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At least 613 records · Page 34

Microstructure Scale Lithium-Ion Battery Modeling, Part IV: The Representativity of Microstructure Parameters and Electrochemical Response

Lithium-ion battery electrochemical models require an accurate description of the electrodes microstructures to be predictive, that can be achieved through nanoscale imaging. Such observations are however limited by their field of view (FOV), as they provide only a subset of the whole electrode volume that does not necessarily represent the whole electrode microstructure heterogeneity, and therefore can bias the analysis. A representativity analysis has been performed on the microstructure parameters and, in a novel way, on the full cell electrochemical response to evaluate the predictions representativeness, and thus relevance, of a microstructure scale electrochemical model. The microstructure parameter deviation propagations to the electrochemical response have been quantified for different charge rates. This defines a threshold for the microstructure parameters FOV for a desired maximum deviation of the electrochemical response. Electrochemical model shows cell representative section areas are increasing with C-rate, due to higher in-plane heterogeneities, indicating larger FOVs are required specifically for fast charge modeling. Representativity analysis determines a cell FOV of 144.4 × 154.4 μm 2 is large enough to establish a convergence on the representative section areas for low-intermediate C-rate (≤2.5 C), therefore positively concludes on the model representativeness for these rates, but is not large enough to conclude for higher rates.

25 ENERGY STORAGE↗

Machine learning insights into microstructural origins of transport and mechanical properties in porous microstructures

Multifunctional porous materials are increasingly needed across various fields, but their complex microstructures create significant challenges due to the intricate microstructure-property relationships. This complexity, combined with limitations of traditional analysis methods, hinders efforts to understand and optimize microstructure–property relationships. Here, to address this, we integrate physics-based mesoscale modeling with interpretable machine learning (ML) to uncover how microstructural features govern effective diffusivity and elastic modulus. At constant porosity, we show diffusivity varies by over 150 × and modulus by ∼50 ×, highlighting the power of microstructure engineering. Statistical analysis reveals bimodal behavior in diffusivity and unimodal in modulus. ML identifies connectivity as the dominant factor, while modulus is also sensitive to domain size and feature interactions. Controlled simulations further highlight domain shape as a critical feature for modulus. This framework enables efficient exploration of microstructure-property correlations, offering new insights to guide the design of advanced porous materials.

Bicontinuous microstructure↗

Kinetics of small single particle combustion of zirconium alloy

We present quantitative kinetic information regarding small, 1-10 {mu}m in diameter, single particle combustion of Zr-rich metal alloy foils subjected to either mechanical impacts or laser-ablation. The lights from combustion of metal fragments were recorded on a high-speed camera. The particle size was determined by the motion analysis of individual particle trajectory based on an aerodynamic drag law and further verified by the microstructure and chemical composition analysis of recovered post-burn particles. The measured particle sizes show a log-normal distribution centered at around 3.1 {mu}m in diameter, and the composition of recovered particles is that of fully oxidized ZrO{sub 2}. The temperature evolution of each particle along the space/time-trajectory is determined based on the thermal emission from combustion using a single-color photographic spectro-pyrometry. The result indicates that the particle has reached the maximum combustion temperature of 4000 K, well beyond the melting temperature of ZrO{sub 2}, and undergone the solidification of molten ZrO{sub 2} during the cooling stage. It also shows that the maximum combustion temperature decreases linearly with increasing the particle diameter, following the correlation t aD{sup 1.5-1.8} between the burn time (t) and the particle diameter (D). Combining the particle size, the burn time, and the particle temperature, both temperature and mass burn rates are obtained as a function of particle size. As the particle size increases, the temperature burn rate decreases, whereas the mass burn rate goes in the opposite direction.

