Influence of preparation method on the performance of vanadia-niobia catalysts for the oxidative dehydrogenation of propane

The influence of various preparation methods on the performance of V-Nb-0 catalysts has been investigated. It was found that the activity and selectivity of a vanadium site depend on the nature of the neighbouring atoms. Vanadium neighbours provide activity, while niobium neighbours provide selectivity. Careful preparation of these catalysts ensures a homogeneous distribution and good mixing of the vanadium and niobium. It was also found that the vanadium becomes mobile upon reduction and this results in better distribution of vanadium in used catalysts

Lattice distortions in coccolith calcite crystals originate from occlusion of biomacromolecules

During biomineralization, organisms control the formation and morphology of a mineral using biomacromolecules. The biomacromolecules that most strongly interact with the growing crystals frequently get occluded within. Such an observation has been recently obtained for the calcium carbonate producing coccolithophore species Pleurochrysis carterae. Coccolithophores are unicellular algae that produce calcified scales built from complex-shaped calcite crystals, termed coccoliths. It is unclear how widespread the phenomenon of biomacromolecular occlusion within calcite crystals is in calcifying haptophytes such as coccolithophores. Here, the coccoliths of biological replicates of the bloom forming Emiliania huxleyi are compared with that of Pleurochrysis carterae, two species with different coccolith morphologies and crystal growth mechanisms. From high-resolution synchrotron X-ray diffraction, changes in the lattice parameters of coccolith calcite, after heating to 450 °C, are observed and associated with macrostrain originating from occluded biomacromolecules. We propose a mechanism governing the biomacromolecules’ interaction with the growing coccolith crystals and their likely origin

Mapping of individual dislocations with dark-field X-ray microscopy

This article presents an X-ray microscopy approach for mapping deeply embedded dislocations in three dimensions using a monochromatic beam with a low divergence. Magnified images are acquired by inserting an X-ray objective lens in the diffracted beam. The strain fields close to the core of dislocations give rise to scattering at angles where weak beam conditions are obtained. Analytical expressions are derived for the image contrast. While the use of the objective implies an integration over two directions in reciprocal space, scanning an aperture in the back focal plane of the microscope allows a reciprocal-space resolution of DQ/Q < 5 x10^-5 in all directions, ultimately enabling highprecision mapping of lattice strain and tilt. The approach is demonstrated on three types of samples: a multi-scale study of a large diamond crystal in transmission, magnified section topography on a 140 mm-thick SrTiO3 sample and a reflection study of misfit dislocations in a 120 nm-thick BiFeO3 film epitaxially grown on a thick substrate. With optimal contrast, the half-widths at half-maximum of the dislocation lines are 200 nm

Diffraction tomography and Rietveld refinement of a hydroxyapatite bone phantom

A model sample consisting of two different hydroxyapatite (hAp) powders was used as a bone phantom to investigate the extent to which X-ray diffraction tomography could map differences in hAp lattice constants and crystallite size. The diffraction data were collected at beamline 1-ID, the Advanced Photon Source, using monochromatic 65 keV X-radiation, a 25 x 25 microm pinhole beam and translation/rotation data collection. The diffraction pattern was reconstructed for each volume element (voxel) in the sample, and Rietveld refinement was used to determine the hAp lattice constants. The crystallite size for each voxel was also determined from the 00.2 hAp diffraction peak width. The results clearly show that differences between hAp powders could be measured with diffraction tomography

Mapping of individual dislocations with dark-field X-ray microscopy

International audienceThis article presents an X-ray microscopy approach for mapping deeply embedded dislocations in three dimensions using a monochromatic beam with a low divergence. Magnified images are acquired by inserting an X-ray objective lens in the diffracted beam. The strain fields close to the core of dislocations give rise to scattering at angles where weak beam conditions are obtained. Analytical expressions are derived for the image contrast. While the use of the objective implies an integration over two directions in reciprocal space, scanning an aperture in the back focal plane of the microscope allows a reciprocal-space resolution of ÁQ/Q < 5 Â 10 À5 in all directions, ultimately enabling high-precision mapping of lattice strain and tilt. The approach is demonstrated on three types of samples: a multi-scale study of a large diamond crystal in transmission, magnified section topography on a 140 mm-thick SrTiO 3 sample and a reflection study of misfit dislocations in a 120 nm-thick BiFeO 3 film epitaxially grown on a thick substrate. With optimal contrast, the half-widths at half-maximum of the dislocation lines are 200 nm

Ordering of protein and water molecules at their interfaces with chitin nano crystals

Synchrotron X-ray diffraction was applied to study the structure of biogenic α-chitin crystals composing the tendon of the spider Cupiennius salei. Measurements were carried out on pristine chitin crystals stabilized by proteins and water, as well as after their deproteinization and dehydration. We found substantial shifts (up to Δq/q = 9% in the wave vector q-space) in the (020) diffraction peak position between intact and purified chitin samples. However, chitin lattice parameters extracted from the set of reflections (hkl), which did not contain the (020)-reflection, showed no systematic variation between the pristine and the processed samples. The observed shifts in the (020) peak position are discussed in terms of the ordering-induced modulation of the protein and water electron density near the surface of the ultra-thin chitin fibrils, due to strong protein/chitin and water/chitin interactions. The extracted modulation periods can be used as a quantitative parameter characterizing the interaction length