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At least 811 records · Page 45

Microstructure development during rapid alloy solidification

Abstract Solidification processing of structural alloys can take place over an extremely wide range of solid–liquid interface velocities spanning six orders of magnitude, from the low-velocity constitutional supercooling limit of microns/s to the high-velocity absolute stability limit of m/s. In between these two limits, the solid–liquid interface is morphologically unstable and typically forms cellular-dendritic microstructures, but also other microstructures that remain elusive. Rapid developments in additive manufacturing have renewed the interest in modeling the high-velocity range, where approximate analytical theories provide limited predictions. In this article, we discuss recent advances in phase-field modeling of rapid solidification of metallic alloys, including a brief description of state-of-the-art experiments used for model validation. We describe how phase-field models can cope with the dual challenge of carrying out simulations on experimentally relevant length- and time scales and incorporating nonequilibrium effects at the solid–liquid interface that become dominant at rapid rates. We present selected results, illustrating how phase-field simulations have yielded unprecedented insights into high-velocity interface dynamics, shedding new light on both the absolute stability limit and the formation of banded microstructures that are a hallmark of rapid alloy solidification near this limit. We also discuss state-of-the-art experiments used to validate those insights. Graphical abstract

36 MATERIALS SCIENCE↗

Development of a Novel Magnesium Alloy for Thixomolding® of Automotive Components (Final Report)

Magnesium (Mg) alloy die-castings are increasingly used in the automobile industry to achieve cost effective mass reduction, especially in systems where multiple components can be integrated into a single thin wall die-casting. However, there are several component quality restrictions in thin-walled Mg die castings, including variability in dimensional accuracy, part-to-part variation in mechanical properties, and porosity in the final part, which has limited the continued growth of die-cast components in the automobile industry. An alternative to die-casting is the process of thixomolding®. While the die-casting process relies on filling a mold at high speeds with the alloy in the completely molten state, the thixomolding® process fills a mold with a thixotropic alloy in a semi-solid slurry state at a temperature between the liquidus and solidus temperatures. Ideally, the material should be ~30–65% solid rather than being completely liquid at the beginning of the injection process. Advantages of the thixomolding® process include a finer grain structure, lower porosity, improved dimensional accuracy, improved part-to part consistency, improved mechanical properties, particularly ductility in the component, the ability to reduce wall thickness for mass savings, and longer tool life due to lower process temperatures. The objective of this collaborative project between Oak Ridge National Laboratory, FCA US LLC, and Leggera Technologies was to develop one or more novel Mg alloys more suitable for thixomolding® automotive structural components than the current die-casting alloys used for this process. The primary interest was to improve ductility while maintaining tensile and fatigue strengths, as these are properties that are critical for use in body and chassis structural applications. Since good corrosion resistance is also desirable for this application, this property was also considered when evaluating promising alloy compositions. An initial evaluation of existing components thixomolded® using AM60 was performed and microstructure, and tensile properties were evaluated for the baseline alloy. Targets were established for ease of processing (characterized by the melting range defined as the difference between the liquidus and the solidus), strength, and ductility. Computational modeling was used to identify promising alloys and selected alloys were cast in laboratory scale heats. Properties measured from laboratory scale heats were used to down-select two alloys for further evaluation and component fabrication. Two alloys were prepared in industrial scale heats, cut into small pieces (chips), and thixomolding® trials were initiated. Trial components were successfully fabricated using one alloy composition, but it was concluded that further refinement of the thixomolding® process parameters are required to successfully fabricate component using second alloy. Microstructure and mechanical properties were evaluated on the material removed from the fabricated component and properties were compared to the baseline alloy. Although mechanical properties of the alloys showed improvement over the baseline alloy, it was determined that modifications to the thixomolding® process would result in better microstructure control with further improvement in properties leading to successful commercialization. A provisional patent application has already been filed on the new alloys developed as part of the project.

