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Sample records for grazing incidence small-angle

  1. Grazing-incidence small-angle X-ray scattering: application to the study of quantum dot lattices

    SciTech Connect

    Buljan, Maja Radić, Nikola; Bernstorff, Sigrid; Dražić, Goran; Bogdanović-Radović, Iva; Holý, Václav

    2012-01-01

    The modelling of grazing-incidence small-angle X-ray scattering (GISAXS) from three-dimensional quantum dot lattices is described. The ordering of quantum dots in three-dimensional quantum dot lattices is investigated by grazing-incidence small-angle X-ray scattering (GISAXS). Theoretical models describing GISAXS intensity distributions for three general classes of lattices of quantum dots are proposed. The classes differ in the type of disorder of the positions of the quantum dots. The models enable full structure determination, including lattice type, lattice parameters, the type and degree of disorder in the quantum dot positions and the distributions of the quantum dot sizes. Applications of the developed models are demonstrated using experimentally measured data from several types of quantum dot lattices formed by a self-assembly process.

  2. Grazing incidence small angle X-ray scattering study of silver nanoparticles in ion-exchanged glasses

    NASA Astrophysics Data System (ADS)

    Cheng, Weidong; Wu, Zhaojun; Gu, Xiaohua; Xing, Xueqing; Mo, Guang; Wu, Zhonghua

    2015-05-01

    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.

  3. Asymmetric grazing incidence small angle x-ray scattering and anisotropic domain wall motion in obliquely grown nanocrystalline Co films.

    PubMed

    Quirós, C; Peverini, L; Díaz, J; Alija, A; Blanco, C; Vélez, M; Robach, O; Ziegler, E; Alameda, J M

    2014-08-22

    Strong asymmetries have been observed in grazing incidence small angle x-ray scattering (GISAXS) in situ patterns obtained from 30 nm-thick nanocrystalline Co films prepared by oblique sputtering (15°-75° off-sample normal). These asymmetries have been qualitatively simulated by a simple model consisting of an ensemble of 8 nm-wide inclined Co nanocolumns. It is found that narrow inclined features appear in the diffuse background resembling those characteristic of faceted systems, which can be used to obtain straightforward non-destructive estimations of buried nanocolumnar grains inclination, even for oblique angles below 45°, when the stronger and broader asymmetric features of the pattern are not yet fully formed. Furthermore, using magneto-optical microscopy, a marked change in the magnetic domain's nucleation and growth process has been observed in the sample prepared at 75°, with the stronger GISAXS asymmetries. Easy axis magnetization reversal starts by a random and homogeneous nucleation of small (∼μm) elongated domains aligned with the nanocolumn's long axis and proceeds through the preferred propagation of head-to-head domain walls (DWs) along the applied field direction. This peculiar magnetic behavior indicates that the strongly anisotropic nanostructuring created by the oblique growth process is equivalent, from a magnetic point of view, to an array of self-assembled buried nanowires. These results show how GISAXS and magneto-optical microscopy can be combined as a powerful tool for correlating the morphology and magnetism of thin nanostructured systems.

  4. Probing kinetics and dynamics of nanocomposites with grazing-incidence small-angle x-ray scattering.

    NASA Astrophysics Data System (ADS)

    Wang, Jin

    2009-03-01

    Synthesizing complex nanocomposites and superstructures is of great interest in all areas of materials science and involving biology, chemistry, physics and engineering applications such as the fabrication of novel electronic, magnetic, and photonic devices. Since the entire synthesis and assembly process can take place far from equilibrium conditions, a controlled process has to be guided by a thorough understanding of the kinetics and dynamics in the composites. This requires measurement of the structure in situ and in real time with subnanometer spatial resolution and millisecond to subsecond temporal resolution. As an increasingly important structural-characterization technique, grazing-incidence small-angle x-ray scattering (GISAXS) finds vast applications in the research of nanostructures and nanocomposites at surfaces and interfaces. Most significantly, as a complementary method to conventional surface-sensitive tools such as scanning probe microscopy and electron microscopy, GISAXS can be used in situ and in real time to monitor the formation of the nanostructure or nanocomposite, which makes it most suitable for studying the kinetics of nanoassembly processes. The GISAXS technique can also be an integral part of numerous research, for example, those involving kinetics of mesoscaled ordered block copolymer thin films, kinetics of sol-gel processes, quantum dots, nanoparticles in ultrathin films, and dynamics and phase transitions 2D nanocrystal superlattices. Here, I will focus on the applications of GISAXS in real-time structure characterization, the dynamics in polymer/nanoparticle nanocomposies, and the challenges to elucidate nanostructure formation in nanoscience and nanotechnology.

  5. Trends in anomalous small-angle X-ray scattering in grazing incidence for supported nanoalloyed and core-shell metallic nanoparticles

    NASA Astrophysics Data System (ADS)

    Andreazza, P.; Khelfane, H.; Lyon, O.; Andreazza-Vignolle, C.; Ramos, A. Y.; Samah, M.

    2012-06-01

    As atomic structure and morphology of particles are directly correlated to their functional properties, experimental methods probing local and average features of particles at the nanoscale elicit a growing interest. Anomalous small-angle X-ray scattering (ASAXS) is a very attractive technique to investigate the size, shape and spatial distribution of nanoobjects embedded in a homogeneous matrix or in porous media. The anomalous variation of the scattering factor close to an absorption edge enables element specific investigations. In the case of supported nano-objects, the use of grazing incidence is necessary to limit the probed depth. The combination of grazing incidence with the anomalous technique provides a powerful new method, anomalous grazing incidence small-angle X-ray scattering (AGISAXS), to disentangle complex chemical patterns in supported multi-component nano-structures. Nevertheless, a proper data analysis requires accurate quantitative measurements associated to an adapted theoretical framework. This paper presents anomalous methods applied to nanoalloys phase separation in the 1-10 nm size range, and focuses on the application of AGISAXS in bimetallic systems: nanocomposite films and core-shell supported nanoparticles.

  6. Detection of short range order in SiO2 thin-films by grazing-incidence wide and small-angle X-ray scattering

    NASA Astrophysics Data System (ADS)

    Nagata, Kohki; Ogura, Atsushi; Hirosawa, Ichiro; Suwa, Tomoyuki; Teramoto, Akinobu; Ohmi, Tadahiro

    2016-04-01

    The effects of the fabrication process conditions on the microstructure of silicon dioxide thin films of <10 nm thickness are presented. The microstructure was investigated using grazing-incidence wide and small-angle X-ray scattering methods with synchrotron radiation. The combination of a high brilliance light source and grazing incident configuration enabled the observation of very weak diffuse X-ray scattering from SiO2 thin films. The results revealed different microstructures, which were dependent on oxidizing species or temperature. The micro-level properties differed from bulk properties reported in the previous literature. It was indicated that these differences originate from inner stress. The detailed structure in an amorphous thin film was not revealed owing to detection difficulties.

  7. 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)

    SciTech Connect

    Rawolle, M.; Koerstgens, V.; Ruderer, M. A.; Metwalli, E.; Guo, S.; Mueller-Buschbaum, P.; Herzog, G.; Benecke, G.; Schwartzkopf, M.; Buffet, A.; Perlich, J.; Roth, S. V.

    2012-10-15

    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.

  8. Quantitative determination of the lateral density and intermolecular correlation between proteins anchored on the membrane surfaces using grazing incidence small-angle X-ray scattering and grazing incidence X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Abuillan, Wasim; Vorobiev, Alexei; Hartel, Andreas; Jones, Nicola G.; Engstler, Markus; Tanaka, Motomu

    2012-11-01

    As a physical model of the surface of cells coated with densely packed, non-crystalline proteins coupled to lipid anchors, we functionalized the surface of phospholipid membranes by coupling of neutravidin to biotinylated lipid anchors. After the characterization of fine structures perpendicular to the plane of membrane using specular X-ray reflectivity, the same membrane was characterized by grazing incidence small angle X-ray scattering (GISAXS). Within the framework of distorted wave Born approximation and two-dimensional Percus-Yevick function, we can analyze the form and structure factors of the non-crystalline, membrane-anchored proteins for the first time. As a new experimental technique to quantify the surface density of proteins on the membrane surface, we utilized grazing incidence X-ray fluorescence (GIXF). Here, the mean intermolecular distance between proteins from the sulfur peak intensities can be calculated by applying Abelé's matrix formalism. The characteristic correlation distance between non-crystalline neutravidin obtained by the GISAXS analysis agrees well with the intermolecular distance calculated by GIXF, suggesting a large potential of the combination of GISAXS and GIXF in probing the lateral density and correlation of non-crystalline proteins displayed on the membrane surface.

  9. Grazing-incidence small-angle X-ray scattering in a twofold rough-interface medium: a new theoretical approach using the q-eigenwave formalism.

    PubMed

    Chukhovskii, F N; Roshchin, B S

    2015-11-01

    Based on the rigorous Green function formalism to describe the grazing-incidence small-angle X-ray scattering (GISAXS) problem, a system of two linked integral equations is derived with respect to amplitudes of the reflected and transmitted plane q-eigenwaves (eigenstate functions) propagating through two homogeneous media separated from each other by a rough surface interface. To build up the coupled solutions of these basic equations beyond the perturbation theory constraint 2kσθ0 < 1, a simple iteration procedure is proposed as opposed to the self-consistent wave approach [Chukhovskii (2011). Acta Cryst. A67, 200-209; Chukhovski (2012). Acta Cryst. A68, 505-512]. Using the first-order iteration, analytical expressions for the averaged specular and non-specular scattering intensity distributions have been obtained. These expressions are further analysed in terms of the GISAXS parameters {k, θ, θ0} and surface finish ones {σ, l, h}, where θ and θ0 are the scattering and incidence angles of the X-rays, respectively, σ is the root-mean-square roughness, l is the correlation length, h is the fractal surface model index, k = 2π/λ, and λ is the X-ray wavelength. A direct way to determine the surface finish parameters from the experimental specular and diffuse scattering indicatrix scan data is discussed for an example of GISAXS measurements from rough surfaces of α-quartz and CdTe samples. PMID:26522410

  10. In situ monitoring of laser-induced periodic surface structures formation on polymer films by grazing incidence small-angle X-ray scattering.

    PubMed

    Rebollar, Esther; Rueda, Daniel R; Martín-Fabiani, Ignacio; Rodríguez-Rodríguez, Álvaro; García-Gutiérrez, Mari-Cruz; Portale, Giuseppe; Castillejo, Marta; Ezquerra, Tiberio A

    2015-04-01

    The formation of laser-induced periodic surface structures (LIPSS) on model spin-coated polymer films has been followed in situ by grazing incidence small-angle X-ray scattering (GISAXS) using synchrotron radiation. The samples were irradiated at different repetition rates ranging from 1 up to 10 Hz by using the fourth harmonic of a Nd:YAG laser (266 nm) with pulses of 8 ns. Simultaneously, GISAXS patterns were acquired during laser irradiation. The variation of both the GISAXS signal with the number of pulses and the LIPSS period with laser irradiation time is revealing key kinetic aspects of the nanostructure formation process. By considering LIPSS as one-dimensional paracrystalline lattice and using a correlation found between the paracrystalline disorder parameter, g, and the number of reflections observed in the GISAXS patterns, the variation of the structural order of LIPSS can be assessed. The role of the laser repetition rate in the nanostructure formation has been clarified. For high pulse repetition rates (i.e., 10 Hz), LIPSS evolve in time to reach the expected period matching the wavelength of the irradiating laser. For lower pulse repetition rates LIPSS formation is less effective, and the period of the ripples never reaches the wavelength value. Results support and provide information on the existence of a feedback mechanism for LIPSS formation in polymer films.

  11. Characterization of Lipid-Templated Silica and Hybrid Thin Film Mesophases by Grazing Incidence Small-Angle X-ray Scattering

    PubMed Central

    Dunphy, Darren R.; Alam, Todd M.; Tate, Michael P.; Hillhouse, Hugh W.; Smarsly, Bernd; Collord, Andrew D.; Carnes, Eric; Baca, Helen K.; Köhn, Ralf; Sprung, Michael; Wang, Jin; Brinker, C. Jeffrey

    2009-01-01

    The nanostructure of silica and hybrid thin film mesophases templated by phospholipids via an evaporation-induced self-assembly (EISA) process was investigated by grazing-incidence small-angle X-ray scattering (GISAXS). Diacyl phosphatidylcholines with two tails of 6 or 8 carbons were found to template 2D hexagonal mesophases, with the removal of lipid from these lipid/silica films by thermal or UV/O3 processing resulting in a complete collapse of the pore volume. Monoacyl phosphatidylcholines with single tails of 10–14 carbons formed 3D micellular mesophases; the lipid was found to be extractable from these 3D materials, yielding a porous material. In contrast to pure lipid/silica thin film mesophases, films formed from the hybrid bridged silsesquioxane precursor bis(triethoxysilyl)ethane exhibited greater stability toward (both diacyl and monoacyl) lipid removal. Ellipsometric, FTIR, and NMR studies show that the presence of phospholipid suppresses siloxane network formation, while actually promoting condensation reactions in the hybrid material. 1D X-ray scattering and FTIR data were found to be consistent with strong interactions between lipid headgroups and the silica framework. PMID:19496546

  12. New reactor dedicated to in operando studies of model catalysts by means of surface x-ray diffraction and grazing incidence small angle x-ray scattering.

    PubMed

    Saint-Lager, M-C; Bailly, A; Dolle, P; Baudoing-Savois, R; Taunier, P; Garaudée, S; Cuccaro, S; Douillet, S; Geaymond, O; Perroux, G; Tissot, O; Micha, J-S; Ulrich, O; Rieutord, F

    2007-08-01

    A new experimental setup has been developed to enable in situ studies of catalyst surfaces during chemical reactions by means of surface x-ray diffraction (SXRD) and grazing incidence small angle x-ray scattering. The x-ray reactor chamber was designed for both ultrahigh-vacuum (UHV) and reactive gas environments. A laser beam heating of the sample was implemented; the sample temperature reaches 1100 K in UHV and 600 K in the presence of reactive gases. The reactor equipment allows dynamical observations of the surface with various, perfectly mixed gases at controlled partial pressures. It can run in two modes: as a bath reactor in the pressure range of 1-1000 mbars and as a continuous flow cell for pressure lower than 10(-3) mbar. The reactor is connected to an UHV preparation chamber also equipped with low energy electron diffraction and Auger spectroscopy. This setup is thus perfectly well suited to extend in situ studies to more complex surfaces, such as epitaxial films or supported nanoparticles. It offers the possibility to follow the chemically induced changes of the morphology, the structure, the composition, and growth processes of the model catalyst surface during exposure to reactive gases. As an example the Pd(8)Ni(92)(110) surface structure was followed by SXRD under a few millibars of hydrogen and during butadiene hydrogenation while the reaction was monitored by quadrupole mass spectrometry. This experiment evidenced the great sensitivity of the diffracted intensity to the subtle interaction between the surface atoms and the gas molecules.

  13. Probing the surface microstructure of layer-by-layer self-assembly chitosan/poly(l-glutamic acid) multilayers: A grazing-incidence small-angle X-ray scattering study.

    PubMed

    Zhao, Nie; Yang, Chunming; Wang, Yuzhu; Zhao, Binyu; Bian, Fenggang; Li, Xiuhong; Wang, Jie

    2016-01-01

    This study characterized the surface structure of layer-by-layer self-assembly chitosan/poly(L-glutamic acid) multilayers through grazing-incidence small-angle X-ray scattering (GISAXS), X-ray reflectivity (XRR), and atomic force microscopy (AFM). A weakly long-period ordered structure along the in-plane direction was firstly observed in the polyelectrolyte multilayer by the GISAXS technique. This structure can be attributed to the specific domains on the film surface. In the domain, nanodroplets that were formed by polyelectrolyte molecules were orderly arranged along the free surface of the films. This ordered structure gradually disappeared with the increasing bilayer number because of the complex merging behavior of nanodroplets into large islands. Furthermore, resonant diffuse scattering became evident in the GISAXS patterns as the number of bilayers in the polyelectrolyte multilayer was increased. Notably, the lateral cutoff length of resonant diffuse scattering for these polyelectrolyte films was comparable with the long-period value of the ordered nanodroplets in the polyelectrolyte multilayer. Therefore, the nanodroplets could be considered as a basic transmission unit for structure propagation from the inner interface to the film surface. It suggests that the surface structure with length scale larger than the size of nanodroplets was partially complicated from the interface structure near the substrate, but surface structure smaller than the cutoff length was mainly depended on the conformation of nanodroplets. PMID:26478320

  14. 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

    PubMed Central

    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

    2014-01-01

    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. PMID:25294982

  15. Grazing incidence beam expander

    SciTech Connect

    Akkapeddi, P.R.; Glenn, P.; Fuschetto, A.; Appert, Q.; Viswanathan, V.K.

    1985-01-01

    A Grazing Incidence Beam Expander (GIBE) telescope is being designed and fabricated to be used as an equivalent end mirror in a long laser resonator cavity. The design requirements for this GIBE flow down from a generic Free Electron Laser (FEL) resonator. The nature of the FEL gain volume (a thin, pencil-like, on-axis region) dictates that the output beam be very small. Such a thin beam with the high power levels characteristic of FELs would have to travel perhaps hundreds of meters or more before expanding enough to allow reflection from cooled mirrors. A GIBE, on the other hand, would allow placing these optics closer to the gain region and thus reduces the cavity lengths substantially. Results are presented relating to optical and mechanical design, alignment sensitivity analysis, radius of curvature analysis, laser cavity stability analysis of a linear stable concentric laser cavity with a GIBE. Fabrication details of the GIBE are also given.

  16. Hypersonic phononic stopbands at small angles of wave incidence in porous silicon multilayers

    NASA Astrophysics Data System (ADS)

    Aliev, Gazi N.; Goller, Bernhard

    2015-08-01

    We report theoretical simulation and experimental observation of the mode conversion effect in a hypersonic distributed Bragg reflector of porous silicon. Acoustic transmission of longitudinal waves through the multilayered structure has been measured in the frequency range 0-3 GHz. It is found that the measured transmittance at the gap frequencies is always higher than that theoretically predicted for normal incidence. We attribute this to non-perpendicular wave propagation that was not deliberately sought, which subsequently increases the center gap transmittance due to the mode conversion effect. Oblique incidence with angles of about 1° results in truncated gap depth in acoustic transmission spectra from about  -80 dB, and deeper, to about  -40 dB and shallower. The spectra were simulated by employing the stiffness matrix method. Porosity-dependent acoustic viscous damping was included in the calculations. A way to optimize reflectors in the frequency range, where the forbidden gaps for longitudinal and shear waves overlap, is discussed.

  17. SLOPE PROFILOMETRY OF GRAZING INCIDENCE OPTICS.

    SciTech Connect

    TAKACS,P.Z.

    2003-01-14

    Profiling instruments are well-suited to the measurement of grazing incidence optics, such as those found in synchrotron radiation beam lines. Slope measuring profilers, based upon the principle of the pencil beam interferometer, have proven to be especially useful in measuring the figure and slope errors on cylindrical aspheres. The Long Trace Profiler, in various configurations, is the most widely used of this class of profiler. Current performance provides slope measurement accuracy at the microradian level and height measurements accurate to 25 nm over 1 meter trace lengths.

  18. Figure and finish of grazing incidence mirrors

    SciTech Connect

    Takacs, P.Z. ); Church, E.L. . Army Armament Research, Development and Engineering Center)

    1989-08-01

    Great improvement has been made in the past several years in the quality of optical components used in synchrotron radiation (SR) beamlines. Most of this progress has been the result of vastly improved metrology techniques and instrumentation permitting rapid and accurate measurement of the surface finish and figure on grazing incidence optics. A significant theoretical effort has linked the actual performance of components used as x-ray wavelengths to their topological properties as measured by surface profiling instruments. Next-generation advanced light sources will require optical components and systems to have sub-arc second surface figure tolerances. This paper will explore the consequences of these requirements in terms of manufacturing tolerances to see if the present manufacturing state-of-the-art is capable of producing the required surfaces. 15 refs., 14 figs., 2 tabs.

  19. Aplanatic grazing incidence diffraction grating: a new optical element

    SciTech Connect

    Hettrick, M.C.

    1986-09-15

    We present the theory of a grazing incidence reflection grating capable of imaging at submicron resolution. The optic is mechanically ruled on a spherical or cylindrical surface with varied groove spacings, delivering diffraction-limited response and a wide field of view at a selected wavelength. Geometrical aberrations are calculated on the basis of Fermat's principle, revealing significant improvements over a grazing incidence mirror. Aplanatic and quasi-aplanatic versions of the grating have applications in both imaging and scanning microscopes, microprobes, collimators, and telescopes. A 2-D crossed system of such gratings, similar to the grazing incidence mirror geometry of Kirkpatrick and Baez, could potentially provide spatial resolutions of --200 A.

  20. Small angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Cousin, Fabrice

    2015-10-01

    Small Angle Neutron Scattering (SANS) is a technique that enables to probe the 3-D structure of materials on a typical size range lying from ˜ 1 nm up to ˜ a few 100 nm, the obtained information being statistically averaged on a sample whose volume is ˜ 1 cm3. This very rich technique enables to make a full structural characterization of a given object of nanometric dimensions (radius of gyration, shape, volume or mass, fractal dimension, specific area…) through the determination of the form factor as well as the determination of the way objects are organized within in a continuous media, and therefore to describe interactions between them, through the determination of the structure factor. The specific properties of neutrons (possibility of tuning the scattering intensity by using the isotopic substitution, sensitivity to magnetism, negligible absorption, low energy of the incident neutrons) make it particularly interesting in the fields of soft matter, biophysics, magnetic materials and metallurgy. In particular, the contrast variation methods allow to extract some informations that cannot be obtained by any other experimental techniques. This course is divided in two parts. The first one is devoted to the description of the principle of SANS: basics (formalism, coherent scattering/incoherent scattering, notion of elementary scatterer), form factor analysis (I(q→0), Guinier regime, intermediate regime, Porod regime, polydisperse system), structure factor analysis (2nd Virial coefficient, integral equations, characterization of aggregates), and contrast variation methods (how to create contrast in an homogeneous system, matching in ternary systems, extrapolation to zero concentration, Zero Averaged Contrast). It is illustrated by some representative examples. The second one describes the experimental aspects of SANS to guide user in its future experiments: description of SANS spectrometer, resolution of the spectrometer, optimization of spectrometer

  1. Analysis of FEL optical systems with grazing incidence mirrors

    SciTech Connect

    Knapp, C.E.; Viswanathan, V.K.; Bender, S.C.; Appert, Q.D.; Lawrence, G.; Barnard, C.

    1986-01-01

    The use of grazing incidence optics in resonators alleviates the problem of damage to the optical elements and permits higher powers in cavities of reasonable dimensions for a free electron laser (FEL). The design and manufacture of a grazing incidence beam expander for the Los Alamos FEL mock-up has been completed. In this paper, we describe the analysis of a bare cavity, grazing incidence optical beam expander for an FEL system. Since the existing geometrical and physical optics codes were inadequate for such an analysis, the GLAD code was modified to include global coordinates, exact conic representation, raytracing, and exact aberration features to determine the alignment sensitivities of laser resonators. A resonator cavity has been manufactured and experimentally setup in the Optical Evaluation Laboratory at Los Alamos. Calculated performance is compared with the laboratory measurements obtained so far.

  2. Grazing incidence toroidal mirror pairs in imaging and spectroscopic applications.

    PubMed

    Malvezzi, A M; Tondello, G

    1983-08-15

    The optical performance of pairs of toroidal mirrors in grazing incidence has been studied analytically and numerically. Two types of toroidal surface are possible: football and bicycle tire. In grazing incidence and for configurations that compensate up to second-order aberrations, there are significant differences in performance between the two types. For football-type tori the best configuration appears to be Z-shaped with tangential and sagittal foci at the middle point between the mirrors. For bicycle tire-type tori the best configuration is U-shaped with the tangential focus at the middle point and the sagittal at infinity.

  3. Parametric x-ray radiation for the grazing incidence geometry

    SciTech Connect

    Feranchuk, I. D.; Benediktovitch, A. I.

    2010-03-24

    A new scheme for generation of parametric x-ray radiation without beam and crystal destruction is proposed. The beam of ultrarelativistic charged particles propagates in vacuum near the crystal surface while the photons are emitted under conditions of grazing incidence diffraction. Spectral and angular properties of the radiation are calculated and restrictions on beam parameters are investigated.

  4. Diffraction of H from LiF(001): From slow normal incidence to fast grazing incidence

    NASA Astrophysics Data System (ADS)

    Muzas, A. S.; Gatti, F.; Martín, F.; Díaz, C.

    2016-09-01

    Describing diffraction of atomic and molecular projectiles at fast grazing incidence presents a real challenge for quantum theoretical simulations due to the high incidence energy (100 eV-1 keV) used in experiments. This is one of the main reasons why most theoretical simulations performed to date are based on reduced dimensional models. Here we analyze two alternatives to reduce the computational effort, while preserving the real dimensionality of the system. First, we show that grazing incidence conditions are already fulfilled for incidence angles ⩽ 5 ° , i.e., incidence angles higher than those typically used in experiments. Thus, accurate comparisons with experiment can be performed considering diffraction at grazing incidence, but with smaller total incidence energies, whilst keeping the same experimental normal energy in the calculations. Second, we show that diffraction probabilities obtained at fast grazing incidence are fairly well reproduced by simulations performed at slow normal incidence. This latter approach would allow one to simulate several experimental spectra, measured at the same normal incidence energy for several incidence crystallographic directions, with only one calculation. This approach requires to keep the full dimensionality of the system.

  5. Novel micro-reactor flow cell for investigation of model catalysts using in situ grazing-incidence X-ray scattering.

    PubMed

    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.

  6. Grazing incidence off Rowland spectrometer with shifted slit.

    PubMed

    Antsiferov, P S; Dorokhin, L A; Krainov, P V

    2016-05-01

    The article presents the analysis of the scheme of grazing incidence spectrometer with the normal to the line of site registration of the spectrum. The scheme is intended for the usage of the micro channel plate assembly as a spectrum detector. The main feature is the displacement of the entrance slit from the Rowland circle. The results of the experimental test of the spectral resolution (λ/δλ around 200) are presented and compared with the theoretical estimations. PMID:27250391

  7. Astronomical applications of grazing incidence telescopes with polynomial surfaces

    NASA Technical Reports Server (NTRS)

    Cash, W.; Shealy, D. L.; Underwood, J. H.

    1979-01-01

    The report has examined the claim that grazing incidence telescopes having surfaces described by generalized equations have image characteristics superior to those of the paraboloid-hyperboloid and Wolter-Schwarzschild configurations. With emphasis on specific applications in solar and cosmic X-ray/EUV astronomy, raytracing has shown that in many cases there is no advantage in the polynomial design, and in those cases where advantages are theoretically to be expected, the advantages are outweighed by practical considerations.

  8. Grazing Incidence Optics for X-rays Interferometry

    NASA Technical Reports Server (NTRS)

    Shipley, Ann; Zissa, David; Cash, Webster; Joy, Marshall

    1999-01-01

    Grazing incidence mirror parameters and constraints for x-ray interferometry are described. We present interferometer system tolerances and ray trace results used to define mirror surface accuracy requirements. Mirror material, surface figure, roughness, and geometry are evaluated based on analysis results. We also discuss mirror mount design constraints, finite element analysis, environmental issues, and solutions. Challenges associated with quantifying high accuracy mirror surface quality are addressed and test results are compared with theoretical predictions.

  9. Grazing incidence telescopes for x-ray astronomy

    NASA Astrophysics Data System (ADS)

    Gorenstein, Paul

    2012-01-01

    With grazing incidence telescopes, x-ray astronomy became a major branch of astrophysics. They are an indispensable tool in the study of >106 K thermal and non-thermal high energy phenomena occurring in objects from the solar system to the most distant sites in the universe. They have shed light upon dark matter and dark energy. Four cosmic missions with focusing grazing incidence x-ray telescopes based upon the Wolter 1 geometry are currently in space. They include two observatory class facilities launched in 1999, NASA's high resolution x-ray and ESA's high throughput XMM-Newton. Two others are Japan's Suzaku, performing a variety of studies, and the Swift XRT, which finds precise positions for the x-ray afterglows of gamma-ray bursts. Four new cosmic missions with Wolter-like focusing telescopes are scheduled for launch. They will provide much broader bandwidth (NuSTAR and Astro-H), perform a new sky survey with more exposure time and a broader energy range than previous surveys (eROSITA), have an imaging detector with much better energy resolution (Astro-H), and measure polarization (GEMS). The Kirkpatrick-Baez and the lobster-eye are two types of potentially useful grazing incidence telescopes that have not yet been in orbit. It may not be possible to improve upon Chandra's 0.5 arcsec resolution without new technology.

  10. X-ray small-angle scattering from sputtered CeO{sub 2}/C bilayers

    SciTech Connect

    Haviar, S.; Dubau, M.; Khalakhan, I.; Vorokhta, M.; Matolinova, I.; Matolin, V.; Vales, V.; Endres, J.; Holy, V.; Buljan, M.; Bernstorff, S.

    2013-01-14

    Surface and interface morphology of cerium oxide/carbon bilayers used as thin-film catalysts is studied by grazing-incidence small-angle x-ray scattering, scanning electron microscopy, and atomic-force microscopy, and the dependence of the structural parameters on the thicknesses of the constituting layers is investigated. The applicability of x-ray scattering and its advantages over standard analytical methods are discussed.

  11. Grazing-incidence iridescence from a butterfly wing.

    PubMed

    Lawrence, Chris; Vukusic, Peter; Sambles, Roy

    2002-01-20

    The Troides magellanus butterfly exhibits a specialized iridescence that is visible only when its hind wings are both illuminated and viewed at near-grazing incidence. The effect is due to the presence of a constrained bigrating structure in its wing scales that has been previously observed in only one other species of butterfly (Ancyluris meliboeus). However, whereas the Ancyluris presents wide-angle flickering iridescence, the Troides butterfly uses pigmentary coloration at all but a narrow tailored range of angles, producing a characteristic effect. PMID:11905567

  12. Spherical mirror grazing incidence x-ray optics

    NASA Technical Reports Server (NTRS)

    Cash, Jr., Webster C. (Inventor)

    1997-01-01

    An optical system for x-rays combines at least two spherical or near spherical mirrors for each dimension in grazing incidence orientation to provide the functions of a lens in the x-ray region. To focus x-ray radiation in both the X and the Y dimensions, one of the mirrors focusses the X dimension, a second mirror focusses the Y direction, a third mirror corrects the X dimension by removing comatic aberration and a fourth mirror corrects the Y dimension. Spherical aberration may also be removed for an even better focus. The order of the mirrors is unimportant.

  13. Sputtering at grazing ion incidence: Influence of adatom islands

    SciTech Connect

    Rosandi, Yudi; Redinger, Alex; Michely, Thomas; Urbassek, Herbert M.

    2010-09-15

    When energetic ions impinge at grazing incidence onto an atomically flat terrace, they will not sputter. However, when adatom islands (containing N atoms) are deposited on the surface, they induce sputtering. We investigate this effect for the specific case of 83 deg. -incident 5 keV Ar ions on a Pt (111) surface by means of molecular-dynamics simulation and experiment. We find that - for constant coverage {Theta} - the sputter yield has a maximum at island sizes of N congruent with 10-20. A detailed picture explaining the decline of the sputter yield toward larger and smaller island sizes is worked out. Our simulation results are compared with dedicated sputtering experiments, in which a coverage of {Theta}=0.09 of Pt adatoms are deposited onto the Pt (111) surface and form islands with a broad distribution around a most probable size of N congruent with 20.

  14. Fluence thresholds for grazing incidence hard x-ray mirrors

    SciTech Connect

    Aquila, A.; Ozkan, C.; Sinn, H.; Tschentscher, T.; Mancuso, A. P.; Gaudin, J.; Sobierajski, R.; Klepka, M. T.; Dłużewski, P.; Morawiec, K.; Störmer, M.; Bajt, S.; Ohashi, H.; Koyama, T.; Tono, K.; Inubushi, Y. [RIKEN and others

    2015-06-15

    X-ray Free Electron Lasers (XFELs) have the potential to contribute to many fields of science and to enable many new avenues of research, in large part due to their orders of magnitude higher peak brilliance than existing and future synchrotrons. To best exploit this peak brilliance, these XFEL beams need to be focused to appropriate spot sizes. However, the survivability of X-ray optical components in these intense, femtosecond radiation conditions is not guaranteed. As mirror optics are routinely used at XFEL facilities, a physical understanding of the interaction between intense X-ray pulses and grazing incidence X-ray optics is desirable. We conducted single shot damage threshold fluence measurements on grazing incidence X-ray optics, with coatings of ruthenium and boron carbide, at the SPring-8 Angstrom compact free electron laser facility using 7 and 12 keV photon energies. The damage threshold dose limits were found to be orders of magnitude higher than would naively be expected. The incorporation of energy transport and dissipation via keV level energetic photoelectrons accounts for the observed damage threshold.

  15. Fluence thresholds for grazing incidence hard x-ray mirrors

    NASA Astrophysics Data System (ADS)

    Aquila, A.; Sobierajski, R.; Ozkan, C.; Hájková, V.; Burian, T.; Chalupský, J.; Juha, L.; Störmer, M.; Bajt, S.; Klepka, M. T.; DłuŻewski, P.; Morawiec, K.; Ohashi, H.; Koyama, T.; Tono, K.; Inubushi, Y.; Yabashi, M.; Sinn, H.; Tschentscher, T.; Mancuso, A. P.; Gaudin, J.

    2015-06-01

    X-ray Free Electron Lasers (XFELs) have the potential to contribute to many fields of science and to enable many new avenues of research, in large part due to their orders of magnitude higher peak brilliance than existing and future synchrotrons. To best exploit this peak brilliance, these XFEL beams need to be focused to appropriate spot sizes. However, the survivability of X-ray optical components in these intense, femtosecond radiation conditions is not guaranteed. As mirror optics are routinely used at XFEL facilities, a physical understanding of the interaction between intense X-ray pulses and grazing incidence X-ray optics is desirable. We conducted single shot damage threshold fluence measurements on grazing incidence X-ray optics, with coatings of ruthenium and boron carbide, at the SPring-8 Angstrom compact free electron laser facility using 7 and 12 keV photon energies. The damage threshold dose limits were found to be orders of magnitude higher than would naively be expected. The incorporation of energy transport and dissipation via keV level energetic photoelectrons accounts for the observed damage threshold.

  16. Design and development of grazing incidence x-ray mirrors

    NASA Astrophysics Data System (ADS)

    Zuo, Fuchang; Mei, Zhiwu; Ma, Tao; Deng, Loulou; Shi, Yongqiang; Li, Liansheng

    2016-01-01

    X-ray pulsar navigation has attracted extensive attentions from academy and engineering domains. The navigation accuracy is can be enhanced through design of X-ray mirrors to focus X-rays to a small detector. The Wolter-I optics, originally proposed based on a paraboloid mirror and a hyperboloid mirror for X-ray imaging, has long been widely developed and employed in X-ray observatory. Some differences, however, remain in the requirements on optics between astronomical X-ray observation and pulsar navigation. The simplified Wolter-I optics, providing single reflection by a paraboloid mirror, is more suitable for pulsar navigation. In this paper, therefore, the grazing incidence X-ray mirror was designed further based on our previous work, with focus on the reflectivity, effective area, angular resolution and baffles. To evaluate the performance of the manufactured mirror, the surface roughness and reflectivity were tested. The test results show that the grazing incidence mirror meets the design specifications. On the basis of this, the reflectivity of the mirror in the working bandwidth was extrapolated to evaluate the focusing ability of the mirror when it works together with the detector. The purpose of our current work to design and develop a prototype mirror was realized. It can lay a foundation and provide guidance for the development of multilayer nested X-ray mirror with larger effective area.

  17. Wavefront Sensing Analysis of Grazing Incidence Optical Systems

    NASA Technical Reports Server (NTRS)

    Rohrbach, Scott; Saha, Timo

    2012-01-01

    Wavefront sensing is a process by which optical system errors are deduced from the aberrations in the image of an ideal source. The method has been used successfully in near-normal incidence, but not for grazing incidence systems. This innovation highlights the ability to examine out-of-focus images from grazing incidence telescopes (typically operating in the x-ray wavelengths, but integrated using optical wavelengths) and determine the lower-order deformations. This is important because as a metrology tool, this method would allow the integration of high angular resolution optics without the use of normal incidence interferometry, which requires direct access to the front surface of each mirror. Measuring the surface figure of mirror segments in a highly nested x-ray telescope mirror assembly is difficult due to the tight packing of elements and blockage of all but the innermost elements to normal incidence light. While this can be done on an individual basis in a metrology mount, once the element is installed and permanently bonded into the assembly, it is impossible to verify the figure of each element and ensure that the necessary imaging quality will be maintained. By examining on-axis images of an ideal point source, one can gauge the low-order figure errors of individual elements, even when integrated into an assembly. This technique is known as wavefront sensing (WFS). By shining collimated light down the optical axis of the telescope and looking at out-of-focus images, the blur due to low-order figure errors of individual elements can be seen, and the figure error necessary to produce that blur can be calculated. The method avoids the problem of requiring normal incidence access to the surface of each mirror segment. Mirror figure errors span a wide range of spatial frequencies, from the lowest-order bending to the highest order micro-roughness. While all of these can be measured in normal incidence, only the lowest-order contributors can be determined

  18. Grazing Incidence Pumping for Efficient X-ray Lasers

    SciTech Connect

    Dunn, J; Keenan, R; Patel, P K; Price, D F; Smith, R F; Shlyaptsev, V N

    2004-09-30

    We report progress in developing efficient pumping of laser-driven x-ray lasers that opens new possibilities for both high average power x-ray lasers as well as producing progressively shorter wavelength lasers. The new scheme of grazing incidence pumping (GRIP) is described. In essence, a chosen electron density region of a pre-formed plasma column, produced by a longer pulse at normal incidence onto a slab target, is selectively pumped by focusing the short pulse {approx}ps laser at a determined grazing incidence angle to the target. The controlled use of refraction of the pumping laser in the plasma results in several benefits: The pump laser path length is longer and there is an increase in the laser absorption in the gain region for creating a collisional Ni-like ion x-ray laser. There is also an inherent traveling wave, close to c, that increases the overall pumping efficiency. The scheme requires careful tailoring of the pump and plasma conditions to the specific x-ray laser under investigation but the main advantage is a 3 - 30 times reduction in the laser pump energy for mid-Z materials. We report several examples of this new x-ray laser on two different laser systems. The first demonstrates a 10 Hz x-ray laser operating at 18.9 nm pumped with a total of 150 mJ of 800 nm wavelength from a Ti:Sapphire laser. The second case is shown where the COMET laser is used both at 527 nm and 1054 nm wavelength to pump higher Z materials with the goal of extending the wavelength regime of tabletop x-ray lasers below 10 nm.

  19. Ground effects on aircraft noise. [near grazing incidence

    NASA Technical Reports Server (NTRS)

    Willshire, W. L., Jr.; Hilton, D. A.

    1979-01-01

    A flight experiment was conducted to investigate air-to-ground propagation of sound near grazing incidence. A turbojet-powered aircraft was flown at low altitudes over the ends of two microphone arrays. An eight-microphone array was positioned along a 1850 m concrete runway. The second array consisted of 12 microphones positioned parallel to the runway over grass. Twenty-eight flights were flown at altitudes ranging from 10 m to 160 m. The acoustic data recorded in the field reduced to one-third-octave band spectra and time correlated with the flight and weather information. A small portion of the data was further reduced to values of ground attenuation as a function of frequency and incidence angle by two different methods. In both methods, the acoustic signals compared originated from identical sources. Attenuation results obtained by using the two methods were in general agreement. The measured ground attenuation was largest in the frequency range of 200 to 400 Hz. A strong dependence was found between ground attenuation and incidence angle with little attenuation measured for angles of incidence greater than 10 to 15 degrees.

  20. Study of the in-plane magnetic structure of a layered system using polarized neutron scattering under grazing incidence geometry

    NASA Astrophysics Data System (ADS)

    Maruyama, R.; Bigault, T.; Wildes, A. R.; Dewhurst, C. D.; Soyama, K.; Courtois, P.

    2016-05-01

    The in-plane magnetic structure of a layered system with a polycrystalline grain size less than the ferromagnetic exchange length was investigated using polarized neutron off-specular scattering and grazing incidence small angle scattering measurements to gain insight into the mechanism that controls the magnetic properties which are different from the bulk. These complementary measurements with different length scales and the data analysis based on the distorted wave Born approximation revealed the lateral correlation on a length scale of sub- μm due to the fluctuating orientation of the magnetization in the layer. The obtained in-plane magnetic structure is consistent with the random anisotropy model, i.e. competition between the exchange interactions between neighboring spins and the local magnetocrystalline anisotropy.

  1. Grazing Incidence Pumping for High Efficiency X-ray Lasers

    SciTech Connect

    Dunn, J; Keenan, R; Shlyaptsev, V N

    2005-10-03

    Over the last decade, most laser-driven collisional excitation x-ray lasers have relied on the absorption of the pump energy incident at normal incidence to a pre-formed plasma. The main advantage is that the inversion can be created at various plasma regions in space and time where the amplification and ray propagation processes are best served. The main disadvantage is that different plasma regions regardless of the contribution to the inversion have to be pumped simultaneously in order to make the laser work. This leads to a loss of efficiency. The new scheme of grazing incidence pumping (GRIP) addresses this issue. In essence, a chosen electron density region of a pre-formed plasma column, produced by a longer pulse at normal incidence onto a slab target, is selectively pumped by focusing a short pulse of 100 fs-10 ps duration laser at a determined grazing incidence angle to the target surface. The exact angle is dependent on the pump wavelength and relates to refraction of the drive beam in the plasma. The controlled use of refraction of the pumping laser in the plasma results in several benefits: The pump laser path length is longer and there is an increase in the laser absorption in the gain region for creating a collisional Ni-like ion x-ray laser. There is also an inherent traveling wave, close to c, that increases the overall pumping efficiency. This can lead to a 3-30 times reduction in the pump energy for mid-Z, sub-20 nm lasers. We report several examples of this new x-ray laser on two different laser systems. The first demonstrates a 10 Hz x-ray laser operating at 18.9 nm pumped with a total of 150 mJ of 800 nm wavelength from a Ti:Sapphire laser. The second case is shown where the COMET laser is used both at 527 nm and 1054 nm wavelength to pump higher Z materials with the goal of extending the wavelength regime of tabletop x-ray lasers below 10 nm.

  2. The design and evaluation of grazing incidence relay optics

    NASA Technical Reports Server (NTRS)

    Davis, John M.; Chase, R. C.; Silk, J. K.; Krieger, A. S.

    1989-01-01

    X-ray astronomy, both solar and celestial, has many needs for high spatial resolution observations which have to be performed with electronic detectors. If the resolution is not to be detector limited, plate scales in excess of 25 microns arc/sec, corresponding to focal lengths greater than 5 m, are required. In situations where the physical size is restricted, the problem can be solved by the use of grazing incidence relay optics. A system was developed which employs externally polished hyperboloid-hyperboloid surfaces to be used in conjunction with a Wolter-Schwarzschild primary. The secondary is located in front of the primary focus and provides a magnification of 4, while the system has a plate scale of 28 microns arc/sec and a length of 1.9 m. The design, tolerance specification, fabrication and performance at visible and X-ray wavelengths of this optical system are described.

  3. Grazing-Incidence Neutron Optics based on Wolter Geometries

    NASA Technical Reports Server (NTRS)

    Gubarev, M. V.; Ramsey, B. D.; Mildner, D. F. R.

    2008-01-01

    The feasibility of grazing-incidence neutron imaging optics based on the Wolter geometries have been successfully demonstrated. Biological microscopy, neutron radiography, medical imaging, neutron crystallography and boron neutron capture therapy would benefit from high resolution focusing neutron optics. Two bounce optics can also be used to focus neutrons in SANS experiments. Here, the use of the optics would result in lower values of obtainable scattering angles. The high efficiency of the optics permits a decrease in the minimum scattering vector without lowering the neutron intensity on sample. In this application, a significant advantage of the reflective optics over refractive optics is that the focus is independent of wavelength, so that the technique can be applied to polychromatic beams at pulsed neutron sources.

  4. Manufacturing and testing of a grazing incidence mirror

    NASA Astrophysics Data System (ADS)

    Grindel, Manfred W.; Stolz, Christopher J.

    Fabrication and testing of aspheric surfaces has always been a challenge for the optical industry. A mirror that is part of an ellipsoid is particularly difficult to manufacture when the axis of rotation does not intersect the surface and the radii change in two directions. Another difficulty in fabrication is the stringent specifications imposed by the nature of the application of the mirror. The physical requirements are for a 50 mm thick piece of fused silica with a 400 x 100 mm surface area platinum coated for use at grazing incidence. The mirror is used to image energy from a synchroton radiation source at one focus. The tolerances require a high figure accuracy, small slope deviations, and a minimum of surface roughness. The purpose of this paper is to present the methods used to fabricate and test such an elliptical mirror as described.

  5. Image processing for grazing incidence fast atom diffraction

    NASA Astrophysics Data System (ADS)

    Debiossac, Maxime; Roncin, Philippe

    2016-09-01

    Grazing incidence fast atom diffraction (GIFAD, or FAD) has developed as a surface sensitive technique. Compared with thermal energies helium diffraction (TEAS or HAS), GIFAD is less sensitive to thermal decoherence but also more demanding in terms of surface coherence, the mean distance between defects. Such high quality surfaces can be obtained from freshly cleaved crystals or in a molecular beam epitaxy (MBE) chamber where a GIFAD setup has been installed allowing in situ operation. Based on recent publications by Atkinson et al. (2014) and Debiossac et al. (2014), the paper describes in detail the basic steps needed to measure the relative intensities of the diffraction spots. Care is taken to outline the underlying physical assumptions.

  6. Development of metrology instruments for grazing incidence mirrors

    SciTech Connect

    Takacs, P.Z. ); Church, E.L. ); Qian, Shi-nan . Hefei National Synchrotron Radiation Lab.); Liu, Wuming . Inst. of High Energy Physics)

    1989-10-01

    The effective utilization of synchrotron radiation (SR) from high-brightness sources requires the use of optical components with very smooth surfaces and extremely precise shapes. Most manufacturers are not capable of measuring the figure and finish quality of the aspheric optics required for use in grazing incidence beam lines. Over the past several years we have developed measurement techniques and metrology instrumentation that have allowed us to measure the surface profile and roughness of large cylinder optics, up to one meter in length. Based on our measurements and feedback, manufacturers have been able to advance the state-of-the-art in mirror fabrication and are now able to produce acceptable components. Our analysis techniques enable designers to write meaningful specifications and predict the performance of real surfaces in their particular beamline configurations. Commercial instruments are now available for measuring surface microroughness with spatial periods smaller than about one millimeter. No commercial instruments are available for measuring the surface figure on cylindrical aspheres over long spatial periods, from one millimeter up to one meter. For that reason we developed a Long Trace Profiler (LTP) that measures surface profile over the long period range in a non-contact manner to extremely high accuracy. Examples of measured surfaces and data analysis techniques will be discussed, and limitations on the quality of optical surfaces related to intrinsic material properties will also be discussed. 15 refs., 14 figs., 2 tabs.

  7. Development of adjustable grazing incidence optics for Generation-X

    NASA Astrophysics Data System (ADS)

    Reid, Paul B.; Murray, Stephen S.; Trolier-McKinstry, Susan; Freeman, Mark; Juda, Michael; Podgorski, William; Ramsey, Brian; Schwartz, Daniel

    2008-07-01

    For X-ray astronomy, 0.1 arc-second imaging resolution will result in a significant advance in our understanding of the Universe. Similarly, the advent of low cost high performance X-ray mirrors will also increase the likelihood of more X-ray telescopes being funded and built. We discuss the development plans of two different types of adjustable grazing incidence optics: one being a tenth arc-second resolution bimorph mirror approach also suitable for extremely large collecting areas, and the second being a few arc-second radially adjustable mirror approach more suitable for modest sized telescopes. Bimorph mirrors will be developed using thin (0.1 - 0.4 mm) thermally formed glass or electroplated metal mirror segments with thin film piezo-electric actuators deposited directly on the mirror back surface. Mirror figure will be adjusted on-orbit. Radially adjustable mirrors will employ discreet radially electrostrictive actuators for mirror alignment and low spatial error frequency figure correction during assembly and alignment. In this paper we report on. In this paper we describe mirror design and our development plans for both mirror concepts.

  8. Development of Grazing Incidence Optics for Neutron Imaging and Scattering

    NASA Technical Reports Server (NTRS)

    Gubarev, M. V.; Khaykovich, B.; Liu, D.; Ramsey, B. D.; Zavlin, V. E.; Kilaru, K.; Romaine, S.; Rosati, R. E.; Bruni, R.; Moncton, D. E.

    2012-01-01

    Because of their wave nature, thermal and cold neutrons can be reflected from smooth surfaces at grazing incidence angles, be reflected by multilayer coatings or be refracted at boundaries of different materials. The optical properties of materials are characterized by their refractive indices which are slightly less than unity for most elements and their isotopes in the case of cold and thermal neutrons as well as for x-rays. The motivation for the optics use for neutrons as well as for x-rays is to increase the signal rate and, by virtue of the optic's angular resolution, to improve the signal-to-noise level by reducing the background so the efficiency of the existing neutron sources use can be significantly enhanced. Both refractive and reflective optical techniques developed for x-ray applications can be applied to focus neutron beams. Typically neutron sources have lower brilliance compared to conventional x-ray sources so in order to increase the beam throughput the neutron optics has to be capable of capturing large solid angles. Because of this, the replicated optics techniques developed for x-ray astronomy applications would be a perfect match for neutron applications, so the electroformed nickel optics under development at the Marshall Space Flight Center (MSFC) can be applied to focus neutron beams. In this technique, nickel mirror shells are electroformed onto a figured and superpolished nickel-plated aluminum cylindrical mandrel from which they are later released by differential thermal contraction. Cylindrical mirrors with different diameters, but the same focal length, can be nested together to increase the system throughput. The throughput can be increased further with the use of the multilayer coatings deposited on the reflectivr surface of the mirror shells. While the electroformed nickel replication technique needs to be adopted for neutron focusing, the technology to coat the inside of cylindrical mirrors with neutron multilayers has to be

  9. A High Efficiency Grazing Incidence Pumped X-ray Laser

    SciTech Connect

    Dunn, J; Keenan, R; Price, D F; Patel, P K; Smith, R F; Shlyaptsev, V N

    2006-08-31

    The main objective of the project is to demonstrate a proof-of-principle, new type of high efficiency, short wavelength x-ray laser source that will operate at unprecedented high repetition rates (10Hz) that could be scaled to 1kHz or higher. The development of a high average power, tabletop x-ray laser would serve to complement the wavelength range of 3rd and future 4th generation light sources, e.g. the LCLS, being developed by DOE-Basic Energy Sciences. The latter are large, expensive, central, synchrotron-based facilities while the tabletop x-ray laser is compact, high-power laser-driven, and relatively inexpensive. The demonstration of such a unique, ultra-fast source would allow us to attract funding from DOE-BES, NSF and other agencies to pursue probing of diverse materials undergoing ultrafast changes. Secondly, this capability would have a profound impact on the semiconductor industry since a coherent x-ray laser source would be ideal for ''at wavelength'' {approx}13 nm metrology and microscopy of optics and masks used in EUV lithography. The project has major technical challenges. We will perform grazing-incidence pumped laser-plasma experiments in flat or groove targets which are required to improve the pumping efficiency by ten times. Plasma density characterization using our existing unique picosecond x-ray laser interferometry of laser-irradiated targets is necessary. Simulations of optical laser propagation as well as x-ray laser production and propagation through freely expanding and confined plasma geometries are essential. The research would be conducted using the Physics Directorate Callisto and COMET high power lasers. At the end of the project, we expect to have a high-efficiency x-ray laser scheme operating below 20 nm at 10Hz with a pulse duration of {approx}2 ps. This will represent the state-of-the-art in x-ray lasers and would be a major step forward from our present picosecond laser-driven x-ray lasers. There is an added bonus of creating

  10. Grazing exit versus grazing incidence geometry for x-ray absorption near edge structure analysis of arsenic traces

    SciTech Connect

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

    2009-04-01

    In the presented study the grazing exit x-ray fluorescence was tested for its applicability to x-ray absorption near edge structure analysis of arsenic in droplet samples. The experimental results have been compared to the findings of former analyses of the same samples using a grazing incidence (GI) setup to compare the performance of both geometries. Furthermore, the investigations were accomplished to gain a better understanding of the so called self-absorption effect, which was observed and investigated in previous studies using a GI geometry. It was suggested that a normal incidence-grazing-exit geometry would not suffer from self-absorption effects in x-ray absorption fine structure (XAFS) analysis due to the minimized path length of the incident beam through the sample. The results proved this assumption and in turn confirmed the occurrence of the self-absorption effect for GI geometry. Due to its lower sensitivity it is difficult to apply the GE geometry to XAFS analysis of trace amounts (few nanograms) of samples but the technique is well suited for the analysis of small amounts of concentrated samples.

  11. Grazing-incidence X-ray diffraction from a crystal with subsurface defects

    SciTech Connect

    Gaevskii, A. Yu. Golentus, I. E.

    2015-03-15

    The diffraction of X rays incident on a crystal surface under grazing angles under conditions of total external reflection has been investigated. An approach is proposed in which exact solutions to the dynamic problem of grazing-incidence diffraction in an ideal crystal are used as initial functions to calculate the diffuse component of diffraction in a crystal with defects. The diffuse component of diffraction is calculated for a crystal with surface defects of a dilatation-center type. Exact formulas of the continuum theory which take into account the mirror-image forces are used for defect-induced atomic displacements. Scattering intensity maps near Bragg peaks are constructed for different scan modes, and the conditions for detecting primarily the diffuse component are determined. The results of dynamic calculations of grazing-incidence diffraction in defect-containing crystals are compared with calculations in the kinematic approximation.

  12. Varied-space grazing incidence gratings in high resolution scanning spectrometers

    SciTech Connect

    Hettrick, M.C.; Underwood, J.H.

    1986-10-01

    We discuss the dominant geometrical aberrations of a grazing incidence reflection grating and new techniques which can be used to reduce or eliminate them. Convergent beam geometries and the aberration correction possible with varied groove spacings are each found to improve the spectral resolution and speed of grazing incidence gratings. In combination, these two techniques can result in a high resolution (lambda/..delta..lambda > 10/sup 4/) monochromator or scanning spectrometer with a simple rotational motion for scanning wavelength or selecting the spectral band. 21 refs., 4 figs.

  13. A grazing incidence x-ray streak camera for ultrafast, single-shot measurements

    SciTech Connect

    Feng, Jun; Engelhorn, K.; Cho, B.I.; Lee, H.J.; Greaves, M.; Weber, C.P.; Falcone, R.W.; Padmore, H. A.; Heimann, P.A.

    2010-02-18

    An ultrafast x-ray streak camera has been realized using a grazing incidence reflection photocathode. X-rays are incident on a gold photocathode at a grazing angle of 20 degree and photoemitted electrons are focused by a large aperture magnetic solenoid lens. The streak camera has high quantum efficiency, 600fs temporal resolution, and 6mm imaging length in the spectral direction. Its single shot capability eliminates temporal smearing due to sweep jitter, and allows recording of the ultrafast dynamics of samples that undergo non-reversible changes.

  14. Grazing incidence technique to obtain spatially resolved spectra from laser heated plasmas

    NASA Technical Reports Server (NTRS)

    Behring, W. E.; Underwood, J. H.; Brown, C. M.; Feldman, U.; Seely, John F.

    1988-01-01

    An experimental method is described in which a grazing incidence spectrograph is used to obtain spatially resolved spectra of laser heated plasmas in the 6-370-A region. In the experiment, small target spheres were irradiated by tightly focused laser beams. A tilted grazing incidence elliptical mirror placed 1.3 m from the target focuses the plasma radiation on the spectrograph slit at a distance of 0.7 m producing a useful degree of spatial resolution in the recorded spectral lines. The spectrum from a copper target is presented together with an X-ray pinhole camera image of the plasma.

  15. Design, fabrication and performance of two grazing incidence telescopes for celestial extreme ultraviolet astronomy

    NASA Technical Reports Server (NTRS)

    Lampton, M.; Cash, W.; Malina, R. F.; Bowyer, S.

    1977-01-01

    The design and performance of grazing incidence telescopes for celestial extreme ultraviolet (EUV) astronomy are described. The telescopes basically consist of a star tracker, collimator, grazing incidence mirror, vacuum box lid, vacuum housing, filters, a ranicon detector, an electronics box, and an aspect camera. For the survey mirror a Wolter-Schwarzschild type II configuration was selected. Diamond-turning was used for mirror fabrication, a technique which machines surfaces to the order of 10 microns over the required dimensions. The design of the EUV spectrometer is discussed with particular reference to the optics for a primarily spectroscopic application and the fabrication of the f/10 optics.

  16. Soller collimators for small angle neutron scattering

    SciTech Connect

    Crawford, R.K.; Epperson, J.E.; Thiyagarajan, P.

    1988-09-30

    Small angle diffractometers at pulsed sources need to have fairly short flight paths if they are to make use of the long-wavelength portion of the spectrum without encountering problems from frame overlap or sacrificing intensity with band-limiting or pulse-removing choppers. With such short flight paths, achieving the necessary angular collimation in the incident beam while utilizing the full source size (/approximately/10 cm diameter) and a reasonable sample size (/approximately/1 cm diameter) requires the use of converging multiple-aperture collimation. If the collimation channels are all focused to the same point on the detector then the large sample size will not affect Q/sub min/ or the Q-resolution, even if the sample-to-detector distance is short. The Small Angle Diffractometer (SAD) at IPNS uses crossed converging soller collimators to provide focusing multiple-aperture collimation having /approximately/400 converging beam channels with essentially no ''dead'' space between them. This entire collimator system occupies a distance of only /approximately/60 cm along the incident flight path, while providing angular collimation of 0.003 radians FWHM. The dimensions for the SAD upstream collimator are L/sub c/ = 32.8 cm, d/sub 1/ = 0.974 mm, d/sub 2/ = 0.851 mm, while for the SAD downstream collimator L/sub c/ = 25.0 cm, d/sub 1/ - 0.844 mm, d/sub 2/ = 0.750 mm. Each of these collimators has 20 blades defining 21 horizontal or vertical channels. 4 refs., 6 figs.

  17. Biomedical nuclear and X-ray imager using high-energy grazing incidence mirrors

    DOEpatents

    Ziock, Klaus-Peter; Craig, William W.; Hasegawa, Bruce; Pivovaroff, Michael J.

    2005-09-27

    Imaging of radiation sources located in a subject is explored for medical applications. The approach involves using grazing-incidence optics to form images of the location of radiopharmaceuticals administered to a subject. The optics are "true focusing" optics, meaning that they project a real and inverted image of the radiation source onto a detector possessing spatial and energy resolution.

  18. Coherent Reflection of He Atom Beams from Rough Surfaces at Grazing Incidence

    SciTech Connect

    Zhao, Bum Suk; Schewe, H. Christian; Meijer, Gerard; Schoellkopf, Wieland

    2010-09-24

    We report coherent reflection of thermal He atom beams from various microscopically rough surfaces at grazing incidence. For a sufficiently small normal component k{sub z} of the incident wave vector of the atom the reflection probability is found to be a function of k{sub z} only. This behavior is explained by quantum reflection at the attractive branch of the Casimir-van der Waals interaction potential. For larger values of k{sub z} the overall reflection probability decreases rapidly and is found to also depend on the parallel component k{sub x} of the wave vector. The material specific k{sub x} dependence for this classic reflection at the repulsive branch of the potential is discussed in terms of an averaging out of the surface roughness under grazing incidence conditions.

  19. Reactive scattering of H{sub 2} from metal surfaces under fast-grazing-incidence conditions

    SciTech Connect

    Diaz, C.; Martin, F.

    2010-07-15

    We have studied the interaction of molecular hydrogen with metal surfaces under fast-grazing-incidence conditions, by means of classical dynamics calculations based on density functional theory six-dimensional potential energy surfaces. We have performed calculations on two activated systems, H{sub 2}/NiAl(110) and H{sub 2}/Cu(111), and on two nonactivated systems, H{sub 2}/Pd(111) and H{sub 2}/Pd(110). We show that for rather open surfaces the computed 1-R probabilities (where R represents the reflectivity) as a function of the normal collision energy at grazing incidence (along low-Miller-index directions) mimic reasonably well the dissociative adsorption probabilities obtained at normal incidence and thermal energies from the dissociation threshold up to the saturation limit. Our results indicate that fast grazing incidence experiments could be used as complement to traditional sticking experiments at thermal energies to determine dissociative adsorption saturation limits, which are usually unreachable due to limitations in traditional molecular beam experiments

  20. Opto-Mechanical Analyses for Performance Optimization of Lightweight Grazing-Incidence Mirrors

    NASA Technical Reports Server (NTRS)

    Roche, Jacqueline; Kolodziejczak, Jeff; Odell, Steve; Eisner, Ronald; Ramsey, Brian; Gubarev, Mikhail

    2013-01-01

    New technology in grazing-incidence mirror fabrication and assembly is necessary to achieve sub-arcsecond optics for large-area x-ray telescopes. In order to define specifications, an understanding of performance sensitivity to design parameters is crucial. MSFC is undertaking a systematic study to specify a mounting approach, mirror substrate, and testing method. Because the lightweight mirrors are typically flimsy, they are susceptible to significant distortion due to mounting and gravitational forces. Material properties of the mirror substrate along with its thickness and dimensions significantly affect the distortions caused by mounting and gravity. A parametric study of these properties and their relationship to mounting and testing schemes will indicate specifications for the design of the next generation of lightweight grazing-incidence mirrors. Initial results will be reported.

  1. Opto-mechanical Analyses for Performance Optimization of Lightweight Grazing-incidence Mirrors

    NASA Technical Reports Server (NTRS)

    Roche, Jacqueline; Kolodsiejczak, Jeffrey; Odell, Stephen; Elsner, Ronald; Weisskopf, Martin; Ramsey, Brian; Gubarev, Mikhail

    2013-01-01

    New technology in grazing-incidence mirror fabrication and assembly is necessary to achieve sub-arcsecond optics for large-area x-ray telescopes. In order to define specifications, an understanding of performance sensitivity to design parameters is crucial. MSFC is undertaking a systematic study to specify a mounting approach, mirror substrate, and testing method. Because the lightweight mirrors are typically flimsy, they are susceptible to significant distortion due to mounting and gravitational forces. Material properties of the mirror substrate along with its thickness and dimensions significantly affect the distortions caused by mounting and gravity. A parametric study of these properties and their relationship to mounting and testing schemes will indicate specifications for the design of the next generation of lightweight grazing-incidence mirrors. Initial results will be reported.

  2. Gamma rays from grazing incidence cosmic rays in the earth's atmosphere

    NASA Technical Reports Server (NTRS)

    Ulmer, Andrew

    1994-01-01

    Interactions of grazing incidence, ultra high-energy cosmic rays with the earth's atmosphere may provide a new method of studying energetic cosmic rays with gamma-ray satellites. It is found that these cosmic ray interactions may produce gamma-rays on millisecond timescales which may be detectable by satellites. An extremely low gamma-ray background for transient gamma-ray events and a large area of interaction, the earth's surface, make the scheme plausible. The effective cross section of detection of interactions for cosmic rays above 10(exp 20) eV is found to be more than two orders of magnitude higher than Earth-based detection techniques. This method may eventually offer an efficient way of probing this region of the cosmic-ray energy spectrum where events are scarce. In this paper, a conceptual model is presented for the production of short bursts of gamma-rays based on these grazing incidence encounters with the Earth's atmosphere.

  3. Differential Deposition to Correct Surface Figure Deviations in Astronomical Grazing-Incidence X-Ray Optics

    NASA Technical Reports Server (NTRS)

    Kilaru, Kiranmayee; Ramsey, Brian D.; Gubarev, Mikhail V.

    2011-01-01

    A coating technique is being developed to correct the surface figure deviations in reflective-grazing-incidence X-ray optics. These optics are typically designed to have precise conic profiles, and any deviation in this profile, as a result of fabrication, results in a degradation of the imaging performance. To correct the mirror profiles, physical vapor deposition has been utilized to selectively deposit a filler material inside the mirror shell. The technique, termed differential deposition, has been implemented as a proof of concept on miniature X-ray optics developed at MSFC for medical-imaging applications. The technique is now being transferred to larger grazing-incidence optics suitable for astronomy and progress to date is reported.

  4. Grazing incidence neutron spin echo spectroscopy: instrumentation aspects and scientific opportunities

    NASA Astrophysics Data System (ADS)

    Holderer, O.; Frielinghaus, H.; Wellert, S.; Lipfert, F.; Monkenbusch, M.; von Klitzing, R.; Richter, D.

    2014-07-01

    Grazing Incidence Neutron Spin Echo Spectroscopy (GINSES) opens new possibilities for observing the thermally driven dynamics of macromolecules close to a rigid interface. The information about the dynamics can be retrieved as a function of scattering depth of the evanescent neutron wave, on the length scale in the range of some 10-100 nm. Using a classical neutron spin echo spectrometer with a laterally collimated beam, dynamics can be measured in grazing incidence geometry. We show examples of how the interface modifies the dynamics of microemulsions, membranes and microgels. Instrumental details and possible improvements for this technique will be presented. The key issue is the low intensity for dynamics measurements with an evanescent neutron wave. Conceptual questions how a specialised instrument could improve the experimental technique will be discussed.

