Search results for " EXAFS"
showing 10 items of 20 documents
Decorated pottery study: Analysis of pigments by x-ray absorbance spectroscopy measurements
2007
Characterization of pigments on decorated pottery fragments has been fully carried out by nondestructive x-ray absorbance spectroscopy (XAS). The samples were a series of pottery shards excavated from the archeological site of Caltagirone (Sicily, Italy), a well-known ceramic production center. Aesthetical criteria and morphological observations allowed us to attribute the samples to quite different historical periods, starting from the 18th century B.C. up to the 16th century A.D. An extensive time interval led us to suppose that different materials and techniques were used for the production of the ceramic paste and also for the preparation of pigments. XAS measurements were performed at …
Equilibrium, Structural and Biological Activity Studies on [Organotin(IV)]n+ Complexes
2008
Organotin(IV) compounds are characterized by the presence of at least one covalent C–Sn bond. The compounds contain tetravalent {Sn} centers and are classified as mono-, di-, tri-, and tetraorganotin(IV), depending on the number of alkyl (R) or aryl (Ar) moieties bound. The anions are usually Cl, F, O2, OH,–COO, or –S. It seems that the nature of the anionic group has only secondary importance in biological activity. The rapid rise in the industrial (catalyst in PVC and foam production), agricultural (fungicides and acaricides), and biological applications (wood, stone, and glass preservatives) of organotin(IV) compounds during the last few decades has led to their accumulation in the envir…
A new cell for the study of in situ chemical reactions using X-ray absorption spectroscopy
2005
An in situ cell for reductive and oxidative treatments at different temperatures that allows the possibility of recording data as a function of temperature has been designed and constructed for X-ray absorption experiments at the GILDA beamline BM08 of ESRF. The cell is linked to a mass quadrupole spectrometer providing control of the reaction gases and monitoring of the products. The apparatus allows measurements to be performed both in transmission and fluorescence geometry. The cell was tested by studying the CO oxidation reaction promoted by a Pt/ceria-zirconia-supported catalyst. The CO(2) yield is correlated with the structural results confirming the existence of a strong metal-suppor…
Effects of heat treatments on the properties of copper phthalocyanine films deposited by glow-discharge-induced sublimation
2006
Copper phthalocyanine films have been deposited by glow-discharge-induced sublimation. The films have undergone postdeposition heat treatments in air at 250 and 290 °C for different times, ranging from 30 min to 14 h. The properties of as-deposited and heated films have been investigated by different techniques in order to determine the effects of heat treatments on the film properties. Fourier transform infrared analysis and UV−visible optical absorption analysis point out a gradual evolution of the film structure from a mixture of α and β polymorphs to the only β polymorph in the sample heated at 290 °C for 14 h. A pronounced decrease of carbon and nitrogen atomic percentages against an o…
Al driven peculiarities of local coordination and magnetic properties in single phase Alx CrFeCoNi high entropy alloys
2021
The authors thank the Helmholtz-Zentrum Berlin for the provision of access to synchrotron radiation facilities and allocation of synchrotron radiation at the PM2-VEKMAG, BAMline, and UE46_PGM-1 beamlines of BESSY II at HZB as well as measurement time for magnetometry at HZB CoreLab for Quantum Materials. A. S. acknowledges personal funding from CALIPSOplus project (the Grant Agreement no. 730872 from the EU Framework Programme for Research and Innovation HORIZON 2020). The financial support for the VEKMAG project and the PM2-VEKMAG beamline by the German Federal Ministry for Education and Research (Nos. BMBF 05K10PC2, 05K10WR1, 05K10KE1) and by HZB is cordially acknowledged by all co-author…
Structure and oxide ion conductivity: local order, defect interactions and grain boundary effects in acceptor-doped ceria
2014
The long-range and short-range structure of nanocrystalline and microcrystalline acceptor-doped ceria is investigated by a combined approach using EXAFS, XANES, Raman, and XRD, and correlated with the oxide-ion conductivity in the bulk and in grain boundaries. Compared to Yb3+ and Er3+, the positive influence of Sm3+ is attributed to the ability to repel oxygen vacancies, and to keep a localized disorder around the dopant. The long-range structural analysis shows lattice contraction for Yb- and Er-doping and lattice expansion for Sm-doping. The short-range analysis around the dopants and cerium highlights that a more complex structural rearrangement has to be assumed to explain the compleme…
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…
Evidence for a Double Doping Regime in Nd:YAG nanopowders
2009
Nanopowders of Yttrium Aluminium Garnet doped with neodymium (Nd:YAG) were investigated by X-Ray Absorption Fine Structure (XAFS) at the Nd LIII-edge in the 1.3 - 20.8 % doping range. XANES spectra appear similar in the full range of the Nd concentration. However, a significant decrease in the white line intensity of XANES is revealed as the quantity of Nd doping ions increases. Plotting the white line intensity as a function of Nd doping ions reveals two linear trends with two different slopes, identifying a threshold value where the neodymium concentration reaches 5 at.% This experimental finding provides support for the existence of a double doping regime in Nd:YAG nanopowders.
Large atomic disorder in nanostructured LaNi5 alloys: A la L3-edge extended X-ray absorption fine structure study
2010
Abstract Local structure of the nanostructured LaNi 5 alloys, prepared by ball-milling, has been studied using La L 3 -edge extended X-ray absorption fine structure spectroscopy. The near-neighbor distances tend to decrease with the ball-milling, and the mean square relative displacements (MSRD) show substantial increase suggesting an increased atomic disorder. High temperature annealing helps in partial recovery of atomic order in the ball-milled samples for milling times upto 20 h, however, the long-time ball-milled samples seems to gain only a local random order. The results suggest that reduced unit-cell volume together with large atomic-disorder might be causing a higher energy-barrier…