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DOE OSTI2025

Generalizable Image Segmentation for Microstructure Characterization Through Integrated SEM and EBSD Analysis

We demonstrate generalizable semantic segmentation using minimal ground truth data. Correlated scanning electron microscopy (SEM) images and electron backscatter diffraction (EBSD) measurements of frictionstir processed 316L stainless steel plates were used to train deep learning models for grain boundary segmentation. Secondary electron (SE) imaging taken at an accelerating voltage of 10 keV correlated to EBSD-derived grain boundaries produced the best performing model. Notably, an ensemble of three models trained on a single SE image produced accurate segmentation over a series of BSE images of samples manufactured under different processing parameters, with a resultant mean absolute error in grain size of 0.34 µm. The striking generalizability of the models likely results from the similar escape depths of the SE training input and the EBSD training output and the reduced probability of dislocation artifacts appearing in the image. This finding highlights the importance of considering the physical principles behind imaging in the development of robust segmentation models for microstructure characterization.

Taufique, Mohammad Fuad Nur↗

DOE OSTI2025

In situ deformation of antigorite-olivine two-phase mixtures: Implications for dynamics and seismic anisotropy in the mantle wedge

Water released from hydrous minerals in subducting slabs reacts with the overlying plate, resulting in widespread serpentinization in the mantle wedge. Deformation of serpentinized peridotites has been invoked to explain forearc seismic anisotropy, yet studies of the mechanical properties and deformation behaviors of serpentine-bearing multiphase aggregates remain limited. Here we deformed olivine-antigorite mixtures containing 70, 50, and 20 vol.% of antigorite at 2.5 – 7.6 GPa, 673 K and strain rates of ∼10 –5 –10 –4 s –1 . Elasto-viscoplastic self-consistent simulations, constrained by synchrotron X-ray diffraction (XRD) data, were used to estimate lattice strain, stress–strain partitioning, crystallographic preferred orientations (CPO) development, and aggregate strength. Selected run products were also analyzed by electron backscatter diffraction for comparison with the CPO results obtained from XRD experiments. We found olivine transitions from A- or B-type to C-type when antigorite fraction drops to 20 vol.%, coinciding with a microstructural change from interconnected weak layers to a load-bearing framework (LBF). An additional run on a sample Atg50/Ol50 with preexisting microstructures suggested the formation of LBF was promoted by these microstructures, although the preexisting antigorite CPO has been overprinted at 20.8 % strain and could be erased completely by subsequent deformation in nature. Estimated viscosity of the two-phase mixtures suggests that low-degree serpentinization (≤20 %) in the mantle wedge may increase the strength of olivine-rich peridotite and hinder slab-mantle decoupling, whereas high-degree serpentinization (≥50–70 %) weakens the peridotite and favors decoupling if sufficient viscosity contrast (>10) develops. Seismic anisotropy shows a nonlinear dependence on antigorite fraction: antigorite CPO governs the anisotropy of the mixtures with ≥50 vol.% antigorite, whereas olivine CPO dominates at low fractions (∼20 vol.%). The presence of pre-existing microstructures reduces seismic anisotropy of the deformed mixtures, however the persistence of pre-existing CPO in actively subducting slabs remains uncertain, making their significance over geological timescales questionable.

Crystallographic preferred orientation↗

DOE OSTI2025

Elucidating the corrosion mechanism of Ni-based superalloys in the presence of uranium-containing chloride molten salt

The United States Department of Energy (DOE) is committed to the advancement of nuclear reactor technology through initiatives such as the Advanced Reactor Development Program (ARDP), in an effort to diversify the United States energy portfolio towards more sustainable energy options. The ARDP includes demonstration by industry partners of molten chloride fast reactors (MCFRs). Construction of MCFRs requires qualified nuclear structural materials. Unfortunately, there are no current materials that are fully qualified by the Nuclear Regulatory Commission for the construction of molten salt reactors, including MCFRs. Adapting current structural material qualifications requires expansion of our current knowledgebase on the property-performance relationships regarding corrosion performance. In this investigation, we assess microstructural changes in a Ni-based superalloy after exposure to a UCl3¬-containing chloride salt eutectic mixture through a correlated multi-modal approach combining several advanced characterization techniques, including scanning electron microscopy/focused ion beam (SEM/FIB) and transmission electron microscopy (TEM). SEM/FIB analysis will illustrate changes in elemental composition, microstructure, and isotopic information acquired from energy x-ray dispersive spectroscopy (EDS), electron backscatter diffraction (EBSD), and secondary ion mass spectroscopy (SIMS), respectively. This information will then aid in identifying localized regions to elucidate the corrosion mechanism with TEM through a combination of electron diffraction, electron energy loss spectroscopy (EELS), and additional EDS. The findings from this investigation will further expand our assessment of the corrosion performance of structural materials in molten salt chloride systems, aiding to developing fully qualified materials for construction of MCFRs.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Experimental investigation of the dependence of void nucleation and growth on initial microstructure in high-purity titanium under tension