  5. Grazing incidence reflection coefficients of rhodium, osmium, platinum, and gold from 50 to 300 A

    NASA Technical Reports Server (NTRS)

    Hettrick, M. C.; Edelstein, J.; Flint, S. A.

    1985-01-01

    Reflectance measurements were made of several metals illuminated from various angles with light at 14 wavelengths in the interval 46.5-283 A. The metals, Rh, Os, Pt and Au were deposited as 125 A films on a binding substrate through electron beam epitaxy. Measurements were made with a grazing incidence monochromator and a reflectometer. The data generally showed lowered reflectance with increasing angles of illumination and shorter wavelengths. The reflectance peak, however, was located at wavelengths of 100-160 A, particularly at large grazing incidences. The wavelengths correspond with the 5p to epsilon-d transition in all of the elements. Rh displayed the highest overall reflectance, and both Rh and Os were more efficient than Au or Pt.

  6. High Repetition Rate Grazing Incidence Pumped X-ray Laser operating at 18.9 nm

    SciTech Connect

    Keenan, R; Dunn, J; Patel, P K; Price, D F; Smith, R F; Shlyaptsev, V N

    2004-05-11

    We have demonstrated a 10 Hz Ni-like Mo X-ray laser operating at 18.9 nm with 150 mJ total pump energy by employing a novel pumping scheme. The grazing incidence scheme is described, where a picosecond pulse is incident at a grazing angle to a Mo plasma column produced by a slab target irradiated by a 200 ps laser pulse. This scheme uses refraction of the short pulse at a pre-determined electron density to increase absorption to pump a specific gain region. The high efficiency inherent to this scheme allows a reduction in the pump energy where 70 mJ long pulse energy and 80 mJ short pulse energy are sufficient to produce lasing at a 10 Hz repetition rate. Under these conditions and by optimizing the delay between the pulses, we achieve strong amplification and saturation for 4 mm long targets.

  7. Mechanisms of pattern formation in grazing-incidence ion bombardment of Pt(111)

    SciTech Connect

    Hansen, Henri; Redinger, Alex; Messlinger, Sebastian; Stoian, Georgiana; Michely, Thomas; Rosandi, Yudi; Urbassek, Herbert M.; Linke, Udo

    2006-06-15

    Ripple patterns forming on Pt(111) due to 5 keV Ar{sup +} grazing-incidence ion bombardment were investigated by scanning tunneling microscopy in a broad temperature range from 100 to 720 K and for ion fluences up to 3x10{sup 20} ions/m{sup 2}. A detailed morphological analysis together with molecular dynamics simulations of single ion impacts allow us to develop atomic scale models for the formation of these patterns. The large difference in step edge versus terrace damage is shown to be crucial for ripple formation under grazing incidence. The importance of distinct diffusion processes--step adatom generation at kinks and adatom lattice gas formation--for temperature dependent transitions in the surface morphology is highlighted. Surprisingly, ion bombardment effects like thermal spike induced adatom production and planar subsurface channeling are important for pattern ordering.

  8. Opto-mechanical Analyses for Performance Optimization of Lightweight Grazing-incidence Mirrors

    NASA Technical Reports Server (NTRS)

    Roche, Jacqueline M.; Kolodziejczak, Jeffery J.; Odell, Stephen L.; Elsner, Ronald F.; Weisskopf, Martin C.; Ramsey, Brian; Gubarev, Mikhail V.

    2013-01-01

    New technology in grazing-incidence mirror fabrication and assembly is necessary to achieve subarcsecond optics for large-area x-ray telescopes. In order to define specifications, an understanding of performance sensitivity to design parameters is crucial. MSFC is undertaking a systematic study to specify a mounting approach, mirror substrate, and testing method. Lightweight mirrors are typically flimsy and are, therefore, susceptible to significant distortion due to mounting and gravitational forces. Material properties of the mirror substrate along with its dimensions significantly affect the distortions caused by mounting and gravity. A parametric study of these properties and their relationship to mounting and testing schemes will indicate specifications for the design of the next generation of lightweight grazing-incidence mirrors. Here we report initial results of this study.

  9. Final Report for "Accurate Numerical Models of the Secondary Electron Yield from Grazing-incidence Collisions".

    SciTech Connect

    Seth A Veitzer

    2008-10-21

    Effects of stray electrons are a main factor limiting performance of many accelerators. Because heavy-ion fusion (HIF) accelerators will operate in regimes of higher current and with walls much closer to the beam than accelerators operating today, stray electrons might have a large, detrimental effect on the performance of an HIF accelerator. A primary source of stray electrons is electrons generated when halo ions strike the beam pipe walls. There is some research on these types of secondary electrons for the HIF community to draw upon, but this work is missing one crucial ingredient: the effect of grazing incidence. The overall goal of this project was to develop the numerical tools necessary to accurately model the effect of grazing incidence on the behavior of halo ions in a HIF accelerator, and further, to provide accurate models of heavy ion stopping powers with applications to ICF, WDM, and HEDP experiments.

  10. Time-domain theory of gyrotron traveling wave amplifiers operating at grazing incidence

    SciTech Connect

    Ginzburg, N. S.; Sergeev, A. S.; Zotova, I. V.; Zheleznov, I. V.

    2015-01-15

    Time-domain theory of the gyrotron traveling wave tube (gyro-TWT) operating at grazing incidence has been developed. The theory is based on a description of wave propagation by a parabolic equation. The results of the simulations are compared with experimental results of the observation of subnanosecond pulse amplification in a gyro-TWT consisting of three gain sections separated by severs. The theory developed can also be used successfully for a description of amplification of monochromatic signals.

  11. Triple-path collector optics for grazing incident x-ray emission spectrometer

    NASA Astrophysics Data System (ADS)

    Tokushima, T.; Horikawa, Y.; Shin, S.

    2011-07-01

    A new type of collector optics was developed for grazing incident x-ray emission spectrometer. The collector optics used two cylindrical mirrors to add two extra light paths while keeping the center light path that directly illuminates the grating. The design and properties of the spectrometer using the triple-path collector optics were evaluated using ray-tracing simulations, and validity of this design in terms of throughput and energy resolution was confirmed by the experimentally obtained spectra.

  12. Triple-path collector optics for grazing incident x-ray emission spectrometer.

    PubMed

    Tokushima, T; Horikawa, Y; Shin, S

    2011-07-01

    A new type of collector optics was developed for grazing incident x-ray emission spectrometer. The collector optics used two cylindrical mirrors to add two extra light paths while keeping the center light path that directly illuminates the grating. The design and properties of the spectrometer using the triple-path collector optics were evaluated using ray-tracing simulations, and validity of this design in terms of throughput and energy resolution was confirmed by the experimentally obtained spectra. PMID:21806173

  13. Advanced grazing-incidence techniques for modern soft-matter materials analysis

    PubMed Central

    Hexemer, Alexander; Müller-Buschbaum, Peter

    2015-01-01

    The complex nano-morphology of modern soft-matter materials is successfully probed with advanced grazing-incidence techniques. Based on grazing-incidence small- and wide-angle X-ray and neutron scattering (GISAXS, GIWAXS, GISANS and GIWANS), new possibilities arise which are discussed with selected examples. Due to instrumental progress, highly interesting possibilities for local structure analysis in this material class arise from the use of micro- and nanometer-sized X-ray beams in micro- or nanofocused GISAXS and GIWAXS experiments. The feasibility of very short data acquisition times down to milliseconds creates exciting possibilities for in situ and in operando GISAXS and GIWAXS studies. Tuning the energy of GISAXS and GIWAXS in the soft X-ray regime and in time-of flight GISANS allows the tailoring of contrast conditions and thereby the probing of more complex morphologies. In addition, recent progress in software packages, useful for data analysis for advanced grazing-incidence techniques, is discussed. PMID:25610632

  14. Advanced grazing-incidence techniques for modern soft-matter materials analysis

    DOE PAGES

    Hexemer, Alexander; Müller-Buschbaum, Peter

    2015-01-01

    The complex nano-morphology of modern soft-matter materials is successfully probed with advanced grazing-incidence techniques. Based on grazing-incidence small- and wide-angle X-ray and neutron scattering (GISAXS, GIWAXS, GISANS and GIWANS), new possibilities arise which are discussed with selected examples. Due to instrumental progress, highly interesting possibilities for local structure analysis in this material class arise from the use of micro- and nanometer-sized X-ray beams in micro- or nanofocused GISAXS and GIWAXS experiments. The feasibility of very short data acquisition times down to milliseconds creates exciting possibilities forin situandin operandoGISAXS and GIWAXS studies. Tuning the energy of GISAXS and GIWAXS in themore » soft X-ray regime and in time-of flight GISANS allows the tailoring of contrast conditions and thereby the probing of more complex morphologies. In addition, recent progress in software packages, useful for data analysis for advanced grazing-incidence techniques, is discussed.« less

  15. Advanced grazing-incidence techniques for modern soft-matter materials analysis

    SciTech Connect

    Hexemer, Alexander; Müller-Buschbaum, Peter

    2015-01-01

    The complex nano-morphology of modern soft-matter materials is successfully probed with advanced grazing-incidence techniques. Based on grazing-incidence small- and wide-angle X-ray and neutron scattering (GISAXS, GIWAXS, GISANS and GIWANS), new possibilities arise which are discussed with selected examples. Due to instrumental progress, highly interesting possibilities for local structure analysis in this material class arise from the use of micro- and nanometer-sized X-ray beams in micro- or nanofocused GISAXS and GIWAXS experiments. The feasibility of very short data acquisition times down to milliseconds creates exciting possibilities forin situandin operandoGISAXS and GIWAXS studies. Tuning the energy of GISAXS and GIWAXS in the soft X-ray regime and in time-of flight GISANS allows the tailoring of contrast conditions and thereby the probing of more complex morphologies. In addition, recent progress in software packages, useful for data analysis for advanced grazing-incidence techniques, is discussed.

  16. Small Angle X-Ray Scattering Detector

    DOEpatents

    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., q.sub.max /q.sub.min.congruent.100.

  17. Grazing-incidence high-resolution stigmatic spectrograph with two optical elements.

    PubMed

    Malvezzi, A M; Garifo, L; Tondello, G

    1981-07-15

    Using two optical toroidal elements, a mirror and a grating, both working at grazing incidence, a spectrometer can be built that is stigmatic in the XUV region at one wavelength. Good compensation of the aberrations is achieved when the intermediate sagittal image is nearly at infinity. By varying the angle of incidence on the grating with simple movements, a given couple of optical elements could cover stigmatically a rather extended spectral range. If coupled with bidimensional array detectors, such a spectrograph could find applications in planned solar XUV telescopes.

  18. Growth of nano-dots on the grazing-incidence mirror surface under FEL irradiation.

    PubMed

    Kozhevnikov, I V; Buzmakov, A V; Siewert, F; Tiedtke, K; Störmer, M; Samoylova, L; Sinn, H

    2016-01-01

    A new phenomenon on X-ray optics surfaces has been observed: the growth of nano-dots (40-55 nm diameter, 8-13 nm height, 9.4 dots µm(-2) surface density) on the grazing-incidence mirror surface under irradiation by the free-electron laser (FEL) FLASH (5-45 nm wavelength, 3° grazing-incidence angle). With a model calculation it is shown that these nano-dots may occur during the growth of a contamination layer due to polymerization of incoming hydrocarbon molecules. The crucial factors responsible for the growth of nano-dots in the model are the incident peak intensity and the reflection angle of the beam. A reduction of the peak intensity (e.g. replacement of the FEL beam by synchrotron radiation) as well as a decrease of the incident angle by just 1° (from 3° to 2°) may result in the total disappearance of the nano-dots. The model calculations are compared with surface analysis of two FLASH mirrors. PMID:26698048

  19. Growth of nano-dots on the grazing-incidence mirror surface under FEL irradiation.

    PubMed

    Kozhevnikov, I V; Buzmakov, A V; Siewert, F; Tiedtke, K; Störmer, M; Samoylova, L; Sinn, H

    2016-01-01

    A new phenomenon on X-ray optics surfaces has been observed: the growth of nano-dots (40-55 nm diameter, 8-13 nm height, 9.4 dots µm(-2) surface density) on the grazing-incidence mirror surface under irradiation by the free-electron laser (FEL) FLASH (5-45 nm wavelength, 3° grazing-incidence angle). With a model calculation it is shown that these nano-dots may occur during the growth of a contamination layer due to polymerization of incoming hydrocarbon molecules. The crucial factors responsible for the growth of nano-dots in the model are the incident peak intensity and the reflection angle of the beam. A reduction of the peak intensity (e.g. replacement of the FEL beam by synchrotron radiation) as well as a decrease of the incident angle by just 1° (from 3° to 2°) may result in the total disappearance of the nano-dots. The model calculations are compared with surface analysis of two FLASH mirrors.

  20. Partially coherent X-ray wavefront propagation simulations including grazing-incidence focusing optics.

    PubMed

    Canestrari, Niccolo; Chubar, Oleg; Reininger, Ruben

    2014-09-01

    X-ray beamlines in modern synchrotron radiation sources make extensive use of grazing-incidence reflective optics, in particular Kirkpatrick-Baez elliptical mirror systems. These systems can focus the incoming X-rays down to nanometer-scale spot sizes while maintaining relatively large acceptance apertures and high flux in the focused radiation spots. In low-emittance storage rings and in free-electron lasers such systems are used with partially or even nearly fully coherent X-ray beams and often target diffraction-limited resolution. Therefore, their accurate simulation and modeling has to be performed within the framework of wave optics. Here the implementation and benchmarking of a wave-optics method for the simulation of grazing-incidence mirrors based on the local stationary-phase approximation or, in other words, the local propagation of the radiation electric field along geometrical rays, is described. The proposed method is CPU-efficient and fully compatible with the numerical methods of Fourier optics. It has been implemented in the Synchrotron Radiation Workshop (SRW) computer code and extensively tested against the geometrical ray-tracing code SHADOW. The test simulations have been performed for cases without and with diffraction at mirror apertures, including cases where the grazing-incidence mirrors can be hardly approximated by ideal lenses. Good agreement between the SRW and SHADOW simulation results is observed in the cases without diffraction. The differences between the simulation results obtained by the two codes in diffraction-dominated cases for illumination with fully or partially coherent radiation are analyzed and interpreted. The application of the new method for the simulation of wavefront propagation through a high-resolution X-ray microspectroscopy beamline at the National Synchrotron Light Source II (Brookhaven National Laboratory, USA) is demonstrated.

  1. An analysis of grazing incidence metal mirrors in a laser ICF reactor driver

    SciTech Connect

    Bieri, R.; Guinan, M.

    1991-07-12

    Grazing incidence metal mirrors (GIMMs) are examined to replace dielectric mirrors for the final elements in a laser beam line for an inertial confinement fusion reactor. For a laser driver with a wavelength from 250 to 500 nm in a 10-ms pulse, irradiated mirrors made of Al, Al alloys, or Mg were found to have calculated laser damage limits of 0.3--2.3 J/cm{sup 2} of beam energy and neutron lifetime fluence limits of over 5 {times} 10{sup 20} 14 MeV n/cm{sup 2} when used at grazing incidence and operated at room temperature or at 77 K. A final focusing system including mirrors made of Al alloy 7475 at room temperature or at liquid nitrogen temperatures used with a driver which delivers 5 MJ of beam energy in 32 beams would require 32 mirrors of roughly 10 m{sup 2} each. This chapter includes calculations of damage limits for GIMMs and discusses critical issues relevant to the integrity and lifetime of such mirrors in a reactor environment. The reflectivities of various metals are calculated from measured optical constants at room temperature and at cryogenic temperatures for 250- to 500-nm light at both normal and grazing incidence. Then, for the mirrors in a representative system, the thermal absorption and conduction rates of the best candidate metals are used with the maximum allowable cyclic thermal stress to give the maximum allowed surface-temperature rise and surface thermal load. The allowed surface thermal load and surface reflectivity give the maximum beam energy density and the minimum size for each mirror. For mirrors made of aluminum alloy 7475 and initially operated at room temperature, the resulting optical damage threshold and allowable temperature rise give a required mirror size for each final mirror. Critical issues relevant to the integrity and lifetime of such mirrors in a reactor environment are briefly discussed.

  2. Application of grazing incidence x-ray fluorescence technique to discriminate and quantify implanted solar wind

    SciTech Connect

    Kitts, K.; Choi, Y.; Eng, P. J.; Ghose, S. K.; Sutton, S. R.; Rout, B.

    2009-03-15

    NASA launched the Genesis return mission to obtain pristine solar wind samples in order to better understand solar wind mechanics, solar physics, and solar system evolution. Unfortunately, the probe crash-landed shattering the collector plates necessitating the application of a grazing incidence x-ray fluorescence technique. This nondestructive methodology differentiates the terrestrial contamination from the low concentration implanted solar wind. Using this technique, the elemental depth distribution is obtained resulting in the determination of absolute solar wind elemental abundance. We describe this application and present the solar wind Fe concentration determination as an example.

  3. Mounting for Fabrication, Metrology, and Assembly of Full Shell Grazing Incidence Optics

    NASA Technical Reports Server (NTRS)

    Roche, Jacqueline M.; Gubarev, Mikhail V.; O'Dell, Stephen L.; Kolodziejczak, Jeffery; Weisskopf, Martin C.; Ramsey, Brian D.; Elsner, Ronald F.

    2014-01-01

    Future x-ray telescopes will likely require lightweight mirrors to attain the large collecting areas needed to accomplish the science objectives. Understanding and demonstrating processes now is critical to achieving sub-arcsecond performance in the future. Consequently, designs not only of the mirrors but of fixtures for supporting them during fabrication, metrology, handling, assembly, and testing must be adequately modeled and verified. To this end, MSFC is using finite-element modeling to study the effects of mounting on full-shell grazing-incidence mirrors, during all processes leading to flight mirror assemblies. Here we report initial results of this study.

  4. Electron emission induced by resonant coherent ion-surface interaction at grazing incidence

    SciTech Connect

    Garcia de Abajo, F.J. ); Ponce, V.H. ); Echenique, P.M. )

    1992-10-19

    A new spectroscopy based on the resonant coherently induced electron loss to the continuum in ion-surface scattering under grazing incidence is proposed. A series of peaks, corresponding to the energy differences determined by the resonant interaction with the rows of atoms in the surface, is predicted to appear in the energy distribution of electrons emitted from electronic states bound to the probe. Calculations for MeV He{sup +} ions scattered at a W(001) surface along the {l angle}100{r angle} direction with a glancing angle of 0--2 mrad show a total yield close to 1.

  5. SPRED: a multichannel grazing-incidence spectrometer for plasma impurity diagnosis

    SciTech Connect

    Fonck, R.J.; Ramsey, A.T.; Yelle, R.V.

    1982-03-01

    A compact vacuum ultraviolet spectrometer system has been developed to provide time-resolved impurity spectra from tokamak plasmas. Two interchangeable aberration-corrected toroidal diffraction gratings with flat focal fields provide simultaneous coverage over the ranges 100 to 1100 A or 160 to 1700 A. The detector is an intensified self-scanning photodiode array. Spectral resolution is 2 A with the higher dispersion grating. Minimum readout time for a full spectrum is 20 ms, but up to 7 individual spectral lines can be measured with a 1 ms time resolution. The sensitivity of the system is comparable to that of a conventional grazing incidence monochromator.

  6. Grazing-incidence cylindric mirror with multiple reflection for the soft X-ray spectral range

    NASA Astrophysics Data System (ADS)

    Alexandrov, Yu. M.; Fedin, D. A.; Fedorchuk, R. V.; Koshevoi, M. O.; Kozhevnikov, I. V.; Murashova, V. A.; Pisarzyk, T.; Rupasov, A. A.; Shikanov, A. S.; Yakimenko, M. N.; Vinogradov, A. V.

    1991-10-01

    New possibilities of the SR beam control are opened with the use of grazing incidence elements based on the "whispering gallery" effect. Experimental investigations of such an X-ray optical element have been performed on the S-60 synchrotron at the Lebedev Institute. By using the absolute spectral characteristics of the X-ray photofilm RAR 2497 (Kodak) and the SR spectral shape we have determined the output-angle integral spectral coefficient of reflection of the studied mirror. A high value of the reflection coefficient makes it possible to use such an X-ray optical element as the effective reflector for soft X-ray beams.

  7. Grazing-incidence XRF analysis of layered samples: Detailed study of amplitude calculation

    NASA Astrophysics Data System (ADS)

    Miqueles, Eduardo X.; Pérez, Carlos A.; Suárez, Vanessa I.; Vescovi, Rafael F. C.

    2015-09-01

    In this article, we propose a new mathematical approach for the computation of electromagnetic wave amplitudes in grazing incidence X-ray fluorescence (GIXRF)-an analytical method for surface and near-surface layer analysis. The new contribution comes from an applied point of view, in order to have stable and fast algorithms to simulate the fluorescence intensity from a stacking of thin layer films. The calculation of transmitted/reflected amplitudes is an important part of the direct and/or inverse problem. An analysis of the amplitude versus layer thickness is also given.

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

    SciTech Connect

    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. Plane waves at or near grazing incidence in the parabolic approximation. [acoustic equations of motion for sound fields

    NASA Technical Reports Server (NTRS)

    Mcaninch, G. L.; Myers, M. K.

    1980-01-01

    The parabolic approximation for the acoustic equations of motion is applied to the study of the sound field generated by a plane wave at or near grazing incidence to a finite impedance boundary. It is shown how this approximation accounts for effects neglected in the usual plane wave reflection analysis which, at grazing incidence, erroneously predicts complete cancellation of the incident field by the reflected field. Examples are presented which illustrate that the solution obtained by the parabolic approximation contains several of the physical phenomena known to occur in wave propagation near an absorbing boundary.

  10. Performance analysis of grazing incidence imaging systems. [X ray telescope aberrations

    NASA Technical Reports Server (NTRS)

    Winkler, C. E.; Korsch, D.

    1977-01-01

    An exact expression relating the coordinates of a point on the incident ray, a point of reflection from an arbitrary surface, and a point on the reflected ray is derived. The exact relation is then specialized for the case of grazing incidence, and first order and third order systematic analyses are carried out for a single reflective surface and then for a combination of two surfaces. The third order treatment yields a complete set of primary aberrations for single element and two element systems. The importance of a judicious choice for a coordinate system in showing field curvature to clearly be the predominant aberration for a two element system is discussed. The validity of the theory is verified through comparisons with the exact ray trace results for the case of the telescope.

  11. Image defects from surface and alignment errors in grazing incidence telescopes

    NASA Technical Reports Server (NTRS)

    Saha, Timo T.

    1989-01-01

    The rigid body motions and low frequency surface errors of grazing incidence Wolter telescopes are studied. The analysis is based on surface error descriptors proposed by Paul Glenn. In his analysis, the alignment and surface errors are expressed in terms of Legendre-Fourier polynomials. Individual terms in the expression correspond to rigid body motions (decenter and tilt) and low spatial frequency surface errors of mirrors. With the help of the Legendre-Fourier polynomials and the geometry of grazing incidence telescopes, exact and approximated first order equations are derived in this paper for the components of the ray intercepts at the image plane. These equations are then used to calculate the sensitivities of Wolter type I and II telescopes for the rigid body motions and surface deformations. The rms spot diameters calculated from this theory and OSAC ray tracing code agree very well. This theory also provides a tool to predict how rigid body motions and surface errors of the mirrors compensate each other.

  12. The production of low-energy neutral oxygen beams by grazing-incidence neutralization

    NASA Technical Reports Server (NTRS)

    Albridge, R. G.; Haglund, R. F.; Tolk, N. H.; Daech, A. F.

    1987-01-01

    The Vanderbilt University neutral oxygen facility produces beams of low-energy neutral oxygen atoms by means of grazing-incidence collisions between ion beams and metal surfaces. Residual ions are reflected by applied electric fields. This method can utilize initial ion beams of either O(+) or O2(+) since a very large percentage of molecular oxygen ions are dissociated when they undergo grazing-incidence neutralization. The method of neutralization is applicable to low-energy beams and to all ions. Particular emphasis is on O and N2 beams for simulation of the low Earth orbit space environment. Since the beam is a pure O-neutral beam and since measurements of the interaction of the beam with solid surfaces are made spectroscopically, absolute reaction rates can be determined. The technique permits the beams to be used in conjunction with electron and photon irradiation for studies of synergistic effects. Comparisons of optical spectra of Kapton excited by 2.5-keV O, O(+), and O2(+) show significant differences. Optical spectra of Kapton excited by neutral oxygen beams of less than 1 keV have been recorded.

  13. Grazing-incidence spectrometer for soft X-ray solar imaging spectroscopy.

    PubMed

    Frassetto, Fabio; Coraggia, Stefano; Miotti, Paolo; Poletto, Luca

    2013-07-29

    The design and realization of a stigmatic grazing-incidence instrument for space applications to solar imaging spectroscopy is presented. We propose an optical layout in which imaging and spectral capabilities are decoupled by the use of crossed cylindrical mirrors. The design consists of a double telescope and a spectrograph: telescope I consists of a single cylindrical mirror with parabolic section, focusing the radiation on the entrance slit of the spectrograph in the spectral dispersion plane; telescope II consists of two cylindrical mirrors with aspherical section in Wolter configuration focusing the radiation on the spectrograph focal plane in the direction perpendicular to the spectral dispersion plane; the spectrograph consists of a grazing-incidence spherical variable-line-spaced grating with flat-field properties. Telescope II is crossed with respect to the grating and telescope I, i.e., is mounted with its tangential planes coincident with the grating equatorial plane, to decouple spectral and spatial focusing properties. The spectral resolution is preserved also for off-axis angles. The instrument that has been realized operates in the 4-26 nm spectral range and has a field of view of 0.5 deg to image the full Sun disk.

  14. Kinetic simulations of the Chodura and Debye sheaths for magnetic fields with grazing incidence

    NASA Astrophysics Data System (ADS)

    Coulette, David; Manfredi, Giovanni

    2016-02-01

    When an unmagnetized plasma comes in contact with a material surface, the difference in mobility between the electrons and the ions creates a non-neutral layer known as the Debye sheath (DS). However, in magnetic fusion devices, the open magnetic field lines intersect the structural elements of the device with near grazing incidence angles. The magnetic field tends to align the particle flow along its own field lines, thus counteracting the mechanism that leads to the formation of the DS. Recent work using a fluid model (Stangeby 2012 Nucl. Fusion 52 083012) showed that the DS disappears when the incidence angle is smaller than a critical value (around {{5}{^\\circ}} for ITER-like parameters). Here, we study this transition by means of numerical simulations of a kinetic model both in the collisionless and weakly collisional regimes. We show that the main features observed in the fluid model are preserved: for grazing incidence, the space charge density near the wall is reduced or suppressed, the ion flow velocity is subsonic, and the electric field and plasma density profiles are spread out over several ion Larmor radii instead of a few Debye lengths as in the unmagnetized case. As there is no singularity at the DS entrance in the kinetic model, this phenomenon depends smoothly on the magnetic field incidence angle and no particular critical angle arises. The simulation results and the predictions of the fluid model are in good agreement, although some discrepancies subsist, mainly due to the assumptions of isothermal closure and diagonality of the pressure tensor in the fluid model.

  15. Applicability of a cut-off reflector for grazing incidence X-ray fluorescence analysis

    NASA Astrophysics Data System (ADS)

    Tiwari, M. K.; Sawhney, K. J. S.

    2003-11-01

    The applicability of a cut-off reflector, instead of the commonly used multilayer reflector, for grazing incidence X-ray fluorescence (GI-XRF) analysis is demonstrated. Owing to the precise angular adjustment possible in the total reflection X-ray fluorescence (TXRF) spectrometer developed in house, it is possible to adjust the cut-off reflector so as to pass all X-ray energies up to Cu-K α, eliminating Cu-K β and higher X-ray energies emitted from a Cu target X-ray generator. The advantage of this technique is that one gets a higher flux of Cu-K α radiation (>98%) compared to 80-90% from a good quality multilayer optics. Moreover, the same cut-off reflector, used at different grazing angles, serves the purpose for different primary beam energies. The suitability of such an arrangement for GI-XRF analysis for surface characterization has been demonstrated by analyzing a 50 ng aqueous residue of Fe on top of a float glass substrate. The GI-XRF results thus obtained are compared with those obtained using a multilayer monochromator in the primary beam as well as with theoretical calculations.

  16. Differential Deposition for Surface Figure Corrections in Grazing Incidence X-Ray Optics

    NASA Technical Reports Server (NTRS)

    Ramsey, Brian D.; Kilaru, Kiranmayee; Atkins, Carolyn; Gubarev, Mikhail V.; Broadway, David M.

    2015-01-01

    Differential deposition corrects the low- and mid- spatial-frequency deviations in the axial figure of Wolter-type grazing incidence X-ray optics. Figure deviations is one of the major contributors to the achievable angular resolution. Minimizing figure errors can significantly improve the imaging quality of X-ray optics. Material of varying thickness is selectively deposited, using DC magnetron sputtering, along the length of optic to minimize figure deviations. Custom vacuum chambers are built that can incorporate full-shell and segmented Xray optics. Metrology data of preliminary corrections on a single meridian of full-shell x-ray optics show an improvement of mid-spatial frequencies from 6.7 to 1.8 arc secs HPD. Efforts are in progress to correct a full-shell and segmented optics and to verify angular-resolution improvement with X-ray testing.

  17. Aberrations of varied line-space grazing incidence gratings in converging light beams

    NASA Technical Reports Server (NTRS)

    Hettrick, M. C.

    1984-01-01

    Analyses of the imaging properties of several designs for varied-line space gratings in converging beams of light in grazing-incidence spectrometers are presented. An explicit model is defined for the case of a plane-reflection grating intercepting light that converges and is reflected to a stigmatic point associated with the zero-order image of the grating. Smooth spatial variation of the grating constant then permits aberration correction. The aberrations are expressed as polynomials in the grating lens coordinates using power series expansions. Application of the model is illustrated in terms of aberrations experienced with the short wavelength spectrometer on the EUVE satellite. Attention is given to straight and parallel in-plane grooves, curved groove in-plane designs and off-plane grooves. Aberrations due to dispersions and misalignment are also considered.

  18. Mirror and grating surface figure requirements for grazing incidence synchrotron radiation beamlines: Power loading effects

    SciTech Connect

    Hulbert, S.L.; Sharma, S.

    1987-01-01

    At present, grazing incidence mirrors are used almost exclusively as the first optical element in VUV and soft x-ray synchrotron radiation beamlines. The performance of these mirrors is determined by thermal and mechanical stress-induced figure errors as well as by figure errors remaining from the grinding and polishing process. With the advent of VUV and soft x-ray undulators and wigglers has come a new set of thermal stress problems related to both the magnitude and the spatial distribution of power from these devices. In many cases the power load on the entrance slits and gratings in these beamlines is no longer negligible. The dependence of thermally-induced front-end mirror figure errors on various storage ring and insertion device parameters (especially those at the National Synchrotron Light Source) and the effects of these figure errors on two classes of soft x-ray beamlines are presented.

  19. Mirror and grating surface figure requirements for grazing incidence synchrotron radiation beamlines: Power loading effects

    SciTech Connect

    Hulbert, S.L.; Sharma, S.

    1987-10-21

    At present, grazing incidence mirrors are used almost exclusively as the first optical element in VUV and soft x-ray synchrotron radiation beam lines. The performance of these mirrors is determined by thermal and mechanical stress-induced figure errors as well as by figure errors remaining from the grinding and polishing process. With the advent of VUV and soft x-ray undulators and wigglers has come a new set of thermal stress problems related to both the magnitude and the spatial distribution of power from these devices. In many cases the power load on the entrance slits and gratings in these beamlines is no longer negligible. The dependence of thermally-induced front-end mirror figure errors on various storage ring and insertion device parameters (especially those at the NSLS) and the effects of these figure errors on a class of soft x-ray beam lines are presented. 17 refs., 5 figs., 2 tabs.

  20. Design of grazing-incidence multilayer supermirrors for hard-x-ray reflectors.

    PubMed

    Joensen, K D; Voutov, P; Szentgyorgyi, A; Roll, J; Gorenstein, P; Høghøj, P; Christensen, F E

    1995-12-01

    Extremely broadband grazing-incidence multilayers for hard-x-ray reflection can be obtained by a gradual change of the layer thicknesses down through the structure. Existing approaches for designing similar neutron optics, called supermirrors, are shown to provide respectable performance when applied to x-ray multilayers. However, none of these approaches consider the effects of imperfect layer interfaces and absorption in the overlying layers. Adaptations of neutron designs that take these effects into account are presented, and a thorough analysis of two specific applications (a single hard-x-ray reflector and a hard-x-ray telescope) shows that an improved performance can be obtained. A multilayer whose bilayer thicknesses are given by a power law expression is found to provide the best solution; however, it is only slightly better than some of the adapted neutron designs.

  1. Development of differential deposition technique for figure corrections in grazing incidence x-ray optics

    NASA Astrophysics Data System (ADS)

    Kilaru, Kiranmayee; Ramsey, Brian D.; Gubarev, Mikhail V.

    2009-08-01

    A differential deposition technique is being developed to correct the low- and mid-spatial-frequency deviations in the axial figure profile of Wolter-type grazing-incidence X-ray optics. These deviations arise due to various factors in the fabrication process and they degrade the performance of optics by limiting the achievable angular resolution. In the differential deposition technique, material is selectively deposited in varying thickness along the length of the optic to minimize these deviations, thereby improving the overall figure. The process is being tested on focusing X-ray optics being developed at MSFC for small-animal radionuclide imaging. The required spatial resolution for these optics is 100 μm (30 arc secs), which can be achieved with the electroformnickel- replication fabrication technique regularly employed at MSFC. However, by improving the figure quality of the optics through differential deposition, we aim to significantly improve the resolution beyond this value.

  2. High-frequency backscatter from a finned cylinder at grazing incidence - Comparison of two theoretical methods

    NASA Astrophysics Data System (ADS)

    Michaeli, A.

    1986-02-01

    A closed-form, high-frequency approximation is obtained for the diffracted-reflected-diffracted field contribution to the backscattered field resulting from the grazing illumination of a perfectly conducting, infinitely long, finned cylinder by a normally incident cylindrical transverse magnetic (TM) wave. The result, which is valid for any relative magnitudes of the cylinder radius and the fin width provided both of them are electrically large, is derived by two different methods. One of them is the radiation integral method related to the physical theory of diffraction. The other is the complex ray tracing method related to the spectral theory of diffraction (STD). Relative merits and disadvantages of the two methods are pointed out.

  3. Differential Deposition Technique for Figure Corrections in Grazing Incidence X-ray Optics

    NASA Technical Reports Server (NTRS)

    Kilaru, Kiranmayee; Ramsey, Brian D.; Gubarev, Mikhail

    2009-01-01

    A differential deposition technique is being developed to correct the low- and mid-spatial-frequency deviations in the axial figure profile of Wolter type grazing incidence X-ray optics. These deviations arise due to various factors in the fabrication process and they degrade the performance of the optics by limiting the achievable angular resolution. In the differential deposition technique, material of varying thickness is selectively deposited along the length of the optic to minimize these deviations, thereby improving the overall figure. High resolution focusing optics being developed at MSFC for small animal radionuclide imaging are being coated to test the differential deposition technique. The required spatial resolution for these optics is 100 m. This base resolution is achievable with the regular electroform-nickel-replication fabrication technique used at MSFC. However, by improving the figure quality of the optics through differential deposition, we aim at significantly improving the resolution beyond this value.

  4. Grazing incidence X-ray absorption characterization of amorphous Zn-Sn-O thin film

    NASA Astrophysics Data System (ADS)

    Moffitt, S. L.; Ma, Q.; Buchholz, D. B.; Chang, R. P. H.; Bedzyk, M. J.; Mason, T. O.

    2016-05-01

    We report a surface structure study of an amorphous Zn-Sn-O (a-ZTO) transparent conducting film using the grazing incidence X-ray absorption spectroscopy technique. By setting the measuring angles far below the critical angle at which the total external reflection occurs, the details of the surface structure of a film or bulk can be successfully accessed. The results show that unlike in the film where Zn is severely under coordinated (N < 4), it is fully coordinated (N = 4) near the surface while the coordination number around Sn is slightly smaller near the surface than in the film. Despite a 30% Zn doping, the local structure in the film is rutile-like.

  5. Grazing-incidence X-ray diffraction study of rubrene epitaxial thin films.

    PubMed

    Fumagalli, Enrico; Campione, Marcello; Raimondo, Luisa; Sassella, Adele; Moret, Massimo; Barba, Luisa; Arrighetti, Gianmichele

    2012-09-01

    The growth of organic semiconductors as thin films with good and controlled electrical performances is nowadays one of the main tasks in the field of organic semiconductor-based electronic devices. In particular it is often required to grow highly crystalline and precisely oriented thin films. Here, thanks to grazing-incidence X-ray diffraction measurements carried out at the ELETTRA synchrotron facility, it is shown that rubrene thin films deposited by organic molecular beam epitaxy on the surface of tetracene single crystals have the structure of the known orthorhombic polymorph, with the (2 0 0) plane parallel to the substrate surface. Moreover, the exact epitaxial relationship between the film and the substrate crystalline structures is determined, demonstrating the presence of a unique in-plane orientation of the overlayer. PMID:22898945

  6. Adaptive grazing incidence optics for the next generation of x-ray observatories

    NASA Astrophysics Data System (ADS)

    Lillie, C.; Pearson, D.; Plinta, A.; Metro, B.; Lintz, E.; Shropshire, D.; Danner, R.

    2010-09-01

    Advances in X-ray astronomy require high spatial resolution and large collecting area. Unfortunately, X-ray telescopes with grazing incidence mirrors require hundreds of concentric mirror pairs to obtain the necessary collecting area, and these mirrors must be thin shells packed tightly together... They must also be light enough to be placed in orbit with existing launch vehicles, and able to be fabricated by the thousands for an affordable cost. The current state of the art in X-ray observatories is represented by NASA's Chandra X-ray observatory with 0.5 arc-second resolution, but only 400 cm2 of collecting area, and by ESA's XMM-Newton observatory with 4,300 cm2 of collecting area but only 15 arc-second resolution. The joint NASA/ESA/JAXA International X-ray Observatory (IXO), with {15,000 cm2 of collecting area and 5 arc-second resolution which is currently in the early study phase, is pushing the limits of passive mirror technology. The Generation-X mission is one of the Advanced Strategic Mission Concepts that NASA is considering for development in the post-2020 period. As currently conceived, Gen-X would be a follow-on to IXO with a collecting area >= 50 m2, a 60-m focal length and 0.1 arc-second spatial resolution. Gen-X would be launched in {2030 with a heavy lift Launch Vehicle to an L2 orbit. Active figure control will be necessary to meet the challenging requirements of the Gen-X optics. In this paper we present our adaptive grazing incidence mirror design and the results from laboratory tests of a prototype mirror.

  7. The Marshall Grazing Incidence X-ray Spectrometer (MaGIXS)

    NASA Astrophysics Data System (ADS)

    Champey, P. R.; Winebarger, A. R.; Kobayashi, K.; Savage, S. L.; Cirtain, J. W.; Cheimets, P.; Hertz, E.; Golub, L.; Ramsey, B.; McCracken, J.; Heilmann, R.; Schattenburg, M.; Bruccoleri, A.

    2015-12-01

    The Marshall Grazing Incidence X-ray Spectrometer (MaGIXS) is a NASA soundingrocket instrument designed to observe soft X-ray emissions at 0.5 - 2.0 keV energies in thesolar atmosphere. The primary science goal is to differentiate steady, low-frequency heatingevents from sporadic, high-frequency heating events in the active region core For the first time, high-temperature, low-emission plasma will be observed directly with 5 arcsec spatialand 22 mÅ spectral resolution. The novel optical design consists of a Wolter I telescope anda 3-optic grazing-incidence spectrograph. The X-ray spectrograph utilizes a finite conjugatemirror pair and a planar, nanoprinted-silicon varied line space grating, which is being devel-oped by the Massachusetts Institute of Technology (MIT). The telescope and spectrographmirrors will be nickel replicated and coated with iridium. Mandrel fabrication and nickelreplication will be done at MSFC as part of its replicated X-ray optics program. Mounting,alignment, and integration of the ight optics will be performed at the Harvard-SmithsonianCenter for Astrophysics (SAO). The MaGIXS science camera is being developed at MSFCand is based on CLASP heritage, which obtained read noise performance of 5.5 e?- RMS. Thecamera will include a e2v Technologies 2kx2k frame transfer CCD with 4-channel readout(500 kpixel/s/channel). We will present an overview of the MaGIXS optical system andfabrication of the telescope and spectrograph mirrors.

  8. Fractal Approach in Petrology: Combining Ultra-Small Angle (USANA) and Small Angle Neutron Scattering (SANS)

    SciTech Connect

    LoCelso, F.; Triolo, F.; Triolo, A.; Lin, J.S.; Lucido, G.; Triolo, R.

    1999-10-14

    Ultra small angle neutron scattering instruments have recently covered the gap between the size resolution available with conventional intermediate angle neutron scattering and small angle neutron scattering instruments on one side and optical microscopy on the other side. Rocks showing fractal behavior in over two decades of momentum transfer and seven orders of magnitude of intensity are examined and fractal parameters are extracted from the combined USANS and SANS curves.

  9. Grazing-incidence monochromator for the 15--800 A wavelength range at the storage ring VEPP-2M

    SciTech Connect

    Gluskin, E. S.; Kuzminykh, V. S.; Trakhtenberg, E. M.; Koscheev, S. V.; Devyatov, V. G.; Cherkashin, A. E.; Blau, W.; Meisel, A.; Ehrhardt, H.

    1989-07-01

    A new Rowland monochromator with a fixed output slit, which operates according to the grazing-incidence scheme, is described. The device is notable for the capability to change the Rowland radius within 1--3 m. The monochromator was tested using synchrotron radiation from the storage ring VEPP-2M.

  10. Electron emission induced by resonant coherent interaction in ion-surface scattering at grazing incidence

    SciTech Connect

    Garcia de Abajo, F.J. ); Ponce, V.H.; Echenique, P.M. )

    1994-01-15

    The resonant coherent interaction of an ion with an oriented crystal surface, under grazing-incidence conditions with respect to a special direction of the crystal, gives rise to electron loss to the continuum from electronic bound states of the ion. The calculations presented below predict large probabilities for electron emission due to this mechanism. The electrons are emitted with well defined energies, expressed in terms of the condition of resonance. Furthermore, the emission takes place around certain preferential directions, which are determined by both the latter condition and the symmetry of the surface lattice. Our calculations for MeV He[sup +] ions scattered at a W(001) surface along the [l angle]100[r angle] direction with glancing angle of 0--2 mrad indicate a yield of emission close to 1. Using heavier projectiles, one obtains smaller yields, but still large enough to be measurable in some cases (e.g., [approx]0.9 for 53 MeV B[sup 4+] and an angle of incidence of 1 mrad). Besides, the initial bound state is energy shifted due to the interaction with both the crystal potential and the velocity-dependent image potential. This results in a slight shift of the peaks of emission, which suggests a possible spectroscopy for analyzing the dynamical interaction of electronic bound states with solid surfaces.

  11. Dynamic grazing incidence fast atom diffraction during molecular beam epitaxial growth of GaAs

    SciTech Connect

    Atkinson, P. Eddrief, M.; Etgens, V. H.; Khemliche, H. Debiossac, M.; Mulier, M.; Lalmi, B.; Roncin, P.; Momeni, A.

    2014-07-14

    A Grazing Incidence Fast Atom Diffraction (GIFAD) system has been mounted on a commercial molecular beam epitaxy chamber and used to monitor GaAs growth in real-time. In contrast to the conventionally used Reflection High Energy Electron Diffraction, all the GIFAD diffraction orders oscillate in phase, with the change in intensity related to diffuse scattering at step edges. We show that the scattered intensity integrated over the Laue circle is a robust method to monitor the periodic change in surface roughness during layer-by-layer growth, with oscillation phase and amplitude independent of incidence angle and crystal orientation. When there is a change in surface reconstruction at the start of growth, GIFAD intensity oscillations show that there is a corresponding delay in the onset of layer-by-layer growth. In addition, changes in the relative intensity of different diffraction orders have been observed during growth showing that GIFAD has the potential to provide insight into the preferential adatom attachment sites on the surface reconstruction during growth.

  12. Impedance Scaling for Small Angle Transitions

    SciTech Connect

    Stupakov, G.; Bane, Karl; Zagorodnov, I.; /DESY

    2010-10-27

    Based on the parabolic equation approach to Maxwell's equations we have derived scaling properties of the high frequency impedance/short bunch wakefields of structures. For the special case of small angle transitions we have shown the scaling properties are valid for all frequencies. Using these scaling properties one can greatly reduce the calculation time of the wakefield/impedance of long, small angle, beam pipe transitions, like one often finds in insertion regions of storage rings. We have tested the scaling with wakefield simulations of 2D and 3D models of such transitions, and found that the scaling works well. In modern ring-based light sources one often finds insertion devices having extremely small vertical apertures (on the order of millimeters) to allow for maximal undulator fields reaching the beam. Such insertion devices require that there be beam pipe transitions from these small apertures to the larger cross-sections (normally on the order of centimeters) found in the rest of the ring. The fact that there may be many such transitions, and that these transitions introduce beam pipe discontinuities very close to the beam path, means that their impedance will be large and, in fact, may dominate the impedance budget of the entire ring. To reduce their impact on impedance, the transitions are normally tapered gradually over a long distance. The accurate calculation of the impedance or wakefield of these long transitions, which are typically 3D objects (i.e. they do not have cylindrical symmetry), can be quite a challenging numerical task. In this report we present a method of obtaining the impedance of a long, small angle transition from the calculation of a scaled, shorter one. Normally, the actual calculation is obtained from a time domain simulation of the wakefield in the structure, where the impedance can be obtained by performing a Fourier transform. We shall see that the scaled calculation reduces the computer time and memory requirements

  13. One-dimensional ion-beam figuring for grazing-incidence reflective optics.

    PubMed

    Zhou, Lin; Idir, Mourad; Bouet, Nathalie; Kaznatcheev, Konstantine; Huang, Lei; Vescovi, Matthew; Dai, Yifan; Li, Shengyi

    2016-01-01

    One-dimensional ion-beam figuring (1D-IBF) can improve grazing-incidence reflective optics, such as Kirkpatrick-Baez mirrors. 1D-IBF requires only one motion degree of freedom, which reduces equipment complexity, resulting in compact and low-cost IBF instrumentation. Furthermore, 1D-IBF is easy to integrate into a single vacuum system with other fabrication processes, such as a thin-film deposition. The NSLS-II Optical Metrology and Fabrication Group has recently integrated the 1D-IBF function into an existing thin-film deposition system by adding an RF ion source to the system. Using a rectangular grid, a 1D removal function needed to perform 1D-IBF has been produced. In this paper, demonstration experiments of the 1D-IBF process are presented on one spherical and two plane samples. The final residual errors on both plane samples are less than 1 nm r.m.s. The surface error on the spherical sample has been successfully reduced by a factor of 12. The results show that the 1D-IBF method is an effective method to process high-precision 1D synchrotron optics.

  14. Development Status of Adjustable Grazing Incidence Optics for 0.5 Arcsecond X-Ray Imaging

    NASA Technical Reports Server (NTRS)

    Reid, Paul B.; Aldcroft, Thomas L.; Allured, Ryan; Cotroneo, Vincenzo; Johnson-Wilke, Raegan L.; Marquez, Vanessa; McMuldroch, Stuart; O'Dell, Stephen L.; Ramsey, Brian D.; Schwartz, Daniel A.; Trolier-McKinstry, Susan; Vikhlinin, Alexey; Wilke, Rudeger H. T.; Zhao, Rui

    2014-01-01

    We describe progress in the development of adjustable grazing incidence X-ray optics for 0.5 arcsec resolution cosmic X-ray imaging. To date, no optics technology is available to blend high resolution imaging like the Chandra X-ray Observatory, with square meter collecting area. Our approach to achieve these goals simultaneously is to directly deposit thin film piezoelectric actuators on the back surface of thin, lightweight Wolter-I or Wolter- Schwarschild mirror segments. The actuators are used to correct mirror figure errors due to fabrication, mounting and alignment, using calibration and a one-time figure adjustment on the ground. If necessary, it will also be possible to correct for residual gravity release and thermal effects on-orbit. In this paper we discuss our most recent results measuring influence functions of the piezoelectric actuators using a Shack-Hartmann wavefront sensor. We describe accelerated and real-time lifetime testing of the piezoelectric material, and we also discuss changes to, and recent results of, our simulations of mirror correction.

  15. New figuring model based on surface slope profile for grazing-incidence reflective optics.

    PubMed

    Zhou, Lin; Huang, Lei; Bouet, Nathalie; Kaznatcheev, Konstantine; Vescovi, Matthew; Dai, Yifan; Li, Shengyi; Idir, Mourad

    2016-09-01

    Surface slope profile is widely used in the metrology of grazing-incidence reflective optics instead of surface height profile. Nevertheless, the theoretical and experimental model currently used in deterministic optical figuring processes is based on surface height, not on surface slope. This means that the raw slope profile data from metrology need to be converted to height profile to perform the current height-based figuring processes. The inevitable measurement noise in the raw slope data will introduce significant cumulative error in the resultant height profiles. As a consequence, this conversion will degrade the determinism of the figuring processes, and will have an impact on the ultimate surface figuring results. To overcome this problem, an innovative figuring model is proposed, which directly uses the raw slope profile data instead of the usual height data as input for the deterministic process. In this paper, first the influence of the measurement noise on the resultant height profile is analyzed, and then a new model is presented; finally a demonstration experiment is carried out using a one-dimensional ion beam figuring process to demonstrate the validity of our approach. PMID:27577760

  16. Technology development of adjustable grazing incidence x-ray optics for sub-arc second imaging

    NASA Astrophysics Data System (ADS)

    Reid, P. B.; Aldcroft, T. L.; Cotroneo, V.; Davis, W.; Johnson-Wilke, R. L.; McMuldroch, S.; Ramsey, B. D.; Schwartz, D. A.; Trolier-McKinstry, S.; Vikhlinin, A.; Wilke, R. H. T.

    2012-09-01

    We report on technical progress made over the past year developing thin film piezoelectric adjustable grazing incidence optics. We believe such mirror technology represents a solution to the problem of developing lightweight, sub-arc second imaging resolution X-ray optics. Such optics will be critical to the development next decade of astronomical X-ray observatories such as SMART-X, the Square Meter Arc Second Resolution X-ray Telescope. SMART-X is the logical heir to Chandra, with 30 times the collecting area and Chandra-like imaging resolution, and will greatly expand the discovery space opened by Chandra’s exquisite imaging resolution. In this paper we discuss deposition of thin film piezoelectric material on flat glass mirrors. For the first time, we measured the local figure change produced by energizing a piezo cell - the influence function, and showed it is in good agreement with finite element modeled predictions. We determined that at least one mirror substrate material is suitably resistant to piezoelectric deposition processing temperatures, meaning the amplitude of the deformations introduced is significantly smaller than the adjuster correction dynamic range. Also, using modeled influence functions and IXO-based mirror figure errors, the residual figure error was predicted post-correction. The impact of the residual figure error on imaging performance, including any mid-frequency ripple introduced by the corrections, was modeled. These, and other, results are discussed, as well as future technology development plans.

  17. Trapping and desorption of energetic Cu atoms on Cu(111) and (001) surfaces at grazing incidence

    SciTech Connect

    Hanson, D.E.; Kress, J.D.; Voter, A.F.; Liu, X.

    1999-10-01

    Molecular-dynamics (MD) simulations of Cu atoms impacting both Cu(111) and (001) surfaces at grazing incidence have been performed to study trapping (or surface skipping), desorption, and energy dissipation. An energetic Cu atom (10{le}E{le}100thinspeV) can become trapped by the mean attractive potential above the surface, oscillating normal to the surface. While in this trapped state, it can traverse hundreds of {Angstrom} as it dissipates energy to the surface. Until the atom either desorbs or comes to rest, it experiences an energy loss, that is piecewise linear in time, typically comprised of two or more linear regions. In each region, the energy loss rate, dE/dt, is approximately constant. The process can be characterized by two parameters: the desorption probability at each oscillation and an average energy loss rate (per oscillation) that is independent of energy. These parameter values are the same for both the (111) and (001) surfaces. A phenomenological model based on these parameters is presented, and the predictions of sticking probability, average energy transfer to the surface, and total distance traveled, agree with full MD simulations. The dependence of the desorption probability on the surface temperature was also studied. {copyright} {ital 1999} {ital The American Physical Society}

  18. Grazing incidence X-ray reflectivity - Studies for the AXAF observatory

    NASA Technical Reports Server (NTRS)

    Slane, P.; Schwartz, D.; Van Speybroeck, L.; Jones, D.; Chappell, J.; Bilbro, J.; Shapiro, A.; Dave, S.; Kidd, P.; Texter, S.

    1992-01-01

    The energy bandwidth and total throughput of a grazing incidence optics system is a strong function of the X-ray reflectivity of the surface coating. In support of the Advanced X-ray Astrophysics Facility (AXAF), studies are underway to evaluate and characterize the reflectivity of potential AXAF coatings. Here we report on results obtained for Au, Ir, and Ni coatings produced by electron-beam evaporation, evaporation with ion-assist, and sputtering. Effects of coating thickness and deposition angle have been evaluated at 6.4 and 8.1 keV; the highest reflectivities are those of the thinner, about 200 A vs about 700 A, coatings. While considerable variations exist, the best Ir samples have higher reflectivity than any of the Au coatings. Data results have been compared with models for theoretical reflectivity, particularly with regard to the effective density of the coatings. Independent measurements of the coating densities have been carried out for comparison with the reflectivity results.

  19. Analysis of buried interfaces in multilayer mirrors using grazing incidence extreme ultraviolet reflectometry near resonance edges.

    PubMed

    Sertsu, M G; Nardello, M; Giglia, A; Corso, A J; Maurizio, C; Juschkin, L; Nicolosi, P

    2015-12-10

    Accurate measurements of optical properties of multilayer (ML) mirrors and chemical compositions of interdiffusion layers are particularly challenging to date. In this work, an innovative and nondestructive experimental characterization method for multilayers is discussed. The method is based on extreme ultraviolet (EUV) reflectivity measurements performed on a wide grazing incidence angular range at an energy near the absorption resonance edge of low-Z elements in the ML components. This experimental method combined with the underlying physical phenomenon of abrupt changes of optical constants near EUV resonance edges enables us to characterize optical and structural properties of multilayers with high sensitivity. A major advantage of the method is to perform detailed quantitative analysis of buried interfaces of multilayer structures in a nondestructive and nonimaging setup. Coatings of Si/Mo multilayers on a Si substrate with period d=16.4  nm, number of bilayers N=25, and different capping structures are investigated. Stoichiometric compositions of Si-on-Mo and Mo-on-Si interface diffusion layers are derived. Effects of surface oxidation reactions and carbon contaminations on the optical constants of capping layers and the impact of neighboring atoms' interactions on optical responses of Si and Mo layers are discussed. PMID:26836858

  20. Analysis of buried interfaces in multilayer mirrors using grazing incidence extreme ultraviolet reflectometry near resonance edges.

    PubMed

    Sertsu, M G; Nardello, M; Giglia, A; Corso, A J; Maurizio, C; Juschkin, L; Nicolosi, P

    2015-12-10

    Accurate measurements of optical properties of multilayer (ML) mirrors and chemical compositions of interdiffusion layers are particularly challenging to date. In this work, an innovative and nondestructive experimental characterization method for multilayers is discussed. The method is based on extreme ultraviolet (EUV) reflectivity measurements performed on a wide grazing incidence angular range at an energy near the absorption resonance edge of low-Z elements in the ML components. This experimental method combined with the underlying physical phenomenon of abrupt changes of optical constants near EUV resonance edges enables us to characterize optical and structural properties of multilayers with high sensitivity. A major advantage of the method is to perform detailed quantitative analysis of buried interfaces of multilayer structures in a nondestructive and nonimaging setup. Coatings of Si/Mo multilayers on a Si substrate with period d=16.4  nm, number of bilayers N=25, and different capping structures are investigated. Stoichiometric compositions of Si-on-Mo and Mo-on-Si interface diffusion layers are derived. Effects of surface oxidation reactions and carbon contaminations on the optical constants of capping layers and the impact of neighboring atoms' interactions on optical responses of Si and Mo layers are discussed.

  1. Micro-focusing of attosecond pulses by grazing-incidence toroidal mirrors.

    PubMed

    Poletto, L; Frassetto, F; Calegari, F; Anumula, S; Trabattoni, A; Nisoli, M

    2013-06-01

    The design of optical systems for micro-focusing of extreme-ultraviolet (XUV) attosecond pulses through grazing-incidence toroidal mirrors is presented. Aim of the proposed configuration is to provide a micro-focused image through a high demagnification of the XUV source with the following characteristics: i) almost negligible aberrations; ii) long exit arm to easily accommodate at the output the experimental setups required for the applications of the focused attosecond pulses; iii) possibility to have an intermediate region where the XUV beam is collimated, in order to insert a plane split-mirror for the generation of two XUV pulse replicas to be used in a XUV-pump/XUV-probe setup. We present the analytical and numerical study of two optical configurations characterized by two sections based on the use of toroidal mirrors. The first section provides a demagnified image of the source in an intermediate focus that is free from defocusing but has a large coma aberration. The second section consists of a relay mirror that is mounted in Z-shaped geometry with respect to the previous one, in order to give a stigmatic image with a coma that is opposite to that provided by the first section. An example is provided to demonstrate the capability to achieve spot sizes in the 5-15 μm range with a demagnification higher than 10 in a compact envelope.

  2. New figuring model based on surface slope profile for grazing-incidence reflective optics.

    PubMed

    Zhou, Lin; Huang, Lei; Bouet, Nathalie; Kaznatcheev, Konstantine; Vescovi, Matthew; Dai, Yifan; Li, Shengyi; Idir, Mourad

    2016-09-01

    Surface slope profile is widely used in the metrology of grazing-incidence reflective optics instead of surface height profile. Nevertheless, the theoretical and experimental model currently used in deterministic optical figuring processes is based on surface height, not on surface slope. This means that the raw slope profile data from metrology need to be converted to height profile to perform the current height-based figuring processes. The inevitable measurement noise in the raw slope data will introduce significant cumulative error in the resultant height profiles. As a consequence, this conversion will degrade the determinism of the figuring processes, and will have an impact on the ultimate surface figuring results. To overcome this problem, an innovative figuring model is proposed, which directly uses the raw slope profile data instead of the usual height data as input for the deterministic process. In this paper, first the influence of the measurement noise on the resultant height profile is analyzed, and then a new model is presented; finally a demonstration experiment is carried out using a one-dimensional ion beam figuring process to demonstrate the validity of our approach.

  3. High repetition rate collisional soft x-ray lasers based on grazing incidence pumping

    SciTech Connect

    Luther, B M; Wang, Y; Larotonda, M A; Alessi, D; Berrill, M; Rocca, J J; Dunn, J; Keenan, R; Shlyaptsev, V N

    2005-11-18

    We discuss the demonstration of gain-saturated high repetition rate table-top soft x-ray lasers producing microwatt average powers at wavelengths ranging from 13.9 to 33 nm. The results were obtained heating a pre-created plasma with a picosecond optical laser pulse impinging at grazing incidence onto a pre-created plasma. This pumping geometry increases the energy deposition efficiency of the pump beam into the gain region, making it possible to saturate soft x-ray lasers in this wavelength range with a short pulse pump energy of only 1 J at 800 nm wavelength. Results corresponding to 5 Hz repetition rate operation of gain-saturated 14.7 nm Ni-like Pd and 32.6 nm line Ne-like Ti lasers pumped by a table-top Ti:sapphire laser are reported. We also discuss results obtained using a 1 {omega} 1054 nm pre-pulse and 2{omega} 527 nm short pulse from a Nd:glass pump laser. This work demonstrates the feasibility of producing compact high average power soft x-ray lasers for applications.

  4. Finite element analyses of thin film active grazing incidence x-ray optics

    NASA Astrophysics Data System (ADS)

    Davis, William N.; Reid, Paul B.; Schwartz, Daniel A.

    2010-09-01

    The Chandra X-ray Observatory, with its sub-arc second resolution, has revolutionized X-ray astronomy by revealing an extremely complex X-ray sky and demonstrating the power of the X-ray window in exploring fundamental astrophysical problems. Larger area telescopes of still higher angular resolution promise further advances. We are engaged in the development of a mission concept, Generation-X, a 0.1 arc second resolution x-ray telescope with tens of square meters of collecting area, 500 times that of Chandra. To achieve these two requirements of imaging and area, we are developing a grazing incidence telescope comprised of many mirror segments. Each segment is an adjustable mirror that is a section of a paraboloid or hyperboloid, aligned and figure corrected in situ on-orbit. To that end, finite element analyses of thin glass mirrors are performed to determine influence functions for each actuator on the mirrors, in order to develop algorithms for correction of mirror deformations. The effects of several mirror mounting schemes are also studied. The finite element analysis results, combined with measurements made on prototype mirrors, will be used to further refine the correction algorithms.

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

    SciTech Connect

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

    2015-05-15

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

  6. Development of grazing incidence devices for space-borne time of flight mass spectrometry

    NASA Astrophysics Data System (ADS)

    Cadu, A.; Devoto, P.; Louarn, P.; Sauvaud, J.-A.

    2012-04-01

    Time of flight mass spectrometer is widely used to study space plasmas in planetary and solar missions. This space-borne instrument selects ions in function of their energy through an electrostatic analyzer. Particles are then post-accelerated to energies in the range of 20 keV to cross a carbon foil. At the foil exit, electrons are emitted and separated from ion beam in the time of flight section. A first detector (a Micro-Channel Plate or MCP) emits a start signal at electron arrival and a second one emits a stop signal at incident ion end of path. The time difference gives the speed of the particle and its mass can be calculated, knowing its initial energy. However, current instruments suffer from strong limitations. The post acceleration needs very high voltage power supplies which are heavy, have a high power consumption and imply technical constraints for the development. A typical instrument weighs from 5 to 6 kg, includes a 20 kV power supply, consumes a least 5 W and encounters corona effect and electrical breakdown problems. Moreover, despite the particle high energy range, scattering and straggling phenomena in the carbon foil significantly reduce the instrument overall resolution. Some methods, such as electrostatic focus lenses or reflectrons, really improve mass separation but global system efficiency remains very low because of the charge state dependence of such devices. The main purpose of our work is to replace carbon foil by grazing incidence MCP's - also known as MPO's, for Micro Pore Optics - for electron emission. Thus, incident particles would back-scatter onto the channel inner surface with an angle of a few degrees. With this solution, we can decrease dispersion sources and lower the power supplies to post accelerate ions. The result would be a lighter and simpler instrument with a substantial resolution improvement. We have first simulated MPO's behavior with TRIM and MARLOWE Monte-Carlo codes. Energy scattering and output angle computed

  7. Adjustable Grazing Incidence X-ray Optics with 0.5 Arc Second Resolution

    NASA Astrophysics Data System (ADS)

    Reid, Paul

    We seek to develop adjustable grazing incidence optics for x-ray astronomy. The goal of this development is thin, lightweight mirrors with angular resolution of 0.5 arc seconds, comparable to the Chandra X-ray Observatory. The new mirror design consists of thin segments of a Wolter-I grazing incidence mirror, with piezo-electric material deposited directly on the back surface of the mirror. Depositing a pattern of independently addressable electrodes on top of the piezoelectric material produces an array of independent piezo cells. Energizing a particular cell introduces a localized deformation in the mirror without the need for a reaction structure. By applying the appropriate voltage to the piezo cells, it is possible to correct mirror figure errors that result from mirror fabrication, gravity release, mounting, and thermal effects. Because the thin mirrors segments are lightweight, they can be densely nested to produce collecting area thirty times that of Chandra, on an affordably priced mission. This Supporting Technology program is a follow-on to an existing APRA program. In the existing program we demonstrated the first successful deposition of piezoelectric material on thermally formed glass substrates. We showed that the localized deformations produced by the piezo cells match finite element predictions, and the piezo cell adjustment range meets requirements necessary to achieve the desired figure correction. We have also shown through simulation that representative mirror figure errors can be corrected via modeled influence functions to achieve 0.5 arc sec imaging performance. This provides a firm foundation on which to develop further the technology. We will continue to optimize the deposition of thin piezoelectric films onto thermally formed glass and electroplated metal mirror segments to improve yield and manufacturability. We will deposit piezoelectric material onto conical mirror segments and demonstrate figure correction in agreement with prediction

  8. Small-angle scattering from fat fractals

    NASA Astrophysics Data System (ADS)

    Anitas, Eugen M.

    2014-06-01

    A number of experimental small-angle scattering (SAS) data are characterized by a succession of power-law decays with arbitrarily decreasing values of scattering exponents. To describe such data, here we develop a new theoretical model based on 3D fat fractals (sets with fractal structure, but nonzero volume) and show how one can extract structural information about the underlying fractal structure. We calculate analytically the monodisperse and polydisperse SAS intensity (fractal form factor and structure factor) of a newly introduced model of fat fractals and study its properties in momentum space. The system is a 3D deterministic mass fractal built on an extension of the well-known Cantor fractal. The model allows us to explain a succession of power-law decays and respectively, of generalized power-law decays (GPLD; superposition of maxima and minima on a power-law decay) with arbitrarily decreasing scattering exponents in the range from zero to three. We show that within the model, the present analysis allows us to obtain the edges of all the fractal regions in the momentum space, the number of fractal iteration and the fractal dimensions and scaling factors at each structural level in the fractal. We applied our model to calculate an analytical expression for the radius of gyration of the fractal. The obtained quantities characterizing the fat fractal are correlated to variation of scaling factor with the iteration number.

