probe a combinatorial sample space and reveal the incorporation of MeGCCO into the micelles and the molecular associations between surfactant molecules. Such data make it possible to efficiently assess the effects of the new amphiphiles in the formulation. A specific finding of this study is that formulations containing comparatively monodisperse and homogeneous surfactant mixtures can be reliably tuned by addition of NaCl, which swells the surfactant micelles with a monotonic dependence on salt concentration. In contrast, the presence of multiple different surfactants destroys clear correlations with NaCl concentration, even in otherwise similar series of formulations.

  17. Strongly correlated electrons at high pressure: an approach by inelastic X-Ray scattering; Electrons correles sous haute pression: une approche par diffusion inelastique des rayons X

    Energy Technology Data Exchange (ETDEWEB)

    Rueff, J.P

    2007-06-15

    Inelastic X-ray scattering (IXS) and associated methods has turn out to be a powerful alternative for high-pressure physics. It is an all-photon technique fully compatible with high-pressure environments and applicable to a vast range of materials. Standard focalization of X-ray in the range of 100 microns is typical of the sample size in the pressure cell. Our main aim is to provide an overview of experimental results obtained by IXS under high pressure in 2 classes of materials which have been at the origin of the renewal of condensed matter physics: strongly correlated transition metal oxides and rare-earth compounds. Under pressure, d and f-electron materials show behaviors far more complex that what would be expected from a simplistic band picture of electron delocalization. These spectroscopic studies have revealed unusual phenomena in the electronic degrees of freedom, brought up by the increased density, the changes in the charge-carrier concentration, the over-lapping between orbitals, and hybridization under high pressure conditions. Particularly we discuss about pressure induced magnetic collapse and metal-insulator transitions in 3d compounds and valence fluctuations phenomena in 4f and 5f compounds. Thanks to its superior penetration depth, chemical selectivity and resonant enhancement, resonant inelastic X-ray scattering has appeared extremely well suited to high pressure physics in strongly correlated materials. (A.C.)

  18. Small-angle X-ray-scattering investigation and structural-model study of the fatty-acid synthetase from pig liver

    International Nuclear Information System (INIS)

    Folkhard, W.; Felser, B.; Pilz, I.; Kratky, O.; Dutler, H.; Vogel, H.

    1977-01-01

    The structure of the fatty acid synthetase from pig liver was studied on models based upon structural and functional properties selected from pertinent results available from numerous investigations carried out with fatty acid synthetase from this and other sources. When comparing small-angle X-ray-scattering curves calculated with these models and curves obtained from small-angle X-ray-scattering experiments carried out with the pig-liver enzyme, we tried to select a model which would lead to an acceptable correlation between the calculated and the experimental curves and at the same time fulfil the known structural and the functional requirements. The comparison of the curves was started with a model of low complexity. The observed discrepancy, together with arguments from the structural and the functional properties, helped decide which is the next most reasonable model to be considered. This procedure was repeated for five models of increasing complexity. In the model which led to the best fit the multienzyme complex is composed of two halves in an asymmetric conformation including hollow spaces. This highly anisotropic model would imply that the two halves change their conformation each time a synthetic cycle is completed and that the growing fatty acid is handed over from one half to the other. (orig.) [de

  19. Precision mechanical design of an ultrahigh-resolution inelastic x-ray scattering spectrometer system with CDFDW optics at the APS

    International Nuclear Information System (INIS)

    Shu, D; Stoupin, S; Khachatryan, R; Goetze, K A; Roberts, T; Shvyd'ko, Y; Mundboth, K; Collins, S

    2013-01-01

    There are many scientific applications, especially involving topics related to the equilibrium atomic-scale dynamics of condensed matter, that require both a narrower and a steeper resolution function and access to a broader dynamic range than are currently available. To meet these important scientific needs, a prototype of a novel ultrahigh-resolution inelastic x-ray scattering spectrometer system has been designed and constructed at undulator-based beamline 30-ID at the Advanced Photon Source, Argonne National Laboratory. This prototype is designed to meet challenging mechanical and optical specifications for performing so-called CDFDW angular-dispersive x-ray crystal optics, which include a central ultra-thin CFW crystal and a pair of dispersing elements. The abbreviation CDFDW stands for: C – collimating crystal, D – dispersing-element crystal (two D-crystals are used in each CDFDW), F – anomalous transmission filter, and W – wavelength-selector crystal [1]. The mechanical design of the ultrahigh-resolution inelastic x-ray scattering spectrometer, as well as the preliminary test results of its precision positioning performance are presented in this paper.