An experimental investigation of failure mechanisms in relation to the initial microstructure in high-purity titanium samples is presented. The initial microstructure of the specimens was measured in 3D using diffraction-contrast tomography (DCT). Ex-situ X-ray computed tomography (XCT) was used to visualize voids in specimens at various levels of deformation attained by interrupted tensile testing. Electron backscatter diffraction (EBSD) mapping was used to characterize the deformed microstructures per specimen. The investigation showed that the location of failures was unrelated to the formation of the first voids, but rather the nucleation and growth of cracks were from heavily deformed surface regions. The areas surrounding the failure-causing cracks had the highest propensity for void development of any area in the specimen. This facilitated crack propagation through the specimen via “linking up”. The failure of the specimens by microvoid coalescence was bolstered by “dimpled” fracture surfaces. Paint composed of gallium embedded in rubber was used to track the displacement of points along the loading direction of the specimens, to relate the location of failure to the material's initial microstructure. However, the correlation proved difficult, due to complex microstructural evolution involving voids, grain fragmentations, and profuse twinning. Nevertheless, it was shown that necking occurred near the largest grain in the gauge section of the specimens. This is likely caused by the decrease in strength of larger grains, causing strain to concentrate in their vicinity. Here, a comprehensive picture of the failure processes in high-purity titanium under axial loading is presented and discussed in the paper.

36 MATERIALS SCIENCE↗

DOE OSTI2025

NSUF RTE completion report for 23-4780: Microstructural Defect Induced Thermal Conductivity Reduction in Uranium Nitride and Thorium Nitride

Uranium nitride (UN) is known to have a higher thermal conductivity than traditional oxide fuels, which could lead to a more efficient energy transport and lower local temperature during its lifetime. But the thermal transport performance of UN in extreme environments has not been systematic studied. This study investigated the irradiation induced microstructural defects in UN and the impacts on thermal conductivity. The samples were produced by spark plasma sintering at University of Texas-San Antonio (UTSA), Los Alamos National Laboratory (LANL), and Idaho National Laboratory (INL). Thermal conductivity of UN before and after 2MeV proton irradiation were measured by using laser metrology at INL in a temperature range of 77-295K. Thermal conductivity measurements in this wide, cryogenic temperature range is critical to understand the phonon scattering mechanisms between the thermal energy carrier, phonons, and different types of irradiation-induced defects. In order to ensure the measurements were conducted in the same grains and minimize the impact of the local heterogeneities, the measurement locations were highlighted by fiducial marks using the focused ion beam (FIB) with grain orientation identified using the electron backscatter diffraction (EBSD) at the Center of Advanced Energy Studies (CAES). Irradiation experiment was conducted at the Ion Beam Laboratory at Texas A&M University (TAMU). A total of 6 samples were irradiated with different irradiation doses and temperatures. After irradiation, the microstructure was characterized by using Transmission Electron Microscope (TEM) at CAES (also in the FIB marks).

36 - MATERIALS SCIENCE↗

DOE OSTI2026

In-situ observations of cyclic deformation in an extruded Mg-2Nd-1Y-0.1Zr-0.1Ca alloy

