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At least 415 records · Page 23

Evolution of dislocation substructures in metals via high-strain-rate nanoindentation

Deformation at high strain rates often results in high stresses on many engineering materials, potentially leading to catastrophic failure without proper design. High-strain-rate mechanical testing is thus needed to improve the design of future structural materials for a wide range of applications. Although several high-strain-rate mechanical testing techniques have been developed to provide a fundamental understanding of material responses and microstructural evolution under high-strain-rate deformation conditions, these tests are often very time consuming and costly. In this work, we utilize a high-strain-rate nanoindentation testing technique and system in combination with transmission electron microscopy to reveal the deformation mechanisms and dislocation substructures that evolve in pure metals from low (10 –2 s –1 ) to very high indentation strain rates (10 4 s –1 ), using face-centered cubic aluminum and body-centered cubic molybdenum as model materials. The results help to establish the conditions under which micro- and macro-scale tests can be compared with validity and also provide a promising pathway that could lead to accelerated high-strain-rate testing at substantially reduced costs.

36 MATERIALS SCIENCE↗

Radiation damage of a two-dimensional carbon fiber composite (CFC)

Carbon fiber composites (CFC) are, among other applications, already in use as low-impedance collimating elements for intercepting TeV-level protons machines, like the CERN Large Hadron Collider. Towards a comprehensive understanding of these materials’ properties and behavior, a series of radiation damage campaigns have been undertaken in order to quantitively investigate the response of AC-150 K CFC to high proton fluences. The CFCs dimensional changes, stability, micro-structural evolution, and structural integrity below and above 5 × 10 20 p/cm 2 fluence threshold were studied. The irradiating particles were protons of kinetic energies in the range of 130–200 MeV. The effects of the irradiation temperature (~90–180°C and 280–500°C) combined with the proton fluence on the dimensional stability and the microstructural evolution of this anisotropic two-dimensional composite structure were studied using precision dilatometry and X-ray diffraction. Our results shed light on the fluence-based limitations for these composite materials. Furthermore, we compare these results with reference unirradiated graphite, and we discuss the similarities and differences in the dimensional changes and post-irradiation annealing properties.

36 MATERIALS SCIENCE↗

Mirostructure Characterization of Friction Consolidated Copper-Nickel using a Machine Learning Approach: Developing Process to Microstructure Associations

Friction consolidation (FC) is a solid phase processing approach where discrete material forms such as powders, chips, nuggets, etc. are densified via shear deformation. The precursors are placed in a billet container and brought in contact with a rotating tool that applying the desirable amount of normal force. Under the combined action of the rotation and normal pressure, the discrete precursor is consolidated through porosity reduction and shear deformation. FC is increasingly being studied as an attractive approach to manufacturing fully dense parts from powder forms owing to its ability to mix, alloy and consolidate difficult-to-process precursors in minimal number of process steps. Material consolidation and deformation in shear consolidation processes have been studied extensively previously for different material combinations previously. However, despite the extensive research in this area, understanding of the mechanistic processes in pore consolidation, deformation-induced mixing and material solubility during FC is still evolving. Material development using solid phase processing approaches such as FC is often performed based on research experience/education, which can be biased. Conventional analysis and simulation tools in this area tend to be successful only when material thermodynamic pathways and microstructural evolution sequences resulting from processing are clearly defined or known. They are not as effective for emerging advanced manufacturing technologies where material evolution pathways are not well established. The ability to predict optimal process parameters based on material chemistry and bulk properties is essential to accelerate materials design and processing, as are an understanding of the relevant structure-processing-property relationships. These structure-processing-property-performance relationships are at the core of materials science research. Microstructure characterization provides the link to these four core areas, often through visualizing material microstructure using imaging techniques. However, linking microstructure image data (i.e., micrographs) to variables of interest (e.g., processing parameters, material chemistry) in a reproducible, generalizable, and quantitative manner is a significant challenge. Typically, quantitatively linking image data to processing history relies on significant domain knowledge and manual or subject matter expert (SME)-heuristic based image analysis. Such an approach to image analysis has the potential to be biased, inefficient, and difficult to replicate.

