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At least 883 records · Page 49
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Microstructural, Oxidation, and Mechanical Behavior of NbTi-Based Refractory Alloys with 5 to 10 Pct Co, Cr, and Ni Additions

NbTi-based refractory alloys with additions of Co, Cr, and Ni represent an interesting medium-entropy alloy system with potential for protective oxide film formation, high strength, and ductility. This study investigates the microstructural evolution, oxidation behavior, and mechanical properties of NbTi-based alloys containing 5 to 10 at. pct Co, Cr, and Ni. CALPHAD predictions suggest that this composition range can be heat treated to obtain a predominantly body-centered cubic matrix phase. Mechanical properties, including microhardness, yield strength, maximum strength, and specific strength are evaluated through isothermal compression tests conducted between room temperature and 800 °C. The oxidation kinetics of these alloys are assessed through discontinuous oxidation tests. Parabolic oxidation kinetics were observed for NbTi–10Ni and NbTi–5Co, while linear oxidation kinetics were found for NbTi–10Cr and NbTi–10(CoCrNi). Microstructures and oxide layers are characterized using X-ray diffraction, electron backscatter diffraction, energy-dispersive X-ray spectroscopy, and scanning electron microscopy. All alloys exhibit significant mechanical softening between room temperature and 800 °C, with elastic-perfectly plastic flow observed at 800 °C. The addition of 10 pct Cr to NbTi resulted in two BCC phases up to 1050 °C, conflicting with CALPHAD predictions of a single-phase solid solution at this temperature, and resulting in higher flow stress at 800 °C. NbTi–10(CoCrNi) exhibited the lowest flow stress at 800 °C despite having more ‘cocktail effect’ potential and insufficient molar fractions of Co, Cr, or Ni to form a desirable protective oxide film.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Corrosion Response of Ni-19Cr-5Fe in Molten NaCl-MgCl 2 Salt

Ni-based alloys are strong candidates for use in high-temperature molten salt reactors due to their superior corrosion resistance and mechanical stability compared to stainless steels. In this study, the static corrosion behavior of a Ni-19Cr-5Fe model alloy was systematically evaluated in a purified molten NaCl-MgCl 2 salt at 700°C for 30, 240, and 500 h. Post-exposure analyses were conducted to assess microstructural evolution, corrosion depth, and elemental depletion profiles. Corrosion rates, quantified by chromium depletion depth, followed an inverse power-law trend with increasing exposure time, indicating diffusion-limited kinetics. This trend is attributed to limitations in mass transport in the static salt and to the progressive local depletion of reactive chromium species. Coupled electron backscatter diffraction and energy dispersive X-ray spectroscopy analysis further revealed that the grain boundary character significantly influences corrosion susceptibility: high-angle grain boundaries exhibited pronounced Cr depletion and pitting, while low-angle and Σ3 boundaries remained comparatively resistant. These results offer valuable insight into the role of microstructure in corrosion processes and reinforce the importance of time-dependent material evaluation in molten salt environments relevant to advanced reactor designs.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

An Integrated High-Speed Microstructural Characterization Method Using Simultaneous XRD, Stereo-DIC, and PCI

High-speed characterization of the deformation mechanisms in polycrystalline metals requires the quantification of full strain fields and local microstructural evolutions simultaneously. In this paper, we present a novel experimental method to integrate phase-contrast imaging (PCI), stereographic digital image correlation (stereo-DIC), and full-ring X-ray diffraction (XRD) to allow for the simultaneous characterization of polycrystalline metals at 1MHz or higher. A Kolsky bar was integrated into the synchrotron X-ray source in Sector 32 ID-B at the Advance Photon Source (APS) at Argonne National Laboratory. When the sample is dynamically loaded, the diagnostic methods of full-ring XRD, PCI, and stereo-DIC are properly synchronized to record the deformation behavior at both continuum and microstructural scales as a function of the loading history. An advanced high-strength steel (AHSS) is used as a model material to demonstrate the capabilities of this new experimental method.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Deep operator network surrogate for phase-field modeling of metal grain growth during solidification