  9. Test results for an AOA-Xinetics grazing incidence x-ray deformable mirror

    NASA Astrophysics Data System (ADS)

    Lillie, Charles; Egan, Richard; Landers, Franklin; Cavaco, Jeffrey; Ezzo, Kevin; Khounsary, Ali

    2014-09-01

    X-ray telescopes use grazing incidence mirrors to focus X-ray photons from celestial objects. To achieve the large collecting areas required to image faint sources, thousands of thin, doubly curved mirrors are arranged in nested cylindrical shells to approximate a filled aperture. These mirrors require extremely smooth surfaces with precise figures to provide well-focused beams and small image spot sizes. The Generation-X telescope proposed by SAO would have a 12-meter aperture, a 50 m2 collecting area and 0.1 arc-second spatial resolution. This resolution would be obtained by actively controlling the mirror figure with piezoelectric actuators deposited on the back of each 0.4 mm thick mirror segment. To support SAO's Generation-X study, Northrop Grumman used internal funds to look at the feasibility of using Xinetics deformable mirror technologies to meet the Generation-X requirements. We designed and fabricated two 10 x 30 cm Platinum-coated silicon mirrors with 108 surface-parallel electrostrictive Lead Magnesium Niobate (PMN) actuators bonded to the mirror substrates. These mirrors were tested at optical wavelengths by Xinetics to assess the actuator's performance, but no funds were available for X-ray tests. In 2013, after receiving an invitation to evaluate the mirror's performance at Argonne National Laboratory, the mirrors were taken out of storage, refurbished, retested at Xinetics and transported to ANL for metrology measurements with a Long Trace Profilometer, a Fizeau laser interferometer, and X-ray tests. This paper describes the development and testing of the adaptive x-ray mirrors at AOAXinetics. Marathe, et al, will present the results of the tests at Argonne.

  10. X-ray imaging with grazing-incidence microscopes developed for the LIL program

    SciTech Connect

    Rosch, R.; Boutin, J. Y.; Le Breton, J. P.; Gontier, D.; Jadaud, J. P.; Reverdin, C.; Soullie, G.; Lidove, G.; Maroni, R.

    2007-03-15

    This article describes x-ray imaging with grazing-incidence microscopes, developed for the experimental program carried out on the Ligne d'Integration Laser (LIL) facility [J. P. Le Breton et al., Inertial Fusion Sciences and Applications 2001 (Elsevier, Paris, 2002), pp. 856-862] (24 kJ, UV--0.35 nm). The design includes a large target-to-microscope (400-700 mm) distance required by the x-ray ablation issues anticipated on the Laser MegaJoule facility [P. A. Holstein et al., Laser Part. Beams 17, 403 (1999)] (1.8 MJ) which is under construction. Two eight-image Kirkpatrick-Baez microscopes [P. Kirkpatrick and A. V. Baez J. Opt. Soc. Am. 38, 766 (1948)] with different spectral wavelength ranges and with a 400 mm source-to-mirror distance image the target on a custom-built framing camera (time resolution of {approx}80 ps). The soft x-ray version microscope is sensitive below 1 keV and its spatial resolution is better than 30 {mu}m over a 2-mm-diam region. The hard x-ray version microscope has a 10 {mu}m resolution over an 800-{mu}m-diam region and is sensitive in the 1-5 keV energy range. Two other x-ray microscopes based on an association of toroidal/spherical surfaces (T/S microscopes) produce an image on a streak camera with a spatial resolution better than 30 {mu}m over a 3 mm field of view in the direction of the camera slit. Both microscopes have been designed to have, respectively, a maximum sensitivity in the 0.1-1 and 1-5 keV energy range. We present the original design of these four microscopes and their test on a dc x-ray tube in the laboratory. The diagnostics were successfully used on LIL first experiments early in 2005. Results of soft x-ray imaging of a radiative jet during conical shaped laser interaction are shown.

  11. Interfacial Microstructures in Multilayer Semiconductors Studied by Grazing Incident X-Ray Scattering and Fluorescence Yield.

    NASA Astrophysics Data System (ADS)

    Ming, Zhi-Hong

    The grazing incident x-ray scattering and fluorescence yield utilizing synchrotron radiation have been used to study multilayer semiconductors consisting of Si _{rm 1-x}Ge_ {rm x} and Si epilayers grown by MBE. The angular dependence of x-ray reflectivity, diffuse scattering and Ge K_{alpha} fluorescence emission have been studied. The research emphasizes on the microstructures of interfaces in these layered structures. The rms interfacial roughness, layer thickness, and optical constants were obtained by fitting measured specular reflectivity data to a theoretical model, which incorporated Fresnel's laws of optics with interfacial roughness. The height fluctuation of interface was associated with a self-affine surface defined in terms of fractional Brownian motion. The lateral-, cross-correlation length and texture coefficient have been obtained by comparison of the transverse and longitudinal diffuse scattering experimental data with theoretical models. The Ge density profile in the epilayer is studied by the angular dependence of Ge K_{alpha} fluorescence yield. The samples studied in this dissertation include bulk Si, normal and inverted SiGe/Si heterostructures, ultrathin Ge layers buried in bulk Si, and SiGe/Si superlattices. The results indicate that normal and inverted SiGe/Si heterointerfaces have similar interfacial microstructures in terms of rms roughness, lateral-correlation length, texture coefficient, and Ge density profile. The evidence of x-ray standing wave has been found in the superlattices. The cross-correlation of interfacial roughness at different interfaces has been observed in superlattice samples and ultrathin Ge layers in Si bulk. The longitudinal diffuse scattering show similar oscillation patterns as reflectivity for these samples. The cross-correlation length for ultrathin Ge layers in Si has been estimated to be comparable with layer thickness. In the EXAFS study of 4 A Ge layer in bulk Si, the lattice strain of Ge layer has been

  12. Electromagnetic wave scattering at near-grazing incidence from a gently undulating, rough surface

    NASA Technical Reports Server (NTRS)

    Vesecky, J. F.; Sperley, E. J.; Zebker, H. A.

    1988-01-01

    Models to estimate the reflection coefficient of a statistically rough surface, for example the works of Beckmann, Smith, and Vesecky are discussed. Bistatic radar experiments carried out during the Apollo 16 mission provide a data set with which to compare theoretical models and experimental data. These bistatic S-band radar experiments provide experimental estimates of the Moon's bistatic, forward scatter, reflection coefficient for grazing angles of 2.5 to 78 deg. Theoretical expressions for the reflection coefficient are developed for comparison with these experimental data. At grazing angles below 10 deg the models of Smith and Vesecky compare favorably with the data. Beckmann's model falls significantly more rapidly with decreasing grazing angle than does the data.

  13. Efficiency of a Grazing-incidence Off-plane Grating in the Soft-x-ray Region

    NASA Technical Reports Server (NTRS)

    Seely, J. F.; Laming, J. M.; Goray, L. I.; Kjornrattanawanich, B.; Holland, G. E.; Flanagan, K. A.; Heilmann, R. K.; Chang, C.-H.; Schattenburg, M. L.; Rasmussen, A. P.

    2006-01-01

    Efficiency measurements of a grazing-incidence diffraction grating in the off-plane mount were performed using polarized synchrotron radiation. The grating had 5000 grooves/mm, an effective blaze angle of 14 deg., and was gold coated. The efficiencies in the two polarization orientations (TM and TE) were measured in the 1.5-5.O nm wavelength range and were compared with the efficiencies calculated using the PCGrate-SX code. The TM and TE efficiencies differ, offering the possibility of performing unique science studies of astrophysical, solar, and laboratory sources by exploiting the polarization sensitivity of the off-plane grating.

  14. Morphology of open films of discotic hexagonal columnar liquid crystals as probed by grazing incidence X-ray diffraction.

    PubMed

    Grelet, Eric; Dardel, Sébastien; Bock, Harald; Goldmann, Michel; Lacaze, Emmanuelle; Nallet, Frédéric

    2010-04-01

    The structure and the orientation of thermotropic hexagonal columnar liquid crystals are studied by grazing incidence X-ray diffraction (GIXD) for different discotic compounds in the geometry of open supported thin films. Whatever the film deposition mode (either spin-coating or vacuum evaporation) and the film thickness, a degenerate planar alignment with the liquid crystalline columns parallel to the substrate is found. However, if a specific thermal process is applied to the liquid crystal film, homeotropic anchoring (columns normal to the interface) can be stabilized in a metastable state. PMID:20411293

  15. Module-type flat-field grazing-incidence spectrographs for large Tokamak (JT-60) plasma diagnosis

    NASA Astrophysics Data System (ADS)

    Nagata, Hiroshi; Kihara, Naoto; Yamashita, Takaji; Sugie, Tatsuo; Kubo, Hirotaka; Shiho, Makoto

    1990-09-01

    Module-type flat-field grazing-incidence spectrographs with holographic gratings and multichannel detectors for large TOKAMAK (JT-60) plasma diagnosis are developed. The spectrographs cover the different wavelength regions from 0.5-122 nm, and are set to measure impurity lines in the plasma every 20 ms with space resolution of 7 cm. The flat-field imaging properties with designed wavelength resolution were confirmed, and results of tokamak plasma measurements proved the value of these spectrographs for plasma diagnosis.

  16. Time-resolved in situ investigations of reactive sputtering processes by grazing incidence X-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Lützenkirchen-Hecht, Dirk; Frahm, Ronald

    2006-09-01

    We have applied the time-resolved grazing incidence X-ray absorption fine structure technique to study in situ the atomic short range order and the electronic structure of reactively sputter deposited thin films. Results obtained during the reactive deposition of amorphous Ta-pentoxide thin films deposited in oxygen containing atmospheres will be presented. A new calculation scheme for a detailed reflection mode EXAFS data analysis giving bond distances, coordination numbers and Debye-Waller factors is presented. The atomic short range structure of the amorphous Ta 2O 5 thin films is compared to that of crystalline β-Ta 2O 5.

  17. Proposed design class of grazing incidence echelle spectrometers - Critical analysis and reevaluation

    NASA Technical Reports Server (NTRS)

    Hettrick, M. C.; Jelinsky, P.; Bowyer, S.; Malina, R. F.

    1984-01-01

    The class of miltibounce grazing spectrometers proposed by Cash (1982) and by McClintock and Cash (1982) is analyzed, and performance values significantly lower than asserted by these authors are found. Ray tracing calculations used to examine the design parameters given in the above papers are reported, as is the efficiency which results from use of accepted reflectance data. Several schemes which can improve some of the performance parameters are indicated.

  18. Determination of the geometric corrugation of graphene on SiC(0001) by grazing incidence fast atom diffraction

    SciTech Connect

    Zugarramurdi, A.; Debiossac, M.; Lunca-Popa, P.; Mayne, A. J.; Borisov, A. G.; Mu, Z.; Roncin, P.; Khemliche, H.; Momeni, A.

    2015-03-09

    We present a grazing incidence fast atom diffraction (GIFAD) study of monolayer graphene on 6H-SiC(0001). This system shows a Moiré-like 13 × 13 superlattice above the reconstructed carbon buffer layer. The averaging property of GIFAD results in electronic and geometric corrugations that are well decoupled; the graphene honeycomb corrugation is only observed with the incident beam parallel to the zigzag direction while the geometric corrugation arising from the superlattice is revealed along the armchair direction. Full-quantum calculations of the diffraction patterns show the very high GIFAD sensitivity to the amplitude of the surface corrugation. The best agreement between the calculated and measured diffraction intensities yields a corrugation height of 0.27 ± 0.03 Å.

  19. Correction of Spherical Aberration in Grazing-Incidence X-ray Optics by Combination of Spherical-Concave Mirrors

    SciTech Connect

    Suzuki, Y.; Takeuchi, A.

    2011-09-09

    In grazing-incidence total-reflection mirror optics for x-rays, spherical aberrations and coma are the most serious aberrations for microfocusing and microimaging. High-resolution imaging is believed to be possible only when an aspherical mirror system is used. However, the spherical aberrations of a spherical-concave mirror in a grazing-incidence condition can be eliminated by sequential reflection of spherical mirrors of similar shapes. A sub-micrometer one-dimensional focusing is easily achieved by the spherical-aberration-corrected tandem-spherical mirror optics. By configuring four spherical mirrors in an analogy of the crossed mirror optics (Kirkpatrick-Baez optics), it is possible to achieve sub-micrometer focused beam size in the hard x-ray region. Preliminary experiments on x-ray microfocusing have been carried out at beamline 20XU of SPring-8, and a 0.5 {mu}mx0.4 {mu}m beam size was achieved at 8 keV.

  20. Ultra-small-angle neutron scattering with azimuthal asymmetry

    PubMed Central

    Gu, X.; Mildner, D. F. R.

    2016-01-01

    Small-angle neutron scattering (SANS) measurements from thin sections of rock samples such as shales demand as great a scattering vector range as possible because the pores cover a wide range of sizes. The limitation of the scattering vector range for pinhole SANS requires slit-smeared ultra-SANS (USANS) measurements that need to be converted to pinhole geometry. The desmearing algorithm is only successful for azimuthally symmetric data. Scattering from samples cut parallel to the plane of bedding is symmetric, exhibiting circular contours on a two-dimensional detector. Samples cut perpendicular to the bedding show elliptically dependent contours with the long axis corresponding to the normal to the bedding plane. A method is given for converting such asymmetric data collected on a double-crystal diffractometer for concatenation with the usual pinhole-geometry SANS data. The aspect ratio from the SANS data is used to modify the slit-smeared USANS data to produce quasi-symmetric contours. Rotation of the sample about the incident beam may result in symmetric data but cannot extract the same information as obtained from pinhole geometry. PMID:27275140

  1. Small angle elastic scattering of protons off of spinless nuclei

    SciTech Connect

    Ling, A.G.

    1988-07-01

    Elastic differential cross sections and analyzing powers for 800 MeV protons incident on /sup 12/C, /sup 40/Ca, and /sup 208/Pb in the momentum transfer range 20 MeV/c < q < 130 MeV/c have been measured. The data was taken with the High Resolution Spectrometer (HRS) at the Los Alamos Meson Physics Facility. Special delay-line drift chambers with dead regions for the beam to pass through them were used to obtain the data. Through the interference of the Coulomb and nuclear contributions to the differential cross section in the small angle region, the ratio of the real to imaginary part of the forward nuclear amplitude ..cap alpha../sub n/(0) = Ref/sub n/(0)/Imf/sub n/(0) is extracted. The importance of knowing this quantity at lower energies in order to study the differences between relativistic and non-relativistic scattering theories is discussed. 130 refs., 60 figs., 12 tabs.

  2. An application of the grazing-angle incidence hard x-ray optical nanoscope in ultra-high density digital data read-out device

    NASA Astrophysics Data System (ADS)

    Bezirganyan, Hakob P.; Bezirganyan, Siranush E.; Bezirganyan, Petros H., Jr.; Bezirganyan, Hayk H., Jr.

    2008-08-01

    We present in this theoretical paper a set-up of grazing-angle incidence hard x-ray nanoscope (GIXN), which is the essential part of ultra-high density digital data read-out device. The GIXN consists of the asymmetrically cut single crystal, which is operating like an image magnifier. The X-ray high-resolution diffractive optical lens (zone plate) and spatially resolving detector (CCD camera) are arranged like in classical schemes of the X-ray imaging microscopy. Proposed nanoscope operates based on grazing-angle incidence x-ray backscattering diffraction (GIXB) technique applied in the specular beam suppression mode. Grazing-angle incident X-ray configuration allows the handling of data from very large surface area of the X-ray optical memory disk (X-ROM) and, consequently, the data read-out speed is much faster than in optical data read-out systems.

  3. van der Waals effects on grazing-incidence fast-atom diffraction for H on LiF(001)

    NASA Astrophysics Data System (ADS)

    Bocan, G. A.; Fuhr, J. D.; Gravielle, M. S.

    2016-08-01

    We theoretically address grazing incidence fast atom diffraction (GIFAD) for H atoms impinging on a LiF(001) surface. Our model combines a description of the H-LiF(001) interaction obtained from density functional theory calculations with a semiquantum treatment of the dynamics. We analyze simulated diffraction patterns in terms of the incidence channel, the impact energy associated with the motion normal to the surface, and the relevance of van der Waals (vdW) interactions. We then contrast our simulations with experimental patterns for different incidence conditions. Our most important finding is that for normal energies lower than 0.5 eV and incidence along the <100 > channel, the inclusion of vdW interactions in our potential energy surface yields a greatly improved accord between simulations and experiments. This agreement strongly suggests a non-negligible role of vdW interactions in H-on-LiF(001) GIFAD in the low-to-intermediate normal energy regime.

  4. Seismic scattering of low-grazing-angle acoustic waves incident on the seafloor

    NASA Astrophysics Data System (ADS)

    Greaves, Robert John

    The goal of this thesis is to develop a methodology to interpret sound scattered from the seafloor in terms of seafloor structure and subseafloor geological properties. Specifically, this work has been directed towards the interpretation of matched-filtered, beamformed monostatic acoustic reverberation data acquired on the west flank of the Mid-Atlantic Ridge when the seafloor is insonified by a band-limited, low-grazing-angle acoustic pulse. This research is based on the hypothesis that observed backscatter signals are produced by a combination of seafloor (interface) scattering and subseafloor (volume) scattering from structure having variations at scale lengths similar to the wavelength of the insonifying acoustic field. Analysis of monostatic reverberation data acquired during the Site A experiment (Run 1) of the Acoustic Reverberation Special Research Program 1993 Acoustics Cruise suggests that the scattered signals cannot be accounted for quantitatively in terms of large- scale slope, even though a strong correspondence between high intensity backscatter and seafloor ridges is observed. In order to investigate and quantify the actual sources of seafloor scattering, a numerical modeling study of seafloor models is undertaken using a finite- difference solution to the elastic wave equation. Geological data available at Site A and published reports describing geological properties of similar deep ocean crustal regions are used to develop a realistic seafloor model for the study area with realistic constraints on elastic parameters. Wavelength-scale heterogeneity in each model, in the form of seafloor roughness and subseafloor volume heterogeneity is defined using stochastic distributions with Gaussian autocorrelations. These distributions are quantified by their correlation lengths and standard deviation in amplitude. In order to incorporate all seafloor structure in a single parameterization of seafloor scattering, large-scale slope and wavelength

  5. Determination of the structure and heating mechanisms of coronal loops from soft X-ray observations with the solar probe. [grazing incidence telescope

    NASA Technical Reports Server (NTRS)

    Davis, J. M.; Krieger, A. S.

    1978-01-01

    High resolution soft X-ray imaging from the solar probe is justified in terms of the expected scientific returns which include the determination of the temperature and density structure of a coronal loop. The advantages of the grazing incidence telescope over the multiple pinhole camera are discussed. An instrument package is described which includes a grazing incidence mirror, a thermal prefilter, a three position filter wheel and a focal plane detector baselined as an 800 by 800 back-illuminated charge coupled device. The structural assembly together with the data processing equipment would draw heavily on the designs being developed for the Solar Polar Mission.

  6. An analysis of two classes of grazing incidence mirrors for use with Rowland circle spectrometers

    NASA Technical Reports Server (NTRS)

    Green, James; Bowyer, Stuart

    1986-01-01

    Results are presented of a comparative analysis of Hettrick Bowyer Type II (HBII) and Wolter-Schwarzschild Type II (WSII) optics for use with Rowland circle spectrometers. The HBII can substitute, with few exceptions, for a WSII in any Rowland circle with little change in spectrometer performance or design. However, the HBII telescope offers several clear advantages over the WSII in these configurations. Because the HBII employs a virtual focus, it requires a much shorter instrument length than a WSII. For example, a 3-m Rowland circle spectrometer, fed by an optimized, f/10, 1-m diameter WSII, has a total instrument length of 6 m. If a HBII is used to feed the identical spectrometer, the entire instrument length can be as little as 3 m. In addition, the improved imaging gained with the larger graze angles of the HBII design results in better resolution in slitless operation modes.

  7. Computer-Controlled Cylindrical Polishing Process for Development of Grazing Incidence Optics for Hard X-Ray Region

    NASA Technical Reports Server (NTRS)

    Khan, Gufran Sayeed; Gubarev, Mikhail; Speegle, Chet; Ramsey, Brian

    2010-01-01

    The presentation includes grazing incidence X-ray optics, motivation and challenges, mid spatial frequency generation in cylindrical polishing, design considerations for polishing lap, simulation studies and experimental results, future scope, and summary. Topics include current status of replication optics technology, cylindrical polishing process using large size polishing lap, non-conformance of polishin lap to the optics, development of software and polishing machine, deterministic prediction of polishing, polishing experiment under optimum conditions, and polishing experiment based on known error profile. Future plans include determination of non-uniformity in the polishing lap compliance, development of a polishing sequence based on a known error profile of the specimen, software for generating a mandrel polishing sequence, design an development of a flexible polishing lap, and computer controlled localized polishing process.

  8. Extended-range grazing-incidence spectrometer for high-resolution extreme ultraviolet measurements on an electron beam ion trap.

    PubMed

    Beiersdorfer, P; Magee, E W; Brown, G V; Hell, N; Träbert, E; Widmann, K

    2014-11-01

    A high-resolution grazing-incidence grating spectrometer has been implemented on the Livermore electron beam ion traps for performing very high-resolution measurements in the soft x-ray and extreme ultraviolet region spanning from below 10 Å to above 300 Å. The instrument operates without an entrance slit and focuses the light emitted by highly charged ions located in the roughly 50 μm wide electron beam onto a cryogenically cooled back-illuminated charge-coupled device detector. The measured line widths are below 0.025 Å above 100 Å, and the resolving power appears to be limited by the source size and Doppler broadening of the trapped ions. Comparisons with spectra obtained with existing grating spectrometers show an order of magnitude improvement in spectral resolution.

  9. Extended-range grazing-incidence spectrometer for high-resolution extreme ultraviolet measurements on an electron beam ion trap

    SciTech Connect

    Beiersdorfer, P.; Magee, E. W.; Brown, G. V.; Träbert, E.; Widmann, K.; Hell, N.

    2014-11-15

    A high-resolution grazing-incidence grating spectrometer has been implemented on the Livermore electron beam ion traps for performing very high-resolution measurements in the soft x-ray and extreme ultraviolet region spanning from below 10 Å to above 300 Å. The instrument operates without an entrance slit and focuses the light emitted by highly charged ions located in the roughly 50 μm wide electron beam onto a cryogenically cooled back-illuminated charge-coupled device detector. The measured line widths are below 0.025 Å above 100 Å, and the resolving power appears to be limited by the source size and Doppler broadening of the trapped ions. Comparisons with spectra obtained with existing grating spectrometers show an order of magnitude improvement in spectral resolution.

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

    PubMed

    Jiang, Hui; Wang, Zhanshan; Zhu, Jingtao

    2013-05-01

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

  11. Grazing-incidence neutron-induced fluorescence probes density profiles of labeled molecules at solid/liquid interfaces.

    PubMed

    Schneck, Emanuel; Jentschel, Michael; Gege, Christian; Tanaka, Motomu; Demé, Bruno

    2013-03-26

    We report on the use of characteristic prompt γ-fluorescence after neutron capture induced by an evanescent neutron wave to probe densities and depth profiles of labeled molecules at solid/liquid interfaces. In contrast to classical scattering techniques and X-ray fluorescence, this method of "grazing-incidence neutron-induced fluorescence" combines direct chemical specificity, provided by the label, with sensitivity to the interface, inherent to the evanescent wave. We demonstrate that the formation of a supported lipid membrane can be quantitatively monitored from the characteristic fluorescence of (157)Gd(3+) ions bound to the headgroup of chelator lipids. Moreover, we were able to localize the (157)Gd(3+) ions along the surface normal with nanometer precision. This first proof of principle with a well-defined model system suggests that the method has a great potential for biology and soft matter studies where spatial resolution and chemical sensitivity are required.

  12. Surface complexation studied via combined grazing-incidence EXAFS and surface diffraction: Arsenate on hematite (0001) and (10-12)

    USGS Publications Warehouse

    Waychunas, G.; Trainor, T.; Eng, P.; Catalano, J.; Brown, G.; Davis, J.; Rogers, J.; Bargar, J.

    2005-01-01

    X-ray diffraction [crystal-truncation-rod (CTR)] studies of the surface structure of moisture-equilibrated hematite reveal sites for complexation not present on the bulk oxygen-terminated surface, and impose constraints on the types of inner-sphere sorption topologies. We have used this improved model of the hematite surface to analyze grazing-incidence EXAFS results for arsenate sorption on the c(0001) and r(10-12) surfaces measured in two electric vector polarizations. This work shows that the reconfiguration of the surface under moist conditions is responsible for an increased adsorption density of arsenate complexes on the (0001) surface relative to predicted ideal termination, and an abundance of "edge-sharing" bidentate complexes on both studied surfaces. We consider possible limitations on combining the methods due to differing surface sensitivities, and discuss further analysis possibilities using both methods. ?? Springer-Verlag 2005.

  13. On the Alignment and Focusing of the Marshall Grazing Incidence X-ray Spectrometer (MaGIXS)

    NASA Technical Reports Server (NTRS)

    Champey, Patrick; Winebarger, Amy; Kobayashi, Ken; Savage, Sabrina; Cirtain, Jonathan; Cheimets, Peter; Hertz, Edward; Golub, Leon; Ramsey, Brian; McCracken, Jeff

    2016-01-01

    The Marshall Grazing Incidence X-ray Spectrometer (MaGIXS) is a NASA sounding rocket instrument that is designed to observe soft X-ray emissions from 24 - 6.0 A (0.5 - 2.0 keV energies) in the solar atmosphere. For the rst time, high-temperature, low-emission plasma will be observed directly with 5 arcsecond spatial resolution and 22 mA spectral resolution. The unique optical design consists of a Wolter - I telescope and a 3-optic grazing- incidence spectrometer. The spectrometer utilizes a nite conjugate mirror pair and a blazed planar, varied line spaced grating, which is directly printed on a silicon substrate using e-beam lithography. The grating design is being nalized and the grating will be fabricated by the Massachusetts Institute of Technology (MIT) and Izentis LLC. Marshall Space Flight Center (MSFC) is producing the nickel replicated telescope and spectrometer mirrors using the same facilities and techniques as those developed for the ART-XC and FOXSI mirrors. The Smithsonian Astrophysical Observatory (SAO) will mount and align the optical sub-assemblies based on previous experience with similar instruments, such as the Hinode X-Ray Telescope (XRT). The telescope and spectrometer assembly will be aligned in visible light through the implementation of a theodolite and reference mirrors, in addition to the centroid detector assembly (CDA) { a device designed to align the AXAF-I nested mirrors. Focusing of the telescope and spectrometer will be achieved using the X-ray source in the Stray Light Facility (SLF) at MSFC. We present results from an alignment sensitivity analysis performed on the on the system and we also discuss the method for aligning and focusing MaGIXS.

  14. Thermomechanical design of the grazing incidence metal mirror of the prometheus-L IFE reactor

    SciTech Connect

    Ghoniem, N.M.; El-Azab, A.

    1994-12-31

    In Laser IFE reactors the reflectivity and absorptivity of the grazing metal mirror depend on the neutron dose received by the mirror surface. In addition to these irradiation effects, the surface deformation due to neutron irradiation-induced swelling and due to thermal loads change the focusing quality of the mirror. In the present work, a thorough review of the irradiation effects on the changes in mirror surface quality is presented. A mirror design methodology, which considers the deformation due to the loads associated with laser beam and the deformation due to neutron-irradiation induced swelling is discussed. The basic philosophy considered in the design is to separate the functions and choose the best possible materials to perform these specific functions. An aluminum thin layer, for the purpose of reflection of the laser beam, is deposited on a SiC substrate. The SiC substrate provides a rigid bulk, through which coolant is provided to remove the heat absorbed during laser pulses, and avoids the need for a thicker aluminum layer that undergoes more swelling than SiC. A concrete frame is designed to provide the ultimate resistance against thermally-induced deformation. Other features of the design will also be presented.

  15. Small-angle neutron scattering from samples of expanded carbon

    SciTech Connect

    Bogdanov, S. G. Valiev, E. Z.; Dorofeev, Yu. A.; Pirogov, A. N.; Skryabin, Yu. N.; Makotchenko, V. G.; Nazarov, A. S.; Fedorov, V. E.

    2006-12-15

    The subatomic structure of expanded graphite has been investigated by small-angle neutron scattering. Samples were synthesized during quick thermal decomposition of intercalated compounds based on oxidized graphite. They had a low bulk density (up to 0.1 g/cm{sup 3}) and were characterized by considerable small-angle scattering. It has been established that majority of the volume of expanded graphite samples is occupied by participles with characteristic sizes in two ranges: from 6 to 8 nm and from 20 to 30 nm. Small particles have properties of a surface fractal with the dimension D{sub s} = 2.4-2.6, whereas the larger particles are mainly smooth and have the dimension D{sub s} = 2.0-2.1. The specific surface of the samples studied was determined from the small-angle scattering data.

  16. Impedance Scaling for Small-angle Tapers and Collimators

    SciTech Connect

    Stupakov, G.; /SLAC

    2010-02-11

    In this note I will prove that the impedance calculated for a small-angle collimator or taper, of arbitrary 3D profile, has a scaling property that can greatly simplify numerical calculations. This proof is based on the parabolic equation approach to solving Maxwell's equation developed in Refs. [1, 2]. We start from the parabolic equation formulated in [3]. As discussed in [1], in general case this equation is valid for frequencies {omega} >> c/a where a is a characteristic dimension of the obstacle. However, for small-angle tapers and collimators, the region of validity of this equation extends toward smaller frequencies and includes {omega} {approx} c/a.

  17. Development and prospects of Very Small Angle Neutron Scattering (VSANS) techniques

    NASA Astrophysics Data System (ADS)

    Xuo, Tai-Sen; Cheng, He; Chen, Yuan-Bo; Wang, Fang-Wei

    2016-07-01

    Very Small Angle Neutron Scattering (VSANS) is an upgrade of the traditional Small Angle Neutron Scattering (SANS) technique which can cover three orders of magnitude of length scale from one nanometer to one micrometer. It is a powerful tool for structure calibration in polymer science, biology, material science and condensed matter physics. Since the first VSANS instrument, D11 in Grenoble, was built in 1972, new collimation techniques, focusing optics (multi-beam converging apertures, material or magnetic lenses, and focusing mirrors) and higher resolution detectors combined with the long flight paths and long incident neutron wavelengths have been developed. In this paper, a detailed review is given of the development, principles and application conditions of various VSANS techniques. Then, beam current gain factors are calculated to evaluate those techniques. A VSANS design for the China Spallation Neutron Source (CSNS) is thereby presented. Supported by National Natural Science Foundation of China (21474119, 11305191)

  18. Ultra Small-Angle Neutron Scattering Study of Porous Glass

    SciTech Connect

    Desai, Reshma R.; Desa, J. A. Erwin; Sen, D.; Mazumder, S.

    2011-07-15

    Compacts of silica micro-spheres prepared for different times at sintering temperatures of 640 deg. C and 740 deg. C have been studied by Ultra Small-Angle Neutron Scattering (USANS) and Scanning Electron Microscopy (SEM). Stress versus strain measurements display several breakage points related to a range of nearest neighbour coordination around each microsphere.

  19. Small angle neutron scattering from nanometer grain sized materials

    SciTech Connect

    Epperson, J.E.; Siegel, R.W.

    1991-11-01

    Small angie neutron scattering has been utilized, along with a number of complementary characterization methods suitable to the nanometer size scale, to investigate the structures of cluster-assembled nanophase materials. Results of these investigations are described and problems and opportunities in using small angle scattering for elucidating nanostructures are discussed.

  20. Study of magnetism at surfaces by scattering of neutrons at grazing incidence

    SciTech Connect

    Felcher, G.P.

    1984-07-01

    Neutrons can provide information on magnetic phenomena at surfaces. The simplest experiment involves the measurement of the reflectivity of a well-collimated beam from the surface, as a function either of the neutron wavelength or of the angle of incidence theta/sub i/. Using polarized neutrons, the spin-dependent reflectivity of a magnetically-active material can determine the depth profile of the magnetic induction B. A prototype instrument at the Intense Pulsed Neutron Source at Argonne has already demonstrated the feasibility of this technique in determining the penetration depth of an external magnetic field in superconductors. Further experiments are being planned to study the magnetic disturbances close to the surface of ferromagnets; a first experiment on films of iron oxides showed a remarkable change of the magnetic depth profile with increasing oxidation.

  1. Small Angle X-ray Scattering for Nanoparticle Research.

    PubMed

    Li, Tao; Senesi, Andrew J; Lee, Byeongdu

    2016-09-28

    X-ray scattering is a structural characterization tool that has impacted diverse fields of study. It is unique in its ability to examine materials in real time and under realistic sample environments, enabling researchers to understand morphology at nanometer and angstrom length scales using complementary small and wide angle X-ray scattering (SAXS, WAXS), respectively. Herein, we focus on the use of SAXS to examine nanoscale particulate systems. We provide a theoretical foundation for X-ray scattering, considering both form factor and structure factor, as well as the use of correlation functions, which may be used to determine a particle's size, size distribution, shape, and organization into hierarchical structures. The theory is expanded upon with contemporary use cases. Both transmission and reflection (grazing incidence) geometries are addressed, as well as the combination of SAXS with other X-ray and non-X-ray characterization tools. We conclude with an examination of several key areas of research where X-ray scattering has played a pivotal role, including in situ nanoparticle synthesis, nanoparticle assembly, and operando studies of catalysts and energy storage materials. Throughout this review we highlight the unique capabilities of X-ray scattering for structural characterization of materials in their native environment.

  2. Surface structure of sterically stabilized ferrofluids in a normal magnetic field: Grazing-incidence x-ray study

    NASA Astrophysics Data System (ADS)

    Vorobiev, A.; Gordeev, G.; Konovalov, O.; Orlova, D.

    2009-03-01

    We studied the internal structure of sterically stabilized water- and oil-based ferrofluids in the vicinity of the free interface with a gas by means of x-ray reflectometry and grazing-incidence x-ray diffraction. It was found that in-depth distribution of the magnetic nanoparticles in the layer close to the interface is essentially inhomogeneous. In the case of water-based ferrofluids an enhanced concentration of surfactant and subsequent reduced concentration of the particles were detected in the 100-200-Å -thick interface-adjacent layer. Scattering patterns possessing characteristic features of powder diffraction revealed partial ordering of the surfactant in a multilamellar structure. External magnetic fields applied perpendicular to the interface effectively reduced thickness of the depleted layer bringing the particles from the bulk to the surface. However no field-induced correlations between the particles were detected. In the top 500-Å -thick layer of an oil-based ferrofluid depletion of the particles density was also present; however, no special arrangement of the surfactant molecules was manifested by the experimental data. Interestingly, for all samples we observed wavy surface deformation appearing in the normal magnetic field of a strength H much smaller than the critical values Hc calculated according to the conventional theory of ferrofluid surface instability. This deformation with lateral periodicity of a few millimeters has an amplitude smoothly increasing up to a few microns at H=0.5Hc .

  3. Advanced laser-backlit Grazing-Incidence X-Ray Imaging Systems for Inertial Confinement Fusion Research. I. Design.

    PubMed

    Bennett, G R

    2001-09-01

    By use of a focusing configuration analogous to a Gregorian or a Cassegrain telescope, the on-axis aberration of a grazing-incidence spheric-based Kirkpatrick-Baez compound microscope may be precisely corrected. For finite fields, the off-axis performance degrades too rapidly for high-spatial-resolution imaging of even the smallest objects of interest. However, by use of ray-trace optimization it is possible to perturb the system such that the perfect, but impractical, on-axis performance is modestly degraded and uniformly distributed over a chosen object field. By use of this and other performance-enhancing features, two example ultrahigh-spatial-resolution laser-backlit x-ray microscope designs suitable for inertial confinement fusion (ICF) research have been developed. A companion paper [Appl. Opt. 40, 4588 (2001)] describing the tolerance analysis indicates that <0.5-mum spatial resolution at x-ray energies as high as 25 KeV is possible. As a prototype step, simpler noncompound devices are under consideration for Sandia National Laboratories' Z accelerator/Z-Beamlet ICF facility. PMID:18360499

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

    PubMed

    Ree, Moonhor

    2014-05-01

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

  5. Grazing-incidence x-ray scattering from stepped interfaces in AlAs/GaAs superlattices

    NASA Astrophysics Data System (ADS)

    Kondrashkina, E. A.; Stepanov, S. A.; Opitz, R.; Schmidbauer, M.; Köhler, R.; Hey, R.; Wassermeier, M.; Novikov, D. V.

    1997-10-01

    The features of surface and interface roughness in crystalline AlAs/GaAs superlattices grown by molecular beam epitaxy on vicinal (001) GaAs substrates are studied by grazing-incidence x-ray scattering (GIXS). The effects of different growth modes [step-flow or two-dimensional- (2D-) nucleation], different substrate preparations, and growth interruptions on the roughness are investigated. The results of GIXS are compared with atomic force microscopy (AFM) images of sample surfaces. For samples grown in the step-flow mode, both of the methods display a distinct anisotropy in the lateral size of roughness along the substrate miscut direction and perpendicular to it. The lateral correlation lengths given by GIXS correspond to the size of step bunches observed by AFM, while individual steps are resolved by AFM only. GIXS reveals also a strong interface-interface correlation or inheritance of roughness for all the samples which is not accessible by AFM. Moreover, the angle of inclination of the direction of this inheritance from the surface normal is found to be dependent on the growth conditions. Two effects in the skew inheritance have been observed by means of 2D mapping of GIXS in the reciprocal space: (i) in the direction of substrate miscut the angle of skew inheritance inverted its sign, (ii) in the direction perpendicular to the miscut a strongly skew inheritance appeared as an effect of growth interruptions. Conclusions concerning the improvement of GIXS experiments applied to the studies of multilayers are derived.

  6. Observing the Sun in hard X-rays using grazing incidence optics: the FOXSI and HEROES projects

    NASA Astrophysics Data System (ADS)

    Christe, Steven; Glesener, Lindsay; Krucker, Sam; Shih, Albert Y.; Gaskin, Jessica; Wilson, Colleen

    2014-06-01

    Solar flares accelerate particles up to high energies through various acceleration mechanisms which are not currently understood. Hard X-rays are the most direct diagnostic of flare-accelerated electrons. However past and current hard x-ray observation lack the sensitivity and dynamic range necessary to observe the faint signature of accelerated electrons in the acceleration region, the solar corona. These limitations can be easily overcome through the use of HXR focusing optics coupled with solid state pixelated detectors. We present results from the recent flights of two sub-orbital payloads that have applied grazing incidence HXR optics to solar observations. FOXSI, short for Focusing Optics X-Ray Solar Imager, was launched on a sounding rocket in November 2012 from White Sanda and observed a solar flare. HEROES, short for High Energy Replicated Optics to Explore the Sun, observed the sun for 7 hours from a high altitude balloon on September 21, 2013. We present recent results as well as the capabilities of a possible future satellite mission

  7. Time-resolved x-ray pinhole camera with grazing incidence mirror to eliminate bremsstrahlung noise signal on Z

    SciTech Connect

    Nash, T. J.; Chandler, G. A.; Bailey, J. E.; Rochau, G.; Leeper, R. J.; Nielsen, D. S.; Moore, T.

    2006-10-15

    An on-axis time-resolved x-ray pinhole camera has been used on the 20 MA 100 ns driver Z to image the converging shock wave in dynamic Hohlraum experiments and to image pellet hot spots in inertial confinement fusion implosions. This instrument is susceptible to detecting significant amounts of pinch bremsstrahlung radiation with energies at hundreds of keV and yields of roughly 1 kJ. Quite often the bremsstrahlung noise signals have overwhelmed the desired x-ray images. In an effort to eliminate this large source of noise we have incorporated a 6 deg. gold-coated grazing incidence mirror into the time-resolved x-ray pinhole camera system. The mirror reflects soft x rays at energies under 2 keV but does not reflect bremsstrahlung radiation at hundreds of keV. We will present data from the instrument without the mirror showing large amounts of bremsstrahlung noise contamination and data with the mirror in the system showing greatly reduced noise levels.

  8. An Investigation of Differential Deposition for Figure Corrections in Full-Shell Grazing-Incidents X-Ray Optics

    NASA Technical Reports Server (NTRS)

    Gubarev, Mikhail V.; Kilaru, Kirenmayee; Ramsey, Brian D.

    2009-01-01

    We are investigating differential deposition as a way of correcting small figure errors inside full-shell grazing-incidence x-ray optics. The optics in our study are fabricated using the electroformed-nickel-replication technique, and the figure errors arise from fabrication errors in the mandrel, from which the shells are replicated, as well as errors induced during the electroforming process. Combined, these give sub-micron-scale figure deviations which limit the angular resolution of the optics to approx. 10 arcsec. Sub-micron figure errors can be corrected by selectively depositing (physical vapor deposition) material inside the shell. The requirements for this filler material are that it must not degrade the ultra-smooth surface finish necessary for efficient x-ray reflection (approx. 5 A rms), and must not be highly stressed. In addition, a technique must be found to produce well controlled and defined beams within highly constrained geometries, as some of our mirror shells are less than 3 cm in diameter.

  9. Depth-profiling of vertical sidewall nanolayers on structured wafers by grazing incidence X-ray flourescence

    NASA Astrophysics Data System (ADS)

    Hönicke, P.; Beckhoff, B.; Kolbe, M.; List, S.; Conard, T.; Struyff, H.

    2008-12-01

    The Physikalisch-Technische Bundesanstalt (PTB), Germany's national metrology institute, developed an alignment strategy to specify elemental depth profiling in vertical sidewall layers on structured wafers. For this purpose, PTB's irradiation chamber for 200 mm and 300 mm silicon wafers was used to combine total-reflection X-ray fluorescence (TXRF) and grazing incidence XRF (GIXRF) techniques by employing monochromatized undulator radiation of the BESSY II electron storage ring. 3-D test structures were fabricated to develop an optimal alignment strategy allowing for depth profiling in such nanolayers. The test structures consisted of silicon bars with widths/spacings either in the μm or in the nm range. In order to be able to differentiate the sidewalls more easily from the remainder of the structures, they were provided with an additional silicon nitride layer. Four structure types of different bar width and density parameters on two 200 mm silicon wafers were investigated. The alignment procedure developed in the present work consists of three main steps and allows for distinct excitation of multiple sidewalls of one kind. Information about depth-dependent sidewall contamination, layer thickness and composition can be obtained by this approach. First results obtained on these test structures demonstrate the application potential of this new technique. In principle, depth-dependent chemical speciation should also be possible using GIXRF in combination with near edge absorption X-ray fine structure (NEXAFS).

  10. Surface structure of sterically stabilized ferrofluids in a normal magnetic field: grazing-incidence x-ray study.

    PubMed

    Vorobiev, A; Gordeev, G; Konovalov, O; Orlova, D

    2009-03-01

    We studied the internal structure of sterically stabilized water- and oil-based ferrofluids in the vicinity of the free interface with a gas by means of x-ray reflectometry and grazing-incidence x-ray diffraction. It was found that in-depth distribution of the magnetic nanoparticles in the layer close to the interface is essentially inhomogeneous. In the case of water-based ferrofluids an enhanced concentration of surfactant and subsequent reduced concentration of the particles were detected in the 100-200-A -thick interface-adjacent layer. Scattering patterns possessing characteristic features of powder diffraction revealed partial ordering of the surfactant in a multilamellar structure. External magnetic fields applied perpendicular to the interface effectively reduced thickness of the depleted layer bringing the particles from the bulk to the surface. However no field-induced correlations between the particles were detected. In the top 500-A -thick layer of an oil-based ferrofluid depletion of the particles density was also present; however, no special arrangement of the surfactant molecules was manifested by the experimental data. Interestingly, for all samples we observed wavy surface deformation appearing in the normal magnetic field of a strength H much smaller than the critical values H_{c} calculated according to the conventional theory of ferrofluid surface instability. This deformation with lateral periodicity of a few millimeters has an amplitude smoothly increasing up to a few microns at H=0.5H_{c} . PMID:19391940

  11. Advanced laser-backlit Grazing-Incidence X-Ray Imaging Systems for Inertial Confinement Fusion Research. I. Design.

    PubMed

    Bennett, G R

    2001-09-01

    By use of a focusing configuration analogous to a Gregorian or a Cassegrain telescope, the on-axis aberration of a grazing-incidence spheric-based Kirkpatrick-Baez compound microscope may be precisely corrected. For finite fields, the off-axis performance degrades too rapidly for high-spatial-resolution imaging of even the smallest objects of interest. However, by use of ray-trace optimization it is possible to perturb the system such that the perfect, but impractical, on-axis performance is modestly degraded and uniformly distributed over a chosen object field. By use of this and other performance-enhancing features, two example ultrahigh-spatial-resolution laser-backlit x-ray microscope designs suitable for inertial confinement fusion (ICF) research have been developed. A companion paper [Appl. Opt. 40, 4588 (2001)] describing the tolerance analysis indicates that <0.5-mum spatial resolution at x-ray energies as high as 25 KeV is possible. As a prototype step, simpler noncompound devices are under consideration for Sandia National Laboratories' Z accelerator/Z-Beamlet ICF facility.

  12. Ruthenium-Platinum Thin Film Analysis Using Grazing Incidence X-ray Diffraction

    SciTech Connect

    Jones, L.

    2004-09-03

    Ruthenium (Ru, Z = 44) is a Platinum Group Metal that has a standard hexagonal close packed (HCP) crystalline structure. Platinum (Pt, Z = 78) has a face-centered cubic (FCC) crystalline structure. When these metals are co-sputtered onto a silicon substrate, creating a few nm-thin film, they form an alloy with a combination of HCP and FCC structure. Direct methanol fuel cells rely on an anode catalyst to draw hydrogen from liquid methanol. Highly efficient fuel cells based on polymer electrolyte catalysts, known as proton-exchange membrane fuel cells, have been developed, but require large amounts of a costly platinum catalyst. Thin-film nanostructure bimetallic alloys have been produced to reduce the amount of expensive Platinum needed for catalysis, and also to improve the electrochemical properties of the catalyst. Supported RuPt particles have been shown to have superior activity as anode catalysts for methanol electro-oxidation and demonstrate an improvement in resistance to poisoning in comparison to unalloyed Pt. The percentage of Ruthenium in a RuPt thin film and the process by which the alloy is produced will dictate the crystalline structure, and thus the electrochemical properties of the film. Pure Ruthenium, Pure Platinum, and eight intermediate samples at differing percent composition of Ruthenium were characterized by their X-ray diffraction patterns. The incident beam is from the Stanford Synchrotron Radiation Laboratory beam and operates at approximately a 1.4 Angstrom wavelength. The results show that 0% Ru through 46.17% Ru exhibit a majority FCC structure, 56.07% Ru and 60.61% Ru are mixed phase, and from 67.03% Ru through 100% Ru, the samples exhibit a HCP structure.

  13. Small angle X-ray scattering coupled with in situ electromechanical probing of nanoparticle-based resistive strain gauges

    NASA Astrophysics Data System (ADS)

    Decorde, Nicolas; Sangeetha, Neralagatta M.; Viallet, Benoit; Viau, Guillaume; Grisolia, Jérémie; Coati, Alessandro; Vlad, Alina; Garreau, Yves; Ressier, Laurence

    2014-11-01

    A comprehensive study on the electromechanical behavior of nanoparticle-based resistive strain gauges in action through normal and grazing incidence small angle X-ray scattering (SAXS/GISAXS) investigations is presented. The strain gauges were fabricated from arrays of colloidal gold nanoparticle (NP) wires assembled on flexible polyethylene terephthalate and polyimide substrates by convective self-assembly. Microstructural changes (mean interparticle distance variations) within these NP wires under uniaxial stretching estimated by SAXS/GISAXS are correlated to their macroscopic electrical resistance variations. SAXS measurements suggest a linear longitudinal extension and transversal contraction of the NP wires with applied strain (0 to ~13%). The slope of this longitudinal variation is less than unity, implying a partial strain transfer from the substrate to the NP wires. The simultaneously measured electrical resistance of the strain gauges shows an exponential variation within the elastic domain of the substrate deformation, consistent with electron tunnelling through the interparticle gaps. A slower variation observed within the plastic domain suggests the formation of new electronic conduction pathways. Implications of transversal contraction of the NP wires on the directional sensitivities of strain gauges are evaluated by simulating electronic conduction in models mimicking a realistic NP arrangement. A loss of directionality of the NP-based strain gauges due to transversal current flow within the NP wires is deduced.A comprehensive study on the electromechanical behavior of nanoparticle-based resistive strain gauges in action through normal and grazing incidence small angle X-ray scattering (SAXS/GISAXS) investigations is presented. The strain gauges were fabricated from arrays of colloidal gold nanoparticle (NP) wires assembled on flexible polyethylene terephthalate and polyimide substrates by convective self-assembly. Microstructural changes (mean

  14. A SMALL-ANGLE DRILL-HOLE WHIPSTOCK

    DOEpatents

    Nielsen, D.E.; Olsen, J.L.; Bennett, W.P.

    1963-01-29

    A small angle whipstock is described for accurately correcting or deviating a drill hole by a very small angle. The whipstock is primarily utilized when drilling extremely accurate, line-of-slight test holes as required for diagnostic studies related to underground nuclear test shots. The invention is constructed of a length of cylindrical pipe or casing, with a whipstock seating spike extending from the lower end. A wedge-shaped segment is secured to the outer circumference of the upper end of the cylinder at a position diametrically opposite the circumferential position of the spike. Pin means are provided for affixing the whipstock to a directional drill bit and stem to alloy orienting and setting the whipstock properly in the drill hole. (AEC)

  15. SANS (small-angle neutron scattering) from polymers and colloids

    SciTech Connect

    Hayter, J.B.

    1987-01-01

    Small-angle neutron scattering (SANS) has been remarkably successful in providing detailed quantitative structural information on complex everyday materials, such as polymers and colloids, which are often of considerable industrial as well as academic interest. This paper reviews some recent SANS experiments on polymers and colloids, including ferrofluids, and discusses the use of these apparently complex systems as general physical models of the liquid or solid state.

  16. The small angle neutron spectrometer at the HANARO reactor, Korea

    NASA Astrophysics Data System (ADS)

    Seong, B.-S.; Han, Y.-S.; Lee, C.-H.; Lee, J.-S.; Hong, K.-P.; Park, K.-N.; Kim, H.-J.

    A new small angle neutron spectrometer (SANS) has been installed on the CN beam tube at the 30 MW HANARO Research Reactor in the Korea Atomic Energy Research Institute (KAERI). The SANS is to be used for the study of microstructural inhomogeneities in materials in the 1 nm to 100 nm size range. In this paper, the design characteristics of the spectrometer are presented in detail, and several SANS results for standard samples are presented which illustrate its performance.

  17. Grazing incidence x-ray diffraction analysis of zeolite NaA membranes on porous alumina tubes.

    PubMed

    Kyotani, Tomohiro

    2006-07-01

    Zeolite NaA-type membranes hydrothermally synthesized on porous alumina tubes, for dehydration process, were characterized by grazing incidence 2 theta scan X-ray diffraction analysis (GIXRD). The fine structure of the membrane was studied fractionally for surface layer and for materials embedded in the porous alumina tube. The thickness of the surface layer on the porous alumina tube in the membranes used in this study was approximately 2-3 microm as determined from transmission electron microscopy with focused ion beam thin-layer specimen preparation technique (FIB-TEM). To discuss the effects of the membrane surface morphology on the GIXRD measurements, CaA-type membrane prepared by ion exchange from the NaA-type membrane and surface-damaged NaA-type membrane prepared by water leaching were also studied. For the original NaA-type membrane, 2 theta scan GIXRD patterns could be clearly measured at X-ray incidence angles (alpha) ranging from 0.1 to 2.0 deg in increments of 0.1 deg. The surface layers of the 2 - 3 microm on the porous alumina tube correspond to the alpha values up to ca. 0.2 deg. For the CaA-type and the surface-damaged NaA-type membranes, however, diffraction patterns from the surface layer could not be successfully detected and the others were somewhat broad. For all the three samples, diffraction intensities of both zeolite and alumina increased with depth (X-ray incidence angle, alpha) in the porous alumina tube region. The depth profile analysis of the membranes based on the GIXRD first revealed that amount of zeolite crystal embedded in the porous alumina tube is much larger than that in the surface layer. Thus, the 2 theta scan GIXRD is a useful method to study zeolite crystal growth mechanism around (both inside and outside) the porous alumina support during hydrothermal synthesis and to study water permeation behavior in the dehydration process.

  18. Theory of oblique and grazing incidence Talbot‑Lau interferometers and demonstration in a compact source x‑ray reflective interferometer.

    PubMed

    Wen, Han; Kemble, Camille K; Bennett, Eric E

    2011-12-01

    With the advent of Talbot-Lau interferometers for x-ray phase-contrast imaging, oblique and grazing incidence configurations are now used in the pursuit of sub-micron grating periods and high sensitivity. Here we address the question whether interferometers having oblique incident beams behave in the same way as the well-understood normal incidence ones, particularly when the grating planes are non-parallel. We derive the normal incidence equivalence of oblique incidence geometries from wave propagation modeling. Based on the theory, we propose a practical method to correct for non-parallelism of the grating planes, and demonstrate its effectiveness with a polychromatic hard x-ray reflective interferometer.

  19. Multilayer and grazing incidence X-ray/EUV optics for astronomy and projection lithography; Proceedings of the Meeting, San Diego, CA, July 19-22, 1992

    NASA Technical Reports Server (NTRS)

    Hoover, Richard B. (Editor); Walker, Arthur B. C., Jr. (Editor)

    1993-01-01

    The present volume on multilayer and grazing incidence X-ray/EUV optics for astronomy and projection lithography discusses AXAF grazing incidence mirrors, the theory and high throughput optics of grazing incidence optics, multilayer mirror fabrication and characterization, and multilayer optics for X-ray projection lithography. Attention is given to the VETA-I X-ray detection system, a motion detection system for AXAF X-ray ground testing, image analysis of the AXAF VETA-I X-ray mirror, and optical constants from mirror reflectivities measured at synchrotrons. Topics discussed include the application of aberration theory to calculate encircled energy of Wolter I-II telescopes, W/C multilayers deposited on plastic films, nonspecular X-ray scattering from Si/Mo multilayers, and multilayer thin-film design as FUV polarizers. Also discussed are thin-film filter lifetesting results in the EUV, chromospheric and coronal observations with multilayer optics, present and future requirements of soft X-ray projection lithography, and the imaging Schwarzschild multilayer X-ray microscope.

  20. Slumping technique for the manufacturing of a representative x-ray grazing incidence mirror module for future space missions

    NASA Astrophysics Data System (ADS)

    Ghigo, Mauro; Proserpio, Laura; Basso, Stefano; Citterio, Oberto; Civitani, Marta M.; Pareschi, Giovanni; Salmaso, Bianca; Sironi, Giorgia; Spiga, Daniele; Tagliaferri, Giampiero; Vecchi, Gabriele; Zambra, Alberto; Parodi, Giancarlo; Martelli, Francesco; Gallieni, Daniele; Tintori, Matteo; Bavdaz, Marcos; Wille, Eric; Ferrario, Ivan; Burwitz, Vadim

    2013-09-01

    The Astronomical Observatory of Brera (INAF-OAB, Italy), with the financing support of the European Space Agency (ESA), has concluded a study regarding a glass shaping technology for the production of grazing incidence segmented x-ray optics. This technique uses a hot slumping phase, in which pressure is actively applied on thin glass foils being shaped, to form a cylindrical approximation of Wolter I x-ray segments, and a subsequent cold slumping phase, in which the final Wolter I profile is then freeze into the glass segments during their integration in elemental X-ray Optical Units. The final goal of this study was the manufacturing of a prototype containing a number of slumped pair plates (meaning parabola and hyperbola couples) having representative dimensions to be tested both in UV light and in x-rays at the Panter facility (Germany). In this paper, the INAF-OAB slumping technique, comprising a shaping step and an integration step is described, together with the results obtained on the manufactured prototype modules: the first prototype was aimed to test the ad-hoc designed and built semi-automatic Integration MAchine (IMA) and debug its control software. The most complete module comprises 40 slumped segments of Schott D263 glass type of dimension 200 mm x 200 mm and thickness of 0.4 mm, slumped on Zerodur K20 mould and stacked together through glued BK7 glass structural ribs to form the first entire x-ray optical module ever built totally composed by glass. A last prototype was aimed at demonstrate the use of Schott glass AF32 type instead of D263. In particular, a new hot slumping experimental set-up is described whose advantage is to permit a better contact between mould and glass during the shaping process. The integration procedure of the slumped segments into the elemental module is also reviewed.

  1. Grazing incidence neutron optics

    NASA Technical Reports Server (NTRS)

    Gubarev, Mikhail V. (Inventor); Ramsey, Brian D. (Inventor); Engelhaupt, Darell E. (Inventor)

    2012-01-01

    Neutron optics based on the two-reflection geometries are capable of controlling beams of long wavelength neutrons with low angular divergence. The preferred mirror fabrication technique is a replication process with electroform nickel replication process being preferable. In the preliminary demonstration test an electroform nickel optics gave the neutron current density gain at the focal spot of the mirror at least 8 for neutron wavelengths in the range from 6 to 20 .ANG.. The replication techniques can be also be used to fabricate neutron beam controlling guides.

  2. Grazing Incidence Neutron Optics

    NASA Technical Reports Server (NTRS)

    Gubarev, Mikhail V. (Inventor); Ramsey, Brian D. (Inventor); Engelhaupt, Darell E. (Inventor)

    2013-01-01

    Neutron optics based on the two-reflection geometries are capable of controlling beams of long wavelength neutrons with low angular divergence. The preferred mirror fabrication technique is a replication process with electroform nickel replication process being preferable. In the preliminary demonstration test an electroform nickel optics gave the neutron current density gain at the focal spot of the mirror at least 8 for neutron wavelengths in the range from 6 to 20.ANG.. The replication techniques can be also be used to fabricate neutron beam controlling guides.

  3. Modified small angle magnetization rotation method in multilayer magnetic microwires

    NASA Astrophysics Data System (ADS)

    Torrejón, J.; Badini, G.; Pirota, K.; Vázquez, M.

    2007-09-01

    The small angle magnetization rotation (SAMR) technique is a widely used method to quantify magnetostriction in elongated ultrasoft magnetic materials. In the present work, we introduce significant optimization of the method, particularly simplification of the required equipment, profiting of the very peculiar characteristics of a recently introduced family of multilayer magnetic microwires consisting of a soft magnetic core, insulating intermediate layer and a hard magnetic outer layer. The introduced modified SAMR method is used not only to determine the saturation magnetostriction constant of the soft magnetic nucleus but also the magnetoelastic and magnetostatic coupling. This new method has a great potential in multifunctional sensor applications.

  4. Calculations of transonic boattail flow at small angle of attack

    NASA Technical Reports Server (NTRS)

    Nakayama, A.; Chow, W. L.

    1979-01-01

    A transonic flow past a boattailed afterbody under a small angle of attack was examined. It is known that the viscous effect offers significant modifications of the pressure distribution on the afterbody. Thus, the formulation for the inviscid flow was based on the consideration of a flow past a nonaxisymmetric body. The full three dimensional potential equation was solved through numerical relaxation, and quasi-axisymmetric boundary layer calculations were performed to estimate the displacement effect. It was observed again that the viscous effects were not negligible. The trend of the final results agreed well with the experimental data.

  5. Emerging applications of small angle solution scattering in structural biology

    PubMed Central

    Chaudhuri, Barnali N

    2015-01-01

    Small angle solution X-ray and neutron scattering recently resurfaced as powerful tools to address an array of biological problems including folding, intrinsic disorder, conformational transitions, macromolecular crowding, and self or hetero-assembling of biomacromolecules. In addition, small angle solution scattering complements crystallography, nuclear magnetic resonance spectroscopy, and other structural methods to aid in the structure determinations of multidomain or multicomponent proteins or nucleoprotein assemblies. Neutron scattering with hydrogen/deuterium contrast variation, or X-ray scattering with sucrose contrast variation to a certain extent, is a convenient tool for characterizing the organizations of two-component systems such as a nucleoprotein or a lipid-protein assembly. Time-resolved small and wide-angle solution scattering to study biological processes in real time, and the use of localized heavy-atom labeling and anomalous solution scattering for applications as FRET-like molecular rulers, are amongst promising newer developments. Despite the challenges in data analysis and interpretation, these X-ray/neutron solution scattering based approaches hold great promise for understanding a wide variety of complex processes prevalent in the biological milieu. PMID:25516491

  6. Determining Equilibrium Lamellar Thickness by Small Angle Light Scattering

    NASA Astrophysics Data System (ADS)

    Li, Ying; Akpalu, Yvonne

    2002-03-01

    The crystallization and melting behavior of homogeneous copolymers of ethylene with butene and hexene is studied by small angle light scattering (SALS). We show that the final melting temperature (T_m^f), which corresponds to equilibrium between a melt with an overall ethylene sequence concentration (equal to the mole fraction of crystallizable units) and the thickest lamellar crystals can be determined from the SALS melting measurements. The T_m^f values, determined from the temperature at which the SALS HV or VV invariant vanishes during the melting, are substantially higher (7 to 10 °C) than those obtained from small angle x-ray (SAXS), wide angle x-ray scattering (WAXS) and differential scanning calorimetry (DSC). Thus our measurements indicate that SAXS, WAXS and DSC underestimate the lamellar thickness (l_f) of the largest crystals, a parameter necessary for estimating thermodynamic and kinetic parameters for ethylene copolymers. We also investigate T_m^f as a function of crystallization time (ranging from 1 hr to 72 hr) and heating rate. We discuss the implications of our SALS approach for estimating T_m^f, lf and lamellar morphological parameters from x-ray scattering.

  7. Grazing incidence liquid metal mirrors (GILMM) as the final optics for laser inertial fusion energy power plants

    SciTech Connect

    Moir, R W

    1999-06-25

    A thin film of liquid metal serves as a grazing incident liquid metal mirror (GILMM) for robust final optics of an inertial fusion energy (IFE) power plant. The amount of laser light the mirror can withstand, called the damage limit, of a sodium film 85{degree} from normal arbitrarily set by surface temperature rise of 200 C to limit liquid ablation is 57 J/cm{sup 2} normal to the beam for a 20 ns pulse and 1.3 J/cm{sup 2} for a 10 ps pulse of 0.35 pm light. Liquid aluminum can handle 106 J/cm{sup 2}. The damage limit actually should be set by avoiding liquid ablation due to the rapid surface heating which is expected to result in even higher temperatures rises than 200 C and even higher power densities. The liquid surface is kept flat to the required accuracy by a combination of polished substrate, adaptive optics, surface tension and low Reynolds number, laminar flow in the film. The film's substrate must be polished to {+-}0.015 m. Then surface tension keeps the surface smooth over short distances (<10 mm) and low Reynolds number laminar flow keeps the surface smooth by keeping the film thickness constant to less than {+-} 0.01 pm over long distance >10 mm. Adaptive (deformable) optics techniques keep the substrate flat to within {+-}0.06 {micro}m over 100 mm distance and {+-}0.6 {micro}m over 1,000 mm distances. The mirror can withstand the x-ray pulse when located 30 m away from the microexplosions of nominal yield of 400 MJ (50 MJ x rays) when Li is used but for higher atomic number liquids like Na and Al there may be too high a temperature rise forcing use of other x-ray attenuation methods such as xenon gas, which may be needed for first wall protecting anyway. The cumulative damage from neutrons causing warpage of the liquid film's substrate can be compensated by adaptive optics techniques giving the mirrors long life, perhaps 30 years. The GILMM should be applicable to both direct and indirect drive and pulse lengths appropriate to slow compression

  8. Grazing incidence liquid metal mirrors (GILMM) for radiation hardened final optics for laser inertial fusion energy power plants

    SciTech Connect

    Moir, R W

    1999-06-30

    A thin film of liquid metal is suggested as a grazing incident liquid metal mirror (GILMM) for robust final optics of a laser inertial fusion energy (IFE) power plant. The amount of laser light the mirror can withstand, called the damage limit, of a sodium film 85{sup o} from normal is calculated to be 57 J/cm{sup 2} normal to the beam for a 20 ns pulse and 1.3 J/cm{sup 2} for a 10 ps pulse of 0.35 {micro}m light (2 m{sup 2} and 90 m{sup 2} of mirror area per 100 kJ of laser energy at 20 ns and 10 ps, respectively). Feasibility relies on keep the liquid surface flat to the required accuracy by a combination of polished substrate, adaptive (deformable) optics, surface tension and low Reynolds number, laminar flow in the film. The film's substrate must be polished to {+-} 0.015 pm. Then surface tension keeps the surface smooth over short distances (<10 mm) and low Reynolds number laminar flow keeps the surface smooth by keeping the film thickness constant to less than + 0.01 w over long distance >10 mm. Adaptive optics techniques keep. the substrate flat to within {+-} 0.06 pm over 100 mm distance and {+-}0.6 {micro}m over 1000 mm distances. The mirror can stand the x-ray pulse when located 30 m away from the microexplosions of nominal yield of 400 MJ (50 MJ of X rays) when Li is used but for higher atomic number liquids like Na there may be too high a temperature rise forcing use of other x-ray attenuation methods such as attenuation by xenon gas. The cumulative damage from neutrons causing warpage of the liquid film's substrate can be compensated by adaptive optics techniques giving the mirrors long life, perhaps 30 years. The GILMM should be applicable to both direct and indirect drive and pulse lengths appropriate to slow compression ({approx}20 ns) or fast ignition ({approx}10 ps). For direct drive laser beams near the poles (70{sup o}, where 90{sup o} is vertical), stable thin films become more challenging. Proof of concept experiments are needed to verify the

  9. Measurement of two-dimensional small angle deviation with a prism interferometer

    SciTech Connect

    Chatterjee, Sanjib; Kumar, Y. Pavan

    2008-09-20

    A new technique for the measurement of two-dimensional small angular deviation is presented. A compound prism, which effectively produces a combination of two right-angled prisms in orthogonal directions, and plane reference surfaces have been utilized for the measurement of the orthogonal components of the angular tilt of an incident plane wavefront. Each orthogonal component of the angular tilt is separately measured from the angular rotation of the resultant wedge fringes between two plane wavefronts generated due to splitting of the incident plane wavefront by the corresponding set of right-angled prism and plane reference surface. The technique is shown to have high sensitivity for the measurement of small angle deviation. A monolithic prism interferometer, which is practically insensitive to vibration, is also proposed. Results obtained for the measurement of a known tilt angle are presented.