36 MATERIALS SCIENCE↗

Microstructure and in-service degradation of baffle former bolts – in-core components of light water reactors

This report presents a microstructure evaluation of the baffle former bolt, a commercial pressurized water reactor component. Using SEM, EDS, and EBSD analysis the material was identified as AISI 316 steel with an annealed austenite microstructure. Findings include abnormal grain growth in a fraction of the grains and the absence of retained ferrite. Notable observations include an overlapping of pre- and post-irradiation deformation, including defect-free channel formation as an active deformation mechanism in the near-surface layer of BFB. Specimen surfaces, exposed to high-temperature, high-pressure water, exhibited signs of in-service corrosion degradation. EBSD and EDS analyses highlighted intergranular corrosion, possible grain boundary oxidation with depths less than 3 µm, and, unexpectedly, short cracks filled with Cr-rich oxides measuring around 5-6 µm. The presence of defect-free channels from EBSD data suggests episodes of high mechanical stresses during service. The specimens provide a potentially unique insight into the in-service degradation of NPP components, strain localization, and crack initiation processes. An intact corrosion layer reveals a complex component's in-service history. Further research is underway for a detailed analysis.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Understanding the microstructural evolution of hypersaline cemented paste backfill with low-field NMR relaxation

Highlights: • Microstructural evolution of CPB, prepared with tap and hypersaline water, is monitored using low-field NMR relaxometry. • T{sub 1} and T{sub 2} NMR relaxation measurements compared with mechanical strength via UCS tests • Hypersaline mixing water results in slower structural evolution and lower mechanical strength. Cemented paste backfill (CPB) comprising mineral tailings, binders and mixing water is an important potential support material in the mining industry. As the mechanical properties of CPB are significantly influenced by its microstructural characteristics the development of measurement tools to better understand its pore structure evolution is important for its increased utilisation. This study reports the application of low-field nuclear magnetic resonance (NMR) relaxation time measurements to characterise the microstructural evolution of CPB materials over 56 days of hydration, contrasting common tap water and hypersaline water (~22 wt% salt) as mixing water. Distinct NMR relaxation time populations were evidenced within each CPB sample, revealing the presence of both capillary (T{sub 1,2} ≈ 10 ms) and gel pore water (T{sub 1,2} ≈ 300–500 μs), with time-dependent relaxation measurements facilitating characterisation of capillary pore structure evolution over the hydration period assessed. Hypersaline samples demonstrated a time-lag in this measured capillary pore evolution, relative to those hydrated with tap water, while pore structure evolution rates were observed to increase with increased CPB binder content. Further, both T{sub 1} and T{sub 2} NMR relaxation times were found to correlate with the uniaxial compressive strength of the CPB materials investigated, facilitating the formulation of a predictive correlation function between NMR relaxation characteristics and mechanical properties.

36 MATERIALS SCIENCE↗

Multiscale characterization and comparison of historical and modern nuclear graphite grades

Beginning with Chicago Pile I, graphite has been used as a moderator material in nuclear power stations and is considered a potential material for use in future Generation IV advanced reactors. The microstructure of graphite is responsible for much of its mechanical and thermo-physical properties, and how it responds to irradiation. To understand graphite microstructure, it is necessary to understand its porosity at the macro- and micro-scales; and to understand its porosity, it is necessary to characterize the morphological connectivity of the void content and the two main phases of graphite: filler and binder. Here, using several microscopy and analytical techniques, a detailed examination of the heterogeneity, microstructure and pore structure of different graphite grades and their binder and filler phases is presented. Significant differences were found between coarser and finer nuclear grades. Coarse grades have a more diverse range of filler particles, pores and thermal cracks. Finer grades have a more well-defined pore size distribution, fewer variations of filler particles sizes and do not contain as many large thermal cracks. Fine grades tend to have a well-connected network of pores whereas coarser grades contain a larger content of closed porosity. The framework developed within this work can be applied and used to assess the various graphite grades that would down-select materials for specific use in graphite moderated reactor designs.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Unraveling kinking: A plasticity enhancing failure mode in high strength nano metallic laminates

Kinking is an important and plasticity-enhancing deformation/failure mode in numerous mechanically anisotropic materials including high-strength nano metallic laminates (NMLs). However, our current limited understanding of the mechanics of kinking and its dependence on microstructural attributes is insufficient for thoroughly comprehending and eventually being able to control failure behaviors of materials. In this study, we investigate kinking dependencies on microstructural attributes in NMLs via in situ micropillar compression, multiscale microstructure characterization, dislocation dynamic simulations, and crystal plasticity modeling. Additionally, by examining several NML systems (Cu/Fe, Ag/Fe, Al-4Mg/Fe), we demonstrate that the development of internal stresses during loading activates local layer-parallel glide triggering kinking in NMLs. Furthermore, this work reveals the effect of key microstructural features including layer thickness, layer waviness, interface barrier strength, and work hardening capacity on kink band formation in NMLs. More broadly, our efforts represent a generically applicable approach for probing large-strain deformation behavior of complex materials via synergetic modeling and experimental efforts.