36 MATERIALS SCIENCE↗

Annealing influence on the microstructure of irradiated U-Mo monolithic fuel foils

In this study we compared the microstructure evolution of U-Mo fuel foils produced with and without heat treatment at low burn-up via advanced post-irradiation examination. The aim of this study is to observe after irradiation the ways in which the fabrication processes have influenced fuel behavior at early-stage irradiation, as for very low burn up microstructural studies are lacking. In this work it was observed that the larger grain size detected in the heat-treated samples before irradiation led to decreased grain refinement after irradiation. Grain refinement was associated with the presence of small nano-size bubbles and precipitates. This phenomenon is hypothesized to influence early fuel swelling during reactor irradiation. Grain refinement was also observed to increase in regions where γ-U decomposition was present. Thus, it was enhanced in the samples fabricated without heat treatment. The heat treatment also increased the thickness of the U-Mo/Zr interface, namely of the UZr 2 layer. However, the influence of this layer on fuel performance needs further investigation. On one side, it may contribute to better mechanical bonding; on the other, it may influence swelling and blistering in the interaction layer as porosity increases when this layer is increased. This was observed especially in the presence of increased area containing low Mo concentration, and thus containing a higher fraction of the α-U phase, which is highly susceptible to irradiation induced swelling. Strong evidence of reverse transformation under irradiation (α-U + γ'-U2Mo → bcc γ-U) was observed in these samples. While the precipitates (carbides and oxide) seem to be unaffected by the irradiation at these low burnups. However, further analyses are necessary at higher burn-up to assess the exact impact different heat treatments have on fuel performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Process-Structure-Property Relations for As-Deposited Solid-State Additively Manufactured High-Strength Aluminum Alloy

Solid-state additive manufacturing methods provide innovative solutions to circumvent problems associated with materials susceptible to hot cracking by avoiding liquid solid phase transformations. In this work, the process parameter influence on microstructural evolution and mechanical response of a fully dense aluminum alloy 7050 (AA7050) component manufactured via a rapid, solid-state additive manufacturing process known as Additive Friction Stir Deposition (AFS-D) was quantified for the first time. Three sections (starting dwell, transient, crossover of roads) of the deposition that exhibit differing thermomechanical processing histories were evaluated for the resulting microstructure and mechanical response. The microstructural characterization was performed on the as-deposited AA7050 via Electron Backscatter Diffraction (EBSD), TEM, optical microscopy, and Scanning Electron Microscopy (SEM). The microstructural characterization revealed refined constituent particles and grains throughout the as-deposited AA7050 microstructure. Furthermore, quasi-static tensile experiments were conducted in both the build and transverse directions, in order to quantify the orientation influence on tensile properties of the as-deposited AA7050 build. Spatially dependent tensile properties were observed in the material due to heat input variation coarsening of secondary phases towards the initial layers of the AFS-D build. Post-mortem analysis revealed that voids nucleated and coalesced from the overgrowth of the strengthening precipitates present in the material, resulting in fracture.

36 MATERIALS SCIENCE↗

Simulation and analysis of small angle scattering (SAS) patterns of Ni-based superalloy microstructures generated by a phase-field model

This paper investigates the relationship between microstructural features and small-angle scattering (SAS) patterns in Ni-based superalloys using a combined phase-field and SAS simulation approach coupled with microstructure analyses. The simulated SAS patterns accurately capture key experimental observations previously reported in the literature, including the time-dependent transition from circular to square-shaped precipitates and the development of anisotropic SAS patterns. Importantly, our analysis reveals the correlations between characteristic length scales extracted from SAS profiles and microstructural descriptors, such as precipitate size and inter-precipitate distance. These findings provide a comprehensive understanding of the link between SAS profiles and microstructure evolution in Ni-based superalloys, offering valuable insights for materials characterization and design.