  10. A 10 Hz Grazing Incidence pumped Ni-like Mo laser at 18.9 nm with 150 mJ pump energy

    SciTech Connect

    Keenan, R; Dunn, J; Patel, P K; Price, D F; Smith, R F; Shlyaptsev, V N

    2004-09-30

    The first demonstration of the grazing incidence pumping (GRIP) scheme for laser-driven x-ray lasers (XRLs) is described utilizing 2-pulse pumping. A long pulse is incident normal to the target to produce a plasma with a particular density profile. Then a short pulse is incident at a grazing angle, chosen to optimally couple the short pulse laser energy into the specific density region where the inversion process will occur. The short pulse is simultaneously absorbed and refracted at a maximum electron density specified by the chosen pump angle then turns back into the gain region. The increased path length gives improved absorption allowing a reduction in the drive energy required for lasing. A Ni-like Mo XRL at 18.9 nm has been demonstrated with only 150 mJ total pump energy and a repetition rate of 10 Hz. We report high gains of 60 cm{sup -1} and the achievement of gain saturation for targets of 4 mm length.

  11. Structural investigations of fat fractals using small-angle scattering

    NASA Astrophysics Data System (ADS)

    Anitas, Eugen M.

    2015-01-01

    Experimental small-angle scattering (SAS) data characterized, on a double logarithmic scale, by a succession of power-law decays with decreasing values of scattering exponents, can be described in terms of fractal structures with positive Lebesgue measure (fat fractals). Here we present a theoretical model for fat fractals and show how one can extract structural information about the underlying fractal using SAS method, for the well known fractals existing in the literature: Vicsek and Menger sponge. We calculate analytically the fractal structure factor and study its properties in momentum space. The models allow us to obtain the fractal dimension at each structural level inside the fractal, the number of particles inside the fractal and about the most common distances between the center of mass of the particles.

  12. SMALL ANGLE CRAB COMPENSATION FOR LHC IR UPGRADE

    SciTech Connect

    CALAGA,R.; DORDA, U.; OHMI, D.; OIDE, K.; TOMAS, R.; ZIMMERMANN, F.

    2007-06-25

    A small angle (< 1 mrad) crab scheme is an attractive option for the LHC luminosity upgrade to recover the geometric luminosity loss from the finite crossing angle [I]. The luminosity loss increases steeply to unacceptable levels as the IP beta function is reduced below its nominal value (see Fig. 1 in Ref. [2]). The crab compensation in the LHC can be accomplished using only two sets of deflecting RF cavities, placed in collision-free straight sections of the LHC to nullify the effective crossing angles at IPI & IP5. We also explore a 400 MHz superconducting cavity design and discuss the pertinent RF challenges. We present IR optics configurations with low-angle crab crossing, study the beam-beam performance and proton-beam emittance growth in the presence of crab compensation, lattice errors, and crab RF noise sources.

  13. Small angle neutron scattering studies of vesicle stability

    SciTech Connect

    Mang, J.T.; Hjelm, R.P.

    1997-10-01

    Small angle neutron scattering (SANS) was used to investigate the structure of mixed colloids of egg yolk phosphatidylcholine (EYPC) with the bile salt, cholylglycine (CG), in D{sub 2}O as a function of pressure (P) and temperature (T). At atmospheric pressure, the system forms an isotropic phase of mixed, single bilayer vesicles (SLV`s). Increasing the external hydrostatic pressure brought about significant changes in particle morphology. At T = 25 C, application of a pressure of 3.5 MPa resulted in the collapse of the SLV`s. Further increase of P, up to 51.8 MPa, resulted in a transition from a phase of ordered (stacked), collapsed vesicles to one of stacked, ribbon-like particles. A similar collapse of the vesicles was observed at higher temperature (T = 37 C) with increasing P, but at this temperature, no ribbon phase was found at the highest pressure explored.

  14. Small-angle scattering study of Aspergillus awamori glycoprotein glucoamylase

    NASA Astrophysics Data System (ADS)

    Schmidt, A. E.; Shvetsov, A. V.; Kuklin, A. I.; Lebedev, D. V.; Surzhik, M. A.; Sergeev, V. R.; Isaev-Ivanov, V. V.

    2016-01-01

    Glucoamylase from fungus Aspergillus awamori is glycoside hydrolase that catalyzes the hydrolysis of α-1,4- and α-1,6-glucosidic bonds in glucose polymers and oligomers. This glycoprotein consists of a catalytic domain and a starch-binding domain connected by an O-glycosylated polypeptide chain. The conformation of the linker, the relative arrangement of the domains, and the structure of the full-length enzyme are unknown. The structure of the recombinant glucoamylase GA1 was studied by molecular modelling and small-angle neutron scattering (SANS) methods. The experimental SANS data provide evidence that glucoamylase exists as a monomer in solution and contains a glycoside component, which makes a substantial contribution to the scattering. The model of full-length glucoamylase, which was calculated without taking into account the effect of glycosylation, is consistent with the experimental data and has a radius of gyration of 33.4 ± 0.6 Å.

  15. A novel small-angle neutron scattering detector geometry.

    PubMed

    Kanaki, Kalliopi; Jackson, Andrew; Hall-Wilton, Richard; Piscitelli, Francesco; Kirstein, Oliver; Andersen, Ken H

    2013-08-01

    A novel 2π detector geometry for small-angle neutron scattering (SANS) applications is presented and its theoretical performance evaluated. Such a novel geometry is ideally suited for a SANS instrument at the European Spallation Source (ESS). Motivated by the low availability and high price of (3)He, the new concept utilizes gaseous detectors with (10)B as the neutron converter. The shape of the detector is inspired by an optimization process based on the properties of the conversion material. Advantages over the detector geometry traditionally used on SANS instruments are discussed. The angular and time resolutions of the proposed detector concept are shown to satisfy the requirements of the particular SANS instrument.

  16. A novel small-angle neutron scattering detector geometry

    PubMed Central

    Kanaki, Kalliopi; Jackson, Andrew; Hall-Wilton, Richard; Piscitelli, Francesco; Kirstein, Oliver; Andersen, Ken H.

    2013-01-01

    A novel 2π detector geometry for small-angle neutron scattering (SANS) applications is presented and its theoretical performance evaluated. Such a novel geometry is ideally suited for a SANS instrument at the European Spallation Source (ESS). Motivated by the low availability and high price of 3He, the new concept utilizes gaseous detectors with 10B as the neutron converter. The shape of the detector is inspired by an optimization process based on the properties of the conversion material. Advantages over the detector geometry traditionally used on SANS instruments are discussed. The angular and time resolutions of the proposed detector concept are shown to satisfy the requirements of the particular SANS instrument. PMID:24046504

  17. Small angle scattering from protein/sugar conjugates

    NASA Astrophysics Data System (ADS)

    Jackson, Andrew; White, John

    2006-11-01

    The Maillard reaction between free amine groups on proteins and sugars is well known. We have examined the effect of the reaction of the casein group of milk proteins with sugars on their nanoscale structure and aggregation. The small angle neutron scattering from beta casein and sodium caseinate and their sugar conjugates have been studied as a function of solution concentration. At high conjugate concentration (greater than ca. 5 mg/ml) the addition of sugar reduces supra-micellar aggregation of the protein whilst at lower concentration, where the protein is expected to be deaggregated already, little effect is seen. Guinier analysis of the scattering data show a radius of gyration of around 75 A˚ for beta casein in solution and around 80 A˚ for the sucrose conjugate.

  18. Experimental demonstration of a collinear triple pulse grazing-incidence pumping scheme for a transient collisional pumped x-ray laser

    NASA Astrophysics Data System (ADS)

    Künzel, S.; Cojocaru, G. V.; Gärtner, F.; Aurand, B.; Li, L.; Ursescu, D.; Zeitoun, Ph; Oliva, E.; Zielbauer, B.; Kuehl, T.; Fajardo, M.

    2016-11-01

    We present a nickel-like Molybdenum x-ray laser (XRL) based on the transient collisional excitation scheme. Extending the double grazing-incidence pumping scheme to a triple pulse scheme with a nanosecond pre-pulse and two consecutive 3 ps pulses the output power of the XRL can be ∼6 times increased compared to existing configurations, while using a relatively low total pump energy of 0.7 J. Additionally we show that this setup can be extended to a double stage, oscillator and amplifier stage, XRL.

  19. Monte-Carlo simulation of an ultra small-angle neutron scattering instrument based on Soller slits

    SciTech Connect

    Rieker, T.; Hubbard, P.

    1997-09-01

    Monte Carlo simulations are used to investigate an ultra small-angle neutron scattering instrument for use at a pulsed source based on a Soller slit collimator and analyzer. The simulations show that for a q{sub min} of {approximately}le-4 {angstrom}{sup -1} (15 {angstrom} neutrons) a few tenths of a percent of the incident flux is transmitted through both collimators at q=0.

  20. Design of axisymmetric multi-mirror grazing incidence system to increase the numerical aperture of neutron and X-ray microscopes

    NASA Astrophysics Data System (ADS)

    Aoki, Sadao; Watanabe, Norio; Asami, Hiroshi; Shimada, Akihiro

    2016-04-01

    An axisymmetric multi-mirror system for neutron and X-ray microscopes is proposed to increase their numerical aperture and collection efficiency. A Wolter type-I mirror is used as the basis of the multi-mirror system at grazing incidence. The addition of an even number of hyperboloid mirrors to the Wolter type-I mirror can satisfy both an equal optical path length and Abbe's sine condition. The numerical aperture increases in proportion to the number of mirrors. The optical parameters of the system with four tandem mirrors are calculated for neutrons and X-rays with a wavelength of 0.4 nm by assuming that the average grazing angle of incidence is 5.4 mrad and the magnification is 10. The inner diameters of the mirrors are limited to <10 mm considering the total length of the optical system. Tolerance of off-axis distance was calculated using a ray-tracing computer simulation. Ray tracing shows that a blur size <14 nm will be possible at an off-axis displacement of 10 μm.

  1. Multiple scattering in grazing-incidence X-ray diffraction: impact on lattice-constant determination in thin films.

    PubMed

    Resel, Roland; Bainschab, Markus; Pichler, Alexander; Dingemans, Theo; Simbrunner, Clemens; Stangl, Julian; Salzmann, Ingo

    2016-05-01

    Dynamical scattering effects are observed in grazing-incidence X-ray diffraction experiments using an organic thin film of 2,2':6',2''-ternaphthalene grown on oxidized silicon as substrate. Here, a splitting of all Bragg peaks in the out-of-plane direction (z-direction) has been observed, the magnitude of which depends both on the incidence angle of the primary beam and the out-of-plane angle of the scattered beam. The incident angle was varied between 0.09° and 0.25° for synchrotron radiation of 10.5 keV. This study reveals comparable intensities of the split peaks with a maximum for incidence angles close to the critical angle of total external reflection of the substrate. This observation is rationalized by two different scattering pathways resulting in diffraction peaks at different positions at the detector. In order to minimize the splitting, the data suggest either using incident angles well below the critical angle of total reflection or angles well above, which sufficiently attenuates the contributions from the second scattering path. This study highlights that the refraction of X-rays in (organic) thin films has to be corrected accordingly to allow for the determination of peak positions with sufficient accuracy. Based thereon, a reliable determination of the lattice constants becomes feasible, which is required for crystallographic structure solutions from thin films.

  2. Multiple scattering in grazing-incidence X-ray diffraction: impact on lattice-constant determination in thin films.

    PubMed

    Resel, Roland; Bainschab, Markus; Pichler, Alexander; Dingemans, Theo; Simbrunner, Clemens; Stangl, Julian; Salzmann, Ingo

    2016-05-01

    Dynamical scattering effects are observed in grazing-incidence X-ray diffraction experiments using an organic thin film of 2,2':6',2''-ternaphthalene grown on oxidized silicon as substrate. Here, a splitting of all Bragg peaks in the out-of-plane direction (z-direction) has been observed, the magnitude of which depends both on the incidence angle of the primary beam and the out-of-plane angle of the scattered beam. The incident angle was varied between 0.09° and 0.25° for synchrotron radiation of 10.5 keV. This study reveals comparable intensities of the split peaks with a maximum for incidence angles close to the critical angle of total external reflection of the substrate. This observation is rationalized by two different scattering pathways resulting in diffraction peaks at different positions at the detector. In order to minimize the splitting, the data suggest either using incident angles well below the critical angle of total reflection or angles well above, which sufficiently attenuates the contributions from the second scattering path. This study highlights that the refraction of X-rays in (organic) thin films has to be corrected accordingly to allow for the determination of peak positions with sufficient accuracy. Based thereon, a reliable determination of the lattice constants becomes feasible, which is required for crystallographic structure solutions from thin films. PMID:27140152

  3. Multiple scattering in grazing-incidence X-ray diffraction: impact on lattice-constant determination in thin films

    PubMed Central

    Resel, Roland; Bainschab, Markus; Pichler, Alexander; Dingemans, Theo; Simbrunner, Clemens; Stangl, Julian; Salzmann, Ingo

    2016-01-01

    Dynamical scattering effects are observed in grazing-incidence X-ray diffraction experiments using an organic thin film of 2,2′:6′,2′′-ternaphthalene grown on oxidized silicon as substrate. Here, a splitting of all Bragg peaks in the out-of-plane direction (z-direction) has been observed, the magnitude of which depends both on the incidence angle of the primary beam and the out-of-plane angle of the scattered beam. The incident angle was varied between 0.09° and 0.25° for synchrotron radiation of 10.5 keV. This study reveals comparable intensities of the split peaks with a maximum for incidence angles close to the critical angle of total external reflection of the substrate. This observation is rationalized by two different scattering pathways resulting in diffraction peaks at different positions at the detector. In order to minimize the splitting, the data suggest either using incident angles well below the critical angle of total reflection or angles well above, which sufficiently attenuates the contributions from the second scattering path. This study highlights that the refraction of X-rays in (organic) thin films has to be corrected accordingly to allow for the determination of peak positions with sufficient accuracy. Based thereon, a reliable determination of the lattice constants becomes feasible, which is required for crystallographic structure solutions from thin films. PMID:27140152

  4. Practical applications of small-angle neutron scattering.

    PubMed

    Hollamby, Martin J

    2013-07-14

    Recent improvements in beam-line accessibility and technology have led to small-angle neutron scattering (SANS) becoming more frequently applied to materials problems. SANS has been used to study the assembly, dispersion, alignment and mixing of nanoscale condensed matter, as well as to characterise the internal structure of organic thin films, porous structures and inclusions within steel. Using time-resolved SANS, growth mechanisms in materials systems and soft matter phase transitions can also be explored. This review is intended for newcomers to SANS as well as experts. Therefore, the basic knowledge required for its use is first summarised. After this introduction, various examples are given of the types of soft and hard matter that have been studied by SANS. The information that can be extracted from the data is highlighted, alongside the methods used to obtain it. In addition to presenting the findings, explanations are provided on how the SANS measurements were optimised, such as the use of contrast variation to highlight specific parts of a structure. Emphasis is placed on the use of complementary techniques to improve data quality (e.g. using other scattering methods) and the accuracy of data analysis (e.g. using microscopy to separately determine shape and size). This is done with a view to providing guidance on how best to design and analyse future SANS measurements on materials not listed below. PMID:23552189

  5. Small angle x-ray scattering with edge-illumination

    PubMed Central

    Modregger, Peter; Cremona, Tiziana P.; Benarafa, Charaf; Schittny, Johannes C.; Olivo, Alessandro; Endrizzi, Marco

    2016-01-01

    Sensitivity to sub-pixel sample features has been demonstrated as a valuable capability of phase contrast x-ray imaging. Here, we report on a method to obtain angular-resolved small angle x-ray scattering distributions with edge-illumination- based imaging utilizing incoherent illumination from an x-ray tube. Our approach provides both the three established image modalities (absorption, differential phase and scatter strength), plus a number of additional contrasts related to unresolved sample features. The complementarity of these contrasts is experimentally validated by using different materials in powder form. As a significant application example we show that the extended complementary contrasts could allow the diagnosis of pulmonary emphysema in a murine model. In support of this, we demonstrate that the properties of the retrieved scattering distributions are consistent with the expectation of increased feature sizes related to pulmonary emphysema. Combined with the simplicity of implementation of edge-illumination, these findings suggest a high potential for exploiting extended sub-pixel contrasts in the diagnosis of lung diseases and beyond. PMID:27491917

  6. Small-angle neutron scattering at pulsed spallation sources

    SciTech Connect

    Seeger, P.A.; Hjelm, R.P. Jr.

    1990-01-01

    The importance of small-angle neutron scattering (SANS) in biological, chemical, physical, and engineering research mandates that all intense neutron sources be equipped with SANS instruments. Four existing instruments are described, and the general differences between pulsed-source and reactor-based instrument designs are discussed. The basic geometries are identical, but dynamic range is achieved by using a broad band of wavelengths (with time-of-flight analysis) rather than by moving the detector. This allows a more optimized collimation system. Data acquisition requirements at a pulsed source are more severe, requiring large, fast histogramming memories. Data reduction is also more complex, as all wave length-dependent and angle-dependent backgrounds and non-linearities must be accounted for before data can be transformed to intensity vs Q. A comparison is shown between the Los Alamos pulsed instrument and D-11 (Institute Laue-Langevin), and examples from the four major topics of the conference are shown. The general conclusion is that reactor-based instruments remain superior at very low Q or if only a narrow range of Q is required, but that the current generation of pulsed-source instruments is competitive at moderate Q and may be faster when a wide range of Q is required. In principle, a user should choose which facility to use on the basis of optimizing the experiment; in practice the tradeoffs are not severe and the choice is usually made on the basis of availability.

  7. New Very Small Angle Neutron Scattering (VSANS) Instrument

    NASA Astrophysics Data System (ADS)

    Van Every, E.; Deyhim, A.; Kulesza, J.

    2016-09-01

    The design of a new Very Small Angle Neutron Scattering (VSANS) Instrument for use in National Institute of Standards And Technology (NIST) will be discussed. This instrument is similar to a shorter instrument we designed and delivered to ANSTO in Australia called the Bilby SANS instrument. The NIST VSANS and the ANSTO Bilby SANS instruments have very similar dimensions for length and diameter and have similar requirements for internal detector motion, top access port, walkway supports, and ports; however, the Bilby SANS instrument vacuum requirement was lower (7.5×10-5 Torr) and the entire (60,000 pound) vessel was required to move 1.5 meters on external rails with a repeatability of 100 um, which ADC achieved. The NIST VSANS length is 24 meter, internal diameter 2.3 meter with three internal carriages. The NIST VSANS instrument, which covers the usual SANS range will also allow configuration to cover the range between q ∼⃒ 10-4 A-1 to 10-3 A-1 with a sample beam current of (104 neutrons/s). The key requirements are a second position-sensitive detector system having a 1 mm pixel size and a longer sample-detector flight path of 20 m (i.e., a 40 m instrument).

  8. Small-angle scattering model for multilamellar vesicles

    SciTech Connect

    Frielinghaus, Henrich

    2007-11-15

    A small-angle neutron-x-ray-light-scattering model for multilamellar vesicles is developed on the basis of a simple geometry. N spherical shells with radii of an arithmetic series are allowed for displacements {delta}R which are limited by {delta}R

  9. Magnetic small-angle neutron scattering of bulk ferromagnets.

    PubMed

    Michels, Andreas

    2014-09-24

    We summarize recent theoretical and experimental work in the field of magnetic small-angle neutron scattering (SANS) of bulk ferromagnets. The response of the magnetization to spatially inhomogeneous magnetic anisotropy and magnetostatic stray fields is computed using linearized micromagnetic theory, and the ensuing spin-misalignment SANS is deduced. Analysis of experimental magnetic-field-dependent SANS data of various nanocrystalline ferromagnets corroborates the usefulness of the approach, which provides important quantitative information on the magnetic-interaction parameters such as the exchange-stiffness constant, the mean magnetic anisotropy field, and the mean magnetostatic field due to jumps ΔM of the magnetization at internal interfaces. Besides the value of the applied magnetic field, it turns out to be the ratio of the magnetic anisotropy field Hp to ΔM, which determines the properties of the magnetic SANS cross-section of bulk ferromagnets; specifically, the angular anisotropy on a two-dimensional detector, the asymptotic power-law exponent, and the characteristic decay length of spin-misalignment fluctuations. For the two most often employed scattering geometries where the externally applied magnetic field H0 is either perpendicular or parallel to the wave vector k0 of the incoming neutron beam, we provide a compilation of the various unpolarized, half-polarized (SANSPOL), and uniaxial fully-polarized (POLARIS) SANS cross-sections of magnetic materials. PMID:25180625

  10. Small angle x-ray scattering with edge-illumination

    NASA Astrophysics Data System (ADS)

    Modregger, Peter; Cremona, Tiziana P.; Benarafa, Charaf; Schittny, Johannes C.; Olivo, Alessandro; Endrizzi, Marco

    2016-08-01

    Sensitivity to sub-pixel sample features has been demonstrated as a valuable capability of phase contrast x-ray imaging. Here, we report on a method to obtain angular-resolved small angle x-ray scattering distributions with edge-illumination- based imaging utilizing incoherent illumination from an x-ray tube. Our approach provides both the three established image modalities (absorption, differential phase and scatter strength), plus a number of additional contrasts related to unresolved sample features. The complementarity of these contrasts is experimentally validated by using different materials in powder form. As a significant application example we show that the extended complementary contrasts could allow the diagnosis of pulmonary emphysema in a murine model. In support of this, we demonstrate that the properties of the retrieved scattering distributions are consistent with the expectation of increased feature sizes related to pulmonary emphysema. Combined with the simplicity of implementation of edge-illumination, these findings suggest a high potential for exploiting extended sub-pixel contrasts in the diagnosis of lung diseases and beyond.

  11. Small Angle Neutron Scattering of Solutions of Arborescent Graft Polymers

    NASA Astrophysics Data System (ADS)

    Choi, Sangwook; Briber, R. M.; Bauer, B. J.; Topp, Andreas; Gauthier, Mario

    1998-03-01

    Arborescent graft polymers are branched macromolecules resulting from successive cycles of chloromethylation and anionic grafting reactions. Small angle neutron scattering (SANS) was used to measure the size and shape of arborescent graft polymers in solution. Guinier plots were used to analyze the data at small q. The radius of gyration of arborescent graft polymers was found to be almost independent of temperature as the solution was cooled towards the phase separation temperature. The optical cloud point temperature was found to be 15 ^0C. At the phase separation temperature two peaks were observed in the I versus q SANS data. The first peak is due to the interference between molecules while the second peak comes from the single particle form factor. The value of q at the peak from the form factor was almost constant as temperature was changed from 40 ^0C to 20 ^0C. The peak position shifted to higher q at the phase separation temperature. This indicates that the size of molecules decreased as the molecules began to aggregate below the phase separation temperature. The value of A2 for arborescent graft polymers was found to be independent of temperature and close to zero.

  12. Characterization of photosynthetic supramolecular assemblies using small angle neutron scattering

    SciTech Connect

    Tiede, D.M.; Marone, P.; Wagner, A.M.; Thiyagarajan, P.

    1995-12-31

    We are using small angle neutron scattering (SANS) to resolve structural features of supramolecular assemblies of photosynthetic proteins in liquid and frozen solutions. SANS resolves the size, shape, and structural homogeneity of macromolecular assemblies in samples identical to those used for spectroscopic assays of photosynthetic function. Likely molecular structures of the supramolecular assemblies can be identified by comparing experimental scattering data with scattering profiles calculated for model supramolecular assemblies built from crystal structures of the individual proteins. SANS studies of the Rhodobacter sphaeroides reaction center, RC, presented here, show that the detergent solubilized RC exists in a variety of monomeric and aggregation states. The distribution between monomer and aggregate was found to depend strongly upon detergent, temperature and nature of additives, such as ethylene glycol used for low temperature spectroscopy and polyethylene glycol used for crystallization. Likely aggregate structures are being identified by fitting the experimental scattering profiles with those calculated for model aggregates built-up using the RC crystal structure. This work establishes the foundation for using SANS to identify intermediates in the RC crystallization pathways, and for determining likely structures of complexes formed between the RC and its physiological reaction partners, cytochrome c, and the LHI antenna complex.

  13. Small angle x-ray scattering with edge-illumination.

    PubMed

    Modregger, Peter; Cremona, Tiziana P; Benarafa, Charaf; Schittny, Johannes C; Olivo, Alessandro; Endrizzi, Marco

    2016-01-01

    Sensitivity to sub-pixel sample features has been demonstrated as a valuable capability of phase contrast x-ray imaging. Here, we report on a method to obtain angular-resolved small angle x-ray scattering distributions with edge-illumination- based imaging utilizing incoherent illumination from an x-ray tube. Our approach provides both the three established image modalities (absorption, differential phase and scatter strength), plus a number of additional contrasts related to unresolved sample features. The complementarity of these contrasts is experimentally validated by using different materials in powder form. As a significant application example we show that the extended complementary contrasts could allow the diagnosis of pulmonary emphysema in a murine model. In support of this, we demonstrate that the properties of the retrieved scattering distributions are consistent with the expectation of increased feature sizes related to pulmonary emphysema. Combined with the simplicity of implementation of edge-illumination, these findings suggest a high potential for exploiting extended sub-pixel contrasts in the diagnosis of lung diseases and beyond. PMID:27491917

  14. Physical characteristics of human transferrin from small angle neutron scattering.

    PubMed Central

    Martel, P; Kim, S M; Powell, B M

    1980-01-01

    The technique of small angle neutron scattering has been used to determine the molecular shape, the volume, and the molecular weight of pooled human transferrin in an aqueous solution isotonic with blood. Analysis of the measurements assuming a spheroidal molecular shape indicates that an oblate spheroid with semi-axes of length 46.6 +/- 1.4, 46.6 +/- 1.4 and 15.8 +/- 3.8 A, and a molecular volume of (144 +/- 45) X 10(3) A3 is the best simple approximation to the shape of the transferrin molecule. The radius of gyration, Rg, determined from a Guinier plot is 30.25 +/- 0.49 A, in agreement with Rg calculated for the oblate spheroidal shape. The molecular weight is determined to be (75 +/- 5) X 10(3). The shape-independent molecular volume is found to be (98 +/- 10) X 10(3) A3. The difference in the two volumes suggests that transferrin is not a uniform spheroid but may have a more complex shape. PMID:7260293

  15. Practical applications of small-angle neutron scattering.

    PubMed

    Hollamby, Martin J

    2013-07-14

    Recent improvements in beam-line accessibility and technology have led to small-angle neutron scattering (SANS) becoming more frequently applied to materials problems. SANS has been used to study the assembly, dispersion, alignment and mixing of nanoscale condensed matter, as well as to characterise the internal structure of organic thin films, porous structures and inclusions within steel. Using time-resolved SANS, growth mechanisms in materials systems and soft matter phase transitions can also be explored. This review is intended for newcomers to SANS as well as experts. Therefore, the basic knowledge required for its use is first summarised. After this introduction, various examples are given of the types of soft and hard matter that have been studied by SANS. The information that can be extracted from the data is highlighted, alongside the methods used to obtain it. In addition to presenting the findings, explanations are provided on how the SANS measurements were optimised, such as the use of contrast variation to highlight specific parts of a structure. Emphasis is placed on the use of complementary techniques to improve data quality (e.g. using other scattering methods) and the accuracy of data analysis (e.g. using microscopy to separately determine shape and size). This is done with a view to providing guidance on how best to design and analyse future SANS measurements on materials not listed below.

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

    NASA Astrophysics Data System (ADS)

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

    2014-09-01

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

  17. Diffraction by a strip at almost grazing angle

    NASA Astrophysics Data System (ADS)

    Andronov, Ivan V.; Bouche, Daniel P.

    2016-07-01

    The problem of high-frequency diffraction by a soft strip at almost grazing incidence is considered. By using the parabolic equation method, and variable separation in elliptical coordinates, we derive the two terms asymptotic approximation of the solution. First we consider the boundary layer near the surface of the strip and derive an asymptotic representation for the velocities on the surface. Then we apply Green's formula to derive the asymptotic representation for the far field. Both asymptotic representations in the boundary layer and for the far field are expressed in the form of rapidly converging integrals containing Whittaker or Coulomb wave functions. The approximation for the total scattering cross-section is checked to match to known asymptotic results: the physical optics approximation for the not too small angles of incidence on one side and the asymptotic expression for the limiting case of grazing incidence on the other side. Simple approximations for the total scattering cross-section in powers of the scaled angle are derived.

  18. Internal structure of copper(II)-phthalocyanine thin films on SiO{sub 2}/Si substrates investigated by grazing incidence x-ray reflectometry

    SciTech Connect

    Brieva, A. C.; Jenkins, T. E.; Jones, D. G.; Stroessner, F.; Evans, D. A.; Clark, G. F.

    2006-04-01

    The internal structure of copper(II)-phthalocyanine (CuPc) thin films grown on SiO{sub 2}/Si by organic molecular beam deposition has been studied by grazing incidence x-ray reflectometry (GIXR) and atomic force microscopy. The electronic density profile is consistent with a structure formed by successive monolayers of molecules in the {alpha} form with the b axis lying in the substrate surface plane. The authors present an electronic density profile model of CuPc films grown on SiO{sub 2}/Si. The excellent agreement between the model and experimental data allows postdeposition monitoring of the internal structure of the CuPc films with the nondestructive GIXR technique, providing a tool for accurate control of CuPc growth on silicon-based substrates. In addition, since the experiments have been carried out ex situ, they show that these structures can endure ambient conditions.

  19. Oxide thickness dependence of swift heavy ion-induced surface tracks formation in silicon dioxide on silicon structures at grazing incidence

    SciTech Connect

    Carvalho, A. M. J. F.; Touboul, A. D.; Marinoni, M.; Ramonda, M.; Guasch, C.; Saigne, F.; Bonnet, J.; Gasiot, J.

    2007-12-15

    The influence of the oxide thickness in the surface tracks formation in thin silicon dioxide layered-silicon substrate (SiO{sub 2}-Si) irradiated with swift heavy ion is dealt with. In this respect, SiO{sub 2}-Si samples with different oxide thicknesses have been characterized using atomic force microscopy before and after 7.51 MeV/u Xe ion irradiation at a grazing incident angle of 1 deg. relative to the surface plane. Experimental evidence of the existence of a threshold thickness in the formation of swift heavy ion-induced surface tracks has been addressed and discussed according to the thermal spike theory. This experimental upshot can be helpful when assessing metal-oxide-semiconductor ultrathin-gate oxide reliability issues and for growth of silicon-based nanostructures.

  20. An ultrahigh-density digital data read-out method based on grazing-angle incidence x-ray backscattering diffraction

    NASA Astrophysics Data System (ADS)

    Bezirganyan, Hakob Akop P.; Bezirganyan, Hayk H., Jr.; Bezirganyan, Siranush E.; Bezirganyan, Petros H., Jr.; Mossikyan, Youri G.

    2005-10-01

    An ultrahigh-density x-ray optical data storage medium useful for terabyte-scale memory applications and named X-ROM is proposed. The X-ROM is a nanocrystalline semiconductor layer, in which non-diffracting nanosized reflectors of x-radiation are embedded. The procedure of digital data read-out from the X-ROM can be performed e.g. by the application of a grazing-angle incidence x-ray backscattering diffraction technique under conditions of specular vacuum wave suppression. The surface storage digital data density of the proposed device, with 20 nm/bit linear size of the single-bit domain, is higher by two orders of magnitude than the volumetric data density actually achieved for a three-dimensional optical data storage medium.

  1. Small angle light scattering characterization of single micrometric particles in microfluidic flows

    NASA Astrophysics Data System (ADS)

    Dannhauser, David; Romeo, Giovanni; Causa, Filippo; Netti, Paolo A.

    2013-04-01

    A CCD-camera based small angle light scattering (SALS) apparatus has been used to characterize single micrometric particles flowing in a micro-channel. The measured scattering vector spans the range 2x10-2 - 6:8x101μm-1. The incident laser light is collimated to a spot of about 50 μm in diameter at the sample position with a divergence lower than 0.045 rad. Such small collimated laser beam opens the possibility to perform on-line SALS of micron-sized particles flowing in micro-channels. By properly designing the micro-channel and using a viscoelastic liquid as suspending medium we are able to realize a precise 3D focusing of the target particles. The forward scattering emitted from the particle is collected by a lens with high numerical aperture. At the focal point of that lens a homemade beam stop is blocking the incident light. Finally, a second lens maps the scattered light on the CCD sensor, allowing to obtain far field images on short distances. Measurements with mono-disperse polystyrene particles, both in quiescent and in-flow conditions have been realized. Experiments in-flow allow to measure the single particle scattering. Results are validated by comparison with calculations based on the Lorenz-Mie theory. The quality of the measured intensity profiles confirms the possibility to use our apparatus in real multiplex applications, with particles down to 1 μm in radius.

  2. Multiple excitation of Fuchs-Kliewer phonons by Ne⁺ ions back-scattered by the LiF(100) surface at grazing incidence.

    PubMed

    Lucas, A A; Sunjic, M; Benedek, G

    2013-09-01

    An analytic model is developed to describe the inelastic processes occurring when keV Ne(+) ions are scattered at grazing incidence by the (100) surface of LiF. The large energy losses (up to 30 eV) of the reflected Ne(+) particles reported by Borisov et al (1999 Phys. Rev. Lett. 83 5378) are shown to arise specifically from the long-range coupling between the projectiles and the so-called Fuchs-Kliewer (FK) optical phonons of LiF whose fields extend far outside the surface. The strength of the coupling is estimated, allowing one to compute the average number of excited FK phonon quanta (ħωS = 0.071 eV) and hence the mean energy losses. For emerging, neutralized Ne(0), a distinct energy loss mechanism is shown to occur, namely the excitation of FK phonons and other types of surface collective modes associated with the screening of the F(0) 'hole' left behind by the neutralization process. This mechanism contributes a large fraction of the loss, additional to that suffered by the incident Ne(+) ion. The model explains the experimental observations quantitatively (1999 Phys. Rev. Lett. 83 5378). The paper ends with a discussion of the large energy broadening of the observed loss peaks.

  3. EDITORIAL Proceedings of the XIV International Conference on Small-Angle Scattering, SAS-2009

    NASA Astrophysics Data System (ADS)

    Ungar, Goran; Heenan, Richard

    2010-10-01

    There are 52 papers in these Proceedings. The papers are divided into 10 thematic sections and a section for invited papers and reviews. The sections and the respective section editors are given below. Section Editor(s) Invited Papers and Reviews Peter Griffiths, Wim Bras, Rudolf Winter Beamlines and Instrumentation Elliot Gilbert, Wim Bras, Nigel Rhodes Theory, Data processing and Modelling Jan Skov Pedersen, Carlo Knupp Biological Systems and Membranes Richard Heenan, Cameron Neylon Ceramics, Glasses and Porous Materials Rudolf Winter Colloids and Solutions Peter Griffiths Hierarchical Structures and Fibres Steve Eichhorn, Karen Edler Metallic and Magnetic Systems Armin Hoell Polymers Patrick Fairclough Time resolved Diffraction, Kinetic and Dynamical Studies João Cabral, Christoph Rau We are grateful to all section editors and the many anonymous referees for their invaluable effort which made the publication of the Proceedings possible. The refereeing process was strict and thorough, some papers were rejected and most were improved. The resulting compendium gives a good overview of recent developments in small-angle X-ray and neutron scattering theory, application, methods of analysis and instrumentation. Thus it should be a useful source of reference for a number of years to come. The papers are a good reflection of the material presented at the meeting. Because of the general high quality of the articles, it was difficult to decide which to highlight and be fair to all contributors. The following in particular have caught the attention of the editors. Highlighted papers A statistical survey of publications reporting the application of SAXS and SANS by Aldo Craievich (paper 012003) is recommended reading for anyone needing convincing about the vibrancy of this scientific field and the ever expanding use of these techniques. Two aspects of coherent X-ray scattering, made available by the advent of the 3rd generation synchrotron sources, are discussed in the

  4. Multi-use high/low-temperature and pressure compatible portable chamber for in situ grazing-incidence X-ray scattering studies.

    PubMed

    Ferrer, Pilar; Rubio-Zuazo, Juan; Heyman, Catherine; Esteban-Betegón, Fatima; Castro, Germán R

    2013-05-01

    The multipurpose portable ultra-high-vacuum-compatible chamber described in detail in this article has been designed to carry out grazing-incidence X-ray scattering techniques on the BM25-SpLine CRG beamline at the ESRF. The chamber has a cylindrical form, built on a 360° beryllium double-ended conflate flange (CF) nipple. The main advantage of this chamber design is the wide sample temperature range, which may be varied between 60 and 1000 K. Other advantages of using a cylinder are that the wall thickness is reduced to a minimum value, keeping maximal solid angle accessibility and keeping wall absorption of the incoming X-ray beam constant. The heat exchanger is a customized compact liquid-nitrogen (LN2) continuous-flow cryostat. LN2 is transferred from a storage Dewar through a vacuum-isolated transfer line to the heat exchanger. The sample is mounted on a molybdenum support on the heat exchanger, which is equipped with a BORALECTRIC heater element. The chamber versatility extends to the operating pressure, ranging from ultra-high vacuum (<10(-10) mbar) to high pressure (up to 3 × 10(3) mbar). In addition, it is equipped with several CF ports to allocate auxiliary components such as capillary gas-inlet, viewports, leak valves, ion gun, turbo pump, etc., responding to a large variety of experiment requirements. A movable slits set-up has been foreseen to reduce the background and diffuse scattering produced at the beryllium wall. Diffraction data can be recorded either with a point detector or with a bi-dimensional CCD detector, or both detectors simultaneously. The system has been designed to carry out a multitude of experiments in a large variety of environments. The system feasibility is demonstrated by showing temperature-dependence grazing-incidence X-ray diffraction and conductivity measurements on a 20 nm-thick La0.7Ca0.3MnO3 thin film grown on a SrTiO3(001) substrate. PMID:23592627

  5. X-ray diffraction from polycrystalline multilayers in grazing-incidence geometry: Measurement of crystallite size depth distribution

    SciTech Connect

    Fewster, P.F.; Andrew, N.L.; Holy, V.; Barmak, K.

    2005-11-01

    A method to measure the crystallite size and its distribution as a function of depth in multilayer thin films is described. The principle relies on the idea that when x-rays are scattered at an interface the incident and scattered waves create a standing wave whose periodicity can be varied and thereby enhance the scattering at certain depths. Practical examples of this method are given for Nb/Al periodic multilayers, one of which indicates considerable macrostrain for the surface layer and a variation in microstrain as a function of depth. The theoretical modeling of the scattering process is presented, which includes the influence of the general density modulation and interfacial roughness. Both these contributions are shown to be necessary to account for the experimental scattering profiles.

  6. Mapping the local nanostructure inside a specimen by tomographic small-angle x-ray scattering

    SciTech Connect

    Schroer, C.G.; Kuhlmann, M.; Roth, S.V.; Gehrke, R.; Stribeck, N.; Almendarez-Camarillo, A.; Lengeler, B.

    2006-04-17

    Small-angle x-ray scattering is combined with scanning microtomography to reconstruct the small-angle diffraction pattern in the direction of the tomographic rotation axis at each location on a virtual section through a specimen. These data yield information about the local nanoscale structure of the sample. With rotational symmetry present in the diffraction patterns, e.g., for isotropic or fiber-textured scatterers, the full reciprocal space information in the small-angle scattering regime can be reconstructed at each location inside the specimen. The method is illustrated investigating a polymer rod made by injection molding.

  7. Comparative studies on the influence of beta-sitosterol and stigmasterol on model sphingomyelin membranes: a grazing-incidence X-ray diffraction study.

    PubMed

    Hac-Wydro, Katarzyna; Flasiński, Michał; Broniatowski, Marcin; Dynarowicz-Łatka, Patrycja; Majewski, Jarosław

    2010-05-27

    Sterols are essential constituents of membranes, both in the plant world and in human organisms. Therefore, their activity on model lipid systems has systematically been studied. Despite intensive investigations, differences in the effect induced by beta-sitosterol (beta-sito) and stigmasterol (stigma) (two major phytosterols) are very controversial and still under debate. To compare the influence of these compounds on model membranes, we have performed grazing incidence X-ray diffraction (GIXD) experiments on phytosterol/sphingomyelin (Sph) monolayers. The analysis of the X-ray scattering and the resulting in-plane parameters provided information on the lateral organization of pure lipid films and the mixed systems. The obtained results prove a nonideal mixing between the investigated lipids in the monolayers and the existence of strong interactions between phytosterols and Sph. Both the plant sterols incorporated into sphingolipid film condense the monolayer and order Sph chains. The results of GIXD experiments, compared with those obtained previously from Langmuir monolayer studies allowed us to observe the comparable influence of beta-sito and stigma on model membrane organization.

  8. First measurements of highly ionized impurity emission distribution by grazing-incidence flat-field extreme ultraviolet spectrometer in HL-2A.

    PubMed

    Cui, Zhengying; Dong, Chunfeng; Zhou, Hangyu; Morita, Shigeru; Sun, Ping; Fu, Bingzhong; Lu, Ping; Ding, Xuantong; Yang, Qingwei; Duan, Xuru

    2014-11-01

    A space-resolved grazing-incidence flat-field extreme ultraviolet (EUV) spectrometer has been developed in the HL-2A tokamak to measure vertical impurity emission profiles with simultaneous spectral, temporal, and spatial resolution. The spectrometer working in the wavelength range of 30-500 Å has been equipped with a gold-coated varied-line-spacing holographic grating with curvature of 5606 mm and a back illuminated charge-coupled device with size of 6.6 × 26.6 mm(2) (255 × 1024 pixels). A lower half of the HL-2A plasma with averaged minor radius of 40 cm is observed when the spectrometer with horizontal dispersion is placed at a distance of 7.5 m away from the plasma center. An excellent spatial resolution of 12 mm is achieved when a space-resolved slit with vertical width of 0.5 mm is adopted. The radial profiles of intrinsic impurities in several ionization stages have been measured with high throughput and extremely low stray light. PMID:25430333

  9. High-resolution grazing-incidence grating spectrometer for temperature measurements of low-Z ions emitting in the 100-300 Å spectral band.

    PubMed

    Widmann, K; Beiersdorfer, P; Magee, E W; Boyle, D P; Kaita, R; Majeski, R

    2014-11-01

    We have constructed a high-resolution grazing-incidence spectrometer designed for measuring the ion temperature of low-Z elements, such as Li(+) or Li(2 +), which radiate near 199 Å and 135 Å, respectively. Based on measurements at the Livermore Electron Beam Ion Trap we have shown that the instrumental resolution is better than 48 mÅ at the 200 Å setting and better than 40 mÅ for the 135-Å range. Such a high spectral resolution corresponds to an instrumental limit for line-width based temperature measurements of about 45 eV for the 199 Å Li(+) and 65 eV for the 135 Å Li(2 +) lines. Recently obtained survey spectra from the Lithium Tokamak Experiment at the Princeton Plasma Physics Laboratory show the presence of these lithium emission lines and the expected core ion temperature of approximately 70 eV is sufficiently high to demonstrate the feasibility of utilizing our high-resolution spectrometer as an ion-temperature diagnostic.

  10. High-resolution grazing-incidence grating spectrometer for temperature measurements of low-Z ions emitting in the 100–300 Å spectral band

    SciTech Connect

    Widmann, K. Beiersdorfer, P.; Magee, E. W.; Boyle, D. P.; Kaita, R.; Majeski, R.

    2014-11-15

    We have constructed a high-resolution grazing-incidence spectrometer designed for measuring the ion temperature of low-Z elements, such as Li{sup +} or Li{sup 2+}, which radiate near 199 Å and 135 Å, respectively. Based on measurements at the Livermore Electron Beam Ion Trap we have shown that the instrumental resolution is better than 48 mÅ at the 200 Å setting and better than 40 mÅ for the 135-Å range. Such a high spectral resolution corresponds to an instrumental limit for line-width based temperature measurements of about 45 eV for the 199 Å Li{sup +} and 65 eV for the 135 Å Li{sup 2+} lines. Recently obtained survey spectra from the Lithium Tokamak Experiment at the Princeton Plasma Physics Laboratory show the presence of these lithium emission lines and the expected core ion temperature of approximately 70 eV is sufficiently high to demonstrate the feasibility of utilizing our high-resolution spectrometer as an ion-temperature diagnostic.

  11. The thickness measurement of ultrathin films from new high-k material HfO2 by grazing incidence x-ray reflectivity

    NASA Astrophysics Data System (ADS)

    Jia, Yabin; Gao, Huifang; Li, Xu; Yao, Yaxuan; Wang, Meiling; Tao, Xingfu; Tian, Rongrong; Ren, Lingling; Qin, Lin

    2016-06-01

    The thickness of HfO2 ultrathin films was determined by grazing incidence x-ray reflectivity (GIXRR) with simulation. Two samples were prepared by atomic layer deposition, and the Si substrate of one sample was treated by HF acid (1:20) to erase the native oxide layer, while the other was not. According to the GIXRR, the films consisted of two contamination layers, an interface layer, a HfO2 layer and a native oxide layer (except for the acid-treated sample) from top to bottom. As a result, the HfO2 thickness of the two samples was 1.23 nm and 1.25 nm respectively, and the thicknesses of the interface layers between the HfO2 and the Si substrate were 0.1 nm and 0.95 nm respectively. The chemical states of the film were investigated by ultrasonification and x-ray photoemission spectroscopy (XPS), and the thickness was verified by transmission electron microscopy (TEM). All these phenomena proved that GIXRR is a powerful and effective piece of technology for characterizing HfO2 ultrathin film.

  12. Crystal and electronic structures of pentacene thin films from grazing-incidence x-ray diffraction and first-principles calculations

    SciTech Connect

    Nabok, Dmitrii; Puschnig, Peter; Ambrosch-Draxl, Claudia; Werzer, Oliver; Resel, Roland; Smilgies, Detlef-M.

    2007-12-15

    Combined experimental and theoretical investigations on thin films of pentacene are performed in order to determine the structure of the pentacene thin film phase. Grazing incidence x-ray diffraction is used for studying a pentacene thin film with a nominal thickness of 180 nm. The crystal structure is found to exhibit the lattice parameters a=0.592 nm, b=0.754 nm, c=1.563 nm, {alpha}=81.5 deg. , {beta}=87.2 deg. , and {gamma}=89.9 deg. . These crystallographic unit cell dimensions are used as the only input parameters for ab initio total-energy calculations within the framework of density functional theory revealing the molecular packing within the crystal structure. Moreover, we calculate the electronic band structure of the thin film phase and compare it to that of the bulk phase. We find the intermolecular bandwidths of the thin film phase to be significantly larger compared to the bulk structure, e.g., the valence bandwidth is twice as large. This remarkable effect is traced back to an enhanced intermolecular {pi}-{pi} overlap due to the upright standing molecules in the thin film phase.

  13. Role of the precursor in a triple-pulse pumping scheme of a nickel-like silver soft-x-ray laser in the grazing-incidence-pumping geometry

    SciTech Connect

    Janulewicz, K. A.; Kim, C. M.

    2010-11-15

    Soft x-ray lasers pumped in the grazing incidence geometry show strongly reduced energetic needs but hardly changed conversion efficiency between the pump energy and the output short-wavelength radiation. Numerical analysis presented in the paper concerns with performance of a Ni-like Ag soft-x-ray laser pumped by a triple-pulse structure in the grazing incidence geometry as a function of the puming conditions. It was found that a weak precursor preceding the main preforming and heating pulses by a few nanoseconds is crucial for the energy deposition. Its presence enables in different arrangements a reasonable reduction in the pump energy and relaxation of the steep density gradients as well as a control over partition of the deposited energy. As a consequence, it was concluded that a well energetically balanced three- or multipulse composition seems to be a reasonable way to achieve performance improvement.

  14. Small-angle Compton Scattering to Determine the Depth of a Radioactive Source in Matter

    SciTech Connect

    Oberer, R. B.; Gunn, C. A.; Chiang, L. G.; Valiga, R. E.; Cantrell, J. A.

    2011-04-01

    A gamma-ray peak in a spectrum is often accompanied by a discontinuity in the Compton continuum at the peak. The Compton continuum results from Compton scattering in the detector. The discontinuity at a peak results from small-angle Compton scattering by the gamma rays in matter situated directly between the gamma-ray source and the detector. The magnitude of this discontinuity with respect to the gamma-ray peak is therefore an indicator of the amount of material or shielding between the gamma-ray source and the detector. This small-angle scattering was used to determine the depth of highly-enriched uranium (HEU) solution standards in a concrete floor mockup. The empirical results of the use of this small-angle scattering discontinuity in a concrete floor experiment will be described. A Monte Carlo calculation of the experiment will also be described. In addition, the depth determined from small-angle scattering was used in conjunction with differential attenuation to more accurately measure the uranium content of the mockup. Following these empirical results, the theory of small-angle scattering will be discussed. The magnitude of the discontinuity compared to the peak count rate is directly related to the depth of the gamma-ray source in matter. This relation can be described by relatively simple mathematical expressions. This is the first instance that we are aware of in which the small-angle Compton scattering has been used to determine the depth of a radioactive source. Furthermore this is the first development of the theoretical expressions for the magnitude of the small-angle scattering discontinuity.

  15. Study of interface correlation in W/C multilayer structure by specular and non-specular grazing incidence X-ray reflectivity measurements

    NASA Astrophysics Data System (ADS)

    Biswas, A.; Maidul Haque, S.; Tripathi, S.; De, Rajnarayan; Rai, S.; Bhattacharyya, D.; Sahoo, N. K.

    2015-10-01

    W/C/W tri-layer thin film samples have been deposited on c-Si substrates in a home-built Ion Beam Sputtering system at 1.5 × 10-3 Torr Ar working pressure and 10 mA grid current. The tri-layer samples have been deposited at different Ar+ ion energies between 0.6 and 1.2 keV for W layer deposition and the samples have been characterized by specular and non-specular grazing incidence X-ray reflectivity (GIXR) measurements. By analyzing the GIXR spectra, various interface parameters have been obtained for both W-on-C and C-on-W interfaces and optimum Ar+ ion energy for obtaining interfaces with low imperfections has been found. Subsequently, multilayer W/C samples with 5-layer, 7-layer, 9-layer, and 13-layer have been deposited at this optimum Ar+ ion energy. By fitting the specular and diffused GIXR data of the multilayer samples with the parameters of each interface as fitting variables, different interface parameters, viz., interface width, in-plane correlation length, interface roughness, and interface diffusion have been estimated for each interface and their variation across the depth of the multilayers have been obtained. The information would be useful in realizing W/C multilayers for soft X-ray mirror application in the <100 Å wavelength regime. The applicability of the "restart of the growth at the interface" model in the case of these ion beam sputter deposited W/C multilayers has also been investigated in the course of this study.

  16. Study of interface correlation in W/C multilayer structure by specular and non-specular grazing incidence X-ray reflectivity measurements

    SciTech Connect

    Biswas, A. Bhattacharyya, D.; Sahoo, N. K.; Maidul Haque, S.; Tripathi, S.; De, Rajnarayan; Rai, S.

    2015-10-28

    W/C/W tri-layer thin film samples have been deposited on c-Si substrates in a home-built Ion Beam Sputtering system at 1.5 × 10{sup −3} Torr Ar working pressure and 10 mA grid current. The tri-layer samples have been deposited at different Ar{sup +} ion energies between 0.6 and 1.2 keV for W layer deposition and the samples have been characterized by specular and non-specular grazing incidence X-ray reflectivity (GIXR) measurements. By analyzing the GIXR spectra, various interface parameters have been obtained for both W-on-C and C-on-W interfaces and optimum Ar{sup +} ion energy for obtaining interfaces with low imperfections has been found. Subsequently, multilayer W/C samples with 5-layer, 7-layer, 9-layer, and 13-layer have been deposited at this optimum Ar{sup +} ion energy. By fitting the specular and diffused GIXR data of the multilayer samples with the parameters of each interface as fitting variables, different interface parameters, viz., interface width, in-plane correlation length, interface roughness, and interface diffusion have been estimated for each interface and their variation across the depth of the multilayers have been obtained. The information would be useful in realizing W/C multilayers for soft X-ray mirror application in the <100 Å wavelength regime. The applicability of the “restart of the growth at the interface” model in the case of these ion beam sputter deposited W/C multilayers has also been investigated in the course of this study.

  17. Signal, noise, and resolution in correlated fluctuations from snapshot small-angle x-ray scattering

    SciTech Connect

    Kirian, Richard A.; Schmidt, Kevin E.; Wang Xiaoyu; Doak, R. Bruce; Spence, John C. H.

    2011-07-15

    It has been suggested that the three-dimensional structure of one particle may be reconstructed using the scattering from many identical, randomly oriented copies ab initio, without modeling or a priori information. This may be possible if these particles are frozen in either space or time, so that the conventional two-dimensional small-angle x-ray scattering (SAXS) distribution contains fluctuations and is no longer isotropic. We consider the magnitude of the correlated fluctuation SAXS (CFSAXS) signal for typical x-ray free-electron laser (XFEL) beam conditions and compare this against the errors derived with the inclusion of Poisson photon counting statistics. The resulting signal-to-noise ratio (SNR) is found to rapidly approach a limit independent of the number of particles contributing to each diffraction pattern, so that the addition of more particles to a ''single-particle-per-shot'' experiment may be of little value, apart from reducing solvent background. When the scattering power is significantly less than one photon per particle per Shannon pixel, the SNR grows in proportion to incident flux. We provide simulations for protein molecules in support of these analytical results, and discuss the effects of solvent background scatter. We consider the SNR dependence on resolution and particle size, and discuss the application of the method to glasses and liquids, and the implications of more powerful XFELs, smaller focused beams, and higher pulse repetition rates for this approach. We find that an accurate CFSAXS measurement may be acquired to subnanometer resolution for protein molecules if a 9-keV beam containing 10{sup 13} photons is focused to a {approx}100-nm spot diameter, provided that the effects of solvent background can be reduced sufficiently.

  18. Small angle x-ray scattering with a beryllium compound refractive lens as focusing optic

    SciTech Connect

    Timmann, Andreas; Doehrmann, Ralph; Schubert, Tom; Schulte-Schrepping, Horst; Hahn, Ulrich; Kuhlmann, Marion; Gehrke, Rainer; Roth, Stephan Volkher; Schropp, Andreas; Schroer, Christian; Lengeler, Bruno

    2009-04-15

    At BW4 at HASYLAB a beryllium compound refractive lens (Be-CRL) is used for the focusing in small-angle x-ray scattering experiments. Using it provides the advantages of higher long-term stability and a much easier alignment compared to a setup with focusing mirrors. In our investigations presented here, we show the advantages of using a Be-CRL in small-angle and also ultra small-angle x-ray scattering. We investigated the beam characteristics at the sample position with respect to spot size and photon flux. The spot size is comparable to that of a setup with focusing mirrors but with a gain in flux and better long-term stability. It is also shown that plane mirrors are still necessary to suppress higher order energies passing the monochromator.

  19. Small-angle approximation to the transfer of narrow laser beams in anisotropic scattering media

    NASA Technical Reports Server (NTRS)

    Box, M. A.; Deepak, A.

    1981-01-01

    The broadening and the signal power detected of a laser beam traversing an anisotropic scattering medium were examined using the small-angle approximation to the radiative transfer equation in which photons suffering large-angle deflections are neglected. To obtain tractable answers, simple Gaussian and non-Gaussian functions for the scattering phase functions are assumed. Two other approximate approaches employed in the field to further simplify the small-angle approximation solutions are described, and the results obtained by one of them are compared with those obtained using small-angle approximation. An exact method for obtaining the contribution of each higher order scattering to the radiance field is examined but no results are presented.

  20. Experimental methods in the study of neutron scattering at small angles

    SciTech Connect

    Dragolici, Cristian A.

    2014-11-24

    Small angle scattering (SAS) is the collective name given to the techniques of small angle neutron (SANS) and X-ray (SAXS) scattering. They offer the possibility to analyze particles without disturbing their natural environment. In each of these techniques radiation is elastically scattered by a sample and the resulting scattering pattern is analyzed to provide information about the size, shape and orientation of some component of the sample. Accordingly, a large number of methods and experimental patterns have been developed to ease the investigation of condensed matter by use of these techniques. Some of them are the discussed in this paper.

  1. Irena : tool suite for modeling and analysis of small-angle scattering.

    SciTech Connect

    Ilavsky, J.; Jemian, P.

    2009-04-01

    Irena, a tool suite for analysis of both X-ray and neutron small-angle scattering (SAS) data within the commercial Igor Pro application, brings together a comprehensive suite of tools useful for investigations in materials science, physics, chemistry, polymer science and other fields. In addition to Guinier and Porod fits, the suite combines a variety of advanced SAS data evaluation tools for the modeling of size distribution in the dilute limit using maximum entropy and other methods, dilute limit small-angle scattering from multiple non-interacting populations of scatterers, the pair-distance distribution function, a unified fit, the Debye-Bueche model, the reflectivity (X-ray and neutron) using Parratt's formalism, and small-angle diffraction. There are also a number of support tools, such as a data import/export tool supporting a broad sampling of common data formats, a data modification tool, a presentation-quality graphics tool optimized for small-angle scattering data, and a neutron and X-ray scattering contrast calculator. These tools are brought together into one suite with consistent interfaces and functionality. The suite allows robust automated note recording and saving of parameters during export.

  2. Studying fractal geometry on submicron length scales by small-angle scattering

    SciTech Connect

    Wong, P.; Lin, J.

    1988-08-01

    Recent studies have shown that internal surfaces of porous geological materials, such as rocks and lignite coals, can be described by fractals down to atomic length scales. In this paper, the basic properties of self-similar and self-affine fractals are reviewed and how fractal dimensions can be measured by small-angle scattering experiments are discussed.

  3. Structure of unilamellar vesicles: Numerical analysis based on small-angle neutron scattering data

    SciTech Connect

    Zemlyanaya, E. V. Kiselev, M. A.; Zbytovska, J.; Almasy, L.; Aswal, V. K.; Strunz, P.; Wartewig, S.; Neubert, R.

    2006-12-15

    The structure of polydispersed populations of unilamellar vesicles is studied by small-angle neutron scattering for three types of lipid systems, namely, single-, two-and four-component vesicular systems. Results of the numerical analysis based on the separated-form-factor model are reported.

  4. Design and use of a 6 meter neutron small-angle scattering spectrometer at KUR

    NASA Astrophysics Data System (ADS)

    Komura, S.; Takeda, T.; Fujii, H.; Osamura, K.; Mochiki, K.; Hasegawa, K.

    1983-05-01

    A 6 meter neutron small-angle scattering spectrometer has been constructed at the Kyoto University Reactor (KUR) and has been used successfully in various fields of application. The design principles and the characteristics of the spectrometer are described briefly. Some examples of the scattering measurements are presented.

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

    SciTech Connect

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

    2014-08-15

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

  6. Amazing Grazing.

    ERIC Educational Resources Information Center

    Peterson, Cris

    Countless acres of grasslands stretch across the American West. Centuries ago, bison roamed the range freely and lived off the grass. By the 19th century, herds of cattle grazed the same land. Over time, much of the original grassland was either plowed and planted or trampled to dust, causing the topsoil to dry up and blow away. Today many…

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

    NASA Astrophysics Data System (ADS)

    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.

  8. Hierarchical O(N) computation of small-angle scattering profiles and their associated derivatives

    PubMed Central

    Berlin, Konstantin; Gumerov, Nail A.; Fushman, David; Duraiswami, Ramani

    2014-01-01

    The need for fast approximate algorithms for Debye summation arises in computations performed in crystallography, small/wide-angle X-ray scattering and small-angle neutron scattering. When integrated into structure refinement protocols these algorithms can provide significant speed up over direct all-atom-to-all-atom computation. However, these protocols often employ an iterative gradient-based optimization procedure, which then requires derivatives of the profile with respect to atomic coordinates. This article presents an accurate, O(N) cost algorithm for the computation of scattering profile derivatives. The results reported here show orders of magnitude improvement in computational efficiency, while maintaining the prescribed accuracy. This opens the possibility to efficiently integrate small-angle scattering data into the structure determination and refinement of macromolecular systems. PMID:24701198

  9. Small-angle neutron scattering studies from solutions of bovine nasal cartilage proteoglycan

    SciTech Connect

    Patel, A.; Stivala, S.S.; Damle, S.P.; Gregory, J.D.; Bunick, G.J.; Uberbacher, E.C.

    1985-08-01

    Small-angle neutron scattering, SANS, of the proteoglycan subunit of bovine nasal cartilage in 0.15N LiCl at 25/sup 0/C yielded the radius of gyration, R/sub g/, radius of gyration of the cross-section, R/sub q/, persistence length, a, and the molecular weight, M. The following values were obtained: M = 3.9 x 10/sup 6/, R/sub g/ = 745 A, R/sub q/ = 34.6 A and a = 35.2 A. These values compare favorably with those that were obtained from small angle x-ray scattering, SAXS, of a similar extract. The scattering curve of the proteoglycan subunit in D/sub 2/O showed a characteristic broad peak in the specified angular range similar to that observed from SAXS, thus confirming the polyelectrolyte nature of the proteoglycan. 15 refs., 3 figs., 1 tab. (DT)

  10. BIOISIS: Biological Macromolecules by Small Angle X-ray Scattering (SAXS)

    DOE Data Explorer

    Tainer, John [Scripps Research Institute; Hura, Greg [LBNL; Rambo, Robert P. [LBNL

    BIOISIS is an open access database dedicated to the study of biological macromolecules by small angle X-ray scattering (SAXS). BIOISIS aims to become the complete source for the deposition, distribution and maintenance of small angle X-ray scattering data and technologies. The database is designed around the concept of an ôexperimentö and relates a specific experiment to a set of genes, organisms, computational models and experimental data. As of May 2012, BIOSIS contains 7,118 genes covering four different organisms. Forty-two modeled structures are available. Clicking on a structures reveals scattering curves, experimental conditions, and experimental values. The data are collected at Beamline 12.3.1 of the Advanced Light Source (ALS).[Copied with editing from http://www.bioisis.net/about

  11. Characterization of porous materials using combined small-angle X-ray and neutron scattering techniques

    SciTech Connect

    Hu, Naiping; Borkar, Neha; Kohls, Doug; Schaefer, Dale W.

    2014-09-24

    A combination of ultra small angle X-ray scattering (USAXS) and ultra small angle neutron scattering (USANS) is used to characterize porous materials. The analysis methods yield quantitative information, including the mean skeletal chord length, mean pore chord length, skeletal density, and composition. A mixed cellulose ester (MCE) membrane with a manufacturer-labeled pore size of 0.1 {mu}m was used as a model to elucidate the specifics of the method. Four approaches describing four specific scenarios (different known parameters and form of the scattering data) are compared. Pore chords determined using all four approaches are in good agreement with the scanning electron microscopy estimates but are larger than the manufacturer's nominal pore size. Our approach also gives the average chord of the skeletal solid (struts) of the membrane, which is also consistent for all four approaches. Combined data from USAXS and USANS gives the skeletal density and the strut composition.

  12. Small-angle X-ray scattering method to characterize molecular interactions: Proof of concept.

    PubMed

    Allec, Nicholas; Choi, Mina; Yesupriya, Nikhil; Szychowski, Brian; White, Michael R; Kann, Maricel G; Garcin, Elsa D; Daniel, Marie-Christine; Badano, Aldo

    2015-01-01

    Characterizing biomolecular interactions is crucial to the understanding of biological processes. Existing characterization methods have low spatial resolution, poor specificity, and some lack the capability for deep tissue imaging. We describe a novel technique that relies on small-angle X-ray scattering signatures from high-contrast molecular probes that correlate with the presence of biomolecular interactions. We describe a proof-of-concept study that uses a model system consisting of mixtures of monomer solutions of gold nanoparticles (GNPs) as the non-interacting species and solutions of GNP dimers linked with an organic molecule (dimethyl suberimidate) as the interacting species. We report estimates of the interaction fraction obtained with the proposed small-angle X-ray scattering characterization method exhibiting strong correlation with the known relative concentration of interacting and non-interacting species. PMID:26160052

  13. New analysis of the small-angle-magnetization-rotation method for magnetostriction measurements on amorphous ribbons

    NASA Astrophysics Data System (ADS)

    Severino, A. M.; Missell, F. P.

    1987-09-01

    The small-angle-magnetization-rotation (SAMR) method for measuring the saturation magnetostrictin λ s has been reanalyzed, taking into account the underlying domain structure of the amorphous ribbon. Although the condition for determining λ s reamins unchenged, the modifications introduced allow one to understand many additional features of the experimental data. With the appropriate modifications, the SAMR method can be used to study stress relaxation in amorphous alloys. Examples are given Fe-based and Co-based alloys.