36 MATERIALS SCIENCE↗

3D micromechanical simulation of PBX composites

Previous research studied the constitutive response and interface strength of a bonded bicrystal system containing two HMX explosive grains bound with a HTPB polymer binder by performing FE simulations on real geometry imaged with micro Computed Tomography (µCT). The parameters generated from this past study were successfully applied to 2D mesoscale simulations of µCT imaged HMX-HTPB polycrystal samples. Presently, the mechanical response of PBXs containing a Nitro-Plasticized Estane (NPE) binder with similar microstructural geometry to the HMX-HTPB polycrystal samples were studied. Imaging of a HMX-NPE bicrystal sample allowed for simulation of the new material pairing. However, imaging using µCT techniques on the new polycrystal samples was difficult due to the decrease in contrast between the HMX grains and the NPE binder. Mesoscale polycrystal simulations utilizing a single µCT imaged microstructure were performed on a 3D representative volume element (RVE) comparing the delamination behavior and mechanical response of both HMX-HTPB and HMX-NPE PBXs. Furthermore, this technique shows the ability to virtually explore the mechanical response of a range of hypothetical materials that share common microstructural geometric characteristics in addition to studying numerically altered geometries.

36 MATERIALS SCIENCE↗

Development of grain-scale slip activity and lattice rotation fields in Inconel 718

Using a combination of in-situ high-resolution digital image correlation (HR-DIC), Heaviside-DIC method (H-DIC), and crystal plasticity finite element (CPFE), we investigate the evolution of intragranular lattice rotations and slip activity during monotonic and cyclic loading in a high performance, polycrystalline face centered cubic material. The CPFE employs a quasi-3D model microstructure, which is a highly resolved mirror representation of the experimental in-situ test sample. In agreement, the measurements and calculations reveal that most grains, regardless of their size and lattice orientation, develop intragranular lattice rotation gradients that span the grain. For a small cluster of grains on the deformed material, we perform HR-DIC analysis of slip lines to demonstrate agreement in the active slip systems and changes in this local slip activity across the individual grains. The combined analysis reveals that deforming grains are divided into sub-granular regions of uniform lattice rotation and these regions are most often associated with only one or two active slip systems. The gradient lines that divide them correspond to changes in the predominant slip system. The model is used to examine the evolution of intragranular lattice rotation in a single fully reversed tension-compression cycle. The calculations indicate that intragranular gradients intensify during the reverse loading path as nearest neighboring regions appear to shed lattice rotation, increasing the lattice rotation in some regions, while shutting down rotation in neighboring regions. So these findings provide insight into the irreversible changes that develop within deforming grains at the scale of the grain, particularly the heterogeneous development of intragranular lattice rotation in early stages of deformation, which could serve as precursors to localization.

36 MATERIALS SCIENCE↗

Extreme shear-deformation-induced modification of defect structures and hierarchical microstructure in an Al–Si alloy

Abstract Extreme shear deformation is used for several material processing methods and is unavoidable in many engineering applications in which two surfaces are in relative motion against each other while in physical contact. The mechanistic understanding of the microstructural evolution of multi-phase metallic alloys under extreme shear deformation is still in its infancy. Here, we highlight the influence of shear deformation on the microstructural hierarchy and mechanical properties of a binary as-cast Al-4 at.% Si alloy. Shear-deformation-induced grain refinement, multiscale fragmentation of the eutectic Si-lamellae, and metastable solute saturated phases with distinctive defect structures led to a two-fold increase in the flow stresses determined by micropillar compression testing. These results highlight that shear deformation can achieve non-equilibrium microstructures with enhanced mechanical properties in Al–Si alloys. The experimental and computational insights obtained here are especially crucial for developing predictive models for microstructural evolution of metals under extreme shear deformation.

36 MATERIALS SCIENCE↗

Effect of focused nanosecond laser pulse irradiation on microtribological properties of diamond-like films

We have examined the effect of focused nanosecond laser pulses on the formation and tribological properties of microstructures in the form of a matrix of craters produced in a – C : H : Si : O diamond-like films (DLFs), both undoped and doped with tungsten. The studies are performed by scanning probe microscopy (SPM) using SPM probes of standard design with a tip and probes without a tip (tipless-type probes). A special procedure is developed for assessing the wettability (contact angle) of individual sections of the laser-induced microstructure by the local adhesion force. According to estimates, the material inside the crater becomes softer and more hydrophobic as a result of laser irradiation. This is manifested to the greatest extent in tungsten-doped DLFs, where the crater walls are arranged like terraces formed by ‘nanoflakes’, i.e. grains of the substance. Scanning of microstructures with a tipless probe in the regime of lateral force microscopy demonstrates a decrease in friction in the crater area. (interaction of laser radiation with matter. laser plasma)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Design and development of equi-atomic refractory High Entropy Alloys for use in radiation environments

