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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 595 records · Page 33

Transformation and twinning induced plasticity in metastable Ti-Mo alloys under high strain rate deformation

The development of metastable titanium (Ti) alloys provides an unprecedented opportunity to expand their use in plasticity and damage critical applications like protective structures. However, such applications require knowledge of quasi-static to dynamic mechanical behavior, which is currently lacking. Here we perform in-situ, ultrafast synchrotron x-ray diffraction during high strain rate (Kolsky) pressure bar testing in tension and post-mortem electron microscopy to study TRansformation Induced Plasticity (TRIP) and TWinning Induced Plasticity (TWIP) in metastable Ti-Mo alloys. Two alloys, namely Ti-12Mo and Ti-15Mo (wt.%), were selected for study having different β -phase chemical stabilities. TWIP was observed in both Ti-12Mo and Ti-15Mo by in-situ synchrotron diffraction during high strain rate testing. Post-mortem microstructural characterization also revealed the presence of TRIP in Ti-12Mo. TWIP in Ti-15Mo was found to under-perform in terms of total elongation compared to TRIP/TWIP in Ti-12Mo. Ti-12Mo exhibited an average elongation of 17% compared to only 12% for Ti-15Mo with deformation at 1000 s -1 . In conclusion, TRIP resulted in significantly finer microstructure evolution and alleviated local strain accumulations in Ti-12Mo, suggesting TRIP can be used to tune available strength/ductility combinations in metastable Ti alloys under high strain rate deformation conditions.

36 MATERIALS SCIENCE↗

SA508 low alloy steel to 316L stainless steel dissimilar metal joint made by powder metallurgy hot isostatic pressing

Joining ferritic SA508 low alloy steel (LAS) and austenitic 316 L stainless steel (SS) via powder metallurgy hot isostatic pressing (PM-HIP) was evaluated as an alternative method to welding. This study investigated the mechanical and microstructural evolutions of the bimetallic interface under different joint designs and heat treatments. Here, the direct joining of dissimilar metal alloys by PM-HIP method resulted in two designs: 1) powder SA508 to solid bar 316 L (P508–B316L) and 2) powder 316 L solid bar SA508 (P316L-B508). In both cases, P508–B316L and P316L-demonstrated satisfactory tensile strength, however, high hardness and severe depreciation in toughness were located on the bimetallic interface. The mechanisms responsible for the detrimental mechanical properties were verified. Large oxides were observed in P508–B316L due to the prior powder boundary (PPB) oxides present in SA508 powder. The intense sensitization occurred from the formation of M 23 C 6 carbides, consequently from the slow cooling after PM-HIP in P316L-B508. Post-HIP heat treatments were explored to reduce the distance of carbide formation; however, the heat treatment could not eliminate the carbides. The experimental results were compared to the diffusion couple simulation as a function of carbide formation with distance. The analysis also showed the high hardness at the bimetallic interface was primarily contributed by solid solution strengthening. In conclusion, the direct joining of P316L-B508 and P508–B316L via PM-HIP was deemed to be unfeasible, and a transitional material is necessary to impede the diffusion of carbon.

316L stainless Steel↗

The effects of Fe and Al on the phase transformations and mechanical behavior of β-Ti alloy Ti-11at.%Cr

Alloy composition is important for developing desired microstructures in beta-titanium (β-Ti) alloys during thermomechanical processing. In this work, the relatively low-cost alloying elements iron (Fe) and aluminum (Al) were added to a base Ti-11at%chromium (Cr) alloy and in-situ and ex-situ examination of the microstructural evolution and mechanical properties during tension, hardness, elevated temperature X-ray diffraction (XRD) and resonance ultrasound spectroscopy (RUS) were performed. The 400 °C XRD revealed that Ti-11at%Cr underwent β-to-ω and β-to-α transformations. Adding 0.85at% Fe reduced the volume fraction of the ω- and α-phases, and adding 5.3at% Al inhibited the β-to-ω transformation. The 400 °C RUS showed that the alloys containing the ω phase exhibited an increase in shear modulus (G) of ~140%, while the ω-free alloys exhibited an increase of only ~102%. The hardness and strength values of the ω-containing Ti-11Cr and Ti-11Cr-0.85Fe increased with increased ω-phase volume fraction when the ω/α ratio was greater than 0.25. The relationship between ω/α volume ratios and mechanical properties is discussed.

