Contribution of synchrotron radiation to small-angle X-ray scattering studies in hard condensed matter

Synchrotron radiation, by virtue of its special beam characteristics, has revived interest in small-angle X-ray scattering for hard condensed matter and materials science. New techniques have been developed and new scientific themes tackled, ranging from metallurgy to nanotechnology.

Small-angle scattering studies of macromolecular solutions

Advanced methods for the analysis of small-angle scattering data from solutions of biological macromolecules are reviewed.

Structure and dynamics of thin polymer films using synchrotron X-ray scattering

Synchrotron X-ray diffuse scattering and photon correlation spectroscopy in reflection geometry were used to measure the structure and dynamic properties at the surface, interface and in the interior of supported polymer films.

Contrast variation in X-ray and neutron scattering

Methods of contrast variation in X-ray and neutron scattering are reviewed.

Polymer dynamics: from synthetic polymers to proteins

Neutron spin echo spectroscopy reveals the two main reptation limiting processes: constraint release and contour length fluctuation on a molecular scale. The first direct observations of domain dynamics in biopolymers are presented.

Measurement of self-diffusion constant with two-dimensional X-ray photon correlation spectroscopy

Two-dimensional XPCS allows the dynamics of large wavectors in materials opaque to visible light to be probed. The self-diffusion constant of a colloidal dispersion is probed and compared with available models.

Homodyne and heterodyne X-ray photon correlation spectroscopy: latex particles and elastomers

Interferences are observed in coherent X-ray small-angle scattering between a static reference and a fluctuating sample. Heterodyning makes possible the observation of Doppler shifts with sample drift velocities in the nanometres per second range.

Complementary use of small-angle neutron scattering and dynamic light scattering studies for structure analysis and dynamics of polymer gels

Small-angle neutron scattering and dynamic light scattering have been complementarily employed in order to investigate the structure and dynamics of polymer gels. It is demonstrated that complementary use is necessary to explore the dynamics of polymer gels, particularly that of slide-ring gels in which cross-links can slide along the backbone polymer chain.

Probing the flow-induced shish-kebab structure in entangled polyethylene melts by synchrotron X-ray scattering

Flow-induced shish-kebab structure formation in ultrahigh-molecular-weight polyethylene (UHMWPE)/low-molecular-weight polyethylene blend melts was investigated by using synchrotron X-rays. The results confirmed that the formation of shish is due to the topological deformation of the UHMWPE entanglement network and the formation of shish can accelerate the kebab nucleation.

Behaviour of materials in magnetic fields studied by small-angle X-ray scattering

A short oversight of experiments where small-angle X-ray scattering was performed on samples which were kept in high magnetic fields is given. The samples are biological macromolecules, liquid crystals and crystalline materials.

Reordering of magnetic colloid structures in external magnetic fields

A polarized small-angle scattering experiment with a concentrated magnetic fluid is described confirming dipolar chains and domains of hexagonal arrangements.

Field-dependent relaxation behavior of Co-ferrofluid investigated with stroboscopic time-resolved small-angle neutron scattering

The decay of inter-particle order in Co-ferrofluid has been investigated for different inducing magnetic fields. Time constants have been calculated for the relaxation.

Effects of side-chain length on the magnetic response of discotic metallomesogens

The magnetic responses of columnar discotic metallomesogens, cobalt octa(n-alkylthio)porphyrazine with different side-chain lengths (CoSx, where x is the peripheral n-alkyl chain length, x = 10, 12, 14), have been investigated by small-angle neutron scattering. The magnetic field strength required for the alignment of the columnar phase increased with the side-chain length x.

A combined small-angle scattering study of a chemical reaction at specific sites and reaction-induced self-assembly as a problem in open non-equilibrium phenomena

As a problem in open non-equilibrium phenomena, small-angle scattering studies of a chemical reaction at specific sites and reaction-induced self-assembly of the system which is induced by mixing two stable solutions of palladium(II) acetate [Pd(OAc)₂] in N,N-dimethylformamide and the second-generation polyamidoamine dendrimer in methanol are presented.

Scanning X-ray imaging with small-angle scattering contrast

A scanning X-ray imaging technique using the integrated small-angle scattering (SAXS) intensity is presented. The origin of the SAXS contrast is discussed for three biological materials: bone, eggshell and hair.

Hierarchical bionanotubes formed by the self assembly of microtubules with cationic membranes or polypeptides

Synchrotron X-ray diffraction and electron microscopy data are presented for reconstituted protein systems from the bovine central nervous system, which reveal unexpected structures of hierarchical bionanotubes, not predicted by current electrostatic theories.

Simplified tube form factor for analysis of small-angle scattering data from carbon nanotube filled systems

A simplified tube (hollow cylinder) form factor is developed and utilized to analyze ultra-small-angle X-ray scattering data obtained from multi-walled carbon nanotube/bismaleimide composite samples. The form factor is useful for distinguishing between hollow and solid cylinders as well for detecting the presence of aggregation of one-dimensional colloidal fillers in polymers.

A visualized analysis of small-angle neutron scattering intensity: concentration fluctuation in alcohol–water mixtures

Visualized analysis of SANS from a tert-butyl alcohol–water mixture has revealed that the concentration fluctuation is characterized by polydisperse mass fractals.

Hierarchical structures formed by partially crystalline polymers in solution: from fundamentals to applications – a combined conventional, focusing and ultra-small-angle neutron scattering study

Multilevel aggregates with characteristic sizes covering four orders of magnitude, from 1 nm to 10 µm, formed upon cooling decane solutions of poly(ethylene-butene) random copolymers and wax-containing mixed solutions are investigated by combining three small-angle neutron scattering (SANS) techniques (conventional SANS, focusing SANS and ultra-SANS) with microscopy.

Hierarchical structure of niobate nanosheets in aqueous solution

The hierarchical structure of an aqueous dispersion of niobate nanosheets was investigated by (ultra-)small-angle scattering methods.

