Accurate Electron Channeling Contrast Imaging Research Articles

Plasticity induced by nanoindentation in a CrCoNi medium-entropy alloy studied by accurate electron channeling contrast imaging revealing dislocation-low angle grain boundary interactions

In the present work, interactions of nanoindentation-induced dislocations (NIDs) with a low-angle grain boundary (LAGB) are investigated in a single-crystalline CrCoNi medium-entropy alloy (MEA). Microstructural evolutions before and after nanoindentation were examined using accurate electron channeling contrast imaging (A-ECCI). In the as-grown state, the alloy microstructure consists of subgrains separated by LAGBs. After nanoindentation on the (001) plane far away from LAGBs, the load-displacement curves exhibit the typical behavior of metals and alloys with a pop-in marking the elastic-plastic transition. This pop-in is related to the nucleation of NIDs that are observed to form pile-ups on {111} planes. In contrast, when indents are performed in the vicinity of a LAGB with a low misorientation angle of 0.24° and consisting of dislocations spaced ~60 nm apart, different micromechanical responses and deformation mechanisms are observed depending on the distance between the LAGB and the nanoindenter tip. When the distance between the LAGB and the nanoindenter tip is larger than four times the size of the indent (corresponding ratio: R > 4), the LAGB does not affect the micromechanical response nor interact with NIDs. In contrast, when the indenter comes in direct or indirect contact with the LAGB (R < 1), the load-displacement curve deviates at low loads from the elastic stage, and pop-ins are not observed. In this case, the continuous deformation is accommodated by the movement of the pre-existing LAGB dislocations. For intermediate cases with 1 < R < 4, the load of the initial pop-in is dependent on the local defect density. In this latter case, the pile-ups of NIDs directly impinge on the LAGB. Microstructural analyses reveal that the LAGB accommodates plasticity by blocking the NIDs, activating a dislocation nucleation site in the adjacent subgrain/emission of dislocation from the LAGB, and inducing slight motions of its constituent dislocations.

In Situ Macroscopic Tensile Testing in SEM and Electron Channeling Contrast Imaging: Pencil Glide Evidenced in a Bulk β-Ti21S Polycrystal

In this paper, we report the successful combination of macroscopic uniaxial tensile testing of bulk specimen combined with In situ dislocation-scale observations of the evolution of deformation microstructures during loading at several stress states. The dislocation-scale observations were performed by Accurate Electron Channeling Contrast Imaging in order to follow the defects evolution and their interactions with grain boundaries for several regions of interest during macroscopic loading. With this novel in situ procedure, the slip systems governing the deformation in polycrystalline bulk β-Ti21S are tracked during the macroscopic uniaxial tensile test. For instance, curved slip lines that are associated with “pencil glide” phenomenon and tangled dislocation networks are evidenced.

A Dislocation-Scale Characterization of the Evolution of Deformation Microstructures around Nanoindentation Imprints in a TiAl Alloy.

In this work, plastic deformation was locally introduced at room temperature by nanoindentation on a γ-TiAl-based alloy. Comprehensive analyses of microstructures were performed before and after deformation. In particular, the Burgers vectors, the line directions, and the mechanical twinning systems were studied via accurate electron channeling contrast imaging. Accommodation of the deformation are reported and a scenario is proposed. All features help to explain the poor ductility of the TiAl-based alloys at room temperature.

Sub-boundaries induced by dislocational creep in uranium dioxide analyzed by advanced diffraction and channeling electron microscopy

The network of sub-boundaries formed in a sintered UO2 pellet after dislocational creep was examined. Very low angle boundaries, down to 0.1° were reliably detected by Electron BackScattered Diffraction (EBSD). This angular resolution was achieved by optimizing EBSD data collection and processing. Moreover, Accurate-Electron Channeling Contrast Imaging (Accurate-ECCI) was able to image the dislocations produced by creep, directly on the bulk sample. The dislocations were mostly organized in sub-boundaries with low energy configurations. Only a limited number of isolated dislocations were observed. Finally, the deformation substructure obtained after 8% creep deformation (at 1500°C under a 50MPa uniaxial state) was quantified. The original grains with a mean size of 20μm were in average fragmented in sub-grains of about 5μm. The geometrically necessary dislocations density (GND) was evaluated from the filtered EBSD data to 7.9×1012m−2. This value was 10 times higher than that measured on the as-sintered sample. This confirms that the GND density calculation is sensitive to the dislocation increase after 8% deformation by creep.

Characterization of a Sub-Grain Boundary Using Accurate Electron Channeling Contrast Imaging

Characterization of a Sub-Grain Boundary Using Accurate Electron Channeling Contrast Imaging

Accurate electron channeling contrast analysis of a low angle sub-grain boundary

High resolution selected area channeling pattern (HR-SACP) assisted accurate electron channeling contrast imaging (A-ECCI) was used to unambiguously characterize the structure of a low angle grain boundary in an interstitial-free-steel. The boundary dislocations were characterized using TEM-style contrast analysis. The boundary was determined to be tilt in nature with a misorientation angle of 0.13° consistent with the HR-SACP measurements. The results were verified using high accuracy electron backscatter diffraction (EBSD), confirming the approach as a discriminating tool for assessing low angle boundaries.

Sub-micron resolution selected area electron channeling patterns

Collection of selected area channeling patterns (SACPs) on a high resolution FEG-SEM is essential to carry out quantitative electron channeling contrast imaging (ECCI) studies, as it facilitates accurate determination of the crystal plane normal with respect to the incident beam direction and thus allows control the electron channeling conditions. Unfortunately commercial SACP modes developed in the past were limited in spatial resolution and are often no longer offered. In this contribution we present a novel approach for collecting high resolution SACPs (HR-SACPs) developed on a Gemini column. This HR-SACP technique combines the first demonstrated sub-micron spatial resolution with high angular accuracy of about 0.1°, at a convenient working distance of 10mm. This innovative approach integrates the use of aperture alignment coils to rock the beam with a digitally calibrated beam shift procedure to ensure the rocking beam is maintained on a point of interest. Moreover a new methodology to accurately measure SACP spatial resolution is proposed. While column considerations limit the rocking angle to 4°, this range is adequate to index the HR-SACP in conjunction with the pattern simulated from the approximate orientation deduced by EBSD. This new technique facilitates Accurate ECCI (A-ECCI) studies from very fine grained and/or highly strained materials. It offers also new insights for developing HR-SACP modes on new generation high-resolution electron columns.

Accurate electron channeling contrast analysis of dislocations in fine grained bulk materials

Non-destructive, comprehensive dislocations characterization in fine grained Interstitial-Free Steel was realized for the first time by Accurate Electron Channeling Contrast Imaging “A-ECCI” in a Scanning Electron Microscope. Conventional Transmission Electron Microscopy g·b = 0 invisibility criterion and trace analysis were applied to determine Burgers vectors and line directions in this bulk material. This approach relies on the live collection of High Resolution Selected Area Channeling Patterns “HR-SACPs” using an innovative procedure to rock the beam with a remarkable spatial resolution of about 1 μm.