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At least 217 records · Page 12

Microstructure and CPO evolution of dynamically recrystallized olivine during complex deformation conditions: a full-field numerical modeling approach

The rheological properties of mantle rocks are strongly dependent on their crystallographic preferred orientation (CPO). Olivine CPO, defined by the orientation of seismically fast [100] axes parallel to flow direction, is also thought to be a dominant contributor to seismic anisotropy in the Earth's upper mantle. However, the amount of deformation needed to overprint a new CPO on a pre-existing fabric and the impact of the inherited CPOs on the transient microstructure evolution, remain unknown. This study employs a full-field numerical approach (VPFFT-ELLE) to explore the dynamic recrystallization and microstructural evolution of olivine polycrystalline aggregates under complex deformation conditions. We test four combinations of successive pure shear and simple shear boundary conditions. Findings indicate that inherited CPOs influence subsequent deformation in a manner dependent on the kinematic relationship between successive stages. In all cases, a minor strain increment (ε ∼0.3–0.6) is sufficient to erase the previous microstructure and CPO. However, when deformation conditions change dramatically (e.g., stretching direction changes orthogonally), the intensity of the new CPO developed is significantly lower and strain distribution are specially altered. During a transient strain stage, pre-existing microstructures undergo extensive reworking, especially when deformation conditions are changed dramatically, such as switching from simple shear to a pure shear condition with a parallel shortening direction relative to the stretching direction. We estimate the significance of these results in interpreting observations of seismic velocity anisotropy, concluding that P-wave seismic anisotropy is significantly and positively correlated with the evolution of olivine CPO with deformation history. This research underscores the transient nature of microstructural rearrangement in olivine aggregates and the necessity for caution in interpreting seismic anisotropy in regions with complex deformation histories, as inherited CPOs can influence current fabric development and induce deviation to the present deformation conditions.

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↗

High-throughput experimentation for microstructural design in additively manufactured 316L stainless steel

In the present study, a combination of high-throughput (HT) and low-throughput (LT) techniques was used to rapidly determine the processing window and generate processing maps for Selective Laser Melting (SLM) of 316L stainless steel. The HT method includes the fabrication of hundreds of hex nut-shaped specimens, each processed with a unique combination of laser power, scanning speed, and hatch spacing. An easily removable scaffolding permitted rapid sample extraction from the base plate, thus saving machining cost and time. Hardness and immersion density measurements were used for HT characterization to identify a processing window for maximum strength and density. Within the defined processing window, a low-throughput (LT) microstructural interrogation of specimens were performed. The microstructural analysis included quantification at various length scales (i.e., grains size and morphology, texture, primary dendrite arm spacing, and melt pool geometry analysis). Microstructure-based processing maps as a function of volumetric energy density were generated. The combination of HT and LT methods produced a predictive relationship between hardness and primary dendrite arm spacing using a Hall-Petch relationship. A model is proposed to explain the dependence of microstructure on the melt pool geometry. Here, the HT method can be applied for the microstructural design of SLM-fabricated components in other alloys.

316L stainless steel↗

Implications of post-processing induced microstructural changes on the deformation and fracture response of additively manufactured Ti–6Al–4V

Ti–6Al–4V parts fabricated via electron beam melting (EBM) powder bed fusion are often subjected to hot isostatic pressing below the β-transus temperature to mitigate defects. During which the pressure aids in pore closure and the thermal exposure results in coarsening of α phase while retaining the columnar prior-β phase grain morphology present in the as-fabricated condition. The same post-processing treatment can also be carried out above β-transus temperature which is an effective way to modify both the grain morphology and the associated α textures. Here, the objective of this work is to correlate thermally induced microstructural changes to the deformation and fracture response of the EBM processed Ti–6Al–4V. To this end, we have carried out both sub-transus and super-transus heat-treatments of the as-fabricated material. The mechanical response of the as-fabricated and all heat-treated materials are characterized by in-situ tensile tests under a high-resolution digital optical microscope. This enabled us to capture large-scale panoramic images of the deforming microstructure, and overcome the trade-off between the image resolution and the field of view during in-situ experiments. The series of images captured throughout the imposed deformation are subsequently used to perform microstructure-based digital image correlation to measure microstructural-scale strains over a large area. The results of the in-situ tests together with detailed fractographic analyses are then used to elucidate how the heterogeneous deformation spanning over multiple microstructural length-scales, for example, at the scale of lamellae, colonies of lamellae and grain boundaries, affect the overall deformation and fracture response of the post-processed materials.