Creating local contrast in small-angle neutron scattering by dynamic nuclear polarization

Dynamic nuclear polarization and its application to small-angle neutron scattering are discussed.

Spin-echo small-angle neutron scattering study of the domain structure of an Ni layer on a Cu substrate

Spin-echo small-angle neutron scattering is used to study the magnetic domain structure of an Ni layer on a Cu substrate. The experiments demonstrate the possibilities of this novel technique.

Small-angle neutron scattering from extended defects in diamonds

It is shown that natural and synthetic diamonds contain planar and three-dimensional defects, observable by small-angle neutron scattering. These defects appear after annealing and/or deformation of the diamonds.

Core structure of latent heavy-ion tracks in {100} LiF derived by small-angle X-ray scattering

Small-angle X-ray scattering analyses on {100} LiF platelets following irradiation with swift Pb and U ions have revealed continuous highly depleted electron densities close to the ion trajectories, suggesting local ion-induced decomposition of the crystal followed by release of mobile alteration products.

Contribution of small-angle X-ray scattering to microstructural investigation of newly developed Mg–rare earth alloys for structural applications

New magnesium–rare earth alloys, strengthened by a dense fine scale precipitation, have been designed for structural applications up to 523 K. A complementary study using small-angle X-ray scattering is presented here.

Two-dimensional small-angle X-ray scattering from as-grown and heat-treated synthetic quartz

The contribution of molecular water aggregates in the small-angle X-ray scattering of quartz crystals was investigated as a function of the azimuth angle around the primary beam. The presence of Kossel lines randomly decorating the anisotropic two-dimensional pattern and the lack of a clear relationship between Porod invariant and OH content revealed that diffuse scattering plays an important role in the scattering of quartz crystal.

Precursory microstructures in Zr–Cu–Al–Ni bulk metallic glasses examined by anomalous small-angle scattering at the Zr K edge

Microstructures in Zr–Cu–Al–Ni bulk metallic glasses consisting only of metallic elements have been examined by anomalous small-angle scattering at the Zr K edge. The cluster-like scattering was analysed in terms of composition fluctuation.

Microstructural investigation of low-dose neutron irradiation effects in martensitic steels for nuclear application by means of small-angle neutron scattering

The microstructural effect of low-dose neutron irradiation in ferritic/martensitic steels has been investigated by means of small-angle neutron scattering: depending on the initial steel composition different microstructural evolutions are observed during post-irradiation tempering.

Structure of nanoporous zirconia-based powders synthesized by different gel-combustion routes

ZrO₂–2.8 mol% Y₂O₃ powders synthesized by the gel-combustion route were investigated by small-angle X-ray scattering and other techniques. The nanoporous structures of these materials were characterized as functions of the nature of the organic fuel and of the calcination temperature.

Modelling of bacteriophage capsids and free nucleic acids

SAXS-based ab initio modelling of the capsids of isometric bacteriophages allows the solution structure of the constituent hollow spheres to be reconstructed reliably. For the shape of their free nucleic acid, however, other advanced modelling approaches are to be preferred.

Permeability of water through a raft model membrane clarified by time-resolved SANS and SAXS

By the complimentary use of small-angle X-ray and neutron scattering techniques, the permeability of water across a raft model membrane containing ganglioside (G_D3) and the effect of monovalent cations (Na⁺ and K⁺) on the permeability have been investigated. The structures of G_D3 micelle and G_D3/cholesterol mixtures are also discussed.

Charge interaction and temperature effects on the solution structure of lysozyme as revealed by small-angle X-ray scattering

Charge interaction and temperature effects on the solution structure of lysozyme are studied by small-angle X-ray scattering.

Solution structure of Ca²⁺/calmodulin complexed with a lentivirus lytic peptide 1 reveals a novel mode of molecular recognition

The solution structure of Ca²⁺/calmodulin complexed with a lentivirus lytic peptide 1 reveals a novel mode of molecular recognition. The result suggests that this region of the transmembrane glycoprotein is important to viral replication.

Collapse of the hydration shell of a protein prior to thermal unfolding

The change of the hydration shell of hen egg-white lysozyme during the unfolding–refolding process as a function temperature has been analysed. The decrease of the hydration-shell density starts from a lower temperature than the transition temperature of the collapse of the tertiary structure.

Binding of trifluoperazine to apocalmodulin revealed by a combination of small-angle X-ray scattering and nuclear magnetic resonance

Small-angle X-ray scattering and nuclear magnetic resonance studies were performed to investigate the binding of trifluoperazine to Ca²⁺-free calmodulin with N- and C-terminal globular domains connected by a linker.

Initial process of amyloid formation of apomyoglobin and effect of glycosphingolipid G_M1

Using small-angle and wide-angle X-ray scattering techniques it has been possible to clarify the helix-to-sheet (cross-β) transition and the stacking process of the cross-β sheet of apomyoglobin as a model for amyloid.

Upgrade of the small-angle X-ray scattering beamline X33 at the European Molecular Biology Laboratory, Hamburg

A major upgrade of the X33 beamline at the European Molecular Biology Laboratory which has improved the beamline stability and data quality, shortened the measurement time and ensured user-friendly operation is reported.

A modified Ising model for the thermodynamic properties of local and global protein folding–unfolding observed by circular dichroism and small-angle X-ray scattering

The application of a modified Ising model for the thermodynamic properties of local and global protein folding–unfolding is described.

Shape of α-crystallin analyzed by small-angle neutron scattering

The size and shape of aggregates of human recombinant> αA- and αB-crystallins are investigated with small-angle neutron scattering and dynamic light scattering at 310 K and 288 K. The aggregates of αB-crystallin are stable at both temperatures but those of αA-crystallin are deformed at the lower temperature (288 K).

Localization of dihalogenated phenols in vesicle systems determined by contrast variation X-ray scattering

Using contrast variation by means of isomorphous replacement, the localization of dihalogenated phenols in multilamellar vesicles was determined, and was compared with the results of anomalous small-angle scattering.