Development of new structural materials that can withstand the extreme environments of nuclear reactors where the materials are exposed to high dose rate of ~ 30 200 dpa, high temperatures of the order of 500 1000 o C and tens of years of operation is vital for exploiting the “smallest carbon footprint energy source” to its fullest, in order to deal with the energy crisis worldwide. Recently, HEAs have shown superior irradiation properties over conventional alloys like higher resistance to defect formation, lower void swelling, limited irradiation hardening and higher microstructural stability under irradiation, making them potential structural material candidates for reactors. Proper characterization and testing of these materials are essential before they can replace the conventional alloys.

36 MATERIALS SCIENCE↗

Equilibrium and non-equilibrium effects in high pressure phase transformations of carbon

The behavior of carbon in the range 1–100 GPa and 1–10 kK is central to problems in planetary interiors, inertial confinement fusion targets, and high-pressure synthesis of carbon-based materials, but experiments in this regime are difficult and often provide only indirect constraints on phase behavior. As a result, phase boundary loci, structure, and limits of metastability at high pressure remain uncertain. In this work, machine-learning enhanced atomistic simulations are used to address this knowledge gap. We determine the melt line up to 100 GPa, the graphite-diamond phase boundary up to the melt line, and analyze structure of the coexisting phases. We show that the coexisting liquid evolves smoothly with pressure without evidence for a first-order liquid–liquid transition. Orientation-resolved graphite melting simulations indicate that basal-plane interfaces develop a dewetting layer and undergo layer-by-layer melting, producing kinetic hysteresis and an apparent orientation dependence of the melt line. Non-equilibrium quenches from the melt are used to construct a kinetically limiting graphite–diamond phase boundary for rapid quenches from above the melt line, and show that graphite is metastable at pressures of up to ≈ 25 GPa. These results provide bounds on equilibrium and metastable behavior in carbon relevant for interpreting high-pressure experiments and for designing synthesis pathways to specific carbon microstructures.

Lyu, Yanjun [Department of Materials Science and E↗

In situ measurement of damage evolution in shocked magnesium as a function of microstructure

Accurate modeling and prediction of damage induced by dynamic loading in materials have long proved to be a difficult task. Examination of postmortem recovered samples cannot capture the time-dependent evolution of void nucleation and growth, and attempts at analytical models are hindered by the necessity to make simplifying assumptions, because of the lack of high-resolution, in situ, time-resolved experimental data. We use absorption contrast imaging to directly image the time evolution of spall damage in metals at ~1.6-μm spatial resolution. We observe a dependence of void distribution and size on time and microstructure. The insights gained from these data can be used to validate and improve dynamic damage prediction models, which have the potential to lead to the design of superior damage-resistant materials.

36 MATERIALS SCIENCE↗

Characterizing mechanical and microstructural properties of novel montmorillonite-rich polyethylene composites

Montmorillonite (MMT) clays are important industrial materials used as catalysts, chemical sorbents and fillers in polymer–clay nanocomposites. The layered structure of these clays has motivated research into further applications of these low-cost materials, including use as ion exchange media and solid-state ionic conductors. In these applications, the mechanical properties of MMT are key when considering long-term, reliable performance. Previous studies have focused on the mechanical properties of nanocomposites with MMT as the minority component or pure MMT thin films. In this work, the microstructure and mechanical properties of pure MMT and majority MMT/polyethylene composites pressed into dense pellets are examined. Characterization methods such as X-ray diffraction, atomic force microscopy and scanning electron microscopy together with nanoindentation reveal important structure–property relationships in the clay-based materials. Here, utilizing these techniques, we have discovered that MMT processing impacts the layered microstructure, chemical stability and, critically, the elastic modulus and hardness of bulk MMT samples. Particularly, the density of the pellets and the ordering of the clay platelets within them strongly influence the elastic modulus and hardness of the pellets. By increasing pressing force or by incorporating secondary components, the density, and therefore mechanical properties, can be increased. If the layered structure of the clay is destroyed by exfoliation, the mechanical properties will be compromised. Understanding these relationships will help guide new studies to engineer mechanically stable MMT-based materials for industrial applications.