In this study, the evolution of deformation mechanisms during cyclic loading in an extruded, solution-treated Mg–2Nd–1Y–0.1Zr–0.1Ca alloy was investigated using a combination of in-situ loading, scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), and focused ion beam (FIB) nanofabrication. The initial microstructure exhibited a random crystallographic texture with no preferred grain orientation. Flat, rectangular dog-bone specimens were subjected to load-controlled, fully reversed fatigue for 50 cycles, during which the same region was sequentially mapped to track microstructural changes. After 10 cycles of loading deformation twins were observed. During tensile reloading detwinning or narrowing of those twinned regions occurred. After 20 cycles, detwinning ceased and residual twins remained in the material. SEM imaging revealed numerous surface slip traces after cyclic loading. EBSD-assisted slip trace analysis identified the activation of prismatic and pyramidal < c+a> slip systems during low-cycle fatigue. Site-specific scanning transmission electron microscopy (STEM) further revealed that deformation was also accommodated by basal < a> slip and the dissociation of < c+a> dislocations. Center-of-symmetry (COS) analysis confirmed that the dissociation of < c+a> dislocations resulted in the formation of I₁ intrinsic stacking faults after cyclic loading. These findings provide new insights into the complex interplay of dislocation mechanisms governing fatigue deformation in rare-earth-containing Mg alloys.

Cyclic deformation↗

DOE OSTI2025

Reverse martensitic transformation on the corrosion behavior of a 2304 lean duplex stainless steel

This study investigates the influence of the reverse martensitic transformation on the corrosion behavior of 2304 lean duplex stainless steel (LDSS) at low temperatures (400–600°C). The steel underwent cold rolling, followed by isochronal annealing for 0.5 h. Phase transformations and microstructures were analyzed using X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Corrosion resistance was evaluated using a syringe cell with cyclic potentiodynamic polarization in 0.6 M NaCl solution and double-loop electrochemical potentiokinetic reactivation in 0.5 M H 2 SO 4 + 0.001 M KSCN solution. A bimodal breakdown potential behavior, associated with either pitting or transpassivity, was observed in the as-received (AR) and samples annealed at 400°C. Pitting in the AR sample was associated with Al–Mg–Si–Ca–O inclusions, while pitting on the samples annealed at 400°C was linked to local reduced passive film resistance. Severe cold rolling enhanced the pitting resistance of 2304 LDSS. Selective electrochemical etching revealed preferential corrosion at phase interfaces and within the austenite phase. Additionally, annealing at 500°C to 600°C led to a marked decrease in pitting resistance and increased sensitization. Electron backscatter diffraction analysis of the corroded pits in the annealed specimens indicated that pits tend to nucleate and grow in α'-martensite/austenite regions. Furthermore, the nanostructure formed during low-temperature reversion, characterized by dislocation-cell martensite with high dislocation density and stacking faults, may adversely affect corrosion resistance due to heterogeneities associated with alloying element redistribution.

36 MATERIALS SCIENCE↗

DOE OSTI2024

In-Plane Liftout and Push-to-Pull for In Situ Mechanical Testing of Irradiated Inconel X-750

A streamlined sample preparation method for nanomechanical testing is needed to improve the quality of specimens, reduce the cost, and increase the versatility of specimen fabrication. This work outlines an in-plane liftout focused ion beam (FIB) fabrication procedure to prepare electron-transparent specimens for in situ transmission electron microscopy (TEM) nanomechanical testing. Ion etching and electron backscatter diffraction (EBSD) techniques were used to lift out a [110] oriented grain from a neutron-irradiated bulk X-750 alloy. Careful control of voltages and currents ensured precision. Top surface thinning sweeps prevented resurfacing and redeposition while dog-bone geometries were shaped with a 1:4 gauge width-to-milling pattern diameter ratio. Nanotensile testing in the TEM with a picoindenter allowed for the estimation of an ultimate tensile strength of 2.41 GPa, and inspection revealed a high density of bubbles in the X-750 matrix. The proposed fabrication procedure is significant for preparing samples from radioactive materials, studying complex structures that are orientation-dependent, and analyzing desired planar areas.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Multi-objective surrogate-assisted calibration of CPFEM models using macroscopic response and in situ EBSD measurements of grain reorientation trajectories