Small-angle light and X-ray scattering measurements of a protein–oligosaccharide complex mucin in solution

The molecular assembly and chain conformation of a glycoprotein mucin are characterized by using small-angle scattering methods.

Chloride-ion concentration dependence of molecular dimension in the acid-denatured state of equine β-lactoglobulin

The chloride-ion concentration dependence of the molecular shape in the acid-denatured state of equine β-lactoglobulin was observed by small-angle X-ray scattering. The results indicated that the compact molten globule is transformed to an expanded conformation with decreasing chloride-ion concentration. Interestingly, this change accompanied the increase in the helix content as measured by circular dichroic spectra.

Biological solution scattering: recent achievements and future challenges

Solution X-ray and neutron scattering methods are briefly reviewed in view of their appeal and recent progress in data-analysis procedures. Specific examples are discussed highlighting the potential of the techniques and their future developments and applications to structural investigations in the post-genomics era.

ATSAS 2.1 – towards automated and web-supported small-angle scattering data analysis

New features of the small-angle scattering data analysis package ATSAS 2.1 that allow automated data processing and web-based access are described.

Low-resolution models for nucleic acids from small-angle X-ray scattering with applications to electrostatic modeling

It is shown that bead reconstruction algorithms can be used to obtain low-resolution three-dimensional density maps for nucleic acids from SAXS data. In addition, it is shown that the reconstructed bead models can be used to define the molecular geometry in Poisson–Boltzmann calculations to accurately determine the excess number of ions bound under different solution conditions.

Analysis of small-angle X-ray scattering data of protein–detergent complexes by singular value decomposition

We present a method to separate the protein–detergent complex scattering signal from that of `empty' detergent micelles in small-angle X-ray scattering data of protein–detergent mixtures. The approach relies on singular value decomposition and fitting to data collected at different protein–detergent stoichiometries.

Microstructure of ternary system di-lauroyl-phosphatidyl-adenosine/water/cyclo­hexane

Microstructural characterization of 1,2-dilauroyl-sn-glycero-3-phosphatidyl-adenosine micellar solutions upon cyclohexane addition by SANS experiments with internal contrast variation.

Accuracy of molecular mass determination of proteins in solution by small-angle X-ray scattering

A systematic evaluation of the accuracy of molecular mass determination of proteins using small-angle X-ray scattering.

The dynamic behavior of magnetic colloids in suspension

The short-time diffusion of a magnetic charge-stabilized colloidal suspension in the absence of an external applied magnetic field has been investigated by means of X-ray photon correlation spectroscopy.

Study of ferrite ferrofluids by small-angle scattering of polarized neutrons

This work reports the synthesis and the characterization by small-angle scattering of polarized neutrons of ferrofluids consisting of ferrite nanoparticles coated by dodecanoic acid and dispersed in cyclohexane.

Vesicles as reactors of nanoparticles: an anomalous small-angle X-ray scattering study of the domains rich in copper ions

The gaps among the stacks of multilamellar vesicles used for the synthesis of nanoparticles are shown and characterized by ASAXS and freeze-fracture methods.

Salt-concentration dependence of the structure and form factors for the wormlike micelle made from a dual surfactant in aqueous solutions

The small-angle X-ray scattering from dual-surfactant aqueous solutions made from sodium lauryl ether sulfate and coconut fatty acid amido propyl betaine was systematically measured as a function of the net sodium cation concentration and the surfactant concentration. The low-q behaviour of the form factor was consistent with long rigid cylinders while the middle- and high-q profiles fitted well with a core–shell cylinder model.

Small-angle X-ray and small-angle neutron scattering investigations of colloidal dispersions of magnetic nanoparticles and clay nanoplatelets

Mixed colloidal dispersions of clay platelets and magnetic nanoparticles were investigated using small-angle X-ray and neutron scattering. The main contribution to the scattering is due to the magnetic nanoparticles. The scattering intensities are proportional to the concentration of magnetic particles, thus from the scattering point of view the sample is a colloidal dispersion of non-interacting magnetic objects, although the laponite and magnetic particles clearly interact when the sample textures are observed in an optical microscope. The phase separation may be characterized as a liquid–gas transition.

Effect of cations on the structure of sodium bis­(2-ethylhexyl)sulfosuccinate water-in-oil microemulsion

The structure and oligomerization of sodium bis(2-ethylhexyl)sulfosuccinate water-in-oil microemulsion under the presence of monovalent and divalent salts in the water pool are dominated not only by the electrostatic effect between polar headgroups but also by the hydration effect by salts.

X-ray studies of the self-organized structure formed by 1,2-bis­(4'-n-alkoxybenzoyl)hydrazine (BABH-n) homologues. 1. Ia3d-gyroid structure

Examination of the relative intensity of the X-ray 220 reflection with respect to the 211 reference peak as a function of the alkoxy chain length of the title compounds enables the internal structure of the thermotropic Ia3d cubic phase to be clarified.

X-ray fluorescence correlation spectroscopy – a tool to study element-specific dynamics

The dynamics of Au nanoparticles suspended in mixtures of water and glycerol are investigated by X-ray fluorescence correlation spectroscopy. The contrast of the measured time-correlation functions scales as expected with the Au particle concentration. The time constants for translational diffusion and sedimentation in water/glycerol show only qualitative agreement with the expected values.

Mesoscopic structure of dry-pressed clay samples from small-angle X-ray scattering measurements

Small-angle X-ray scattering is used to investigate the meso-structure of dry-pressed samples of nano-layered platelet-shaped clay particles, as water is absorbed into individual particles. The orientational order of the assembly is nematic. Orientation distributions are monitored and show a moderate decrease of this order with water uptake.