36 MATERIALS SCIENCE↗

Volumetric analysis and mesh generation of real and artificial microstructural geometries

Producing a viable finite element mesh of realistic microstructural structural geometry is a critical step in analyzing the thermo-mechanical behavior of complex multi-material composites. Advancements in imaging technology such as micro computed tomography have allowed modelers to access high resolution mesoscale geometries for direct numerical simulation. However, converting from voxel based 3D images to usable finite element meshes has been challenging. A robust method including algorithms and software scripts for generating finite element meshes from 3D imaged microstructures is presented in this paper. It includes a routine for inserting cohesive elements around material interfaces to enable modeling of interface properties including delamination and damage. The algorithms and procedures presented in this method leverage currently available software packages for processing surface based geometry into volume based meshes. In addition to converting real geometry from physical imaging systems, algorithms for producing numerically generated and statistically equivalent microstructural geometry are also included. These artificial microstructures can be a valuable resource for modelers when physical specimens do not exist or are limited in quantity: Method establishes a workflow from voxel data to viable finite element mesh including interface information, and Includes a method for synthetic geometry generation based on metrics from real microstructures.

36 MATERIALS SCIENCE↗

Pre-Irradiation Comparison of W-Based Alloys for the PHENIX Campaign: Microstructure, Composition, and Mechanical Properties

Tungsten is the material of choice as the plasma-facing material in future plasma-burning fusion reactors. During operation, plasma-facing materials will be simultaneously exposed to 14-MeV neutrons, low-energy D/He particles, and high heat loads. Neutron irradiation of tungsten results in bulk material damage, including knock-on damage causing loops and voids, and transmutation reactions leading to the transmutation of tungsten to rhenium and osmium. Under irradiation to high dose, Re and Os atoms can amalgamate into precipitates that drastically alter the material properties, noticeably increasing the hardness. However, the early-stage development of Re and Os precipitates under a fast neutron spectrum has not been investigated.In this work, the microstructure and hardening behavior of W-Re alloys containing 0 to 2.2 wt% Re, TiC-doped W, and powder-injection-molded W are investigated prior to neutron irradiation at 500ºC and 800ºC to ~0.1 displacement per atom in the High Flux Isotope Reactor (HFIR) to establish a baseline understanding of the starting microstructures.Transmission electron microscopy analysis indicates a dislocation-heavy microstructure, and scanning transmission electron microscopy–energy dispersive spectroscopy shows no spatial segregation of Re and W. Similarly, surface compositional studies performed with electron backscatter diffraction and X-ray photoelectron spectroscopy showed no presence of Re, indicating the Re did not segregate or form new phases during fabrication. Here, the alloys in their as-fabricated state showed no Re segregation or second-phase development, with no significant differences between their microstructures and Vickers hardness values.

36 MATERIALS SCIENCE↗

Microstructural Characterization and Simulation of High Temperature Inelastic Deformation and Fracture of Al-Li 2070

A combined experimental and simulation investigation is carried out to characterize the high temperature deformation behavior of a recently developed Al-Li alloy, AA2070, over a temperature range including typical forging temperatures. Focus is placed on providing explanations for the temperature-dependent plastic and fracture behavior observed for this material using macroscale tensile tests, microscale imaging and analysis, and physics-based micromechanical modeling. It is shown that AA2070 experiences non-monotonic elongation to failure with a rise in temperature. Detailed fractography and microstructural analysis, including dynamic recrystallization analysis, provide insight into this interesting and practically useful behavior. In addition, a validated crystal plasticity model is called upon to explain the unique texture observed in the necked region of the ductile tensile specimen. The insights provided by this investigation will allow improved design of high temperature forming operations for AA2070 and similar alloys which can extend the application of third generation Al-Li alloys.

