Electron Backscatter Diffraction Imaging Research Articles

Hydrogen-induced crack behavior of a precipitation-strengthened Ni50Cr20Co15Al10V5 high entropy alloy

The hydrogen-induced cracking behavior and mechanism of an L12-strengthened Ni50Cr20Co15Al10V5 high entropy alloy was evaluated using the tensile test after hydrogen charging. The microstructures and hydrogen-induced cracks were characterized by electron backscatter diffraction and electron channeling contrast imaging methods. The results revealed that hydrogen decreased the strain hardening rate and induced pronounced cracks, leading to significant degradation in elongation. After deformation, the local strain was concentrated in the precipitate-matrix interfaces. The precipitate-matrix boundary and the interior of precipitates were prone to hydrogen embrittlement, where hydrogen-induced cracks tended to propagate, attributing to the hydrogen-enhanced decohesion mechanism.

Grain boundary-mediated strain response mechanism of AZ31 gradient- structure Mg alloy plate under uniaxial tensile loading

The changes in strain gradient induced by grain boundaries are crucial for enhancing the plasticity of gradient magnesium (Mg) alloys. The change of strain distribution influence by grain boundaries during plastic deformation of the gradient structure was examined. In this paper, the gradient structure AZ31 Mg-alloy plate with the surface fine grain (FG) to the center coarse grain (CG) was fabricated using hard plate rolling (HPR). The microstructure and strain distribution of Mg-alloy with a gradient structure were analyzed by electron backscatter diffraction (EBSD) and Digital image correlation (DIC) during uniaxial tensile. The findings indicate that the gradient structure sample (GS sample) displays a uniform strain distribution during the tensile process. Coarse-grain sample (CG sample) have obvious strain concentration, which leads to premature fracture. Based on EBSD characterization, low-angle grain boundaries (LAGBs) accumulates in the CG during plastic deformation. Orientation of CG tends to the (0001) basal. At the same time, the density of geometrically necessary dislocations (GNDs) inside CG has changed, which improves the Heterogeneous deformation induced (HDI) stress of gradient structure. During the uniaxial tensile, LAGBs accumulates in CG and changes the strain distribution of the gradient structure, which induces the accumulation of GNDs, and hence improving the properties of the GS Mg-alloy. These findings unveil the mechanism of strength-plasticity synergism of GS alloys from a new perspective and offer insights into the application of GS in Mg-alloys.

Influence of the as quenched state and tempering temperature on the final microstructure and hardness of a high strength medium carbon steel

The present study aimed to investigate the impact of the as-quenched microstructure and tempering temperature on the final microstructure and hardness of a medium-carbon, low-alloy steel using dilatometry, Electron backscatter diffraction (EBSD) and scanning electron microscopy (SEM). The results revealed substantial differences in the continuous heating stage of tempering in bainitic and martensitic samples, primarily attributed to the auto-tempering process during cooling. Tempering was carried out at 550 and 620 °C, and dilatometry results, along with microstructure analysis, indicated incomplete decomposition of retained austenite (RA) at both temperatures during a 30-min hold in the bainitic sample. The results show that non-decomposed RA, following the tempering of bainite, transformed into blocky fresh martensite, while no evidence of fresh martensite was observed in the martensitic sample. A new approach using EBSD and SEM images revealed that the decomposition of M/A (martensite/austenite constituent) zones in the bainitic sample resulted in the formation of a chain of aggregated chromium carbide zones at the grain boundaries. In contrast, the martensitic zone exhibited a uniform distribution of carbides in the microstructure. The stability of the phases was examined using the TCFE10 (thermodynamics) and MOBFE5 (mobility) modules of the DICTRA Themo-Calc software. Hardness measurements on all samples indicated decreases by about 18–24 % in the martensitic sample after tempering, while the bainitic sample exhibited a 5 % increase in hardness after tempering, attributed to secondary hardening and fresh martensite formation.