36 MATERIALS SCIENCE↗

Directed energy deposition of radially functionally graded nickel based superalloys IN625 and IN738: Microstructure and mechanical properties

This study investigates the microstructure and mechanical properties of radially functionally graded (RFG) materials fabricated from nickel-based superalloys IN625 and IN738 using directed energy deposition (DED). RFG cylindrical deposits with radial gradients of IN625-IN738 and IN738-IN625 were successfully fabricated and confirmed to be crack-free through tailored composition grading, scan strategy and process parameters that minimized thermal gradients and solidification velocities. Microstructural analysis revealed distinct variations across the gradient, characterized by differences in dendrite arm spacing, microsegregation, and the formation of distinct γ' precipitates and carbide/boride phases (MC, M 6 C, M 2 C, and MB 2 ) in as-deposited (AD) conditions, which evolved into M 23 C 6 and M 2 B upon subsequent heat treatment (HT). EBSD showed predominant columnar grains with a [100] texture, while microhardness profiles demonstrated consistent variation across the gradients. Mechanical testing highlighted the synergy of the graded structure, combining IN738's strength with IN625's ductility, resulting in enhanced properties such as a yield strength of 1131 MPa, ultimate tensile strength of 1382 MPa, and elongation of 12 % for HT IN625-IN738 grading. Numerical simulations employing CALPHAD thermodynamic calculations and finite element thermal modeling are used to establish phase evolution and microstructural feature correlation with thermal profiles, aiding in the optimization of process-structure-property relationship.

Additive manufacturing↗

Predicting extreme anisotropy and shape variations in impact testing of tantalum single crystals

We report recent Taylor cylinder impact tests carried out for Ta single crystals showed strong variations in dimensional changes for different crystallographic directions aligned with the cylindrical axis. In order to capture the effect of crystallography on the deformation characteristics and final shapes of the impacted cylinders, a single crystal material subroutine is adapted and embedded in the solid mechanics/dynamics Finite Element solver Abaqus to simulate the aforementioned single crystal Ta Taylor impact experiments. Details of the coupled model implementation, and insights on the role played by single crystal anisotropic flow on the deformation behavior across a broad range of strain rates and temperatures for different single crystal orientations are presented and discussed. We demonstrate the predictive capability of the adopted crystal plasticity model to capture the significant role played by crystal orientation-induced anisotropy, as well as strain hardening and adiabatic heating, on the dynamic deformation response of crystalline materials. This re-emphasizes the need of microstructure-aware models to improve the accuracy of simulations for high-consequence engineering design.

36 MATERIALS SCIENCE↗

Bridging Nano- and Microscale X-Ray Tomography for Battery Research by Leveraging Artificial Intelligence

X-ray computed tomography (CT) is a non-destructive imaging technique in which contrast originates from the materials' absorption coefficient. The recent development of laboratory nanoscale CT (nano-CT) systems has pushed the spatial resolution for battery material imaging to voxel sizes of 50 nm, a limit previously achievable only with synchrotron facilities. Given the non-destructive nature of CT, in situ and operando studies have emerged as powerful methods to quantify morphological parameters, such as tortuosity factor, porosity, surface area and volume expansion, during battery operation or cycling. Combined with artificial intelligence and machine learning analysis techniques, nano-CT has enabled the development of predictive models to analyse the impact of the electrode microstructure on cell performances or the influence of material heterogeneities on electrochemical responses. In this Review, we discuss the role of X-ray CT and nano-CT experimentation in the battery field, discuss the incorporation of artificial intelligence and machine learning analyses and provide a perspective on how the combination of multiscale CT imaging techniques can expand the development of predictive multiscale battery behavioural models.

diagnostics↗

Rapid Simulation of Irradiation Damage in PWR Internals (NSUF 2019 Milestone Report)

This document summarizes the progress made by Oak Ridge National Laboratory (ORNL) in collaboration with the University of Michigan on “Rapid Simulation of Irradiation Damage in PWR Internals,” a research project led by the University of Michigan and supported by US Department of Energy Office of Nuclear Energy Nuclear Science User Facilities Consolidated Innovative Nuclear Research program. In this reporting period, samples that were exposed to combined neutron and ion irradiation were prepared and shipped to the University of Michigan for further analysis. This report summarizes the specimen preparation performed at ORNL’s Low Activation Materials Development and Analysis facility. The benchmarking work of microstructural characterization on reactor-irradiated samples with different dose levels was completed.

36 MATERIALS SCIENCE↗