Papers by Author: Sandra Piazolo

Abstract: The understanding of the dynamics of substructures during deformation and annealing is fundamental in our ability to predict microstructural and physical properties such as rheological behaviour of crystalline materials. Here, we present an overview of new insights into substructure dynamics through a combination of in-situ heating experiments, detailed Electron Backscatter Diffraction (EBSD) analysis and numerical modelling.

Abstract: n-situ 3D X-ray diffraction (3DXRD) annealing experiments were conducted at the ID-11 beamline at the European Synchrotron Radiation Facility in Grenoble. This allowed us to non-destructively document and subsequently analyse the development of substructures during heating, without the influence of surface effects. A sample of deformed single crystal halite was heated to between 260-400 °C. Before and after heating a volume of 500 by 500 by 300 μm was mapped using a planar beam, which was translated over the sample volume at intervals of 5-10 µm in the vertical dimension. In the following we present partially reconstructed orientation maps over one layer before and after heating for 240min at 260 °C. Additional small syn-heating maps over a constrained sample rotation of 12-30º. The purpose of this was to illuminate a few reflections from 1 or 2 subgrains and follow their evolution during heating. Preliminary results show that significant changes occurred within the sample volume, for which, surface effects can be excluded. Results show a number of processes, including: i) change in subgrain boundary misorientation angle and ii) subgrain subdivision into areas of similar lattice orientation with new subgrain boundary formation. These results demonstrate that 3DXRD coupled with in-situ heating is a successful non-destructive technique for examining real-time post-deformational annealing in strongly deformed crystalline materials with complicated microstructures.

Abstract: The Weighted Burgers Vector (WBV) is defined as the sum, over all types of dislocations, of [(density of intersections of dislocation lines with a map) x (Burgers vector)]. It can be calculated, for any crystal system, solely from orientation gradients in a map view, unlike the full dislocation density tensor, which requires gradients in the third dimension. No assumption is made about gradients in the third dimension and they may be non-zero. The only assumption involved is that elastic strains are small so the lattice distortion is entirely due to dislocations. Orientation gradients can be estimated from gridded orientation measurements obtained by EBSD mapping, so the WBV can be calculated as a vector field on an EBSD map. The magnitude of the WBV gives a lower bound on the magnitude of the dislocation density tensor when that magnitude is defined in a coordinate invariant way. The direction of the WBV can constrain the types of Burgers vectors of geometrically necessary dislocations present in the microstructure, most clearly when it is broken down in terms of lattice vectors. The WBV has five advantages over other measures of local lattice distortion. 1. It is a vector and hence carries more information than any scalar measure of local misorientation. 2. It has an explicit mathematical link to the individual Burgers vectors of dislocations. 3. Since it is derived via tensor calculus, it is not dependent on the map coordinate system, in contrast to existing measures of local misorientation which are not only scalar but dependent on the coordinate system used. 4. Calculation involves no assumptions about energy minimisation. 5. The numerical differentiation involved in calculating the WBV may introduce errors, but there is a direct mathematical link to a contour integral. The net Burgers vector content of dislocations intersecting an area of a map can be simply calculated by an integration round the edge of that area, a method which is fast and complements point-by-point WBV calculations. Errors in orientation measurement will have a much smaller effect here, and dislocations can be detected which are otherwise lost in the noise of any local calculation.

Abstract: Annealing is an important mechanism of microstructural modification both in rocks and metals. In order to relate directly changes in crystallographic orientation to migrating boundaries the researcher has the option to investigate either samples where the grain boundary motion can be directly tracked or a series of samples exhibiting successively higher degrees of annealing. Here we present results from rock samples collected from two well characterised contact aureoles (a volume of rock heated by the intrusion of a melt in its vicinity): One quartz sample in which patterns revealed by Cathodoluminescence (CL) indicate the movement of grain boundaries and a series of calcite samples of known temperature history. Electron backscatter diffraction (EBSD) analysis is used to link the movement of grain, twin boundaries and substructures with the crystallographic orientation / misorientation of a respective boundary. Results from the quartz bearing rock show: (a) propagation of substructures and twin boundaries in swept areas both parallel and at an angle to the growth direction, (b) development of slightly different crystallographic orientations and new twin boundaries at both the growth interfaces and within the swept area, and (c) a gradual change in crystallographic orientation in the direction of growth. Observations are compatible with a growth mechanism where single atoms are attached and detached both at random and at preferential sites i.e. crystallographically controlled sites or kinks in boundary ledges. Strain fields caused by defects and/or trace element incorporation may facilitate nucleation sites for new crystallographic orientations at distinct growth interfaces but also at continuously migrating boundaries. Calcite samples show with increasing duration and temperature of annealing: (a) systematic decrease of the relative frequency of low angle grain boundaries (gbs), (b) decrease in lattice distortion within grains, (c) development of distinct subgrains with little internal lattice distortion, (d) change in lobateness of gbs and frequency of facet parallel gbs and (e) change in position of second phase particles. These observations point to an increasing influence of grain boundary anisotropy with increasing annealing temperature, while at the same time the influence of second phase particles and subtle driving-force variations decrease. This study illustrates the usefulness of using samples from natural laboratories and combining different analysis techniques in microprocess analysis.

