RESUMEN
Four gold coins minted in the V century have been studied with non-destructive synchrotron radiation techniques, namely X-Ray Fluorescence (XRF) and X-ray Absorption Near Edge Spectroscopy (XANES). XRF data analyzed coupling standard and statistical methods were used to distinguish the composition of the alloy constituting the coins from that of successive deposits processes. Our analysis presents a quantification of the trace elements present in the metallic alloy providing interesting details for historical insight. Furthermore, on the basis of the XRF maps, some regions of interest were selected for XANES at the K-edge of Fe. Our analysis of the Fe spectra points out two main phases which can be related to Fe oxides naturally present in soil. From the relative abundance of these oxides, information on the site where the coins were found can be obtained, providing additional information on their fate across the centuries.
RESUMEN
We have studied the local structure of LaO0.5F0.5BiS2-x Se x by Bi L1-edge extended x-ray absorption fine structure (EXAFS). We find a significant effect of Se substitution on the local atomic correlations with a gradual elongation of average in-plane Bi-S bondlength. The associated mean square relative displacement, measuring average local distortions in the BiS2 plane, hardly shows any change for small Se substitution, but decreases significantly for [Formula: see text]. The Se substitution appears to suppress the local distortions within the BiS2 plane that may optimize in-plane orbital hybridization and hence the superconductivity. The results suggest that the local structure of the BiS2-layer is one of the key ingredients to control the physical properties of the BiS2-based dichalcogenides.
RESUMEN
The possibility of tuning the magnetic behaviour of nanostructured 3d transition metal oxides has opened up the path for extensive research activity in the nanoscale world. In this work we report on how the antiferromagnetism of a bulk material can be broken when reducing its size under a given threshold. We combined X-ray diffraction, high-resolution transmission electron microscopy, extended X-ray absorption fine structure and magnetic measurements in order to describe the influence of the microstructure and morphology on the magnetic behaviour of NiO nanoparticles (NPs) with sizes ranging from 2.5 to 9 nm. The present findings reveal that size effects induce surface spin frustration which competes with the expected antiferromagnetic (AFM) order, typical of bulk NiO, giving rise to a threshold size for the AFM phase to nucleate. Ni(2+) magnetic moments in 2.5 nm NPs seem to be in a spin glass (SG) state, whereas larger NPs are formed by an uncompensated AFM core with a net magnetic moment surrounded by a SG shell. The coupling at the core-shell interface leads to an exchange bias effect manifested at low temperature as horizontal shifts of the hysteresis loop (~1 kOe) and a coercivity enhancement (~0.2 kOe).
RESUMEN
Extended X-ray absorption fine structure (EXAFS) has been measured at both the K edges of gallium and arsenic in GaAs, from 14 to 300 K, to investigate the local vibrational and thermodynamic behaviour in terms of bond expansion, parallel, and perpendicular mean square relative displacements and third cumulant. The separate analysis of the two edges allows a self-consistent check of the results and suggests that a residual influence of Ga EXAFS at the As edge cannot be excluded. The relation between bond expansion, lattice expansion, and expansion due to anharmonicity of the effective potential is quantitatively clarified. The comparison with previous EXAFS results on other crystals with the diamond or zincblende structure shows that the values of a number of parameters determined from EXAFS are clearly correlated with the fractional ionicity and with the strength and temperature interval of the lattice negative expansion.
RESUMEN
A compact, double-sided laser-heating system for diamond-cell synchrotron applications is described. The optical table, containing laser, spectrometer, and all optics for visual observation and measuring temperatures and pressures has an area of less than 1/2 m(2) and weighs less than 20 kg. All components can be remotely controlled at micron levels with simple dc motors and pneumatic drives. The design allows quick alignment of the laser-heated hot spot with the x-ray beam and the spectrometer. The prealigned system can be set up at most synchrotron beamlines within about 1 h. We carried out measurements on a variety of materials above one megabar and up to over 4000 K at both the x-ray diffraction beamline ID 27 and the x-ray absorption beamline ID 24 at the European Synchrotron Facility. A new measurement of the melting temperature of iron by x-ray absorption spectroscopy is presented.
RESUMEN
Structural transformations at high pressure in amorphous and quartz-like crystalline GeO(2) have been investigated by using a Paris-Edinburgh press coupled to EXAFS spectroscopy. From both the germanium absorption edge position and the Ge-O distance evolution, new detailed information has been obtained about the pressure behavior of the short range order. Crystalline GeO(2) undergoes a transformation from four- to six-fold coordination at about 8.5 GPa, but at least the whole 6-12 GPa pressure range should be considered as the transition region. On the other hand, amorphous GeO(2) is characterized by a much more gradual structural change and the full octahedral state is not reached at 13 GPa as commonly believed. Furthermore, no support to the recently claimed fully pentahedral intermediate state can be given. EXAFS signals of glassy GeO(2) beyond the first Ge-O shell qualitatively confirm the continuous breakdown of the intermediate range order up to 10 GPa.
RESUMEN
The NaCl-to-Cmcm phase transition and the Cmcm structure of InAs under high pressure are studied by x-ray diffraction. The lattice parameters and fractional coordinates are given as a function of pressure. We propose a mechanism responsible for this type of symmetry breaking under pressure. We show that the ppσ interactions do not play a major role in the stabilization of the NaCl structure. Consequently the NaCl-to-Cmcm transition occurs only in compounds with a large charge transfer. General conclusions on the behavior of III-V semiconductors under pressure are drawn.
RESUMEN
Solid bromine has been studied by x-ray absorption spectroscopy experiments up to a maximum pressure of 75 GPa. The data analysis of the extended fine structure reveals that the intramolecular distance first increases, reaching its maximum value at 25+/-5 GPa. From this value the intramolecular distance abruptly begins to decrease evidencing a nonpreviously observed phase transformation taking place at 25+/-5 GPa. A maximum variation of 0.08 A is observed at 65+/-5 GPa where again a phase transition occurs. This last transformation could correspond with the recently observed change to an incommensurate modulated phase. We discuss the possible generalization of the observed new phase transition at 25+/-5 GPa to the case of the other halogens.
RESUMEN
Using x-ray absorption spectroscopy, we have studied the effect of pressure on femtometer-scale bond strain due to anisotropic magnetostriction in a thin FeCo film. At 7 GPa local magnetostrictive strain is found to be larger than at ambient, in agreement with spin-polarized ab initio electronic structure calculations, but contrary to the expected effect of compression on bond stiffness. The availability of high pressure data on local magnetostrictive strain opens new capabilities for validating theoretical predictions and can lead to the development of materials with the desired properties.