Crystal plasticity finite element method (CPFEM) models are widely used to simulate the deformation behaviour of polycrystalline materials, but their calibration is often limited by their high computational cost and the non-convexity of the optimisation landscape. Here, this study develops a multi-objective surrogate-assisted calibration workflow that couples a multi-objective genetic algorithm (MOGA) with an adaptively trained deep neural network (DNN) surrogate model to efficiently identify CPFEM parameters from experimental data. The workflow is demonstrated on three crystal plasticity (CP) formulations of increasing complexity — Voce hardening (VH), two-coefficient latent hardening (LH2), and six-coefficient latent hardening (LH6) — using in situ electron backscatter diffraction (EBSD) measurements of Alloy 617 under uniaxial tensile loading. The CPFEM models are calibrated against the experimentally observed stress–strain response and reorientation trajectories of eight grains, then validated against eight additional trajectories and overall texture evolution. Across the CP formulations, the macroscopic response was reproduced reliably, while differences emerged in the robustness and accuracy of the grain-scale predictions. Including grain reorientation trajectories in the multi-objective calibration improved texture evolution predictions and filtered out physically inconsistent parameter sets that can arise from calibrating against only the stress–strain data. The workflow also demonstrates good transferability of calibrated parameters from a low- to a high-fidelity microstructural model. These results provide practical guidance for integrating in situ microstructural data into CPFEM through efficient, repeatable, and physically meaningful multi-objective calibration.

Crystal plasticity finite element method↗

DOE OSTI2025

Laser‐Powder Melt Pool Solidification Dynamics and Microstructural Engineering of Ti‐5553 Microlattices

The fine geometric and topological control afforded by additive manufacturing technologies has enabled the manufacture of architected materials across length scales, and enabling tunable mechanical performance as a function of local and global design. Progress has been made to tune the mechanical response of architected materials through geometry, but understanding how the geometry and processing conditions will inform the microstructure remains a challenge due to the rapid solidification in laser powder bed fusion. This study uses in situ X-ray imaging and electron backscatter diffraction microscopy to demonstrate that the melt pool size, microstructure morphology, and elastic strain distribution is influenced by a combination of lattice geometry and laser processing conditions. These results indicate that within larger melt pools the local thermal gradients are sufficient to enable a columnar-to-equiaxed transition across the melt pool. Furthermore, the solidification mechanisms producing these microstructures are examined across the first 5 ms of melting and solidification, described via in situ high-speed X-ray imaging and mirrored via multiphysics simulation.

additive manufacturing↗

DOE OSTI2026

Process-driven roadmap for depositing super duplex stainless steel via wire Arc additive manufacturing

Here, this study systematically investigates the effects of shielding gas, bead spacing, weld mode, and travel speed on the phase balance, porosity, and hardness of wire arc additively manufactured (WAAM) super duplex stainless steel (ER2594). Robotic WAAM was employed to fabricate multilayer walls under systematically varied process conditions, followed by phase transformation simulations, X-ray computed tomography (XCT), electron backscatter diffraction (EBSD), and microhardness evaluation. Thermodynamic simulations predicted rapid cooling of AM process can suppress the potential formation of deleterious precipitates which was later validated via cross-sectional microstructure analyses of printed samples. XCT revealed porosity levels below 0.2% for all deposits, with reduced travel speed significantly lowering defect volume. Microstructural analyses revealed the evolution of various austenite precipitates, including grain boundary austenite (GBA), Widmanstätten austenite (WA), and intergranular austenite (IGA), sequentially upon cooling of the ferrite phase. Among all process parameters, weld transfer mode exhibited the strongest influence on phase balance; pulsed mode promoted higher ferrite retention (~ 36%) compared to RapidX mode. No consistent relationship between stabilized phase fraction and captured microhardness was observed. This work provides critical insights for optimizing WAAM parameters to control phase balance and mechanical performance, which is essential for producing high-integrity super duplex stainless-steel components for nuclear and marine applications.

Grain orientation↗

DOE OSTI2025

Microstructure Clones

Background: A material’s microstructure drives its material performance. Contemporary crystal plasticity experiments compare full-field strain measurements of polycrystal specimens to models. Because each specimen is unique, it is impossible to know which features of the observed deformation are deterministic vs statistical; thus, differences between model and experiment may or may not be significant. Objective: This paper introduces the invention of microstructure clones. Microstructure clones are 2D oligocrystal specimens that have nearly identical microstructures to remedy the aforementioned experimental limitations. Having specimens with nearly identical microstructures will allow for multiple destructive tests of a microstructure (either as repeats or intentionally different experiments), an ability to “see the future” by providing insight into how a specimen will deform, variability quantification, and experimental investigations of response to small microstructural changes. Methods: This work introduces microstructure clones. Repeatability of these clones is demonstrated in tensile bars of pure nickel. Local strain measurements from digital image correlation are compared between clone specimens and compared to results from a crystal plasticity finite element model. Results: Two sets of microstructure clones were tested in this study and displayed very consistent deformation responses within each clone set. Small observed differences in deformation invite investigation into microstructure stochasticity and the effect of small microstructural and loading differences. Conclusions: Microstructure clones represent a significant shift in understanding structure–property relationships. This work reshapes experimental crystal plasticity to allow for experiments that control for specific variables, quantification of microstructural stochasticity (and other sources of stochasticity), and opportunities for replicating experiments.