36 MATERIALS SCIENCE↗

Microstructure reconstruction of battery polymer separators by fusing 2D and 3D image data for transport property analysis

A new approach to generate high-fidelity 3D microstructure reconstructions by leveraging resolution and sample volume characteristics from 2D and 3D microscopy methods is presented here. This approach is employed to model the microstructure of a highly orthotropic polypropylene separator used in lithium-ion batteries, which have challenging multi-scale features of fibrils (<100 nm) and lamellae (>100 nm) to resolve in 3D. Phase contrast nano X-ray computed tomographic data are used to reconstruct the lamellae phase, while 2D scanning electron microscopy data are used to characterize sub-100 nm microstructure features such as the thin fibrils that are beyond the effective resolution of X-ray computed tomography. Fibril geometries are reconstructed stochastically based on the 2D higher resolution data, and integrated with the lamellae geometries in 3D space. Transport property analyses are performed to investigate the bias of microstructure models without considering the fibrils. A sensitivity study is also conducted to facilitate understanding of the relationship between microstructure characteristics and transport properties.

25 ENERGY STORAGE↗

Simulation-guided analysis of resonant soft X-ray scattering for determining the microstructure of triblock copolymers

Resonant soft X-ray scattering (RSoXS) probes structure with chemical sensitivity that is useful for determining the morphology of multiblock copolymers. However, the hyperspectral scattering data produced by this technique can be challenging to interpret. Here, in this study, we use computational scattering simulations to extract the microstructure of a model triblock copolymer from the energy-dependent scattering from RSoXS. An ABC triblock terpolymer formed from poly(4-methylcaprolactone) (P4MCL), poly(2,2,2-trifluoroethylacrylate) (PTFEA), and poly (dodecylacrylate) (PDDA), P4MCL-block-PTFEA-block-PDDA, was synthesized as the model triblock system. Through quantitative evaluation of simulated scattering data from a physics-informed set of candidate structure models against experimental RSoXS data, we find the best agreement with hexagonally packed core–shell cylinders. This result is also consistent with electron-density reconstruction from hard X-ray scattering data evaluated against electron-density maps generated with the same model set. These results demonstrate the utility of simulation-guided scattering analysis to study complex microstructures that are challenging to image by microscopy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effect of stress evolution on microstructural behavior in U-Mo/Al dispersion fuel [Effect of stress on microstructural evolution in U-Mo/Al dispersion fuel]

U-Mo/Al dispersion fuel irradiated to high burnup at high power (high fission rate) exhibited microstructural changes such as deformation of the fuel particles, pore growth, and rupture of the Al matrix. The driving force for these microstructural changes was meat swelling caused by a combination of fuel particle swelling and interaction layer growth. Five miniplates with well-recorded fabrication data and irradiation conditions were selected, and their PIE data was analyzed. ABAQUS finite element analysis (FEA) was utilized to simulate the microstructural evolution of the plates. Using the simulation results shear stress, effective stress and hydrostatic stress exerted on both the fuel particles and the Al matrix were determined. The effects of fabrication and irradiation variables on stress-induced microstructural evolutions, such as pore growth in the interaction layers and Al matrix rupture, were investigated. The observed microstructural changes were consistent with the calculated stress distribution in the meat.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

X-ray computed tomography of microstructure evolution during matrix impregnation and curing in unidirectional fiber beds

Microstructural evolution during axial impregnation and subsequent curing of a preceramic polymer in unidirectional ceramic fiber beds is studied using X-ray computed tomography. The principal goal is to identify connections between void locations, void sizes, local fiber bed porosity, fiber movement, and impregnation conditions. The degree of saturation after impregnation is found to increase with instantaneous capillary number. But, because of the need to create pathways for gas escape during curing, fiber beds with high saturation after impregnation show the largest reductions in saturation during curing. Notwithstanding, saturation after curing increases with instantaneous capillary number. Voids tend to form in the largest channels between fibers, where the local fiber bed porosity is high, during both impregnation and curing. Here, void formation is typically accompanied by fiber movement that increases both the local fiber bed porosity near voids and the overall non-uniformity in the fiber bed, as measured by local porosity entropy.

