A versatile X-ray phase retarder for lock-in XMCD measurements.

X-ray magnetic circular dichroism (XMCD) is a technique commonly used to probe magnetic properties of materials with element and orbital selectivity, which requires the use of circularly polarized (CP) X-rays. It is possible to accomplish XMCD experiments with fixed CP and alternating the magnetic field orientation, but most reliable data are obtained when alternating the magnetization orientation and the polarization between right and left helicities. A versatile strategy has been developed to perform XMCD experiments using a hard X-ray quarter-wave plate, at both polychromatic dispersive and conventional monochromatic optics, in combination with synchronous data acquisition. The switching frequency waveform is fed into a lock-in amplifier to detect and amplify the XMCD signal. The results on a reference sample demonstrate an improvement in data quality and acquisition time. The instrumentation successfully generated 98% of CP X-rays switching the beam helicity at 13 Hz, with the possibility of faster helicity switching once it is installed at the new Brazilian fourth-generation source, SIRIUS.

Evolution of electronic and magnetic properties of nominal magnetite nanoparticles at high pressure probed by x-ray absorption and emission techniques.

We present a study of electronic and magnetic properties of nominal magnetite nanoparticles (NPs) (~6 nm) at high pressure in the presence of silicon pressure medium using x-ray absorption near edge structure (XANES), x-ray magnetic circular dichroism (XMCD) and non-resonant x-ray emission spectroscopy (XES). XANES data show a reduction of Fe charge state, a change in local environment around Fe at tetrahedral sites, and a reduced occupation of Fe 4p  orbitals, not seen in previous pressure studies of bulk magnetite. XMCD data show a continuous magnetic moment reduction of ~50% between ambient pressure and 20 GPa, similar to what was observed in previous bulk magnetite studies. XES spectra of NPs indicate a gradual change in spin configuration away from the high-spin state consistent with a postulated charge transfer from Fe 4p  to 3d states and the observed reduction in XMCD signal. Taken together, the results point to substantial differences in the response of electronic and magnetic properties of the nano-counterparts of bulk magnetite at high pressure.

In-depth understanding of the relation between CuAlO2 particle size and morphology for ozone gas sensor detection at a nanoscale level.

A morphology-dependent nanomaterial for energy and environment applications is one of the key challenges for materials science and technology. In this study, we investigate the effect of the particle size of CuAlO2 nanostructures prepared through the facile and hydrothermal process to detect ozone gas. Phase analysis and structural information were obtained using X-ray diffraction and micro-Raman studies. The chemical states of CuAlO2 atomic species were determined by X-ray photoelectron spectroscopy. Electron microscopy images revealed the flower and hexagonal shape constituted of pentagon and oval CuAlO2 nanoparticles with average size ∼40 and 80 nm. The specific surface area was measured and found to be 59.8 and 70.8 m(2) g(-1), respectively. The developed CuAlO2 nanostructures not only possess unique morphology but also influence the ozone gas sensing performance. Among the two structures, CuAlO2, with hexagonal morphology, exhibited superior ozone detection for 200 ppb at 250 °C, with a response and good recovery time of 25 and 39 s compared to the flower morphology (28 and 69 s). These results show that not only does the morphology play an major role but also the particle size, surface area, gas adsorption/desorption, and grain-grain contact, as proposed in the gas sensing mechanism. Finally, we consider CuAlO2 material as a good candidate for environment monitoring applications.