Effects of local strain on the plastic deformation and fracture mechanism of heterogeneous multilayered aluminum

Elucidating the effect of local strain on the mechanical properties is of great significance for the design of high-performance layered metals. For this purpose, we conceived the present study, featured by tailoring the local strain by layer thickness design, and simultaneous monitoring of local strain and geometrically necessary dislocations (GNDs) via coupling in-situ electron backscatter diffraction (EBSD) and high-resolution digital image correlation (DIC). In addition, synchrotron X-ray micro-computed tomography (μCT) was employed to analyze the microcracks that serve as another form of strain localization. Such detailed experimental studies revealed that the interfacial strain gradient was rapidly elevated, and the strain localization band was effectively dispersed as the layer thickness decreased. This leads to two typical transitions, from grain-boundary-related to layer-interface-related plastic deformation mode, and from macroscopic shear to zig-zag fracture mode. Their influences on the mechanical properties, as well as underlying mechanisms, were discussed based on the relationship among the layer thickness, strain gradient, strain localization, GND density, and microcracks. Our work not only contributes to the fundamental understanding of the mechanical behavior of multilayered metals but also offers guidance for the structural design of high-performance metals aimed at achieving superior strength-ductility combinations.

Granitic mush compaction by impingement of a large felsic enclave: Evidence from the Aztec Wash pluton (Nevada, USA)

Abstract Compaction and melt extraction are key processes in the generation of melt-dominated magma bodies. We analyze magmatic fabrics in the Aztec Wash pluton (15.7 Ma; Nevada, USA) to understand magma dynamics during emplacement of a large (2 m diameter) felsic enclave (LFE) in a silicic magma body. We hypothesize that the LFE moved through crystal-poor magma, settling into crystal-rich magma. We analyze four granite samples collected near the enclave: two 0.25 m below the enclave (E-5 and E-2); one 0.5 m below (E-6); and one 2.5 m to the side (E-3, far field). We use the scanning electron microscope (SEM) to gather data using backscattered electron (BSE) microscopy, energy dispersive spectroscopy (EDS), and electron backscatter diffraction (EBSD) imaging. BSE maps show large (up to 10 mm) euhedral alkali feldspar grains in E-5 and E-2, while E-6 and E-3 have large (up to 6 mm) alkali feldspar with distinct irregular and wavy rims. Dark BSE alkali feldspar rims correlate with Ba depletion in EDS maps. Broken feldspars in E-5 and E-2 have mismatched zones in BSE and orientation differences in EBSD. Grain orientation spread (GOS) maps show that alkali feldspar has the highest degree of intragrain deformation, followed by plagioclase, then quartz. Histograms of the angle between the vertical plane and the pole to the (010) plane demonstrate clustering in E-5, suggesting an enhanced fabric. Differences in rim texture suggest melt extraction beneath the enclave and melt retained in the far field. EBSD data reveal an enhanced foliation beneath the LFE. We conclude that mush under the LFE was deformed during emplacement of the LFE, expelling melt and reorienting grains.

Revealing the inhomogeneous nature of microstructure and texture evolution in the cold-rolled CoCrFeMnNi alloy during static recrystallization

In the present investigation, equiatomic CoCrFeMnNi high entropy alloy (HEA) was subjected to 80% cold rolling (as-rolled) followed by isothermal annealing treatment at 700 °C for different time periods. Microstructural characterization was performed using electron back-scattered diffraction (EBSD) and electron channeling contrast imaging (ECCI) techniques on the as-rolled and annealed samples. The as-rolled microstructure consisted of elongated grains mainly composed of strong α-fiber and weak γ-fiber textures. The as-rolled sample showed the formation of ingrain SBs in the γ-fiber grains, which served as preferential sites for grain nucleation. The annealing treatment of as-rolled samples at 700 °C cause static recovery (SRV) before 5 minutes of heat-treatment, whereas static recrystallization (SRX) was observed after 5 minutes of heat-treatment in the CoCrFeMnNi alloy samples. A faster rate of recrystallization kinetics was observed after 15 minutes of heat-treatment. The annealing treatment reduced the intensity of α-fiber and enhanced the Copper, Cube and P ({011}<122>) texture components. Copper components originated from coarse recrystallized grains, which were the results of localized grain growth phenomena. Unusual behavior of banded featured α-fiber grains was observed during the annealing process. These banded grains in the partially annealed samples consisted of subgrain-boundaries and showed a delayed response to recrystallization as compared to grains with other orientations. Stored energy (SE) and Taylor factor (M) calculations were also used to understand the delayed recrystallization response of the banded featured/retained deformed grains. The microhardness value of the as-rolled sample was approximately 450 Hv, which decreased to around 230 Hv for the fully recrystallized grains.