36 MATERIALS SCIENCE↗

Design of a separate effects MiniFuel irradiation experiment investigating microstructure evolution in high burnup UO 2

The microstructural evolution of UO 2 fuel pellets during commercial operation in light water reactors (LWRs) is known to vary significantly across the pellet radius due to spatial variations in local temperature and burnup. The primary obstacle to extending LWR refueling cycles to 24-month intervals is the susceptibility of certain high burnup fuel microstructures to fuel fragmentation, relocation, and dispersal (FFRD) during a loss of coolant accident (LOCA). Although FFRD of the high burnup structure in the rim region of a pellet is well studied, the fine fragmentation that has been observed in a second region, near the midradius of the pellet (termed the “dark zone”) following mock LOCA testing of high burnup commercial fuel rods is less understood. This paper describes the design, analysis, and execution of a separate effects MiniFuel irradiation experiment that aims to identify the specific temperature and burnup regimes under which FFRD-susceptible dark zone microstructures form. The small disc specimens (3 mm diameter by ∼0.3 mm thick) enable more precise control of the relatively uniform temperature and burnup conditions. A total of 42 specimens were fabricated with typical LWR fuel densities (∼96%–98% of theoretical density) and grain sizes (∼12 μm) and are being irradiated over a range of temperatures (600°C–1000°C) and discharge burnups (50–72 MWd/kg-U) that bound the midradius region of high burnup LWR fuel. Fuel specimens with identical 235 U enrichments were inserted in two irradiation locations in the High Flux Isotope Reactor and are currently undergoing irradiation to further evaluate the impact of rate effects (fission rate, time at temperature) on the microstructural evolution. The fuel fabrication and the thermal and neutronic simulations used for designing the experiment are detailed in this paper. A secondary objective of the experiment is to observe fission gas release (FGR) under the various irradiation conditions, and this work provides first-order predictions of FGR from all fuel specimens. The insights gained from these experiments will inform future high burnup core designs that could minimize the formation of susceptible microstructures and ultimately enable 24-month refueling cycles while minimizing the fraction of the fuel susceptible to FFRD.

FFRD↗

Predicting material microstructure evolution via data-driven machine learning

The recent rapid rise in data-driven practices in the materials science domain has led to the development of efficient, generalizable, and accurate approaches for several applications, including: material property prediction, mining (micro)structure- property and (micro)structure-processing relationships, and characterization of material microstructures. Central to the materials science domain is linking microstructure to properties and performance, and critical to building such linkages is understanding how microstructures evolve as a function of environmental exposure or processing conditions (e.g., time, temperature, applied stress or strain, irradiation). This preview article summarizes recent work on the development of recurrent neural networks for predicting spatio-temporal microstructure evolution detailed by Yang et al in their manuscript entitled 'Self-supervised Learning and Prediction of Microstructure Evolution with Recurrent Neural Networks'.

