Mesoscale model and X-ray computed micro-tomographic imaging of damage progression in ultra-high-performance concrete
Not Available
36 MATERIALS SCIENCE↗
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An investigation of fracture behaviors of NBG-18 nuclear graphite using in situ mechanical testing coupled with micro-CT
Nuclear graphite contains defects spanning from nanoscale basal cracks to sub-mm scale voids. This study aims to establish an experimental method to investigate pre-existing defects and 3-D crack growth inside nuclear graphite, NBG-18. Three-point bending tests were performed on single-edge notched beam specimens with and without coupling with micro-CT. The fracture toughness was measured to be 1.17 ± 0.06 MPa $\sqrt{{m}}$. Cracks were observed to initiate from the pores and thermal cracks on the edge of the notch and then defect or twist to grow along the pre-existing defects. Crack bridging, defection, and twisting were the primary toughening mechanisms. The crack resistance curve exhibited a trend of rising-plateau-rising that can be related to the interaction of crack front and the pre-existing defects. In conclusion, the results highlight the capability of laboratory micro-CT-based experimental method for the visualization of multi-scale defect interactions, which remains to be a challenge in the characterization of nuclear graphite.
36 MATERIALS SCIENCE↗
Micromechanical and fatigue in situ synchrotron characterization of an additively manufactured superalloy with porosity
Additive manufacturing (AM) has the potential to transform component production, but its widespread adoption is constrained by defects, such as pores, that compromise structural integrity. Here, this study investigates the influence of porosity on the micromechanical and fatigue response of AM Inconel 718 (IN718), a widely used aerospace superalloy. One baseline specimen with minimal stochastic porosity and another intentionally seeded with lack of fusion (LOF) pores were examined using high-energy X-ray diffraction microscopy (HEDM) and micro-computed tomography during cyclic loading. Fatigue cracks in the LOF specimen initiated more frequently and at lower cycle counts than in the baseline specimen. The number fraction of fatigue cracks that grew was comparatively higher in the LOF specimen. Grain-level metrics, including stress and diffraction spot widths, were quantified using far-field HEDM. Across the thousands of grains detected in both specimens, the pores in the LOF specimen increased the variability of stress and spot width evolution in the azimuthal direction, the latter serving as a surrogate measure of plastic deformation. However, no correlations emerged between these metrics and grain proximity to fatigue crack initiation sites or pores, underscoring the limitations of grain-averaged metrics for predicting fatigue. Nonetheless, the rich dataset reported here provides a foundation for future modeling efforts.
High-energy X-ray diffraction microscopy↗
Inhibition of Micro-pitting by Tribofilm-Forming ZrO 2 Nanocrystal Lubricant Additives: A Micro-pitting Rig and Transmission Electron Microscope Study
The drive to reduce fuel consumption in transportation has encouraged the emergence of low viscosity lubricants to reduce viscous losses in the engine, drivetrain, and other components. However, viscosity reduction increases the risk of surface damage, thus motivating the development of new anti-wear (AW) additives. Capped ZrO 2 nanocrystals (NCs) in base oils have been shown to form AW tribofilms within microscale sliding contacts. However, the potential of ZrO 2 NCs to protect surfaces subjected to rolling-sliding contact from macroscale damage, such as micro-pitting, remains unexplored. Here, we explore the ability of ZrO 2 NCs to form protective tribofilms under harsh conditions using a micro-pitting rig (MPR), consisting of a three ring-on-roller configuration. The experiments were conducted in polyalphaolephin (PAO) base oil, with and without 5 nm diameter ZrO 2 NCs, at two levels of slide-to-roll ratio (SRR) (30% and 0%) and at variable test durations up to long durations (119 h). MPR results showed the use of ZrO 2 NCs gives rise to the formation of a tribofilm covering the roller surfaces and decreases the initiation and propagation of micro-pits compared to tests in pure PAO base stock. Transmission electron microscopy (TEM) performed on focused ion beam (FIB) milled cross-sectional samples of the roller surfaces revealed the growth of dense and 50–100 nm thick ZrO 2 -based tribofilms independent of (SRR), indicating the potential for robust micro-pitting fatigue protection. Nevertheless, small cracks localized within the near surface region of the roller tested at the most severe conditions (30% SRR and 119 h) were observed. The initiation of these cracks was directly related to the presence of manganese sulphide (MnS) inclusions in the steel, revealed using TEM combined with energy dispersive spectroscopy (EDS). Furthermore, the results highlight the benefits of the protective tribofilms formed by ZrO 2 NCs and suggest approaches for further optimizing their use.