  14. Small-angle x-ray scattering of intercalation compounds of graphite, fluorographite, and graphite oxide

    SciTech Connect

    Perevozkin, V.Yu.; Yur'ev, G.S.; Nazarov, A.S.; Danilenko, A.M.; Lisitsa, V.V.; Makotchenko, V.G.; Paasonen, V.M.; Yakovlev, I.I.

    1988-05-01

    Graphite intercalation compounds are interesting as cathode materials in chemical current sources and catalysts and are good conductors of electricity. Small-angle x-ray scattering was studied on natural graphite, intercalation compounds of fluorinated graphite, graphite oxide, and the products of reduction of the compounds. It was shown that scattering takes place in regions with a lower density and the size of the density inhomogeneities was determined.

  15. Two-dimensional position-sensitive detectors for small-angle neutron scattering

    SciTech Connect

    McElhaney, S.A.; Vandermolen, R.I.

    1990-05-01

    In this paper, various detectors available for small angle neutron scattering (SANS) are discussed, along with some current developments being actively pursued. A section has been included to outline the various methodologies of position encoding/decoding with discussions on trends and limitations. Computer software/hardware vary greatly from institute and experiment and only a general discussion is given to this area. 85 refs., 33 figs.

  16. A 6-Meter Neutron Small-Angle Scattering Spectrometer at KUR

    NASA Astrophysics Data System (ADS)

    Komura, Shigehiro; Takeda, Takayoshi; Fujii, Hironobu; Toyoshima, Yoshinori; Osamura, Kozo; Mochiki, Koichi; Hasegawa, Ken'ichi

    1983-02-01

    A 6-meter neutron small-angle scattering spectrometer has been constructed at Kyoto University Reactor (KUR) and has been used successfully for various fields of application in these three years. This paper describes overall design principles and the characteristics of the various parts of the spectrometers which can be assembled and disassembled easily at KUR. Some examples of scattering measurements are presented to show the performance of the spectrometer.

  17. Pore size distribution of shaley rock by small angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Hall, P. L.; Mildner, D. F. R.; Borst, R. L.

    1983-08-01

    Information concerning pore microstructure of shaly rocks is of considerable relevance to petroleum exploration and production. Pore sizes and distributions within shaly samples have been determined by small angle neutron scattering. The data are indicative of a considerable spread of pore dimension, showing inhomogeneities with a range from 20 Å and greater. The cumulative pore volumes are compared with those derived from mercury intrusion porosimetry and nitrogen adsorption and desorption isotherms.

  18. Pore size distribution of shaly rock by small angle neutron scattering

    SciTech Connect

    Hall, P.L.; Mildner, D.F.R.; Borst, R.L.

    1983-08-01

    Information concerning pore microstructure of shaly rocks is of considerable relevance to petroleum exploration and production. Pore sizes and distributions within shaly samples have been determined by small angle neutron scattering. The data are indicative of a considerable spread of pore dimension, showing inhomogeneities with a range from 20 A and greater. The cumulative pore volumes are compared with those derived from mercury intrusion porosimetry and nitrogen adsorption and desorption isotherms.

  19. Monte Carlo-based rigid body modelling of large protein complexes against small angle scattering data.

    PubMed

    Meesters, Christian; Pairet, Bruno; Rabenhorst, Anja; Decker, Heinz; Jaenicke, Elmar

    2010-06-01

    We present a modular, collaborative, open-source architecture for rigid body modelling based upon small angle scattering data, named sas_rigid. It is designed to provide a fast and extensible scripting interface using the easy-to-learn Python programming language. Features include rigid body modelling to result in static structures and three-dimensional probability densities using two different algorithms. PMID:20598639

  20. Study of High-Frequency Impedance of Small-Angle Tapers and Collimators

    SciTech Connect

    Stupakov, Gennady; Podobedov, B.; /Brookhaven

    2010-06-04

    Collimators and transitions in accelerator vacuum chambers often include small-angle tapering to lower the wakefields generated by the beam. While the low-frequency impedance is well described by Yokoya's formula (for axisymmetric geometry), much less is known about the behavior of the impedance in the high frequency limit. In this paper we develop an analytical approach to the highfrequency regime for round collimators and tapers. Our analytical results are compared with computer simulations using the code ECHO.

  1. Small-angle neutron scattering of nanocrystalline terbium with random paramagnetic susceptibility.

    PubMed

    Balaji, G; Ghosh, S; Döbrich, F; Eckerlebe, H; Weissmüller, J

    2008-06-01

    We report magnetic small-angle neutron scattering (SANS) data for the nanocrystalline rare earth metal Terbium in its paramagnetic state. Whereas critical scattering dominates at large momentum transfer, q, the (magnetic-) field response of the scattering at small q arises from the spatial nonuniformity of the paramagnetic susceptibility tensor. The finding of an interrelation between SANS and the susceptibility suggests a way for characterizing the nonuniform magnetic interactions in hard magnets by neutron scattering. PMID:18643454

  2. Effect of the concentration of inhomogeneities on the multiple small-angle neutron scattering

    SciTech Connect

    Abov, Yu. G.; Dzheparov, F. S.; Elyutin, N. O.; Lvov, D. V. Tyulyusov, A. N.

    2013-03-15

    The interference effects manifested during multiple small-angle neutron scattering (MSANS) on a chaotically arranged close-packed ensemble of scatterers have been studied. MSANS measurements have been performed for mixtures of Al and Ti-Zr alloy powders. It is shown that the results can be satisfactorily described based on a theory that takes into account spatial correlations in the arrangement of powder grains.

  3. SFF analysis of the small angle scattering data for investigation of a vesicle systems structure

    NASA Astrophysics Data System (ADS)

    Zemlyanaya, E. V.; Kiselev, M. A.; Zhabitskaya, E. I.; Gruzinov, A. Yu.; Aksenov, V. L.; Ipatova, O. M.; Druzhilovskaya, O. S.

    2016-06-01

    Experimental data on the small angle synchrotron X-ray scattering (SAXS) are analyzed on a basis of Separated form factors method (SFF) for a study of the drug delivery Phospholipid Transport Nano System (PTNS). Basic parameters of polydispersed population of PTNS nanoparticles (average radius of PTNS-particles, polydispersity of radius, thickness of membrane) have been determined. The results are discussed in comparison with the SFF results for the “classical” vesicular system of dimyristoylphosphocholine (DMPC).

  4. Understanding inelastically scattered neutrons from water on a time-of-flight small-angle neutron scattering (SANS) instrument

    NASA Astrophysics Data System (ADS)

    Do, Changwoo; Heller, William T.; Stanley, Christopher; Gallmeier, Franz X.; Doucet, Mathieu; Smith, Gregory S.

    2014-02-01

    It is generally assumed by most of the small-angle neutron scattering (SANS) user community that a neutron's energy is unchanged during SANS measurements. Here, the scattering from water, specifically light water, was measured on the EQ-SANS instrument, a time-of-flight (TOF) SANS instrument located at the Spallation Neutron Source of Oak Ridge National Laboratory. A significant inelastic process was observed in the TOF spectra of neutrons scattered from water. Analysis of the TOF spectra from the sample showed that the scattered neutrons have energies consistent with room-temperature thermal energies (~20 meV) regardless of the incident neutron's energy. With the aid of Monte Carlo particle transport simulations, we conclude that the thermalization process within the sample results in faster neutrons that arrive at the detector earlier than expected based on the incident neutron energies. This thermalization process impacts the measured SANS intensities in a manner that will ultimately be sample- and temperature-dependent, necessitating careful processing of the raw data into the SANS cross-section.

  5. Using a Hexagonal Mirror for Varying Light Intensity in the Measurement of Small-Angle Variation.

    PubMed

    Hsieh, Meng-Chang; Lin, Jiun-You; Chang, Chia-Ou

    2016-08-16

    Precision positioning and control are critical to industrial-use processing machines. In order to have components fabricated with excellent precision, the measurement of small-angle variations must be as accurate as possible. To achieve this goal, this study provides a new and simple optical mechanism by varying light intensity. A He-Ne laser beam was passed through an attenuator and into a beam splitter. The reflected light was used as an intensity reference for calibrating the measurement. The transmitted light as a test light entered the optical mechanism hexagonal mirror, the optical mechanism of which was created by us, and then it entered the power detector after four consecutive reflections inside the mirror. When the hexagonal mirror was rotated by a small angle, the laser beam was parallel shifted. Once the laser beam was shifted, the hitting area on the detector was changed; it might be partially outside the sensing zone and would cause the variation of detection intensity. This variation of light intensity can be employed to measure small-angle variations. The experimental results demonstrate the feasibility of this method. The resolution and sensitivity are 3 × 10(-40) and 4 mW/° in the angular range of 0.6°, respectively, and 9.3 × 10(-50) and 13 mW/° in the angular range of 0.25°.

  6. Using a Hexagonal Mirror for Varying Light Intensity in the Measurement of Small-Angle Variation.

    PubMed

    Hsieh, Meng-Chang; Lin, Jiun-You; Chang, Chia-Ou

    2016-01-01

    Precision positioning and control are critical to industrial-use processing machines. In order to have components fabricated with excellent precision, the measurement of small-angle variations must be as accurate as possible. To achieve this goal, this study provides a new and simple optical mechanism by varying light intensity. A He-Ne laser beam was passed through an attenuator and into a beam splitter. The reflected light was used as an intensity reference for calibrating the measurement. The transmitted light as a test light entered the optical mechanism hexagonal mirror, the optical mechanism of which was created by us, and then it entered the power detector after four consecutive reflections inside the mirror. When the hexagonal mirror was rotated by a small angle, the laser beam was parallel shifted. Once the laser beam was shifted, the hitting area on the detector was changed; it might be partially outside the sensing zone and would cause the variation of detection intensity. This variation of light intensity can be employed to measure small-angle variations. The experimental results demonstrate the feasibility of this method. The resolution and sensitivity are 3 × 10(-40) and 4 mW/° in the angular range of 0.6°, respectively, and 9.3 × 10(-50) and 13 mW/° in the angular range of 0.25°. PMID:27537893

  7. Using a Hexagonal Mirror for Varying Light Intensity in the Measurement of Small-Angle Variation

    PubMed Central

    Hsieh, Meng-Chang; Lin, Jiun-You; Chang, Chia-Ou

    2016-01-01

    Precision positioning and control are critical to industrial-use processing machines. In order to have components fabricated with excellent precision, the measurement of small-angle variations must be as accurate as possible. To achieve this goal, this study provides a new and simple optical mechanism by varying light intensity. A He-Ne laser beam was passed through an attenuator and into a beam splitter. The reflected light was used as an intensity reference for calibrating the measurement. The transmitted light as a test light entered the optical mechanism hexagonal mirror, the optical mechanism of which was created by us, and then it entered the power detector after four consecutive reflections inside the mirror. When the hexagonal mirror was rotated by a small angle, the laser beam was parallel shifted. Once the laser beam was shifted, the hitting area on the detector was changed; it might be partially outside the sensing zone and would cause the variation of detection intensity. This variation of light intensity can be employed to measure small-angle variations. The experimental results demonstrate the feasibility of this method. The resolution and sensitivity are 3 × 10−40 and 4 mW/° in the angular range of 0.6°, respectively, and 9.3 × 10−50 and 13 mW/° in the angular range of 0.25°. PMID:27537893

  8. Small-angle scatter tomography with a photon-counting detector array

    NASA Astrophysics Data System (ADS)

    Pang, Shuo; Zhu, Zheyuan; Wang, Ge; Cong, Wenxiang

    2016-05-01

    Small-angle x-ray scatter imaging has a high intrinsic contrast in cancer research and other applications, and provides information on molecular composition and micro-structure of the tissue. In general, the implementations of small-angle coherent scatter imaging can be divided into two main categories: direct tomography and angular dispersive computerized tomography. Based on the recent development of energy-discriminative photon-counting detector array, here we propose a computerized tomography setup based on energy-dispersive measurement with a photon-counting detector array. To show merits of the energy-dispersive approach, we have performed numerical tests with a phantom containing various tissue types, in comparison with the existing imaging approaches. The results show that with an energy resolution of ~6 keV, the energy dispersive tomography system with a broadband tabletop x-ray would outperform the angular dispersive system, which makes the x-ray small-angle scatter tomography promising for high-specificity tissue imaging.

  9. Nanostructure surveys of macroscopic specimens by small-angle scattering tensor tomography

    NASA Astrophysics Data System (ADS)

    Liebi, Marianne; Georgiadis, Marios; Menzel, Andreas; Schneider, Philipp; Kohlbrecher, Joachim; Bunk, Oliver; Guizar-Sicairos, Manuel

    2015-11-01

    The mechanical properties of many materials are based on the macroscopic arrangement and orientation of their nanostructure. This nanostructure can be ordered over a range of length scales. In biology, the principle of hierarchical ordering is often used to maximize functionality, such as strength and robustness of the material, while minimizing weight and energy cost. Methods for nanoscale imaging provide direct visual access to the ultrastructure (nanoscale structure that is too small to be imaged using light microscopy), but the field of view is limited and does not easily allow a full correlative study of changes in the ultrastructure over a macroscopic sample. Other methods of probing ultrastructure ordering, such as small-angle scattering of X-rays or neutrons, can be applied to macroscopic samples; however, these scattering methods remain constrained to two-dimensional specimens or to isotropically oriented ultrastructures. These constraints limit the use of these methods for studying nanostructures with more complex orientation patterns, which are abundant in nature and materials science. Here, we introduce an imaging method that combines small-angle scattering with tensor tomography to probe nanoscale structures in three-dimensional macroscopic samples in a non-destructive way. We demonstrate the method by measuring the main orientation and the degree of orientation of nanoscale mineralized collagen fibrils in a human trabecula bone sample with a spatial resolution of 25 micrometres. Symmetries within the sample, such as the cylindrical symmetry commonly observed for mineralized collagen fibrils in bone, allow for tractable sampling requirements and numerical efficiency. Small-angle scattering tensor tomography is applicable to both biological and materials science specimens, and may be useful for understanding and characterizing smart or bio-inspired materials. Moreover, because the method is non-destructive, it is appropriate for in situ measurements and

  10. JGIXA - A software package for the calculation and fitting of grazing incidence X-ray fluorescence and X-ray reflectivity data for the characterization of nanometer-layers and ultra-shallow-implants

    NASA Astrophysics Data System (ADS)

    Ingerle, D.; Pepponi, G.; Meirer, F.; Wobrauschek, P.; Streli, C.

    2016-04-01

    Grazing incidence XRF (GIXRF) is a very surface sensitive, nondestructive analytical tool making use of the phenomenon of total external reflection of X-rays on smooth polished surfaces. In recent years the method experienced a revival, being a powerful tool for process analysis and control in the fabrication of semiconductor based devices. Due to the downscaling of the process size for semiconductor devices, junction depths as well as layer thicknesses are reduced to a few nanometers, i.e. the length scale where GIXRF is highly sensitive. GIXRF measures the X-ray fluorescence induced by an X-ray beam incident under varying grazing angles and results in angle dependent intensity curves. These curves are correlated to the layer thickness, depth distribution and mass density of the elements in the sample. But the evaluation of these measurements is ambiguous with regard to the exact distribution function for the implants as well as for the thickness and density of nanometer-thin layers. In order to overcome this ambiguity, GIXRF can be combined with X-ray reflectometry (XRR). This is straightforward, as both techniques use similar measurement procedures and the same fundamental physical principles can be used for a combined data evaluation strategy. Such a combined analysis removes ambiguities in the determined physical properties of the studied sample and, being a correlative spectroscopic method, also significantly reduces experimental uncertainties of the individual techniques. In this paper we report our approach to a correlative data analysis, based on a concurrent calculation and fitting of simultaneously recorded GIXRF and XRR data. Based on this approach we developed JGIXA (Java Grazing Incidence X-ray Analysis), a multi-platform software package equipped with a user-friendly graphic user interface (GUI) and offering various optimization algorithms. Software and data evaluation approach were benchmarked by characterizing metal and metal oxide layers on

  11. Cylindrical aggregates of chlorophylls studied by small-angle neutron scatter

    SciTech Connect

    Worcester, D.L.; Katz, J.J.

    1994-12-31

    Neutron small-angle scattering has demonstrated tubular chlorophyll aggregates formed by self-assembly of a variety of chlorophyll types in nonpolar solvents. The size and other properties of the tubular aggregates can be accounted for by stereochemical properties of the chlorophyll molecules. Features of some of the structures are remarkably similar to light harvesting chlorophyll complexes in vivo, particularly for photosynthetic bacteria. These nanotube chlorophyll structures may have applications as light harvesting biomaterials where efficient energy transfer occurs from an excited state which is highly delocalized.

  12. Using small angle solution scattering data in Xplor-NIH structure calculations.

    PubMed

    Schwieters, Charles D; Clore, G Marius

    2014-07-01

    This contribution describes the use of small and wide angle X-ray and small angle neutron scattering for biomolecular structure calculation using the program Xplor-NIH, both with and without NMR data. The current algorithms used for calculating scattering curves are described, and the use of scattering data as a structural restraint is given concrete form as a fragment of an Xplor-NIH structure calculation script. We review five examples of the use of scattering data in structure calculation, including the treatment of single domain proteins, nucleic acids, structure determination of large proteins, and the use of ensemble representations to characterize small and large amplitude motions.

  13. Analysis of C-S-H gel and cement paste by small-angle neutron scattering

    SciTech Connect

    Allen, Andrew J. . E-mail: andrew.allen@nist.gov; Thomas, Jeffrey J. . E-mail: jthomas@northwestern.edu

    2007-03-15

    The role of small-angle X-ray and neutron scattering (SAXS and SANS) in the characterization of cement is briefly reviewed. The unique information obtainable from SANS analysis of C-S-H gel in hydrating cement is compared with that obtainable by other neutron methods. Implications for the nature of C-S-H gel, as detected by SANS, are considered in relation to current models. Finally, the application of the SANS method to cement paste is demonstrated by analyzing the effects of calcium chloride acceleration and sucrose retardation on the resulting hydrated microstructure.

  14. Direct Observation Of Nanoparticle-Surfactant Interactions Using Small Angle Neutron Scattering

    NASA Astrophysics Data System (ADS)

    Kumar, Sugam; Aswal, V. K.

    2010-12-01

    Interactions of anionic silica nanoparticles with anionic, cationic and nonionic surfactants have directly been studied by contrast variation small angle neutron scattering (SANS). The measurements are performed on 1 wt% of both silica nanoparticles and surfactants of anionic sodium dodecyle sulphate (SDS), cationic dodecyltrimethyl ammonium bromide (DTAB) and non-ionic polyoxyethylene 10 lauryl ether (C12E10) in aqueous solution. We show that there is no direct interaction in the case of SDS with silica particles, whereas strong interaction for DTAB leads to the aggregation of silica particles. The interaction of C12E10 is found through the micelles adsorbed on the silica particles.

  15. From small angle x-ray scattering to reflectivity: Instrumentation and sample study

    SciTech Connect

    Hua, D.W.; Beaucage, G.; Kent, M.S.

    1996-02-01

    In this study, we described the first results from an x-ray reflectometer which has been modified from an existing Kratky small angle x-ray scattering (SAXS) camera at the UNM/Sandia scattering center. Typically, seven orders of magnitude of reflectivity can be obtained over a range of 0.02 to 0.5 A{sup {minus}1} in {ital q}. This allows the resolution of surface features of 10 to 1000 A. The conversion to reflectometer is reversible and can be achieved in a short time, allowing for dual use of an existing Kratky camera. {copyright} {ital 1996 Materials Research Society.}

  16. Correlation between fractal dimension and surface characterization by small angle X-ray scattering in marble.

    PubMed

    Salinas-Nolasco, Manlio Favio; Méndez-Vivar, Juan

    2010-03-16

    Among several analysis techniques applied to the study of surface passivation using dicarboxylic acids, small angle X-ray scattering (SAXS) has proved to be relevant in the physicochemical interpretation of the surface association resulting between calcium carbonate and the molecular structure of malonic acid. It is possible to establish chemical affinity principles through bidimensional geometric analysis in terms of the fractal dimension obtained experimentally by SAXS. In this Article, we present results about the adsorption of malonic acid on calcite, using theoretical and mathematical principles of the fractal dimension.

  17. Effect of Dzyaloshinski-Moriya interaction on elastic small-angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Michels, Andreas; Mettus, Denis; Honecker, Dirk; Metlov, Konstantin L.

    2016-08-01

    For magnetic materials containing many lattice imperfections (e.g., nanocrystalline magnets), the relativistic Dzyaloshinski-Moriya (DM) interaction may result in nonuniform spin textures due to the lack of inversion symmetry at interfaces. Within the framework of the continuum theory of micromagnetics, we explore the impact of the DM interaction on the elastic magnetic small-angle neutron scattering (SANS) cross section. It is shown that the DM interaction gives rise to a polarization-dependent asymmetric term in the spin-flip SANS cross section. Analysis of this feature may provide a means to determine the DM constant.

  18. Small-angle and surface scattering from porous and fractal materials.

    SciTech Connect

    Sinha, S. K.

    1998-09-18

    We review the basic theoretical methods used to treat small-angle scattering from porous materials, treated as general two-phase systems, and also the basic experimental techniques for carrying out such experiments. We discuss the special forms of the scattering when the materials exhibit mass or surface fractal behavior, and review the results of recent experiments on several types of porous media and also SANS experiments probing the phase behavior of binary fluid mixtures or polymer solutions confined in porous materials. Finally, we discuss the analogous technique of off-specular scattering from surfaces and interfaces which is used to study surface roughness of various kinds.

  19. Small Angle Neutron Scattering Observation of Chain Retraction after a Large Step Deformation

    SciTech Connect

    Blanchard, A.; Heinrich, M.; Pyckhout-Hintzen, W.; Richter, D.; Graham, R.S.; Likhtman, A.E.; McLeish, T.C.B.; Read, D.J.; Straube, E.; Kohlbrecher, J.

    2005-10-14

    The process of retraction in entangled linear chains after a fast nonlinear stretch was detected from time-resolved but quenched small angle neutron scattering (SANS) experiments on long, well-entangled polyisoprene chains. The statically obtained SANS data cover the relevant time regime for retraction, and they provide a direct, microscopic verification of this nonlinear process as predicted by the tube model. Clear, quantitative agreement is found with recent theories of contour length fluctuations and convective constraint release, using parameters obtained mainly from linear rheology. The theory captures the full range of scattering vectors once the crossover to fluctuations on length scales below the tube diameter is accounted for.

  20. Sample environments and techniques combined with small angle X-ray scattering.

    PubMed

    Bras, W; Ryan, A J

    1998-03-31

    The number of synchrotron radiation-based Small Angle X-ray Scattering beamlines has increased considerably over the last decade. With the high X-ray flux and collimation of these beamlines it not only has become possible to perform time-resolved experiments on time scales down to the millisecond/frame range, but also it allows experimenters to utilise new sample environments and use simultaneous several experimental techniques on one sample. An overview of recent developments in this field is given.

  1. Characterising density fluctuations in liquid yttria aluminates with small angle x-ray scattering

    SciTech Connect

    Greaves, G. Neville; Wilding, Martin C.; Vu Van, Quang; Majerus, Odile; Hennet, Louis

    2009-01-29

    Small angle x-ray scattering (SAXS) has been measured in the wavevector range 0.01

  2. Study of Nano-Precipitates Using Small-Angle Neutron Scattering

    SciTech Connect

    Chen, Wei-Ren

    2008-01-01

    Small-Angle-Neutron-Scattering (SANS) experiments were performed on a Ni-based nano-precipitate strengthened superalloy. A theoretical model for SANS absolute intensity distribution, I(Q), was developed to extract the structural properties. During the deformation process, a change in the morphology of precipitates was discovered. However, the average inter-precipitate distance and the average volume of precipitate were found to remain invariant. This microstructural information resolved by SANS is in good agreement with the results obtained from the quantitative transmission-electron-microscopy (TEM) image analysis.

  3. Small angle X-ray and neutron scattering on cadmium sulfide nanoparticles in silicate glass

    NASA Astrophysics Data System (ADS)

    Kuznetsova, Yu. V.; Rempel, A. A.; Meyer, M.; Pipich, V.; Gerth, S.; Magerl, A.

    2016-08-01

    Small angle X-ray and neutron scattering on Cd and S doped glass annealed at 600 °C shows after the first 12 h nucleation and growth of spherical CdS nanoparticles with a radius of up to 34±4 Å. After the nucleation is completed after 24 h, further growth in this amorphous environment is governed by oriented particle attachment mechanism as found for a liquid medium. Towards 48 h the particle shape has changed into spheroidal with short and long axis of 40±2 Å and 120±2 Å, respectively.

  4. DAMMIF, a program for rapid ab-initio shape determination in small-angle scattering

    PubMed Central

    Franke, Daniel; Svergun, Dmitri I.

    2009-01-01

    DAMMIF, a revised implementation of the ab-initio shape-determination program DAMMIN for small-angle scattering data, is presented. The program was fully rewritten, and its algorithm was optimized for speed of execution and modified to avoid limitations due to the finite search volume. Symmetry and anisometry constraints can be imposed on the particle shape, similar to DAMMIN. In equivalent conditions, DAMMIF is 25–40 times faster than DAMMIN on a single CPU. The possibility to utilize multiple CPUs is added to DAMMIF. The application is available in binary form for major platforms.

  5. Study of chemically unfolded β-casein by means of small-angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Aschi, Adel; Gharbi, Abdelhafidh; Daoud, Mohamed; Douillard, Roger; Calmettes, Patrick

    2007-01-01

    β-casein is a flexible amphiphilic milk protein which forms an unfolded conformation in presence of very high denaturant concentrations. The structure of β-casein formed at the bulk was studied by small-angle neutron scattering (SANS). The value of the second virial coefficient of the protein solutions indicates that the interactions between the polypeptide chain and solvent are repulsive. The protein conformation is similar to an excluded volume chain. The corresponding values of the contour length, L, the statistical length, b and the apparent radius of the chain cross-section, Rc are given.

  6. Small angle neutron scattering from nanocrystalline Pd and Co compacted at elevated temperatures

    SciTech Connect

    Sanders, P.G.; Weertman, J.R.; Barker, J.G.; Siegel, R.W.

    1994-05-01

    Nanocrystalline (n-) Cu and Pd, prepared by inert gas condensation and in situ room temperature (RT) and elevated temperature (warm) compactions, have been studied by small angle neutron scattering (SANS). Previous work on RT compacted and subsequently annealed n-Pd seemed to show that all the scattering could be accounted for by a distribution of pores. Analysis of more extensive SANS measurements, together with results of prompt gamma activation analysis, indicates that the SANS can be explained by the presence of pores and hydrogen. Warm compaction reduces the hydrogen impurity level, while increasing the bulk density and decreasing the pore size. This can lead to a dramatic hardness increase in these materials.

  7. Application of small-angle neutron scattering to the study of forces between magnetically chained monodisperse ferrofluid emulsion droplets

    SciTech Connect

    Jain, Dr Nirmesh; Liu, Dr C K; Hawkett, Dr B. S.; Warr, G. G.; Hamilton, William A

    2014-01-01

    The optical magnetic chaining technique (MCT) developed by Leal-Calderon, Bibette and co-workers in the 1990 s allows precise measurements of force profiles between droplets in monodisperse ferrofluid emulsions. However, the method lacks an in-situ determination of droplet size and therefore requires the combination of separately acquired measurements of droplet chain periodicity versus an applied magnetic field from optical Bragg scattering and droplet diameter inferred from dynamic light scattering (DLS) to recover surface force-distance profiles between the colloidal particles. Compound refractive lens (CRL) focussed small-angle scattering (SANS) MCT should result in more consistent measurements of droplet size (form factor measurements in the absence of field) and droplet chaining period (from structure factor peaks when the magnetic field is applied); and, with access to shorter length scales, extend force measurements to closer approaches than possible by optical measurements. We report on CRL-SANS measurements of monodisperse ferrofluid emulsion droplets aligned in straight chains by an applied field perpendicular to the incident beam direction. Analysis of the scattering from the closely spaced droplets required algorithms that carefully treated resolution and its effect on mean scattering vector magnitudes in order to determine droplet size and chain periods to sufficient accuracy. At lower applied fields scattering patterns indicate structural correlations transverse to the magnetic field direction due to the formation of intermediate structures in early chain growth.

  8. Wavelength-independent constant period spin-echo modulated small angle neutron scattering.

    PubMed

    Sales, Morten; Plomp, Jeroen; Habicht, Klaus; Tremsin, Anton; Bouwman, Wim; Strobl, Markus

    2016-06-01

    Spin-Echo Modulated Small Angle Neutron Scattering (SEMSANS) in Time-of-Flight (ToF) mode has been shown to be a promising technique for measuring (very) small angle neutron scattering (SANS) signals and performing quantitative Dark-Field Imaging (DFI), i.e., SANS with 2D spatial resolution. However, the wavelength dependence of the modulation period in the ToF spin-echo mode has so far limited the useful modulation periods to those resolvable with the limited spatial resolution of the detectors available. Here we present our results of an approach to keep the period of the induced modulation constant for the wavelengths utilised in ToF. This is achieved by ramping the magnetic fields in the coils responsible for creating the spatially modulated beam in synchronisation with the neutron pulse, thus keeping the modulation period constant for all wavelengths. Such a setup enables the decoupling of the spatial detector resolution from the resolution of the modulation period by the use of slits or gratings in analogy to the approach in grating-based neutron DFI.

  9. Small-angle neutron and dynamic light scattering study of gelatin coacervates

    NASA Astrophysics Data System (ADS)

    Mohanty, B.; Aswal, V. K.; Goyal, P. S.; Bohidar, H. B.

    2004-08-01

    The state of intermolecular aggregates and that of folded gelatin molecules could be characterized by dynamic laser light and small-angle neutron scattering experiments, which implied spontaneous segregation of particle sizes preceding coacervation, which is a liquid-liquid phase transition phenomenon. Dynamic light scattering (DLS) data analysis revealed two particle sizes until precipitation was reached. The smaller particles having a diameter of 50 nm (stable nanoparticles prepared by coacervation method) were detected in the supernatant, whereas the inter-molecular aggregates having a diameter of 400 nm gave rise to coacervation. Small-angle neutron scattering (SANS) experiments revealed that typical mesh size of the networks exist in polymer dense phase (coacervates) [1]. Analysis of the SANS structure factor showed the presence of two length scales associated with this system that were identified as the correlation length or mesh size, xi = 10.6 Å of the network and the other is the size of inhomogeneities = 21.4 Å. Observations were discussed based on the results obtained from SANS experiments performed in 5% (w/v) gelatin solution at 60oC (xi = 50 Å, zeta = 113 Å) and 5% (w/v) gel at 28oC (xi = 47 Å, zeta = 115 Å) in aqueous phase [2] indicating smaller length scales in coacervate as compared to sol and gel.

  10. SASfit: a tool for small-angle scattering data analysis using a library of analytical expressions

    PubMed Central

    Breßler, Ingo; Kohlbrecher, Joachim; Thünemann, Andreas F.

    2015-01-01

    SASfit is one of the mature programs for small-angle scattering data analysis and has been available for many years. This article describes the basic data processing and analysis workflow along with recent developments in the SASfit program package (version 0.94.6). They include (i) advanced algorithms for reduction of oversampled data sets, (ii) improved confidence assessment in the optimized model parameters and (iii) a flexible plug-in system for custom user-provided models. A scattering function of a mass fractal model of branched polymers in solution is provided as an example for implementing a plug-in. The new SASfit release is available for major platforms such as Windows, Linux and MacOS. To facilitate usage, it includes comprehensive indexed documentation as well as a web-based wiki for peer collaboration and online videos demonstrating basic usage. The use of SASfit is illustrated by interpretation of the small-angle X-ray scattering curves of monomodal gold nanoparticles (NIST reference material 8011) and bimodal silica nanoparticles (EU reference material ERM-FD-102). PMID:26500467

  11. Small-angle neutron and X-ray scattering reveal conformational changes in rhodopsin activation

    NASA Astrophysics Data System (ADS)

    Shrestha, Utsab R.; Bhowmik, Debsindhu; Perera, Suchitrhanga M. C. D.; Chawla, Udeep; Struts, Andrey V.; Graziono, Vito; Pingali, Sai Venkatesh; Heller, William T.; Qian, Shuo; Brown, Michael F.; Chu, Xiang-Qiang

    2015-03-01

    Understanding G-protein-coupled receptor (GPCR) activation plays a crucial role in the development of novel improved molecular drugs. During photo-activation, the retinal chromophore of the visual GPCR rhodopsin isomerizes from 11-cis to all-trans conformation, yielding an equilibrium between inactive Meta-I and active Meta-II states. The principal goals of this work are to address whether the activation of rhodopsin leads to a single state or a conformational ensemble, and how protein organizational structure changes with detergent environment in solution. We use both small-angle neutron scattering (SANS) and small-angle X-ray scattering (SAXS) techniques to answer the above questions. For the first time we observe the change in protein conformational ensemble upon photo-activation by SANS with contrast variation, which enables the separate study of the protein structure within the detergent assembly. In addition, SAXS study of protein structure within detergent assembly suggests that the detergent molecules form a belt of monolayer (micelle) around protein with different geometrical shapes to keep the protein in folded state.

  12. Small-angle scattering for structural biology—Expanding the frontier while avoiding the pitfalls

    PubMed Central

    Jacques, David A; Trewhella, Jill

    2010-01-01

    The last decade has seen a dramatic increase in the use of small-angle scattering for the study of biological macromolecules in solution. The drive for more complete structural characterization of proteins and their interactions, coupled with the increasing availability of instrumentation and easy-to-use software for data analysis and interpretation, is expanding the utility of the technique beyond the domain of the biophysicist and into the realm of the protein scientist. However, the absence of publication standards and the ease with which 3D models can be calculated against the inherently 1D scattering data means that an understanding of sample quality, data quality, and modeling assumptions is essential to have confidence in the results. This review is intended to provide a road map through the small-angle scattering experiment, while also providing a set of guidelines for the critical evaluation of scattering data. Examples of current best practice are given that also demonstrate the power of the technique to advance our understanding of protein structure and function. PMID:20120026

  13. A Hierarchical Algorithm for Fast Debye Summation with Applications to Small Angle Scattering

    PubMed Central

    Gumerov, Nail A.; Berlin, Konstantin; Fushman, David; Duraiswami, Ramani

    2012-01-01

    Debye summation, which involves the summation of sinc functions of distances between all pair of atoms in three dimensional space, arises in computations performed in crystallography, small/wide angle X-ray scattering (SAXS/WAXS) and small angle neutron scattering (SANS). Direct evaluation of Debye summation has quadratic complexity, which results in computational bottleneck when determining crystal properties, or running structure refinement protocols that involve SAXS or SANS, even for moderately sized molecules. We present a fast approximation algorithm that efficiently computes the summation to any prescribed accuracy ε in linear time. The algorithm is similar to the fast multipole method (FMM), and is based on a hierarchical spatial decomposition of the molecule coupled with local harmonic expansions and translation of these expansions. An even more efficient implementation is possible when the scattering profile is all that is required, as in small angle scattering reconstruction (SAS) of macromolecules. We examine the relationship of the proposed algorithm to existing approximate methods for profile computations, and show that these methods may result in inaccurate profile computations, unless an error bound derived in this paper is used. Our theoretical and computational results show orders of magnitude improvement in computation complexity over existing methods, while maintaining prescribed accuracy. PMID:22707386

  14. A small-angle x-ray scattering system with a vertical layout

    NASA Astrophysics Data System (ADS)

    Wang, Zhen; Chen, Xiaowei; Meng, Lingpu; Cui, Kunpeng; Wu, Lihui; Li, Liangbin

    2014-12-01

    A small-angle x-ray scattering (SAXS) system with a vertical layout (V-SAXS) has been designed and constructed for in situ detection on nanostructures, which is well suitable for in situ study on self-assembly of nanoparticles at liquid interface and polymer processing. A steel-tower frame on a reinforced basement is built as the supporting skeleton for scattering beam path and detector platform, ensuring the system a high working stability and a high operating accuracy. A micro-focus x-ray source combining parabolic three-dimensional multi-layer mirror and scatteringless collimation system provides a highly parallel beam, which allows us to detect the very small angle range. With a sample-to-detector distance of 7 m, the largest measurable length scale is 420 nm in real space. With a large sample zone, it is possible to install different experimental setups such as film stretching machine, which makes the system perfect to follow the microstructures evolution of materials during processing. The capability of the V-SAXS on in situ study is tested with a drying experiment of a free latex droplet, which confirms our initial design.

  15. Laser desorption mass spectrometry and small angle neutron scattering of heavy fossil materials

    SciTech Connect

    Hunt, J.E.; Winans, R.E.; Thiyagarajan, P.

    1997-09-01

    The determination of the structural building blocks and the molecular weight range of heavy hydrocarbon materials is of crucial importance in research on their reactivity and for their processing. The chemically and physically heterogenous nature of heavy hydrocarbon materials, such as coals, heavy petroleum fractions, and residues, dictates that their structure and reactivity patterns be complicated. The problem is further complicated by the fact that the molecular structure and molecular weight distribution of these materials is not dependent on a single molecule, but on a complex mixture of molecules which vary among coals and heavy petroleum samples. Laser Desorption mass spectrometry (LDMS) is emerging as a technique for molecular weight determination having found widespread use in biological polymer research, but is still a relatively new technique in the fossil fuel area. Small angle neutron scattering (SANS) provides information on the size and shape of heavy fossil materials. SANS offers the advantages of high penetration power even in thick cells at high temperatures and high contrast for hydrocarbon systems dispersed in deuterated solvents. LDMS coupled with time of flight has the advantages of high sensitivity and transmission and high mass range. We have used LDMS to examine various heavy fossil-derived materials including: long chain hydrocarbons, asphaltenes from petroleum vacuum resids, and coals. This paper describes the application of laser desorption and small angle neutron scattering techniques to the analysis of components in coals, petroleum resids and unsaturated polymers.

  16. A small-angle x-ray scattering system with a vertical layout.

    PubMed

    Wang, Zhen; Chen, Xiaowei; Meng, Lingpu; Cui, Kunpeng; Wu, Lihui; Li, Liangbin

    2014-12-01

    A small-angle x-ray scattering (SAXS) system with a vertical layout (V-SAXS) has been designed and constructed for in situ detection on nanostructures, which is well suitable for in situ study on self-assembly of nanoparticles at liquid interface and polymer processing. A steel-tower frame on a reinforced basement is built as the supporting skeleton for scattering beam path and detector platform, ensuring the system a high working stability and a high operating accuracy. A micro-focus x-ray source combining parabolic three-dimensional multi-layer mirror and scatteringless collimation system provides a highly parallel beam, which allows us to detect the very small angle range. With a sample-to-detector distance of 7 m, the largest measurable length scale is 420 nm in real space. With a large sample zone, it is possible to install different experimental setups such as film stretching machine, which makes the system perfect to follow the microstructures evolution of materials during processing. The capability of the V-SAXS on in situ study is tested with a drying experiment of a free latex droplet, which confirms our initial design.

  17. Small angle scattering methods to study porous materials under high uniaxial strain

    SciTech Connect

    Le Floch, Sylvie Balima, Félix; Pischedda, Vittoria; Legrand, Franck; San-Miguel, Alfonso

    2015-02-15

    We developed a high pressure cell for the in situ study of the porosity of solids under high uniaxial strain using neutron small angle scattering. The cell comprises a hydraulically actioned piston and a main body equipped with two single-crystal sapphire windows allowing for the neutron scattering of the sample. The sample cavity is designed to allow for a large volume variation as expected when compressing highly porous materials. We also implemented a loading protocol to adapt an existing diamond anvil cell for the study of porous materials by X-ray small angle scattering under high pressure. The two techniques are complementary as the radiation beam and the applied pressure are in one case perpendicular to each other (neutron cell) and in the other case parallel (X-ray cell). We will illustrate the use of these two techniques in the study of lamellar porous systems up to a maximum pressure of 0.1 GPa and 0.3 GPa for the neutron and X-ray cells, respectively. These devices allow obtaining information on the evolution of porosity with pressure in the pore dimension subdomain defined by the wave-numbers explored in the scattering process. The evolution with the applied load of such parameters as the fractal dimension of the pore-matrix interface or the apparent specific surface in expanded graphite and in expanded vermiculite is used to illustrate the use of the high pressure cells.

  18. Uncertainties in Small-Angle Measurement Systems Used to Calibrate Angle Artifacts.

    PubMed

    Stone, Jack A; Amer, Mohamed; Faust, Bryon; Zimmerman, Jay

    2004-01-01

    We have studied a number of effects that can give rise to errors in small-angle measurement systems when they are used to calibrate artifacts such as optical polygons. Of these sources of uncertainty, the most difficult to quantify are errors associated with the measurement of imperfect, non-flat faces of the artifact, causing the instrument to misinterpret the average orientation of the surface. In an attempt to shed some light on these errors, we have compared autocollimator measurements to angle measurements made with a Fizeau phase-shifting interferometer. These two instruments have very different operating principles and implement different definitions of the orientation of a surface, but (surprisingly) we have not yet seen any clear differences between results obtained with the autocollimator and with the interferometer. The interferometer is in some respects an attractive alternative to an autocollimator for small-angle measurement; it implements an unambiguous and robust definition of surface orientation in terms of the tilt of a best-fit plane, and it is easier to quantify likely errors of the interferometer measurements than to evaluate autocollimator uncertainty.

  19. Uncertainties in Small-Angle Measurement Systems Used to Calibrate Angle Artifacts

    PubMed Central

    Stone, Jack A.; Amer, Mohamed; Faust, Bryon; Zimmerman, Jay

    2004-01-01

    We have studied a number of effects that can give rise to errors in small-angle measurement systems when they are used to calibrate artifacts such as optical polygons. Of these sources of uncertainty, the most difficult to quantify are errors associated with the measurement of imperfect, non-flat faces of the artifact, causing the instrument to misinterpret the average orientation of the surface. In an attempt to shed some light on these errors, we have compared autocollimator measurements to angle measurements made with a Fizeau phase-shifting interferometer. These two instruments have very different operating principles and implement different definitions of the orientation of a surface, but (surprisingly) we have not yet seen any clear differences between results obtained with the autocollimator and with the interferometer. The interferometer is in some respects an attractive alternative to an autocollimator for small-angle measurement; it implements an unambiguous and robust definition of surface orientation in terms of the tilt of a best-fit plane, and it is easier to quantify likely errors of the interferometer measurements than to evaluate autocollimator uncertainty. PMID:27366616

  20. Small-Angle Neutron Scattering for Structural Biology of Protein-RNA Complexes.

    PubMed

    Gabel, Frank

    2015-01-01

    This chapter deals with the applications of small-angle neutron scattering (SANS) for the structural study of protein-RNA complexes in solution. After a brief historical introduction, the basic theory and practical requirements (e.g., sample state) for SANS experiments will be treated. Next, model-free parameters, such as the molecular mass and the radius of gyration, which can be obtained without a priori structural information, will be introduced. A more detailed section on the specific properties of SANS (with respect to its sister technique, small-angle X-ray scattering), and their implications on possibilities and limits of model building and interpretation will be discussed with a focus on protein-RNA systems. A practical illustration of the information content of SANS data will be given by applying ab initio modeling to a tRNA-synthetase system of known high-resolution structure. Finally, two present state-of-the-art examples that combine SANS data with complementary structural biology techniques (NMR and crystallography) will be presented and possible future developments and applications will be discussed.

  1. Wavelength-independent constant period spin-echo modulated small angle neutron scattering.

    PubMed

    Sales, Morten; Plomp, Jeroen; Habicht, Klaus; Tremsin, Anton; Bouwman, Wim; Strobl, Markus

    2016-06-01

    Spin-Echo Modulated Small Angle Neutron Scattering (SEMSANS) in Time-of-Flight (ToF) mode has been shown to be a promising technique for measuring (very) small angle neutron scattering (SANS) signals and performing quantitative Dark-Field Imaging (DFI), i.e., SANS with 2D spatial resolution. However, the wavelength dependence of the modulation period in the ToF spin-echo mode has so far limited the useful modulation periods to those resolvable with the limited spatial resolution of the detectors available. Here we present our results of an approach to keep the period of the induced modulation constant for the wavelengths utilised in ToF. This is achieved by ramping the magnetic fields in the coils responsible for creating the spatially modulated beam in synchronisation with the neutron pulse, thus keeping the modulation period constant for all wavelengths. Such a setup enables the decoupling of the spatial detector resolution from the resolution of the modulation period by the use of slits or gratings in analogy to the approach in grating-based neutron DFI. PMID:27370470

  2. A small-angle x-ray scattering system with a vertical layout

    SciTech Connect

    Wang, Zhen; Chen, Xiaowei; Meng, Lingpu; Cui, Kunpeng; Wu, Lihui; Li, Liangbin

    2014-12-15

    A small-angle x-ray scattering (SAXS) system with a vertical layout (V-SAXS) has been designed and constructed for in situ detection on nanostructures, which is well suitable for in situ study on self-assembly of nanoparticles at liquid interface and polymer processing. A steel-tower frame on a reinforced basement is built as the supporting skeleton for scattering beam path and detector platform, ensuring the system a high working stability and a high operating accuracy. A micro-focus x-ray source combining parabolic three-dimensional multi-layer mirror and scatteringless collimation system provides a highly parallel beam, which allows us to detect the very small angle range. With a sample-to-detector distance of 7 m, the largest measurable length scale is 420 nm in real space. With a large sample zone, it is possible to install different experimental setups such as film stretching machine, which makes the system perfect to follow the microstructures evolution of materials during processing. The capability of the V-SAXS on in situ study is tested with a drying experiment of a free latex droplet, which confirms our initial design.

  3. Morphological characterization of carbon-nanofiber-reinforced epoxy nanocomposites using ultra-small angle scattering

    SciTech Connect

    Justice, R.S.; Anderson, D.P.; Brown, J.M.; Arlen, M.J.; Colleary, A.J.; Lafdi, K.; Schaefer, D.W.

    2010-07-01

    Studies of the properties of nanocomposites reinforced with vapor-grown carbon nanofibers (VGCFs) can be found throughout the literature. Electrical, mechanical, viscoelastic, and rheological properties are just a few of the characteristics that have been well discussed. Although these properties depend on morphology, morphological characterization is rare. Due to its 2-dimensional nature, microscopy is of limited value when analyzing network morphologies. This work will show how the characterization of the three-dimensional geometry and network formation of VGCFs can be determined using ultra-small angle scattering techniques. Ultra-small angle x-ray and neutron scattering (USAXS and USANS) were used to characterize the morphology of carbon nanofibers suspended in epoxy. Using a simplified tube model, we estimate the dimensions of suspended fibers. The assumption of tubular fibers accounts for the increased surface area observed with USAXS that is not accounted for using a solid rod model. Furthermore, USANS was used to search for a structural signature associated with the electrical percolation threshold. USANS extends to longer dimensional scales than USAXS, which measures a smaller range of momentum transfer. To determine the electrical percolation threshold, AC impedance spectroscopy was employed to verify that an electrically conductive, percolated network forms at VGCNF loadings of 0.8% < CNF wt% < 1.2%. These values correlate with the USANS data, where a morphological transition is seen at {approx}1.2% loading.

  4. Wavelength-independent constant period spin-echo modulated small angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Sales, Morten; Plomp, Jeroen; Habicht, Klaus; Tremsin, Anton; Bouwman, Wim; Strobl, Markus

    2016-06-01

    Spin-Echo Modulated Small Angle Neutron Scattering (SEMSANS) in Time-of-Flight (ToF) mode has been shown to be a promising technique for measuring (very) small angle neutron scattering (SANS) signals and performing quantitative Dark-Field Imaging (DFI), i.e., SANS with 2D spatial resolution. However, the wavelength dependence of the modulation period in the ToF spin-echo mode has so far limited the useful modulation periods to those resolvable with the limited spatial resolution of the detectors available. Here we present our results of an approach to keep the period of the induced modulation constant for the wavelengths utilised in ToF. This is achieved by ramping the magnetic fields in the coils responsible for creating the spatially modulated beam in synchronisation with the neutron pulse, thus keeping the modulation period constant for all wavelengths. Such a setup enables the decoupling of the spatial detector resolution from the resolution of the modulation period by the use of slits or gratings in analogy to the approach in grating-based neutron DFI.

  5. Small angle scattering methods to study porous materials under high uniaxial strain.

    PubMed

    Le Floch, Sylvie; Balima, Félix; Pischedda, Vittoria; Legrand, Franck; San-Miguel, Alfonso

    2015-02-01

    We developed a high pressure cell for the in situ study of the porosity of solids under high uniaxial strain using neutron small angle scattering. The cell comprises a hydraulically actioned piston and a main body equipped with two single-crystal sapphire windows allowing for the neutron scattering of the sample. The sample cavity is designed to allow for a large volume variation as expected when compressing highly porous materials. We also implemented a loading protocol to adapt an existing diamond anvil cell for the study of porous materials by X-ray small angle scattering under high pressure. The two techniques are complementary as the radiation beam and the applied pressure are in one case perpendicular to each other (neutron cell) and in the other case parallel (X-ray cell). We will illustrate the use of these two techniques in the study of lamellar porous systems up to a maximum pressure of 0.1 GPa and 0.3 GPa for the neutron and X-ray cells, respectively. These devices allow obtaining information on the evolution of porosity with pressure in the pore dimension subdomain defined by the wave-numbers explored in the scattering process. The evolution with the applied load of such parameters as the fractal dimension of the pore-matrix interface or the apparent specific surface in expanded graphite and in expanded vermiculite is used to illustrate the use of the high pressure cells.

  6. Structural analysis of Fe–Mn–O nanoparticles in glass ceramics by small angle scattering

    SciTech Connect

    Raghuwanshi, Vikram Singh; Harizanova, Ruzha; Tatchev, Dragomir; Hoell, Armin; Rüssel, Christian

    2015-02-15

    Magnetic nanocrystals containing Fe and Mn were obtained by annealing of silicate glasses with the composition 13.6Na{sub 2}O–62.9SiO{sub 2}–8.5MnO–15.0Fe{sub 2}O{sub 3−x} (mol%) at 580 °C for different periods of time. Here, we present Small Angle Neutron Scattering using Polarized neutrons (SANSPOL) and Anomalous Small Angle X-ray Scattering (ASAXS) investigation on these glass ceramic samples. Analysis of scattering data from both methods reveals the formation of spherical core–shell type of nanoparticles with mean sizes between 10 nm and 100 nm. ASAXS investigation shows the particles have higher concentration of iron atoms and the shell like region surrounding the particles is enriched in SiO{sub 2}. SANSPOL investigation shows the particles are found to be magnetic and are surrounded by a non-magnetic shell-like region. - Graphical abstract: Magnetic spherical core–shell nanoparticles in glass ceramics: SANSPOL and ASAXS investigations. - Highlights: • Formation and growth mechanisms of magnetic nanoparticles in silicate glass. • SANSPOL and ASAXS methods employed to evaluate quantitative information. • Analyses showed formation of nanoparticles with spherical core–shell structures. • Core of the particle is magnetic and surrounded by weak magnetic shell like region.

  7. Irradiation Induced Defect Characterization in Reactor Pressure Vessel Steel by Small Angle Neutron Scattering

    NASA Astrophysics Data System (ADS)

    Han, Yougn-Soo; Shin, Eun-Joo; Lee, Chang-Hee; Park, Duck-Gun

    The degradation of the mechanical properties of the RPV (Reactor Pressure Vessel) steel during an irradiation in a nuclear power plant is closely related to the irradiation induced defects. The size of these defects is known to be a few nanometer, and the small angle neutron scattering technique is regarded as the best non destructive technique to characterize the nano sized inhomogeneities in bulk samples. The investigated the RPV steel has been used in YeongKwang nuclear power plant at Korea and the Cu content of the RPV steel is 0.06 wt%. The RPV steel was irradiated in the HANARO reactor at KAERI. The small angle neutron scattering experiments were performed by the SANS instrument in the HANARO reactor. The nano sized irradiation induced defects were quantitatively analyzed by SANS and the type of the irradiation induced defects was discussed in detail. The relation between irradiation induced defects and the yield strength was investigated. The characteristics of irradiation induced defects in low Cu containing RPV steel were discussed.

  8. Crystal structure analysis in solution-processed uniaxially oriented polycrystalline thin film of non-peripheral octahexyl phthalocyanine by grazing incidence wide-angle x-ray scattering techniques

    NASA Astrophysics Data System (ADS)

    Ohmori, Masashi; Uno, Takashi; Nakatani, Mitsuhiro; Nakano, Chika; Fujii, Akihiko; Ozaki, Masanori

    2016-10-01

    Uniaxially oriented thin films of metal-free non-peripherally octahexyl-substituted phthalocyanine (C6PcH2), which exhibits high carrier mobility, have been fabricated by the bar-coating technique, which is a simple solution process. The molecular orientation and molecular steps in the thin film were observed by the polarized spectroscopy and the atomic force microscopy, respectively. The three-dimensional molecular packing structure in the thin film was investigated by the grazing incidence wide-angle X-ray scattering technique with an in-plane sample rotation. The crystal orientation was clarified, and the three-dimensional molecular packing structure of the thin film was found to match the single crystal structure. Moreover, the X-ray diffraction patterns of the oriented thin films were simulated by using the lattice parameters of C6PcH2 single crystal to reproduce the observed X-ray diffraction patterns.

  9. Effects of oxygen partial pressure and annealing temperature on the residual stress of hafnium oxide thin-films on silicon using synchrotron-based grazing incidence X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Biswas, Debaleen; Sinha, Anil Kumar; Chakraborty, Supratic

    2016-10-01

    Synchrotron radiation-based grazing incidence X-ray diffraction (GI-XRD) technique is employed here to estimate the residual stress of < 10 nm thin hafnium oxide film deposited on Si (100) substrate at different argon/oxygen ratios using reactive rf sputtering. A decrease in residual stress, tensile in nature, is observed at higher annealing temperature for the samples deposited with increasing argon ratio in the Ar/O2 plasma. The residual stress of the films deposited at higher pAr (Ar:O2 = 4:1) is also found to be decreased with increasing annealing temperature. But the stress is more or less constant with annealing temperature for the films deposited at lower Ar/O2 (1:4) ratio. All the above phenomena can be explained on the basis of swelling of the interfacial layer and enhanced structural relaxation in the presence of excess Hf in hafnium oxide film during deposition.

  10. Observation of Enhancement of the Morin Transition Temperature in Iridium-Doped α-Fe2O3 Thin Film by 57Fe-Grazing Incidence Synchrotron Radiation Mössbauer Spectroscopy

    NASA Astrophysics Data System (ADS)

    Mitsui, Takaya; Mibu, Ko; Seto, Makoto; Kurokuzu, Masayuki; Pati, Satya Prakash; Nozaki, Tomohiro; Sahashi, Masashi

    2016-06-01

    The Morin transition of a (0001)-oriented iridium-doped α-Fe2O3 thin film deposited on an Al2O3(0001) substrate was studied by 57Fe-grazing incidence synchrotron radiation Mössbauer spectroscopy (GISRMS). Temperature-dependent spectra proved that the iridium doping markedly enhanced the Morin temperature of the α-Fe2O3 thin film; the iron spin directions were perpendicular to the film plane at temperatures below 100 °C, while they were in-plane at temperatures above 150 °C. The antiferromagnetic ordering was maintained far above 400 °C. The results demonstrated the availabilities of 57Fe-GISRMS, which enables a very quick evaluation of the magnetism in antiferromagnetic ultrathin films at high temperatures.

  11. Pinhole-type two-dimensional ultra-small-angle X-ray scattering on the micrometer scale.

    PubMed

    Kishimoto, Hiroyuki; Shinohara, Yuya; Suzuki, Yoshio; Takeuchi, Akihisa; Yagi, Naoto; Amemiya, Yoshiyuki

    2014-01-01

    A pinhole-type two-dimensional ultra-small-angle X-ray scattering set-up at a so-called medium-length beamline at SPring-8 is reported. A long sample-to-detector distance, 160.5 m, can be used at this beamline and a small-angle resolution of 0.25 µm(-1) was thereby achieved at an X-ray energy of 8 keV. PMID:24365910

  12. Pinhole-type two-dimensional ultra-small-angle X-ray scattering on the micrometer scale

    PubMed Central

    Kishimoto, Hiroyuki; Shinohara, Yuya; Suzuki, Yoshio; Takeuchi, Akihisa; Yagi, Naoto; Amemiya, Yoshiyuki

    2014-01-01

    A pinhole-type two-dimensional ultra-small-angle X-ray scattering set-up at a so-called medium-length beamline at SPring-8 is reported. A long sample-to-detector distance, 160.5 m, can be used at this beamline and a small-angle resolution of 0.25 µm−1 was thereby achieved at an X-ray energy of 8 keV. PMID:24365910

  13. Structure-property relationships in Waspaloy via small angle scattering and electrical resistivity measurements

    SciTech Connect

    Whelchel, R.; Gerhardt, Dr. Rosario; Littrell, Ken

    2010-01-01

    The mechanical properties in superalloys are controlled by the distribution of the {gamma}{prime} precipitate phase. Electrical measurements have been shown to be sensitive to certain aspects of the precipitation process and show promise for predicting the evolving microstructural state in superalloys. Aging experiments were conducted on Waspaloy samples for temperatures between 600 and 950 C for times ranging from 2min to 500h. Particle size distributions were obtained by modeling of small angle scattering (SAS) data, whereas, small precipitate size information, strain, and lattice mismatch data were obtained from X-ray diffraction. The microstructural information was then used to create a figure of merit of electron scattering intended to correlate electrical properties to the precipitate microstructure. The proposed figure of merit shows an empirical correlation with the electrical resistivity data, demonstrating the sensitivity of the resistivity measurements to the precipitation process and coarsening behavior.

  14. Convex and concave successions of power-law decays in small-angle scattering

    NASA Astrophysics Data System (ADS)

    Anitas, E. M.

    2016-08-01

    The small-angle scattering (SAS) structure factor from a new model of a 3D deterministic fractal in which the relative positions and the number of structural units vary with fractal iteration number is calculated. It is shown that, depending on the relative positions of scattering units inside the fractal, we can obtain various types of power-law successions, such as: convex/concave - when the absolute value of the scattering exponent of the first power-law decay is higher/smaller than that of the subsequent power- law decay, or any combination of them (i.e. convex-concave or concave-convex). The obtained results can explain experimental SAS (neutron or X-rays) data which are characterized by a succession of power-law decays of arbitrary length.

  15. Time resolved small angle x-ray scattering reactivity studies on coals, asphaltenes, and polymers.

    SciTech Connect

    Seifert, S.; Thiyagarajan, P.; Winans, R. E.

    1999-07-02

    The objective of this study is to examine changes in the structures of coals, asphaltenes, and polymers in situ with small angle X-ray scattering (SAXS) during thermal treatments. We have built a SAXS instrument at the Basic Energy Sciences Synchrotrons Radiation Center at the Advanced Photon Source that allows us to obtain scattering data on very small samples and in the millisecond time domain. The Argonne Premium Coal samples, petroleum derived asphaltenes, and polymers with functionality to model fossil fuels were used in this study. The information that can be derived from these experiments includes: changes in fractal dimensionality, surface topology, and size and type of porosity. The information is correlated with other methods on the same samples.

  16. Small-Angle X-Ray Scattering From RNA, Proteins, And Protein Complexes

    SciTech Connect

    Lipfert, Jan; Doniach, Sebastian; /Stanford U., Phys. Dept. /Stanford U., Appl. Phys. Dept. /SLAC, SSRL

    2007-09-18

    Small-angle X-ray scattering (SAXS) is increasingly used to characterize the structure and interactions of biological macromolecules and their complexes in solution. Although still a low-resolution technique, the advent of high-flux synchrotron sources and the development of algorithms for the reconstruction of 3-D electron density maps from 1-D scattering profiles have made possible the generation of useful low-resolution molecular models from SAXS data. Furthermore, SAXS is well suited for the study of unfolded or partially folded conformational ensembles as a function of time or solution conditions. Here, we review recently developed algorithms for 3-D structure modeling and applications to protein complexes. Furthermore, we discuss the emerging use of SAXS as a tool to study membrane protein-detergent complexes. SAXS is proving useful to study the folding of functional RNA molecules, and finally we discuss uses of SAXS to study ensembles of denatured proteins.

  17. Sample holder for small-angle x-ray scattering static and flow cell measurements

    SciTech Connect

    Lipfert, Jan; Millett, Ian S.; Seifert, Soenke; Doniach, Sebastian

    2006-04-15

    We present the design of a sample holder for small-angle x-ray scattering (SAXS) that can be used for both static and flow cell measurements, allowing to switch between these two types of measurement without having to realign the detector and camera geometry. The device makes possible high signal-to-noise experiments with sample volumes as small as 16 {mu}l and can be thermocontrolled using a standard circulating water bath. The setup has been used successfully for a range of biological SAXS measurements, including peptides, detergent micelles, membrane proteins, and nucleic acids. As a performance test, we present scattering data for horse heart cytochrome c, collected at the BESSRC CAT beam line 12-ID of the Advanced Photon Source. The design drawings are provided in the supplementary material.

  18. Clustering of water molecules in ultramicroporous carbon: In-situ small-angle neutron scattering

    DOE PAGES

    Bahadur, Jitendra; Contescu, Cristian I.; Rai, Durgesh K.; Gallego, Nidia C.; Melnichenko, Yuri B.

    2016-10-19

    The adsorption of water is central to most of the applications of microporous carbon as adsorbent material. We report early kinetics of water adsorption in the microporous carbon using in-situ small-angle neutron scattering. It is observed that adsorption of water occurs via cluster formation of molecules. Interestingly, the cluster size remains constant throughout the adsorption process whereas number density of clusters increases with time. The role of surface chemistry of microporous carbon on the early kinetics of adsorption process was also investigated. Lastly, the present study provides direct experimental evidence for cluster assisted adsorption of water molecules in microporous carbonmore » (Do-Do model).« less

  19. Nanopores in track-etched polymer membranes characterized by small-angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Cornelius, T. W.; Schiedt, B.; Severin, D.; Pépy, G.; Toulemonde, M.; Apel, P. Yu; Boesecke, P.; Trautmann, C.

    2010-04-01

    Nanochannels and nanowires with diameters ranging from 30 to 400 nm were produced by etching ion tracks in thin polyarylate and polycarbonate foils. The shape and the size distribution of dry and wet nanochannels, as well as of nanowires grown therein, were examined by small-angle x-ray scattering. The x-ray intensity as a function of the scattering vector exhibits pronounced oscillations showing that both the channels and the wires have a highly cylindrical geometry and a very narrow size distribution. UV exposure before chemical etching significantly improves the monodispersity of the nanopores. For fixed etching conditions, the scattering patterns provide evidence that the diameter of dry and water-filled channels as well as for embedded nanowires are identical, demonstrating that the pores in the polymer are completely filled.

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

    SciTech Connect

    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.

  1. The crystallization of hectorite clays as monitored by small angle X-ray scattering and NMR

    SciTech Connect

    Carrado, K. A.; Xu, L.; Seifert, S.; Gregory, D.; Song, K.; Botto, R. E.

    1999-12-13

    The authors have probed the 48-hr crystallization of a magnesium silicate clay called hectorite. Small angle X-ray scattering (SAXS) at the Advanced Photon Source using aliquots ex situ has revealed that data is consistent with ex situ XRD, TGA, AFM, and IR data in that all these techniques see clay crystallite beginning to form in the first few hours of reaction. Tetraethylammonium (TEA) ions are used to aid crystallization and become incorporated as the exchange cations within the interlayers. {sup 13}C NMR shows that 80% of the final TEA loading is accomplished in the first 10 hrs. {sup 29}Si NMR displays a visible clay silicate peak after just 1 hr. In addition, the first in situ study of clay crystallization of any kind was performed by in situ SAXS. Results are consistent with the ex situ data as well as showing the sensitivity of SAXS to sol gel reactions occurring on the order of minutes.

  2. Small-angle neutron scattering and molecular dynamics structural study of gelling DNA nanostars.

    PubMed

    Fernandez-Castanon, J; Bomboi, F; Rovigatti, L; Zanatta, M; Paciaroni, A; Comez, L; Porcar, L; Jafta, C J; Fadda, G C; Bellini, T; Sciortino, F

    2016-08-28

    DNA oligomers with properly designed sequences self-assemble into well defined constructs. Here, we exploit this methodology to produce bulk quantities of tetravalent DNA nanostars (each one composed of 196 nucleotides) and to explore the structural signatures of their aggregation process. We report small-angle neutron scattering experiments focused on the evaluation of both the form factor and the temperature evolution of the scattered intensity at a nanostar concentration where the system forms a tetravalent equilibrium gel. We also perform molecular dynamics simulations of one isolated tetramer to evaluate the form factor numerically, without resorting to any approximate shape. The numerical form factor is found to be in very good agreement with the experimental one. Simulations predict an essentially temperature-independent form factor, offering the possibility to extract the effective structure factor and its evolution during the equilibrium gelation. PMID:27586949

  3. Small angle x-ray diffraction studies of mucopolysaccharides in collagen.

    PubMed Central

    Lam, R; Claffey, W J; Geil, P H

    1978-01-01

    Small angle X-ray diffraction (SAXD) was used to locate mucopolysaccharides (MPS) at regular intervals along the collagen axis under physiological conditions. Ruthenium red was used to stain the MPS specifically. The difference in electron density between ruthenium red-stained and unstained moist native rat tail tendon should correspond to the position of the MPS. This difference was calculated from the SAXD intensity data by using difference Fourier transform calculations. Phases calculated independently from the amino acid sequence of collagen by two laboratories were used in this calculation, and the results were compared. At least four to seven bands of MPS per 660 A were found at regular intervals along the collagen axis. Some of these bands match in position to the cross-striations observed by freeze-etching. Electron micrographs of ruthenium red-stained native fibrils also showed bands close in position to the ones calculated. Images FIGURE 3 FIGURE 4 FIGURE 6 FIGURE 7 PMID:83884

  4. A microstructural comparison of two nuclear-grade martensitic steels using small-angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Coppola, R.; Fiori, F.; Little, E. A.; Magnani, M.

