Orientation relations during the α-ω phase transition of zirconium: in situ texture observations at high pressure and temperature.

Transition metals Ti, Zr, and Hf have a hexagonal close-packed structure (α) at ambient conditions, but undergo phase transformations with increasing temperature and pressure. Of particular significance is the high-pressure hexagonal ω phase which is brittle compared to the α phase. There has been a long debate about transformation mechanisms and orientation relations between the two crystal structures. Here we present the first high pressure experiments with in situ synchrotron x-ray diffraction texture studies on polycrystalline aggregates. We follow crystal orientation changes in Zr, confirming the original suggestion by Silcock for an α→ω martensitic transition for Ti, with (0001)(α)||(1120)(ω), and a remarkable orientation memory when ω reverts back to α.

Nanostructure of calcium silicate hydrates in cements.

Calcium silicate hydrate (CSH) is the major volume phase in the matrix of Portland cement concrete. Total x-ray scattering measurements with synchrotron x rays on synthetic CSH(I) shows nanocrystalline ordering with a particle diameter of 3.5(5) nm, similar to a size-broadened 1.1 nm tobermorite crystal structure. The CSH component in hydrated tricalcium silicate is found to be similar to CSH(I). Only a slight bend and additional disorder within the CaO sheets is required to explain its nanocrystalline structure.

Deformation experiments in the diamond-anvil cell: texture in copper to 30 GPa.

The combination of the diamond-anvil cell, synchrotron x-ray diffraction in radial geometry and simultaneous Rietveld refinement with texture analysis allows us to quantitatively investigate the plastic deformation behaviour of materials at very high pressures. Our study of copper to 30 GPa shows in ideal experimental geometry a [110] fibre texture component, as is typical for axial compression of soft face centred cubic metals. Locally a plane strain texture develops which is energetically favoured (curling). A transition from compressional to plane strain/pure shear texture can be monitored by analysing individual images taken at different positions in the diamond cell.

Deformation textures produced in diamond anvil experiments, analysed in radial diffraction geometry.

Diamond anvil cells may not only impose pressure upon a sample but also a compressive stress that produces elastic and plastic deformation of polycrystalline samples. The plastic deformation may result in texture development if the material deforms by slip or mechanical twinning, or if grains have a non-equiaxed shape. In radial diffraction geometry, texture is revealed by variation of intensity along Debye rings relative to the compression direction. Diffraction images (obtained by CCD or image plate) can be used to extract quantitative texture information. Currently the most elegant and powerful method is a modified Rietveld technique as implemented in the software package MAUD. From texture data one can evaluate the homogeneity of strain in a diamond anvil cell, the strain magnitude and deformation mechanisms, the latter by comparing observed texture patterns with results from polycrystal plasticity simulations. Some examples such as olivine, magnesiowuestite, MgSiO(3) perovskite and ε-iron are discussed.

Crystallographic texture for tube and plate of the superelastic/shape-memory alloy Nitinol used for endovascular stents.

The superelastic/shape-memory material, Nitinol, an approximately equiatomic alloy of Ni and Ti, is rapidly becoming one of the most important metallic implant materials in the biomedical industry, in particular for the manufacture of endovascular stents. As such stents are invariably laser-machined from Nitinol tubes or sheets rolled into tubes, it is important to fully understand the physical phenomena that may affect the mechanical behavior of this material. With tubing and plate, one major issue is crystallographic texture, which can play a key role in influencing the mechanical properties of Nitinol. In this article, we present a study on how geometry and heat treatment can affect the texture of Nitinol, with specific quantification of the texture of Nitinol tube used for the production of endovascular stents.

Texturing of the Earth's inner core by Maxwell stresses.

Elastic anisotropy in the Earth's inner core has been attributed to a preferred lattice orientation, which may be acquired during solidification of the inner core or developed subsequent to solidification as a result of plastic deformation. But solidification texturing alone cannot explain the observed depth dependence of anisotropy, and previous suggestions for possible deformation processes have all relied on radial flow, which is inhibited by thermal and chemical stratification. Here we investigate the development of anisotropy as the inner core deforms plastically under the influence of electromagnetic (Maxwell) shear stresses. We estimate the flow caused by a representative magnetic field using polycrystal plasticity simulations for epsilon-iron, where the imposed deformation is accommodated by basal and prismatic slip. We find that individual grains in an initially random polycrystal become preferentially oriented with their c axes parallel to the equatorial plane. This pattern is accentuated if deformation is accompanied by recrystallization. Using the single-crystal elastic properties of epsilon-iron at core pressure and temperature, we average over the simulated orientation distribution to obtain a pattern of elastic anisotropy which is similar to that observed seismologically.

Crystal alignment of carbonated apatite in bone and calcified tendon: results from quantitative texture analysis.