  20. Purification, crystallization, small-angle X-ray scattering and preliminary X-ray diffraction analysis of the SH2 domain of the Csk-homologous kinase

    International Nuclear Information System (INIS)

    Gunn, Natalie J.; Gorman, Michael A.; Dobson, Renwick C. J.; Parker, Michael W.; Mulhern, Terrence D.

    2011-01-01

    The Src-homology 2 (SH2) domain of Csk-family protein tyrosine kinases acts as a conformational switch to regulate their catalytic activity, which in turn promotes the inhibition of their proto-oncogenic targets, the Src-family kinases. Here, the expression, purification, small-angle X-ray scattering and preliminary diffraction analysis of the SH2 domain of the Csk-homologous kinase is reported. The C-terminal Src kinase (Csk) and Csk-homologous kinase (CHK) are endogenous inhibitors of the proto-oncogenic Src family of protein tyrosine kinases (SFKs). Phosphotyrosyl peptide binding to their Src-homology 2 (SH2) domains activates Csk and CHK, enhancing their ability to suppress SFK signalling; however, the detailed mechanistic basis of this activation event is unclear. The CHK SH2 was expressed in Escherichia coli and the purified protein was characterized as monomeric by synchrotron small-angle X-ray scattering in-line with size-exclusion chromatography. The CHK SH2 crystallized in 0.2 M sodium bromide, 0.1 M bis-Tris propane pH 6.5 and 20% polyethylene glycol 3350 and the best crystals diffracted to ∼1.6 Å resolution. The crystals belonged to space group P2, with unit-cell parameters a = 25.8, b = 34.6, c = 63.2 Å, β = 99.4°

  1. Direct monitoring of calcium-triggered phase transitions in cubosomes using small-angle X-ray scattering combined with microfluidics

    DEFF Research Database (Denmark)

    Ghazal, Aghiad; Gontsarik, Mark; Kutter, Jörg P.

    2016-01-01

    This article introduces a simple microfluidic device that can be combined with synchrotron small-angle X-ray scattering (SAXS) for monitoring dynamic structural transitions. The microfluidic device is a thiol-ene-based system equipped with 125 µm-thick polystyrene windows, which are suitable for ....... The combination of microfluidics with X-ray techniques can be used for investigating protein unfolding, for monitoring the formation of nanoparticles in real time, and for other biomedical and pharmaceutical investigations.......-ray experiments. The device was prepared by soft lithography using elastomeric molds followed by a simple UV-initiated curing step to polymerize the chip material and simultaneously seal the device with the polystyrene windows. The microfluidic device was successfully used to explore the dynamics...

  2. Structural evolution of regenerated silk fibroin under shear: Combined wide- and small-angle x-ray scattering experiments using synchrotron radiation

    International Nuclear Information System (INIS)

    Rossle, Manfred; Panine, Pierre; Urban, Volker S.; Riekel, Christine

    2004-01-01

    The structural evolution of regenerated Bombyx mori silk fibroin during shearing with a Couette cell has been studied in situ by synchrotron radiation small- and wide-angle x-ray scattering techniques. An elongation of fibroin molecules was observed with increasing shear rate, followed by an aggregation phase. The aggregates were found to be amorphous with β-conformation according to infrared spectroscopy. Scanning x-ray microdiffraction with a 5 (micro)m beam on aggregated material, which had solidified in air, showed silk II reflections and a material with equatorial reflections close to the silk I structure reflections, but with strong differences in reflection intensities. This silk I type material shows up to two low-angle peaks suggesting the presence of water molecules that might be intercalated between hydrogen-bonded sheets.

