Search results for "SAXS"

The Pyridyl Functional Groups Guide the Formation of Pd Nanoparticles Inside A Porous Poly(4-Vinyl-Pyridine)

2015

The reactivity of palladium acetate inside a poly(4-vinylpyridine-co-divinylbenzene) polymer is strongly influenced by the establishment of interaction between the Pd precursor and the pyridyl functional group in the polymer. Diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and simultaneous X-ray absorption near edge structure (XANES) and small angle X-ray scattering (SAXS) techniques have been applied to monitor the reactivity of palladium acetate in the presence of H-2 and CO as a function of temperature. H-2 reduces palladium acetate to Pd nanoparticles and acetic acid. The pyridyl groups in the polymer play a vital role both in stabilizing the formed acetic acid, thu…

FTIR and SAXS study on MBCO-saccharide amorphous systems: protein-matrix reciprocal effects

2010

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…

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…

Synchrotron Radiation and Chemistry: Studies of Materials for Renewable Energy Sources

2014

We present an overview of selected applications of synchrotron radiation methods to topical chemical research. The analysis is limited to the studies on materials for renewable energy sources, focussing on topics peculiar to chemical research, such as reactivity and synthesis routes; in particular, the paper takes into account subjects having some relevance for the production and storage of energy based on hydrogen. Hydrogen production and storage are taken into account in the sections concerning: (i) Dye-sensitized solar cells, (ii) Metal-organic frameworks and (iii) Hydrides for hydrogen storage; production of energy by fuel cell devices is treated in (iv) Oxide ion and proton conductors …

Synthesis of Nd:YAG nanopowder using the citrate method with microwave irradiation

2010

Abstract Nd:YAG nanopowders were prepared using the Pechini process with microwave irradiation ( MWs ). A reference sample was also prepared using conventional heating. XRD pattern analysis showed that nanopowder obtained by means of conventional heating and calcination for 1 h at 900 °C has a structure made up of the garnet phase together with the hexagonal phase that disappeared after two additional hours of thermal treatment. The MWs powder calcined for 1 h consists of the single garnet phase. SAXS data analysis indicated that nanoparticles are characterized by a sharp interface. TEM investigation showed crystalline particles with remarkable agglomeration in both samples, although a more…

Structural and electrochemical investigation on re-cast Nafion membranes for polymer electrolyte fuel cells (PEFCs) application

2006

Abstract Starting from a 5 wt% ion power Nafion® solution and dissolving the dry residue in a suitable solvent (10 wt% solution in dimethylacetammide), re-cast Nafion films were developed for polymer electrolyte fuel cells (PEFCs) application. The used Doctor-Blade casting technique allowed to prepare scaled-up membranes comparable to the commercial Nafion ones with good mechanical resistance, thickness homogeneity and an excellent reproducibility. The differences between the re-cast membrane nanostructure and that of the commercial Nafion were investigated by synchrotron small-angle X-ray scattering. The obtained re-cast membrane shows at ambient conditions a semi-crystalline structure wit…

Astringency and the interactions between a human salivary proline-rich protein and tannins

2015

International audience

SAXS Study on Myoglobin Embedded in Amorphous Saccharide Matrices

2011

We report on Small Angle X-ray Scattering (SAXS) measurements performed on samples of carboxy-myoglobin and met-myoglobin embedded in low hydrated matrices of four different saccharides (trehalose, sucrose, maltose and lactose). Results confirm the already reported occurrence of inhomogeneities, which are not peculiar of trehalose samples, but appear also in maltose and lactose, and in some cases also sucrose, being dependent on the sample hydration and on the presence of sodium dithionite. This behaviour confirms our previous interpretation about the nature of the inhomogeneities, and prompt it as a possible general behaviour for highly concentrated sugar matrices.

Water and temperature contribution to the structuration of starch matrices in the presence of flavour

2015

The effect of hydrothermal treatments and flavours addition on starch structure and its physical properties were studied. Native wheat starch was treated at 2 different hydrations (water-starch ratios: 50/50 and 80/20 g w/w) and temperatures (65 and 85 °C) in the presence of flavours (ethyl hexanoate and 2-hexanone). The freshly prepared samples were subjected to DSC and flavour analysis. Flavour inclusion complex could not be detected by DSC, however the result of flavour analysis proved that there were flavours interactions with starch. Both ethyl hexanoate and 2-hexanone interacted with starch at similar rates. The highest flavour loss was found in the samples at high hydration and heate…