36 MATERIALS SCIENCE↗
Mechanistic Understanding of Interphase-driven Aging in Silicon Anodes
Conventional solid electrolyte interphases (SEIs) strongly adhere to micro-silicon (µ-Si) and crack under volume changes, causing poor cycling performance. Nano-silicon improves cycling performance but remains costly with limited calendar life. Here potentiostatic ageing tests demonstrate that both calendar and cycle ageing are governed by SEI cracking and dissolution with different relative contributions. When the system is not dominated by SEI dissolution, the relative calendar life of Si anodes could correlates positively with their cycle life. LiF-rich SEI that enables long cycle life in µ-Si is therefore expected to enhance calendar life as well. Using this framework, we screened electrolytes, SEIs and electrodes and validated them with full-cell storage. LiF-rich SEI minimizes cracking and dissolution, enabling μ-Si to achieve excellent calendar life, whereas nano-silicon suffers from SEI dissolution and needs reduced electrolyte–electrode contact for better calendar life. This work clarifies calendar-ageing behaviour and accelerates electrolytes and SEI development for long-life Si anodes.
Johnson, Christopher S.↗
In-Situ Visualization of a Growing Brittle Crack in Aluminum Oxynitride Using Synchrotron X-Rays and the Double-Cleavage Drilled Compression Geometry
Brittle fracture is difficult to study in situ due to the speed of a growing crack and the often-catastrophic nature of failure in brittle materials. As a result, the influence of microstructural considerations, such as orientation, grain boundary locations, and strain field, on the crack path remains poorly understood. Presented in this study is a method addressing this knowledge gap, which utilizes the double-cleavage drilled compression geometry to achieve quasi-stable fracture in aluminum oxynitride (AlON). Synchrotron X-ray micro-computed tomography is used to characterize the crack shape and length, while high-energy diffraction microscopy provides information on the strains, orientations, and shapes of grains in the microstructure surrounding the crack tip. During testing, the crack grew in discrete and irregular jumps while the fracture toughness falls within reported ranges. The crack in AlON is found to have no greater tendency to crack intergranularly as compared to transgranularly, and grains which are cracked transgranularly do not display a trend in orientation or stress when compared to those around which the crack followed a grain boundary. The high resolution of the crack path and microstructural data provides a path forward for modeling and understanding 3D brittle fracture.
Gorske, Sara F.↗
On the strength and fracture toughness of an additive manufactured CrCoNi medium-entropy alloy
An additively manufactured (nominally equiatomic) CrCoNi alloy was processed by laser powder bed fusion (LPBF). At ambient temperatures (298 K), this medium-entropy alloy displayed a yield strength, σ y of ~691 ± 9 MPa, and an ultimate tensile strength, σ u of ~926 ± 15.2 MPa; at cryogenic temperatures (77 K), yield and tensile strengths increased respectively to σ y ~ 944 ± 6 MPa and σ u ~ 1382 ± 11 MPa. These strength levels are 57 and 44% higher than that of the wrought alloy, due to strengthening from the solidification cellular structures intertwined with dislocations in the LPBF CrCoNi. The crack-initiation fracture toughness, K JIc was measured to be ~183.7 ± 28 MPa√m at 298 K; this value marginally decreased by ~4% to ~176 ± 11 MPa√m at 77 K. These K JIc values of the LPBF CrCoNi were 11% and 35% lower than the wrought CrCoNi alloy at 298 K and 77 K, respectively. Here, the resistance to crack growth of the LPBF CrCoNi from its hierarchical micro- and meso-structures was evaluated using nonlinear-elastic fracture mechanics by measuring R-curve behavior in the form of the J-integral as a function of crack extension. The specific features of the hierarchical microstructures at different length-scales provide a basis for the strengthening and toughening properties of this additively manufactured medium-entropy alloy. This correlation between the deformation and the hierarchical microstructures at different length-scales may provide future guidance for improving the fracture toughness properties of medium-entropy alloys.