A deep operator network (DeepONet) has been constructed that generates accurate representations of phase-field model simulations for evolving two dimensional metal grain morphology growing from melt. These representations serve as lower resolution, computationally efficient stand-ins for quick parameter space exploration of solutions to the the Allen-Cahn equations that dictate the phase-field model simulations. The experimental target for the phase-field model is a uranium casting system cooling a 434 g uranium charge from a maximum temperature of 1400° C at an average rate of 30° C / min , traversing the crystallographic phases of the pure metal. Experimental parameters inform the phase-field model, whose higher resolution computational model solutions are used to train the DeepONet in a given parameter space with the aim of developing a faster, more efficient method for predicting the solidifying metal's microstructure at different potential experimental values. The final DeepONet generates high accuracy, lower resolution predictions with cumulative relative approximation error over all timesteps of less than 0.5%, while ensuring solutions remain within physically feasible ranges. Further, these relative error values are comparable with other state-of-the-art DeepONet models for microstructure evolution, while significantly reducing the amount of training data required. Training a convolutional neural network simultaneously with the DeepONet, enforcing realistic values at the complex metal grain boundaries, and mathematically encoding boundary conditions into the structure of the DeepONet improved prediction accuracy and computational efficiency over a standard DeepONet model.

36 MATERIALS SCIENCE↗
DOE OSTI2017

The characterization of microstructure and chemistry of transmutation fuels

The goal of the fast reactor development programs is fabrication and certification of a nuclear fuel system that performs all functions of a conventional fuel while destroying recycled actinides. Metal fuels, such as U-Pu-Zr fuels, are considered to be candidates for this application. The physical and mechanical properties, as well as behavior laws and correlations of metal alloy fuel, all of which define the behavior and performance of metal alloy fuels has been investigated in detail. The results indicated that the prospect for fueling a future fast spectrum reactor using metal fuels is excellent. There are several challenges associated with the fuel implementation in reactor environment. One of the limiting factors in lifetime and safety of thermal and fast reactor systems is fuel swelling and resulting fission product transport to cladding. Understanding diffusion kinetics and phases formed between metal fuel and cladding upon exposure to high temperatures typical in reactor environment is critical for ensuring integrity, safety, and performance of the material, advancement of this type of fuel in the future, and securing long-term success of the nuclear fleet. The first step to understanding fuel-cladding interaction is investigation of an as-cast fuel microstructure. Despite the importance of these fuels, detailed description of microstructures in these materials is extremely limited. The majority of published results are based on characterization of as-cast microstructures of these fuels in scanning electron microscopes (SEM). In this work, we present the results from microstructural characterization of metallic Pu-based fuels, which is essential in the validation of current and future atomistic and meso-scale modeling efforts. A firm understanding of microstructural evolution in reactor materials is imperative and will lead to deeper understanding of in-reactor degradation behavior, creating a new generation of radiation-resistant materials and fuels with the potential for significant increases in burn-up.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Evolution of the structure and chemical composition of the interface between multi-component silicate glasses and yttria-stabilized zirconia after 40,000 h exposure in air at 800 °C

The chemical and structural stability of two commercial multicomponent silicate glasses (SCN and G6) in contact with yttria-stabilized zirconia (YSZ) was investigated after exposure times of up to 40,000 h in air at 800 °C. With exposure time, interfacial layers develop at the SCN-YSZ and G6-YSZ interfaces, which were characterized in detail using both quantitative chemical analysis and atomic-resolution imaging. At the SCN-YSZ interface, a Ca-Ba-Si-O reaction phase was found to grow by diffusion control. In G6-YSZ, Raman spectroscopy and electron microscopy revealed a disorganized interfacial reaction later between G6 and YSZ, and the occurrence of cubic to tetragonal to monoclinic phase transformations in YSZ. Finally, this microstructural evolution is discussed in terms of devitrification resistance of glass and diffusion processes at interfaces.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Sintering and characterization of SrBi{sub 2}Ta{sub 2}O{sub 9} obtained by high-pressure processing at low temperatures

