Search results for " X-ray Scattering"
showing 10 items of 154 documents
Small-angle x-ray scattering experiments for investigating the validity of the two-phase model
1973
A New method for evaluating SAXS curves of polymer samples with lamellar structure is applied to two typical scattering curves measured with a solution-crystallized linear polyethylene and a melt-crystallized branched polyethylene respectively. The method permits a rigorous check of the validity of the two-phase model and yields, without additional measurement, the volume fractions of the two phases and the difference in their densities. The densities can than be obtained by measuring the overall density of the sample. The results are: ρc = 0.996 g/cm3,ρa = 0.854 g/cm3, wa = 0.20 for the solution-crystallized sample; ρc = 0.967 g/cm3,ρa = 0.850 g/cm3, wa = 0.36 for the melt-crystallized sam…
Proteins in amorphous saccharide matrices: Structural and dynamical insights on bioprotection
2013
Bioprotection by sugars, and in particular trehalose peculiarity, is a relevant topic due to the implications in several fields. The underlying mechanisms are not yet clearly elucidated, and remain the focus of current investigations. Here we revisit data obtained at our lab on binary sugar/water and ternary protein/sugar/water systems, in wide ranges of water content and temperature, in the light of the current literature. The data here discussed come from complementary techniques (Infrared Spectroscopy, Molecular Dynamics simulations, Small Angle X-ray Scattering and Calorimetry), which provided a consistent description of the bioprotection by sugars from the atomistic to the macroscopic …
Small-angle x-ray scattering studies of melting
1980
The course of melting of melt-crystallized polyethylene fractions and of a poly(ethylene oxide)-polystyrene-poly(ethylene oxide) triblock copolymer has been followed by small-angle x-ray scattering (SAXS). Changes in the intensity and shape of the SAXS curves indicated that both surface melting and melting over the full crystallite thickness (full-strand melting) take place. Full strand melting is the final, irreversible process. Comparison with an analytical model indicates that in the earlier stages of the irreversible, full-strand process the crystallites melt out randomly throughout the bulk. Later stages may occur by the simultaneous melting of a larger stack of crystallites.
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…
Wide Angle X-ray Scattering as a Technique of Choice to Probe Asphaltene Hierarchical Structures
2020
Bitumens are composite systems extensively used in road pavements. Due to their complex nature, a rational understanding of the relationships between composition, structure and performances of these materials is still far from being achieved, so research attempting to shed more light in this field is required. Here, we exploit Wide Angle X-ray Scattering (WAXS) as a technique of choice to shed light on the bitumen structure at different length scales. Diagnostic fingerprints, characterizing the WAXS profile, are correlated to specific Bragg distances which can be reasonably attributed to the molecular and supramolecular aggregation taking place at various levels of complexity leading to the…
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.