Microstructure↗

Radiation driven diffusion in γU-Mo

A monolithic fuel design based on a U-Mo alloy has been selected as the fuel type for conversion of the United States High-Performance Research Reactors (HPRRs). A critical phenomenon of interest with U-Mo monolithic fuel is the large amount of swelling that takes place during operation, particularly at high fission densities. The accurate prediction of fuel evolution under irradiation requires implementation of correct thermodynamic and kinetic properties into mesoscale and continuum level fuel performance modeling codes. One such property where there exists incomplete data is the diffusion of relevant species under irradiation. Fuel performance swelling predictions rely on an accurate representation of diffusion in order to determine the rate of fission gas swelling and the local microstructural evolution. In this work, we present molecular dynamics simulations of the radiation driven diffusion of U, Mo and Xe in U-Mo nuclear fuels. Diffusion coefficients for each species are determined over a range of temperatures and compositions. In this work, updated diffusion coefficients are presented that are applicable under irradiation that incorporate both intrinsic and radiation driven diffusion.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

In situ synchrotron tensile investigations on ultrasonic additive manufactured (UAM) zirconium

The microstructure evolution during room temperature uniaxial tensile straining of ultrasonic additive manufactured (UAM) zirconium was evaluated using the Advanced Photon Source (APS) facility. Miniature dog-bone tensile specimens of two orientations were cut from a UAM-fabricated zirconium bar for in situ synchrotron tensile tests. Wide-angle X-ray scattering (WAXS) scanning was used to unveil the changes in microstructure of the entire gauge regions throughout the straining. A series of WAXS data analysis methods were utilized to quantify both elastic and plastic deformation mechanisms within the strained specimens. Stress concentrations were identified during early stages of plastic deformation, which become candidate necking positions and eventually lead to failure. Additionally, fracture surface analysis implied that these stress concentration locations may be correlated to the fabrication defects, providing insightful guidance for future improvements of the UAM zirconium fabrication process.

36 MATERIALS SCIENCE↗

Evaluation of microstructural changes in fresh cement paste using AC impedance spectroscopy vs. oscillation rheology and 1H NMR relaxometry

AC impedance spectroscopy (ACIS) is a promising technique for monitoring the microstructure evolution of fresh cement paste in real-time. This paper compared the change of bulk electric resistivity (ρ{sub bulk}) obtained from ACIS with the developments of storage modulus (G′) and the mean transverse relaxation times (T{sub 2}) of fresh Portland cement pastes within 5 h. It was found that the three different phases (Phase I, II, and III) on the microstructural build-up process of fresh paste can be accurately distinguished by analyzing ρ{sub bulk}, as well as G′ and T{sub 2}. The use of ρ{sub bulk} fails to characterize the microstructural changes in Phase I due to the great sensitivity on the electrical conductivity of the interstitial solution. However, it can successfully reflect the developing features of microstructure in Phases II and III, and reliably evaluate the impacts of water to cement ratio, superplasticizer, and supplementary cementitious materials on the microstructural development.

36 MATERIALS SCIENCE↗

In Situ Synchrotron Tensile Investigations on Ultrasonic Additive Manufactured (UAM) Zirconium

The microstructure evolution of ultrasonic additive manufactured (UAM) zirconium under room temperature uniaxial tensile straining is reported. Miniature dog-bone tensile specimens of two orientations were cut from a UAM zirconium bar for in situ synchrotron tensile tests. Wide-angle X-ray scattering (WAXS) scanning at the Advanced Photon Source (APS) at Argonne National Laboratory was used to unveil the changes in microstructure of the entire gauge regions throughout the straining. A series of WAXS data analysis methods were utilized to quantify both elastic and plastic deformation mechanisms within the strained specimens. Stress concentrations were identified during early stage of plastic deformation, which become candidate necking positions and eventually lead to failure. Fracture surface analysis implied that these stress concentration locations may be correlated to the fabrication defects, providing insightful guidance for future improvement of the UAM zirconium process.

