Advanced characterization techniques for high-angular and high-spatial resolutions in the scanning electron microscope

High-angular resolution electron diffraction-based techniques aim at measuring relative lattice rotations and elastic strains with an accuracy about 1.10-4 (<0.01°) in the scanning electron microscope (SEM). These metrics are essential for the fine characterization of deformation structures in terms of grain internal disorientations and geometrically necessary dislocation densities. To this purpose, relative deformations between electron diffraction patterns are retrieved with subpixel accuracy using digital image correlation (DIC) techniques. Here, a novel DIC approach is proposed. It relies on a linear homography [1], i.e., a geometric transformation often met in photogrammetry to model projections. The method is implemented in ATEX-software [2], developed at the University of Lorraine. Its performances are illustrated from both a semi-conductor and a metal. First, lattice rotation and elastic strain fields are investigated in the vicinity of a giant screw dislocation in GaN single crystal using the electron backscattered diffraction technique (Fig. 1). Second, the proposed method is coupled with the on-axis Transmission Kikuchi Diffraction (TKD) configuration to characterize a nanocrystalline aluminium obtained by severe plastic deformation. On-axis TKD consists in observing a thin foil in transmission in the SEM, using a scintillator is placed beneath the specimen, perpendicularly to the electron beam. Thanks to this coupling, high-spatial (3-6 nm) and high-angular (~0.01°) resolutions are simultaneously achieved in SEM. [3]

Mechanical properties, microstructure and crystallographic texture of magnesium AZ91-D alloy welded by Friction Stir Welding (FSW)

The objective of the study was to characterize the properties of a magnesium alloy welded by friction stir welding (FSW). The results led to a better understanding of the relationship between this process and the microstructure and anisotropic properties of alloy materials. Welding principally leads to a large reduction in grain size in welded zones due to the phenomenon of dynamic recrystallization. The most remarkable observation was that crystallographic textures appeared from a base metal without texture in two zones: the thermo-mechanically affected and stir welded zones. The latter zone has the peculiarity of possessing a marked texture with two components on the basal plane and the pyramidal plane. These characteristics disappeared in the TMAZ, which had only one component following the basal plane. These modifications have been explained by the nature of the plastic deformation in these zones, which occurs at a moderate temperature in the TMAZ and high temperature in the SWZ

Ultrafine grained plates of Al-Mg-Si alloy obtained by Incremental Equal Channel Angular Pressing : microstructure and mechanical properties

In this study, an Al-Mg-Si alloy was processed using via Incremental Equal Channel Angular Pressing (I-ECAP) in order to obtain homogenous, ultrafine grained plates with low anisotropy of the mechanical properties. This was the first attempt to process an Al-Mg-Si alloy using this technique. Samples in the form of 3 mm-thick square plates were subjected to I-ECAP with the 90˚ rotation around the axis normal to the surface of the plate between passes. Samples were investigated first in their initial state, then after a single pass of I-ECAP and finally after four such passes. Analyses of the microstructure and mechanical properties demonstrated that the I-ECAP method can be successfully applied in Al-Mg-Si alloys. The average grain size decreased from 15 - 19 µm in the initial state to below 1 µm after four I-ECAP passes. The fraction of high angle grain boundaries in the sample subjected to four I-ECAP passes lay within 53-57 % depending on the examined plane. The mechanism of grain refinement in Al-Mg-Si alloy was found to be distinctly different from that in pure aluminium with the grain rotation being more prominent than the grain subdivision, which was attributed to lower stacking fault energy and the reduced mobility of dislocations in the alloy. The ultimate tensile strength increased more than twice, whereas the yield strength - more than threefold. Additionally, the plates processed by I-ECAP exhibited low anisotropy of mechanical properties (in plane and across the thickness) in comparison to other SPD processing methods, which makes them attractive for further processing and applications

Modeling of large strain hardening during grain refinement

Strain hardening was modeled at large strains taking into account the geometrically necessary dislocations (GNDs) with the help of a recent grain refinement model. The GND density was studied experimentally with orientation imagining for oxygen-free high-conductivity copper deformed in equal channel angular pressing and in simple shear to the same equivalent strain. The results show that the GND density can be predicted fairly well by the model in accord with experiments, and also affects stage IV hardening

Formation of micro shear bands during cyclic deformation of sub-microcrystalline nickel

Cyclic deformation of sub-microcrystalline nickel at high plastic strain amplitude generated macro shear bands, causing fatal cracking. The macro shear bands consisted of several micro shear bands, each band containing a single layer of elliptical grains that appeared at less than 50° with respect to the loading axis. Micro texture investigations in micro shear bands revealed almost the same texture with similar shear values as in macro shear bands. During cyclic deformation local overlapping of evolving micro shear bands resulted in formation of fatal macro shear bands

Shear banding in sub-microcrystalline nickel at 4 K

A flat specimen of sub-microcrystalline nickel was tensile tested at 4 K until fractureoccurred and subsequently investigated by electron backscatter diffraction in a high reso-lution scanning electron microscope in order to deduce the local texture in the near crackarea. Thus, two sets of intersecting fine slip markings observed on the surface (under ±55°with respect to the tensile axis) could be explained as a result of localized simple shear inthe bulk material underneath the slip markings. The overall amount of shear in the regionnear the crack was estimated to be 1.25 based on texture simulations using the viscoplasticself-consistent polycrystal mode

Novel EBSD-TEM like technique: texture analysis, orientation and phase maps on nanostructured materials

International audienc

Notes on representing grain size distributions obtained by electron backscatter diffraction

Grain size distributions measured by electron backscatter diffraction are commonly represented by histograms using either number or area fraction definitions. It is shown here that they should be presented in forms of density distribution functions for direct quantitative comparisons between different measurements. Here we make an interpretation of the frequently seen parabolic tales of the area distributions of bimodal grain structures and a transformation formula between the two distributions are given in this paper