machine learning (ML), materials characterization↗

Scaling CFB risers: Maintaining microstructure dynamics

Over the years there have been numerous approaches to develop a scaleup methodology for circulating fluidized beds. Many of these past approaches have relied on macroscopic definitions of similitude to define dimensionless groups such as Reynolds number, Froude number, density ratios, and dimensional ratios involving different length scales. These approaches have demonstrated various levels of success, but often fail when used outside the bounds of experimental datasets. The issue with these methods is that they rely on macroscopic similitude with the hopes that those conditions would provide microscopic similitude as it does in single phase systems where the Buckingham Pi techniques have given reasonable success. Two of the main reasons for failure are 1) changing fluidization regimes and 2) changing material properties that result in the material falling into a different Geldart group. Both are certain to change the microstructure (local instantaneous volume solids fraction) and changes to the microstructure affect the interphase transport properties of the reactor system, namely the mass transfer and heat transfer. Here, this work presents a new approach towards scaling based upon maintaining similitude at the microscale. It reviews a novel dimensionless flow regime map developed from analysis of the deterministic chaos parameters and higher order moments to ensure microstructure similitude. The work then examines four cases from the literature to assess the scaling approach used: (1) same particle-different scale risers for Geldart Group B particles, (2) Glicksman scaling of atmospheric circulating fluidized bed combustor, (3) same particle-different scale risers for Geldart Group A particles and (4) Glicksman scaling for pressurized gasification. General findings are that none of the scaling approaches produced directly applicable microstructure similar behavior based upon the chaotic and higher moment analysis. The positive take away is that the approach can define scale conditions that will provide similar microstructure that can be us to predict transport behavior.

42 ENGINEERING↗

Microstructural and nanomechanical studies of PVD Cr coatings on SiC for LWR fuel cladding applications

The microstructure and nanomechanical properties of pure Cr coatings deposited on SiC with various physical vapor deposition (PVD) methods have been investigated for the mitigation of hydrothermal corrosion of SiC-SiC f (SiC fiber-reinforced SiC matrix) composite fuel cladding in light water reactors (LWR). Cr coatings (4–7 μm thick) were deposited on unbiased SiC substrates using six variants of magnetron sputtering processes: (i) standard (S-DCMS), (ii) pulsed (P-DCMS), (iii) ion-assisted (I-DCMS), and (iv) pulsed ion-assisted direct current magnetron sputtering (PI-DCMS), (v) high-power impulse magnetron sputtering (HiPIMS), and (vi) bipolar HiPIMS (B-HiPIMS). Microstructural characterization and nanoindentation testing were used to evaluate effects of deposition technique on coating microstructure and nanomechanical properties. The application of positive reverse pulses to the sputter target induced coarsening of the columnar grain structure, while ion bombardment of substrates during deposition promoted densification of the coating microstructure. Both effects are exemplified in B-HiPIMS deposition, resulting in a high-density microstructure with compressive residual stress. Material pile-up around nano-indents and plastic work during nanoindentation were analyzed to understand deformation behavior of the coatings. Finally, the results suggest the B-HiPIMS process to be among the promising methods for the deposition of Cr coatings on SiC-SiC f for LWR cladding application.

36 MATERIALS SCIENCE↗

Accelerating phase-field-based microstructure evolution predictions via surrogate models trained by machine learning methods

Abstract The phase-field method is a powerful and versatile computational approach for modeling the evolution of microstructures and associated properties for a wide variety of physical, chemical, and biological systems. However, existing high-fidelity phase-field models are inherently computationally expensive, requiring high-performance computing resources and sophisticated numerical integration schemes to achieve a useful degree of accuracy. In this paper, we present a computationally inexpensive, accurate, data-driven surrogate model that directly learns the microstructural evolution of targeted systems by combining phase-field and history-dependent machine-learning techniques. We integrate a statistically representative, low-dimensional description of the microstructure, obtained directly from phase-field simulations, with either a time-series multivariate adaptive regression splines autoregressive algorithm or a long short-term memory neural network. The neural-network-trained surrogate model shows the best performance and accurately predicts the nonlinear microstructure evolution of a two-phase mixture during spinodal decomposition in seconds, without the need for “on-the-fly” solutions of the phase-field equations of motion. We also show that the predictions from our machine-learned surrogate model can be fed directly as an input into a classical high-fidelity phase-field model in order to accelerate the high-fidelity phase-field simulations by leaping in time. Such machine-learned phase-field framework opens a promising path forward to use accelerated phase-field simulations for discovering, understanding, and predicting processing–microstructure–performance relationships.