    1997-06-01

    Results are presented of a small-angle neutron scattering (SANS) study on two 10-13% Cr martensitic stainless steels of interest for nuclear applications, viz. DIN 1.4914 (MANET specification, for fusion reactors) and AISI 410. The investigation has focussed principally on microstructural effects associated with the differences in chromium content between the two alloys. The size distribution functions determined from nuclear and magnetic SANS components for the two steels given identical heat treatments are in accord with an interpretation based on the presence of ˜ 1 nm size CCr aggregates in the microstructure. Much larger (˜ 10 nm) scattering inhomogeneities with different magnetic contrast are also present and tentatively identified as carbides.

  5. Toward a Taxonomy of the Denatured State: Small Angle Scattering Studies of Unfolded Proteins

    SciTech Connect

    Millett, I.S.; Doniach, S.; Plaxco, K.W.

    2005-02-15

    Despite the critical role the unfolded state plays in defining protein folding kinetics and thermodynamics (Berg et al., 2002; Dunker, 2002; Shortle, 2002; Wright and Dyson, 2002), our understanding of its detailed structure remains rather rudimentary; the heterogeneity of the unfolded ensemble renders difficult or impossible its study by traditional, atomic-level structural methods. Consequently, recent years have seen a significant expansion of small-angle X-ray and neutron scattering (SAXS and SANS, respectively) techniques that provide direct, albeit rotationally and time-averaged, measures of the geometric properties of the unfolded ensemble. These studies have reached a critical mass, allowing us for the first time to define general observations regarding the nature of the geometry - and possibly the chemistry and physics - of unfolded proteins.

  6. Small Angle X-ray Scattering in Structural Investigation of Selected Biological Systems

    SciTech Connect

    Kozak, Maciej

    2007-11-26

    Small angle X-ray scattering method (SAXS) is a technique complementary to the protein crystallography, allowing determination of the structural parameters such as the radius of gyration or the maximum size characterizing the macromolecules, and providing information on the conformational changes taking place in solution. The use of SAXS method enables a comparison of the protein crystal structure with the data collected in solution. Recent development of the measurement techniques (mainly those based on synchrotron radiation) and calculation methods has permitted introduction of advanced techniques also in the field of structural analysis of biomolecules (e.g. for determination of the shape of the protein molecule in solution). The paper presents a few selected methods of structural analysis of biological systems based on the SAXS data and illustrates their performance on the example of xylanase from Trichoderma longibrachiatum and a model phospholipid system.

  7. Small Angle X-ray Scattering in Structural Investigation of Selected Biological Systems

    NASA Astrophysics Data System (ADS)

    Kozak, Maciej

    2007-11-01

    Small angle X-ray scattering method (SAXS) is a technique complementary to the protein crystallography, allowing determination of the structural parameters such as the radius of gyration or the maximum size characterizing the macromolecules, and providing information on the conformational changes taking place in solution. The use of SAXS method enables a comparison of the protein crystal structure with the data collected in solution. Recent development of the measurement techniques (mainly those based on synchrotron radiation) and calculation methods has permitted introduction of advanced techniques also in the field of structural analysis of biomolecules (e.g. for determination of the shape of the protein molecule in solution). The paper presents a few selected methods of structural analysis of biological systems based on the SAXS data and illustrates their performance on the example of xylanase from Trichoderma longibrachiatum and a model phospholipid system.

  8. A new small-angle neutron scattering spectrometer at China Mianyang research reactor

    NASA Astrophysics Data System (ADS)

    Peng, Mei; Sun, Liangwei; Chen, Liang; Sun, Guangai; Chen, Bo; Xie, Chaomei; Xia, Qingzhong; Yan, Guanyun; Tian, Qiang; Huang, Chaoqiang; Pang, Beibei; Zhang, Ying; Wang, Yun; Liu, Yaoguang; Kang, Wu; Gong, Jian

    2016-02-01

    A new pinhole small-angle neutron scattering (SANS) spectrometer, installed at the cold neutron source of the 20 MW China Mianyang Research Reactor (CMRR) in the Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, has been put into use since 2014. The spectrometer is equipped with a multi-blade mechanical velocity selector, a multi-beam collimation system, and a two-dimensional He-3 position sensitive neutron detector. The q-range of the spectrometer covers from 0.01 nm-1 to 5.0 nm-1. In this paper, the design and characteristics of the SANS spectrometer are described. The q-resolution calculations, together with calibration measurements of silver behenate and a dispersion of nearly monodisperse poly-methyl-methacrylate nanoparticles indicate that our SANS spectrometer has a good performance and is now in routine service.

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

    NASA Astrophysics Data System (ADS)

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

    1995-03-01

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

  10. Structure of nanocrystalline palladium and copper studied by small angle neutron scattering

    SciTech Connect

    Sanders, P.G.; Weertman, J.R.; Barker, J.G.

    1996-12-01

    The structure of nanocrystalline palladium and copper, made by inert gas condensation and compaction, was studied using small angle neutron scattering (SANS), optical microscopy, and scanning electron microscopy. The effects of annealing and warm compaction were also examined with these techniques. The SANS results were interpreted using a maximum entropy routine, combined with knowledge of the Archimedes density and hydrogen concentration determined by prompt gamma activation analysis (PGAA). Similar hydrogen concentrations were detected by SANS and PGAA. This hydrogen content, which was approximately 5 at.{percent} in samples compacted at room temperature, was reduced by both annealing and warm compaction. Defects in several size classes were observed, including missing grain pores ({approx_equal}1{endash}50 nm diameter) and defects of micrometer size. Warm compaction produced a lower number density of pores in nanocrystalline palladium, which led to increased density. The observed structure was correlated with Vickers microhardness and fracture surface morphology. {copyright} {ital 1996 Materials Research Society.}

  11. Polyhydroxyalkanoate-based natural synthetic hybrid copolymer films: A small-angle neutron scattering study

    NASA Astrophysics Data System (ADS)

    Foster, L. John R.; Knott, Robert; Sanguanchaipaiwong, Vorapat; Holden, Peter J.

    2006-11-01

    Polyhydroxyalkanoates have attracted attention as biodegradable alternatives to conventional thermoplastics and as biomaterials. Through modification of their biosynthesis using Pseudomonas oleovorans, we have manipulated the material properties of these biopolyesters and produced a natural-synthetic hybrid copolymer of polyhydroxyoctanoate- block-diethylene glycol (PHO- b-DEG). A mixture of PHO and PHO-DEG were solvent cast from analytical grade chloroform and analysed using small-angle neutron scattering. A scattering pattern, easily distinguished above the background, was displayed by the films with a diffraction ring at q∼0.12 Å -1. This narrow ring of intensity is suggestive of a highly ordered system. Analysis of the diffraction pattern supported this concept and showed a d-spacing of approximately 50 Å. In addition, conformation of the hybrid polymer chains can be manipulated to support their self-assembly into ordered microporous films.

  12. Mixed micelles of alkyltrimethylammonium halides A small-angle neutron-scattering study

    NASA Astrophysics Data System (ADS)

    Aswal, V. K.; Goyal, P. S.

    1998-01-01

    Mixed micelles of alkyltrimethylammonium halides have been studied using small-angle neutron scattering (SANS). The experiments were carried out on mixed micellar solutions (CTAB + DTAB, CTAB + TTAB and TTAB + DTAB) of surfactants with the same head group but different chain lengths. The measurements were also made from the mixture of surfactants with the same chain length but different head groups of CTAB + CDAB and CTAB + CTAC. The surfactant components were mixed in the molar proportions of 1:1 and the total concentration was kept 0.2 M. It is found that size, aggregation number and the fractional charge on the micelle in the mixed systems have values in between those for the pure-component systems.

  13. Tackiness of pressure-sensitive adhesives: An ultra-small-angle X-ray scattering investigation

    NASA Astrophysics Data System (ADS)

    Müller-Buschbaum, P.; Ittner, T.; Petry, W.

    2004-05-01

    The debonding of a model pressure-sensitive adhesive (PSA) poly-n-buthylacrylate is investigated by a combination of the mechanical tack test, optical microscopy and in situ ultra-small-angle X-ray scattering. From the mechanical test, macroscopic values such as force-distance curves are determined. The force-distance curve exhibits the typical non-linear behavior. With microscopy the macroscopic cavitation structure is observed. Scattering addresses the structure of the PSA on a microscopic level for the first time. As a new feature, a sub-structure of the usual optically resolvable macroscopic fibrils between the PSA surface and the probe punch is detected. The sub-structure exists over a large distance between the PSA and the probe surface and remains constant in diameter. This behavior of the sub-structure as well as the dependence of the force plateau on the film thickness are compared with theoretical predictions.

  14. Small angle x-ray scattering studies of carbon anodes used in lithium rechargeable batteries.

    SciTech Connect

    Sandi, G.; Carrado, K. A.; Winans, R. E.; Seifert, S.; Johnson, C. S.

    1999-11-16

    In ANL laboratories, disordered carbons with predictable surface area and porosity properties have been prepared using inorganic templates containing well defined pore sizes. The carbons have been tested in electrochemical cells as anodes in lithium secondary batteries. They deliver high specific capacity and display excellent performance in terms of the number of cycles run. In situ small angle X-ray scattering (SAXS) during electrochemical cycling was carried out at the Advanced Photon Source, at ANL. In order to monitor the carbon electrode structural changes upon cycling, an electrochemical cell was specially designed to allow for the application of electrical current and the collection of SAXS data at the same time. Results show that upon cycling the structure of the carbon remains unchanged, which is desirable in reversible systems.

  15. Small angle neutron and X-ray scattering studies of carbons prepared using inorganic templates

    SciTech Connect

    Sandi, G.; Thiyagarajan, P.; Winans, R.E.; Carrado, K.A.

    1997-09-01

    Small angle neutron (SANS) and X-ray (SAXS) scattering analyses of carbons derived from organic-loaded inorganic template materials, used as anodes in lithium ion cells, have been performed. Two clays were used as templates to load the organic precursors, pillared montmorrillonite (PILC), a layered silicate clay whose sheets have been permanently propped open by sets of thermally stable molecular props, and sepiolite, a natural channeled clay. Five different organic precursors were used to load the PILC: pyrene, styrene, pyrene/trioxane copolymer, ethylene and propylene, whereas only propylene and ethylene were used to load sepiolite. Pyrolysis took place at 700{degrees}C under nitrogen. Values such as hole radius, fractal dimension, cutoff length and density of the final carbons will be compared as a function of the clay and carbon precursors.

  16. Small angle neutron scattering analysis of novel carbons for lithium secondary batteries.

    SciTech Connect

    Sandi, G.; Thiyagarajan, P.; Winans, R.; Carrado, K.

    1998-01-14

    Small angle neutron scattering analyses of carbonaceous materials used as anodes in lithium ion cells have been performed. The carbons have been synthesized using pillared clays (PILCs) as inorganic templates. Pillared clays are layered silicates whose sheets have been permanently propped open by sets of thermally stable molecular props. The calcined PILC was loaded with five different organic precursors and heated at 700 C under nitrogen. When the inorganic pillars were removed by acid treatment, carbon sheets are produced with holes. The fitting of the data in the high q region suggested that the carbon sheets have voids with radii ranging from 4 to 8 {angstrom}. Similar radii were obtained for the PILC and PILC/organic precursor, which suggests that the carbon was well distributed in the clay prior to pyrolysis.

  17. Micelle structural studies on oil solubilization by a small-angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Putra, Edy Giri Rachman; Seong, Baek Seok; Ikram, Abarrul

    2009-02-01

    A small-angle neutron scattering (SANS) technique was applied to reveal the micelle structural changes. The micelle structural changes of 0.3 M sodium dodecyl sulfate (SDS) concentration by addition of various oil, i.e. n-hexane, n-octane, and n-decane up to 60% (v/v) have been investigated. It was found that the size, aggregation number and the structures of the micelles changed exhibiting that the effective charge on the micelle decreases with an addition of oil. There was a small increase in minor axis of micelle while the correlation peak shifted to a lower momentum transfer Q and then to higher Q by a further oil addition.

  18. Multiple magnetic scattering in small-angle neutron scattering of Nd–Fe–B nanocrystalline magnet

    PubMed Central

    Ueno, Tetsuro; Saito, Kotaro; Yano, Masao; Ito, Masaaki; Shoji, Tetsuya; Sakuma, Noritsugu; Kato, Akira; Manabe, Akira; Hashimoto, Ai; Gilbert, Elliot P.; Keiderling, Uwe; Ono, Kanta

    2016-01-01

    We have investigated the influence of multiple scattering on the magnetic small-angle neutron scattering (SANS) from a Nd–Fe–B nanocrystalline magnet. We performed sample-thickness- and neutron-wavelength-dependent SANS measurements, and observed the scattering vector dependence of the multiple magnetic scattering. It is revealed that significant multiple scattering exists in the magnetic scattering rather than the nuclear scattering of Nd–Fe–B nanocrystalline magnet. It is considered that the mean free path of the neutrons for magnetic scattering is rather short in Nd–Fe–B magnets. We analysed the SANS data by the phenomenological magnetic correlation model considering the magnetic microstructures and obtained the microstructural parameters. PMID:27321149

  19. The complete VS ribozyme in solution studied by small-angle X-ray scattering

    SciTech Connect

    Lipfert, Jan; Ouellet, Jonathan; Norman, David G.; Doniach, Sebastian; Lilley, David M.J.

    2008-10-06

    We have used small-angle X-ray solution scattering to obtain ab initio shape reconstructions of the complete VS ribozyme. The ribozyme occupies an electron density envelope with an irregular shape, into which helical sections have been fitted. The ribozyme is built around a core comprising a near-coaxial stack of three helices, organized by two three-way helical junctions. An additional three-way junction formed by an auxiliary helix directs the substrate stem-loop, juxtaposing the cleavage site with an internal loop to create the active complex. This is consistent with the current view of the probable mechanism of trans-esterification in which adenine and guanine nucleobases contributed by the interacting loops combine in general acid-base catalysis.

  20. Characterization of Nanocomposite filler Morphology using Ultra Small-Angle X-ray Scattering

    SciTech Connect

    Justice, Ryan S.; Schaefer, Dale W.

    2010-10-22

    Loading polymer matrices with nanoscale fillers is widely believed to have the potential to push polymer properties to extreme values. Realization of anticipated properties, however, has proven elusive. Recent nanocomposite research suggests better characterization of the large-scale morphology will provide insight explaining these shortfalls. This work will present ultra-small angle X-ray scattering as a viable tool for elucidating the hierarchical filler morphology that exists within polymer nanocomposites. Scattering analysis tools developed by our group will be applied to scattering data from nanocomposites filled with carbon nanotubes, layered silicates, and colloidal silica. The relationship between imaging data and scattering data will be discussed in the context of filler dispersion. Finally, the impact of large-scale filler morphology on mechanical and electrical properties will be discussed.

  1. The complete VS ribozyme in solution studied by small-angle X-ray scattering

    PubMed Central

    Lipfert, Jan; Ouellet, Jonathan; Norman, David G.; Doniach, Sebastian; Lilley, David M.J.

    2010-01-01

    SUMMARY We have used small-angle X-ray solution scattering to obtain ab initio shape reconstructions of the complete VS ribozyme. The ribozyme occupies an electron density envelope with an irregular shape, into which helical sections have been fitted. The ribozyme is built around a core comprising a near-coaxial stack of three helices, organized by two three-way helical junctions. An additional three-way junction formed by an auxiliary helix directs the substrate stem-loop, juxtaposing the cleavage site with an internal loop to create the active complex. This is consistent with the current view of the probable mechanism of transesterification in which adenine and guanine nucleobases contributed by the interacting loops combine together in general acid-base catalysis. PMID:18786398

  2. Small-angle neutron scattering and molecular dynamics structural study of gelling DNA nanostars

    NASA Astrophysics Data System (ADS)

    Fernandez-Castanon, J.; Bomboi, F.; Rovigatti, L.; Zanatta, M.; Paciaroni, A.; Comez, L.; Porcar, L.; Jafta, C. J.; Fadda, G. C.; Bellini, T.; Sciortino, F.

    2016-08-01

    DNA oligomers with properly designed sequences self-assemble into well defined constructs. Here, we exploit this methodology to produce bulk quantities of tetravalent DNA nanostars (each one composed of 196 nucleotides) and to explore the structural signatures of their aggregation process. We report small-angle neutron scattering experiments focused on the evaluation of both the form factor and the temperature evolution of the scattered intensity at a nanostar concentration where the system forms a tetravalent equilibrium gel. We also perform molecular dynamics simulations of one isolated tetramer to evaluate the form factor numerically, without resorting to any approximate shape. The numerical form factor is found to be in very good agreement with the experimental one. Simulations predict an essentially temperature-independent form factor, offering the possibility to extract the effective structure factor and its evolution during the equilibrium gelation.

  3. Small-angle scattering instruments on a 1 MW long pulse spallation source

    SciTech Connect

    Olah, G.A.; Hjelm, R.P.; Seeger, P.A.

    1995-12-01

    Two small-angle neutron scattering instruments have been designed and optimized for installation at a 1 MW long pulse spallation source. The first of these instruments allows access to length scales in materials from 10 to 400 {angstrom}, and the second instrument from 40 to 1200 {angstrom}. Design characteristics were determined and optimization was done using the MCLIB Monte Carlo instrument simulation package. The code has been {open_quote}benchmarked{close_quote} by simulating the {open_quote}as-built{close_quote} D11 spectrometer at ILL and a performance comparison of the three instruments was made. Comparisons were made by evaluating the scattered intensity for {delta} scatterers at different Q values for various instrument configurations needed to span a Q-range of 0.0007 - 0.44 {angstrom}{sup {minus}1}.

  4. Multiple magnetic scattering in small-angle neutron scattering of Nd-Fe-B nanocrystalline magnet.

    PubMed

    Ueno, Tetsuro; Saito, Kotaro; Yano, Masao; Ito, Masaaki; Shoji, Tetsuya; Sakuma, Noritsugu; Kato, Akira; Manabe, Akira; Hashimoto, Ai; Gilbert, Elliot P; Keiderling, Uwe; Ono, Kanta

    2016-06-20

    We have investigated the influence of multiple scattering on the magnetic small-angle neutron scattering (SANS) from a Nd-Fe-B nanocrystalline magnet. We performed sample-thickness- and neutron-wavelength-dependent SANS measurements, and observed the scattering vector dependence of the multiple magnetic scattering. It is revealed that significant multiple scattering exists in the magnetic scattering rather than the nuclear scattering of Nd-Fe-B nanocrystalline magnet. It is considered that the mean free path of the neutrons for magnetic scattering is rather short in Nd-Fe-B magnets. We analysed the SANS data by the phenomenological magnetic correlation model considering the magnetic microstructures and obtained the microstructural parameters.

  5. Study of the enzyme ascorbate oxidase by small angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Maritano, S.; Carsughi, F.; Fontana, M. P.; Marchesini, A.

    1996-09-01

    We report a study of the large scale structure of the "blue" copper enzyme ascorbate oxidase by small angle neutron scattering. The enzyme has been extracted from zucchini and studied in solutions of two different preparations. Contrast variation method was used by performing the measurements in water, heavy water and mixtures of H 2OD 2O. Our data show that, at least at the concentrations used here, the gyration radius of the enzyme is about 34 Å; with such a value our analysis is most consistent with a value of 70 KDa for the molecular weight of ascorbate oxidase in the conditions of our experiment. This is in contrast to the generally accepted value of 140 KDa, obtained by other techniques at high concentrations (e.g. greater than 2 mg ml -1). The possible origins of such a discrepancy are discussed.

  6. Multiple magnetic scattering in small-angle neutron scattering of Nd-Fe-B nanocrystalline magnet.

    PubMed

    Ueno, Tetsuro; Saito, Kotaro; Yano, Masao; Ito, Masaaki; Shoji, Tetsuya; Sakuma, Noritsugu; Kato, Akira; Manabe, Akira; Hashimoto, Ai; Gilbert, Elliot P; Keiderling, Uwe; Ono, Kanta

    2016-01-01

    We have investigated the influence of multiple scattering on the magnetic small-angle neutron scattering (SANS) from a Nd-Fe-B nanocrystalline magnet. We performed sample-thickness- and neutron-wavelength-dependent SANS measurements, and observed the scattering vector dependence of the multiple magnetic scattering. It is revealed that significant multiple scattering exists in the magnetic scattering rather than the nuclear scattering of Nd-Fe-B nanocrystalline magnet. It is considered that the mean free path of the neutrons for magnetic scattering is rather short in Nd-Fe-B magnets. We analysed the SANS data by the phenomenological magnetic correlation model considering the magnetic microstructures and obtained the microstructural parameters. PMID:27321149

  7. Small-angle scattering as a tool to study the thermal denaturation of DNA

    NASA Astrophysics Data System (ADS)

    Wood, Kathleen; Knott, Robert; Tonchev, Ognyan; Angelov, Dimitar; Theodorakopoulos, Nikos; Peyrard, Michel

    2014-10-01

    DNA thermal denaturation is the breaking of the base pairs, leading to a splitting of the two strands of the double helix. While it is easy to measure the fraction of open base pairs (f) vs. temperature, determining the fraction (p) of fully open molecules is much harder. Previously, the simultaneous recording of f and p could only be achieved for special sequences. We show that small-angle scattering of X-rays or neutrons allows the measurement of p for any sequence. We illustrate the method with a SAXS investigation of two sequences designed to exhibit different melting profiles and compare the SAXS data with nano-calorimetric measurements of the melting curve.

  8. Probing coal reactivity by time-resolved small angle x-ray scattering.

    SciTech Connect

    Winans, R. E.

    1999-01-22

    The objective of this study is to observe changes in coal structure in situ with small angle X-ray scattering (SAXS) during solvent swelling and during pyrolysis. We have built a SAXS instrument at the Basic Energy Sciences Synchrotrons Research Center at the Advanced Photon Source that allows us to obtain scattering patterns in the millisecond time domain. The eight Argonne Premium Coal samples were used in this study. The information that can be derived from these experiments, such as changes in fractal dimensionality and in size and type of porosity, was found to be very rank-dependent. In the swelling experiments, it was noted that for certain coals, structural changes occurred in just a few minutes.

  9. Spin echo small angle neutron scattering using a continuously pumped {sup 3}He neutron polarisation analyser

    SciTech Connect

    Parnell, S. R.; Li, K.; Yan, H.; Stonaha, P.; Li, F.; Wang, T.; Baxter, D. V.; Snow, W. M.; Washington, A. L.; Walsh, A.; Chen, W. C.; Parnell, A. J.; Fairclough, J. P. A.; Pynn, R.

    2015-02-15

    We present a new instrument for spin echo small angle neutron scattering (SESANS) developed at the Low Energy Neutron Source at Indiana University. A description of the various instrument components is given along with the performance of these components. At the heart of the instrument are a series of resistive coils to encode the neutron trajectory into the neutron polarisation. These are shown to work well over a broad range of neutron wavelengths. Neutron polarisation analysis is accomplished using a continuously operating neutron spin filter polarised by Rb spin-exchange optical pumping of {sup 3}He. We describe the performance of the analyser along with a study of the {sup 3}He polarisation stability and its implications for SESANS measurements. Scattering from silica Stöber particles is investigated and agrees with samples run on similar instruments.

  10. Small-angle neutron scattering from polymer hydrogels with memory effect for medicine immobilization

    SciTech Connect

    Kulvelis, Yu. V. Lebedev, V. T.; Trunov, V. A.; Pavlyuchenko, V. N.; Ivanchev, S. S.; Primachenko, O. N.; Khaikin, S. Ya.

    2011-12-15

    Hydrogels synthesized based on cross-linked copolymers of 2-hydroxyethyl methacrylate and functional monomers (acrylic acid or dimethylaminoethyl methacrylate), having a memory effect with respect to target medicine (cefazolin), have been investigated by small-angle neutron scattering. The hydrogels are found to have a two-level structural organization: large (up to 100 nm) aggregates filled with network cells (4-7 nm in size). The structural differences in the anionic, cationic, and amphiphilic hydrogels and the relationship between their structure and the ability of hydrogels to absorb moisture are shown. A relationship between the memory effect during cefazolin immobilization and the internal structure of hydrogels, depending on their composition and type of functional groups, is established.

  11. Beyond the small-angle approximation for MBR anisotropy from seeds

    NASA Astrophysics Data System (ADS)

    Stebbins, Albert; Veeraraghavan, Shoba

    1995-02-01

    In this paper we give a general expression for the energy shift of massless particles traveling through the gravitational field of an arbitrary matter distribution as calculated in the weak field limit in an asymptotically flat space-time. It is not assumed that matter is nonrelativistic. We demonstrate the surprising result that if the matter is illuminated by a uniform brightness background that the brightness pattern observed at a given point in space-time (modulo a term dependent on the observer's velocity) depends only on the matter distribution on the observer's past light cone. These results apply directly to the cosmological MBR anisotropy pattern generated in the immediate vicinity of an object such as a cosmic string or global texture. We apply these results to cosmic strings, finding a correction to previously published results in the small-angle approximation. We also derive the full-sky anisotropy pattern of a collapsing texture knot.

  12. Adsorption of CO2 in porous MCM-41 and MCM-48 using small angle scattering

    NASA Astrophysics Data System (ADS)

    Wang, Bo; Das, Narayan; Warren, Garfield; Rupp, John; Mastalerz, Maria; Prisk, Timothy; Sokol, Paul

    2012-02-01

    Adsorption of CO2 onto the surface of nanopores in organic rich materials, such as shale and coals, is of great interest for understanding the processes associated with geological sequestration. These natural materials have complex pore structures which make the interpretation of experimental sorption measurements complicated. MCMs are synthetic materials with a well-defined regular porous structure that provides an ideal substrate to evaluate the models for the adsorption of gases (CO2) into nanopores. Samples of MCM-41 and MCM-48 were synthesized at Indiana University and were characterized by nitrogen adsorption isotherms and Small Angle X-ray Scattering (SAXS). SANS studies were carried out on MCMs with different pore sizes as a function of pore filling and the results are interpreted in terms of layer growth models.

  13. Online ion-exchange chromatography for small-angle X-ray scattering

    PubMed Central

    Hutin, Stephanie; Brennich, Martha; Maillot, Benoit; Round, Adam

    2016-01-01

    Biological small-angle X-ray scattering (BioSAXS) is a powerful technique to determine the solution structure, particle size, shape and surface-to-volume ratio of macromolecules. However, a drawback is that the sample needs to be monodisperse. To ensure this, size-exclusion chromatography (SEC) has been implemented on many BioSAXS beamlines. Here, the integration of ion-exchange chromatography (IEC) using both continuous linear and step gradients on a beamline is described. Background subtraction for continuous gradients by shifting a reference measurement and two different approaches for step gradients, which are based on interpolating between two background measurements, are discussed. The results presented here serve as a proof of principle for online IEC and subsequent data treatment. PMID:27710930

  14. Elucidating the Molecular Deformation Mechanism of Entangled Polymers in Fast Flow by Small Angle Neutron Scattering

    NASA Astrophysics Data System (ADS)

    Wang, Yangyang; Sanchez-Diaz, Luis; Cheng, Shiwang; Hong, Kunlun; Chen, Wei-Ren; Liu, Jianning; Lin, Panpan; Wang, Shi-Qing

    Understanding the viscoelastic properties of polymers is of fundamental and practical importance because of the vast and ever expanding demand of polymeric materials in daily life. Our current theoretical framework for describing the nonlinear flow behavior of entangled polymers is built upon the tube model pioneered by de Gennes, Doi, and Edwards. In this work, we critically examine the central hypothesis of the tube model for nonlinear rheology using small angle neutron scattering (SANS). While the tube model envisions a unique non-affine elastic deformation mechanism for entangled polymers, our SANS measurements show that the evolution of chain conformation of a well-entangled polystyrene melt closely follows the affine deformation mechanism in uniaxial extension, even when the Rouse Weissenberg number is much smaller than unity. This result provides a key clue for understanding the molecular deformation mechanism of entangled polymers in fast flow. Several implications from our analysis will be discussed in this talk.

  15. PREFACE Proceedings of the XIV International Conference on Small-Angle Scattering, SAS-2009

    NASA Astrophysics Data System (ADS)

    King, Stephen; Terrill, Nicholas

    2010-10-01

    The XIV International Conference on Small-Angle Scattering, SAS-2009, was held in Oxford UK, 13-18 September 2009, and was jointly organised under the auspices of the International Union of Crystallography Commission on SAS by a team from the Diamond Light Source and the ISIS Pulsed Neutron Source - their first such joint venture - with help from the UK Science and Technology Facilities Council. It was the first time that this long running and successful series of conferences on the application, science and technology of small-angle scattering techniques had been staged in the UK. The UK has a proud heritage in small-angle scattering: as home to one of the world's first SANS instruments (at AERE Harwell), as the site of the world's first 2nd generation X-ray Synchrotron (the SRS at Daresbury with its suite of SAXS beamlines), and latterly as the location of the world's most successful pulsed source SANS instrument. Indeed, 2009 also marked the 25th Anniversary of neutron operations at ISIS and the opening of a Second Target Station. Whilst the SRS ceased operations in 2008, its mantle has been inherited by the Diamond synchrotron. Many delegates took the opportunity to visit both Diamond and ISIS during a conference excursion. Despite the prevailing global economic downturn, we were delighted that 434 delegates from 32 different countries were able to attend SAS-2009; two-thirds were drawn from the UK, Germany, Japan, the USA and France, but there were also sizeable contingents from Australia, Korea, Taiwan and South America. In many ways this geographical spread reflects the present and emerging distribution, respectively, of 3rd generation X-ray synchrotrons and high-flux neutron sources, although the scope of the conference was not solely limited to these probes. Financial support from the IUCr enabled us to grant bursaries to attend SAS-2009 to 12 delegates from emerging countries (Algeria, Argentina, Brazil, India, Nepal, Romania, Russia and the Ukraine). The

  16. Focusing of Gaussian beam passed under small angle to optical axis of uniaxial crystal

    NASA Astrophysics Data System (ADS)

    Ivanov, M. O.; Shostka, N. V.

    2016-07-01

    We showed both experimentally and analytically, the effect of focusing of a Gaussian beam propagated under small angle ϕ with respect to the optical axis of a uniaxial crystal, on the generation of a bottle beam. At ϕ = 0° two foci that correspond to ordinary and extraordinary parts of a beam form a closed 3D structure of a bottle beam. At this point, the beam, in the foci points, has radially and azimuthally aligned polarizations. Increasing the value of ϕ leads to dramatic changes in the intensity and polarization structure of a bottle beam. Starting from the value of ϕ = ±2° the closed 3D symmetric structure of a bottle beam breaks down. At ϕ = ±5° both beams are focused at the same transverse plane, while its polarization evolves to x- and y-linear. With a further increase in angle ϕ two foci ‘switch’ their spatial positions and move further away.

  17. Drag measurements on long thin cylinders at small angles and high Reynolds numbers

    NASA Astrophysics Data System (ADS)

    Keith, William L.; Cipolla, Kimberly M.; Hart, David R.; Furey, Deborah A.

    2005-06-01

    Measurements of the drag caused by turbulent boundary layer mean wall shear stress on cylinders at small angles of attack and high length Reynolds numbers (8×106small angles of tow have a significant effect on the tangential drag coefficient values. A scaling for the orthogonal force on the cylinders was determined and provides a correction to published normal drag coefficient values for pure cross-flow. The presence of the axial turbulent boundary layer has a significant effect on these orthogonal forces.

  18. Enhanced small-angle scattering connected to the Widom line in simulations of supercooled water

    NASA Astrophysics Data System (ADS)

    Wikfeldt, K. T.; Huang, C.; Nilsson, A.; Pettersson, L. G. M.

    2011-06-01

    We present extensive simulations on the TIP4P/2005 water model showing significantly enhanced small-angle scattering (SAS) in the supercooled regime. The SAS is related to the presence of a Widom line (TW) characterized by maxima in thermodynamic response functions and Ornstein-Zernike correlation length. Recent experimental small-angle x-ray scattering data [Huang et al., J. Chem. Phys. 133, 134504 (2010)], 10.1063/1.3495974 are excellently reproduced, albeit with an increasing temperature offset at lower temperatures. Assuming the same origin of the SAS in experiment and model this suggests the existence of a Widom line also in real supercooled water. Simulations performed at 1000 bar show an increased abruptness of a crossover from dominating high-density (HDL) to dominating low-density (LDL) liquid and strongly enhanced SAS associated with crossing TW, consistent with a recent determination of the critical pressure of TIP4P/2005 at 1350 bar. Furthermore, good agreement with experimental isothermal compressibilities at 1000, 1500, and 2000 bar shows that the high pressure supercooled thermodynamic behavior of water is well described by TIP4P/2005. Analysis of the tetrahedrality parameter Q reveals that the HDL-LDL structural transition is very sharp at 1000 bar, and that structural fluctuations become strongly coupled to density fluctuations upon approaching TW. Furthermore, the tetrahedrality distribution becomes bimodal at ambient temperatures, an observation that possibly provides a link between HDL-LDL fluctuations and the structural bimodality in liquid water indicated by x-ray spectroscopic techniques. Computed x-ray absorption spectra are indeed found to show sensitivity to the tetrahedrality parameter.

  19. Probing the conformation of FhaC with small-angle neutron scattering and molecular modeling.

    PubMed

    Gabel, Frank; Lensink, Marc F; Clantin, Bernard; Jacob-Dubuisson, Françoise; Villeret, Vincent; Ebel, Christine

    2014-07-01

    Probing the solution structure of membrane proteins represents a formidable challenge, particularly when using small-angle scattering. Detergent molecules often present residual scattering contributions even at their match point in small-angle neutron scattering (SANS) measurements. Here, we studied the conformation of FhaC, the outer-membrane, β-barrel transporter of the Bordetella pertussis filamentous hemagglutinin adhesin. SANS measurements were performed on homogeneous solutions of FhaC solubilized in n-octyl-d17-βD-glucoside and on a variant devoid of the α helix H1, which critically obstructs the FhaC pore, in two solvent conditions corresponding to the match points of the protein and the detergent, respectively. Protein-bound detergent amounted to 142 ± 10 mol/mol as determined by analytical ultracentrifugation. By using molecular modeling and starting from three distinct conformations of FhaC and its variant embedded in lipid bilayers, we generated ensembles of protein-detergent arrangement models with 120-160 detergent molecules. The scattered curves were back-calculated for each model and compared with experimental data. Good fits were obtained for relatively compact, connected detergent belts, which occasionally displayed small detergent-free patches on the outer surface of the β barrel. The combination of SANS and modeling clearly enabled us to infer the solution structure of FhaC, with H1 inside the pore as in the crystal structure. We believe that our strategy of combining explicit atomic detergent modeling with SANS measurements has significant potential for structural studies of other detergent-solubilized membrane proteins. PMID:24988353

  20. Structural and Thermodynamic Properties of Septin 3 Investigated by Small-Angle X-Ray Scattering

    PubMed Central

    Ortore, Maria Grazia; Macedo, Joci N.A.; Araujo, Ana Paula U.; Ferrero, Claudio; Mariani, Paolo; Spinozzi, Francesco; Itri, Rosangela

    2015-01-01

    Septins comprise a family of proteins involved in a variety of cellular processes and related to several human pathologies. They are constituted by three structural domains: the N- and C-terminal domains, highly variable in length and composition, and the central domain, involved in the guanine nucleotide (GTP) binding. Thirteen different human septins are known to form heterogeneous complexes or homofilaments, which are stabilized by specific interactions between the different interfaces present in the domains. In this work, we have investigated by in-solution small-angle x-ray scattering the structural and thermodynamic properties of a human septin 3 construct, SEPT3-GC, which contains both of both interfaces (G and NC) responsible for septin-septin interactions. In order to shed light on the role of these interactions, small-angle x-ray scattering measurements were performed in a wide range of temperatures, from 2 up to 56°C, both with and without a nonhydrolysable form of GTP (GTPγS). The acquired data show a temperature-dependent coexistence of monomers, dimers, and higher-order aggregates that were analyzed using a global fitting approach, taking into account the crystallographic structure of the recently reported SEPT3 dimer, PDB:3SOP. As a result, the enthalpy, entropy, and heat capacity variations that control the dimer-monomer dissociation equilibrium in solution were derived and GTPγS was detected to increase the enthalpic stability of the dimeric species. Moreover, a temperature increase was observed to induce dissociation of SEPT3-GC dimers into monomers just preceding their reassembling into amyloid aggregates, as revealed by the Thioflavin-T fluorescence assays. PMID:26083929

  1. Probing the Conformation of FhaC with Small-Angle Neutron Scattering and Molecular Modeling

    PubMed Central

    Gabel, Frank; Lensink, Marc F.; Clantin, Bernard; Jacob-Dubuisson, Françoise; Villeret, Vincent; Ebel, Christine

    2014-01-01

    Probing the solution structure of membrane proteins represents a formidable challenge, particularly when using small-angle scattering. Detergent molecules often present residual scattering contributions even at their match point in small-angle neutron scattering (SANS) measurements. Here, we studied the conformation of FhaC, the outer-membrane, β-barrel transporter of the Bordetella pertussis filamentous hemagglutinin adhesin. SANS measurements were performed on homogeneous solutions of FhaC solubilized in n-octyl-d17-βD-glucoside and on a variant devoid of the α helix H1, which critically obstructs the FhaC pore, in two solvent conditions corresponding to the match points of the protein and the detergent, respectively. Protein-bound detergent amounted to 142 ± 10 mol/mol as determined by analytical ultracentrifugation. By using molecular modeling and starting from three distinct conformations of FhaC and its variant embedded in lipid bilayers, we generated ensembles of protein-detergent arrangement models with 120–160 detergent molecules. The scattered curves were back-calculated for each model and compared with experimental data. Good fits were obtained for relatively compact, connected detergent belts, which occasionally displayed small detergent-free patches on the outer surface of the β barrel. The combination of SANS and modeling clearly enabled us to infer the solution structure of FhaC, with H1 inside the pore as in the crystal structure. We believe that our strategy of combining explicit atomic detergent modeling with SANS measurements has significant potential for structural studies of other detergent-solubilized membrane proteins. PMID:24988353

  2. Speciation of deeply buried TiOx nanolayers with grazing-incidence x-ray fluorescence combined with a near-edge x-ray absorption fine-structure investigation

    NASA Astrophysics Data System (ADS)

    Pollakowski, Beatrix; Beckhoff, Burkhard; Reinhardt, Falk; Braun, Stefan; Gawlitza, Peter

    2008-06-01

    Nondestructive methods based on electron emission may encounter serious difficulties when probing the chemical state of deeply buried nanolayers due to restricted information depth. The purpose of the present work is to evaluate to which extent photon emission can overcome these restrictions. Grazing-incidence x-ray fluorescence combined with a near-edge x-ray absorption fine-structure investigation (GIXRF-NEXAFS) offers access to depth-resolving analysis of buried nanolayers with respect to both the chemical speciation and the layer composition. By varying the angle of incidence, the penetration depth can be tuned from a few to several hundreds of nanometers. The information depth of the emitted fluorescence radiation is in the same general range as the soft x-ray regime. Initial measurements were performed on nominally 30 nm thick titanium nanolayers oxidized to different extents and buried below 5 nm carbon layers. These layered structures were produced by means of ion beam sputtering deposition. The plane grating monochromator beamline for undulator radiation in the laboratory of the Physikalisch-Technische Bundesanstalt at the electron storage ring BESSY II provides tunable radiation of both well-known flux and high spectral purity for GIXRF-NEXAFS studies. The current results confirm that GIXRF-NEXAFS has the potential to substantially contribute to the speciation of deeply buried nanolayers. The analysis of measurements at a constant incident angle demonstrated that it is not possible to find an angle of incidence for the NEXAFS region to ensure a stable penetration depth. However, appropriate angular corrections can ensure a constant mean penetration depth, in particular, in the vicinity of absorption edges.

  3. High-throughput biological small-angle X-ray scattering with a robotically loaded capillary cell

    PubMed Central

    Nielsen, S. S.; Møller, M.; Gillilan, R. E.

    2012-01-01

    With the rise in popularity of biological small-angle X-ray scattering (BioSAXS) measurements, synchrotron beamlines are confronted with an ever-increasing number of samples from a wide range of solution conditions. To meet these demands, an increasing number of beamlines worldwide have begun to provide automated liquid-handling systems for sample loading. This article presents an automated sample-loading system for BioSAXS beamlines, which combines single-channel disposable-tip pipetting with a vacuum-enclosed temperature-controlled capillary flow cell. The design incorporates an easily changeable capillary to reduce the incidence of X-ray window fouling and cross contamination. Both the robot-control and the data-processing systems are written in Python. The data-processing code, RAW, has been enhanced with several new features to form a user-friendly BioSAXS pipeline for the robot. The flow cell also supports efficient manual loading and sample recovery. An effective rinse protocol for the sample cell is developed and tested. Fluid dynamics within the sample capillary reveals a vortex ring pattern of circulation that redistributes radiation-damaged material. Radiation damage is most severe in the boundary layer near the capillary surface. At typical flow speeds, capillaries below 2 mm in diameter are beginning to enter the Stokes (creeping flow) regime in which mixing due to oscillation is limited. Analysis within this regime shows that single-pass exposure and multiple-pass exposure of a sample plug are functionally the same with regard to exposed volume when plug motion reversal is slow. The robot was tested on three different beamlines at the Cornell High-Energy Synchrotron Source, with a variety of detectors and beam characteristics, and it has been used successfully in several published studies as well as in two introductory short courses on basic BioSAXS methods. PMID:22509071

  4. Phase separation and ordering process in Al-Li alloys studied by small-angle neutron scattering and neutron diffraction

    SciTech Connect

    Furusaka, M.; Fujikawa, S.I.; Tranquada, J.M.

    1993-07-01

    To study phase separation kinetics of Al-9.5at.%Li polycrystalline alloys in which precipitates have ordered Al{sub 3}Li ({delta}{prime}) structure, profile analysis of small-angle neutron scattering and superlattice reflections (100) and (110) were done. A small-angle scattering instrument and a triple-axis spectrometer in elastic mode were used in the measurements. Strong texture was observed in the reflections. Therefore, measurements were done using the crystal orientation where the intensity of the reflection was at the maximum. Profiles of small-angle scattering and superlattice reflections were almost identical at higher momentum transfer side. At lower momentum transfer side, small-angle scattering showed interference effects, but superlattice reflection did not show any sign of interference. Integrated intensities of superlattice reflections were obtained and compared with small-angle scattering intensity. The order parameter was not saturated in the {delta}{prime} precipitates at the early stage of the phase separation process.

  5. Optical and Geometric Properties of Free Silica Nanoparticles Studied by Small-Angle X-Ray Scattering

    NASA Astrophysics Data System (ADS)

    Langer, Burkhard; Raschpichler, Christopher; Gruner, Mathias; Antonsson, Egill; Goroncy, Christian; Graf, Christina; Rühl, Eckart

    2016-09-01

    Elastic small-angle X-ray scattering (SAXS) of free silica (SiO2) nanoparticles is reported (d = 100-180 nm). The particles were prepared by a modified Stöber synthesis in narrow size distributions with controlled surface roughness and functionalization. Angle-resolved small-angle X-ray scattering patterns are shown to be sensitive to these changes in particle properties. It is reported that there is an exponential decrease in scattered X-ray intensity towards larger scattering angles as well as distinct oscillations, which is fully explained by Mie theory. Small-angle X-ray scattering of mesoporous nanoparticles with rough surfaces is compared to that of microporous nanoparticles with smooth surfaces, revealing distinct differences that are rationalized by diffuse scattering from nanoparticle pores in addition to the dominating contribution of Mie scattering. Furthermore, results from small-angle X-ray scattering experiments on functionalized silica nanoparticles are presented, where the incorporation of the dye fluorescein isothiocyanate is found to cause changes in the optical properties of the nanoparticles, as compared to non-functionalized samples. Small, but distinct deviations in particle size derived from electron microscopy and from small-angle X-ray scattering are observed. These are rationalized by particle shrinking occurring in electron microscopy as well as slight changes in optical properties of the nanoparticle samples.

  6. PREFACE Proceedings of the XIV International Conference on Small-Angle Scattering, SAS-2009

    NASA Astrophysics Data System (ADS)

    King, Stephen; Terrill, Nicholas

    2010-10-01

    The XIV International Conference on Small-Angle Scattering, SAS-2009, was held in Oxford UK, 13-18 September 2009, and was jointly organised under the auspices of the International Union of Crystallography Commission on SAS by a team from the Diamond Light Source and the ISIS Pulsed Neutron Source - their first such joint venture - with help from the UK Science and Technology Facilities Council. It was the first time that this long running and successful series of conferences on the application, science and technology of small-angle scattering techniques had been staged in the UK. The UK has a proud heritage in small-angle scattering: as home to one of the world's first SANS instruments (at AERE Harwell), as the site of the world's first 2nd generation X-ray Synchrotron (the SRS at Daresbury with its suite of SAXS beamlines), and latterly as the location of the world's most successful pulsed source SANS instrument. Indeed, 2009 also marked the 25th Anniversary of neutron operations at ISIS and the opening of a Second Target Station. Whilst the SRS ceased operations in 2008, its mantle has been inherited by the Diamond synchrotron. Many delegates took the opportunity to visit both Diamond and ISIS during a conference excursion. Despite the prevailing global economic downturn, we were delighted that 434 delegates from 32 different countries were able to attend SAS-2009; two-thirds were drawn from the UK, Germany, Japan, the USA and France, but there were also sizeable contingents from Australia, Korea, Taiwan and South America. In many ways this geographical spread reflects the present and emerging distribution, respectively, of 3rd generation X-ray synchrotrons and high-flux neutron sources, although the scope of the conference was not solely limited to these probes. Financial support from the IUCr enabled us to grant bursaries to attend SAS-2009 to 12 delegates from emerging countries (Algeria, Argentina, Brazil, India, Nepal, Romania, Russia and the Ukraine). The

  7. A new approach to quantification of metamorphism using ultra-small and small angle neutron scattering.

    SciTech Connect

    Anovitz, Lawrence {Larry} M; Lynn, Gary W; Cole, David R

    2009-12-01

    In this paper we report the results of a study using small angle and ultra-small angle neutron scattering techniques (SANS and USANS) to examine the evolution of carbonates during contact metamorphism. Data were obtained from samples collected along two transects in the metamorphosed Hueco limestone at the Marble Canyon, Texas, contact aureole. These samples were collected from the igneous contact out to {approx}1700 m. Scattering curves obtained from these samples show mass fractal behavior at low scattering vectors, and surface fractal behavior at high scattering vectors. Significant changes are observed in the surface and mass fractal dimensions as well as the correlation lengths (pore and grain sizes), surface area to volume ratio and surface Gibbs Free energy as a function of distance, including regions of the aureole outside the range of classic metamorphic petrology. A change from mass-fractal to non-fractal behavior is observed at larger scales near the outer boundary of the aureole that implies significant reorganization of pore distributions early in the metamorphic history. Surface fractal results suggest significant smoothing of grain boundaries, coupled with changes in pore sizes. A section of the scattering curve with a slope less than -4 appears at low-Q in metamorphosed samples, which is not present in unmetamorphosed samples. A strong spike in the surface area to volume ratio is observed in rocks near the mapped metamorphic limit, which is associated with reaction of small amounts of organic material to graphite. It may also represent an increase in pore volume or permeability, suggesting that a high permeability zone forms at the boundary of the aureole and moves outwards as metamorphism progresses. Neutron scattering data also correlate well with transmission electron microscopic (TEM) observations, which show formation of micro- and nanopores and microfractures during metamorphism. The scattering data are, however, quantifiable for a bulk rock

  8. A new approach to quantification of metamorphism using ultra-small and small angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Anovitz, Lawrence M.; Lynn, Gary W.; Cole, David R.; Rother, Gernot; Allard, Lawrence F.; Hamilton, William A.; Porcar, Lionel; Kim, Man-Ho

    2009-12-01

    In this paper we report the results of a study using small angle and ultra-small angle neutron scattering techniques (SANS and USANS) to examine the evolution of carbonates during contact metamorphism. Data were obtained from samples collected along two transects in the metamorphosed Hueco limestone at the Marble Canyon, Texas, contact aureole. These samples were collected from the igneous contact out to ˜1700 m. Scattering curves obtained from these samples show mass fractal behavior at low scattering vectors, and surface fractal behavior at high scattering vectors. Significant changes are observed in the surface and mass fractal dimensions as well as the correlation lengths (pore and grain sizes), surface area to volume ratio and surface Gibbs Free energy as a function of distance, including regions of the aureole outside the range of classic metamorphic petrology. A change from mass-fractal to non-fractal behavior is observed at larger scales near the outer boundary of the aureole that implies significant reorganization of pore distributions early in the metamorphic history. Surface fractal results suggest significant smoothing of grain boundaries, coupled with changes in pore sizes. A section of the scattering curve with a slope less than -4 appears at low- Q in metamorphosed samples, which is not present in unmetamorphosed samples. A strong spike in the surface area to volume ratio is observed in rocks near the mapped metamorphic limit, which is associated with reaction of small amounts of organic material to graphite. It may also represent an increase in pore volume or permeability, suggesting that a high permeability zone forms at the boundary of the aureole and moves outwards as metamorphism progresses. Neutron scattering data also correlate well with transmission electron microscopic (TEM) observations, which show formation of micro- and nanopores and microfractures during metamorphism. The scattering data are, however, quantifiable for a bulk rock in a

  9. Small-angle x-ray scattering study of crazing in bulk thermoplastic polymers

    NASA Astrophysics Data System (ADS)

    Salomons, Gregory John

    Crazing is a form of tension-induced deformation consisting of microscopic cracks spanned by load-bearing fibrils. This is generally considered to be the primary source of plastic strain response of rubber-modified thermoplastics subjected to applied tensile stress. An understanding of the mechanisms involved in crazing is, therefore, valuable as a means of identifying structure-property relationships. Extensive studies on single crazes in thin films have been done,sp{1-6} however, experiments on crazing in bulk materials have been fraught with problems, such as difficulties with the production of uniform crazes and accurate temperature control.sp7 A new apparatus has been designed to overcome many of these problems; a symmetric tensile stretching mechanism and a radiant heating technique combined with real-time small-angle x-ray scattering (RTSAXS) is used to examine craze fibril structure. The analysis of small-angle x-ray scattering (SAXS) data is highly model-dependent requiring precise structural models to ensure accurate interpretation. Recently, improved measurement techniques have called into question some aspects of the long accepted models applied to SAXS interpretation of craze structures.sp{8,9} A detailed examination of the models applicable to craze fibril structure is presented here, including a newly proposed model involving power-law density distributions within the fibrils. It is shown that the best description of craze fibrils comes from a Gaussian density distribution. This is in contrast to the traditional models which describe the fibrils as having uniform density with sharp boundaries.sp{1,2} RTSAXS studies of High Impact Polystyrene (HIPS) and Polystyrene (PS) blended with 2 wt.% Polybutadiene (PB) were performed using a constant strain rate of 5 × 10sp{-4} ssp{-1} and temperatures from 30 to 70sp°C. Crazing deformation modes were identified and the macroscopic deformation characteristics for the two materials were compared revealing a

  10. Nanostructural features in silica-polyvinyl acetate nanocomposites characterized by small-angle scattering.

    SciTech Connect

    Narayanan, R. A.; Thiyagarajan, P.; Zhu, A. J.; Ash, J.; Shofner, M. L.; Schadler, L. S.; Kumar, S. K.; Sternstein, S. S.; ORNL; Rensselaer Polytechnic Inst.

    2007-09-10

    Small-angle scattering (SAS) experiments were carried out on nanocomposites of poly(vinyl acetate) (PVAc) and fumed silica nanoparticles with different surface areas and chemical treatment, in the wave-vector (Q) range: 0.0002-1 Angstrom{sup -1}. SAS data on composites with matrices of two different molecular weights indicate that the particle aggregation is independent of the molecular weight of the matrix for a fixed filler concentration and surface treatment. Particle size distributions derived from the SAS data suggest that particle aggregation is reduced when the native surface hydroxyl groups are blocked by various surface treatments, which also reduce the bonding strength to the polymer matrix. The unified exponential/power-law analysis of the SAS data shows three levels of hierarchy in the organization of silica particles. The first level consists of small aggregates of silica particles. At the second level we observe polydispersed aggregates resembling mass-fractal objects that is corroborated by TEM. The polydispersed aggregates further associate to form agglomerates at the third level. The relevance of these findings to the mechanism of nanofiller reinforcement of linear amorphous polymers above T{sub g} is discussed.

  11. Small-angle Neutron Scattering and Contrast Variation: A Powerful Combination for Studying Biological Structures

    SciTech Connect

    Heller, William T

    2010-01-01

    The use of small-angle scattering (SAS) in the biological sciences continues to increase, driven as much by the need to study increasingly complex systems that are often resistant to crystallization or are too large for NMR as by the availability of user facilities and advancements in the modelling of biological structures from SAS data. SAS, whether with neutrons (SANS) or X-rays (SAXS), is a structural probe of length scales ranging from 10 to 10,000 {angstrom}. When applied to biological complexes in dilute solution, it provides size and shape information that can be used to produce structural models that can provide insight into function. SANS enables the use of contrast-variation methods through the unique interaction of neutrons with hydrogen and its isotope deuterium. SANS with contrast variation enables the visualization of components within multisubunit complexes, making it a powerful tool for probing protein-protein and protein-nucleic acid complexes, as well as the interaction of proteins with lipids and detergents.

  12. Nanostructural Features in Silica-polyvinyl Acetate Nanocomposites Characterized by Small-Angle Scattering

    SciTech Connect

    Raghavan, Aravinda N; Thiyagarajan, P.; Zhu, Dr. Ai-Jun; Ash, Dr. Benjamin J.; Shofner, M. L.; Schadler, Linda; Kumar, Sanat K; Sternstein, S. S.

    2007-01-01

    Small-angle scattering (SAS) experiments were carried out on nanocomposites of poly(vinyl acetate) (PVAc) and fumed silica nanoparticles with different surface areas and chemical treatment, in the wave-vector (Q) range: 0.0002-1 A-1 . SAS data on composites with matrices of two different molecular weights indicate that the particle aggregation is independent of the molecular weight of the matrix for a fixed filler concentration and surface treatment. Particle size distributions derived from the SAS data suggest that particle aggregation is reduced when the native surface hydroxyl groups are blocked by various surface treatments, which also reduce the bonding strength to the polymer matrix. The unified exponential/power-law analysis of the SAS data shows three levels of hierarchy in the organization of silica particles. The first level consists of small aggregates of silica particles. At the second level we observe polydispersed aggregates resembling mass-fractal objects that is corroborated by TEM. The polydispersed aggregates further associate to form agglomerates at the third level. The relevance of these findings to the mechanism of nanofiller reinforcement of linear amorphous polymers above Tg is discussed.

  13. Comparative analysis of the nucleosome structure of cell nuclei by small-angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Isaev-Ivanov, V. V.; Lebedev, D. V.; Lauter, H.; Pantina, R. A.; Kuklin, A. I.; Islamov, A. Kh.; Filatov, M. V.

    2010-05-01

    The nucleosome structure in native nuclei of normal (chicken erythrocyte and rat leukocyte nuclei) and anomalously proliferating (the human cervical adenocarcinoma cell line HeLa and the Chinese hamster fibroblast cell line A238) cells has been investigated using small-angle neutron scattering. The experimental results obtained allow one to make the inference that the parameters of the nucleosome structure for the chicken erythrocyte and rat leukocyte nuclei (on average over the nucleus) are close to the universally accepted values and that the distance distribution function is bimodal. The bimodality of the distance distribution function reflects a narrow distribution of distances between nucleosomes (on average over the nucleus) at the fibril level of the chromatin organization. The histone core of the nucleosome structure in the nuclei of the HeLa and A238 cells (on average over the nucleus) is considerably less compact than that in the chicken erythrocyte and rat leukocyte nuclei, and the distance distribution function does not exhibit indications of the bimodality.

  14. Collagen Orientation and Crystallite Size in Human Dentin: A Small Angle X-ray Scattering Study

    SciTech Connect

    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.

  15. Structural modeling of proteins by integrating small-angle x-ray scattering data

    NASA Astrophysics Data System (ADS)

    Zhang, Yong-Hui; Peng, Jun-Hui; Zhang, Zhi-Yong

    2015-12-01

    Elucidating the structure of large biomolecules such as multi-domain proteins or protein complexes is challenging due to their high flexibility in solution. Recently, an “integrative structural biology” approach has been proposed, which aims to determine the protein structure and characterize protein flexibility by combining complementary high- and low-resolution experimental data using computer simulations. Small-angle x-ray scattering (SAXS) is an efficient technique that can yield low-resolution structural information, including protein size and shape. Here, we review computational methods that integrate SAXS with other experimental datasets for structural modeling. Finally, we provide a case study of determination of the structure of a protein complex formed between the tandem SH3 domains in c-Cb1-associated protein and the proline-rich loop in human vinculin. Project supported by the National Key Basic Research Program of China (Grant Nos. 2013CB910203 and 2011CB911104), the National Natural Science Foundation of China (Grant No. 31270760), the Strategic Priority Research Program of the Chinese Academy of Sciences (Grant No. XDB08030102), and the Specialized Research Fund for the Doctoral Program of Higher Education of China (Grant No. 20113402120013).

  16. Using Small Angle Neutron Scattering on Glucose Oxidase immobilized on Single Layer Graphene

    NASA Astrophysics Data System (ADS)

    Rai, Durgesh; Gurusaran, M.; Qian, S.; Weiss, K.; Urban, V.; Li, P.; Ma, L.; Ajayan, P.; Narayanan, T.; Sekar, K.; Viswanathan, S.; Renugopalakrishanan, V.

    2015-03-01

    Reliable blood glucose monitoring using biosensors is valuable for health evaluations and medication in wake of chronic diabetic issues accompanying deviations from evolutionary human lifestyle. Glucose oxidase (GOx) is an ideal enzyme because of its specificity and the ability to electrochemically transduce from the enzymatic reaction. We use graphene-based electrode with GOx sensor matrix so that the emitted electrons from sensor matrix can flow across graphene nearly without scattering; crucial for constructing ultrasensitive-sensors. Thereafter, establishing a structure-property based relationships to tune the sensor topology with electrochemically output forms the main focus of the device development process. We have developed a methodology to obtain low-resolution hierarchical models of the aggregate matrix using Small Angle Neutron Scattering (SANS) technique. A Unified Fit model is used in tandem with GNOM, DAMMIN and DAMAVER to construct low-resolution models for GOx matrices. A detailed explanation of a general methodology for obtaining quantitative details aggregate structures along with qualitative models will be presented.

  17. Interactive graphical system for small-angle scattering analysis of polydisperse systems

    NASA Astrophysics Data System (ADS)

    Konarev, P. V.; Volkov, V. V.; Svergun, D. I.

    2016-09-01

    A program suite for one-dimensional small-angle scattering analysis of polydisperse systems and multiple data sets is presented. The main program, POLYSAS, has a menu-driven graphical user interface calling computational modules from ATSAS package to perform data treatment and analysis. The graphical menu interface allows one to process multiple (time, concentration or temperature-dependent) data sets and interactively change the parameters for the data modelling using sliders. The graphical representation of the data is done via the Winteracter-based program SASPLOT. The package is designed for the analysis of polydisperse systems and mixtures, and permits one to obtain size distributions and evaluate the volume fractions of the components using linear and non-linear fitting algorithms as well as model-independent singular value decomposition. The use of the POLYSAS package is illustrated by the recent examples of its application to study concentration-dependent oligomeric states of proteins and time kinetics of polymer micelles for anticancer drug delivery.

  18. Ensemble Activation of G-Protein -Coupled Receptors Revealed by Small-Angle Neutron Scattering

    NASA Astrophysics Data System (ADS)

    Chu, Xiang-Qiang; Perera, Suchithranga; Shrestha, Utsab; Chawla, Udeep; Struts, Andrey; Qian, Shuo; Brown, Michael

    2014-03-01

    Rhodopsin is a G-protein -coupled receptor (GPCR) involved in visual light perception and occurs naturally in a membrane lipid environment. Rhodopsin photoactivation yields cis-trans isomerization of retinal giving equilibrium between inactive Meta-I and active Meta-II states. Does photoactivation lead to a single Meta-II conformation, or do substates exist as described by an ensemble-activation mechanism (EAM)? We use small-angle neutron scattering (SANS) to investigate conformational changes in rhodopsin-detergent and rhodopsin-lipid complexes upon photoactivation. Meta-I state is stabilized in CHAPS-solubilized rhodopsin, while Meta-II is trapped in DDM-solubilized rhodopsin. SANS data are acquired from 80% D2O solutions and at contrast-matching points for both DDM and CHAPS samples. Our experiments demonstrate that for detergent-solubilized rhodopsin, SANS with contrast variation can detect structural differences between the rhodopsin dark-state, Meta-I, Meta-II, and ligand-free opsin states. Dark-state rhodopsin has more conformational flexibility in DDM micelles compared to CHAPS, which is consistent with an ensemble of activated Meta-II states. Furthermore, time-resolved SANS enables study of the time-dependent structural transitions between Meta-I and Meta-II, which is crucial to understanding the ensemble-based activation.

  19. Density of hydrophobically confined deeply cooled water investigated by small angle X-ray scattering

    SciTech Connect

    Liu, Kao-Hsiang; Zhang, Yang; Jeng, U-Ser; Mou, Chung-Yuan

    2015-09-07

    Water’s behavior near hydrophobic surfaces has attracted great attention due to chemical and geological applications. Here, we report small angle X-ray scattering (SAXS) studies of water confined in the hydrophobic nanoporous carbon material, CMK-1-14, from ambient to deeply cooled temperatures. By monitoring the scattering intensity of the first Bragg peak, which is directly related to the scattering length density contrast between the carbon matrix and the confined water, the average density of the hydrophobically confined water was determined from 300 K to 150 K at ambient pressure. Furthermore, differential scanning calorimetry and X-ray diffraction measurements showed that the majority of such hydrophobically confined water did not crystallize in the investigated temperature range. By exploiting the fast speed of SAXS measurements and the continuous temperature ramping, the average density profile and the deduced thermal expansion coefficient (α{sub p}) were obtained. We found that the well-known density maximum of water at 277 K downshifted to 260 K, and the density minimum which has been observed in hydrophilic confinement disappeared. In addition, the previously measured large density decreasing of 18% at low temperature was recalibrated to a more reasonable 10% instead. Consequently, the recalculated α{sub p} peak was found to be quite similar to that of the water confined in hydrophilic MCM-41-S-15 suggesting an intrinsic property of water, which does not sensitively depend on the confinement surface.

  20. Investigation of the tripoli porous structure by small-angle neutron scattering

    SciTech Connect

    Avdeev, M. V.; Blagoveshchenskii, N. M.; Garamus, V. M.; Novikov, A. G. Puchkov, A. V.

    2011-12-15

    The characteristics of the tripoli porous structure have been investigated by small-angle neutron scattering (SANS). Tripoli is a finely porous sedimentary rock formed by small spherical opal particles. Its main component is aqueous silica SiO{sub 2} {center_dot} nH{sub 2}O (80-90%). Tripoli is widely used in practice as a working medium for sorption filters and in some other commercial and construction technologies. The shape of the experimental SANS curves indicates the presence of small and large pores in tripoli. The small-pore size was estimated to be {approx}100 Angstrom-Sign . The size of large pores turned out to be beyond the range of neutron wave vector transfers Q that are available for the instrument used; however, their size was indirectly estimated to be {approx}(2000-2500) Angstrom-Sign . The pores of both groups behave as surfacetype fractal scatterers with the fractal dimension D {approx} 2.2-2.6. The densities of pores of these two groups differ by approximately three orders of magnitude ({approx}10{sup 16} and {approx}10{sup 13} cm{sup -3} for small and large pores, respectively); the fraction of large pores amounts to 70-80% of the total pore volume. The found pore characteristics (their densities, sizes, and relative volumes) are in satisfactory agreement (when a comparison is possible) with the absorption data.

  1. Structural Studies of Bleached Melanin by Synchrotron Small-angle X-ray Scattering¶

    SciTech Connect

    Littrell, Kenneth C.; Gallas, James M.; Zajac, Gerry W.; Thiyagarajan, Pappannan

    2003-01-01

    Small-angle X-ray scattering was used to measure the effects of chemical bleaching on the size and morphology of tyrosine-derived synthetic melanin dispersed in aqueous media. The average size as measured by the radius of gyration of the melanin particles in solution, at neutral to mildly basic pH, decreases from 16.5 to 12.5 angstroms with increased bleaching. The melanin particles exhibit scattering characteristic of sheet-like structures with a thickness of approximately 11 angstroms at all but the highest levels of bleaching. The scattering data are well described by the form factor for scattering from a pancake-like circular cylinder. These data are consistent with the hypothesis that unbleached melanin, at neutral to mildly basic pH, is a planar aggregate of 6- to 10-nm-sized melanin protomolecules, hydrogen bonded through their quinone and phenolic perimeters. The observed decrease in melanin particle size with increased bleaching is interpreted as evidence for deaggregation, most probably the result of oxidative disruption of hydrogen bonds and an increase in the number of charged, carboxylic acid groups, whereby the melanin aggregates disassociate into units composed of decreasing numbers of protomolecules.