36 MATERIALS SCIENCE↗
Deep learning approaches to semantic segmentation of fatigue cracking within cyclically loaded nickel superalloy
Improvements to synchrotron-based micro-computed tomography scanning capabilities have gifted researchers the ability to characterize 4D material thermomechanical responses more thoroughly than ever before. These advancements, however, have brought about new challenges in analyzing the resulting deluge of data. We report on a nickel-based superalloy specimen imaged 26 times in-situ during cyclic loading at Argonne National Laboratory Advanced Photon Source beamline 1ID, in order to monitor crack growth within the microstructure. Therefore, several deep learning approaches which utilize convolutional neural networks are implemented to segment crack features from reconstructed tomography scans. U-Net architecture implementations are found to be especially effective, achieving IoU = 0.995 +/- 0.004 and Matthews correlation coefficient scores of Φ = 0.826 +/- 0.085. These advancements broaden possibilities for scientists seeking to automate segmentation analyses of similar large datasets.
36 MATERIALS SCIENCE↗
Towards machine-learning a fully-coupled constitutive model for thermal-hydraulic fracture in geothermal systems: phase I (Final Report)
This project, entitled “Towards machine-learning a fully-coupled constitutive model for thermal-hydraulic fracture in geothermal systems: phase I,” addresses challenges in understanding and controlling subsurface fracture networks, which are crucial for applications like deep geothermal heat mining and deep-crustal minerals/metals/hydrogen extraction. The research focuses on advancing the understanding of coupled thermal-hydro-mechanical-chemical (THMC) processes in geologic materials, particularly under the high temperature and pressure conditions found in the deep crust. This seed grant focused specifically on thermal cracking and the development of new constitutive models. Significant progress was made in both experimental and theoretical domains. To study micro-scale fracture formation, the project demonstrated the ability to create thermal cracking under stress in granite samples using a Paterson Gas-medium Deformation Apparatus.
15 GEOTHERMAL ENERGY↗
Understanding intrinsic healing process in cementitious cracks through modeling and experiments
Not Available
36 MATERIALS SCIENCE↗
Direct observations and characterization of crack closure during microstructurally small fatigue crack growth via in-situ high-energy X-ray characterization
This study provides direct observation of the crack closure mechanism of a naturally occurring, tortuous, 3D microstructurally small fatigue crack (SFC) in additively manufactured Inconel 718. In-situ non-destructive characterization is performed using high-energy X-ray diffraction techniques to capture the evolution of the 3D microstructure and micromechanical response in the vicinity of the crack front. Based on the stress state of twelve grains analyzed at the crack tip, the crack closure events of the SFC front was found to be spatially heterogeneous with respect to loading progression governed by the local stress state of the grains (specifically the stress reversal from compression to tension). From this analysis, three grains that displayed different degrees of crack closure were further investigated, based on the orientation of the crack relative to the grains and the associated modality of crack growth. The stress normal to the crack plane and the associated degree of Mode I crack behavior were correlated with events of the crack opening earlier during the loading cycle. This was further corroborated by diffraction spot spreading analysis that quantified the crystallographic lattice distortion caused by the opening crack. Additionally, the detailed characterization of the opening behavior of the grains located at the crack tip and their associated states of stress elucidates the mechanism governing crack closure and will inform future modeling efforts of this phenomenon.