Phase behavior of platelet-shaped nanosilicate colloids in saline solutions – a small-angle X-ray scattering study

Precise characterization of the phase diagram for suspensions of sodium fluorohectorite colloids in saline solutions is achieved from small-angle X-ray scattering measurements. Radial intensity profiles are also addressed.

Structural models of metastable phases occurring during the crystallization process of saturated/unsaturated tri­acylglycerols

Structural models are developed for the metastable phases of saturated/unsaturated triacylglycerols appearing at the very beginning of crystallization from the melt based on experimental time-resolved SAXS/WAXS studies of isothermal crystallization in various fats.

Repulsive interlamellar interaction induced by addition of colloidal particles

The addition of colloidal particles between lamellar membrane slits induced a repulsive interlamellar interaction which showed a unique interlamellar distance dependence.

Small-angle neutron scattering study of aqueous solutions of pentanediol and hexanediol

Aqueous solutions of 1,2-pentanediol, 1,5-pentanediol, 1,2-hexanediol and 1,6-hexanediol have been studied by small-angle neutron scattering, and the results analysed with the help of the Kirkwood–Buff formalism. The 1,2-hexanediol solutions exhibit the strongest attractive diol–diol interaction and the excess coordination numbers are in agreement with the possibility of forming micelles.

Structural characterization of N-lignoceroyl (C24:0) sphingomyelin bilayer membranes: a re-evaluation

Sphingomyelin is one of the major sphingolipid components of many animal plasma membranes. SAXS and XRD studies revealed that N-lignocerol (C24:0) sphingomyelin bilayers have a ripple phase and an additional low-temperature stable phase.

Small-angle X-ray scattering investigation of water droplets in mist

Small-angle X-ray scattering measurements of water droplets in a mist were carried out using the BL15XU beamline at SPring-8.

The two-Yukawa model and its applications: the cases of charged proteins and copolymer micellar solutions

An analytical model for the structure factor, based on an effective interaction potential made of an attractive Yukawa term plus a repulsive Yukawa term, has been applied to charged proteins and copolymer micellar solutions.

Unraveling the equilibrium chain exchange kinetics of polymeric micelles using small-angle neutron scattering – architectural and topological effects

Using time-resolved small-angle neutron scattering it is possible to extract the equilibrium exchange kinetics of polymeric micelles. This paper provides insight into the effect of topological constraints on the expulsion time by comparing results from A-B diblock and A-B-A triblock copolymer micelles.

Shear-induced structural transition in the lamellar phase of the C₁₆E₇/D₂O system. Time evolution of small-angle neutron scattering at a constant shear rate

The time evolution of the small-angle scattering of the lamellar phase of a nonionic surfactant C₁₆H₃₃(OC₂H₄)₇OH (C₁₆E₇) in D₂O at a constant shear rate (0.3–30 s⁻¹) is measured. The results indicate a discontinuous decrease in the repeat distance and so suggest some sort of transition.

Small-angle fibre diffraction studies of corneal matrix structure: a depth-profiled investigation of the human eye-bank cornea

The depth-profiled ultrastructure of the collagen fibrillar matrix in the swollen human eye-bank cornea was studied by microbeam small-angle X-ray scattering at a spatial resolution of 25 µm to provide information about collagen fibril diameter, spacing and orientation.

Large-scale and local-scale structures in polymer-blend films: a grazing-incidence ultra-small-angle X-ray scattering and sub-microbeam grazing-incidence small-angle X-ray scattering investigation

Large-scale structures in polymer-blend films are probed by grazing-incidence ultra-small-angle X-ray scattering. By using flow the structural complexity is increased and sub-microbeam grazing-incidence small-angle X-ray scattering allows the local structure to be probed.

Structural changes in gradient colloidal thin gold films deposited from aqueous solution

A gradient in a colloidal thin film prepared from solution is investigated using microbeam grazing-incidence small-angle X-ray scattering. A cross-over and oscillation between a complete layer and depleted regions are detected.

GISAXS study of cavities and {113} defects induced by neon and helium implantation in silicon

The morphology of nanocavities and {113} defects formed by implantation of neon and helium ions in Si(001) is investigated by means of grazing incidence small-angle X-ray scattering experiments.

Self-assembled films of hydrophobin protein HFBIII from Trichoderma reesei

Self-assembled films of hydrophobin HFBIII from the fungus Trichoderma reesei were studied at an air/water interface and on a solid substrate using grazing-incidence X-ray diffraction and reflectivity.

Micellar structure of amphiphilic poly(2-oxazoline) diblock copolymers

Poly[(n-nonyl-2-oxazoline)-b-(methyl-2-oxazoline)] diblock copolymers in aqueous solution form micelles of core-shell type. The core block is stretched, whereas the shell block is coiled.

Grazing-incidence small-angle X-ray scattering study of porous dielectrics used in advanced microelectronic interconnections

The nano-structure of porous ultra-low-k dielectrics, grown using four different processes, is studied by grazing-incidence small-angle X-ray scattering. It is shown that the pore morphology can be either well defined percolated isotropic pores or anisotropic density fluctuations.

Time-resolved grazing-incidence small-angle X-ray scattering studies of lipid multibilayers with the insertion of amyloid peptide during the swelling process

The structural transition of 1,2-dipalmitoyl-sn-glycero-3-phosphocholine (DPPC) multibilayers with the insertion of amyloid peptide 1–40 was studied by grazing-incidence small-angle X-ray scattering at different bilayer hydration levels. With the insertion of the amyloid peptide, the ripple phase of the membrane bilayers was suppressed at high humidity and the whole film can be swollen more uniformly at lower incubation time than the pure DPPC film supported on a silicon wafer.

Study of amorphous nanocrystalline thin silicon films by grazing-incidence small-angle X-ray scattering

The nanostructure of thin silicon films composed of amorphous and crystalline phases was analysed by Raman spectroscopy and grazing-incidence small-angle X-ray scattering. By Raman spectroscopy the crystalline fraction and the average individual crystal sizes were estimated while grazing-incidence small-angle X-ray scattering detected nano sized `objects', presumably voids that are non-spherical in shape, non-uniformly distributed across the depth of the samples.