Characterisation of the creep cavitation process on grain boundaries in a polycrystalline nickel-base alloy 247

ABSTRACT Hot gas components such as gas turbine blades are loaded with constant centrifugal stress at high temperatures and thus the formation of creep cavitation on grain boundaries is expedited. Conventionally cast polycrystalline Nickel-base superalloys used as blade materials are prone to creep cavitation as unfavourably orientated grain boundaries exist. This research presents a diffusion-based probabilistic creep model which describes the creep cavitation process on grain boundaries. It includes the three mechanisms: pore nucleation, growth, and coalescence. The calibration of the model has been carried out by analysing Alloy 247 as-received specimens and specimens with pre-strain. For the evaluation of the pore numbers and sizes, a deep learning model for pore detection was trained on light microscopic and scanning electron microscopy images. Electron backscatter diffraction images are analysed for further investigations regarding grain orientations and grain boundary angles to the loading direction. The calibrated model allows predictions of pore size distributions over time.

Strain-induced martensite formation in cryorolled AISI 317 L stainless steel

AISI 317 L stainless steel replaces 316 L grade in some applications due to its superior mechanical strength and corrosion resistance. Aiming at expanding its applicability to structural applications, ongoing studies are dedicated to overcoming the trade-off between strength and ductility. The stacking fault energy decreases with deformation temperature and favors stacking faulting, (nano)twinning and strain-induced martensite (SIM) formation, resulting in severe microstructural fragmentation. The effect of temperature on deformation behavior of AISI 317 L steel was investigated in samples rolled at room temperature to thickness reductions of 50% and 85% and at 77 K to reductions in thickness of 10% and 50%. The microstructural evolution was followed by scanning electron microscopy, Vickers microhardness, X-ray diffraction, magnetization, electron backscatter diffraction (EBSD) and electron channeling contrast imaging (ECCI). The nucleation sites in the early stages of the transformation sequence γ → ε → α’ were identified in the 10% cryorolled sample. The highest volume fraction of α’-martensite reached 45.8% in the cryorolled steel to 50% rolling reduction. Much lower fractions were obtained for samples rolled to 10% reduction at 77 K (2%) and at room temperature to 50% (0.3%) and 85% reductions (1.6%). The texture components after cryorolling were Goss and Brass for austenite; rotated cube, α- and γ-fibers for δ-ferrite and α’-martensite. The ε-martensite presents the typical texture of hcp metals with a c/a ratio above the ideal value and 〈0001〉 − oriented tilted about 21° from the normal direction towards the rolling direction. The results show cryorolling as an effective method for enhancing SIM formation and promoting severe microstructural refinement in AISI 317 L stainless steel.

Effects of Mo content on the microstructure and mechanical properties of laser cladded FeCoCrNiMox (x = 0.2, 0.5) high-entropy alloy coatings

The laser cladding additive manufacturing technology and high-entropy alloys can serve as ideal techniques and materials for the surface repair of high-speed train axles. Coatings of FeCoCrNiMox (x = 0.2, 0.5) were prepared on EA4T axle steel using laser cladding technology, and their phase, structure, and mechanical properties were analyzed using X-ray diffraction (XRD), electron backscatter diffraction (EBSD) and electron channeling contrast imaging (ECCI) characterization techniques. Additionally, the mechanical properties of the coatings were tested, and first-principles calculations were used to verify and calculate the material's mechanical performance. The research findings indicate that an increase in Mo content leads to a greater degree of lattice distortion, causing a leftward shift in diffraction peak positions. Significant differences in the microstructure from the substrate to the coating surface were observed, with columnar grain structure at the bottom of the cladding layer and equiaxed dendrites dominating the coating surface. The increase in Mo content promotes the formation of σ phase while also refining the grain size. ECCI results show that both types of coatings consist of a high-density dislocation cell structure and Mo-rich particles. With an increase in Mo content, the peak hardness of the coating increased from 456.5 HV to 469.4 HV, while the impact energy decreased from 56 J to 16 J, attributed to the increase in dislocation density and the greater quantity of σ phase. First principles calculations verified that the comprehensive mechanical properties of FeCoCrNiMo0.2 are superior, providing theoretical guidance for the optimization and design of the coatings.