36 MATERIALS SCIENCE↗
Discontinuous micro-fibers as intrinsic reinforcement for ductile Engineered Cementitious Composites (ECC)
Engineered Cementitious Composites (ECC) have demonstrated superior mechanical and durability performance than conventional concrete. In the micromechanical reinforcing system of ECC, fibers play a pivotal role in establishing the ultrahigh tensile ductility and autogenous crack width control. This article reviews the state-of-the-art of discontinuous micro-fibers as intrinsic reinforcement of ECC regarding technical performance as well as environmental and economic impacts. Mechanical properties of ECC made with different micro-fibers, man-made or natural, and their embodied energy, emissions and material cost, are comprehensively surveyed. Further, studies on fiber hybridization are discussed regarding the combination of different types of fibers to form synergetic reinforcements that mitigate total material cost, and potentially enhance the composite performance. Lastly, recommendations on fiber selections are highlighted and directions for future research are suggested.
42 ENGINEERING↗
Heterogeneous fatigue damage in a nickel-based single-crystal superalloy unraveled using correlative 3D X-ray technology
Nickel-based single-crystal (Ni-SX) superalloys under cyclic stress are susceptible to cracking at stress-concentration sites, eventually leading to low-cycle fatigue (LCF) failure. LCF cracks typically originate from intrinsic defects (e.g., voids and carbides) within solidified dendrites. However, systematic quantitative experimental analyses of defect-mediated local damage remain limited. To thoroughly understand the microscopic origins and evolution of LCF damage, correlated 3D mapping of dendrites across various regions is essential. Here, in this study, macroscale micro-computed tomography (μ-CT) was initially used to capture internal interdendritic secondary cracks within bulk DD413 superalloy after LCF testing at 760 °C. Subsequently, a multimodal methodology combining synchrotron 3D microdiffraction (3D-μXRD), high-resolution μ-CT, and electron microscopy was established. This approach allowed precise localization of internal damage zones near interdendritic secondary cracks and detailed mapping of the 3D correlated distributions of dendrites, defects, and residual stress/strain fields within these zones at submicron spatial resolution. Finally, the same approach was applied to specimens subjected to interrupted loading at approximately 40 % of the fatigue life to uncover the early damage states of dendrites. The dendrite cores (DCs) and interdendritic regions (IDs) exhibit microscale heterogeneous mechanical responses: nearly defect-free DCs accumulate local irreversible slip along specific slip systems to generate slip bands, while the IDs containing various defects accommodate local microplasticity through the activation of multiple slip systems around these defects. The local tensile stress near defects in the IDs exceeds that in the DC slip band regions by more than threefold, leading to the generation of local damage zones within the IDs. Chain-like defect distributions facilitate the interconnection of these local zones into a continuous damage region, further elevating the overall tensile stress in the IDs. Additionally, geometrically necessary dislocations alone are insufficient as indicators of LCF damage; both the internal stress state and its magnitude must be considered. These experimental results provide critical data and insights for the development of multi-physics fatigue models.
Localized deformation↗
A two-scale study on the influence of biopolymer enhancement on drying granular materials
Cracking resulting from drying (constrained dehydration) poses a significant challenge in geomaterials, impacting their mechanical performance. To address this problem, extensive efforts have been made to prevent or mitigate the occurrence of cracks, with recent attention focused on the utilisation of biopolymers. This letter investigates the influence of varying concentrations of the xanthan biopolymer on the mechanical response of granular materials, examining both macro and micro scales. The strength changes of the soil were evaluated through desiccation experiments, analysing the appearance and progression of failure on the macro scale. The findings of this study demonstrate that failure (cracking) progression is mitigated and eventually eliminated by increasing the concentration of the additive xanthan. Additionally, capillary experiments were conducted to assess the changes in attraction and the development of capillary bridges on the micro-scale. They indicate that the formation of hydrogel bridges significantly enhances particle attraction, thereby increasing its macro-resistance to cracking.