  2. Preliminary analysis of the distribution of water in human hair by small-angle neutron scattering.

    PubMed

    Kamath, Yash; Murthy, N Sanjeeva; Ramaprasad, Ram

    2014-01-01

    Diffusion and distribution of water in hair can reveal the internal structure of hair that determines the penetration of various products used to treat hair. The distribution of water into different morphological components in unmodified hair, cuticle-free hair, and hair saturated with oil at various levels of humidity was examined using small-angle neutron scattering (SANS) by substituting water with deuterium oxide (D(2)O). Infrared spectroscopy was used to follow hydrogen-deuterium exchange. Water present in hair gives basically two types of responses in SANS: (i) interference patterns, and (ii) central diffuse scattering (CDS) around the beam stop. The amount of water in the matrix between the intermediate filaments that gives rise to interference patterns remained essentially constant over the 50-98% humidity range without swelling this region of the fiber extensively. This observation suggests that a significant fraction of water in the hair, which contributes to the CDS, is likely located in a different morphological region of hair that is more like pores in a fibrous structure, which leads to significant additional swelling of the fiber. Comparison of the scattering of hair treated with oil shows that soybean oil, which diffuses less into hair, allows more water into hair than coconut oil. These preliminary results illustrate the utility of SANS for evaluating and understanding the diffusion of deuterated liquids into different morphological structures in hair.

  3. Measuring Material Microstructure Under Flow Using 1-2 Plane Flow-Small Angle Neutron Scattering

    PubMed Central

    Gurnon, A. Kate; Godfrin, P. Douglas; Wagner, Norman J.; Eberle, Aaron P. R.; Butler, Paul; Porcar, Lionel

    2014-01-01

    A new small-angle neutron scattering (SANS) sample environment optimized for studying the microstructure of complex fluids under simple shear flow is presented. The SANS shear cell consists of a concentric cylinder Couette geometry that is sealed and rotating about a horizontal axis so that the vorticity direction of the flow field is aligned with the neutron beam enabling scattering from the 1-2 plane of shear (velocity-velocity gradient, respectively). This approach is an advance over previous shear cell sample environments as there is a strong coupling between the bulk rheology and microstructural features in the 1-2 plane of shear. Flow-instabilities, such as shear banding, can also be studied by spatially resolved measurements. This is accomplished in this sample environment by using a narrow aperture for the neutron beam and scanning along the velocity gradient direction. Time resolved experiments, such as flow start-ups and large amplitude oscillatory shear flow are also possible by synchronization of the shear motion and time-resolved detection of scattered neutrons. Representative results using the methods outlined here demonstrate the useful nature of spatial resolution for measuring the microstructure of a wormlike micelle solution that exhibits shear banding, a phenomenon that can only be investigated by resolving the structure along the velocity gradient direction. Finally, potential improvements to the current design are discussed along with suggestions for supplementary experiments as motivation for future experiments on a broad range of complex fluids in a variety of shear motions. PMID:24561395

  4. Magnetization processes in nanostructured metals and small-angle neutron scattering

    SciTech Connect

    Loeffler, J.F.; Braun, H.B.; Wagner, W.; Kostorz, G.; Wiedenmann, A.

    2005-04-01

    The magnetization process in nanostructured (n-) Fe and Co was investigated via small-angle neutron scattering (SANS). In a zero field, the magnetization exhibits correlations extending over several grains. In intermediate applied magnetic fields around 1 kOe, n-Fe and n-Co samples with small grain sizes exhibit an anisotropic scattering profile with an unusual intensity enhancement for scattering vectors parallel to the field direction. Comparing the experimental data with a modeled granular microstructure containing magnetic domains of arbitrary size and orientation, we conclude that magnetic domains extending over several grains are tilted considerably out of the external field direction in intermediate fields. Since the domain size does not change significantly with the magnitude of the external field, we conclude that the magnetization process does not proceed via domain-wall motion. Together with theoretical arguments showing the existence of marginally stable domains within the random-anisotropy model, our SANS data suggests that the magnetization process proceeds by simultaneous reversal of a few adjacent domains, presumably in the form of small avalanches. This resembles the magnetization process predicted for random-field Ising magnets. Our theoretical analysis of SANS data is general and applies to other systems consisting of magnetic nanoclusters embedded in a nonmagnetic matrix.

  5. Two-dimensional granular flow in a vibrated small-angle funnel

    PubMed

    Lindemann; Dimon

    2000-10-01

    We have studied the flow of a single layer of uniform balls in a small-angle funnel when it is vibrated parallel to the flow. Generally, we measured the flow rate as a function of a dimensionless acceleration Gamma. However, for sufficiently small outlet widths, the flow can jam so we also measured the elapsed times between balls and their correlations to study jam dynamics. In particular, we found that when the funnel angle beta was larger than approximately 4 degrees, a stable jam always formed for Gamma<1 and the flow stopped. For Gamma approximately 1-4, jams still occurred, but now they broke and reformed, although they could last approximately 100 s, resulting in long-time correlations in the flow. The elapsed time distributions in this case show distinct, possibly algebraic, tails. Beyond Gamma approximately 4, the flow no longer jammed and the flow rate became constant. The general behavior has been mapped out in a rough phase diagram.

  6. Location of two antioxidants in oriented model membranes. Small-angle x-ray diffraction study.

    PubMed Central

    Katsaras, J; Stinson, R H; Davis, J H; Kendall, E J

    1991-01-01

    Small-angle x-ray diffraction has been applied in locating either butylated hydroxytoluene (BHT) or delta-tocopherol and their brominated analogues at a concentration of 40 mol% in oriented bilayers of dipalmitoylphosphatidylcholine (DPPC) or DPPC + 15 mol% cholesterol at 20 degrees C. Phases were determined using swelling experiments with structure factors plotted in reciprocal space, creating a relatively smooth curve as the amount of water between the bilayers was changed. Continuous Fourier transforms were also calculated using sampling theory (Shannon, C. E. 1949. Proc. Inst. Radio Engrs. NY. 37:10-21) to further test the consistency of the phase assignments. Fourier synthesis of structure factors resulted in absolute electron density profiles for different bilayers to a resolution of 5-6 A. In addition, difference Patterson maps were constructed to confirm the positions of the bromine atoms in the unit cell. Analysis of the data indicates the following: (a) The BHT molecules are dispersed throughout the alkyl-chain region in DPPC samples with and without cholesterol. (b) The chromanol ring of delta-tocopherol is in the vicinity of the glycerol backbone-headgroup region in samples of DPPC or DPPC + 15 mol% cholesterol. (c) Difference Patterson maps confirm the localization of bromine atoms in the various delta-tocopherol samples and lack of bromine localization in the various BHT samples. PMID:2049525

  7. Small-Angle Neutron Scattering by the Magnetic Microstructure of Nanocrystalline Ferromagnets Near Saturation

    PubMed Central

    Weissmüller, J.; McMichael, R. D.; Michels, A.; Shull, R. D.

    1999-01-01

    The paper presents a theoretical analysis of elastic magnetic small-angle neutron scattering (SANS) due to the nonuniform magnetic microstructure in nanocrystalline ferromagnets. The reaction of the magnetization to the magnetocrystalline and magnetoelastic anisotropy fields is derived using the theory of micromagnetics. In the limit where the scattering volume is a single magnetic domain, and the magnetization is nearly aligned with the direction of the magnetic field, closed form solutions are given for the differential scattering cross-section as a function of the scattering vector and of the magnetic field. These expressions involve an anisotropy field scattering function, that depends only on the Fourier components of the anisotropy field microstructure, not on the applied field, and a micromagnetic response function for SANS, that can be computed from tabulated values of the materials parameters saturation magnetization and exchange stiffness constant or spin wave stiffness constant. Based on these results, it is suggested that the anisotropy field scattering function SH can be extracted from experimental SANS data. A sum rule for SH suggests measurement of the volumetric mean square anisotropy field. When magnetocrystalline anisotropy is dominant, then a mean grain size or the grain size distribution may be determined by analysis of SH.

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

    PubMed

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

    2016-06-01

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

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

    PubMed Central

    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

  10. Using Small-Angle Neutron Scattering to Detect Nanoscopic Lipid Domains

    SciTech Connect

    Pan, Jianjun; Heberle, Frederick A; Petruzielo, Robin S; Katsaras, John

    2013-01-01

    The cell plasma membrane is a complex system, which is thought to be capable of exhibiting non-random lateral organization. Studies of live cells and model membranes have yielded mechanisms responsible for the formation, growth, and maintenance of nanoscopic heterogeneities, although the existence and mechanisms that give rise to these heterogeneities remain controversial. Small-angle neutron scattering (SANS) is a tool ideally suited to interrogate lateral heterogeneity in model membranes, primarily due to its unique spatial resolution (i.e., "5 100 nm) and its ability to resolve structure with minimal perturbation to the membrane. In this review we examine several methods used to analyze the SANS signal arising from freely suspended unilamellar vesicles containing lateral heterogeneity. Specifically, we discuss an analytical model for a single, round domain on a spherical vesicle. We then discuss a numerical method that uses Monte Carlo simulation to describe systems with multiple domains and/or more complicated morphologies. Also discussed are several model-independent approaches that are sensitive to membrane heterogeneity. The review concludes with several recent applications of SANS to the study of membrane raft mixtures.

  11. Small angle neutron scattering contrast variation reveals heterogeneities of interactions in protein gels.

    PubMed

    Banc, A; Charbonneau, C; Dahesh, M; Appavou, M-S; Fu, Z; Morel, M-H; Ramos, L

    2016-06-28

    We propose a quantitative approach to probe the spatial heterogeneities of interactions in macromolecular gels, based on a combination of small angle X-ray (SAXS) and neutrons (SANS) scattering. We investigate the structure of model gluten protein gels and show that the gels display radically different SAXS and SANS profiles when the solvent is (at least partially) deuterated. The detailed analysis of the SANS signal as a function of the solvent deuteration demonstrates heterogeneities of sample deuteration at different length scales. The progressive exchange between the protons (H) of the proteins and the deuteriums (D) of the solvent is inhomogeneous and 60 nm large zones that are enriched in H are evidenced. In addition, at low protein concentration, in the sol state, solvent deuteration induces a liquid/liquid phase separation. Complementary biochemical and structure analyses show that the denser protein phase is more protonated and specifically enriched in glutenin, the polymeric fraction of gluten proteins. These findings suggest that the presence of H-rich zones in gluten gels would arise from the preferential interaction of glutenin polymers through a tight network of non-exchangeable intermolecular hydrogen bonds. PMID:27198847

  12. Survey of background scattering from materials found in small-angle neutron scattering

    PubMed Central

    Barker, J. G.; Mildner, D. F. R.

    2015-01-01

    Measurements and calculations of beam attenuation and background scattering for common materials placed in a neutron beam are presented over the temperature range of 300–700 K. Time-of-flight (TOF) measurements have also been made, to determine the fraction of the background that is either inelastic or quasi-elastic scattering as measured with a 3He detector. Other background sources considered include double Bragg diffraction from windows or samples, scattering from gases, and phonon scattering from solids. Background from the residual air in detector vacuum vessels and scattering from the 3He detector dome are presented. The thickness dependence of the multiple scattering correction for forward scattering from water is calculated. Inelastic phonon background scattering at small angles for crystalline solids is both modeled and compared with measurements. Methods of maximizing the signal-to-noise ratio by material selection, choice of sample thickness and wavelength, removal of inelastic background by TOF or Be filters, and removal of spin-flip scattering with polarized beam analysis are discussed. PMID:26306088

  13. Deterministic fractals: extracting additional information from small-angle scattering data.

    PubMed

    Cherny, A Yu; Anitas, E M; Osipov, V A; Kuklin, A I

    2011-09-01

    The small-angle scattering curves of deterministic mass fractals are studied and analyzed in momentum space. In the fractal region, the curve I(q)q(D) is found to be log-periodic with good accuracy, and the period is equal to the scaling factor of the fractal. Here, D and I(q) are the fractal dimension and the scattering intensity, respectively. The number of periods of this curve coincides with the number of fractal iterations. We show that the log-periodicity of I(q)q(D) in the momentum space is related to the log-periodicity of the quantity g(r)r(3-D) in the real space, where g(r) is the pair distribution function. The minima and maxima positions of the scattering intensity are estimated explicitly by relating them to the pair distance distribution in real space. It is shown that the minima and maxima are damped with increasing polydispersity of the fractal sets; however, they remain quite pronounced even at sufficiently large values of polydispersity. A generalized self-similar Vicsek fractal with controllable fractal dimension is introduced, and its scattering properties are studied to illustrate the above findings. In contrast with the usual methods, the present analysis allows us to obtain not only the fractal dimension and the edges of the fractal region, but also the fractal iteration number, the scaling factor, and the number of structural units from which the fractal is composed.

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

    PubMed Central

    Skou, Soren; Gillilan, Richard E

    2015-01-01

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

  15. Density of hydrophobically confined deeply cooled water investigated by small angle X-ray scattering

    SciTech Connect

    Liu, Kao-Hsiang; Zhang, Yang; Jeng, U-Ser; Mou, Chung-Yuan

    2015-09-07

    The behavior of water near hydrophobic surfaces has attracted great attention due to chemical and geological applications. Here, we report small angle X-ray scattering (SAXS) studies of water confined in the hydrophobic nanoporous carbon material, CMK-1-14, from ambient to deeply cooled temperatures. Moreover, by monitoring the scattering intensity of the first Bragg peak, which is directly related to the scattering length density contrast between the carbon matrix and the confined water, the average density of the hydrophobically confined water was determined from 300 K to 150 K at ambient pressure. Furthermore, differential scanning calorimetry and X-ray diffraction measurements showed that the majority of such hydrophobically confined water did not crystallize in the investigated temperature range. By exploiting the fast speed of SAXS measurements and the continuous temperature ramping, the average density profile and the deduced thermal expansion coefficient (alpha(p)) were obtained. We found that the well-known density maximum of water at 277 K downshifted to 260 K, and the density minimum which has been observed in hydrophilic confinement disappeared. Additionally, the previously measured large density decreasing of 18% at low temperature was recalibrated to a more reasonable 10% instead. Consequently, the recalculated ap peak was found to be quite similar to that of the water confined in hydrophilic MCM-41-S-15 suggesting an intrinsic property of water, which does not sensitively depend on the confinement surface.

  16. Density of hydrophobically confined deeply cooled water investigated by small angle X-ray scattering

    DOE PAGES

    Liu, Kao-Hsiang; Zhang, Yang; Jeng, U-Ser; Mou, Chung-Yuan

    2015-09-07

    The behavior of water near hydrophobic surfaces has attracted great attention due to chemical and geological applications. Here, we report small angle X-ray scattering (SAXS) studies of water confined in the hydrophobic nanoporous carbon material, CMK-1-14, from ambient to deeply cooled temperatures. Moreover, by monitoring the scattering intensity of the first Bragg peak, which is directly related to the scattering length density contrast between the carbon matrix and the confined water, the average density of the hydrophobically confined water was determined from 300 K to 150 K at ambient pressure. Furthermore, differential scanning calorimetry and X-ray diffraction measurements showed thatmore » the majority of such hydrophobically confined water did not crystallize in the investigated temperature range. By exploiting the fast speed of SAXS measurements and the continuous temperature ramping, the average density profile and the deduced thermal expansion coefficient (alpha(p)) were obtained. We found that the well-known density maximum of water at 277 K downshifted to 260 K, and the density minimum which has been observed in hydrophilic confinement disappeared. Additionally, the previously measured large density decreasing of 18% at low temperature was recalibrated to a more reasonable 10% instead. Consequently, the recalculated ap peak was found to be quite similar to that of the water confined in hydrophilic MCM-41-S-15 suggesting an intrinsic property of water, which does not sensitively depend on the confinement surface.« less

  17. The dynamic duo: Combining NMR and small angle scattering in structural biology

    PubMed Central

    Hennig, Janosch; Sattler, Michael

    2014-01-01

    Structural biology provides essential information for elucidating molecular mechanisms that underlie biological function. Advances in hardware, sample preparation, experimental methods, and computational approaches now enable structural analysis of protein complexes with increasing complexity that more closely represent biologically entities in the cellular environment. Integrated multidisciplinary approaches are required to overcome limitations of individual methods and take advantage of complementary aspects provided by different structural biology techniques. Although X-ray crystallography remains the method of choice for structural analysis of large complexes, crystallization of flexible systems is often difficult and does typically not provide insights into conformational dynamics present in solution. Nuclear magnetic resonance spectroscopy (NMR) is well-suited to study dynamics at picosecond to second time scales, and to map binding interfaces even of large systems at residue resolution but suffers from poor sensitivity with increasing molecular weight. Small angle scattering (SAS) methods provide low resolution information in solution and can characterize dynamics and conformational equilibria complementary to crystallography and NMR. The combination of NMR, crystallography, and SAS is, thus, very useful for analysis of the structure and conformational dynamics of (large) protein complexes in solution. In high molecular weight systems, where NMR data are often sparse, SAS provides additional structural information and can differentiate between NMR-derived models. Scattering data can also validate the solution conformation of a crystal structure and indicate the presence of conformational equilibria. Here, we review current state-of-the-art approaches for combining NMR, crystallography, and SAS data to characterize protein complexes in solution. PMID:24687405

  18. Solution Properties of 1,3-Cyclohexadiene Polymers by Small Angle Neutron and Light Scattering

    SciTech Connect

    Yun, Seok I; Melnichenko, Yuri B; Wignall, George D; Hong, Kunlun; Mays, Jimmy; Britt, Phillip F; Terao, Ken; Nakamura, Yo

    2006-01-01

    1,3-Cyclohexdiene polymers (PCHD) and their derivatives are of interest due to the six-member rings in the main chain, which are expected to impart higher mechanical strength and better thermal and chemical stability, as compared to common vinyl polymers. For example, hydrogenated PCHD has the highest glass transition temperature (T{sub g} {approx} 231 C) of all hydrocarbon polymers, and it also shows good heat, weather, impact, abrasion, and chemical resistance as well as low water absorption. In addition, PCHD has unique photochemical properties, such as excellent transparency, due to the isolated double bonds in the main chain. Also, block copolymers containing PCHD show unusual phase separation behavior. For example, a styrene/1,3-CHD block copolymer (PS-b-PCHD) with 50 vol % CHD (1,4/1,2 {approx} 95/5) exhibits a core-shell or hollow cylinder morphology, while a typical styrene/acyclic diene (isoprene or butadiene) block copolymer with similar composition exhibits a lamellar structure. Such phase behavior and many other properties strongly depend on the conformation of the polymer in solution or bulk. However, almost no data have been reported on the conformation of PCHD, probably because of the lack of well-defined and well-characterized samples. Here we report solution properties of PCHD in tetrahydrofuran (THF) and chloroform by multiangle laser light scattering, viscometry, and small-angle neutron scattering (SANS).

  19. Six-dimensional real and reciprocal space small-angle X-ray scattering tomography.

    PubMed

    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.

  20. MISLIFT- AERODYNAMIC LIFT ON WING-BODY COMBINATIONS AT SMALL ANGLES OF ATTACK IN SUPERSONIC FLOW

    NASA Technical Reports Server (NTRS)

    Sawyer, W. C.

    1994-01-01

    Two separate and distinct theories are incorporated in this computer program to estimate the lift-induced pressures existent on a wing-body combination. These are (1) the second-order shock-expansion theory, which is used to obtain the lifting pressures on the body alone at small angles of attack, and (2) the linear-theory integral equations, which is used to evaluate the lifting pressures induced by the wing. These equations relate the local surface slope at a point on the lifting surface to the pressure differential at the point and the influence of the pressures upstream of the point. The numerical solution of these equations is effected by treating the wing-planform as a composite of elemental rectangles and applying summation techniques to satisfy the necessary integral relations. Most of the input required by this program is involved with the description of the missile planform geometry. The output consists of the computed value of the lifting pressure slope (the differential pressure coefficient per degree angle of attack) for each of the elements in the planform array. A force and moment summary is presented for the configuration under consideration.

  1. A Small-Angle Scattering Study of the Bulk Structure of a Symmetric Diblock Copolymer System

    NASA Astrophysics Data System (ADS)

    Papadakis, Christine M.; Almdal, Kristoffer; Mortensen, Kell; Posselt, Dorthe

    1997-12-01

    The bulk structure of a homologous series of symmetric polystyrene-polybutadiene (SB) diblock copolymers is investigated using small-angle X-ray and neutron scattering (SANS). The study focuses on the lamellar thickness, the lamellar correlation length and the concentration profile as a function of the chain length and the preparation method applied. The characteristic length, D, scales with the chain length, N, in the whole range studied, but with a clear change in scaling exponent near χ N = 29, in accordance with theoretical predictions of a crossover from an Intermediate-Segregation Regime (ISR) to the Strong-Segregation Limit (SSL). In the ISR (χ N simeq 5-29), D is found to scale like D propto N^{0.83} and in the SSL (χ N > 29) like D propto N^{0.61} . The temperature dependence of the SANS spectra is studied for a low molar mass sample in an interval around the order-disorder transition temperature (TODT). The peak position is found to vary more strongly with temperature than expected for Gaussian chains. Only a weak discontinuity of the peak position at TODT is observed. In summary, the phase behavior of symmetric SB diblock copolymers in the bulk spans three regimes: the Gaussian regime in the region χ N < 5, the ISR for 5 < χ N < 29 and the SSL for χ N > 29.

  2. Glycerol monooleate reverse micelles in nonpolar solvents: computer simulations and small-angle neutron scattering.

    PubMed

    Bradley-Shaw, Joshua L; Camp, Philip J; Dowding, Peter J; Lewtas, Ken

    2015-03-19

    The formation of glycerol monooleate reverse micelles in n-heptane and toluene at room temperature is studied using molecular-dynamics simulations and small-angle neutron scattering. The glycerol monooleate concentrations under consideration are in the range of 5-20 wt %. Under these conditions, spontaneous reverse-micelle formation is observed on the simulation timescale (up to 30 ns). From simulations, the typical dimensions (semiaxes) of the equivalent ellipsoids with the same masses and moments of inertia are in the range of 15-23 Å, with instantaneous shapes that are slightly nonspherical. By analyzing the scattering form factors from simulation and experiment, the radii of gyration of the reverse micelles are determined to be approximately 15 Å. The number of glycerol monooleate molecules in a reverse micelle is smaller in toluene (∼20) than in n-heptane (∼30), but the overall dimensions are similar due to greater penetration of the toluene in to the reverse micelle. The effects of low concentrations (1 wt %) of water, acetic acid, and ethanol on the reverse-micelle dimensions are determined. The overall structural effects are small, but the distributions of the molecules within the reverse micelles are shown to be sensitive to the molecular polarity.

  3. Structural formation of huntingtin-like aggregates probed by small-angle neutron scattering

    SciTech Connect

    Stanley, Christopher B; Perevozchikova, Tatiana; Berthelier-Jung, Valerie M

    2011-01-01

    In several neurodegenerative disorders, including Huntington s disease (HD), aspects concerning the earliest of protein structures that form along the aggregation pathway have increasingly gained attention since these particular species are likely to be neurotoxic. We used time-resolved small-angle neutron scattering (SANS) to probe in solution these transient structures formed by peptides having the N-terminal sequence context of mutant huntingtin (Htt) exon 1. We obtained snapshots of the formed aggregates as the kinetic reaction ensued to yield quantitative information on their size and mass. At the early stage, small precursor species with an initial radius of gyration (Rg) of 16.1 5.9 and average mass of a dimer to trimer were monitored. Structural growth was treated as two modes with a transition from three-dimensional early aggregate formation to two-dimensional fibril growth and association. Our SANS results on the internal structure of the mature fibrils demonstrate loose packing with about 1 peptide per 4.75 -sheet repeat distance, which is shown to be quantitatively consistent with a -helix model. This research provides new insights into the structures forming along the pathway of Htt exon 1 aggregation and should assist in determining the role that precursors play in neuronal toxicity.

  4. Kinetic small angle neutron scattering of the skyrmion lattice in MnSi

    NASA Astrophysics Data System (ADS)

    Mühlbauer, S.; Kindervater, J.; Adams, T.; Bauer, A.; Keiderling, U.; Pfleiderer, C.

    2016-07-01

    We report a kinetic small angle neutron scattering (SANS) study of the skyrmion lattice (SL) in MnSi. Induced by an oscillatory tilting of the magnetic field direction, the elasticity and relaxation of the SL along the magnetic field direction have been measured with microsecond resolution. For the excitation frequency of 325 {{Hz}} the SL begins to track the tilting motion of the applied magnetic field under tilting angles exceeding {α }{{c}}≳ 0.4^\\circ . Empirically the associated angular velocity of the tilting connects quantitatively with the critical charge carrier velocity of ∼ 0.1 {{mm}} {{{s}}}-1 under current driven spin transfer torques, for which the SL unpins. In addition, a pronounced temperature dependence of the skyrmion motion is attributed to the variation of the skyrmion stiffness. Taken together our study highlights the power of kinetic SANS as a new experimental tool to explore, in a rather general manner, the elasticity and impurity pinning of magnetic textures across a wide parameter space without parasitic signal interferences due to ohmic heating or Oersted magnetic fields.

  5. Investigation of Monodisperse Dendrimeric Polysaccharide Nanoparticle Dispersions Using Small Angle Neutron Scattering

    NASA Astrophysics Data System (ADS)

    Atkinson, John; Nickels, Jonathan; Papp-Szabo, Erzsi; Katsaras, John; Dutcher, John

    2015-03-01

    Phytoglycogen is a highly branched polysaccharide that is very similar to the energy storage molecule glycogen. We have isolated monodisperse phytoglycogen nanoparticles from corn and these particles are attractive for applications in the cosmetic, food and beverage, and biomedical industries. Many of these promising applications are due to the special interaction between the nanoparticles and water, which results in: (1) high solubility; (2) low viscosity and high stability in aqueous dispersions; and (3) a remarkable capacity to sequester and retain water. Our rheology measurements indicate that the nanoparticles behave like hard spheres in water, with the viscosity diverging for concentrations >25% (w/w). Because of this, aqueous suspensions of phytoglycogen provide an ideal platform for detailed testing of theories of colloidal glasses and jamming. To further explore the interaction of the phytoglycogen particles and water, we have performed small angle neutron scattering (SANS) measurements on the Extended Q-Range SANS (EQ-SANS) diffractometer at the Spallation Neutron Source at Oak Ridge National Laboratory. Measurements performed on phytoglycogen dispersions in mixtures of hydrogenated and deuterated water have allowed us to determine the particle size and average particle spacing as a function of the phytoglycogen concentration in the limits of dilute and concentrated dispersions.

  6. Characterization of Physically and Chemically Separated Athabasca Asphaltenes Using Small-Angle X-ray Scattering

    SciTech Connect

    Amundaraín Hurtado, Jesús Leonardo; Chodakowski, Martin; Long, Bingwen; Shaw, John M.

    2012-02-07

    Athabasca asphaltenes were characterized using small-angle X-ray scattering (SAXS). Two methods were used to separate asphaltenes from the Athabasca bitumen: namely, chemical separation by precipitation with n-pentane and physical separation by nanofiltration using a zirconia membrane with a 20 nm average pore size. The permeate and chemically separated samples were diluted in 1-methylnaphtalene and n-dodecane prior to SAXS measurements. The temperature and asphaltene concentration ranges were 50-310 C and 1-10.4 wt %, respectively. Model-independent analysis of SAXS data provided the radius of gyration and the scattering coefficients. Model-dependent fits provided size distributions for asphaltenes assuming that they are dense and spherical. Model-independent analysis for physically and chemically separated asphaltenes showed significant differences in nominal size and structure, and the temperature dependence of structural properties. The results challenge the merits of using chemically separated asphaltene properties as a basis for asphaltene property prediction in hydrocarbon resources. While the residuals for model-dependent fits are small, the results are inconsistent with the structural parameters obtained from model-independent analysis.

  7. Small Angle Neutron Scattering (SANS) Studies on the Structural Evolution of Pyromellitamide Self-assembled Gels

    SciTech Connect

    Scott, Jamieson; Tong, Katie; William, Hamilton; He, Lilin; James, Michael; Thordarson, Pall; Boukhalfa, Sofiane

    2014-10-31

    The kinetics of aggregation of two pyromellitamide gelators; tetrabutyl- (C4) and tetrahexylpyromellitamide (C6), in deuterated cyclohexane has been investigated by small angle neutron scattering (SANS) for up to six days. The purpose of this study was to improve our understanding of how self-assembled gels are formed. Short-term (< 3 hour) time scales revealed multiple phases with the data for the tetrabutylpyromellitamide C4 indicating one dimensional stacking and aggregation corresponding to a multi-fiber braided cluster arrangement that is about 35 Å in diameter. The corresponding tetrahexylpyromellitamide C6 data suggests that the C6 also forms one-dimensional stacks but that these aggregate to a thicker multi-fiber braided cluster that have a diameter of 61.8 Å. Over a longer period of time, the radius, persistence length and contour length all continue to increase in 6 days after cooling. This data suggests that structural changes in self-assembled gels occur over a period exceeding several days and that fairly subtle changes in the structure (e.g. tail-length) can influence the packing of molecules in self-assembled gels on the single-to-few fiber bundle stage.

  8. Quantification of microstructural features in HMX using small angle neutron scattering techniques

    SciTech Connect

    Mang, J.T.; Skidmore, C.B.; Hjelm, R.P.; Howe, P.M.

    1998-12-01

    Microstructural features in raw powders of High Explosives have been qualitatively observed by many researchers, using polarized light and scanning electron microscopy. Here, the authors present a method for non-destructive quantification of volume fraction and structure of intragranular cracks and crystallization voids in a bulk sample (100--300 mg). By employing Small Angle Neutron Scattering (SANS) in conjunction with the method of contrast variation, they can effectively highlight different structural features of a complex system. The technique of contrast variation relies on immersing the sample in a uniform fluid of known neutron scattering length density. By selectively varying the scattering length density of the immersion fluid, scattering contributions from internal and external structures can be separated. This approach is analogous to varying the index of refraction for immersion oil relative to a sample in polarized light microscopy. SANS experiments on HMX were conducted using loose powders (261 and 10 micron mean particle diameters) and pellets made by uniaxial consolidation (without binder) to 7 and 10 volume percent porosity respectively. Detailed modeling of the SANS data indicate significant alteration of the intragranular void/crack/pore structure, with pressing, of the HMX powders.

  9. Pore distributions in nanocrystalline metals from small-angle neutron scattering

    SciTech Connect

    Sanders, P.G.; Weertman, J.R.; Eastman, J.A.

    1998-07-24

    Recent upgrades in inert-gas condensation processing equipment have produced nanocrystalline metal samples with high densities and low-impurity levels. Typical Cu and Pd samples have densities {ge}98% of theoretical and oxygen and hydrogen impurity concentrations {le}0.5 at. %. Lower porosity and impurity levels may make it difficult to produce and maintain samples with the smallest nanocrystalline grain sizes. These improved samples were studied by small-angle neutron scattering (SANS) to determine the volume fraction and size distribution of pores. Excellent correlation was obtained between the total volume fraction of pores and the Archimedes density for Pd, signifying that most of the pores were relatively small and in the detectability range of SANS ({approx}1--100 nm). Nanocrystalline Cu is shown to exhibit a wider pore size distribution. For Pd, the average pore sizes were slightly smaller than the average grain size, while for Cu the pore size and grain size were about the same. Both materials exhibited a trend of increasing pore size with increasing grain size. In terms of processing prerequisites, the principal condition for the production of high-density nanocrystalline Cu is an exceptionally clean synthesis environment, while nanocrystalline Pd requires compaction at elevated temperatures. These differences are the result of Cu having both a lower melting point and a greater susceptibility to contamination by gaseous impurities such as oxygen.

  10. Glassy carbon as an absolute intensity calibration standard for small-angle scattering.

    SciTech Connect

    Zhang, F.; Ilavsky, J.; Long, G.; Allen, A.; Quintana, J.; Jemian, P.; NIST

    2010-05-01

    Absolute calibration of small-angle scattering (SAS) intensity data (measured in terms of the differential scattering cross section per unit sample volume per unit solid angle) is essential for many important aspects of quantitative SAS analysis, such as obtaining the number density, volume fraction, and specific surface area of the scatterers. It also enables scattering data from different instruments (light, X-ray, or neutron scattering) to be combined, and it can even be useful to detect the existence of artifacts in the experimental data. Different primary or secondary calibration methods are available. In the latter case, absolute intensity calibration requires a stable artifact with the necessary scattering profile. Glassy carbon has sometimes been selected as this intensity calibration standard. Here we review the spatial homogeneity and temporal stability of one type of commercially available glassy carbon that is being used as an intensity calibration standard at a number of SAS facilities. We demonstrate that glassy carbon is sufficiently homogeneous and stable during routine use to be relied upon as a suitable standard for absolute intensity calibration of SAS data.

  11. Six-dimensional real and reciprocal space small-angle X-ray scattering tomography

    NASA Astrophysics Data System (ADS)

    Schaff, Florian; Bech, Martin; Zaslansky, Paul; Jud, Christoph; Liebi, Marianne; Guizar-Sicairos, Manuel; Pfeiffer, Franz

    2015-11-01

    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.

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

    DOE PAGES

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

    2015-01-23

    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 targetsmore » for which high-resolution structures have been determined via X-ray crystallography or nuclear magnetic resonance (NMR) spectroscopy. 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.« less

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

    SciTech Connect

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

    2015-01-23

    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. 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.

  14. Counterion Distribution Around Protein-SNAs probed by Small-angle X-ray scattering

    NASA Astrophysics Data System (ADS)

    Krishnamoorthy, Kurinji; Bedzyk, Michael; Kewalramani, Sumit; Moreau, Liane; Mirkin, Chad

    Protein-DNA conjugates couple the advanced cell transfection capabilities of spherical DNA architecture and the biocompatible enzymatic activity of a protein core to potentially create therapeutic agents with dual functionality. An understanding of their stabilizing ionic environment is crucial to better understand and predict their properties. Here, we use Small-angle X-ray scattering techniques to decipher the structure of the counterion cloud surrounding these DNA coated nanoparticles. Through the use of anomalous scattering techniques we have mapped the local concentrations of Rb+ ions in the region around the Protein-DNA constructs. These results are further corroborated with simulations using a geometric model for the excess charge density as function of radial distance from the protein core. Further, we investigate the influence of solution ionic strength on the structure of the DNA corona and demonstrate a reduction in the extension of the DNA corona with increasing concentration of NaCl in solution for the case of both single and double stranded DNA shells. Our work reveals the distribution of counterions in the vicinity of Protein-DNA conjugates and decouples the effect of solution ionic strength on the thickness of the DNA layer.

  15. Microstructure of 3D-Printed Polymer Composites Investigated by Small-Angle Neutron Scattering

    NASA Astrophysics Data System (ADS)

    Kang, Tae Hui; Compton, Brett G.; Heller, William T.; Urban, Voker S.; Duty, Chad E.; Do, Changwoo

    Polymer composites printed from the large scale printer at Manufacturing Demonstration Facility at Oak Ridge National Laboratory have been investigated by small-angle neutron scattering (SANS). For the Acrylonitrile Butadiene Styrene (ABS)/Carbon Fiber (CF) composites, the microstructure of polymer domains and the alignment of CF have been characterized across the layer from the printed piece. CF shows strong anisotropic alignment along the printing direction due to the flow of polymer melt at the nozzle. Order parameter of the anisotropy which ranges from -0.11 to -0.06 exhibits strong correlation with the position within the layer: stronger alignment near the layer interface. It is also confirmed that the existence of CF reduces the polymer domain correlation length significantly and reinforces the mechanical strength of the polymer composites. For the Epoxy/nano-clay platelet composites, the effect of processing condition, nozzle size, and the addition of the another filler, Silicon Carbide (SC), have been investigated by SANS. Nano-clay platelet shows strong anisotropic alignment along the printing direction as well. Order parameter of the anisotropy varies according to nozzle size and presence of the SC, and difference disappears at high Q region. Scientific User Facilities Division and Materials Sciences and Energy Division, Office of Basic Energy Sciences, U.S. Department of Energy.

  16. Small-Angle Neutron Scattering study of the NIST mAb reference material

    NASA Astrophysics Data System (ADS)

    Castellanos, Maria Monica; Liu, Yun; Krueger, Susan; Curtis, Joseph

    Monoclonal antibodies (mAbs) are of great interest to the biopharmaceutical industry because they can be engineered to target specific antigens. Due to their importance, the biomanufacturing initiative at NIST is developing an IgG1 mAb reference material `NIST mAb', which can be used by industry, academia, and regulatory authorities. As part of this collaborative effort, we aim at characterizing the reference material using neutron scattering techniques. We have studied the small-angle scattering profile of the NIST mAb in a histidine buffer at 0 and 150 mM NaCl. Using Monte Carlo simulations, we generate an ensemble of structures and calculate their theoretical scattering profile, which can be directly compared with experimental data. Moreover, we analyze the structure factor to understand the effect of solution conditions on the protein-protein interactions. Finally, we have measured the solution scattering of the NIST mAb, while simultaneously performing freeze/thaw cycles, in order to investigate if the solution structure was affected upon freezing. The results from neutron scattering not only support the development of the reference material, but also provide insights on its stability and guide efforts for its development under different formulations.

  17. Improving small-angle X-ray scattering data for structural analyses of the RNA world

    PubMed Central

    Rambo, Robert P.; Tainer, John A.

    2010-01-01

    Defining the shape, conformation, or assembly state of an RNA in solution often requires multiple investigative tools ranging from nucleotide analog interference mapping to X-ray crystallography. A key addition to this toolbox is small-angle X-ray scattering (SAXS). SAXS provides direct structural information regarding the size, shape, and flexibility of the particle in solution and has proven powerful for analyses of RNA structures with minimal requirements for sample concentration and volumes. In principle, SAXS can provide reliable data on small and large RNA molecules. In practice, SAXS investigations of RNA samples can show inconsistencies that suggest limitations in the SAXS experimental analyses or problems with the samples. Here, we show through investigations on the SAM-I riboswitch, the Group I intron P4-P6 domain, 30S ribosomal subunit from Sulfolobus solfataricus (30S), brome mosaic virus tRNA-like structure (BMV TLS), Thermotoga maritima asd lysine riboswitch, the recombinant tRNAval, and yeast tRNAphe that many problems with SAXS experiments on RNA samples derive from heterogeneity of the folded RNA. Furthermore, we propose and test a general approach to reducing these sample limitations for accurate SAXS analyses of RNA. Together our method and results show that SAXS with synchrotron radiation has great potential to provide accurate RNA shapes, conformations, and assembly states in solution that inform RNA biological functions in fundamental ways. PMID:20106957

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

    NASA Astrophysics Data System (ADS)

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

    2012-10-01

    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.

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

    SciTech Connect

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

    2015-01-01

    A set of quantitative techniques is suggested for assessing SAXS data quality. These are applied in the form of a script, SAXStats, to a test set of 27 proteins, showing that these techniques are more sensitive than manual assessment of data quality. 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.

  20. In situ small angle neutron scattering revealing ion sorption in microporous carbon electrical double layer capacitors.

    PubMed

    Boukhalfa, Sofiane; Gordon, Daniel; He, Lilin; Melnichenko, Yuri B; Nitta, Naoki; Magasinski, Alexandre; Yushin, Gleb

    2014-03-25

    Experimental studies showed the impact of the electrolyte solvents on both the ion transport and the specific capacitance of microporous carbons. However, the related structure-property relationships remain largely unclear and the reported results are inconsistent. The details of the interactions of the charged carbon pore walls with electrolyte ions and solvent molecules at a subnanometer scale are still largely unknown. Here for the first time we utilize in situ small angle neutron scattering (SANS) to reveal the electroadsorption of organic electrolyte ions in carbon pores of different sizes. A 1 M solution of tetraethylammonium tetrafluoroborate (TEATFB) salt in deuterated acetonitrile (d-AN) was used in an activated carbon with the pore size distribution similar to that of the carbons used in commercial double layer capacitors. In spite of the incomplete wetting of the smallest carbon pores by the d-AN, we observed enhanced ion sorption in subnanometer pores under the applied potential. Such results suggest the visible impact of electrowetting phenomena counterbalancing the high energy of the carbon/electrolyte interface in small pores. This behavior may explain the characteristic butterfly wing shape of the cyclic voltammetry curve that demonstrates higher specific capacitance at higher applied potentials, when the smallest pores become more accessible to electrolyte. Our study outlines a general methodology for studying various organic salts-solvent-carbon combinations.

  1. On the small angle twist sub-grain boundaries in Ti3AlC2

    NASA Astrophysics Data System (ADS)

    Zhang, Hui; Zhang, Chao; Hu, Tao; Zhan, Xun; Wang, Xiaohui; Zhou, Yanchun

    2016-04-01

    Tilt-dominated grain boundaries have been investigated in depth in the deformation of MAX phases. In stark contrast, another important type of grain boundaries, twist grain boundaries, have long been overlooked. Here, we report on the observation of small angle twist sub-grain boundaries in a typical MAX phase Ti3AlC2 compressed at 1200 °C, which comprise hexagonal screw dislocation networks formed by basal dislocation reactions. By first-principles investigations on atomic-scale deformation and general stacking fault energy landscapes, it is unequivocally demonstrated that the twist sub-grain boundaries are most likely located between Al and Ti4f (Ti located at the 4f Wyckoff sites of P63/mmc) layers, with breaking of the weakly bonded Al–Ti4f. The twist angle increases with the increase of deformation and is estimated to be around 0.5° for a deformation of 26%. This work may shed light on sub-grain boundaries of MAX phases, and provide fundamental information for future atomic-scale simulations.

  2. On the small angle twist sub-grain boundaries in Ti3AlC2

    PubMed Central

    Zhang, Hui; Zhang, Chao; Hu, Tao; Zhan, Xun; Wang, Xiaohui; Zhou, Yanchun

    2016-01-01

    Tilt-dominated grain boundaries have been investigated in depth in the deformation of MAX phases. In stark contrast, another important type of grain boundaries, twist grain boundaries, have long been overlooked. Here, we report on the observation of small angle twist sub-grain boundaries in a typical MAX phase Ti3AlC2 compressed at 1200 °C, which comprise hexagonal screw dislocation networks formed by basal dislocation reactions. By first-principles investigations on atomic-scale deformation and general stacking fault energy landscapes, it is unequivocally demonstrated that the twist sub-grain boundaries are most likely located between Al and Ti4f (Ti located at the 4f Wyckoff sites of P63/mmc) layers, with breaking of the weakly bonded Al–Ti4f. The twist angle increases with the increase of deformation and is estimated to be around 0.5° for a deformation of 26%. This work may shed light on sub-grain boundaries of MAX phases, and provide fundamental information for future atomic-scale simulations. PMID:27034075

  3. Determining the melt miscibility of commercial polyolefin blends by Small-Angle Light Scattering

    NASA Astrophysics Data System (ADS)

    Peng, Ping

    2005-03-01

    The melt miscibility of high-density polyethylene (HDPE) (Mw = 52 kg/mol, PDI = 2.9) and linear low-density polyethylenes (LLDPEs) based on homogeneous ethylene-1-butene copolymers (EB0187: 18.7 mol% butene branches, Mw = 58.1 kg/mol and EB0059: 5.9 mol% butene branches, Mw = 70 kg/mol) is determined by Small-Angle Light Scattering (SALS) under parallel-polarized optical alignment. Blends with branching density differences (δy) ranging from 5.9 to 18.7 mol% were studied. For the HDPE/EB0187 blend, (δy = 18.7%), cooling and isothermal measurements (2 h) in the melt can be used to determine the miscibility and the phase boundary. When this blend is rapidly cooled room temperature, the resulting SALS patterns show that the size of phase separated domain (˜ 1 μm) is much smaller than the average spherulite size (68 μm). These results consist with our microscopic observations and the transmitted light measured simultaneously with the VV scattering in the melt. From the compositions studied, we can conclude that this blend exhibits UCST behavior. For blends with lower δy, isothermal measurements provide a sensitive means for determining the melt miscibility. Based on the above observations, we can conclude that SALS can be used to determine the melt miscibility of polyolefin blends.

  4. Monomeric Amyloid Beta Peptide in Hexafluoroisopropanol Detected by Small Angle Neutron Scattering

    PubMed Central

    Zhang-Haagen, Bo; Biehl, Ralf; Nagel-Steger, Luitgard; Radulescu, Aurel; Richter, Dieter; Willbold, Dieter

    2016-01-01

    Small proteins like amyloid beta (Aβ) monomers are related to neurodegenerative disorders by aggregation to insoluble fibrils. Small angle neutron scattering (SANS) is a nondestructive method to observe the aggregation process in solution. We show that SANS is able to resolve monomers of small molecular weight like Aβ for aggregation studies. We examine Aβ monomers after prolonged storing in d-hexafluoroisopropanol (dHFIP) by using SANS and dynamic light scattering (DLS). We determined the radius of gyration from SANS as 1.0±0.1 nm for Aβ1–40 and 1.6±0.1 nm for Aβ1–42 in agreement with 3D NMR structures in similar solvents suggesting a solvent surface layer with 5% increased density. After initial dissolution in dHFIP Aβ aggregates sediment with a major component of pure monomers showing a hydrodynamic radius of 1.8±0.3 nm for Aβ1–40 and 3.2±0.4 nm for Aβ1–42 including a surface layer of dHFIP solvent molecules. PMID:26919121

  5. Estimation and modeling of coal pore accessibility using small angle neutron scattering

    SciTech Connect

    Zhang, Rui; Liu, Shimin; Bahadur, Jitendra; Elsworth, Derek; Melnichenko, Yuri; He, Lilin; Wang, Yi

    2015-09-04

    Gas diffusion in coal is controlled by nano-structure of the pores. The interconnectivity of pores not only determines the dynamics of gas transport in the coal matrix but also influences the mechanical strength. In this study, small angle neutron scattering (SANS) was employed to quantify pore accessibility for two coal samples, one of sub-bituminous rank and the other of anthracite rank. Moreover, a theoretical pore accessibility model was proposed based on scattering intensities under both vacuum and zero average contrast (ZAC) conditions. Our results show that scattering intensity decreases with increasing gas pressure using deuterated methane (CD4) at low Q values for both coals. Pores smaller than 40 nm in radius are less accessible for anthracite than sub-bituminous coal. On the contrary, when the pore radius is larger than 40 nm, the pore accessibility of anthracite becomes larger than that of sub-bituminous coal. Only 20% of pores are accessible to CD4 for anthracite and 37% for sub-bituminous coal, where the pore radius is 16 nm. For these two coals, pore accessibility and pore radius follows a power-law relationship.

  6. Estimation and modeling of coal pore accessibility using small angle neutron scattering

    DOE PAGES

    Zhang, Rui; Liu, Shimin; Bahadur, Jitendra; Elsworth, Derek; Melnichenko, Yuri; He, Lilin; Wang, Yi

    2015-09-04

    Gas diffusion in coal is controlled by nano-structure of the pores. The interconnectivity of pores not only determines the dynamics of gas transport in the coal matrix but also influences the mechanical strength. In this study, small angle neutron scattering (SANS) was employed to quantify pore accessibility for two coal samples, one of sub-bituminous rank and the other of anthracite rank. Moreover, a theoretical pore accessibility model was proposed based on scattering intensities under both vacuum and zero average contrast (ZAC) conditions. Our results show that scattering intensity decreases with increasing gas pressure using deuterated methane (CD4) at low Qmore » values for both coals. Pores smaller than 40 nm in radius are less accessible for anthracite than sub-bituminous coal. On the contrary, when the pore radius is larger than 40 nm, the pore accessibility of anthracite becomes larger than that of sub-bituminous coal. Only 20% of pores are accessible to CD4 for anthracite and 37% for sub-bituminous coal, where the pore radius is 16 nm. For these two coals, pore accessibility and pore radius follows a power-law relationship.« less

  7. Small-angle scattering studies of the pore spaces of shaly rocks

    NASA Astrophysics Data System (ADS)

    Hall, Peter L.; Mildner, David F. R.; Borst, Roger L.

    1986-02-01

    Small-angle neutron and X ray scattering (SANS and SAXS) measurements have been performed on shaly rocks from a variety of oil field locations. Thin core sections cut parallel to their bedding planes give circularly symmetric scattering patterns. On the basis of the model of Debye et al., the data indicate characteristic pore dimensions of 9-15 nm. Sections cut normal to the bedding planes exhibit elliptically symmetric scattering indicative of pores flattened in the direction of sedimentary compaction. Fourier inversion of the symmetric SANS data in all cases yields a broad distribution of pore diameters having peaks typically in the range 4-6 nm. These distributions are in reasonable agreement with distributions derived from nitrogen adsorption isotherms, although often in disagreement with nitrogen desorption or mercury porosimetry data. At higher scattering vectors, in the Porod region, differences between the SAXS and SANS data are observed which are explained in terms of the rather different sensitives of the two techniques to empty and filled pores. The data indicate that a significant component of the total porosity is due to pores of less than 2 nm in diameter, in which water is retained under ambient conditions. In several cases, pore dimensions measured by SANS increase after extraction of bitumens by methylene chloride solution, suggesting an intimate microscopic association of hydrocarbon and fine mineral grains.

  8. Study of nanoscale structures in hydrated biomaterials using small-angle neutron scattering

    PubMed Central

    Luk, Arnold; Murthy, N. Sanjeeva; Wang, Wenjie; Rojas, Ramiro; Kohn, Joachim

    2012-01-01

    Distribution of water in three classes of biomedically relevant and degradable polymers was investigated using small-angle neutron scattering. In semicrystalline polymers, such as poly(lactic acid) and poly(glycolic acid), water was found to diffuse preferentially into the noncrystalline regions. In amorphous polymers, such as poly(D,L-lactic acid) and poly(lactic-co-glycolic acid), the scattering after 7-days of incubation was attributed to water in microvoids that form following the hydrolytic degradation of the polymer. In amorphous copolymers containing hydrophobic segments (desaminotyrosyl-tyrosine ethyl ester) and hydrophilic blocks (poly(ethylene glycol) PEG), a sequence of distinct regimes of hydration were observed: homogeneous distribution (~ 10 Å length scales) at <13 wt% PEG (~ 1 water per EG), clusters of hydrated domains (~50 Å radius) separated at 24 wt% PEG (1 to 2 water per EG), uniformly distributed hydrated domains at 41 wt% PEG (~ 4 water per EG), and phase inversion at > 50 wt% PEG ( > 6 water per EG ). Increasing PEG content increased the number of these domains with only a small decrease in distance between the domains. These discrete domains appeared to coalesce to form submicron droplets at ~60 °C, above the melting temperature of crystalline PEG. Significance of such observations on the evolution of μm size channels that form during hydrolytic erosion is discussed. PMID:22227373

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

    PubMed Central

    Skou, Magda; Skou, Søren; Jensen, Thomas G.; Vestergaard, Bente; Gillilan, Richard E.

    2014-01-01

    Owing to the demand for low sample consumption and automated sample changing capabilities at synchrotron small-angle X-ray (solution) scattering (SAXS) beamlines, X-ray microfluidics is receiving continuously increasing attention. Here, a remote-controlled microfluidic device is presented for simultaneous SAXS and ultraviolet absorption measurements during protein dialysis, integrated directly on a SAXS beamline. Microfluidic dialysis can be used for monitoring structural changes in response to buffer exchange or, as demonstrated, protein concentration. By collecting X-ray data during the concentration procedure, the risk of inducing protein aggregation due to excessive concentration and storage is eliminated, resulting in reduced sample consumption and improved data quality. The proof of concept demonstrates the effect of halted or continuous flow in the microfluidic device. No sample aggregation was induced by the concentration process at the levels achieved in these experiments. Simulations of fluid dynamics and transport properties within the device strongly suggest that aggregates, and possibly even higher-order oligomers, are preferentially retained by the device, resulting in incidental sample purification. Hence, this versatile microfluidic device enables investigation of experimentally induced structural changes under dynamically controllable sample conditions. PMID:25242913

  10. Percolating bulk-heterostructures from neutron reflectometry and small angle scattering data

    NASA Astrophysics Data System (ADS)

    Olds, Daniel; Duxbury, Phillip

    2013-03-01

    We present a novel algorithm for efficiently calculating the simulated small angle scattering data of any discretized morphological model of arbitrary scale and resolution, referred to as the distribution function method (DFM). Unlike standard SAS fitting methods, the DFM algorithm allows for the calculation of form factors and structure factors from complex nanoscale morphologies commonly encountered in many modern polymeric and nanoparticle based systems, which have no exact analytical corollary. The computational efficiency of the DFM algorithm suggests it's use in morphological model refinement. We will present a number of simple examples to demonstrate the accuracy and limits of the algorithm, followed by an example of incorporation of the DFM algorithm into reverse Monte Carlo structural refinement of bulk-heterojunction two-phase morphologies, such as those commonly found in organic photovoltaic devices. We will show that morphological features introduced via direct incorporation of experimental neutron reflectometry and SANS data to the models has a direct effect on the results of device simulations. The authors thank CORE-CM at Michigan State University for it's funding of this research.

  11. Fractal Structures on Fe3O4 Ferrofluid: A Small-Angle Neutron Scattering Study

    NASA Astrophysics Data System (ADS)

    Giri Rachman Putra, Edy; Seong, Baek Seok; Shin, Eunjoo; Ikram, Abarrul; Ani, Sistin Ari; Darminto

    2010-10-01

    A small-angle neutron scattering (SANS) which is a powerful technique to reveal the large scale structures was applied to investigate the fractal structures of water-based Fe3O4ferrofluid, magnetic fluid. The natural magnetite Fe3O4 from iron sand of several rivers in East Java Province of Indonesia was extracted and purified using magnetic separator. Four different ferrofluid concentrations, i.e. 0.5, 1.0, 2.0 and 3.0 Molar (M) were synthesized through a co-precipitation method and then dispersed in tetramethyl ammonium hydroxide (TMAH) as surfactant. The fractal aggregates in ferrofluid samples were observed from their SANS scattering distributions confirming the correlations to their concentrations. The mass fractal dimension changed from about 3 to 2 as ferrofluid concentration increased showing a deviation slope at intermediate scattering vector q range. The size of primary magnetic particle as a building block was determined by fitting the scattering profiles with a log-normal sphere model calculation. The mean average size of those magnetic particles is about 60 - 100 Å in diameter with a particle size distribution σ = 0.5.

  12. Small-angle x-ray scattering studies of the manganese stabilizing subunit in photosystem II.

    SciTech Connect

    Svensson, B.; Tiede, D. M.; Barry, B. A.; Univ. of Minnesota

    2002-08-29

    Small-angle X-ray scattering studies (SAXS) were used to determine the size, shape, and oligomeric composition of the manganese stabilizing protein (MSP) of photosystem II. This extrinsic protein subunit plays an important role in photosynthetic oxygen evolution. As its name implies, MSP stabilizes the tetranuclear Mn cluster of the water oxidation complex. Removal of MSP lowers activity and decreases the stability of active-site manganese. Reconstitution of MSP reverses these effects. In this study, MSP was extracted from spinach PSII membranes using CaCl{sub 2} or urea. Through the use of MALDI-TOF mass spectrometry, the molecular weight of MSP was determined to be 26.53 kDa. X-ray scattering results show that both samples display a monodisperse scattering pattern; this pattern is consistent with a homogeneous protein solution. The CaCl{sub 2} extracted and urea extracted MSP samples have radii of gyration of 25.9 {+-} 0.4 and 27.0 {+-} 0.01 {angstrom}, respectively. MSP is shown to be monomeric in solution. This was determined using a cytochrome c standard and the scattering intensity, extrapolated to zero scattering angle, which is proportional to the molecular weight. This SAXS study suggests that, in solution, MSP is a monomeric, elongated prolate ellipsoid with dimensions, 112 x 23 x 23 {angstrom}{sup 3} and an axial ratio of 4.8.

  13. Characterization of lysozyme adsorption in cellulosic chromatographic materials using small-angle neutron scattering.

    PubMed

    Koshari, Stijn H S; Wagner, Norman J; Lenhoff, Abraham M

    2015-06-19

    Measurements of the nanoscale structure of chromatographic adsorbents and the associated distribution of sorbed protein within the media can facilitate improvements in such media. We demonstrate a new technique for this purpose using small-angle neutron scattering (SANS) to characterize the nano- to microscale structure of the chromatographic media and sorbed protein under conditions relevant for preparative chromatographic separations. The adsorption of lysozyme on cellulosic S HyperCel™ (Pall Corporation), a strong cation exchanger, was investigated by SANS. The scattering spectrum is reduced to three contributions arising from (1) the chromatographic medium, (2) discrete protein molecules, and (3) the distribution of sorbed protein within the medium. These contributions are quantified for a range of protein loadings. The total concentration of protein in the chromatographic media can be quantified from the SANS spectrum and the protein is observed to retain its tertiary structure upon adsorption, within the resolution of the method. Further analysis of the SANS spectra shows that protein adsorption is uniform in the media. These measurement techniques provide new and valuable nanoscale information about protein sorption in chromatographic media.

  14. Small-angle neutron scattering reveals a pH-dependent conformational change in cellobiohydrolase I

    SciTech Connect

    Pingali, Sai Venkatesh; O'Neill, Hugh Michael; McGaughey, Joseph; Urban, Volker S; Myles, Dean A A; Petridis, Loukas; Smith, Jeremy C; Evans, Barbara R; Heller, William T

    2011-01-01

    Cellobiohydrolase I (Cel7A) of the fungus Trichoderma reesei (now classified as an anamorph of Hypocrea jecorina) hydrolyzes crystalline cellulose to soluble sugars, making it of key interest for producing fermentable sugars from biomass for biofuel production. The activity of the enzyme is pH-dependent, with its highest activity occurring at pH 4-5. To probe the response of the solution structure of Cel7A to changes in pH, we measured small angle neutron scattering of it in a series of solutions having pH values of 7.0, 6.0, 5.3, and 4.2. As the pH decreases from 7.0 to 5.3, the enzyme structure remains well defined, possessing a spatial differentiation between the cellulose binding domain and the catalytic core that only changes subtly. At pH 4.2, the solution conformation of the enzyme changes to a structure that is intermediate between a properly folded enzyme and a denatured, unfolded state, yet the secondary structure of the enzyme is essentially unaltered. The results indicate that at the pH of optimal activity, the catalytic core of the enzyme adopts a structure in which the compact packing typical of a fully folded polypeptide chain is disrupted and suggest that the increased range of structures afforded by this disordered state plays an important role in the increased activity of Cel7A through conformational selection.

  15. Small-angle neutron scattering correlation functions of bulk magnetic materials

    PubMed Central

    Mettus, Denis; Michels, Andreas

    2015-01-01

    On the basis of the continuum theory of micromagnetics, the correlation function of the spin-misalignment small-angle neutron scattering cross section of bulk ferromagnets (e.g. elemental polycrystalline ferromagnets, soft and hard magnetic nanocomposites, nanoporous ferromagnets, or magnetic steels) is computed. For such materials, the spin disorder which is related to spatial variations in the saturation magnetization and magnetic anisotropy field results in strong spin-misalignment scattering dΣM/dΩ along the forward direction. When the applied magnetic field is perpendicular to the incoming neutron beam, the characteristics of dΣM/dΩ (e.g. the angular anisotropy on a two-dimensional detector or the asymptotic power-law exponent) are determined by the ratio of magnetic anisotropy field strength H p to the jump ΔM in the saturation magnetization at internal interfaces. Here, the corresponding one- and two-dimensional real-space correlations are analyzed as a function of applied magnetic field, the ratio H p/ΔM, the single-particle form factor and the particle volume fraction. Finally, the theoretical results for the correlation function are compared with experimental data on nanocrystalline cobalt and nickel. PMID:26500464

  16. Characterization of fullerenes and fullerene derivatives by small-angle neutron scattering and transmission measurements

    SciTech Connect

    Melnichenko, Y.B.; Wignall, G.D.; Affholter, K.A.

    1997-01-01

    Small-angle neutron scattering (SANS) has been shown to be an appropriate technique for the structural characterization of fullerenes (1) in solvents with strong SANS contrast (e.g. CS{sub 2}) and we have extended initial studies of C{sub 60} (1) to include C{sub 70} and C{sub 84} moieties. Deuterated solvents (e.g. toluene-d{sub 8}) have a high scattering length density (SLD), which is close to that of C{sub 60}, so there is virtually no SANS contrast with the solvent. Hence, these particles are practically {open_quotes}invisible{close_quotes} in such media, though the negative scattering length of hydrogen means that SLD of H{sup 1}-containing materials is much lower, so they have strong contrast with toluene-d{sub 8}. Thus, SANS makes it possible to study the size and shapes of modified buckyballs and this paper describes the first results on cyclohexane-substituted fullerenes.

  17. Small-angle light scattering by airborne particulates: Environnement S.A. continuous particulate monitor

    NASA Astrophysics Data System (ADS)

    Renard, Jean-Baptiste; Thaury, Claire; Mineau, Jean-Luc; Gaubicher, Bertrand

    2010-08-01

    Airborne particulate matter may have an effect on human health. It is therefore necessary to determine and control in real time the evolution of the concentration and mass of particulates in the ambient air. These parameters can be obtained using optical methods. We propose here a new instrument, 'CPM' (continuous particulate monitor), for the measurement of light scattered by ambient particulates at small angles. This geometry allows simultaneous and separate detections of PM10, PM2.5 and PM1 fractions of airborne particulate matter, with no influence of their chemical nature and without using theoretical calculations. The ambient air is collected through a standard sampling head (PM10 inlet according to EN 12341, PM2.5 inlet according to EN 14907; or PM1, TSP inlets, standard US EPA inlets). The analysis of the first measurements demonstrates that this new instrument can detect, for each of the seven defined size ranges, real-time variations of particulate content in the ambient air. The measured concentrations (expressed in number per liter) can be converted into total mass concentrations (expressed in micrograms per cubic meter) of all fractions of airborne particulate matters sampled by the system. Periodic comparison with a beta-attenuation mass monitor (MP101M Beta Gauge Analyzer from Environnement S.A. company) allows the calculation of a calibration factor as a function of the mean particulate density that is used for this conversion. It is then possible to provide real-time relative variations of aerosol mass concentration.

  18. Dynamic Conformations of Nucleosome Arrays in Solution from Small-Angle X-ray Scattering

    NASA Astrophysics Data System (ADS)

    Howell, Steven C.

    Chromatin conformation and dynamics remains unsolved despite the critical role of the chromatin in fundamental genetic functions such as transcription, replication, and repair. At the molecular level, chromatin can be viewed as a linear array of nucleosomes, each consisting of 147 base pairs (bp) of double-stranded DNA (dsDNA) wrapped around a protein core and connected by 10 to 90 bp of linker dsDNA. Using small-angle X-ray scattering (SAXS), we investigated how the conformations of model nucleosome arrays in solution are modulated by ionic condition as well as the effect of linker histone proteins. To facilitate ensemble modeling of these SAXS measurements, we developed a simulation method that treats coarse-grained DNA as a Markov chain, then explores possible DNA conformations using Metropolis Monte Carlo (MC) sampling. This algorithm extends the functionality of SASSIE, a program used to model intrinsically disordered biological molecules, adding to the previous methods for simulating protein, carbohydrates, and single-stranded DNA. Our SAXS measurements of various nucleosome arrays together with the MC generated models provide valuable solution structure information identifying specific differences from the structure of crystallized arrays.

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

    NASA Astrophysics Data System (ADS)

    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.

  20. New Insights into Pore Characteristics and Hydrocarbon Generation of Shale Using Small-Angle Neutron Scattering

    NASA Astrophysics Data System (ADS)

    Ding, M.; Hartl, M.; Wang, Y.; Hjelm, R.

    2014-12-01

    Pore size, distribution, connectivity, and shape as well as hydrocarbon saturation and composition reflect the history of hydrocarbon maturation and migration. However, characterization of the underlying factors and processes controlling hydrocarbons behavior in tight rocks is extremely limited, especially lacking of direct experimental observations. We have studied the pore characteristics of marine and lacustrine shale from the Erdos basin, China during laboratory pyrolysis using small-angle neutron scattering (SANS). Our SANS results show that scattering intensity of smaller pores (< 20 nm)/larger Q values of shale samples increase systematically as temperature increase during pyrolysis from 250 oC to 600oC (Fig.1a). These results in combination with hydrocarbon fractions measurements during the same process (Fig. 1b) provide a quantitative relation between pore characteristics and hydrocarbons generation. Our results indicate that hydrocarbon expulsion primarily causes the observed changes in smaller pores. They also demonstrate that due to its sensitivity to hydrogen, SANS locates all pores whether the pore is filled or not with hydrocarbons. Thus, SANS is particularly suited for probing hydrocarbon behavior in tight shale reservoirs and the factors that impact their pore dynamics for the petroleum industry.

  1. Quasielastic small-angle neutron scattering from heavy water solutions of cyclodextrins.

    PubMed

    Kusmin, André; Lechner, Ruep E; Saenger, Wolfram

    2011-01-14

    We present a model for quasielastic neutron scattering (QENS) by an aqueous solution of compact and inflexible molecules. This model accounts for time-dependent spatial pair correlations between the atoms of the same as well as of distinct molecules and includes all coherent and incoherent neutron scattering contributions. The extension of the static theory of the excluded volume effect [A. K. Soper, J. Phys.: Condens. Matter 9, 2399 (1997)] to the time-dependent (dynamic) case allows us to obtain simplified model expressions for QENS spectra in the low Q region in the uniform fluid approximation. The resulting expressions describe the quasielastic small-angle neutron scattering (QESANS) spectra of D(2)O solutions of native and methylated cyclodextrins well, yielding in particular translational and rotational diffusion coefficients of these compounds in aqueous solution. Finally, we discuss the full potential of the QESANS analysis (that is, beyond the uniform fluid approximation), in particular, the information on solute-solvent interactions (e.g., hydration shell properties) that such an analysis can provide, in principle.