High-pressure processing is a very attractive approach for the production of materials with new and/or improved properties. In this work, pressures in the order of 7.7 GPa and 2.5 GPa were induced in SrBi{sub 2}Ta{sub 2}O{sub 9} samples at different temperatures placed in a specific reaction cell and generated different effects on phase formation. The microstructural evolution during high-pressure processing was investigated by scanning electron microscopy in association with energy dispersion spectroscopy and with the support of an X-ray diffraction analyzer. Frequency response analysis was used to obtain the dielectric curves by electrochemical impedance spectroscopy. A SrBi{sub 2}Ta{sub 2}O{sub 9} single-phase sample, treated at 2.5 GPa and 900 °C, was used to evaluate the electrical properties, obtaining a dielectric response similar to SrBi{sub 2}Ta{sub 2}O{sub 9} samples sintered by conventional processes at temperatures above 1000 °C. In addition, by this method, it was possible to obtain ceramics with uniform microstructure and a relative density of 93%. - Highlights: • The first production of SrBi{sub 2}Ta{sub 2}O{sub 9} using the technique of high-pressure processing. • The ability to produce single-phase SrBi{sub 2}Ta{sub 2}O{sub 9} treated at 2.5 GPa and 900 °C. • The electrical properties are compatible with SBT sintered at high temperatures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Modeling of flash sintering of ionic ceramics

A fundamental understanding of the influence of defects in ionic ceramics at the atomic, microstructural, and macroscopic levels, before, during, and after the flash sintering event is key to the development of ceramic processing operations that lead to fast, low cost, and environmentally safe fabrication of materials. The observed phenomenology of the flash process encompasses multiple time and length scales and have resulted on a wide variety of what sometimes appears to be contradictory explanations. Here, this article summarizes the latest developments on the modeling and simulation of flash sintering, specifically those related to the understanding of the equilibrium and kinetic properties and the corresponding microstructural evolution of ionic ceramics. Challenges and opportunities in the development of theoretical analyses that include unidentified multiphysical effects are discussed, as they pertain to the processing of technologically relevant ceramic materials for advanced structures and devices.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Grain Structure Evolution in Fe-6Si During Directed Energy Deposition

The purpose of this study is to explore the effect of additive manufacturing (AM) process variables on the grain structure of Fe-6Si, a soft-magnetic alloy used in electrical machine and grid applications. Samples were fabricated with laser engineered net shaping (LENS) with varying inter-pass timing and numbers of unidirectional passes. Here the results show that the grain structure was affected by both solidification and solid-state grain growth mechanisms. A model of the LENS process suggests that, although shorter inter-pass times encourage greater nucleation of new grains and therefore grain refinement during solidification, these conditions also help maintain high solid-state temperatures that allow for grain boundary motion to keep pace with the build rate. Grains formed under these conditions may span multiple layers, and the high-temperature gradient promotes directional growth. This new understanding of these microstructure evolution mechanisms will aid in using process conditions to control the competition between solidification and solid-state grain growth to create grain structures that may not be possible with conventional processing.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Grain boundary precipitation phenomena in an alloy 33 (Cr-Fe-Ni-N) subjected to direct-aging treatments (700 °C and 900 °C)