Influence of overlapping friction stir processing on microstructural evolution, texture development, and mechanical performance in Al6061

In the current examination, a large-area stirred zone has been created in Al6061 through the application of overlapping friction stir processing. The investigation focused on examining the microstructural and texture changes in friction stir processed Al6061, using the electron backscattered diffraction technique. Electron backscattered diffraction images provided valuable insights into the recrystallization process, revealing the presence of fine-grained structure with high-angle boundaries in the large-area stirred zone attributed to intense plastic straining and dynamic recrystallization. The use of the tool caused significant plastic straining, resulting in the development of the A- (1 1 1) {1 1 0} texture component. Mechanical testing demonstrated a noteworthy increase in ductility after processing. However, the microhardness and strength were observed to be inferior to the base material due to elevated thermal cycling.

Q-RBSA: high-resolution 3D EBSD map generation using an efficient quaternion transformer network

Gathering 3D material microstructural information is time-consuming, expensive, and energy-intensive. Acquisition of 3D data has been accelerated by developments in serial sectioning instrument capabilities; however, for crystallographic information, the electron backscatter diffraction (EBSD) imaging modality remains rate limiting. We propose a physics-based efficient deep learning framework to reduce the time and cost of collecting 3D EBSD maps. Our framework uses a quaternion residual block self-attention network (QRBSA) to generate high-resolution 3D EBSD maps from sparsely sectioned EBSD maps. In QRBSA, quaternion-valued convolution effectively learns local relations in orientation space, while self-attention in the quaternion domain captures long-range correlations. We apply our framework to 3D data collected from commercially relevant titanium alloys, showing both qualitatively and quantitatively that our method can predict missing samples (EBSD information between sparsely sectioned mapping points) as compared to high-resolution ground truth 3D EBSD maps.

Comparison Between Neutron Bragg Dip and Electron Backscatter Diffraction Images of TlBr Semiconductors

Comparison Between Neutron Bragg Dip and Electron Backscatter Diffraction Images of TlBr Semiconductors

Influence of high‐strain deformation on major element mobility in garnet: Nanoscale evidence from atom probe tomography

AbstractGarnet is a common rock‐forming mineral that occurs in a variety of rock types and over a wide range of pressure (P)–temperature (T) conditions in the Earth's lithosphere. Because garnet is considered a high‐strength mineral stable across an extensive range of conditions (1–25 GPa, &lt;300–2000°C), it is generally accepted that garnets can retain their microstructures and chemical composition during deformation and metamorphism. Therefore, garnet is commonly used as a geothermobarometer and geochronometer to provide P–T and timing constraints on tectonic events. Herein, we study garnet from an eclogite facies mylonite (central Australia) to investigate the mechanisms of element mobility during high‐strain deformation under relatively dry, lower crustal conditions. Electron backscatter diffraction (EBSD) and electron channelling contrast imaging (ECCI) reveal evidence of crystal plasticity associated with brittle deformation in the form of heterogeneous misorientation patterns and low‐angle grain boundaries developed over length scales of 20–50 μm in the rims of garnet porphyroclasts. Atom probe tomography (APT) analysis of a low‐angle grain boundary within a highly strained portion of a clast shows Ca enrichment and Mg depletion along dislocations, whereas APT data along the rim of a mostly undeformed clast reveal a homogeneous distribution of garnet major components in the specimen matrix with the exception of Ca, Fe and Mg enrichment within a healed microfracture. The above‐mentioned results suggest that under relatively dry conditions, crystal plasticity enhances bulk element mobility via pipe diffusion, highlighting the importance of deformation‐induced microstructures on element mobility, with important implications for the robust and reliable use of garnet as a petrological tool.