36 MATERIALS SCIENCE↗

Predicting Microstructural Void Nucleation in Discontinuous Fiber Composites through Coupled in-situ X-ray Tomography Experiments and Simulations

Composite materials have become widely used in engineering applications, in order to reduce the overall weight of structures while retaining their required strength. In this work, a composite material consisting of discontinuous glass fibers in a polypropylene matrix is studied at the microstructural level through coupled experiments and simulations, in order to uncover the mechanisms that cause damage to initiate in the microstructure under macroscopic tension. Specifically, we show how hydrostatic stresses in the matrix can be used as a metric to explain and predict the exact location of microvoid nucleation that occurs during damage initiation within the composite’s microstructure. Furthermore, this work provides evidence that hydrostatic stresses in the matrix can lead to coupled microvoid nucleation and early fiber breakage, and that small fragments of fibers can play an important role in the process of microvoid nucleation. These results significantly improve our understanding of the mechanics that drive the initiation of damage in the complex microstructures of discontinuous fiber reinforced thermoplastics, while also allowing scientists and engineers to predict the microstructural damage behavior of these composites at sub-fiber resolution and with high accuracy.

36 MATERIALS SCIENCE↗

Machine learning-based microstructure prediction during laser sintering of alumina

Abstract Predicting material’s microstructure under new processing conditions is essential in advanced manufacturing and materials science. This is because the material’s microstructure hugely influences the material’s properties. We demonstrate an elegant machine learning algorithm that faithfully predicts the microstructure under new conditions, without the need of knowing the governing laws. We name this algorithm, RCWGAN-GP, which is regression-based conditional generative adversarial networks with Wasserstein loss function and gradient penalty. This algorithm was trained with experimental SEM micrographs from laser-sintered alumina under various laser powers. The RCWGAN-GP realistically regenerates the SEM micrographs under the trained laser powers. Impressively, it also faithfully predicts the alumina’s microstructure under unexplored laser powers. The predicted microstructure features, including the morphology of the sintered particles and the pores, match the experimental SEM micrographs very well. We further quantitatively examined the prediction accuracy of the RCWGAN-GP. We trained the algorithm with computer-created micrograph datasets of secondary-phase growth governed by the well-known Johnson–Mehl–Avrami (JMA) equation. The RCWGAN-GP accurately regenerates the micrographs at the trained time series, in terms of the grains’ shapes, sizes, and spatial distributions. More importantly, the predicted secondary phase fraction accurately follows the JMA curve.

08 HYDROGEN↗

Hierarchical microstructure of Yb-filled skutterudites through ultrasonically atomized spherical powders for enhanced thermoelectric performance

Hierarchical microstructures are widely explored as a strategy to reduce lattice thermal conductivity in thermoelectric materials while preserving favorable electronic transport. Here we demonstrate that ultrasonic atomization of precursor powders provides an intrinsic pathway to generate such architectures in n-type Yb0.3Co4Sb12 skutterudites. Materials were synthesized by both conventional sealed-ampoule and ultrasonic atomization routes, each yielding essentially single-phase skutterudite after densification. However, the atomized spherical powders undergo a distinct reaction-driven microstructural evolution during thermal treatment prior to densification. Electron microscopy reveals that the skutterudite phase within the particles induces swelling, cracking, and fragmentation of the droplets before consolidation. Multimodal structural and microstructural characterizations show that densification of these fragmented powders produces a hierarchical microstructure consisting of submicron grains, micrometer-scale faceted crystallites, and powder-derived domains separated by oxide-decorated boundaries. Comprehensive thermoelectric transport measurements evidence that this multiscale architecture lowers the lattice thermal conductivity while maintaining favorable electronic transport, leading to an average ~10% enhancement in the thermoelectric figure of merit. Complementary 121Sb Mössbauer spectroscopy further indicates lattice softening in the atomized material. These results demonstrate that ultrasonic atomization provides an effective route to engineer hierarchical microstructures in skutterudite thermoelectrics and offers a promising strategy for tailoring thermal transport in energy-conversion materials.