  3. Small angle X-ray scattering by TiO2/ZrO2 mixed oxide particles and a Synroc precursor

    International Nuclear Information System (INIS)

    Gazeau, D.; Zemb, T.; Amal, R.; Bartlett, J.

    1992-09-01

    This high resolution small angle X-ray scattering study of a concentrated oxide sol, precursor of the SYNROC matrix for the storage of the high level radioactive waste, evidences a locally cylindrical microstructure. Locally, nanometric cylinders show disordered axis with some concentration dependent connections. This microstructure explains the paradoxal stability of this oxide dispersions upon the addition of concentrated acidic solutions. This stability has a steric origin and electrostatic repulsions are not needed. The addition of aluminium to the initial titanium-zirconium mixture enhances branching on the locally cylindrical microstructure. Finally, we show that the solid powder obtained after calcination (drying) of the sol has the same specific area (∼ 1000 m 2 /g) than the sol. (Author). 23 refs., 7 figs., 1 tab

  4. Wavelet-based feature extraction applied to small-angle x-ray scattering patterns from breast tissue: a tool for differentiating between tissue types

    International Nuclear Information System (INIS)

    Falzon, G; Pearson, S; Murison, R; Hall, C; Siu, K; Evans, A; Rogers, K; Lewis, R

    2006-01-01

    This paper reports on the application of wavelet decomposition to small-angle x-ray scattering (SAXS) patterns from human breast tissue produced by a synchrotron source. The pixel intensities of SAXS patterns of normal, benign and malignant tissue types were transformed into wavelet coefficients. Statistical analysis found significant differences between the wavelet coefficients describing the patterns produced by different tissue types. These differences were then correlated with position in the image and have been linked to the supra-molecular structural changes that occur in breast tissue in the presence of disease. Specifically, results indicate that there are significant differences between healthy and diseased tissues in the wavelet coefficients that describe the peaks produced by the axial d-spacing of collagen. These differences suggest that a useful classification tool could be based upon the spectral information within the axial peaks

  5. X-ray scattering study of thermal nanopore templating in hybrid films of organosilicate precursor and reactive four-armed porogen

    International Nuclear Information System (INIS)

    Yoon, Jinhwan; Heo, Kyuyoung; Oh, Weontae; Jin, Kyeong Sik; Jin, Sangwoo; Kim, Jehan; Kim, Kwang-Woo; Chang, Taihyun; Ree, Moonhor

    2006-01-01

    The miscibility and the mechanism for thermal nanopore templating in films prepared from spin-coating and subsequent drying of homogenous solutions of curable polymethylsilsesquioxane dielectric precursor and thermally labile, reactive triethoxysilyl-terminated four-armed poly(ε-caprolactone) porogen were investigated in detail by in situ two-dimensional grazing incidence small-angle x-ray scattering analysis. The dielectric precursor and porogen components in the film were fully miscible. On heating, limited aggregations of the porogen, however, took place in only a small temperature range of 100-140 deg. C as a result of phase separation induced by the competition of the curing and hybridization reactions of the dielectric precursor and porogen; higher porogen loading resulted in relatively large porogen aggregates and a greater size distribution. The developed porogen aggregates underwent thermal firing above 300 deg. C without further growth and movement, and ultimately left their individual footprints in the film as spherical nanopores

  6. Aggregation of bovine serum albumin upon cleavage of its disulfide bonds, studied by the time-resolved small-angle X-ray scattering technique with synchrotron radiation

    International Nuclear Information System (INIS)

    Ueki, Tatzuo; Inoko, Yoji; Izumi, Yoshinobu; Tagawa, Hiroyuki; Muroga, Yoshio

    1985-01-01

    A rapid mixing system of the stopped-flow type, used with small-angle X-ray scattering equipment using synchrotron radiation, is described. The process of aggregation of bovine serum albumin was traced with a time interval of 50 s, initiated upon cleavage of its disulfide bonds by reduction with dithiothreitol. The results indicate that a 218-fold molar excess of dithiothreitol over the number of moles of disulfide bonds in bovine serum albumin is sufficient to initiate the reaction immediately after mixing, which reaches equilibrium in about 15 min. On the other hand, half this amount is not sufficient to initiate the reaction, so that the reaction is delayed by about 150 s. Such a single-shot time-resolved experiment showed that experiments with a time interval of 100 ms are possible with repeated multi-shot runs. (Auth.)