Engineering↗
Porosity evolution under increasing tension in wire-arc additively manufactured aluminum using in-situ micro-computed tomography and convolutional neural network
Internal defects such as porosities are often formed in additively manufactured metal components. The pores nucleate, grow, and coalesce to form cracks under loads, leading to eventual catastrophic failure. Here, in this paper, the full-field porosity evolution, including pore growth and coalescence in a wire-arc additively manufactured (WAAM) aluminum alloy cylinder under tension is observed with in-situ X-ray micro-computed tomography (μCT). The pore size distribution, density, and tensile stress are calculated from the volumetric images analyzed by a convolutional neural network (CNN) algorithm, which provides rapid analysis of 12,950 slice images from μCT volumetric images at the reference state and 13 tensile strains. The results show the quantitative evolution of the growth and coalescence of macropores under tension. A strong correlation is found between the local pore volume fraction and the true tensile stress when the tensile strain is larger than 5%.
36 MATERIALS SCIENCE↗
Unveiling the structural transformations in glassy solid electrolyte adapted to high-stress cycles
Brittleness of glass–ceramic and ceramic ion conductors is considered as a main roadblock for their implementation as electrolytes in solid-state batteries where the fractures often occur due to the pressure exerted by metallic lithium. In this regard, nano- and micro-scale ductility of the solid electrolyte allows reducing such pressure without formation of cracks. Among different types of solid state ion conductors, phosphate invert glasses seem to be promising in achieving such ductility. We report the mechanical behavior of lithium phosphorous oxynitride (LiPON) invert glass probed by static and cyclic nanoindentation. Repeated application of high intensity stress results in densification and shear deformation of material allowing LiPON to accommodate the ~ 22% nominal strain imposed by the nanoindenter without cracking. Ability to do this under repeated loading indicates robustness of LiPON when used in lithium metal batteries under cyclic charge and discharge. Using Raman spectroscopy with unsupervised K-means clustering we reveal pressure-induced formation of P 2 O 7 units which migrate to the periphery of the residual hardness impressions with cycling resulting in surface morphology of LiPON superficially similar to that of deformed bulk metallic glass.
36 MATERIALS SCIENCE↗
Fracture resistance of hierarchical Cu–Mo nanocomposite thin films
We report the fracture behavior of high-temperature co-sputtered Cu/Mo nanocomposite thin films was investigated through in situ 3-point bend testing of pre-notched microbeams in SEM. The as-synthesized nanocomposites present hierarchical nano/microstructures composed of a matrix of phase-separated Cu–Mo with nanoscale ligaments dispersed with sub-micron scale Cu-rich islands containing Mo nano-precipitates. Results show a significant crack growth resistance in the hierarchical nanocomposite, several times higher than that measured in Cu/Mo nanoscale multilayers. Based on electron microscopy characterization, three mechanisms of crack growth resistance in the hierarchical structures are proposed: crack bridging by the Cu-rich layer, crack deflection via shear along the Cu/Mo interface, and multiple cracking. This work demonstrates an approach to increase toughness in high strength nanocomposites through interface micro-structure design.
36 MATERIALS SCIENCE↗
Materials Characterization: A Primer for Solid Phase Processing Applications
The Pacific Northwest National Laboratory (PNNL) undertook the Materials Characterization, Prediction, and Control (MCPC) Laboratory Directed Research and Development (LDRD) Project to advance understanding of nuclear material processing and enable multifold acceleration in the development and qualification of new material systems produced via advanced manufacturing methods, such as solid phase processing, for use in national security and advanced energy applications (Smith 2021). As a two-year LDRD investment requiring focused research, the MCPC project applied only a subset of the wide range of available destructive and nondestructive characterization methods to provide data to the predictive modeling and data analytics tasks. The purpose of this report is to review a wide range of destructive and nondestructive characterization methods that are relevant in solid-phase processing (SPP) applications, but not necessarily applied in the MCPC Project as a guide to the planning of characterization activities in future research. Particular attention is given to measured characteristics that can correlate to other material characteristics, with a particular interest in nondestructive evaluation (NDE) that can be applied to samples obtained in the MCPC Project. Destructive examinations include tensile tests, optical and electron microscopy, micro-hardness, and residual stress tests. NDE tests include surface visual inspection, eddy current examination for cracks, 4-point potential drop, ultrasound, x-ray, and computed tomography.
36 MATERIALS SCIENCE↗