Comparison of quartz crystallographic preferred orientations identified with optical fabric analysis, electron backscatter and neutron diffraction techniques.

Three techniques are used to measure crystallographic preferred orientations (CPO) in a naturally deformed quartz mylonite: transmitted light cross-polarized microscopy using an automated fabric analyser, electron backscatter diffraction (EBSD) and neutron diffraction. Pole figure densities attributable to crystal-plastic deformation are variably recognizable across the techniques, particularly between fabric analyser and diffraction instruments. Although fabric analyser techniques offer rapid acquisition with minimal sample preparation, difficulties may exist when gathering orientation data parallel with the incident beam. Overall, we have found that EBSD and fabric analyser techniques are best suited for studying CPO distributions at the grain scale, where individual orientations can be linked to their source grain or nearest neighbours. Neutron diffraction serves as the best qualitative and quantitative means of estimating the bulk CPO, due to its three-dimensional data acquisition, greater sample area coverage, and larger sample size. However, a number of sampling methods can be applied to FA and EBSD data to make similar approximations.

Making EBSD on water ice routine.

Electron backscatter diffraction (EBSD) on ice is a decade old. We have built upon previous work to select and develop methods of sample preparation and analysis that give >90% success rate in obtaining high-quality EBSD maps, for the whole surface area (potentially) of low porosity (<15%) water ice samples, including very fine-grained (<10 µm) and very large (up to 70 mm by 30 mm) samples. We present and explain two new methods of removing frost and providing a damage-free surface for EBSD: pressure cycle sublimation and 'ironing'. In general, the pressure cycle sublimation method is preferred as it is easier, faster and does not generate significant artefacts. We measure the thermal effects of sample preparation, transfer and storage procedures and model the likelihood of these modifying sample microstructures. We show results from laboratory ice samples, with a wide range of microstructures, to illustrate effectiveness and limitations of EBSD on ice and its potential applications. The methods we present can be implemented, with a modest investment, on any scanning electron microscope system with EBSD, a cryostage and a variable pressure capability.

A technique for recording polycrystalline structure and orientation during in situ deformation cycles of rock analogues using an automated fabric analyser.

Two in situ plane-strain deformation experiments on norcamphor and natural ice using synchronous recording of crystal c-axis orientations have been performed with an automated fabric analyser and a newly developed sample press and deformation stage. Without interrupting the deformation experiment, c-axis orientations are determined for each pixel in a 5 × 5 mm sample area at a spatial resolution of 5 µm/pixel. In the case of norcamphor, changes in microstructures and associated crystallographic information, at a strain rate of ∼2 × 10(-5) s(-1), were recorded for the first time during a complete in situ deformation-cycle experiment that consisted of an annealing, deformation and post-deformation annealing path. In the case of natural ice, slower external strain rates (∼1 × 10(-6) s(-1)) enabled the investigation of small changes in the polycrystal aggregate's crystallography and microstructure for small amounts of strain. The technical setup and first results from the experiments are presented.

The analysis of quartz c-axis fabrics using a modified optical microscope.

A new fully automated microfabric analyzer (MiFA) is described that can be used for the fast collection of high-resolution spatial c-axis orientation data from a set of digital polarized light images. At the onset of an analysis the user is presented with an axial-distribution diagram (AVA -'Achsenverteilungsanalyse') of a thin section. It is then a simple matter to build-up c-axis pole figures from selected areas of interest. The c-axis inclination and colatitudes at any pixel site is immediately available to create bulk fabric diagrams or to select measurements in individual areas. The system supports both the interactive selection of c-axis measurement sites and grid array selection. A verification process allows the operator to exclude dubious measurements due to impurities, grain boundaries or bubbles. We present a comparison of bulk and individual c-axis MiFA measurements to pole figures measured with an X-ray texture goniometer and to data collected from a scanning electron microscope furnished with electron backscatter diffraction (EBSD) facility. A second sample, an experimentally deformed quartzite, illustrates that crystal orientations can be precisely linked to any location within an individual grain.