  7. Look fast: Crystallization of conjugated molecules during solution shearing probed in-situ and in real time by X-ray scattering

    KAUST Repository

    Smilgies, Detlef Matthias; Li, Ruipeng; Giri, Gaurav; Chou, Kang Wei; Diao, Ying; Bao, Zhenan; Amassian, Aram

    2012-01-01

    High-speed solution shearing, in which a drop of dissolved material is spread by a coating knife onto the substrate, has emerged as a versatile, yet simple coating technique to prepare high-mobility organic thin film transistors. Solution shearing and subsequent drying and crystallization of a thin film of conjugated molecules is probed in situ using microbeam grazing incidence wide-angle X-ray scattering (μGIWAXS). We demonstrate the advantages of this approach to study solution based crystal nucleation and growth, and identify casting parameter combinations to cast highly ordered and laterally aligned molecular thin films. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Microstructural Parameters in 8 MeV Electron-Irradiated BOMBYX MORI Silk Fibers by Wide-ANGLE X-Ray Scattering Studies (waxs)

    Science.gov (United States)

    Sangappa, Asha, S.; Sanjeev, Ganesh; Subramanya, G.; Parameswara, P.; Somashekar, R.

    2010-01-01

    The present work looks into the microstructural modification in electron irradiated Bombyx mori P31 silk fibers. The irradiation process was performed in air at room temperature using 8 MeV electron accelerator at different doses: 0, 25, 50 and 100 kGy. Irradiation of polymer is used to cross-link or degrade the desired component or to fix the polymer morphology. The changes in microstructural parameters in these natural polymer fibers have been computed using wide angle X-ray scattering (WAXS) data and employing line profile analysis (LPA) using Fourier transform technique of Warren. Exponential, Lognormal and Reinhold functions for the column length distributions have been used for the determination of crystal size, lattice strain and enthalpy parameters.

  9. Very large-scale structures in sintered silica aerogels as evidenced by atomic force microscopy and ultra-small angle X-ray scattering experiments

    CERN Document Server

    Marliere, C; Etienne, P; Woignier, T; Dieudonné, P; Phalippou, J

    2001-01-01

    During the last few years the bulk structure of silica aerogels has been extensively studied mainly by scattering techniques (neutrons, X-rays, light). It has been shown that small silica particles aggregate to constitute a fractal network. Its spatial extension and fractal dimension are strongly dependent on the synthesis conditions (e.g., pH of gelifying solutions). These typical lengths range from 1 to 10 nm. Ultra-small angle X-ray scattering (USAXS) and atomic force microscopy (AFM) experiments have been carried out on aerogels at different steps of densification. The results presented in this paper reveal the existence of a spatial arrangement of the solid part at a very large length scale. The evolution of this very large-scale structure during the densification process has been studied and reveals a contraction of this macro-structure made of aggregates of clusters. (16 refs).

  10. Aggregation of bovine serum albumin upon cleavage of its disulfide bonds, studied by the time-resolved small-angle X-ray scattering technique with synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Ueki, Tatzuo; Inoko, Yoji; Hiragi, Yuzuru; Kataoka, Mikio; Amemiya, Yoshiyuki; Izumi, Yoshinobu; Tagawa, Hiroyuki; Muroga, Yoshio

    1985-11-01

    A rapid mixing system of the stopped-flow type, used with small-angle X-ray scattering equipment using synchrotron radiation, is described. The process of aggregation of bovine serum albumin was traced with a time interval of 50s, initiated upon cleavage of its disulfide bonds by reduction with dithiothreitol. The results indicate that a 218-fold molar excess of dithiothreitol over the number of moles of disulfide bonds in bovine serum albumin is sufficient to initiate the reaction immediately after mixing, which reaches equilibrium in about 15 min. On the other hand, half this amount is not sufficient to initiate the reaction, so that the reaction is delayed by about 150s. Such a single-shot time-resolved experiment showed that experiments with a time interval of 100 ms are possible with repeated multi-shot runs. 26 refs.; 8 figs.