Calcified tissue contains collagen associated with minute crystallites of carbonated apatite. In this study, methods of quantitative X-ray texture analysis were used to determine the orientation distribution and texture strength of apatite in a calcified turkey tendon and in trabecular and cortical regions of osteonal bovine ankle bone (metacarpus). To resolve local heterogeneity, a 2 or 10 microm synchrotron microfocus X-ray beam (lambda = 0.78 A) was employed. Both samples revealed a strong texture. In the case of turkey tendon, 12 times more c axes of hexagonal apatite were parallel to the fibril axis than perpendicular, and a axes had rotational freedom about the c axis. In bovine bone, the orientation density of the c axes was three times higher parallel to the surface of collagen fibrils than perpendicular to it, and there was no preferential alignment with respect to the long axis of the bone (fiber texture). Whereas half of the apatite crystallites were strongly oriented, the remaining half had a random orientation distribution. The synchrotron X-ray texture results were consistent with previous analyses of mineral orientation in calcified tissues by conventional X-ray and neutron diffraction and electron microscopy, but gave, for the first time, a quantitative description.

Laue orientation imaging.

Advantage was taken of the highly focused X-ray beam (10-30 microm) and the broad white spectrum of synchrotron X-rays at the ESRF for automatic recording of Laue patterns from polycrystals and extraction of orientation information. The procedure used is similar to that applied for electron-backscattering patterns in the scanning electron microscope and provides data for local orientation mapping used in texture analysis. Laue patterns are obtained from a thin slice of material in transmission and recorded with a CCD detector. The Laue geometry is converted into a gnomonic projection in which co-zonal reflections lie on straight lines. On applying the Hough transform these lines are merged into a single point, which is recognized by the computer and assigned zone indices [uvw] by comparison with a table of interzonal angles. From the angular positions of several [uvw] the crystal orientation is calculated. The method is illustrated for the orthorhombic magnesium silicate olivine.

3D structure determination from electron-microscope images: electron crystallography of staurolite.

Resolution of better than 2 A has been obtained in many crystals by high-resolution electron microscopy. Although this resolution is sufficient to resolve interatomic spacings, structures are traditionally interpreted by comparing experimental images with contrast calculations. A drawback of this method is that images are 2D projections in which information is invariably obscured by overlap of atoms. 3D electron crystallography, developed by biophysicists to study proteins, has been used to investigate the crystal structure of staurolite. Amplitudes and phases of structure factors are obtained experimentally from high-resolution images (JEOL ARM 1000 at the National Center for Electron Microscopy at LBL), taken in different directions from thin regions where dynamic scattering is minimal. From images in five orientations (containing 59 independent reflections to a resolution of 1.38 A), a 3D electron potential map is constructed which resolves clearly all cations (Al, Si, Fe, including those with partial occupancy) and all O atoms. This method has great potential in crystal structure determinations of small domains in heterogeneous crystals which are inaccessible to X-ray analysis. It is estimated that 3D structure determinations should be possible on regions only about ten unit cells wide and should resolve not only atom positions but also site occupancies. The method is also applicable to space-group determination.

Sequential Basal faults in devonian dolomite, nopah range, death valley area, california.

Dolomite crystals from the Lost Burro Formation (Devonian) in the Nopah Range, eastern California, display basal stacking disorder as evidenced by transmission electron microscopy. Satellites in electron diffraction patterns indicate that stacking of anions and cations is different from that in ideal dolomite. This example conforms to the model of basal defects proposed by Goldsmith and Graf in 1958 to explain nonstoichiometry in dolomite. This dolomite from the Nopah Range was formed by deep burial replacement of micritic limestone, and its peculiar superstructure is tentatively attributed to the late diagenetic conditions during replacement.

Chrysotile asbestos in a California recreational area.

Dustfall along roads and trails being used recreationally in the Clear Creek area of San Benito County, California, located in the New Idria serpentinite, was found to be 90 percent or more chrysotile asbestos. Personal samplers worn by motorcyclists using one of the trails showed concentrations of airborne fibers ranging from 0.3 to 5.3 fibers per milliliter, according to methods prescribed for monitoring occupational exposures. The present workplace standard for brief exposures to asbestos is 10 fibers per milliliter; 5 fibers per milliliter is the proposed standard. The average total dust concentration estimated from personal samplers was approximately 20 milligrams per cubic meter of roughly 90 percent chrysotile. To our knowledge, this is the first demonstration of asbestos exposures of this magnitude, in size ranges known to be pathogenic, resulting from natural deposits not associated with mining, milling, or industrial use.

X-ray fabric analysis of hot-worked and annealed flint.

Two specimens of flint described by Green have been subjected to intensive x-ray fabric analysis. The specimen compressed in the beta-quartz field recrystallized to a fabric with a strong maximum of c-axes parallel to the direction of compression and a weaker equatorial concentration perpendicular to the axis of compression. Annealing of a similar specimen eliminated the equatorial concentration and strengthened the axial concentration six- to eightfold. In the latter specimen, the fabric determined by x-ray analysis agrees closely with Green's optically measured fabric. It is possible to obtain c-axis fabrics directly from the very weak 0003 diffraction peak.