Highlights: • Complex GB precipitation occurs in Alloy 33 upon aging at 700 °C: conventional and DP modes. At 900 °C only the former occurs. • Two types of DP colonies were observed at 700 °C: unidirectional/parallel and multidirectional/irregular precipitates. • X-ray micro analyses reveal that irregular DP products develop more than one precipitate phase within the same DP colony. - Abstract: Precipitation behavior of alloy 33 upon isothermally aging at 700 °C and at 900 °C was studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray energy dispersive spectroscopy (XEDS). The name, alloy 33, reflects the quasi-equal atomic content of the base elements Fe, Ni and Cr close to 33%, with the addition of Mo and N. The most remarkable features of the microstructural evolution resulting from the aging heat treatments are described as follows: aging at 700 °C leads to homogeneous and heterogeneous grain boundary precipitation, where the discontinuous mode is dominant at this temperature. Conversely, the opposite behavior was observed when the alloy is aged at 900 °C: predominantly homogeneous precipitation together with grain boundary precipitation, however with rare evidence for discontinuous precipitation (DP), even after longer aging times. In the present study, the topology and content of the DP colonies generated by the combined effect of grain boundary migration diffusion and precipitation under isothermal aging at 700 °C were particularly investigated. A variety of morphological features were observed: mainly (1) classical-type microstructure with straight and parallel lamellar precipitates with regular interlamellar spacing and (2) another microstructure with irregular and complex DP colonies. According to our analytical electron microscopy observations, the latter shows that there are more than one precipitate phase within the same colony, which is new to the current theory and experimental evidence on this subject.

36 MATERIALS SCIENCE↗
DOE OSTI2016

In-situ transmission electron microscopy growth of nanoparticles under extreme conditions

The formation and time resolved behavior of individual Pb nanoparticles embedded in silica have been studied by in-situ transmission electron microscopy observations at high temperatures (400–1100 °C) and under 200 keV electron irradiation. It is shown that under such extreme conditions, nanoparticles can migrate at long distances presenting a Brownian-like behavior and eventually coalesce. The particle migration phenomenon is discussed considering the influence of the thermal energy and the electron irradiation effects on the atomic diffusion process which is shown to control particle migration. These results and comparison with ex-situ experiments tackle the stability and the microstructure evolution of nanoparticles systems under extreme conditions. It elucidates on the effects of energetic particle irradiation-annealing treatments either as a tool or as a detrimental issue that could hamper their long-term applications in radiation-harsh environments such as in space or nuclear sectors.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Effect of friction stir welding and post-weld heat treatment on a nanostructured ferritic alloy

Nanostructured ferritic alloys (NFAs) are new generation materials for use in high temperature energy systems, such as nuclear fission or fusion reactors. However, joining these materials is a concern, as their unique microstructure is destroyed by traditional liquid-state welding methods. The microstructural evolution of a friction stir welded 14YWT NFA was investigated by atom probe tomography, before and after a post-weld heat treatment (PWHT) at 1123K. The particle size, number density, elemental composition, and morphology of the titanium-yttrium-oxygenenriched nanoclusters (NCs) in the stir and thermally-affected zones were studied and compared with the base metal. No statistical difference in the size of the NCs was observed in any of these conditions. After the PWHT, increases in the number density and the oxygen enrichment in the NCs were observed. Therefore, these new results provide additional supporting evidence that friction stir welding appears to be a viable joining technique for NFAs, as the microstructural parameters of the NCs are not strongly affected, in contrast to traditional welding techniques.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Identifying the microstructural features associated with void nucleation during elevated–temperature deformation of copper

The microstructural-scale mechanisms that produce cracks in metals during deformation at elevated temperatures are relevant to applications that involve thermal exposure. Prior studies of cavitation during high-temperature deformation, for example, creep, suffered from an inability to directly observe the microstructural evolution that occurs during deformation and leads to void nucleation. Here the current study takes advantage of modern high-speed electron backscatter diffraction (EBSD) detectors to observe cavitation in oxygen-free, high-conductivity copper in situ during deformation at 300°C. Most voids formed at the triple junction between a twin boundary and a high-angle grain boundary (HAGB). This finding does not contradict previous studies that suggested that twins are resistant to cracking—it reveals that cracks in HAGBs originate at twin/HAGB triple junctions and that cracks preferentially grow along HAGBs rather than the accompanying twins. Atomistic simulations explored the origins of this observation and suggest that twin/HAGB triple junctions are microstructural weak points.