  11. Look fast: Crystallization of conjugated molecules during solution shearing probed in-situ and in real time by X-ray scattering

    KAUST Repository

    Smilgies, Detlef Matthias

    2012-12-20

    High-speed solution shearing, in which a drop of dissolved material is spread by a coating knife onto the substrate, has emerged as a versatile, yet simple coating technique to prepare high-mobility organic thin film transistors. Solution shearing and subsequent drying and crystallization of a thin film of conjugated molecules is probed in situ using microbeam grazing incidence wide-angle X-ray scattering (μGIWAXS). We demonstrate the advantages of this approach to study solution based crystal nucleation and growth, and identify casting parameter combinations to cast highly ordered and laterally aligned molecular thin films. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Metal ion controlled self-assembly of a chemically reengineered protein drug studied by small-angle X-ray scattering

    DEFF Research Database (Denmark)

    Jesper, Nygaard; Munch, Henrik K.; Thulstrup, Peter W.

    2012-01-01

    . A small-angle X-ray scattering analysis of the bipyridine-modified insulin system confirmed an organization into a novel well-ordered structure based on insulin trimers, as induced by the addition of Fe(II). In contrast, unmodified monomeric insulin formed larger and more randomly structured assemblies......Precise control of the oligomeric state of proteins is of central importance for biological function and for the properties of biopharmaceutical drugs. Here, the self-assembly of 2,2′-bipyridine conjugated monomeric insulin analogues, induced through coordination to divalent metal ions, was studied....... This protein drug system was designed to form non-native homo-oligomers through selective coordination of two divalent metal ions, Fe(II) and Zn(II), respectively. The insulin type chosen for this study is a variant designed for a reduced tendency toward native dimer formation at physiological concentrations...

  13. Transformation from Multilamellar to Unilamellar Vesicles by Addition of a Cationic Lipid to PEGylated Liposomes Explored with Synchrotron Small Angle X-ray Scattering

    International Nuclear Information System (INIS)

    Sakuragi, Mina; Sakurai, Kazuo; Koiwai, Kazunori; Nakamura, Kouji; Masunaga, Hiroyasu; Ogawa, Hiroki

    2011-01-01

    PEGylated liposomes composed of a benzamidine derivative (TRX), hydrogenated soybean phosphatidylcholine (HSPC), and N-(monomethoxy-polyethyleneglycolcarbamyl) distearoyl phosphatidylethanolamine (PEG-PE) were examined in terms of how the addition of TRX affects their structures with small angle x-ray scattering (SAXS) as well as transmission electron microscopy (TEM). TEM images showed the presence of unilamella vesicles for both with and without TRX, though a small amount of multilamella vesicles were observed in absence of TRX. We analyzed SAXS profiles at contained TRX composition combined with contrast variation technique by adding PEG solution and unilamella vesicle model could be reproduced. Subsequently, we analyzed SAXS profiles at no TRX composition. The mixture model of unilamella and multilamella vesicle was reconstructed and we estimated about 10 % multilamella vesicles from a fitting parameter.

  14. Structural evolution of regenerated silk fibroin under shear: Combined wide- and small-angle x-ray scattering experiments using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Rossle, Manfred [European Molecular Biology Laboratory (EMBL), France; Panine, Pierre [European Synchrotron Radiation Facility (ESRF); Urban, Volker S [ORNL; Riekel, Christine [European Synchrotron Radiation Facility (ESRF)

    2004-04-01

    The structural evolution of regenerated Bombyx mori silk fibroin during shearing with a Couette cell has been studied in situ by synchrotron radiation small- and wide-angle x-ray scattering techniques. An elongation of fibroin molecules was observed with increasing shear rate, followed by an aggregation phase. The aggregates were found to be amorphous with {beta}-conformation according to infrared spectroscopy. Scanning x-ray microdiffraction with a 5 {micro}m beam on aggregated material, which had solidified in air, showed silk II reflections and a material with equatorial reflections close to the silk I structure reflections, but with strong differences in reflection intensities. This silk I type material shows up to two low-angle peaks suggesting the presence of water molecules that might be intercalated between hydrogen-bonded sheets.