Structural study of nanocrystalline nickel thin films

Nanocrystalline nickel thin films have been prepared by magnetron sputtering, and have been studied by X-ray diffraction, grazing-incidence small-angle X-ray scattering and atomic force microscopy. Results are given for nanocrystalline Ni (average grain size, unit-cell parameter), intercrystalline matter (size and shape of inhomogeneities) and surface topography of the prepared samples.

Small-angle scattering investigations of magnesium hydride used as a hydrogen storage material

Structural changes in magnesium hydride with and without metal oxide catalysts are characterized using small- and ultra-small-angle neutron scattering, small-angle X-ray scattering, X-ray diffraction and electron microscopy in order to analyse the relation between structure and hydrogen sorption kinetics.

Cylindrical nanochannels in ion-track polycarbonate membranes studied by small-angle X-ray scattering

Small-angle X-ray scattering by nanochannels in track-etched membranes provide global information about the geometry of the nanochannels prepared with a systematic variation of UV irradiation, heavy-ions fluence and membrane material (amorphous polycarbonates).

Residual orientation in micro-injection molded parts

The residual orientation in micro-injection molded polyethylene parts was examined using small-angle neutron scattering, and small- and wide-angle X-ray scattering. The primary cause of residual orientation was found to be oriented crystal growth rather than chain orientation resulting from the injection molding process.

Characterization of two-dimensional ultra-small-angle X-ray scattering apparatus for application to rubber filled with spherical silica under elongation

Two-dimensional ultra-small-angle X-ray scattering apparatus at SPring-8 has been characterized and applied to stretched rubber filled with spherical silica particles.

Iron K-edge anomalous small-angle X-ray scattering at 15-ID-D at the Advanced Photon Source

Analysis of the performance of a pinhole small-angle X-ray scattering instrument at 15-ID-D at the Advanced Photon Source and the development of a reliable method for iron K-edge anomalous small-angle scattering are described.

A focusing-geometry small-angle neutron scattering instrument with a magnetic neutron lens

A focusing-geometry small-angle neutron scattering (FSANS) instrument with a magnetic neutron lens based on an extended Halbach-type sextupole magnet has been constructed and tested. A minimum value of the measurable range, , of  Å⁻¹ could be achieved by the FSANS instrument using a neutron wavelength  Å with for the full width at half maximum.

Wide-q observation from 10⁻⁴ to 2.0 Å⁻¹ using a focusing and polarized neutron small-angle scattering spectrometer, SANS-J-II

A conventional pinhole-type small-angle neutron scattering spectrometer (SANS-J) was successfully reconstructed to be a focusing and polarized neutron small-angle scattering (SANS-J-II) instrument, with a wide q-region from ultra-small-angle scattering of 10⁻⁴ Å⁻¹ to high-q of 2.0 Å⁻¹.

Anomalous small- and wide-angle X-ray scattering and X-ray absorption spectroscopy for Pt and Pt–Ru nanoparticles

Anomalous small- and wide-angle X-ray scattering and X-ray absorption spectroscopy are used to extract structural information on monometallic Pt and bimetallic Pt–Ru nanoparticles.

Reduction of two-dimensional small- and wide-angle X-ray scattering data

The general parametrization of a small- and wide-angle X-ray scattering experiment and a program package for quantitative data reduction are presented.

Monte Carlo simulations of the new small-angle neutron scattering instrument SANS-1 at the Heinz Maier-Leibnitz Forschungsneutronenquelle

The optimization by Monte Carlo simulation of the components of the new small-angle scattering instrument SANS-1 at the Heinz Maier-Leibnitz Forschungsneutronenquelle (FRM II) is described.

New two-dimensional data treatment software for small-angle scattering

A description is given of a new interactive data-treatment program which was mostly developed to analyse two-dimensional small-angle data files. The treatment process is described through specific menus. Several examples show the most useful characteristics of this software.

CMOS flatpanel detectors for SAXS/WAXS experiments

A CMOS flatpanel detector from Hamamatsu Photonics was tested for SAXS/WAXS experiments at SPring-8.

Current status of the 40 m small-angle neutron scattering instrument development at the HANARO research reactor

A Monte Carlo simulation was performed to optimize the newly developed small-angle neutron scattering instrument at the HANARO research reactor. The optimum design of the instrument was obtained based on simulation results.

Performance of the 36 m small-angle neutron scattering spectrometer at BATAN, Serpong, Indonesia

An inter-laboratory comparison of the 36 m small-angle neutron scattering (SANS) spectrometer at BATAN with those of other prominent SANS spectrometers is reported.

Biological small-angle X-ray scattering facility at the Stanford Synchrotron Radiation Laboratory

Beamline 4-2 at the Stanford Synchrotron Radiation Laboratory is a small-angle X-ray scattering/diffraction facility dedicated to structural studies on mostly noncrystalline biological systems. This article outlines recent technological developments and specialized instrumentation for structural biology research at improved time and spatial resolutions.

Development of an ultra-small-angle X-ray scattering instrument for probing the microstructure and the dynamics of soft matter

A low background Bonse–Hart camera for small-angle X-ray scattering is presented. The performance of the instrument is demonstrated by two representative applications in soft matter.

The new V12 ultra-small-angle neutron scattering and tomography instrument at the Hahn–Meitner Institut

The latest developments on instrumentation improvements at the V12 double-crystal and imaging instrument at the Hahn–Meitner Institut are presented. Ways to combine instruments are described and examples of scientific applications from different fields are presented.

A new experimental station for simultaneous X-ray microbeam scanning for small- and wide-angle scattering and fluorescence at BESSY II

A new instrument for microbeam small- and wide-angle X-ray scattering and X-ray fluorescence is available at the microfocus beamline at BESSY II. The instrument is optimized for microbeam scanning experiments of hierarchically structured materials.