36 MATERIALS SCIENCE↗

Controlling phonon lifetimes via sublattice disordering in AgBiSe 2

Understanding and controlling microscopic heat transfer mechanisms in solids is critical to material design in numerous technological applications. Yet, the current understanding of thermal transport in semiconductors and insulators is limited by the difficulty in directly measuring individual phonon lifetimes and mean free paths, and studying their dependence on the microscopic state of the material. Here in this paper, we report our measurements of microscopic phonon scattering rates in AgBiSe 2 , which exhibits a controllable, reversible change directly linked to microstructure evolution near a reversible structural phase transition, that directly impacts the thermal conductivity. We demonstrate a steplike doubling of phonon scattering rates resultant from the cation disordering at the structural transition. To rationalize the neutron scattering data, we leverage a stepwise approach to account for alterations to the thermal conductivity that are imparted by distinct scattering mechanisms. These results highlight the potential of tunable microstructures housed in a stable crystal matrix to provide a practical route to tailor phonon scattering to optimize thermal transport properties.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Modeling Ni redistribution in the hydrogen electrode of solid oxide cells through Ni(OH) 2 diffusion and Ni-YSZ wettability change

Ni redistribution in the hydrogen electrodes of solid oxide cells is an important degradation mechanism. Its driving force is still under debate. This work focuses on the interplay between Ni(OH) 2 diffusion and Ni-YSZ wettability change. With a Ni(OH) 2 diffusion model developed in our previous work, we further employ three models for the Ni-YSZ contact angle to quantify the Ni-YSZ wettability change. The microstructure evolutions in a reconstructed Ni-YSZ electrode are simulated under selected experimental operating conditions. It is shown that the phenomenological model can capture the driving force of Ni spreading/detachment on YSZ surface and the Ni migration reported in experiments can be qualitatively reproduced through the competition between Ni(OH) 2 diffusion and Ni-YSZ wettability change. It is also found that the initial microstructure of the active layer and the microstructure characteristics in the support layer can strongly affect the distribution of steam partial pressure and overpotential, hence the Ni redistribution, in the active layer, which may explain the inconsistencies in experiments. Further, our results show that there are two missing pieces in current theory of Ni redistribution: a mechanism of fast Ni diffusion under humid atmosphere and the physical reason behind the Ni spreading/detachment.

25 ENERGY STORAGE↗

Role of microstructure on flux expulsion of superconducting radio frequency cavities

The trapped residual magnetic flux during the cool-down due to the incomplete Meissner state is a significant source of radio frequency losses in superconducting radio frequency cavities. Here, in this study, we clearly correlate the niobium microstructure in elliptical cavity geometry and flux expulsion behavior. In particular, a traditionally fabricated Nb cavity half-cell from an annealed poly-crystalline Nb sheet after an 800 °C heat treatment leads to a bi-modal microstructure that ties in with flux trapping and inefficient flux expulsion. This non-uniform microstructure is related to varying strain profiles along the cavity shape. A novel approach to prevent this non-uniform microstructure is presented by fabricating a 1.3 GHz single cell Nb cavity with a cold-worked sheet and subsequent heat treatment leading to better flux expulsion after 800 °C/3 h. Microstructural evolution by electron backscattered diffraction-orientation imaging microscopy on cavity cutouts, and flux pinning behavior by dc-magnetization on coupon samples confirms a reduction in flux pinning centers with increased heat treatment temperature. The heat treatment temperature-dependent mechanical properties and thermal conductivity are reported. The significant impact of cold work in this study demonstrates clear evidence for the importance of the microstructure required for high-performance superconducting cavities with reduced losses caused by magnetic flux trapping.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Synergistic Effects of Molten Salt Corrosion and Proton Irradiation on Grain Boundary Strength in Ni-20Cr

Nickel-based alloys are leading contenders for use as structural materials in molten salt reactors. While there have been extensive studies on the impact of fluoride/chloride-based molten salt corrosion on the microstructural evolution of various nickel-based alloys, the effects of simultaneous molten salt corrosion and radiation on the mechanical integrity of grain boundaries (GBs) remain underexplored. In this study, we use a Ni-20Cr model alloy to investigate this issue, subjecting it to simultaneous molten fluoride salt corrosion and proton irradiation. We performed cross-sectional and chemically-sensitive electron microscopy characterization of the microstructures of these materials, identifying the characteristic corrosion-induced microstructure and local chemical heterogeneity near GBs. After developing a sample preparation method for reliable characterization of GB strength, we assess the mechanical degradation of GBs using in situ push-to-pull micro tensile tests. Our findings reveal that voids induced by corrosion are the primary influence on the failure mode of GBs, regardless of whether proton irradiation is present. For materials that exhibit ductile fracture, those subjected to simultaneous corrosion and radiation exhibit lower yield strengths than those exposed to corrosion alone, which may be linked to the previously observed phenomenon of proton irradiation-decelerated intergranular corrosion in molten salt.