  2. How Random are Intrinsically Disordered Proteins? A Small Angle Scattering Perspective

    PubMed Central

    Receveur-Bréchot, Véronique; Durand, Dominique

    2012-01-01

    While the crucial role of intrinsically disordered proteins (IDPs) in the cell cycle is now recognized, deciphering their molecular mode of action at the structural level still remains highly challenging and requires a combination of many biophysical approaches. Among them, small angle X-ray scattering (SAXS) has been extremely successful in the last decade and has become an indispensable technique for addressing many of the fundamental questions regarding the activities of IDPs. After introducing some experimental issues specific to IDPs and in relation to the latest technical developments, this article presents the interest of the theory of polymer physics to evaluate the flexibility of fully disordered proteins. The different strategies to obtain 3-dimensional models of IDPs, free in solution and associated in a complex, are then reviewed. Indeed, recent computational advances have made it possible to readily extract maximum information from the scattering curve with a special emphasis on highly flexible systems, such as multidomain proteins and IDPs. Furthermore, integrated computational approaches now enable the generation of ensembles of conformers to translate the unique flexible characteristics of IDPs by taking into consideration the constraints of more and more various complementary experiment. In particular, a combination of SAXS with high-resolution techniques, such as x-ray crystallography and NMR, allows us to provide reliable models and to gain unique structural insights about the protein over multiple structural scales. The latest neutron scattering experiments also promise new advances in the study of the conformational changes of macromolecules involving more complex systems. PMID:22044150

  3. Discovering New Features of Protein Complexes Structures by Small-Angle X-Ray Scattering

    NASA Astrophysics Data System (ADS)

    Oliveira, C. L. P.; Vorup-Jensen, T.; Andersen, C. B. F.; Andersen, G. R.; Pedersen, J. S.

    In spite of the recent advances in the X-Ray crystallography and nuclear magnetic resonance techniques, the determination of the quaternary structure of large protein complexes is still a challenge in molecular biology and biological sciences. In this respect, small-angle X-ray scattering (SAXS) is a key technique, enabling the determination of the possible structural conformation of complexes in an almost native state. Despite of this book being devoted to scattering techniques by synchrotron radiation, in this chapter we present two examples of application of laboratory-based SAXS to protein solution. The fundaments of the technique are obviously the same and have been deeply described in Chap. 2. In this chapter, we will introduce the application of SAXS to protein solution. Special emphasis is done on data reduction and absolute units calibration. As an example to illustrate the power of this technique, two new data sets for two protein complexes will be presented. This will show how high-quality SAXS data combined with advanced model strategies enables the determination of the quaternary structure of protein complexes.

  4. Small Angle Neutron Scattering (SANS) Studies on the Structural Evolution of Pyromellitamide Self-assembled Gels

    DOE PAGES

    Scott, Jamieson; Tong, Katie; William, Hamilton; He, Lilin; James, Michael; Thordarson, Pall; Boukhalfa, Sofiane

    2014-10-31

    The kinetics of aggregation of two pyromellitamide gelators; tetrabutyl- (C4) and tetrahexylpyromellitamide (C6), in deuterated cyclohexane has been investigated by small angle neutron scattering (SANS) for up to six days. The purpose of this study was to improve our understanding of how self-assembled gels are formed. Short-term (< 3 hour) time scales revealed multiple phases with the data for the tetrabutylpyromellitamide C4 indicating one dimensional stacking and aggregation corresponding to a multi-fiber braided cluster arrangement that is about 35 Å in diameter. The corresponding tetrahexylpyromellitamide C6 data suggests that the C6 also forms one-dimensional stacks but that these aggregate tomore » a thicker multi-fiber braided cluster that have a diameter of 61.8 Å. Over a longer period of time, the radius, persistence length and contour length all continue to increase in 6 days after cooling. This data suggests that structural changes in self-assembled gels occur over a period exceeding several days and that fairly subtle changes in the structure (e.g. tail-length) can influence the packing of molecules in self-assembled gels on the single-to-few fiber bundle stage.« less

  5. Small-angle neutron scattering studies of chlorophyll micelles: Models for bacterial antenna chlorophyll

    PubMed Central

    Worcester, D. L.; Michalski, T. J.; Katz, J. J.

    1986-01-01

    Micelles of hydrated chlorophyll a (P740), bacteriochlorophyll a (P865), bacteriochlorophyll c (P750), and pheophytin a prepared in organic media have been studied by small-angle neutron scattering to determine their shape, size, and mass per unit length. All of the micelles are hollow cylinders of well-defined size. The P740 and P750 cylinders are essentially monolayers of macrocycles crosslinked by water, probably in an arrangement similar to that of crystals of chlorophyll derivatives. The P865 micelle is more nearly a bilayer of macrocycles. We show that the curvature necessary to form cylinders probably results from intrinsic curvature of the five-coordinated chlorophyll macrocycle. Studies of P740 micelle formation and the disaggregating effects of another nucleophile (pyridine) are described. As the P750 micelles are nearly identical in size and optical spectra to the rod-shaped structures observed in chlorosomes, and the P865 micelles have optical properties very similar to the in vivo properties of the long-wavelength antenna of purple photosynthetic bacteria, we propose that features of the hydrated cylindrical micelles of these chlorophylls provide good models for antenna chlorophyll in photosynthetic bacteria. Images PMID:16593703

  6. Small-Angle Neutron Scattering and Fluorescence Studies of Mixed Surfactants with Dodecyl Tails.

    PubMed

    Griffiths; Whatton; Abbott; Kwan; Pitt; Howe; King; Heenan

    1999-07-01

    The mixed micelles formed in solutions of the anionic surfactant sodium dodecylsulfate (SDS) and the nonionic surfactant dodecylmalono-bis-N-methylglucamide (DBNMG) were studied by surface tension, fluorescence, and small-angle neutron scattering. Measurements of the critical micelle concentration (CMC) by surface tension and fluorescence show that these two surfactants mix nonideally. The experimental values of the CMCs for surfactant mixtures for all compositions are less than the ideal prediction proposed by Clint (J. Chem. Soc. 71, 1327 (1975)). Regular solution theory (for example, Penfold et al., Langmuir 11, 2498 (1995)) can be used to calculate the composition of the micelle at the CMC. The micellar composition thus calculated differs significantly from that at higher total surfactant concentrations, the latter being much closer to the stoichiometric composition. The polarity of the micellar environment, as perceived by a solubilized fluorescence probe, is identical for both the single-component and the mixed micelles. The scattering data show that the mixed micelles are comparable in size to the pure nonionic micelle and slightly larger than the anionic micelle. Parallel studies with deuterated SDS showed no evidence of segregation or local ordering within the mixed micelle. The effective charge on the mixed micelle is determined by the amount of ionic surfactant within the micelle. Addition of 0.1 M NaCl to these systems has no effect on the CMC, micelle ellipticity, and aggregation number-a behavior very different from that observed for simple SDS solutions. Copyright 1999 Academic Press.

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

    NASA Astrophysics Data System (ADS)

    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)

  8. Accurate assessment of mass, models and resolution by small-angle scattering

    PubMed Central

    Rambo, Robert P.; Tainer, John A.

    2013-01-01

    Modern small angle scattering (SAS) experiments with X-rays or neutrons provide a comprehensive, resolution-limited observation of the thermodynamic state. However, methods for evaluating mass and validating SAS based models and resolution have been inadequate. Here, we define the volume-of-correlation, Vc: a SAS invariant derived from the scattered intensities that is specific to the structural state of the particle, yet independent of concentration and the requirements of a compact, folded particle. We show Vc defines a ratio, Qr, that determines the molecular mass of proteins or RNA ranging from 10 to 1,000 kDa. Furthermore, we propose a statistically robust method for assessing model-data agreements (X2free) akin to cross-validation. Our approach prevents over-fitting of the SAS data and can be used with a newly defined metric, Rsas, for quantitative evaluation of resolution. Together, these metrics (Vc, Qr, X2free, and Rsas) provide analytical tools for unbiased and accurate macromolecular structural characterizations in solution. PMID:23619693

  9. Angular distributions of reflected and refracted relativistic electron beams crossing a thin planar target at a small angle to its surface

    SciTech Connect

    Serov, A. V.; Mamonov, I. A.; Kol’tsov, A. V.

    2015-10-15

    The scattering of electrons by aluminum, copper, and lead foils, as well as by bimetallic aluminum-lead and aluminum-copper foils, has been studied experimentally. A microtron with an energy of particles of 7.4 MeV has been used as a source of electrons. The beam of particles incident on a target at small angles is split into particles reflected from the foil, which constitute a reflected beam, and particles crossing the foil, which constitute a refracted beam. The effect of the material and thickness of the foil, as well as the angle between the initial trajectory of the beam and the plane of the target, on the direction of motion and the angular divergence of the beam crossing the foil and the beam reflected from the foil has been analyzed. Furthermore, the effect of the sequence of metal layers in bimetallic films on the angles of refraction and reflection of the beam has been examined.

  10. Grazing incidence angle based sensing approach integrated with fiber-optic Fourier transform infrared (FO-FTIR) spectroscopy for remote and label-free detection of medical device contaminations

    SciTech Connect

    Hassan, Moinuddin Ilev, Ilko

    2014-10-15

    Contamination of medical devices has become a critical and prevalent public health safety concern since medical devices are being increasingly used in clinical practices for diagnostics, therapeutics and medical implants. The development of effective sensing methods for real-time detection of pathogenic contamination is needed to prevent and reduce the spread of infections to patients and the healthcare community. In this study, a hollow-core fiber-optic Fourier transform infrared spectroscopy methodology employing a grazing incidence angle based sensing approach (FO-FTIR-GIA) was developed for detection of various biochemical contaminants on medical device surfaces. We demonstrated the sensitivity of FO-FTIR-GIA sensing approach for non-contact and label-free detection of contaminants such as lipopolysaccharide from various surface materials relevant to medical device. The proposed sensing system can detect at a minimum loading concentration of approximately 0.7 μg/cm{sup 2}. The FO-FTIR-GIA has the potential for the detection of unwanted pathogen in real time.

  11. Grazing incidence angle based sensing approach integrated with fiber-optic Fourier transform infrared (FO-FTIR) spectroscopy for remote and label-free detection of medical device contaminations.

    PubMed

    Hassan, Moinuddin; Ilev, Ilko

    2014-10-01

    Contamination of medical devices has become a critical and prevalent public health safety concern since medical devices are being increasingly used in clinical practices for diagnostics, therapeutics and medical implants. The development of effective sensing methods for real-time detection of pathogenic contamination is needed to prevent and reduce the spread of infections to patients and the healthcare community. In this study, a hollow-core fiber-optic Fourier transform infrared spectroscopy methodology employing a grazing incidence angle based sensing approach (FO-FTIR-GIA) was developed for detection of various biochemical contaminants on medical device surfaces. We demonstrated the sensitivity of FO-FTIR-GIA sensing approach for non-contact and label-free detection of contaminants such as lipopolysaccharide from various surface materials relevant to medical device. The proposed sensing system can detect at a minimum loading concentration of approximately 0.7 μg/cm(2). The FO-FTIR-GIA has the potential for the detection of unwanted pathogen in real time.

  12. The Diffraction Pattern Calculator (DPC) toolkit: a user-friendly approach to unit-cell lattice parameter identification of two-dimensional grazing-incidence wide-angle X-ray scattering data

    PubMed Central

    Hailey, Anna K.; Hiszpanski, Anna M.; Smilgies, Detlef-M.; Loo, Yueh-Lin

    2014-01-01

    The DPC toolkit is a simple-to-use computational tool that helps users identify the unit-cell lattice parameters of a crystal structure that are consistent with a set of two-dimensional grazing-incidence wide-angle X-ray scattering data. The input data requirements are minimal and easy to assemble from data sets collected with any position-sensitive detector, and the user is required to make as few initial assumptions about the crystal structure as possible. By selecting manual or automatic modes of operation, the user can either visually match the positions of the experimental and calculated reflections by individually tuning the unit-cell parameters or have the program perform this process for them. Examples that demonstrate the utility of this program include determining the lattice parameters of a polymorph of a fluorinated contorted hexabenzocoronene in a blind test and refining the lattice parameters of the thin-film phase of 5,11-bis(triethylsilylethynyl)anthradithiophene with the unit-cell dimensions of its bulk crystal structure being the initial inputs. PMID:25484845

  13. X-ray reflectivity and grazing incidence diffraction studies of interaction between human adhesion/growth-regulatory galectin-1 and DPPE-GM1 lipid monolayer at an air/water interface.

    PubMed

    Majewski, J; André, S; Jones, E; Chi, E; Gabius, H-J

    2015-07-01

    The specific interaction of ganglioside GM1 with the homodimeric (prototype) endogenous lectin galectin-1 triggers growth regulation in tumor and activated effector T cells. This proven biorelevance directed interest to studying association of the lectin to a model surface, i.e. a 1,2-dihexadecanoyl-sn-glycero-3-phosphoethanolamine/ganglioside GM1 (80 : 20 mol%) monolayer, at a bioeffective concentration. Surface expansion by the lectin insertion was detected at a surface pressure of 20 mN/m. On combining the methods of grazing incidence X-ray diffraction and X-ray reflectivity, a transient decrease in lipid-ordered phase of the monolayer was observed. The measured electron density distribution indicated that galectin-1 is oriented with its long axis in the surface plane, ideal for cis-crosslinking. The data reveal a conspicuous difference to the way the pentameric lectin part of the cholera toxin, another GM1-specific lectin, is bound to the monolayer. They also encourage further efforts to monitor effects of structurally different members of the galectin family such as the functionally antagonistic chimera-type galectin-3.

  14. Characterization of AlInN/AlN/GaN FET structures using x-ray diffraction, x-ray reflectometry and grazing incidence x-ray fluorescence analysis

    NASA Astrophysics Data System (ADS)

    Lesnik, Andreas; Bläsing, Jürgen; Hennig, Jonas; Dadgar, Armin; Krost, Alois

    2014-09-01

    The structural parameters of AlInN/AlN/GaN high mobility field effect transistors (FETs) determine their electrical properties. The AlN-interlayer (spacer) thickness especially plays an important role to enhance the mobility and the density of the two dimensional electron gas (2DEG). However, structural characterization of this ultra-thin AlN-interlayer is ambiguous when only high resolution x-ray diffraction (HRXRD) and x-ray reflectometry (XRR) are taken into account. Here a combined layer analysis was performed using HRXRD, XRR and grazing incidence x-ray fluorescence (GIXRF) for the determination of the AlN-interlayer thickness. A sample series of AlInN/AlN/GaN FETs on Si(1 1 1) has been grown and analysed. The growth time of the AlN-interlayer was changed from 0 to 12 s and the AlInN barrier was grown nearly lattice matched to GaN with a nominal thickness of 5 nm. By the combination of HRXRD, XRR, GIXRF and simultaneous simulation of the data the determination of the spacer thickness was successfully performed.

  15. X-ray reflectivity and grazing incidence diffraction studies of interaction between human adhesion/growth-regulatory galectin-1 and DPPE-GM1 lipid monolayer at an air/water interface.

    PubMed

    Majewski, J; André, S; Jones, E; Chi, E; Gabius, H-J

    2015-07-01

    The specific interaction of ganglioside GM1 with the homodimeric (prototype) endogenous lectin galectin-1 triggers growth regulation in tumor and activated effector T cells. This proven biorelevance directed interest to studying association of the lectin to a model surface, i.e. a 1,2-dihexadecanoyl-sn-glycero-3-phosphoethanolamine/ganglioside GM1 (80 : 20 mol%) monolayer, at a bioeffective concentration. Surface expansion by the lectin insertion was detected at a surface pressure of 20 mN/m. On combining the methods of grazing incidence X-ray diffraction and X-ray reflectivity, a transient decrease in lipid-ordered phase of the monolayer was observed. The measured electron density distribution indicated that galectin-1 is oriented with its long axis in the surface plane, ideal for cis-crosslinking. The data reveal a conspicuous difference to the way the pentameric lectin part of the cholera toxin, another GM1-specific lectin, is bound to the monolayer. They also encourage further efforts to monitor effects of structurally different members of the galectin family such as the functionally antagonistic chimera-type galectin-3. PMID:26542007

  16. Physical interactions of fish protamine and antisepsis peptide drugs with bacterial membranes revealed by combination of specular x-ray reflectivity and grazing-incidence x-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Abuillan, Wasim; Schneck, Emanuel; Körner, Alexander; Brandenburg, Klaus; Gutsmann, Thomas; Gill, Tom; Vorobiev, Alexei; Konovalov, Oleg; Tanaka, Motomu

    2013-07-01

    As a defined model of outer membranes of gram negative bacteria, we investigated the interaction of monolayers of lipopolysacchrides from Salmonella enterica rough strains R90 (LPS Ra) with natural and synthetic peptides. The fine structures perpendicular to the membrane plane and the ion distribution near the interface were determined by specular x-ray reflectivity (XRR) and grazing-incidence x-ray fluorescence (GIXF) in the presence and absence of divalent cations. The unique combination of XRR and GIXF allows for the quantitative identification of different modes of interactions in a high spatial resolution, which cannot be assessed by other experimental methods. Natural fish protamine disrupts the stratified membrane structures in the absence of Ca2+ ions, while staying away from the membrane surface in the presence of Ca2+ ions. In contrast, synthetic antisepsis peptide Pep 19-2.5 weakly adsorbs to the membrane and stays near the uncharged sugar units even in the absence of Ca2+. In the presence of Ca2+, Pep 19-2.5 can reach the negatively charged inner core without destroying the barrier capability against ions.

  17. The Diffraction Pattern Calculator (DPC) toolkit: a user-friendly approach to unit-cell lattice parameter identification of two-dimensional grazing-incidence wide-angle X-ray scattering data.

    PubMed

    Hailey, Anna K; Hiszpanski, Anna M; Smilgies, Detlef-M; Loo, Yueh-Lin

    2014-12-01

    The DPC toolkit is a simple-to-use computational tool that helps users identify the unit-cell lattice parameters of a crystal structure that are consistent with a set of two-dimensional grazing-incidence wide-angle X-ray scattering data. The input data requirements are minimal and easy to assemble from data sets collected with any position-sensitive detector, and the user is required to make as few initial assumptions about the crystal structure as possible. By selecting manual or automatic modes of operation, the user can either visually match the positions of the experimental and calculated reflections by individually tuning the unit-cell parameters or have the program perform this process for them. Examples that demonstrate the utility of this program include determining the lattice parameters of a polymorph of a fluorinated contorted hexabenzocoronene in a blind test and refining the lattice parameters of the thin-film phase of 5,11-bis(triethylsilylethynyl)anthradithiophene with the unit-cell dimensions of its bulk crystal structure being the initial inputs.

  18. Crucial Role of the Double Bond Isomerism in the Steroid B-Ring on the Membrane Properties of Sterols. Grazing Incidence X-Ray Diffraction and Brewster Angle Microscopy Studies.

    PubMed

    Flasiński, Michał; Wydro, Paweł; Broniatowski, Marcin; Hąc-Wydro, Katarzyna; Fontaine, Philippe

    2015-07-01

    Three cholesterol precursors-desmosterol, zymosterol, and lanosterol-were comprehensively characterized in monolayers formed at the air/water interface. The studies were based on registration of the surface pressure (π)-area (A) isotherms complemented with in situ analysis performed with application of modern physicochemical techniques: grazing incidence X-ray diffraction (GIXD) and Brewster angle microscopy (BAM). In this approach we were interested in the correlation between molecular structures of the studied sterols found in the cholesterol biosynthetic pathway and their membrane properties. Our results revealed that only desmosterol behaves in Langmuir monolayers comparably to cholesterol, the molecules of which arrange in the monolayers into a hexagonal lattice, while the two remaining sterols possess extremely different properties. We found that molecules of both zymosterol and lanosterol are organized on the water surface in the two-dimensional oblique unit cells despite the fact that they are oriented perpendicular to the monolayer plane. The comparison of chemical structures of the investigated sterols leads to the conclusion that the only structural motive that can be responsible for such unusual behavior is the double bond in the B sterol ring, which is located in desmosterol in a different position from in the other two sterols. This issue, which was neglected in the scientific literature, seems to have crucial importance for sterol activity in biomembranes. We showed that this structural modification in sterol molecules is directly responsible for their adaptation to proper functioning in biomembranes.

  19. Size And Shape of Detergent Micelles Determined By Small-Angle X-Ray Scattering

    SciTech Connect

    Lipfert, Jan; Columbus, Linda; Chu, Vincent B.; Lesley, Scott A.; Doniach, Sebastian; /Stanford U., Phys. Dept. /Stanford U., Appl. Phys. Dept. /SLAC, SSRL /Pasteur Inst., Paris /Scripps Res. Inst. /Novartis Res. Found.

    2009-04-29

    We present a systematic analysis of the aggregation number and shape of micelles formed by nine detergents commonly used in the study of membrane proteins. Small-angle X-ray scattering measurements are reported for glucosides with 8 and 9 alkyl carbons (OG/NG), maltosides and phosphocholines with 10 and 12 alkyl carbons (DM/DDM and FC-10/FC-12), 1,2-dihexanoyl-sn-glycero-phosphocholine (DHPC), 1-palmitoyl-2-hydroxy-sn-glycero-3-[phospho-rac-(1-glycerol)] (LPPG), and 3-[(3-cholamidopropyl)dimethylammonio]-1-propane sulfonate (CHAPS). The SAXS intensities are well described by two-component ellipsoid models, with a dense outer shell corresponding to the detergent head groups and a less electron dense hydrophobic core. These models provide an intermediate resolution view of micelle size and shape. In addition, we show that Guinier analysis of the forward scattering intensity can be used to obtain an independent and model-free measurement of the micelle aggregation number and radius of gyration. This approach has the advantage of being easily generalizable to protein-detergent complexes, where simple geometric models are inapplicable. Furthermore, we have discovered that the position of the second maximum in the scattering intensity provides a direct measurement of the characteristic head group-head group spacing across the micelle core. Our results for the micellar aggregation numbers and dimensions agree favorably with literature values as far as they are available. We de novo determine the shape of FC-10, FC-12, DM, LPPG, and CHAPS micelles and the aggregation numbers of FC-10 and OG to be ca. 50 and 250, respectively. Combined, these data provide a comprehensive view of the determinants of micelle formation and serve as a starting point to correlate detergent properties with detergent-protein interactions.

  20. Research on ship wake detection by optical method of small angle forward scattering

    NASA Astrophysics Data System (ADS)

    Zhu, Donghua; Rao, Jionghui; Zhang, Xiaohui; Sun, ChunSheng

    2008-03-01

    A ship wake in the ocean contains lots of microsize air bubbles with diameter of 10μm~200μm. When a beam of light propagates through the ship wake, it leads to attenuation of the light energy and change of its spatial distribution due to absorption and scattering caused by ocean water and bubble mass together, but they don't share the same scattering mechanism, leaving absorption out of account. Scattering from micro bubbles can usually be explained by Mie scattering theory. In this paper, a method based on optical scattering theory is proposed for detecting the target of ship wake in the ocean, and an experimental system is built up according to the Lambert-Beer law. In the experiment, a semiconductor laser with wavelength about 532nm was employed as the light source, an experimental device which modeled the target of a ship wake to generate bubble mass in water, and a high-speed PIN photodiode as the detector. Besides, the optical receiving system included a set of optical lens and apertures, which were employed to limit the field of view(FOV) of the receiver detector. After measurement of the small angle forward scattering rays scattered from bubble mass with a small FOV, the target signals was got and processed. Then adjustments were made to the optical receiving system and experiments were implemented with varying the FOV to find out the influence of FOV on target signal SNR and obtain the optimum FOV. The results showed that adjusting the FOV according to different microbubble size density could improve SNR.

  1. Structural characterization of a polymer substituted fullerene (flagellene) by small angle neutron scattering

    SciTech Connect

    Affholter, K.A.; Bunick, G.J.; Wignall, G.D.; Desimone, J.M.; Hunt, M.O. Jr.; Menceloglu, Y.Z.; Samulski, E.T.

    1994-12-31

    Small-angle neutron scattering (SANS) can structurally characterize fullerenes in solvents with strong SANS contrast (e.g. CS{sub 2}). Deuterated solvents (e.g. toluene-d{sub 8}) have a high scattering length density (SLD), which is close to that of C{sub 60} and C{sub 70} moieties. Hence, there is virtually no SANS contrast with the solvent and these particles are practically ``invisible`` in such media. On the other hand, the negative scattering length of hydrogen means that the SLD of H{sup 1}-containing materials is much lower, so they have strong contrast with toluene-d{sub 8}. Thus, SANS makes it possible to study the size and shapes of modified buckyballs such as the polymer-substituted fullerenes, or flagellenes. These consist of C{sub 60} cores to which 1-4 polystryene chains (with a molecular weight, MW {approx_equal} 2000) are attached. The extrapolated cross section at zero angle of scatter [d{Sigma}/d{Omega}(0)] is a function of the number of pendant chains, so SANS can be used to assess the number of ``arms`` which are covalently attached to the fullerene ``sphere.`` Close agreement ({plus_minus}4%) between measured and calculated values of d{Sigma}/d{Omega}(0) along with independent estimates of the radius of gyration (R{sub g}) and second virial coefficient (A{sub 2}) for a calibration linear polystyrene sample serves as a cross check on the validity of this methodology.

  2. SCT: a suite of programs for comparing atomistic models with small-angle scattering data

    PubMed Central

    Wright, David W.; Perkins, Stephen J.

    2015-01-01

    Small-angle X-ray and neutron scattering techniques characterize proteins in solution and complement high-resolution structural studies. They are of particular utility when large proteins cannot be crystallized or when the structure is altered by solution conditions. Atomistic models of the averaged structure can be generated through constrained modelling, a technique in which known domain or subunit structures are combined with linker models to produce candidate global conformations. By randomizing the configuration adopted by the different elements of the model, thousands of candidate structures are produced. Next, theoretical scattering curves are generated for each model for trial-and-error fits to the experimental data. From these, a small family of best-fit models is identified. In order to facilitate both the computation of theoretical scattering curves from atomistic models and their comparison with experiment, the SCT suite of tools was developed. SCT also includes programs that provide sequence-based estimates of protein volume (either incorporating hydration or not) and add a hydration layer to models for X-ray scattering modelling. The original SCT software, written in Fortran, resulted in the first atomistic scattering structures to be deposited in the Protein Data Bank, and 77 structures for antibodies, complement proteins and anionic oligosaccharides were determined between 1998 and 2014. For the first time, this software is publicly available, alongside an easier-to-use reimplementation of the same algorithms in Python. Both versions of SCT have been released as open-source software under the Apache 2 license and are available for download from https://github.com/dww100/sct. PMID:26089768

  3. Nano-Scale Morphology of Melanosomes Revealed by Small-Angle X-Ray Scattering

    PubMed Central

    Gorniak, Thomas; Haraszti, Tamas; Garamus, Vasyl M.; Buck, Andreas R.; Senkbeil, Tobias; Priebe, Marius; Hedberg-Buenz, Adam; Koehn, Demelza; Salditt, Tim; Grunze, Michael; Anderson, Michael G.; Rosenhahn, Axel

    2014-01-01

    Melanosomes are highly specialized organelles that produce and store the pigment melanin, thereby fulfilling essential functions within their host organism. Besides having obvious cosmetic consequences – determining the color of skin, hair and the iris – they contribute to photochemical protection from ultraviolet radiation, as well as to vision (by defining how much light enters the eye). Though melanosomes can be beneficial for health, abnormalities in their structure can lead to adverse effects. Knowledge of their ultrastructure will be crucial to gaining insight into the mechanisms that ultimately lead to melanosome-related diseases. However, due to their small size and electron-dense content, physiologically intact melanosomes are recalcitrant to study by common imaging techniques such as light and transmission electron microscopy. In contrast, X-ray-based methodologies offer both high spatial resolution and powerful penetrating capabilities, and thus are well suited to study the ultrastructure of electron-dense organelles in their natural, hydrated form. Here, we report on the application of small-angle X-ray scattering – a method effective in determining the three-dimensional structures of biomolecules – to whole, hydrated murine melanosomes. The use of complementary information from the scattering signal of a large ensemble of suspended organelles and from single, vitrified specimens revealed a melanosomal sub-structure whose surface and bulk properties differ in two commonly used inbred strains of laboratory mice. Whereas melanosomes in C57BL/6J mice have a well-defined surface and are densely packed with 40-nm units, their counterparts in DBA/2J mice feature a rough surface, are more granular and consist of 60-nm building blocks. The fact that these strains have different coat colors and distinct susceptibilities to pigment-related eye disease suggest that these differences in size and packing are of biological significance. PMID:24621581

  4. Structure and properties of aqueous methylcellulose gels by small-angle neutron scattering.

    PubMed

    Chatterjee, Tirtha; Nakatani, Alan I; Adden, Roland; Brackhagen, Meinolf; Redwine, David; Shen, Hongwei; Li, Yongfu; Wilson, Tricia; Sammler, Robert L

    2012-10-01

    Cold, semidilute, aqueous solutions of methylcellulose (MC) are known to undergo thermoreversible gelation when warmed. This study focuses on two MC materials with much different gelation performance (gel temperature and hot gel modulus) even though they have similar metrics of their coarse-grained chemical structure (degree-of-methylether substitution and molecular weight distribution). Small-angle neutron scattering (SANS) experiments were conducted to probe the structure of the aqueous MC materials at pre- and postgel temperatures. One material (MC1, higher gel temperature) exhibited a single almost temperature-insensitive gel characteristic length scale (ζ(c) = 1090 ± 50 Å) at postgelation temperatures. This length scale is thought to be the gel blob size between network junctions. It also coincides with the length scale between entanglement sites measured with rheology studies at pregel temperatures. The other material (MC2, lower gel temperature) exhibited two distinct length scales at all temperatures. The larger length scale decreased as temperature increased. Its value (ζ(c1) = 1046 ± 19 Å) at the lowest pregel temperature was indistinguishable from that measured for MC1, and reached a limiting value (ζ(c1) = 450 ± 19 Å) at high temperature. The smaller length scale (ζ(c2) = 120 to 240 Å) increased slightly as temperature increased, but remained on the order of the chain persistence length (130 Å) measured at pregel temperatures. The smaller blob size (ζ(c1)) of MC2 suggests a higher bond energy or a stiffer connectivity between network junctions. Moreover, the number density of these blobs, at the same reduced temperature with respect to the gel temperature, is orders of magnitude higher for the MC2 gels. Presumably, the smaller gel length scale and higher number density lead to higher hot gel modulus for the low gel temperature material.

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

    NASA Astrophysics Data System (ADS)

    Lambard, Jacques; Lesieur, Pierre; Zemb, Thomas

    1992-06-01

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

  6. Parameterization of structures in HE composites using surrogate materials: A small angle neutron scattering investigation

    SciTech Connect

    Mang, J.T.; Hjelm, R.P.; Skidmore, C.B.; Howe, P.M.

    1996-07-01

    High explosive materials used in the nuclear stockpile are composites of crystalline high explosives (HE) with binder materials, such as Estane. In such materials, there are naturally occurring density fluctuations (defects) due to cracks, internal (in the HE) and external (in the binder) voids and other artifacts of preparation. Changes in such defects due to material aging can affect the response of explosives due to shock, impact and thermal loading. Modeling efforts are attempting to provide quantitative descriptions of explosive response from the lowest ignition thresholds to the development of full blown detonations and explosions, however, adequate descriptions of these processes require accurate measurements of a number of structural parameters of the HE composite. Since different defects are believed to affect explosive sensitivity in different ways it is necessary to quantitatively differentiate between defect types. The authors report here preliminary results of SANS measurements on surrogates for HE materials. The objective of these measurements was to develop methodologies using SANS techniques to parameterize internal void size distributions in a surrogate material, sugar, to simulate an HE used in the stockpile, HMX. Sugar is a natural choice as a surrogate material, as it has the same crystal structure, has similar intragranular voids and has similar mechanical properties as HMX. It is used extensively as a mock material for explosives. Samples were used with two void size distributions: one with a sufficiently small mean particle size that only small occluded voids are present in significant concentrations, and one where the void sizes could be larger. By using methods in small-angle neutron scattering, they were able to isolate the scattering arising from particle-liquid interfaces and internal voids.

  7. Metastable ripple phase of fully hydrated dipalmitoylphosphatidylcholine as studied by small angle x-ray scattering

    PubMed Central

    Yao, Haruhiko; Matuoka, Sinzi; Tenchov, Boris; Hatta, Ichiro

    1991-01-01

    Fully hydrated dipalmitoylphosphatidylcholine (DPPC) undergoes liquid crystalline to metastable Pβ, phase transition in cooling. A small angle x-ray scattering study has been performed for obtaining further evidence about the structure of this phase. From a high-resolution observation of x-ray diffraction profiles, a distinct multipeak pattern has become obvious. Among them the (01) reflection in the secondary ripple structure is identified clearly. There are peaks assigned straightforwardly to (10) and (20) reflections in the primary ripple structure and peaks assigned to (10) and (20) reflections in the secondary ripple structure. Therefore the multipeak pattern is due to superposition of the reflections cause by the primary and secondary ripple structures. The lattice parameters are estimated as follows: for the primary ripple structure a = 7.09 nm, b = 13.64 nm, and γ = 95°, and for the secondary ripple structure a = 8.2 nm, b = 26.6 nm, and γ = 90°. The lattice parameters thus obtained for the secondary ripple structure are not conclusive, however. The hydrocarbon chains in the primary ripple structure have been reported as being tilted against the bilayer plane and, on the other hand, the hydrocarbon chains in the secondary ripple structure are likely to be perpendicular to the bilayer plane. This fact seems to be related to a sequential mechanism of phase transitions. On heating from the Lβ, phase where the hydrocarbon chains are tilted the primary ripple structure having tilted hydrocarbon chains takes place and on cooling from the Lα phase where the hydrocarbon chains are not tilted the secondary ripple structure with untilted chains tends to be stabilized. It appears that the truly metastable ripple phase is expressed by the second ripple structure although in the course of the actual cooling transition both the secondary and primary ripple structures form and coexist. PMID:19431787

  8. Characterization of Sol-gel Encapsulated Proteins using Small-angle Neutron Scattering

    SciTech Connect

    Luo, Guangming; Zhang, Qiu; Del Castillo, Alexis Rae; Urban, Volker S; O'Neill, Hugh Michael

    2009-01-01

    Entrapment of biomolecules in silica-derived sol-gels has grown into a vibrant area of research since it was originally demonstrated. However, accessing the consequences of entrapment on biomolecules and the gel structure remains a major challenge in characterizing these biohybrid materials. We present the first demonstration that it is possible with small-angle neutron scattering (SANS) to study the conformation of dilute proteins that are entrapped in transparent and dense sol-gels. Using deuterium-labeled green fluorescent protein (GFP) and SANS with contrast variation, we demonstrate that the scattering signatures of the sol-gel and the protein can be separated. Analysis of the scattering curves of the sol-gels using a mass-fractal model shows that the size of the colloidal silica particles and the fractal dimensions of the gels were similar in the absence and presence of protein, demonstrating that GFP did not influence the reaction pathway for the formation of the gel. The major structural difference in the gels was that the pore size was increased 2-fold in the presence of the protein. At the contrast match point for silica, the scattering signal from GFP inside the gel became distinguishable over a wide q range. Simulated scattering curves representing a monomer, end-to-end dimer, and parallel dimer of the protein were calculated and compared to the experimental data. Our results show that the most likely structure of GFP is that of an end-to-end dimer. This approach can be readily applied and holds great potential for the structural characterization of complex biohybrid and other materials.

  9. Small Angle Neutron-Scattering Studies of the Core Structure of Intact Neurosecretory Vesicles.

    NASA Astrophysics Data System (ADS)

    Krueger, Susan Takacs

    Small angle neutron scattering (SANS) was used to study the state of the dense cores within intact neurosecretory vesicles. These vesicles transport the neurophysin proteins, along with their associated hormones, oxytocin or vasopressin, from the posterior pituitary gland to the bloodstream, where the entire vesicle contents are released. Knowledge of the vesicle core structure is important in developing an understanding of this release mechanism. Since the core constituents exist in a dense state at concentrations which cannot be reproduced (in solution) in the laboratory, a new method was developed to determine the core structure from SANS experiments performed on intact neurosecretory vesicles. These studies were complemented by biochemical assays performed to determine the role, if any, played by phospholipids in the interactions between the core constituents. H_2O/D_2 O ratio in the solvent can be adjusted, using the method of contrast variation, such that the scattering due to the vesicle membranes is minimized, thus emphasizing the scattering originating from the cores. The applicability of this method for examining the interior of biological vesicles was tested by performing an initial study on human red blood cells, which are similar in structure to other biological vesicles. Changes in intermolecular hemoglobin interactions, occurring when the ionic strength of the solvent was varied or when the cells were deoxygenated, were examined. The results agreed with those expected for dense protein solutions, indicating that the method developed was suitable for the study of hemoglobin within the cells. Similar SANS studies were then performed on intact neurosecretory vesicles. The experimental results were inconsistent with model calculations which assumed that the cores consisted of small, densely-packed particles or large, globular aggregates. Although a unique model could not be determined, the data suggest that the core constituents form long aggregates of

  10. Recent improvements in small angle x-ray diffraction for the study of muscle physiology

    NASA Astrophysics Data System (ADS)

    Reconditi, Massimo

    2006-10-01

    The molecular mechanism of muscle contraction is one of the most important unresolved problems in biology and biophysics. Notwithstanding the great advances of recent years, it is not yet known in detail how the molecular motor in muscle, the class II myosin, converts the free energy of ATP hydrolysis into work by interacting with its track, the actin filament; neither is it understood how the high efficiency in energy conversion depends on the cooperative action of myosin motors working in parallel along the actin filament. Research in muscle contraction involves the combination of mechanical, biochemical and structural methods in studies that span from tissue to single molecule. Therefore, more than for any other research field, progress in the comprehension of muscle contraction at the molecular level is related to, and in turn contributes to, the advancement of methods in biophysics. This review will focus on the progress achieved by time-resolved small angle x-ray scattering (SAXS) from muscle, an approach made possible by the highly ordered arrangement of both the contractile proteins myosin and actin in the ca 2 µm long structural unit, the sarcomere, that repeats along the whole length of the muscle cell. Among time-resolved structural techniques, SAXS has proved to be the most powerful method of investigation, as it allows the molecular motor to be studied in situ, in intact single muscle cells, where it is possible to combine the structural study with fast mechanical methods that synchronize the action of the molecular motors. The latest development of this technique allows Angstrom-scale measurements of the axial movement of the motors that pull the actin filament towards the centre of the sarcomere, by exploiting the x-ray interference between the two arrays of myosin motors in the two halves of the sarcomere.

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

    PubMed

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

    2008-10-21

    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. PMID:18812651

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

    NASA Astrophysics Data System (ADS)

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

    2008-10-01

    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.

  13. Small-Angle X-ray Study of the Three-Dimensional Collagen/Mineral Superstructure in Intramuscular Fish Bone

    SciTech Connect

    Zhou,H.; Burger, C.; Sics, I.; Hsiao, B.; Chu, B.; Graham, L.; Glimcher, M.

    2007-01-01

    Synchrotron small-angle X-ray scattering (SAXS) was conducted on native intramuscular shad/herring bone samples. Two-dimensional SAXS patterns were quantitatively analyzed with special consideration for preferred orientation effects, leading to new insights into the three-dimensional superstructure of mineralized collagen fibrils in shad/herring bone.

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

    SciTech Connect

    Chen, Lingling

    1996-04-01

    Synchrotron small angle x-ray scattering (SAXS) has been applied to the structural study of several biological systems, including the nitrogenase complex, the heat shock cognate protein (hsc70), and lysozyme folding. The structural information revealed from the SAXS experiments is complementary to information obtained by other physical and biochemical methods, and adds to our knowledge and understanding of these systems.

  15. Ultra small angle x-ray scattering in complex mixtures of triacylglycerols

    NASA Astrophysics Data System (ADS)

    Peyronel, Fernanda; Quinn, Bonnie; Marangoni, Alejandro G.; Pink, David A.

    2014-11-01

    Ultra-small angle x-ray scattering (USAXS) has been used to elucidate, in situ, the aggregation structure of unsheared model edible oils. Each system comprised one or two solid lipids and a combination of liquid lipids. The 3D nano- to micro-structures of each system were characterized. The length scale investigated, using the Bonse-Hart camera at beamline ID-15D at the Advanced Photon Source, ANL, ranged from 300 Å-10 µm. Using the Unified Fit model, level-1 analysis showed that the scatterers were 2D objects with either a smooth, a rough, or a diffuse surface. These 2D objects had an average radius of gyration Rg1 between 200-1500 Å. Level-2 analysis displayed a slope between -1 and -2. Use of the Guinier-Porod model gave s ≈ 1 thus showing that it was cylinders (TAGwoods) aggregating with fractal dimension 1 ≤ D2 ≤ 2. D2 = 1 is consistent with 1D structures formed from TAGwoods, while D2 = 2 implies that the TAGwoods had formed structures characteristic of diffusion or reaction limited cluster-cluster aggregation (DLCA/RLCA). These aggregates exhibited radii of gyration, Rg2, between 2500 and 6500 Å. Level-3 analyses showed diffuse surfaces, for most of the systems. These interpretations are in accord with theoretical models which studied crystalline nano-platelets (CNPs) coated with nano-scale layers arising from phase separation at the CNP surfaces. These layers could be due to either liquid-liquid phase separation with the CNPs coated, uniformly or non-uniformly, by a diffuse layer of TAGs, or solid-liquid phase separation with the CNPs coated by a rough layer of crystallites. A fundamental understanding of the self-organizing structures arising in these systems helps advance the characterization of fat crystal networks from nanometres to micrometres. This research can be used to design novel fat structures that use healthier fats via nano- and meso-scale structural engineering.

  16. Anomalous small angle x-ray scattering studies of amorphous metal-germanium alloys

    SciTech Connect

    Rice, M.

    1993-12-01

    This dissertation addresses the issue of composition modulation in sputtered amorphous metal-germanium thin films with the aim of understanding the intermediate range structure of these films as a function of composition. The investigative tool used in this work is anomalous small-angle X-ray scattering (ASAXS). The primary focus of this investigation is the amorphous iron-germanium (a-Fe{sub x}Ge{sub 100-x}) system with particular emphasis on the semiconductor-rich regime. Brief excursions are made into the amorphous tungsten-germanium (a-W{sub x}Ge{sub 100-x}) and the amorphous molybdenum-germanium (a-Mo{sub x}Ge{sub 100-x}) systems. All three systems exhibit an amorphous structure over a broad composition range extending from pure amorphous germanium to approximately 70 atomic percent metal when prepared as sputtered films. Across this composition range the structures change from the open, covalently bonded, tetrahedral network of pure a-Ge to densely packed metals. The structural changes are accompanied by a semiconductor-metal transition in all three systems as well as a ferromagnetic transition in the a-Fe{sub x}Ge{sub 100-x} system and a superconducting transition in the a-Mo{sub x}Ge{sub 100-x} system. A long standing question, particularly in the a-Fe{sub x}Ge{sub 100-x} and the a-Mo{sub x}Ge{sub 100-x} systems, has been whether the structural changes (and therefore the accompanying electrical and magnetic transitions) are accomplished by homogeneous alloy formation or phase separation. The application of ASAXS to this problem proves unambiguously that fine scale composition modulations, as distinct from the simple density fluctuations that arise from cracks and voids, are present in the a-Fe{sub x}Ge{sub 100-x}, a-W{sub x}Ge{sub 100-x}, and a-Mo{sub x}Ge{sub 100-x} systems in the semiconductor-metal transition region. Furthermore, ASAXS shows that germanium is distributed uniformly throughout each sample in the x<25 regime of all three systems.

  17. Structural behaviour of mixed cationic surfactant micelles: a small-angle neutron scattering study.

    PubMed

    Bergström, L Magnus; Garamus, Vasil M

    2012-09-01

    Self-assembly in mixtures of two single-chain cationic surfactants, with different tail lengths (CTAB and DTAB) as well as of a single-chain (DTAB) and a double-chain (DDAB) cationic surfactant, with identical tail lengths, have been investigated with small-angle neutron scattering (SANS) and rationalised in terms of bending elasticity properties. The growth behaviour of micelles with respect to surfactant composition appears completely different in the two surfactant mixtures. DTAB form small oblate spheroidal micelles in presence of [NaBr]=0.1 M that transform into prolate spheroidal mixed CTAB/DTAB micelles upon adding moderate amounts of CTAB, so as to give a mole fraction y=0.20 in solution. Most unexpectedly, upon further addition of CTAB the mixed CTAB/DTAB micelles grow with an almost equal rate in both length and width directions to form tablets. In contrast to this behaviour, mixed DDAB/DTAB micelles grow virtually exclusively in the length direction, in presence of [NaBr]=0.1 M, to form elongated ellipsoidal (tablet-shaped) and subsequently long wormlike micelles as the fraction of DDAB in the micelles increases. Mixed DDAB/DTAB micelles grow to become as long as 2000Å before an abrupt transition to large bilayer structures occurs. This means that the micelles are much longer at the micelle-to-bilayer transition as compared to the same mixture in absence of added salt. It is found that the point of transition from micelles to bilayers is significantly shifted towards higher fractions of aggregated DTAB as an appreciable amount of salt is added to DDAB/DTAB mixtures, indicating a considerable reduction of the spontaneous curvature with an increasing [NaBr]. By means of deducing the various bending elasticity constants from our experimental results, according to a novel approach by ours, we are able to conclude that the different growth behaviours appear as a consequence of a considerably lower bending rigidity, as well as higher saddle-splay constant

  18. Initial characterization of mudstone nanoporosity with small angle neutron scattering using caprocks from carbon sequestration sites.

    SciTech Connect

    McCray, John; Navarre-Sitchler, Alexis; Mouzakis, Katherine; Heath, Jason E.; Dewers, Thomas A.; Rother, Gernot

    2010-11-01

    Geological carbon sequestration relies on the principle that CO{sub 2} injected deep into the subsurface is unable to leak to the atmosphere. Structural trapping by a relatively impermeable caprock (often mudstone such as a shale) is the main trapping mechanism that is currently relied on for the first hundreds of years. Many of the pores of the caprock are of micrometer to nanometer scale. However, the distribution, geometry and volume of porosity at these scales are poorly characterized. Differences in pore shape and size can cause variation in capillary properties and fluid transport resulting in fluid pathways with different capillary entry pressures in the same sample. Prediction of pore network properties for distinct geologic environments would result in significant advancement in our ability to model subsurface fluid flow. Specifically, prediction of fluid flow through caprocks of geologic CO{sub 2} sequestration reservoirs is a critical step in evaluating the risk of leakage to overlying aquifers. The micro- and nanoporosity was analyzed in four mudstones using small angle neutron scattering (SANS). These mudstones are caprocks of formations that are currently under study or being used for carbon sequestration projects and include the Marine Tuscaloosa Group, the Lower Tuscaloosa Group, the upper and lower shale members of the Kirtland Formation, and the Pennsylvanian Gothic shale. Total organic carbon varies from <0.3% to 4% by weight. Expandable clay contents range from 10% to {approx}40% in the Gothic shale and Kirtland Formation, respectively. Neutrons effectively scatter from interfaces between materials with differing scattering length density (i.e. minerals and pores). The intensity of scattered neutrons, I(Q), where Q is the scattering vector, gives information about the volume of pores and their arrangement in the sample. The slope of the scattering data when plotted as log I(Q) vs. log Q provides information about the fractality or geometry of

  19. Molecular dynamics simulation analysis of small-angle neutron scattering by a solution of stearic acid in benzene

    NASA Astrophysics Data System (ADS)

    Eremin, R. A.; Kholmurodov, Kh. T.; Petrenko, V. I.; Rosta, L.; Avdeev, M. V.

    2014-01-01

    Data of small-angle neutron scattering by a diluted solution of stearic acid in deuterated benzene have been analyzed using the results of molecular dynamics simulation. The molecular dynamics simulation approach has been used to calculate the time-averaged distribution of the neutron scattering length density at the interface between the acid molecule and the solvent. It has been shown that the organization of the solvent at the interface with the acid molecule leads to a modulation of the neutron scattering length density and makes a significant contribution to the scattering. This contribution should be taken into account when interpreting the experimental small-angle neutron scattering curves for both the considered system and its analogues.

  20. Origin of recombination activity at small angle grain boundaries in multicrystalline silicon using multi-seed casting growth method

    NASA Astrophysics Data System (ADS)

    Kojima, Takuto; Tachibana, Tomihisa; Ohshita, Yoshio; Prakash, Ronit R.; Sekiguchi, Takashi; Yamaguchi, Masafumi

    2015-08-01

    The effect of misorientation on the recombination activity of tilt small angle grain boundaries was studied by temperature-dependent electron beam induced current (EBIC) analyses of artificially induced grain boundaries in multicrystal grown by casting from multiple seeds. For small misorientation, there is no significant difference in the recombination of grain boundaries at the middle of a grown ingot, whereas moderate contamination on grain boundaries caused changes in the EBIC contrast, especially at room temperature. The EBIC contrast of moderately contaminated grain boundaries at room temperature has a peak at a misorientation of ∼3°, and for misorientation θ > 6°, the recombinative nature diminishes with increasing misorientation. The results indicate differences in the gettering ability of small angle grain boundaries.

  1. Small-Angle X-ray Scattering Study of Intramuscular Fish Bone: Collagen Fibril Superstructure Determined from Equidistant Meridional Reflections

    SciTech Connect

    Burger,C.; Zhou, H.; Sics, I.; Hsiao, B.; Chu, B.; Graham, L.; Glimcher, M.

    2008-01-01

    New insights into the bone collagen fibril superstructure have been obtained by novel small-angle X-ray scattering analysis. The analysis was carried out on the small-angle equidistant meridional reflections resulting from the periodic structure of collagen fibrils in their axial direction. Conventional two-dimensional analysis is difficult because of the large discrepancy of longitudinal and lateral length scales for individual fibrils, as well as their preferred orientation. The new approach represents an unapproximated analysis of the equidistant meridional reflections, which takes the exact separation of preferred orientation and fibril size effects into account. The analytical results (e.g. axial period, fibril diameter etc.) agree well with the parameters obtained from transmission electron microscopy.

  2. Relationship Between the Atomic Pair Distribution Function and Small-Angle Scattering: Implications for Modeling of Nanoparticles

    SciTech Connect

    Billinge, S.; Farrowa, C.L.

    2009-05-01

    The relationship between the equations used in the atomic pair distribution function (PDF) method and those commonly used in small-angle-scattering (SAS) analyses is explicitly shown. The origin of the sloping baseline, -4{pi}r{rho}{sub 0}, in PDFs of bulk materials is identified as originating from the SAS intensity that is neglected in PDF measurements. The nonlinear baseline in nanoparticles has the same origin, and contains information about the shape and size of the nanoparticles.

  3. Measurement of energy spectra of small-angle scattering and distribution of optical microinhomogeneities in laser ceramics

    SciTech Connect

    Tverdokhleb, P E; Shepetkin, Yu A; Steinberg, I Sh; Belikov, A Yu; Vatnik, S M; Vedin, I A; Kurbatov, P F

    2014-06-30

    The energy spectra of small-angle light scattering from the samples of Nd:YAG ceramics and the spatial distributions of optical microinhomogeneities in them are measured. The spatial profiles of microinhomogeneities are found using the collinear heterodyne microprobe technique. Based on the obtained data, the comparison of noise and lasing characteristics of foreign and domestic samples of laser ceramics is carried out. (extreme light fields and their applications)

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

    NASA Astrophysics Data System (ADS)

    Jääskeläinen, Pentti; Engelhardt, Peter; Hynönen, Ulla; Torkkeli, Mika; Palva, Airi; Serimaa, Ritva

    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 Å and 435 Å.

  5. The method of characteristics for the determination of supersonic flow over bodies of revolution at small angles of attack

    NASA Technical Reports Server (NTRS)

    Ferri, Antonio

    1951-01-01

    The method of characteristics has been applied for the determination of the supersonic-flow properties around bodies of revolution at a small angle of attack. The system developed considers the effect of the variation of entropy due to the curved shock and determines a flow that exactly satisfies the boundary conditions in the limits of the simplifications assumed. Two practical methods for numerical calculations are given. (author)

  6. Jointed magnetic skyrmion lattices at a small-angle grain boundary directly visualized by advanced electron microscopy

    PubMed Central

    Matsumoto, Takao; So, Yeong-Gi; Kohno, Yuji; Sawada, Hidetaka; Ishikawa, Ryo; Ikuhara, Yuichi; Shibata, Naoya

    2016-01-01

    The interactions between magnetic skyrmions and structural defects, such as edges, dislocations, and grain boundaries (GBs), which are all considered as topological defects, will be important issues when magnetic skyrmions are utilized for future memory device applications. To investigate such interactions, simultaneous visualization of magnetic skyrmions and structural defects at high spatial resolution, which is not feasible by conventional techniques, is essential. Here, taking advantages of aberration-corrected differential phase-contrast scanning transmission electron microscopy, we investigate the interaction of magnetic skyrmions with a small-angle GB in a thin film of FeGe1−xSix. We found that the magnetic skyrmions and the small-angle GB can coexist each other, but a domain boundary (DB) was formed in the skyrmion lattice along the small-angle GB. At the core of the DB, unexpectedly deformed magnetic skrymions, which appear to be created by joining two portions of magnetic skyrmions in the adjacent lattices, were formed to effectively compensate misorientations between the two adjacent magnetic skyrmion lattices. These observations strongly suggest the flexible nature of individual magnetic skyrmions, and also the significance of defect engineering for future device applications. PMID:27775056

  7. From nuclei to micro-structure in colloidal crystallization: Investigating intermediate length scales by small angle laser light scattering

    NASA Astrophysics Data System (ADS)

    Beyer, Richard; Franke, Markus; Schöpe, Hans Joachim; Bartsch, Eckhard; Palberg, Thomas

    2015-08-01

    Hard sphere suspensions are well recognized model systems of statistical physics and soft condensed matter. We here investigate the temporal evolution of the immediate environment of nucleating and growing crystals and/or their global scale distribution using time resolved Small Angle Light Scattering (SALS). Simultaneously performed Bragg scattering measurements provide an accurate temporal gauging of the sequence of events. We apply this approach to studies of re-crystallization in several different shear molten hard sphere and attractive hard sphere samples with the focus being on the diversity of observable signal shapes and their change in time. We demonstrate that depending on the preparation conditions different processes occur on length scales larger than the structural scale, which significantly influence both the crystallization kinetics and the final micro-structure. By careful analysis of the SALS signal evolution and by comparing different suggestions for small angle signal shapes to our data, we can for most cases identify the processes leading to the observed signals. These include form factor scattering from crystals surrounded by depletion zones and structure factor scattering from late stage inter-crystallite ordering. The large variety of different small angle signals thus in principle contains valuable information complementary to that gained from Bragg scattering or microscopy. Our comparison, however, also shows that further refinement and adaptation of the theoretical expressions to the sample specific boundary conditions is desired for a quantitative kinetic analysis of micro-structural evolution.

  8. Investigation of the structure of unilamellar dimyristoylphosphatidylcholine vesicles in aqueous sucrose solutions by small-angle neutron and X-ray scattering

    SciTech Connect

    Kiselev, M. A. Zemlyanaya, E. V.; Zhabitskaya, E. I.; Aksenov, V. L.

    2015-01-15

    The structure of a polydispersed population of unilamellar dimyristoylphosphatidylcholine (DMPC) vesicles in sucrose solutions has been investigated by small-angle neutron scattering (SANS) and small-angle X-ray scattering (SAXS). Calculations within the model of separated form factors (SFF) show that the structure of the vesicle system depends strongly on the sucrose concentration.

  9. EDITORIAL Proceedings of the XIV International Conference on Small-Angle Scattering, SAS-2009

    NASA Astrophysics Data System (ADS)

    Ungar, Goran; Heenan, Richard

    2010-10-01

    There are 52 papers in these Proceedings. The papers are divided into 10 thematic sections and a section for invited papers and reviews. The sections and the respective section editors are given below. Section Editor(s) Invited Papers and Reviews Peter Griffiths, Wim Bras, Rudolf Winter Beamlines and Instrumentation Elliot Gilbert, Wim Bras, Nigel Rhodes Theory, Data processing and Modelling Jan Skov Pedersen, Carlo Knupp Biological Systems and Membranes Richard Heenan, Cameron Neylon Ceramics, Glasses and Porous Materials Rudolf Winter Colloids and Solutions Peter Griffiths Hierarchical Structures and Fibres Steve Eichhorn, Karen Edler Metallic and Magnetic Systems Armin Hoell Polymers Patrick Fairclough Time resolved Diffraction, Kinetic and Dynamical Studies João Cabral, Christoph Rau We are grateful to all section editors and the many anonymous referees for their invaluable effort which made the publication of the Proceedings possible. The refereeing process was strict and thorough, some papers were rejected and most were improved. The resulting compendium gives a good overview of recent developments in small-angle X-ray and neutron scattering theory, application, methods of analysis and instrumentation. Thus it should be a useful source of reference for a number of years to come. The papers are a good reflection of the material presented at the meeting. Because of the general high quality of the articles, it was difficult to decide which to highlight and be fair to all contributors. The following in particular have caught the attention of the editors. Highlighted papers A statistical survey of publications reporting the application of SAXS and SANS by Aldo Craievich (paper 012003) is recommended reading for anyone needing convincing about the vibrancy of this scientific field and the ever expanding use of these techniques. Two aspects of coherent X-ray scattering, made available by the advent of the 3rd generation synchrotron sources, are discussed in the

  10. MONITORING GRAZING LANDS

    Technology Transfer Automated Retrieval System (TEKTRAN)

    An important step in developing a ranch or allotment management plan for grazing lands is defining a rangeland monitoring program to evaluate progress toward achieving management objectives. A monitoring program can: 1) help determine the benefits gained from changes in grazing management or invest...

  11. On the structure of concentrated detonation nanodiamond hydrosols with a positive ζ potential: Analysis of small-angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Avdeev, Mikhail V.; Tomchuk, Oleksandr V.; Ivankov, Oleksandr I.; Alexenskii, Alexander E.; Dideikin, Artur T.; Vul, Alexander Ya.

    2016-08-01

    Small-angle neutron scattering (SANS) was applied for the structure characterization of detonation nanodiamond (DND) aqueous suspensions with a positive ζ potential. The contrast variation technique (based on mixtures of light and heavy water) was used to study the structure of DND particles and their clusters in solutions. The results were compared with the data of the previous similar experiments for DND suspensions with a negative ζ potential. The experimental range of the neutron scattering contrast in the system was extended to maximally possible by starting with the initial concentrated suspensions separately prepared in light and heavy water.

  12. Small-angle neutron scattering study of recombinant yeast-derived human hepatitis B virus surface antigen vaccine particle

    NASA Astrophysics Data System (ADS)

    Sato, M.; Ito, Y.; Kameyama, K.; Imai, M.; Ishikawa, N.; Takagi, T.

    1995-02-01

    The overall and internal structure of recombinant yeast-derived human hepatitis B virus surface antigen vaccine particles was investigated by small-angle neutron scattering using the contrast variation method. The vaccine is a nearly spherical particle, and its contrast-matching point was determined to be at about 24% D 2O content, indicating that a large part of the vaccine particle is occupied by lipids and carbohydrates from the yeast. The Stuhrmann plot suggests that the surface antigens exist predominantly in the peripheral region of the particle, which is favorable to the induction of anti-virus antibodies.

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

    SciTech Connect

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

    2006-03-15

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

  14. Single-crystal CVD diamonds as small-angle X-ray scattering windows for high-pressure research

    PubMed Central

    Wang, Suntao; Meng, Yu-fei; Ando, Nozomi; Tate, Mark; Krasnicki, Szczesny; Yan, Chih-shiue; Liang, Qi; Lai, Joseph; Mao, Ho-kwang; Gruner, Sol M.; Hemley, Russell J.

    2012-01-01

    Small-angle X-ray scattering (SAXS) was performed on single-crystal chemical vapor deposition (CVD) diamonds with low nitrogen concentrations, which were fabricated by microwave plasma-assisted chemical vapor deposition at high growth rates. High optical quality undoped 500 µm-thick single-crystal CVD diamonds grown without intentional nitrogen addition proved to be excellent as windows on SAXS cells, yielding parasitic scattering no more intense than a 7.5 µm-thick Kapton film. A single-crystal CVD diamond window was successfully used in a high-pressure SAXS cell. PMID:22675230

  15. Structure of spontaneously formed solid-electrolyte interphase on lithiated graphite determined using small-angle neutron scattering

    DOE PAGES

    Sacci, Robert L.; Banuelos, Jose Leobardo; Veith, Gabriel M.; Littrell, Ken C.; Cheng, Yongqiang Q.; Wildgruber, Christoph U.; Jones, Lacy L.; Ramirez-Cuesta, Anibal J.; Rother, Gernot; Dudney, Nancy J.

    2015-03-25

    We report the first small-angle neutron scattering of a chemically formed solid-electrolyte interphase from LixC6 reacting with ethylene carbonate/dimethyl carbon solvent. This provides a different and perhaps simpler view of SEI formation than the usual electrochemically-driven reaction. We show that an organic layer coats the graphite particles filling in micro-pores and is polymeric in nature being 1-3 nm thick. We used inelastic neutron scattering to probe the chemistry, and we found that the SEI showed similar inelastic scattering to polyethylene oxide.

  16. Structure of the magnetite-oleic acid-decalin magnetic fluid from small-angle neutron scattering data

    NASA Astrophysics Data System (ADS)

    Nagornyi, A. V.; Petrenko, V. I.; Bulavin, L. A.; Avdeev, M. V.; Almásy, L.; Rosta, L.; Aksenov, V. L.

    2014-01-01

    Structural parameters of the magnetite-oleic acid-decalin magnetic fluid at various excesses of oleic acid (up to 25 vol %) have been determined using small-angle neutron scattering. Based on the comparison of the behavior of oleic acid in the magnetic fluid and in the pure solvent (decalin), it has been concluded that the interaction between the molecules of free (unadsorbed) surfactant changes in the presence of magnetic nanoparticles. However, the system remains stable and does not form aggregates of magnetic particles or free oleic acid. These results are compared with the previously presented data for similar benzene-based magnetic fluids.

  17. Small-angle neutron scattering studies of the template-mediated crystallization of ZSM-5 type zeolite

    SciTech Connect

    Iton, L.E.; Brun, T.O.; Epperson, J.E. . Materials Science and Technology Div.); Trouw, F. . Intense Pulsed Neutron Source Program); White, J.W.; Henderson, S.J. )

    1988-03-01

    Small-angle neutron scattering is a useful new approach to the study of zeolite crystallization from aluminosilicate gels and the action of template molecules. It has been applied to gels for synthesis of zeolite ZSM-5 using tetrapropylammonium ions as templates where the scattering length densities of the gel particles and their texture were determined using contrast variation methods. Gels formulated from soluble silicate incorporate template molecules promptly into an amorphous embryonic'' structure and crystallization ensues via a solid hydrogel transformation mechanism. Gels formulated from colloidal silica show different scattering behavior, and a liquid phase transport mechanism is inferred. 8 refs., 4 figs., 2 tabs.

  18. Limiting cases of the small-angle scattering approximation solutions for the propagation of laser beams in anisotropic scattering media

    NASA Technical Reports Server (NTRS)

    Box, M. A.; Deepak, A.

    1981-01-01

    The propagation of photons in a medium with strongly anisotropic scattering is a problem with a considerable history. Like the propagation of electrons in metal foils, it may be solved in the small-angle scattering approximation by the use of Fourier-transform techniques. In certain limiting cases, one may even obtain analytic expressions. This paper presents some of these results in a model-independent form and also illustrates them by the use of four different phase-function models. Sample calculations are provided for comparison purposes

  19. Quaternary structure of alpha-crustacyanin from lobster as seen by small-angle X-ray scattering.

    PubMed

    Dellisanti, Cosma D; Spinelli, Silvia; Cambillau, Christian; Findlay, John B C; Zagalsky, Peter F; Finet, Stéphanie; Receveur-Bréchot, Véronique

    2003-06-01

    The structure of alpha-crustacyanin, the blue carotenoprotein of lobster (Homarus gammarus) carapace, has been investigated for the first time using small-angle X-ray scattering. In this paper, we have determined the dimensions of this protein composed of eight heterodimeric subunits of beta-crustacyanin. Analysis of the scattering spectra and estimation of the shape of alpha-crustacyanin show that the protein fits into a cylinder with an axial length of 238 A and a radius of 47.5 A, in which the eight beta-crustacyanin molecules are probably arranged in a helical manner. PMID:12782314

  20. Determination of some structural and dispersion characteristics of Perftoran emulsions by the small-angle X-ray scattering

    NASA Astrophysics Data System (ADS)

    Aul'chenko, V. M.; Vazina, A. A.; Galimov, P. V.; Korneev, V. N.; Maevskii, E. I.; Matyushin, A. M.; Tuzikov, F. V.; Tuzikova, N. A.

    2005-05-01

    By the method of small-angle X-ray scattering, it is shown that preparation Perftoran—the blood substitute with the function of carrying oxygen—contains a huge amount of spherical micellar particles in an abundance, essentially of smaller sizes, than a particle of an emulsion of perfluorochemicals. The distribution function of the form and the size of micellar particles of preparation Perftoran is determined. The assumption, that a number of clinical properties of a preparation is caused by these particles is put forward.