Inelastic mechanical behaviour of an additively manufactured titanium alloy: a statistical continuum mechanics theory perspective

Statistical continuum mechanics theory was used to simulate the inelastic stress of polycrystalline materials using two-point statistics. For the experimental part, the Electron beam melting (EBM) technique (Arcam EBM Q10 additive machine) was used to fabricate cylindrical rods of Ti-6Al-4V both in horizontal and vertical directions. Electron backscatter diffraction (EBSD) technique was employed to achieve statistically reliable orientation maps of vertically and horizontally printed samples. In this study, high strain rate compression tests at six different strain rates were performed, and the stress–strain curves were generated. This work is amongst the first attempts to model the microstructure of additively manufactured hexagonal alloys under compressive loadings using the statistical continuum mechanics theory. The model is capable of simulating reasonably large microstructures (statistically representative) with a practical computational cost and accuracy, unlike numerical models that require a high computational cost. It should be noted that in additive manufacturing, due to large grains and high anisotropy, microstructures used in the simulations should be large enough to include sufficient information from the material’s structure. Therefore, using finite element models would be very challenging here. On the other hand, the statistical continuum mechanics theory uses the statistical representation of the material’s characteristics for solving the governing equations with Green’s function that enables this methodology to use more microstructure characteristic information without having a noticeable change to the computational cost. The proposed model in this study uses different microstructure characteristics such as crystal grain orientation, total slip systems, active slip systems, gain morphology, and chemical phases that are obtained from EBSD images for simulating the inelastic mechanical behavior of polycrystalline materials. Although this model simulates polycrystalline materials by considering various crystal and grain information, unlike numerical methods, it doesn’t simulate the grain interactions well and we cannot study local deformation and crack nucleation sites. This model works very well for simulating the overall behavior of material instead of each individual grain and failure analysis. This model has shown a good combination of computational cost and accuracy in which the error between the simulated and experimental strength for vertical and horizontal samples was 6.21% and 8.07%, respectively.

Statistical Comparison of Substructures in Pure Aluminum Before and After Creep Deformation, Based on EBSD Image Data.

Electron backscatter diffraction (EBSD) images of extruded pure aluminum were statistically analyzed to investigate creep-induced subgrain structures after applying two different levels of creep stress, corresponding to the power law (PL) and power-law breakdown (PLB) regimes. Kernel average misorientation analysis of EBSD measurements revealed 2D morphologies, which were subdivided by a multi-step segmentation procedure into subgranular arrangements. Various descriptors were employed to characterize the "subgrains" quantitatively, including their size, shape, spatial arrangement, and crystallographic orientation. In particular, the analysis of the orientations of subgrains was conducted by neglecting rotations around the loading axis. This approach facilitated the individual investigation of the {001} and {111} subgrain families with respect to the loading axis for two investigated stress levels plus a reference specimen. For the PL regime, the statistical analysis of subgrain descriptors computed from segmented image data revealed a similar degree of strain accumulation for {111} and {001} subgrains. In contrast, for the PLB regime, the analyzed descriptors indicate that {111} subgrains tend to accumulate significantly more strain than {001} ones. These observations suggest that the mechanisms leading to PLB may be associated with strain localization dependent on intergranular stress, hindering the recovery process within {111} grains.

Cryogenic impact fracture behavior of a high-Mn austenitic steel using electron backscatter diffraction and neutron Bragg-edge transmission imaging

A unique impact fracture behavior is found in a high-Mn austenitic steel (24Mn–4Cr-0.4C-0.3Cu) in this work. The steel exhibits concurrent twinning-induced plasticity (TWIP) effect and the transformation-induced plasticity (TRIP) effect. By analyzing the load-deflection curves recorded during Charpy impact testing, the resistance to crack initiation and propagation is quantified from the absorbed energy. The high-Mn steel demonstrates good resistance to crack initiation at 273 K and 77 K. However, as the temperature decreases from 273 K to 77 K, there is an accelerated transition from stable crack growth to unstable crack growth during impact, resulting in the deterioration of resistance to crack propagation. The plastic deformation of the impact-tested samples, especially in the region close to the crack-path profile was quantitatively analyzed using neutron Bragg-edge transmission (BET) imaging. The deformation zones, divided by using the width of the 200 Bragg edge, exhibit good agreement with the impact absorbed energy characteristics obtained from dynamic load-deflection curves. Moreover, the unstable growth transition point was roughly determined on the impact-tested sample. Then, the electron backscatter diffraction (EBSD) technique is employed to examine the deformation microstructure along the crack-path in the impact-tested samples. The results revealed the dual roles of TRIP effect in impact toughness of the high-Mn steel. On one hand, the TRIP effect plays a positive role in improving resistance to crack initiation and propagation. On the other hand, the excessive accumulation of brittle ε/α՛-martensite caused by the enhanced TRIP effect at 77 K leads to quasi-cleavage fracture, thereby playing a negative role. Finally, we discussed the prominent toughening mechanisms associated with the TWIP and TRIP effects, which greatly impact the impact fracture behavior.

