An improved laboratory-based x-ray absorption fine structure and x-ray emission spectrometer for analytical applications in materials chemistry research

X-ray absorption fine structure (XAFS) and x-ray emission spectroscopy (XES) are advanced x-ray spectroscopies that impact a wide range of disciplines. However, unlike the majority of other spectroscopic methods, XAFS and XES are accompanied by an unusual access model, wherein the dominant use of the technique is for premier research studies at world-class facilities, i.e., synchrotron x-ray light sources. In this paper, we report the design and performance of an improved XAFS and XES spectrometer based on the general conceptual design of Seidler et al. [Rev. Sci. Instrum. 85, 113906 (2014)]. New developments include reduced mechanical degrees of freedom, much-increased flux, and a wider Bragg angle range to enable extended x-ray absorption fine structure (EXAFS) measurement and analysis for the first time with this type of modern laboratory XAFS configuration. This instrument enables a new class of routine applications that are incompatible with the mission and access model of the synchrotron light sources. To illustrate this, we provide numerous examples of x-ray absorption near edge structure (XANES), EXAFS, and XES results for a variety of problems and energy ranges. Highlights include XAFS and XES measurements of battery electrode materials, EXAFS of Ni with full modeling of results to validate monochromator performance, valence-to-core XES for 3d transition metal compounds, and uranium XANES and XES for different oxidation states. Taken en masse, these results further support the growing perspective that modern laboratory-based XAFS and XES have the potential to develop a new branch of analytical chemistry

Vortex microavalanches in superconducting Pb thin films

Local magnetization measurements on 100 nm type-II superconducting Pb thin films show that flux penetration changes qualitatively with temperature. Small flux jumps at the lowest temperatures gradually increase in size, then disappear near T = 0.7Tc. Comparison with other experiments suggests that the avalanches correspond to dendritic flux protrusions. Reproducibility of the first flux jumps in a decreasing magnetic field indicates a role for defect structure in determining avalanches. We also find a temperature-independent final magnetization after flux jumps, analogous to the angle of repose of a sandpile.Comment: 6 pages, 5 figure

Analysis by x-ray microtomography of a granular packing undergoing compaction

Several acquisitions of X-ray microtomography have been performed on a beads packing while it compacts under vertical vibrations. An image analysis allows to study the evolution of the packing structure during its progressive densification. In particular, the volume distribution of the pores reveals a large tail, compatible to an exponential law, which slowly reduces as the system gets more compact. This is quite consistent, for large pores, with the free volume theory. These results are also in very good agreement with those obtained by a previous numerical model of granular compaction.Comment: 4 pages, 4 figures. Latex (revtex4). to be published in Phys. Rev.

1/f noise studies in uncooled narrow gap Hg1−xCdxTe non-equilibrium diodes

We have studied the 1/f noise current in narrow gap semiconductor heterostructure diodes fabricated in mercury cadmium telluride (HgCdTe) and designed to operate in a non-equilibrium mode at room temperature. HgCdTe heterostructure diodes exhibit Auger suppression giving current-voltage characteristics with high peak-to-valley ratios (up to 35), and low extracted saturation current densities (e.g., 20 Acnr−2 at 10 pm at 295K) but high 1/f knee frequencies (e.g., 100 MHz at 10 µm at 295K). A comparison is made with the noise levels found in room temperature non-equilibrium mode heterostructure InAlSb/InSb diodes. The devices are being used at high frequencies for CO2 laser heterodyne detector demonstrators. For the devices to be useful in low frame-rate imaging arrays, the 1/f noise level must be sufficiently low that the signal is not swamped. Ideally, the knee frequency should be below the frame rate. The relationship between the noise current and reverse bias voltage, current density, and temperature will be examined in order to attempt to identify the principal 1/f generation mechanisms

Observations of continuum depression in warm dense matter with X-ray thomson scattering

Detailed measurements of the electron densities, temperatures, and ionization states of compressed CH shells approaching pressures of 50 Mbar are achieved with spectrally resolved x-ray scattering. Laser-produced 9 keV x-rays probe the plasma during the transient state of three-shock coalescence. High signal-to-noise x-ray scattering spectra show direct evidence of continuum depression in highly degenerate warm dense matter states with electron densities ne>1024cm-3. The measured densities and temperatures agree well with radiation-hydrodynamic modeling when accounting for continuum lowering in calculations that employ detailed configuration accounting

Aeromonas species isolated from PINTADO fish (Pseudoplatystoma sp): virulence factors and drug susceptibility

Aeromonas has been described as an emergent foodborne pathogen of increasing importance. In this study, we report that 48% of 50 Pintado fish samples collected at the retail market of São Paulo city were positive for Aeromonas sp, as detected by the direct plating method. When the presence/absence method was used, the positivity was 42%. A. caviae was the most frequent species, followed by A. hydrophila and A. sobria. Production of cytotoxic enterotoxin, observed in suckling mouse assay, was detected in 67% of A. sobria strains, in 60% of A. hydrophila strains and in 40% of A. caviae strains. In vitro tests, performed with HEp-2 cells, showed that 88% of A. hydrophila, 27% of A. sobria and 13% of A. caviae strains were positive for this toxin. The in vivo production of cytotonic enterotoxin, tested after heating the filtrates at 56ºC for 20 minutes, was detected in 17% of A. sobria, in 10% of A. caviae and in none of A. hydrophila strains in vivo. All analyzed strains did not alter HEp-2 cells. 20% and 16% of A. sobria and A. caviae isolates, respectively, presented capacity to adhere to HEp-2 cells. In counterpart, invasion of HEp-2 cells was not observed in any isolate. The Aeromonas isolates were sensitive to the majority of the antimicrobiol agents tested.<br>Bactérias do gênero Aeromonas têm sido descritas como patógenos emergentes de importância crescente em alimentos. Neste estudo, relatamos que 48% das amostras de peixe "Pintado" coletado no comércio de São Paulo, foram positivas para Aeromonas sp quando isoladas pelo método de plaqueamento direto. Quando o método Presença/Ausência foi utilizado, a porcentagem de positividade foi de 42%. A. caviae foi a espécie mais freqüente, seguida por A. hydrophila e A. sobria. Produção de enterotoxina citotóxica, determinada em camundongos recém-nascidos, foi observada em 67% das cepas de A. sobria, em 60% das de A. hydrophila e em 40% das de A. caviae. No teste in vitro em células HEp- 88% das cepas de A. hydrophila, 27% das cepas de A. sobria e 13% das cepas de A. caviae revelaram-se positivas. Com relação a produção de enterotoxina citotônica, testada após o aquecimento do sobrenadante a 56ºC por 20 minutos, 17% das cepas de A. sobria, 10% das de A. caviae e nenhuma das de A. hydrophila foram positivas in vivo e para todas as cepas analisadas, os testes foram negativos em cultura de célula HEp-2. Quanto a capacidade de adesão, 20% das 5 cepas de A. sobria e 16% das 20 cepas de A. caviae aderiram a células HEp-2. A capacidade de invasão em células HEp-2 não foi detectada em nenhuma das cepas testadas. As cepas isoladas foram sensíveis a maior parte dos antimicrobianos testados