(A - Material) fibers↗

Retained austenite thermal stability in a nanostructured bainitic steel

The unique microstructure of nanostructured bainite consists of very slender bainitic ferrite plates and high carbon retained austenite films. As a consequence, the reported properties are opening a wide range of different commercial uses. However, bainitic transformation follows the T{sub 0} criteria, i.e. the incomplete reaction phenomena, which means that the microstructure is not thermodynamically stable because the bainitic transformation stops well before austenite reaches an equilibrium carbon level. This article aims to study the different microstructural changes taking place when nanostructured bainite is destabilized by austempering for times well in excess of that strictly necessary to end the transformation. Results indicate that while bainitic ferrite seems unaware of the extended heat treatment, retained austenite exhibits a more receptive behavior to it. - Highlights: • Nanostructured bainitic steel is not thermodynamically stable. • Extensive austempering in these microstructures has not been reported before. • Precipitation of cementite particles is unavoidable at longer austempering times. • TEM, FEG-SEM and XRD analysis were used for microstructural characterization.

36 MATERIALS SCIENCE↗

Effect of TiO{sub 2} additives to the sintering of Y{sub 2}O{sub 3}

The effect of sintering additive on the microstructure development of yttrium oxide was investigated. Different combinations of yttrium oxide with TiO{sub 2} were used as x-ray diffraction, differential thermal analysis (DTA) were sintering additive. The investigated and microstructure of resulting compacts were characterized by, using scanning electron microscopy, porosity and sintering density for all compacting samples sintered at different sintering temperature under static air.

36 MATERIALS SCIENCE↗

Quantitative description of microstructure defects in hexagonal boron nitrides using X-ray diffraction analysis

A routine for simultaneous quantification of turbostratic disorder, amount of puckering and the dislocation and stacking fault density in hexagonal materials was proposed and tested on boron nitride powder samples that were synthesised using different methods. The routine allows the individual microstructure defects to be recognised according to their effect on the anisotropy of the X-ray diffraction line broadening. For quantification of the microstructure defects, the total line broadening is regarded as a linear combination of the contributions from the particular defects. The total line broadening is obtained from the line profile fitting. As testing material, graphitic boron nitride (h-BN) was employed in the form of hot-isostatically pressed h-BN, pyrolytic h-BN or a h-BN, which was chemically vapour deposited at a low temperature. The kind of the dominant microstructure defects determined from the broadening of the X-ray diffraction lines was verified by high resolution transmission electron microscopy. Their amount was attempted to be verified by alternative methods. - Highlights: • Reliable method for quantification of microstructure defects in BN was suggested. • The method is based on the analysis of anisotropic XRD line broadening. • This XRD line broadening is unique and characteristic of the respective defect. • Thus, the quantification of coexistent microstructure defects is possible. • The method was tested on hexagonal BN, which was produced by different techniques.

36 MATERIALS SCIENCE↗

Effect of powder layer thickness on the microstructural development of additively manufactured SS316

By Increasing the powder layer thickness we could increase material deposition rates and reduce build times during laser powder bed fusion (LPBF). However, increasing the powder layer thickness could also negatively affect the local melting and subsequent microstructure of the printed material. This study systematically investigated, for the first time, the defect evolution and microstructural changes of LPBF stainless steel 316 (SS316) processed by using various powder layer thicknesses of 40, 80, and 120 μm while also varying the laser dwell time for the pulsed laser. Through image analysis, the pore density was found to increase with increasing powder layer thickness, particularly when the dwell time was too high or too low. The maximum achievable density (>99%) was found over a wide processing window when using the smallest powder layer thickness of 40 μm between dwell times of 60 and 100 μs. Increasing the powder layer thicknesses to 80 and 120 μm resulted in maximum densities of 98.7 and 96.8%, respectively, but the window for acceptable laser dwell times that could achieve these densities narrowed considerably. A microstructural analysis of the melt pools was performed to measure the melt pool depths and widths, both of which increased with increasing dwell time. However, increasing the powder layer thickness did not affect the melt pool depth and only minorly affected the width. A sub-grain cellular structure distinguished the melt pool boundaries. The cell size increased with increasing dwell time and decreasing powder layer thickness. Moreover, the cell size was used to calculate a cooling rate that had a magnitude of 10 7 K/s and increased with increasing powder layer thickness.