The new very-small-angle neutron scattering spectrometer at Laboratoire Léon Brillouin

A description is given of a new compact very-small-angle neutron scattering spectrometer featuring a double-supermirror monochromator, multibeam collimation and a high-resolution two-dimensional position-sensitive detector.

Focusing and polarized neutron small-angle scattering spectrometer (SANS-J-II). The challenge of observation over length scales from an ångström to a micrometre

By using a focusing lens, a pinhole small-angle neutron spectrometer was reconstructed into a focusing ultra-small-angle scattering spectrometer (SANS-J-II).

Anomalous grazing-incidence small-angle X-ray scattering investigation on the surface morphology of an FePt magnetic nanoparticle monolayer on functional modulated substrates

Anomalous grazing-incidence small-angle X-ray scattering was used to verify that FePt nanoparticles remain intact under an Au overlayer during annealing at 1073 K.

Investigation of symmetry-breaking flux-line lattice phases in superconductors by small-angle neutron scattering

The interpretation of complicated small-angle diffraction patterns from multiple flux-line lattice domains in the mixed state of a type-II superconductor is discussed, with particular reference to flux lattice phases in niobium.

Structure of nickel nanoparticles in a microcrystalline cellulose matrix studied using anomalous small-angle X-ray scattering

Anomalous small-angle X-ray scattering was used to characterize the size distribution of nickel nanoparticles that were synthesized in a microcrystalline cellulose matrix.

A comparison of methods for the measurement of the particle-size distribution of magnetic nanoparticles

Transmission electron microscopy, magnetic measurements and small-angle neutron scattering are compared as methods for determining the particle-size distribution of magnetic nanoparticles.

Mixed magnetic phase in 6H-type BaFeO_3−δ

The magnetic properties of 6H-type BaFeO_3−δ were studied using small-angle neutron scattering, positive-muon spin relaxation and magnetization measurements.

The application of distance distribution functions to structural analysis of core–shell particles

The internal structure of core–shell particles has been studied by small-angle X-ray scattering using the method of contrast variation. The indirect Fourier transform yielded distance distribution functions that were compared with three models of increasing sophistication: simple core–shell, core shell with spherical disks and core–shell with stochastic electron density variations.

Density fluctuations in oxide glasses investigated by small-angle X-ray scattering

Three examples of the use of small-angle X-ray scattering in the determination of density fluctuations on the nanometre scale in silica glasses are given: the influence of thermal history and OH content; the determination of static compressibility; and temperature scanning small-angle X-ray scattering as an alternative to temperature scanning calorimetry.

On the heterogeneous character of water's amorphous polymorphism

Two spatial regimes of structural heterogeneity have been identified in amorphous ice structures by small-angle neutron scattering experiments. These are a transient contrast change on a nanometre scale being equally reflected by changes in diffraction data, and a Porod-limit scattering on a micrometre scale demonstrating the presence of interfaces in the amorphous samples.

Pore lattice deformation in ordered mesoporous silica studied by in situ small-angle X-ray diffraction

Sorption and capillary condensation in mesoporous silica were studied by in situ small-angle X-ray diffraction using synchrotron radiation. Analysis of the diffraction peaks reveals deformations of the pore lattice due to capillary condensation and evaporation, respectively.

Mesoscopic structure in near-critical mixtures of D₂O and 3-methylpyridine with salts

Small-angle neutron scattering (SANS) experiments were performed on mixtures of 3-methylpyridine, D₂O, and salts to investigate concentration fluctuations and structures in the vicinity of the critical point. The results can be interpreted in terms of a strong coupling of the critical fluctuation and the solvation effect of salt ions.

Polarized small-angle neutron scattering study of two-dimensional spatially ordered systems of nickel nanowires

Polarized small-angle neutron scattering is used for the characterization of the structure and magnetic properties of two-dimensional spatially ordered systems of ferromagnetic nickel nanowires. These systems are promising for high-density data storage devices.

Small-angle X-ray scattering measurements of expanded fluid Se in the semiconductor–metal transition region using synchrotron radiation

Small-angle X-ray scattering measurements for expanded fluid Se were carried out up to the semiconductor–metal transition region. A broad peak in the small-angle X-ray scattering profiles appears, suggesting a correlation length of 50 Å.

Fractal aggregates of the Pt nanoparticles synthesized by the polyol process and poly(N-vinyl-2-pyrrolidone) reduction

Small-angle X-ray scattering was used to characterize the size and aggregation behavior of the Pt nanoparticles synthesized in the polyol process and the unusual poly(N-vinyl-2-pyrrolidone) reduction.

Reverse Monte Carlo analysis for small-angle scattering of expanded fluid Hg: connection to the wide-angle structure factor

A preliminary result of reverse Monte Carlo analysis of small-angle X-ray scattering data for expanded fluid Hg with the help of wide-angle X-ray diffraction data in the same thermodynamic state is presented. To see the large density fluctuation associated with liquid–vapor critical phenomena, a three-dimensional configuration of 100000 Hg atoms is modeled.

Study on two-dimensional small-angle X-ray scattering of in situ silica filled nanocomposite elastomer during deformation

In situ silica filled soft nanocomposite was prepared by the sol–gel reaction of tetraethoxysilane in peroxide-crosslinked isoprene rubber. The morphological change of the in situ silica particles during the uniaxial stretching and retracting processes was investigated by SAXS.

Small-angle X-ray scattering study on conformation of poly(sodium L-glutamate) in NaCl and NaF aqueous solutions

Local conformations of poly(sodium L-glutamate) in NaCl and NaF aqueous solutions are analyzed with small-angle X-ray scattering, circular dichroism and nuclear magnetic resonance techniques.