36 MATERIALS SCIENCE↗
DOE OSTI2026

A physically based mechanical model for Mullins effect in thermoplastic polyurethanes

Despite decades of research, connecting the chemical and physical structure of thermoplastic polyurethanes to their mechanical properties remains highly challenging. Of particular note are their large-deformation and rate-dependent behaviors, which vary greatly with molecular chemistry, including the type and relative content of soft and hard segments. In this work, we develop a physically motivated mechanical theory for predicting the behavior of thermoplastic polyurethanes. The theory incorporates a representation of microstructural evolution during mechanical deformation, which captures the signatures of stress softening over cyclic loading (commonly referred to as the Mullins effect). There are only eight physically motivated fitting parameters, including a direct dependence on the hard segment fraction. The model predicts that increasing the hard segment fraction leads to higher stiffness and greater energy dissipation, in quantitative agreement with published experimental data. Furthermore, we provide a comprehensive analysis of the model and validate its predictions across several independent datasets focused on mechanical characterization. Direct comparisons to experimental data demonstrate its predictive capability on the effect of loading rate, cyclic deformations, and applied tension or compression. Altogether, this work establishes a predictive framework that connects polymer chemistry and microstructure to emergent mechanical behaviors.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Co-, Ni- and Fe-rich grain-boundary phases enhance creep resistance in θ'-strengthened Al-Cu alloys

Here, microstructural evolution and creep response were investigated in the cast Al-5.0Cu-0.3Mn-0.2Zr (wt.%) alloy with and without addition of slow-diffusing, intermetallic-forming elements Fe, Ni, or Co. Baseline Al-5.0Cu-0.3Mn-0.2Zr alloy exhibits high creep resistance at 300 °C, up to ~75 MPa, which is attributed to high-aspect-ratio, intragranular θ'-Al 2 Cu precipitates that effectively suppress dislocation climb. However, θ'-Al 2 Cu precipitate-free zones form along grain boundaries upon heat treatment, whose extent is amplified during subsequent creep. Such weak regions experience dislocation creep, leading to strain localization and acceleration of grain-boundary sliding. Adding Ni and Co, individually or in combination, leads to the formation of grain-boundary precipitates (Al 9 Co 2 , Al 3 Ni 2 ) which are resistant to coarsening, thus suppressing the formation of θ'-Al 2 Cu precipitate-free zones. This microstructure provides high creep resistance at stresses up to 75–80 MPa, with strain rates much lower than in unmodified Al-5.0Cu-0.3Mn-0.2Zr. Adding Fe, which results in extensive decoration of grain boundaries with coarsening-resistant Al 7 Cu 2 Fe, and then increasing the Cu content to compensate for the Cu loss to this new phase, leads to a new Al-7.4Cu-1.6Fe-0.3Mn-0.2Zr alloy with creep resistance at 300 °C that surpasses known cast aluminum alloys. Adding Fe to improve the creep resistance of Al-Cu alloys is both cost-effective and sustainable. Our findings offer guidelines applicable to various alloy systems on controlling the evolution of precipitate-free zones and its ensuing effects on creep deformation.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Linking microstructure to creep behavior in vertically and horizontally built LPBF Haynes 282 compared with wrought material via θ -projection