Abstract: Reflected light optical analysis and Electron Backscatter Diffraction (EBSD) analysis have been used to m easure grain sizes in 2D Al foil samples, annealed for different times. There are significant differences in the results of the two techniques. It is shown that in Al it is possible to detect boundaries in optical images down to a misorientation angle of 7-8º. Nevertheless, in most samples the critical angle of easy etching lies above 10º. The observed differences in grain size measurements between optical analysis and EBSD analysis can be largely attributed to three phenomena: (1) individual samples may behave slighty differently due to differences in the effectiveness of etching (2) the grain size is heterogeneous over large areas and (3) the effect of etching is not only a function of misorientation angle but also grain boundary plane. Despite these uncertainties, optical analysis seems to be reliable for analysis of processes in which mainly grain boundaries with misorientation angle of > 10º are involved i.e. grain growth.

Abstract: Experiments in which the microstructural development can be observed at the same time as the crystallography is described fully opens up new, powerful ways to advance our understanding of microstructural processes such as grain growth, primary and secondary recrystallization and phase transformations. In addition, comparison of results of experiments in different materials can be used to develop general laws for the investigated processes. In this study, we briefly review and compare the results from various ongoing studies undertaken in a variety of materials with emphasis on highlighting (a) the scientific potential of such experiments and (b)similarities and differences in their microstructural evolution. Materials studied include metals e.g. Ti, Ni, Al, Mg, Ti-SULC steel and geological materials such as rocksalt (NaCl), hematite and magnetite. Here, we present experimental results and their interpretation in terms of subgrain to grain-scale processes.

Abstract: First results from grain growth experiments in a columnar structured Al foil show several interesting features: (a) the grain size distribution remains heterogeneous even after up to 300 min. annealing and (b) the Von Neumann-Mullins relation is not always satisfied. To clarify the underlying reasons for these features, in-situ heating experiments within a Scanning Electron Microscope (SEM) were combined with detailed Electron Backscatter Diffraction (EBSD) analysis. These show that the movement of boundaries can be strongly heterogeneous. For example, the complete replacement of one grain by a neighbouring grain without significant change of the surrounding grain boundary topology is frequently seen. Experiments show that grain boundary energy and/or mobility are anisotropic both with respect to misorientation and orientation of grain boundary plane. Low energy and/or mobility boundaries are commonly low angle boundaries, twin boundaries and boundaries that form traces to a low index plane of at least one of the adjacent grains. As a consequence the Von Neumann-Mullins relation is not always satisfied.

Abstract: The localization of deformation in recrystallizing materials is investigated via a series of two-dimensional grain-scale numerical simulations. These simulations couple a grain size and strain dependant viscous rheology with grain size reduction and grain growth processes. The simulations are able to predict the mechanical, microstructural and strain evolution of the polycrystals to high strain, and allow us to examine the nature of the time dependent feedback between mechanical and microstructural behavior. It was found that significant strain localization occurred only when the grain size dependence of the viscosity was non-linear, and was greatly enhanced by the activity of the grain size modifying processes. The intensity and location of the zone of strain localization varied spatially and temporally, with the result that the finite strain state showed a much broader, and hence less intense, zone of localized deformation than the instantaneous state.

Abstract: Misorientation analysis, using EBSD data sets, has enabled us to constrain better recrystallization mechanisms in rocks and minerals. Observed microstructures are not explicable in terms of recovery, boundary bulging and migration alone. We have to invoke either a nucleation process (physics unknown) or grain rotations that are not related to grain or boundary crystallography. Such rotations can occur by diffusion accommodated grain boundary sliding and this mechanism explains best the microstructure and texture of recrystallized grains in some rocks.