  15. Studies on micro-domain structure in segmented polyether polyurethane-ureas by positron annihilation lifetime and small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Yin Chuanyuan; Gu Qingchao

    1997-01-01

    The micro-domain structure of segmented polyether polyurethane-ureas is investigated by means of positron annihilation lifetime spectroscopy, small-angle X-ray scattering and differential scanning calorimetry. The experimental results show that the decrease in the domain volume and free volume results from the increase in the hard segment (polyurethane-urea segment) contents as the number-average molecular weight M n -bar of the soft segments (polyethylene glycol segments) is the same, and that the increase in domain volume and free volume result from the increase in the M n -bar of the soft segments when the hard segment content is the same or nearly the same. These results demonstrate that positron annihilation lifetime spectroscopy is a sensitive technique to probe the micro-domain structure in polymers

  16. Resonant inelastic x-ray scattering studies of magnons and bimagnons in the lightly doped cuprate La2 -xSrxCuO4

    Science.gov (United States)

    Chaix, L.; Huang, E. W.; Gerber, S.; Lu, X.; Jia, C.; Huang, Y.; McNally, D. E.; Wang, Y.; Vernay, F. H.; Keren, A.; Shi, M.; Moritz, B.; Shen, Z.-X.; Schmitt, T.; Devereaux, T. P.; Lee, W.-S.

    2018-04-01

    We investigated the doping dependence of magnetic excitations in the lightly doped cuprate La2 -xSrxCuO4 via combined studies of resonant inelastic x-ray scattering (RIXS) at the Cu L3 edge and theoretical calculations. With increasing doping, the magnon dispersion is found to be essentially unchanged, but the spectral width broadens and the spectral weight varies differently at different momenta. Near the Brillouin zone center, we directly observe bimagnon excitations that possess the same energy scale and doping dependence as previously observed by Raman spectroscopy. They disperse weakly in energy-momentum space, and they are consistent with a bimagnon dispersion that is renormalized by the magnon-magnon interaction at the zone center.

  17. Planning meeting to form the CMSN Team: Building a unified computational model for the resonant X-ray scattering of strongly correlated materials. Final report

    International Nuclear Information System (INIS)

    van Veenendaal, M.

    2008-01-01

    The planning meeting was held May 21-23 2008 at Argonne National Laboratory (ANL). The purpose of the meeting was to establish a network on building computational model for resonant elastic and inelastic x-ray scattering. This course of action was recommended by program officer Dale Koelling after the initial submission of a proposal for a Computational Materials Science Network to Basic Energy Sciences. The meeting consisted of talks and discussion. At the end of the meeting three subgroups were formed. After the successful formation of the team, a new proposal was written which was funded by BES. Since this was a planning meeting there were no proceedings. The program and titles of talks are given.

  18. Solution Structures of Highly Active Molecular Ir Water-Oxidation Catalysts from Density Functional Theory Combined with High-Energy X-ray Scattering and EXAFS Spectroscopy.

    Science.gov (United States)

    Yang, Ke R; Matula, Adam J; Kwon, Gihan; Hong, Jiyun; Sheehan, Stafford W; Thomsen, Julianne M; Brudvig, Gary W; Crabtree, Robert H; Tiede, David M; Chen, Lin X; Batista, Victor S

    2016-05-04

    The solution structures of highly active Ir water-oxidation catalysts are elucidated by combining density functional theory, high-energy X-ray scattering (HEXS), and extended X-ray absorption fine structure (EXAFS) spectroscopy. We find that the catalysts are Ir dimers with mono-μ-O cores and terminal anionic ligands, generated in situ through partial oxidation of a common catalyst precursor. The proposed structures are supported by (1)H and (17)O NMR, EPR, resonance Raman and UV-vis spectra, electrophoresis, etc. Our findings are particularly valuable to understand the mechanism of water oxidation by highly reactive Ir catalysts. Importantly, our DFT-EXAFS-HEXS methodology provides a new in situ technique for characterization of active species in catalytic systems.