Bouteiller, Hugo [ORNL] (ORCID:0009000421322962)↗

Shock-reshock of zirconium to explore the effect of microstructure on the alpha-omega phase transformation

Phase transformations play an important role in the mechanical behavior of materials subjected to extreme loading conditions. A series of shock-reshock experiments were fielded to determine whether the phase transitions in materials are significantly enhanced or inhibited by preexisting microstructural features. Polycrystalline zirconium samples were shock loaded using gas-gun plate impact and soft recovered to examine microstructure using electron backscatter diffraction (EBSD). Drive conditions were varied to study the (hcp) alpha to (hexagonal) omega solidsolid phase transformation. Recovered samples were then subjected to a second shock loading event to determine the change in material behavior as a function of pre-shock microstructure. Crystallography of phase fragments in the final microstructure showed that prior twinning (formed during the shock to a peak stress below the transition threshold) appeared to suppress omega formation/retention after reshock. Conversely, when a material was initially shocked into the omega phase field, retained-omega was not found to have a large impact on subsequent omega formation during reshock. This suggests that nucleation and growth of omega phase are important processes, and the relative activity of nucleation vs. growth processes is modified by a pre-existing substructure. Additionally, orientation relationships reveal a reverse transformation pathway (omega to alpha) dominates the final microstructure, suggesting significant grain growth in the omega phase field is possible even for dynamic timescales.

36 MATERIALS SCIENCE↗

A High-Speed Rotational Diamond Anvil Cell for In Situ Analysis of Hierarchical Microstructural Evolution of Metallic Alloys during Extreme Shear Deformation

High speed shear deformation is ubiquitous in engineering applications, ranging from material processing methods such as friction stir processing/extrusion and in tribological contacts. However, analyzing the microstructural evolution of materials while they are undergoing high speed shear deformation have been a long-standing challenge. This led to predominant reliance on ex situ microscopy before and after shear deformation. But ex situ microscopy lacks the ability to analyze dynamic and transient hierarchical microstructural evolution mechanisms that could occur during shear deformation of materials. Therefore, to better understand the dynamic mechanisms of mass and energy transfer in materials under shear deformation, we developed a first of its kind high-speed rotational diamond anvil cell (HS-RDAC) for synchrotron-based in situ high-energy x-ray diffraction (XRD). We studied the time resolved lattice strain evolution, XRD peak broadening and changes in spatial variation of shear deformation induced alloying in pure metal and metal alloy sheets and powder mixture using the HS-RDAC. These in situ results were combined with detailed ex situ microstructural characterization before and after the shear deformation using transmission electron microscopy and atom probe tomography, which revealed the different stages of evolution of a shear deformation induced hierarchical nanostructure. Multiscale computational simulations including computational fluid dynamics, crystal plasticity, molecular dynamic simulation and density functional theory uncovered the mechanisms behind morphological changes, evolution of defect structures and changes in driving force for shear deformation induced intermixing. In conclusion, this in situ HS-RDAC capability, in combination with ex situ microstructural characterization and computational simulations, can provide new insights into the hierarchical microstructural evolution pathway during shear deformation.

36 MATERIALS SCIENCE↗

Investigation of the relationship between classical and nonclassical ultrasound nonlinearity parameters and microstructural mechanisms in metals

This research studies two nonlinear ultrasound techniques: second harmonic generation and nonlinear resonant ultrasound spectroscopy, and the relationship to microstructural mechanisms in metals. The results show that there is a large change in both the classical, β, and nonclassical, α, ultrasound nonlinearity parameters in response to three specific microstructural mechanisms: precipitate growth in and along the grain boundaries, dislocations, and precipitate pinned dislocations. For example, both β and α increase with the growth of the precipitate radii (precipitate-pinned-dislocations). Additionally, both β and α increase when there is a growth of precipitates in and along the grain boundaries. As expected, β and α decrease when there is a removal of dislocations in the material. The relationship between β and α, and the microstructural mechanisms studied provide a quantitative understanding of the relationship between measured nonlinearity parameters and microstructural changes in metals, helping to demonstrate the possibility of using these two independent, but complementary, nonlinear ultrasound procedures to monitor microstructural damage.