Surface free energies of isotactic polybutene-1 tetragonal and trigonal crystals: the role of conformational entropy of side chains

Lateral surface free energies σ of isotactic polybutene-1 trigonal and tetragonal crystals grown in the melt have been determined from small-angle X-ray scattering experiments, differential scanning calorimetry and in situ observation of crystal growth kinetics. The σ value of the trigonal crystals is about seven times as large as the value theoretically estimated, while σ for the tetragonal crystals is roughly in agreement with the estimation.

Fracture of poly(vinyl­idene fluoride): a combined synchrotron and laboratory in-situ X-ray scattering study

Time-resolved synchrotron X-ray scattering was used to study the plastic zone formation and fracture processes at different strain rates in poly(vinylidene fluoride). This gives new insight into the micro-mechanisms of cavitation, lamellae separation and fibril formation.

Living anionic polymerization of methyl meth­acrylate controlled by metal-free phosphazene catalyst as observed by small-angle neutron scattering, gel-permeation chromatography and UV–visible spectroscopy

Phosphazene (PZN) catalyst, a mixture of PZN and a co-catalyst 1-hydroxycyclohexyl phenyl ketone (Irgacure 184; IRG), and polymethylmethacrylate prepared by catalytic living anionic polymerization using the PZN catalyst and IRG have been observed for the first time by small-angle neutron scattering and UV–visible spectroscopy to elucidate the aggregation behavior of the PZN molecules and the state of living chain ends in a living polymer solution.

Gibbs–Thomson analysis of crystalline poly(9,9-di-n-octyl-2,7-fluorene)

A value of 76 kJ mol⁻¹ as the work of fold for the title polymer was obtained via Gibbs–Thomson analysis. This value significantly exceeds those of typical polymers, reflecting the backbone rigidity while being consistent with the large-loop folds proposed for this particular polymer of conjugated backbone.

Small-angle X-ray scattering from polystyrene polymacromonomers with relatively short main chains

Small-angle X-ray scattering from polymacromonomers is described.

Structural formation and many-body effect of concentrated dendrimer solutions by computer simulations

Structural formation and effective interaction in a charged dendrimer solution are investigated by parallel stochastic molecular dynamics simulations.

Effect of lithium tri­fluoro­methane­sulfonate on the phase diagram of a liquid-crystalline amphiphilic diblock copolymer

Phase transitions and nanometre-scale ordered structures of a binary system of a liquid-crystalline amphiphilic diblock copolymer containing polyethylene oxide and lithium trifluoromethanesulfonate were investigated by differential scanning calorimetry and small-angle X-ray scattering.

Complexity of silicate/aluminosilicate poly­merization: some insights using a small-angle X-ray scattering study

The growth processes of silicate (aluminosilicate) particles starting from clear homogeneous solutions of silicate monomers/oligomers or colloidal solutions of silica nanoparticles were investigated by small-angle X-ray scattering.

Synchrotron X-ray scattering studies on the structural evolution of microbial poly(3-hydroxybutyrate)

The primary and secondary crystallization behaviors of microbially synthesized poly(3-hydroxybutyrate) were studied in detail by time-resolved small-angle X-ray scattering with a synchrotron-radiation source.

A small-angle X-ray scattering study of the effect of chain architecture on the shear-induced crystallization of branched and linear poly(ethylene terephthalate)

Reactive extrusion of PET with branching and chain-extension agents results in enhanced rheological properties. Small-angle X-ray scattering was used to establish the crystallization kinetics and the molecular architecture following a step shear in the melt. Linear PET exhibited isotropic crystallization that was slower with increasing molecular weight, while long-chain-branched PET showed the opposite trend.

A qu­antitative analysis of small- and wide-angle X-ray diffraction curves of homogeneous ethylene-1-octene copolymers

The parameters of lamellar stacks in copolymers were determined from matching of the theoretical and experimental scattering curves and compared with the parameters derived from the correlation function. Determined crystallinity values were compared with the results obtained from the wide-angle X-ray diffraction (WAXD) method.

Time domain effects in the single-chain dynamics of semidilute and concentrated polymer solutions

Two dynamical regimes in time scales are predicted: Zimm and Rouse-like motion. The principal mechanism for the hydrodynamic screening is a dynamic phenomenon.

Synchrotron X-ray scattering and reflectivity studies of the structure of low dielectric constant SiOCH thin films prepared from bis­tri­methylsilylmethane by chemical vapor deposition

A series of low dielectric constant, nanoporous SiOCH dielectric thin films with nanometre-scale thicknesses were prepared by plasma chemical vapor deposition of bistrimethylsilylmethane precursor and oxygen gas, and characterized in detail by grazing-incidence X-ray scattering and specular X-ray reflectivity analyses with synchrotron radiation sources, along with spectroscopic ellipsometry analysis.

Structural analysis of thin films of novel polynorbornene derivatives by grazing incidence X-ray scattering and specular X-ray reflectivity along with ellipsometry

The structure and properties of two novel polynorbornene derivatives, chiral poly(norbornene acid methyl ester) and racemic poly(norbornene acid n-butyl ester) in supported thin films were investigated in detail by synchrotron grazing incidence X-ray scattering, specular reflectivity and ellipsometry.

Synchrotron X-ray reflectivity studies of nanoporous organosilicate thin films with low dielectric constants

Low dielectric constant thin films containing closed nanopores were prepared by thermal processing of blend films of a thermally curable organosilicate precursor and a thermally labile reactive six-arm porogen in various compositions, and their structure and properties were characterized in detail by synchrotron X-ray reflectivity along with thermogravimetry and transmission electron microscopy.

Grazing-incidence small-angle X-ray scattering studies on templating nanopores in networked polymer thin films with a multi-armed porogen

The miscibility of a six-armed star porogen in a crosslinkable organosilicate dielectric precursor and the mechanism of pore generation in the organosilicate thin films by sacrificial thermal degradation of the porogen were quantitatively investigated by using in situ grazing-incidence small-angle X-ray scattering and thermogravimetry.