36 MATERIALS SCIENCE↗

Assessment of MARMOT Grain Growth Model

This report assesses the MARMOT grain growth model by comparing modeling predictions with experimental results from thermal annealing. The purpose here is threefold: (1) to demonstrate the validation approach of using thermal annealing experiments with non-destructive characterization, (2) to test the reconstruction capability and computation efficiency in MOOSE, and (3) to validate the grain growth model and the associated parameters that are implemented in MARMOT for UO 2 . To assure a rigorous comparison, the 2D and 3D initial experimental microstructures of UO 2 samples were characterized using non-destructive Synchrotron x-ray. The same samples were then annealed at 2273K for grain growth, and their initial microstructures were used as initial conditions for simulated annealing at the same temperature using MARMOT. After annealing, the final experimental microstructures were characterized again to compare with the results from simulations. So far, comparison between modeling and experiments has been done for 2D microstructures, and 3D comparison is underway. The preliminary results demonstrated the usefulness of the non-destructive characterization method for MARMOT grain growth model validation. A detailed analysis of the 3D microstructures is in progress to fully validate the current model in MARMOT.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Study of microstructure and silicon segregation in cast iron using color etching and electron microprobe analysis

An investigation on silicon segregation of lamellar, compacted and nodular graphite iron was carried out by applying a selective, immersion color etching and a modified electron microprobe to study the microstructure. The color etched micrographs of the investigated cast irons by revealing the austenite phase have provided data about the chronology and mechanism of microstructure formation. Moreover, electron microprobe has provided two dimensional segregation maps of silicon. A good agreement was found between the segregation profile of silicon in the color etched microstructure and the silicon maps achieved by electron microprobe analysis. However, quantitative silicon investigation was found to be more accurate than color etching results to study the size of the eutectic colonies. - Highlights: • Sensitivity of a color etchant to silicon segregation is quantitatively demonstrated. • Si segregation measurement by EMPA approved the results achieved by color etching. • Color etched micrographs provided data about solidification mechanism in cast irons. • Austenite grain boundaries were identified by measuring the local Si concentration.

36 MATERIALS SCIENCE↗

Microstructure, strengthening mechanisms and hot deformation behavior of an oxide-dispersion strengthened UFG Al6063 alloy

An ultrafine-grained Al6063/Al{sub 2}O{sub 3} (0.8 vol.%, 25 nm) nanocomposite was prepared via powder metallurgy route through reactive mechanical alloying and hot powder extrusion. Scanning electron microcopy, transmission electron microscopy, and back scattered electron diffraction analysis showed that the grain structure of the nanocomposite is trimodal and composed of nano-size grains (< 0.1 {mu}m), ultrafine grains (0.1-1 {mu}m), and micron-size grains (> 1 {mu}m) with random orientations. Evaluation of the mechanical properties of the nanocomposite based on the strengthening-mechanism models revealed that the yield strength of the ultrafine-grained nanocomposite is mainly controlled by the high-angle grain boundaries rather than nanometric alumina particles. Hot deformation behavior of the material at different temperatures and strain rates was studied by compression test and compared to coarse-grained Al6063 alloy. The activation energy of the hot deformation process for the nanocomposite was determined to be 291 kJ mol{sup -1}, which is about 64% higher than that of the coarse-grained alloy. Detailed microstructural analysis revealed that dynamic recrystallization is responsible for the observed deformation softening in the ultrafine-grained nanocomposite. - Highlights: Black-Right-Pointing-Pointer The strengthening mechanisms of Al6063/Al{sub 2}O{sub 3} nanocomposite were evaluated. Black-Right-Pointing-Pointer Hot deformation behavior of the nanocomposite was studied. Black-Right-Pointing-Pointer The hot deformation activation energy was determined using consecutive models. Black-Right-Pointing-Pointer The restoration mechanisms and microstructural changes are presented.

36 MATERIALS SCIENCE↗