Crystal Plasticity↗

DOE OSTI2025

Microstructural Evolution of Steel During Magnetic Field-Assisted Processing

Advancing magnetic field-assisted processing, as an energy-efficient method for tailoring steel microstructures, requires a thorough understanding of how the high magnetic field impacts microstructural evolution, particularly its effect on prior austenite grain structures. The current investigation of a near-eutectoid composition, Fe-C alloy, uses electron backscatter diffraction to examine the morphology and orientation of martensite and pearlite microstructures, and to reconstruct the parent austenite microstructures present during equivalent heating under varied magnetic field strengths (0-T, 2-T, 5-T, and 9-T). It was observed that the magnetic field has a negligible effect on martensite lath/block width, slightly decreases prior austenite grain size, and increases the fraction of austenite grains with annealing twins. Additionally, the magnetic field increases the phase fraction of proeutectoid ferrite but has a negligible effect on pearlite block size and the distribution of boundary misorientation angles. No preferred texture was induced by the magnetic field, regardless of the applied field direction, in the proeutectoid ferrite phase or the martensite and prior austenite microstructures. Furthermore, the observed results contradict previous literature, and the differences are discussed.

Magnetic Materials↗

DOE OSTI2025

Corrosion Response of Ni-19Cr-5Fe in Molten NaCl-MgCl 2 Salt

Ni-based alloys are strong candidates for use in high-temperature molten salt reactors due to their superior corrosion resistance and mechanical stability compared to stainless steels. In this study, the static corrosion behavior of a Ni-19Cr-5Fe model alloy was systematically evaluated in a purified molten NaCl-MgCl 2 salt at 700°C for 30, 240, and 500 h. Post-exposure analyses were conducted to assess microstructural evolution, corrosion depth, and elemental depletion profiles. Corrosion rates, quantified by chromium depletion depth, followed an inverse power-law trend with increasing exposure time, indicating diffusion-limited kinetics. This trend is attributed to limitations in mass transport in the static salt and to the progressive local depletion of reactive chromium species. Coupled electron backscatter diffraction and energy dispersive X-ray spectroscopy analysis further revealed that the grain boundary character significantly influences corrosion susceptibility: high-angle grain boundaries exhibited pronounced Cr depletion and pitting, while low-angle and Σ3 boundaries remained comparatively resistant. These results offer valuable insight into the role of microstructure in corrosion processes and reinforce the importance of time-dependent material evaluation in molten salt environments relevant to advanced reactor designs.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Direct observation of strain-enhanced hydrogen segregation and failure at high-angle grain boundaries in nickel

Understanding the mechanisms underlying hydrogen embrittlement remains difficult, even in single-element metals. Both microstructure and stress state influence hydrogen distribution in metals and alloys, which impacts deformation and failure. Here, in this work, we use in-situ Kelvin probe force microscopy (KPFM) to monitor the hydrogen distribution in pure nickel over time at 1.1 % and 3.5 % strain. The sample strained to 3.5 % results in preferential hydrogen segregation to high-angle grain boundaries whereas the sample strained to 1.1 % does not exhibit preferential hydrogen segregation. Optical digital image correlation (DIC) shows that hydrogen charging results in both localized and reduced strains during tensile testing of a notched sample. Later stages of deformation and failure (e.g. microcracking) are studied by using in-situ transmission X-ray microscopy (TXM). TXM reveals nanoscale structural changes to a propagating crack in a hydrogen environment. Localized void growth and secondary cracking occur at grain boundaries near the primary crack front. Correlative electron backscattering diffraction (EBSD) is used to relate the cracking at grain boundaries to the hydrogen segregation observed in KPFM. These findings are unified in a proposed hydrogen embrittlement mechanism that describes the interaction of hydrogen with grain boundaries, and the role of grain boundaries in hydrogen embrittlement.