Melting behavior of polymorphic crystals of poly(tri­methylene 2,6-naphthalate) studied by simultaneous synchrotron X-ray scattering and thermal analysis

The polymorphic crystallization and melting behavior of poly(trimethylene 2,6-naphthalate) have been investigated using small-angle X-ray scattering and simultaneous wide-angle X-ray scattering and differential scanning calorimetry.

In situ investigation of annealing effect on lamellar stacking structure of polyethylene thin films by synchrotron grazing-incidence small-angle and wide-angle X-ray scattering

The annealing effect on lamellar stacking structure of polyethylene thin films prepared on silicon wafers has been investigated in terms of molecular- and meso -scale regularity by in-situ synchrotron grazing-incidence small-angle and wide-angle X-ray scattering measurements.

In situ and time-resolved ultra small-angle neutron scattering observation on growing poly(methyl methacrylate)-block-polystyrene via reversible addition–fragmentation chain transfer living radical polymerization

We investigated the time evolution of polymerization-induced molecular self-assembly, appearing in a reaction solution of living radical polymerization of poly(methyl methacrylate)-block-polystyrene by employing in situ and time-resolved ultra small-angle neutron scattering and time-resolved gel permeation chromatography methods.

Lamellar crystal thickness transition of melt-crystallized isotactic polybutene-1 observed by small-angle X-ray scattering

The first-order long period, the second-order long period and lamellar crystal thickness l_c of isotactic polybutene-1 have been investigated for crystallization in the melt over a wide range (313.2–363.2 K) of crystallization temperatures by small-angle X-ray scattering experiments and density measurements. The crystal thickness l_c demonstrates two linear dependences on inverse supercooling and a transition from one dependence to the other has been observed around 338.2 K, where l_c becomes comparable with the radius of gyration R_g of the samples.

Structural development of dynamically asymmetric polymer blends under uniaxial stretching

The structural change during uniaxial stretching was investigated by use of time-resolved small-angle X-ray scattering for dynamically asymmetric polymer blends irradiated by an electron beam. A dominant mode at the early stage of the stretch-induced enhancement of concentration fluctuations exists, similar to early stage spinodal decomposition for fluid mixtures.

Concentration fluctuations induced by orientation fluctuations in polybutadiene–4-cyano-4'-n-octylbi­phenyl mixtures

The changes in concentration fluctuations of polymer–liquid crystal binary mixtures with temperature were investigated by small-angle X-ray scattering in their one-phase region and in the isotropic state of the liquid crystal. The concentration fluctuations consist of two modes: an OZD mode expressed by the Ornstein–Zernike–Debye equation with a correlation length ξ and a DB mode expressed by the Debye–Buche equation with a correlation length l.

Small-angle X-ray study of the three-dimensional collagen/mineral superstructure in intramuscular fish bone

Small-angle meridional reflections and near-equatorial diffuse scattering from intramuscular shad/herring bone were analyzed based on two-dimensional fitting schemes that take preferred orientation effects into account.

Qu­antitative analysis of molecularly stacked layer structures in supported organic thin films by synchrotron grazing-incidence X-ray scattering

A grazing-incidence X-ray scattering (GIXS) formula is derived for molecularly stacked layer structures in substrate-supported nanoscale thin films. Using this formula, the GIXS data obtained for S-docosanylcysteine thin films supported with silicon substrates are analyzed quantitatively, providing information on the structural parameters and orientation of the films.

Discrepancy in determination of χ parameters by melting point depression versus small-angle neutron scattering in blends of deuterated polycarbonate and isotactic poly(methyl methacrylate)

The discrepancy in the χ interaction parameters of deuterated polycarbonate/isotactic poly(methyl methacrylate) blends as determined by melting point depression and small-angle scattering is reconciled by relaxing Flory's assumption of complete rejection of solvent from the crystal phase. The phase diagram of crystalline polymer blends, involving liquid–liquid phase separation and solid–liquid phase transitions, has been established.

X-ray reflectivity studies on the deoxyribonucleic acid adsorption by 3-β-[N-(N',N'-di­methylamino­ethane)carbamoyl]cholesterol monolayer with divalent ions

The effect of adding divalent ions on the deoxyribonucleic acid adsorption by a cationic lipid monolayer at the air–water interface was investigated by X-ray reflectivity.

Green thin polymer film metallization using supercritical carbon dioxide

Thin polymer film metallization using supercritical carbon dioxide as a solvent has been characterized by means of X-ray reflectivity and peel test.

Thermal radiation method: proposal of a new technique for measuring interfacial or surface fluctuations

A thermal radiation method is proposed as a new technique for measuring interfacial or surface fluctuations. The principle is explained and an example of an experiment using the method is given.

The puzzle-interlayer model: an approach to the analysis of tightly packed arrangements of hard particles

The small-angle scattering (SAS) structure functions of a random two-phase particle arrangement, constructed from the separated parts of a tessellation (puzzle particles), are analyzed. The SAS intensity depends on the shape of the puzzle pieces and on the thickness of the intermediate layer between them. Based on the chord length distribution densities of the interlayer and of the `puzzle particles', the approach allows the analytical description of a wide spectrum of random particle shapes. The `dead leaves' and the Poisson plane mosaic are considered in more detail.

Multiple-length-scale small-angle X-ray scattering analysis on maghemite nanocomposites

We report small-angle X-ray scattering analysis of maghemite polymer nanocomposites containing spherical particles uniformly distributed in the polymer matrix. Scattering intensity curves show features characteristic of multiscale structured systems. Based on the Beaucage approach, we conclude that the nanoparticle size increases with the iron loading used in the preparation of the nanocomposite.

Evaluation of multiple small-angle neutron scattering including magnetic interactions

Formulae describing multiple small-angle scattering of polarized neutrons by ferromagnetic inhomogeneities are derived. The results show an anomalous distribution of scattered neutrons due to the simultaneous effect of multiple scattering and the spin dependence of the single-scattering cross section.