Substitution site and effects on magnetism in Sr-for-Ca substituted CaBaCo4O7

Under a Creative Commons Attribution (CC BY) license.-- et al.Cationic substitutions in the novel magnetoelectric compound CaBaCo4O7 lead to profound changes in its magnetic and electric behaviors. In this work, we present a structural study of the isovalent substitution Sr-for-Ca in CaBaCo4O7. X-ray diffraction, as well as neutron powder diffraction experiments, are reported for a series of samples Ca1- xSrxBaCo4O7 with 0 ≤ x ≤ 0.10. Special emphasis is given to the identification of the substitution site, as Sr has also been reported to substitute for Ba in this crystal structure. The solubility limit for Sr at the Ca site is shown to be at x ≃ 0.08. The variation of lattice constants with Sr-doping firmly supports the Sr-for-Ca substitution. Rietveld refinements of the Sr-substituted samples are presented, and used as starting point to analyse the local structure around Sr by means of X-ray absorption spectroscopy at the Sr K-edge. Both the near-edge absorption and the extended absorption fine-structure confirm the substitution of Sr for Ca, giving definite support to the proposed nominal formula. In addition, macroscopic magnetization measurements are presented which reveal the striking effects of Sr-substitution over the magnetic landscape of this puzzling compound.This work is part of a research project supported by Agencia Nacional de Promoción Científica y Tecnológica (Argentina), under Grant No. PICT-2011-0752, CONICET under Grant No. PIP 490 2012-2014, and Universidad Nacional de Cuyo. We acknowledge Soleil synchrotron for the beamtime allocation and the MinCyT-Soleil collaboration project for the financial support. We also acknowledge ILL and its staff for the beamtime allocation and technical assistance as well as the MinCyT of Argentina for funding the trip to perform the experiments. G.A. and J.C. thank the CONICET-CSIC program for scientific visits and Grant No. MAT2011-27233-C02-02.Peer Reviewe

In situ multi‐axial loading frame to probe elastomers using X‐ray scattering

International audienceAn in situ tensile-shear loading device has been designed to study elastomer crystallization using synchrotron X‐ray scattering at the Synchrotron Soleil on the DiffAbs beamline. Elastomer tape specimens of thickness 2 mm can be elongated by up to 500% in the longitudinal direction and sheared by up to 200% in the transverse direction. The device is fully automated and plugged into the TANGO control system of the beamline allowing synchronization between acquisition and loading sequences. Experimental results revealing the evolution of crystallization peaks under load are presented for several tension/shear loading sequences

Combined synchrotron X-rays and image correlation analyses of biaxially deformed W/Cu nanocomposite thin films on Kapton

International audienceAbstract In-situ biaxial tensile tests within the elastic domain were conducted with W/Cu nanocomposite thin films deposited on a polyimide cruciform substrate thanks to a biaxial testing machine developed on the DiffAbs beamline at SOLEIL synchrotron. The mechanical behavior of the nanocomposite was characterized at the micro-scale and the macro-scale using simultaneously synchrotron X-ray diffraction and digital image correlation techniques. Strain analyses for equi-biaxial and non equi-biaxial loading paths have been performed. The results show that the two strain measurements match to within 1 × 10-4 in the elastic domain for strain levels less than 0.3% and for both loading paths

Microsecond time-resolved X-ray diffraction for the investigation of fatigue behavior during ultrasonic fatigue loading

International audienceA new method based on time-resolved X-ray diffraction is proposed in order to measure the elastic strain and stress during ultrasonic fatigue loading experiments. Pure Cu was chosen as an example material for the experiments using a 20 kHz ultrasonic fatigue machine mounted on the six-circle diffractometer available at the DiffAbs beamline on the SOLEIL synchrotron facility in France. A two-dimensional hybrid pixel X-ray detector (XPAD3.2) was triggered by the strain gage signal in a synchronous data acquisition scheme (pump–probe-like). The method enables studying loading cycles with a period of 50 µs, achieving a temporal resolution of 1 µs. This allows a precise reconstruction of the diffraction patterns during the loading cycles. From the diffraction patterns, the position of the peaks, their shifts and their respective broadening can be deduced. The diffraction peak shift allows the elastic lattice strain to be estimated with a resolution of ∼10−5. Stress is calculated by the self-consistent scale-transition model through which the elastic response of the material is estimated. The amplitudes of the cyclic stresses range from 40 to 120 MPa and vary linearly with respect to the displacement applied by the ultrasonic machine. Moreover, the experimental results highlight an increase of the diffraction peak broadening with the number of applied cycles

Substitution site and effects on magnetism in Sr-for-Ca substituted CaBaCo4O7

Cationic substitutions in the novel magnetoelectric compound CaBaCo4O7 lead to profound changes in its magnetic and electric behaviors. In this work, we present a structural study of the isovalent substitution Sr-for-Ca in CaBaCo4O7. X-ray diffraction, as well as neutron powder diffraction experiments, are reported for a series of samples Ca1- xSrxBaCo4O7 with 0 = x = 0.10. Special emphasis is given to the identification of the substitution site, as Sr has also been reported to substitute for Ba in this crystal structure. The solubility limit for Sr at the Ca site is shown to be at x ¿ 0.08. The variation of lattice constants with Sr-doping firmly supports the Sr-for-Ca substitution. Rietveld refinements of the Sr-substituted samples are presented, and used as starting point to analyse the local structure around Sr by means of X-ray absorption spectroscopy at the Sr K-edge. Both the near-edge absorption and the extended absorption fine-structure confirm the substitution of Sr for Ca, giving definite support to the proposed nominal formula. In addition, macroscopic magnetization measurements are presented which reveal the striking effects of Sr-substitution over the magnetic landscape of this puzzling compound

Strain induced crystallization and melting of natural rubber during dynamic cycles

Strain-induced crystallization (SIC) of natural rubber (NR) is studied during dynamic cycles at high frequencies (with equivalent strain rates ranging from 7.2 s-1 to 290 s-1). The testing parameters are varied: the frequency, the temperature and the stretching ratio domain. It is found that an increase of the frequency leads to an unexpected form of the CI–¿ curve, with a decrease of the crystallinity during both loading and unloading steps of the cycle. Nevertheless, the interpretation of the curves needs to take into account several phenomena such as (i) instability of the crystallites generated during the loading step, which increases with the frequency, (ii) the memory of the previous alignment of the chains, which depends on the minimum stretching ratio of the cycle ¿min and the frequency, and (iii) self-heating which makes the crystallite nucleation more difficult and their melting easier. Thus, when the stretching ratio domain is above the expected stretching ratio at complete melting ¿melt, the combination of these phenomena, at high frequencies, leads to unexpected results such as complete melting at ¿min, and hysteresis in the CI–¿ curves.Peer ReviewedPostprint (author's final draft

Combination of X-ray synchrotron radiation techniques to gather information for clinicians

International audienceAmong the different techniques specific to synchrotron radiation, the combination of X-ray absorption spectroscopy with X-ray scattering experiments is a powerful tool to characterize samples with a capability to gather structural and electronic information at the cellular level. In the present contribution, selected examples making use of such techniques, point out as well the information that one can have access to. Via the presentation of the physicochemical data, this paper focuses on displaying the information that has a significant clinical character

Visualizing mineralization processes and fossil anatomy using synchronous synchrotron X-ray fluorescence and X-ray diffraction mapping

International audienc