36 - MATERIALS SCIENCE↗

Symposium MT02: Statistical Mechanics-Based Computational Tools for the Study of Phase Transformation in Complex Materials (Final Report)

Symposium MT02 brought together a diverse and interdisciplinary community of scientists specializing in Statistical Mechanics-based computational modeling to investigate phase transformations in materials exhibiting complex disordered structures. As the demand for materials with extreme performance metrics grows—from aerospace components to next-generation optical fibers—the ability to predict microstructural evolution under non-equilibrium conditions has become paramount. The primary goal of this symposium was to identify, evaluate, and discuss advanced computational tools capable of designing precise manufacturing conditions to tailor material properties efficiently. By fostering a dialogue between computational theorists and experimentalists, the symposium sought to establish new protocols for predicting how processing history—such as cooling rates or strain paths—dictates the final microstructure.

36 MATERIALS SCIENCE↗

Defect formation and transmutation behaviors in irradiated tungsten under thermal-neutron shielded and mixed spectrum conditions

Here, this study investigates the microstructural evolution of pure tungsten irradiated under thermal-neutron shielded and mixed spectrum conditions in the High Flux Isotope Reactor (HFIR). Four samples were irradiated at temperatures from 570 °C to 1130 °C up to 0.73 dpa. Neutron spectrum significantly influenced the accumulation of transmutation products, with Re+Os content estimated at ∼0.3–0.6% under thermal-neutron shielded conditions and ∼5.2% under the mixed spectrum condition. Irradiation temperature strongly influences tungsten’s microstructure, with dislocation loops and fine voids forming at lower temperatures and only larger voids and Re/Os segregation observed at higher temperature. Under thermal-neutron shielded conditions, dislocation loops and voids were observed at 570 °C and 790 °C. At the highest irradiation temperature (1130 °C), dislocation loops were no longer observed, while larger but less dense voids remained. Re and Os segregation to void surfaces was evident at 790 °C and 1130 °C, though no precipitation was observed. In contrast, under the mixed-spectrum condition, both spherical and needle-like Re/Os-rich precipitates were observed, frequently accompanied by large voids. Dislocation loops were not observed, but loop-like contrast within the precipitates suggests they may have nucleated on pre-existing loops. Irradiation-induced hardening was assessed for the shielded samples at 570 °C and 790 °C. Dispersed barrier hardening (DBH) analysis, based on TEM-resolved defects, revealed that voids were the dominant contributors to hardening, consistent with literature results. A schematic model is proposed to describe defect and precipitate evolution in tungsten under fusion-relevant transmutation-to-dpa conditions.

Dislocation loops↗

Heterogeneous creep deformation behavior of functionally graded transition joints (GTJs)

Dissimilar metal welds (DMWs) made between ferritic steels and austenitic alloys are used extensively in high-temperature power plant components. These DMWs experience premature creep failure in the ferritic steel’s heat affected zone (HAZ), close to the weld interface. Steep variations in microstructure and chemical composition across the dissimilar weld interface have been the contributing factors for the failure. Graded transition joints (GTJs), developed by functionally grading the chemical composition in layers, have been proposed as potential candidates to replace DMWs. In this research, GTJ coupons were fabricated between 2.25Cr-1Mo steel and Alloy 800H base material using two filler materials: (i) Inconel 82 and (ii) P87. These samples were aged at 600°C for 2000h to accelerate high-temperature microstructural evolution seen in service conditions, before subjecting them to short-term (~1 month) creep tests. Surface strains were measured using digital image correlation (DIC) technique to extract creep strain rates at different locations within GTJs. Both the GTJs exhibited heterogeneous creep strain distribution. Creep strain accumulated in the FGHAZ of 2.25Cr-1Mo steel, similar to type IV failure associated with Cr-Mo steel weldments. Microstructure based creep model framework was developed to describe the discrete creep strain rates observed in various 2.25Cr-1Mo steel regions of GTJs.

36 MATERIALS SCIENCE↗