  19. Resonant inelastic X-ray scattering spectra at the Ir L-edge in Na{sub 2}IrO{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Igarashi, Jun-ichi, E-mail: junichi.igarashi.kiryu@vc.ibaraki.ac.jp [Faculty of Science, Ibaraki University, Mito, Ibaraki 310-8512 (Japan); Nagao, Tatsuya, E-mail: nagao@gunma-u.ac.jp [Faculty of Engineering, Gunma University, Kiryu, Gunma 376-8515 (Japan)

    2016-10-15

    Highlights: • A theoretical framework of resonant inelastic X-ray scattering (RIXS) on the basis of the itinerant electron scheme has been developed. • The RIXS theory is applied to iridate Na{sub 2}IrO{sub 3}. • The origins of the multi-peak structure of the excitation spectra found in the RIXS experiment have been assigned to the magnetic and excitonic excitations. - Abstract: We analyze resonant X-ray scattering (RIXS) spectra in Na{sub 2}IrO{sub 3} on the basis of the itinerant electron picture. Employing a multi-orbital tight-binding model on a honeycomb lattice, we find that the zigzag magnetic order is the most stable with sizable energy gap in the one-electron band within the Hartree–Fock approximation. We derive the RIXS spectra, which are connected to the generalized density–density correlation function. We calculate the spectra as a function of excitation energy ω, within the random phase approximation. The spectra consist of the peaks with ω < 20 meV, and of the peaks with 0.4 < ω < 0.8 eV. The former peaks are composed of four bound states in the density–density correlation function, and may be identified as the magnetic excitations, while the latter peaks are composed of 16 bound states below the energy continuum of individual electron–hole pair excitations, and may be identified as the excitonic excitations. The calculated spectra agree qualitatively with the recent RIXS experiment.

  20. Abstract ID: 176 Geant4 implementation of inter-atomic interference effect in small-angle coherent X-ray scattering for materials of medical interest.

    Science.gov (United States)

    Paternò, Gianfranco; Cardarelli, Paolo; Contillo, Adriano; Gambaccini, Mauro; Taibi, Angelo

    2018-01-01

    Advanced applications of digital mammography such as dual-energy and tomosynthesis require multiple exposures and thus deliver higher dose compared to standard mammograms. A straightforward manner to reduce patient dose without affecting image quality would be removal of the anti-scatter grid, provided that the involved reconstruction algorithms are able to take the scatter figure into account [1]. Monte Carlo simulations are very well suited for the calculation of X-ray scatter distribution and can be used to integrate such information within the reconstruction software. Geant4 is an open source C++ particle tracking code widely used in several physical fields, including medical physics [2,3]. However, the coherent scattering cross section used by the standard Geant4 code does not take into account the influence of molecular interference. According to the independent atomic scattering approximation (the so-called free-atom model), coherent radiation is indistinguishable from primary radiation because its angular distribution is peaked in the forward direction. Since interference effects occur between x-rays scattered by neighbouring atoms in matter, it was shown experimentally that the scatter distribution is affected by the molecular structure of the target, even in amorphous materials. The most important consequence is that the coherent scatter distribution is not peaked in the forward direction, and the position of the maximum is strongly material-dependent [4]. In this contribution, we present the implementation of a method to take into account inter-atomic interference in small-angle coherent scattering in Geant4, including a dedicated data set of suitable molecular form factor values for several materials of clinical interest. Furthermore, we present scatter images of simple geometric phantoms in which the Rayleigh contribution is rigorously evaluated. Copyright © 2017.