Graph neural network for predicting the effective properties of polycrystalline materials: A comprehensive analysis

We develop a polycrystal graph neural network (PGNN) model for predicting the effective properties of polycrystalline materials, using the Li7La3Zr2O12 ceramic as an example. A large-scale dataset with >5000 different three-dimensional polycrystalline microstructures of finite-width grain boundary is generated by Voronoi tessellation and processing of the electron backscatter diffraction images. The effective ion conductivities and elastic stiffness coefficients of these microstructures are calculated by high-throughput physics-based simulations. The optimized PGNN model achieves a low error of <1.4% in predicting all three diagonal components of the effective Li-ion conductivity matrix, outperforming a linear regression model and two baseline convolutional neural network models. Sequential forward selection method is used to quantify the relative importance of selecting individual grain (boundary) features to improving the property prediction accuracy, through which both the critical and unwanted node (edge) feature can be determined. The extrapolation performance of the trained PGNN model is also investigated. The transfer learning performance is evaluated by using the PGNN model pretrained for predicting conductivities to predict the elastic properties of the same set of microstructures.:

Restoration of Noisy Orientation Maps from Electron Backscatter Diffraction Imaging

Restoration of Noisy Orientation Maps from Electron Backscatter Diffraction Imaging

Unravelling anisotropic deformation behaviour of Ti-6Al-4V ELI fabricated by powder bed fusion additive manufacturing

The uniaxial compression tests with respect to the different loading directions (i.e., parallel, and perpendicular to the building direction) were performed to investigate the anisotropic deformation mechanism of Ti–6Al–4 V ELI (extra low interstitial) alloy fabricated by laser powder bed fusion (L-PBF). The tests showed anisotropic mechanical properties; the sample loaded perpendicular to the building direction (TDx) has a higher fracture strain and lower yield strength, but a superior hardening effect than those of the sample loaded along the building direction (BD). Electron backscatter diffraction (EBSD) and digital image correlation (DIC) analyses were conducted used at regions of interest (ROI) in as-built and deformed samples. The kernel average misorientation (KAM) analysis revealed that a trend of dislocation evolution is strikingly different according to the loading directions; uniform KAM distribution is observed in the BD sample, whilst localization at prior β grain boundaries is found in the TDx sample. In addition, it was identified via a microscopic strain distribution map that the unique layered microstructure (i.e., layer band) and prior β grain boundary are more sensitive to compressive loading than the surrounding matrix. The layer band and prior β grain boundary were formed with their directivity during the additive manufacturing process; thus, their morphology is different depending on the loading direction. As a result, the layer band and prior β grain boundary play a key role in anisotropic behaviour, more precisely, the anisotropic deformation behaviour originates from the morphology of the layer band and β grain boundary, which is changed with respect to the loading direction.

A study of the void surface healing mechanism in 316LN steel

Abstract The behavior of void surface healing in 316LN steel samples undergoing thermal plasticity deformation was investigated using the Gleeble 1500 thermomechanical simulator. The characterization of the void surface after plastic deformation was analyzed under different deformation temperatures, deformation amounts, and holding time durations. The morphology evolution and microstructure of the void surface healing zone during thermal plasticity deformation and holding time duration stage were analyzed using electron back scatter diffraction imaging. The mechanism of void surface healing under thermal plasticity deformation was investigated. It was found that the degree of void surface healing increases with the degree of deformation and the duration of the holding time. Dynamic recrystallization occurred continuously at the void surface, resulting in a plethora of crystal defects and a substantial amount of energy. These conditions were conducive to atomic diffusion and migration, thereby promoting the healing process of the void surface. Maintaining high temperature after deformation can continue to provide energy for the diffusion and migration of atoms, promotes the growth of recrystallized grains, and gradually heals the void surface.