Levy, Katherine Marie Scott↗

Identify the influence of microstructure on mesoscale creep and fatigue damage

This report describes the development of a microstructural model that can quantify the uncertainty in the observed rupture life of Grade 91 steel. The model is microstructural, meaning it relates microstructural characteristics of the material to the resulting material response. As such, one of the uses of this model is to identify the key microstructural parameters controlling the development of damage in Grade 91 operating at elevated temperatures. The report describes two veins of work: improvements to the crystal plasticity model required to run the uncertainty quantification analysis and the results of that UQ analysis. For creep, the model identifies the grain boundary diffusivity as the critical parameter controlling the rupture life of the material. The report demonstrates that a reasonable microstructural distribution of grain boundary diffusivity can account for the observed macroscale variation in rupture life at fixed temperature and load.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Effect of thermal aging and irradiation on microstructure and crack growth response of Alloy 690

Nickel-base Alloy 690 and the associated weld Alloys 52 and 152 are typically used for nozzle penetrations in replacement heads for pressurized water reactor (PWR) vessels, because of their excellent overall resistance to general corrosion and environmental degradation, primarily stress corrosion cracking (SCC). However, many of the existing PWRs reactors are expected to operate for 40-80 years. Likewise, advanced water-cooled small modular reactors (SMRs) will use Ni-Cr alloys and are expected to receive initial operating licenses for 60 years. Hence, the thermal stability of Ni-Cr alloys is a potential concern for the long-term performance of both existing and advanced nuclear plants, and possibly spent fuel storage containers. The objective of this research is to understand the microstructural changes occurring in high-Cr, Ni-based Alloy 690 during long time exposure to the reactor operating temperatures, and the effect of these changes on the service performance. One area of particular concern is the potential for long range ordering (LRO), i.e. formation of the intermetallic Ni 2 Cr phase under prolonged exposure to reactor temperatures and/or irradiation, which can increase strength, decrease ductility, and cause dimensional changes or lead to in-service embrittlement of components made with these alloys. Hence, this research focused on the microstructural evolution and the SCC response of Alloy 690 under accelerated thermal aging and irradiation conditions. The materials studied involved Alloy 690 from two sources: (i) Alloy 690 plate from an Alloy 152 dissimilar metal weld (DMW) joining the Alloy 690 plate to Alloy 533 LAS, aged at three different temperatures (370°C, 400°C and 450°C) for up to 75,000h (equivalent to 60 years of service), and (ii) specimens neutron-irradiated in the BOR-60 reactor up to 40 dpa. For aged Alloy 690 specimens, hardness was found to increase with aging time, however, the microstructural characterization by means of synchrotron X-ray did not find evidence of LRO. The microstructural characterization of neutron-irradiated specimens by TEM found no evidence of LRO either. Testing in a primary water environment of Alloy 690 specimens aged to a 60-year service equivalent revealed a fatigue and corrosion fatigue crack growth responses similar to those measured on the un-aged alloy. The SCC CGR response was also low. Overall, the two Alloy 690 heats investigated in this work, aged up to 60-year service equivalents or exposed to neutron irradiation up to 40 dpa, did not exhibit a deterioration in microstructure or performance.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Initial Microstructure Examination of High Burnup Fuel with Varying Operational Burnups

his report presents an initial examination of the microstructure of high burnup UO 2 under pre- and postloss of coolant accident (LOCA) conditions. This work builds upon work previously conducted on high burnup UO 2 fuel at Oak Ridge National Laboratory. Studying microstructure evolutions that occur in UO 2 during irradiation, particularly in high burnup fuel, will provide a deeper understanding of fuel fragmentation under simulated LOCA conditions. High burnup UO 2 microstructural data is also needed to improve constitutive models intended to predict high burnup fuel fragmentation. The objective of this work is to begin the process of examining high burnup fuel microstructural features before and after LOCA testing to better understand mechanisms driving experimental observations. Several high burnup fuel samples were available from historic fuel shipments to ORNL. These samples were leveraged along with state-of-the-art microscopy capabilities. This report summarizes the current ongoing work using these fuel samples to interpret and analyze high burnup fuel microstructures.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