Search results for "small-angle"

Formation and Growth of Pd Nanoparticles Inside a Highly Cross-Linked Polystyrene Support: Role of the Reducing Agent

2014

Simultaneous time-resolved SAXS and XANES techniques were employed to follow in situ the formation of Pd nanoparticles in a porous polystyrene support, using palladium acetate as a precursor and gaseous H2 or CO as reducing agents. These results, in conjunction with data obtained by diffuse reflectance UV–vis and DRIFT spectroscopy and TEM measurements, allowed unraveling of the different roles played by gaseous H2 and CO in the formation of the Pd nanoparticles. In particular, it was found that the reducing agent affects (i) the reduction rate (which is faster in the presence of CO) and (ii) the properties of the hosted nanoparticles, in terms of size (bigger with CO), morphology (spherica…

Double implantation in silica glass for metal cluster composite formation: a study by synchrotron radiation techniques

2001

Silica glass containing metal clusters is studied for both basic and applied aspects, related to the physics of cluster formation and to the optical properties of these materials. To obtain such composite structure, Cu+ Ni, Au+ Cu, Au+ Ag, Cu+ Co, and Cu+ Ag sequential implantations in fused silica were realized. The resulting systems, after possible annealing in various atmospheres, were studied by synchrotron radiation-based techniques, namely, extended X-ray absorption fine structure (EXAFS) spectroscopy, grazing incidence X-ray diffraction (GIXRD), and grazing incidence small angle X-ray scattering (GISAXS). The unique potential of these techniques is the capability to investigate dilut…

Combined small-angle x-ray scattering/extended x-ray absorption fine structure study of coated Co nanoclusters in bis(2-ethylhexyl)sulfosuccinate

2009

Chemically stable cobalt nanostructures have been prepared with Co(II) reduction in the confined space of cobalt bis(2-ethylhexyl)sulfosuccinate, Co(AOT)2, reverse micelles dispersed in n-heptane. The reaction was carried out by adding a solution of sodium borohydride in ethanol (1% weight) to a 0.2M micellar solution of Co(AOT)2 in n-heptane at a reductant to Co(II) molar ratio of 4. This procedure involves the rapid formation of surfactant-coated Co nanoparticles followed by their slow separation as nanostructures embedded in a sodium bis(2-ethylhexyl)sulfosuccinate matrix. The resulting composites, characterized by extended x-ray absorption fine structure and small-angle x-ray scattering…

Fractal approach in petrology: Combining ultra small angle (USANS), and small angle neutron scattering (SANS)

2000

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.

Spherical microgel colloids - Hard spheres from soft matter

1998

While gels are usually considered to be soft materials, we demonstrate that it is possible to model hard sphere behaviour when the gel structure is confined to spherical objects of sizes in the colloidal range. We have measured the static structure factor of microgel spheres dispersed in good solvents, differing in size, crosslink density and swelling behaviour, by light scattering and small angle neutron scattering. Comparing with theoretical calculations for polydisperse hard spheres we show how the interactions in highly concentrated dispersions of spherical microgel colloids are determined by an interplay of the relative length of dangling polymer ends at the surface (determined by the …

Determination of the Composition of Mixed Hydrogenated and Fluorinated Micelles by Small Angle Neutron Scattering

1997

1983

The neutron scattering from mixtures of deuterated and undeuterated poly(ethylene oxide), (D-PEO, H-PEO), in the small angle and intermediate angle region has been measured in the melt. We found no indications of a molecular segregation. The value of molecular weight evaluated agreed with that obtained by other methods. For a sample with a molar mass of 120000 g/mol the radius of gyration 〈rw2〉1/2 was found to be 13,6 nm, which corresponds to a characteristic ratio of C = 6,9. The form factor of a single chain can be described by the Debye equation for a random coil with the same unperturbed dimensions. Our results are compared with rotational isomeric state calculations and measurements in…

Structural Characterization of the “Knitting Pattern” in Polystyrene-block-poly(ethylene-co-butylene)-block-poly(methyl methacrylate) Triblock Copoly…

1998

In a polystyrene-block-polybutadiene-block-poly(methyl methacrylate) triblock copolymer (SBM) a morphological transition from a lamellar (ll) morphology (with sequence ABCB) to the knitting pattern (kp) morphology occurs upon hydrogenation of the center PB block. Structural information of the nonhydrogenated and the hydrogenated material is provided from small angle X-ray scattering (SAXS) and transmission electron microscopy (TEM). For the nonhydrogenated SBM sample the SAXS profile correlates well with a simple periodic lamellar structure. The hydrogenated sample forming the kp morphology displays a more complex SAXS pattern. From the TEM images of the knitting pattern the two-dimensional…

Synthesis and physico-chemical characterization of gold nanoparticles softly coated by AOT

2006

Size-controlled gold nanoparticles/surfactant stable systems were prepared by the combined action of the solvated metal atom dispersion (SMAD) technique and confinement in anhydrous sodium bis(2-ethylhexyl)sulfosuccinate (AOT) micellar solution. From liquid samples, by evaporation of the organic solvent, solid gold nanoparticle-surfactant liquid crystals composites were obtained. Sample characterization was performed by X-ray diffraction (SAXS and WAXS), XPS spectroscopy and UV-vis-NIR spectroscopy. All experimental data consistently revealed the coexistence of two gold nanoparticle size populations: bigger nanoparticles (size 20-50 angstrom) and smaller ones (size of few angstrom). The two…

Physico-chemical characterization of Pd nanoparticles synthesized in w/o microemulsions

1998

Abstract The long time stability of surfactant-coated Pd nanoparticles in w/o microemulsions has been investigated. It has been proven that in suitable conditions, the use of the functionalized surfactant Pd(AOT)2 allows to obtain very stable nanosized Pd particles and to finely control their average size.