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Cross-sections of calcitic prismatic layers in mollusk shells, cut perpendicular to growth direction, reveal well-defined polygonal shapes of individual "grains" clearly visible by light and electron microscopy. For several kinds of shells, it was shown that the average number of edges in an individual prism approaches six during the growth process. Taking into account the rhombohedral symmetry of calcite, often presented in hexagonal axes, all this led to the long-standing opinion that calcitic prisms grow along the c-axis of calcite. In this paper, using X-ray diffraction and electron backscatter diffraction (EBSD), we unambiguously show that calcitic prisms in pearl oyster Pinctada margaritifera predominantly grow perpendicular to the c-axis. The obtained results imply that the hexagon-like habitus of growing crystallites may be not necessarily connected to calcite crystallography and, therefore, other factors should be taken into consideration. We analyze this phenomenon by comparing the organic contents in Pinctada margaritifera and Pinna nobilis shells, the later revealing regular growth of calcitic prisms along the c-axis.

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Using single-crystal x-ray diffraction, we found a formerly unknown twin form in calcite crystals grown from solution to which a mollusc shell-derived 17-kDa protein, Caspartin, was added. This intracrystalline protein was extracted from the calcitic prisms of the Pinna nobilis shells. The observed twin form is characterized by the twinning plane of the (108)-type, which is in addition to the known four twin laws of calcite identified during 150 years of investigations. The established twin forms in calcite have twinning planes of the (001)-, (012)-, (104)-, and (018)-types. Our discovery provides additional evidence on the crucial role of biological macromolecules in biomineralization.

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We performed X-ray photoemission electron microscopy (XPEEM) measurements at the Nanospectroscopy Beamline of the synchrotron light source ELETTRA, Trieste, Italy, to demonstrate the principal possibility of imaging ferroelectric thin films by low-energy photoelectrons. Due to the insulating properties of ferroelectric films, severe surface charging was the major experimental challenge to overcome. This was achieved by grounding an array of gold inter-digital electrodes (with 5 microm blank intervals between them) deposited on top of the films. The images taken with BaTiO(3) films revealed 50-100 nm-sized holes (material discontinuities) on the surface, an observation confirmed by high-resolution scanning electron microscopy (HRSEM). Finer details, e.g. a granular structure, which has been resolved with HRSEM, could not be observed in the XPEEM images. Our measurements indicate that despite some residual charging, a 50 nm lateral resolution can be achieved in XPEEM measurements with ferroelectric films.

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High-resolution synchrotron powder diffraction measurements were carried out at the 32-ID beamline of the Advanced Photon Source of Argonne National Laboratory in order to clarify the structure of geological aragonite, a widely abundant polymorph of CaCO(3). The investigated crystals were practically free of impurity atoms, as measured by wavelength-dispersive X-ray spectroscopy in scanning electron microscopy. A superior quality of diffraction data was achieved by using the 11-channel 111 Si multi-analyzer of the diffracted beam. Applying the Rietveld refinement procedure to the high-resolution diffraction spectra, we were able to extract the aragonite lattice parameters with an accuracy of about 20 p.p.m. The data obtained unambiguously confirm that pure aragonite crystals have orthorhombic symmetry.

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An energy-variable synchrotron diffraction technique is being established as a novel method for the depth-resolved measurement of residual strains in polycrystalline structures. An analytic expression for the diffraction profile is obtained by taking into account the instrument misalignment, change of the height of an incident X-ray beam with energy, and penetration of X-rays into the sample depth. It is shown that the maximum diffraction intensity recorded in the detector is coming from a certain depth beneath the surface of the sample, the depth being energy-dependent. This finding opens a way for precise strain measurements with high depth resolution by changing the X-ray energy in small enough steps. An experimental example, residual strain measurements across an alumina/zirconia multilayer, demonstrates the capability of the method.

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We report on direct imaging, by means of stroboscopic x-ray topography, of phonon-induced dislocation vibrations. X-ray images taken from LiNbO3 crystals excited by 0.58 GHz surface acoustic waves, showed individual acoustic wave fronts as well as their distortions when crossing the dislocation line. The observed contrast is well explained by considering the dynamic deformation field of vibrating dislocation. Comparing simulated deformation maps and x-ray images permitted determination of the local velocities of vibrating dislocations and their viscosity coefficients. We found unexpectedly high velocity values (not far from the speed of sound) and extremely low viscosity coefficients, 2-3 orders of magnitude lower than previously measured in ductile materials.

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We show that intrinsic dislocations in brittle single crystals can be a source of strong local perturbations along the crack path. A theoretical model was developed which predicts substantial crack front deflections. Investigating the crack surfaces in Si crystals with induced dislocation density of 10(9)-10(10) cm(-2) revealed a significant amount of crack front perturbations in the form of V-shaped grooves, which were completely missing in dislocation-free Si specimens. The measured depths of the perturbations were in the range of 2-20 nm and in excellent agreement with the theoretical model.

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Stroboscopic X-ray topography at the synchrotron beam line was used to visualize the propagation of a 580 MHz surface acoustic waves (SAW) in LiNbO3 crystals. For this purpose, the X-ray bursts coming from the synchrotron storage ring with periodicity of 5.68 MHz were synchronized with the SAW frequency in a phase-locked mode. This method allowed us to "stop" the SAW in time and to observe the X-ray diffraction contrast caused by the dynamic deformation field of SAW. The X-ray topographic images showed well-resolved individual acoustic wave fronts of 6 microm SAW as well as their distortions due to SAW scattering by linear dislocations. Some of the images revealed an exceptional contrast of the concentric rings about the dislocation line, which is caused by coherent interaction of the secondary elastic waves. This contrast is similar to the Fresnel zones in optics, and this conclusion is confirmed by direct summation of secondary waves emitted by local elements of a vibrating dislocation string.

RESUMEN

X-ray pulses from the Advanced Photon Source at Argonne National Laboratory were used to measure the speed of X-rays in the energy range between 21 and 60 keV. An LiNbO(3)-based 0.58 GHz surface acoustic wave device served as a temporal analyzer in the stroboscopic time-resolved diffraction measurements. By synchronizing the surface acoustic wave excitation and periodic X-ray illumination of the LiNbO(3) crystal, the temporal modifications in the LiNbO(3) diffraction profiles could be followed and the time points of X-ray arrivals at the analyzer position for different analyzer to storage ring distances determined. The speed of the X-rays was determined as the ratio of measured spacings and corresponding delay time intervals. Within the experimental error bars, the obtained X-ray velocities converged to the tabulated constant for the speed of light in a vacuum.