Grain boundary fracture↗

DOE OSTI2026

Emergence of complex-regular eutectic patterns in Al–Ge: Observations from correlative nano-imaging

Eutectic solidification exemplifies nonequilibrium pattern formation, making it a well-studied moving boundary problem. Yet the mechanisms behind the formation of complex-regular microstructures – particularly in highly anisotropic systems with a significant volume fraction of a faceted phase – remain poorly understood. Our understanding of such systems is made complicated by the nonlinear interface kinetics and unique growth dynamics characteristic of faceted phases. To address these challenges, we investigate a model Al–Ge eutectic system, where the faceted Ge phase constitutes a substantial volume fraction (~0.35) and where the two solid phases arrange into so-called “fishbone” or “feather” complex-regular patterns. Using synchrotron-based x-ray nano-imaging and nanotomography with high spatial resolution (22 nm per pixel), we capture in real-time the evolution of the solid–liquid interfaces and the resulting three-dimensional microstructures in this faceted/non-faceted eutectic system. By integrating these observations with electron backscattered diffraction, we elucidate the crystallographic biases on the solidification process and the mechanisms driving the formation of such complex-regular microstructures. These findings inform a new growth model for irregular eutectics in (near-)symmetrical phase diagrams, offering insight on advanced microstructural design and processing strategies. More broadly, we demonstrate how interfacial curvature is generated in irregular eutectic alloys and how it depends on the volume fraction of the faceted phase.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Understanding the influence of boron in additively manufactured GammaPrint®-700 CoNi-based superalloy

Boron is commonly added to superalloys in small amounts to enhance creep resistance, but can lead to cracking at high concentrations, especially during the additive manufacturing process. Two variants of CoNi-based GammaPrint®-700 superalloy with different B contents (0.08 at% vs 0.16 at%) were printed via laser powder bed fusion (LPBF) with the same printing parameters, with only the high B alloy exhibiting solidification cracking. Atom probe tomography (APT) revealed stronger segregation behaviors in the high B alloy compared to the low B alloy at both the inter-dendritic regions and grain boundaries (GBs). The segregation behavior at inter-dendritic regions was well captured with Scheil simulation and can correlate with the existing cracking susceptibility index (CSI) on cracking tendencies, although high angle GBs are where cracking occurs according to electron backscatter diffraction (EBSD) measurements. Additionally, the extent of GB segregation was compared between the high B and low B alloy. Higher B additions led to significantly more GB B segregation in the high B alloy compared to the low B alloy. Further, for the high B alloy, the cracked region of one GB exhibited higher levels of B compared to the uncracked region of the same GB. However, much higher B contents were also found in two other uncracked GBs in the high B alloy, which demonstrates that higher GB B concentrations are not fully responsible for the cracking. A much larger variance in GB B segregation content was found in the high B alloy compared to the low B alloy. These phenomena were explained with a solidification model with the GB segregation content expressed explicitly by a modified Langmuir-McLean equation. This model linked the GB segregation content with solidification undercooling, which can be used as quantitative cracking criteria for future builds.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Bulk-scale stress–strain hysteresis in layered crystalline solids: A study of graphite and Ti 3 SiC 2

Polycrystalline graphite and the MAX phase Ti 3 SiC 2 are layered crystalline solids with similar deformation mechanisms, including basal slip, ripplocation boundaries (RBs), kink boundaries (KBs), and cracking. The interplay of these mechanisms, notably in energy dissipation, has been much discussed in the past twenty-five years. This study builds upon previous work, investigating deformation with a renewed emphasis on the bulk-scale and given recent findings concerning RBs. Our investigation compares the evolution of energy dissipation, nonlinear recoverable and irrecoverable strain, and damage upon increasing stress for graphite and Ti 3 SiC 2 . Benitez et al.’s (2016) methodology of compressive cyclic loading and post-mortem electron backscatter diffraction (EBSD) to assess the prevalence of kinking based on low-angle grain boundaries (LAGBs) was used. Strains were measured with digital image correlation and EBSD was conducted on Ti 3 SiC 2 leveraging dictionary indexing, which was necessary herein to identify LAGBs accurately. The stress–strain stages of Ti 3 SiC 2 agree with literature on Ti 2 AlC. Damage and energy dissipation were more accelerated in graphite. No significant difference was observed in the fraction of LAGBs between pristine and unloaded Ti 3 SiC 2 . Trends observed and EBSD evidence that KBs were not dominant suggest that RBs are the primary dissipator of energy in both materials.

36 MATERIALS SCIENCE↗