Laser Powder Bed Fusion (LPBF) has emerged as a promising route for fabricating intricate geometries in high-performance alloys. Haynes 282 (H282) is a strong candidate for applications such as heat exchangers or engines due to its excellent creep strength and thermal stability; however, the long-term creep behavior of LPBF-processed H282 remains poorly understood. In this study, the θ -projection method is used to analyze and extrapolate the creep behavior of vertically built LPBF, horizontally built LPBF, compared to wrought H282 tested at 816 °C. Vertically built LPBF H282 exhibits the lowest minimum creep rate (MCR), while the horizontally built condition shows a higher MCR comparable to that of wrought H282. Despite these differences, both LPBF conditions exhibit significantly shorter rupture life and reduced rupture strain than the wrought material, with the most severe degradation observed in the horizontal builds, consistent with an earlier onset of tertiary creep and accelerated strain-rate evolution. Microstructural characterization reveals that both LPBF and wrought H282 exhibit abundant twin-related boundary character; however, their grain boundary topologies differ markedly. The wrought alloy contains a higher fraction of low-angle grain boundaries and continuous twin lamellae, whereas the LPBF microstructure is characterized by a suppressed low-angle boundary population and fragmented twin-related boundaries embedded within irregular high-angle grain boundary networks. Fractographic analysis further reveals predominantly intergranular cracking in LPBF H282, accompanied by grain-boundary-decorated carbides, Al 2 O 3 inclusions, and high-aspect-ratio pores. These results demonstrate that grain boundary topology, rather than minimum creep rate alone, plays a critical role in governing creep damage accumulation and rupture behavior in LPBF and wrought H282.

Creep↗
DOE OSTI2018

Development of microstructure and texture during single and multiple pass friction stir processing of a strain hardenable aluminium alloy

Highlights: • Development of microstructure and texture during single and multiple pass FSP of a strain hardenable aluminium alloy • Strain induced boundary migration (SIBM) is the dominant nucleation mechanism for recrystallization • Weak crystallographic texture development influenced by SIBM with the relative dominance of shear texture components • Stable microstructure and texture development after multiple pass FSP • FSP is a promising method for the secondary processing of strain hardenable aluminium alloys - Abstract: In the present study, microstructure and texture development during single and multiple pass friction stir processing (FSP) of a strain hardenable wrought AlMg alloy (AA5086) was investigated. Subtle differences were observed while comparing with heat treatable alloys in the nucleation mechanism of the recrystallized microstructure observed in the nugget zone. Strain induced boundary migration was the dominant mechanism of microstructure evolution in the alloy, which influenced the crystallographic texture development by weakening it. Micro-texture measurements reveal variations in the crystallographic texture along the thickness of the sample. Recrystallization texture components were observed in the nugget zone indicative of a pronounced static recrystallization in the alloy as compared to the heat treatable alloys. Bulk texture measurements within the nugget zone of the optimally processed sample reveal a relatively dominant C component of shear texture. Average grain size in the nugget zone remained the same and the bulk crystallographic texture components were retained during multiple-pass FSP. The lower strain energies involved and the enhanced recovery processes due to the high temperature materials processing of the alloy during FSP resulted in a stable microstructure and texture. In summary, FSP could be promoted as a competent and suitable secondary processing technique for the bulk production of ultra-fine-grained materials in strain hardenable aluminium alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Exploring the tempering behaviour of additively manufactured high-alloy tool steel using synchrotron X-ray and neutron techniques

Post-processing heat treatment provides a critical pathway toward the commercialisation of additively manufactured (AM) S390 high-speed steel, which is a representative high-alloy tool steel employed in precision manufacturing, offering up to 1.5 times longer tool life and over 20% higher cutting speeds compared to conventional grades. In this study, the phase evolution of AM S390 steel during heat treatment, with particular emphasis on carbide precipitation behaviour, was systematically investigated using a combination of synchrotron X-ray and neutron techniques. The metastable M2C carbides were found to dissolve during austenitisation, while the stable primary carbides MC and M6C experienced coarsening with an average size increase of about 60 nm after just 2 min of tempering. Moreover, the austenite lattice parameters reduced from 3.618 to 3.608 Å within the first 10 min of tempering, suggesting carbon depletion in the steel matrix was likely associated with the formation of secondary carbides. This interpretation was substantiated by small-angle scattering results, which revealed the presence of nanoscale precipitates with a volume fraction of 3.1% after 60 min of tempering. These microstructural evolutions collectively accounted for the observed peak hardness of 921 HV. Furthermore, a comparative analysis of synchrotron and neutron small-angle scattering data highlighted the complementary strengths of each technique, offering critical insight into their suitability for characterising nanoscale features in AM high-alloy steels.

Synchrotron X-ray diffraction↗