36 MATERIALS SCIENCE↗

Hydrogen influences thermal activation parameters for dislocation glide during low cycle fatigue of 316L stainless steel

Measurements of activation areas are used to investigate the effect of hydrogen on the kinetics of dislocation glide during cyclic deformation in cold-worked 316L stainless steel. Non-charged and hydrogen-precharged (H-precharged) specimens were tested in low cycle fatigue (LCF) under plastic strain control. A series of plastic strain rate changes was performed periodically at the peak true plastic strain from the first cycle to half-life, and at various plastic strain values around stable hysteresis loops near half-life to determine the operational activation area, Δ a ∗. Both material conditions demonstrate a rapid increase in Δ a ∗ during the initial rapid softening followed by a region of approximately constant values coinciding with a reduced rate of softening. Near half-life, hydrogen reduces Δ a ∗ at a given true stress due to its effect on the activation distance and obstacle spacing. The magnitudes of Δ a ∗ reveal that bypassing solutes, cutting forest dislocations, and initiating cross slip are important mechanisms of thermally activated dislocation glide at all amplitudes, except hydrogen suppresses cross slip at the lowest plastic strain amplitudes. These results are supported by electron microscopy characterization of deformed microstructures. A Haasen plot analysis indicates that forest dislocations control the kinetics of deformation in both material conditions. It also reveals the presence of athermal obstacles in both non-charged and H-precharged conditions, likely dense dislocation tangles and cell walls. Additionally, the effect of hydrogen on microstructure evolution (by reducing the propensity for cross slip) leads to a dependence of athermal stress on plastic strain amplitude.

Activation area↗

Microstructural stability of tantalum-alloyed ferritic-martensitic steel with neutron irradiation to 7.4 dpa at ~490 °C

Specimens of a reduced-activation ferritic-martensitic steel, called CNA1, were irradiated to 7.4 displacements per atom at ~490 °C in the High Flux Isotope Reactor. Vickers hardness and tensile properties revealed consistent softening that is attributed to some recovery during irradiation, with reduced laths and dislocation density. Detailed microstructural characterization by transmission electron microscopy and energy dispersive x-ray spectroscopy showed radiation-induced dislocation loops, few cavities, and slight dissolution of M 23 C 6 and MX precipitates. Partial amorphization was only observed in M 23 C 6 precipitated in matrix. Transmutation somewhat destabilized M 23 C 6 and MX, with a stronger effect on the later one by noticeable depletion of Ta with enriched W, which is consistent with the transmutation calculations. The microstructural evolution and associated strength changes were discussed with the assistance of computational thermodynamics.

36 MATERIALS SCIENCE↗

Impact of nuclear reactor radiation on the performance of AlN/sapphire surface acoustic wave devices

The performance of an AlN/sapphire surface acoustic wave (SAW) delay line device was characterized in real time under irradiation inside a nuclear reactor. Both its resonant frequency and transmission efficiency were observed to respond to a change in reactor power. The response follows an exponentially saturating behavior after a step power increase, followed by an exponentially decaying recovery after reactor shutdown. A sensitivity analysis based on the governing electro-mechanical equations shows that the frequency shift can be attributed to the softening of sapphire’s elastic constants under neutron radiation. Additionally, a kinetic rate equation is adopted to interpret device response and describe its microstructural evolution. These results suggest that the AlN/sapphire SAW device remains functional under irradiation, is sensitive to neutron and gamma ray fluxes, and offers an opportunity for remote sensing and in-situ measurement of material properties when exposed to nuclear reactor environment.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Development and preliminary validation of a mechanistic multiscale model for fuel-cladding chemical interaction in metallic nuclear fuels

Despite decades of fuel rod material and design improvements, fuel-cladding chemical interaction (FCCI) remains the single-most lifetime-limiting behavior for modern metallic fuel rods. Constraining fuel lifetime increases operating costs, limiting the economic viability of commercializing metallic nuclear fuel technology. A mechanistic multiscale model utilizing the finite element method-based MARMOT and BISON codes was developed to more confidently predict cladding-side FCCI and its impact on fuel performance. The new BISON model incorporates mesoscale models for the effects of fuel microstructure evolution on the transport of wastage-inducing lanthanides through the fuel and for the kinetics of cladding wastage layer growth. The mesoscale models, in turn, build on lanthanide transport property data obtained from the atomistic scale. Preliminary validation studies using wastage thickness and cladding profilometry data from four fuel rods irradiated in Experimental Breeder Reactor II experiment X447 and one fuel rod from Fast Flux Test Facility experiment IFR1 show that the new model predicts cladding wastage and its effects on cladding deformation as well as existing empirical FCCI correlations. The new model is expected to aid in the design of new metallic fuel concepts, including fuel additives, cladding liners, and sodium-free annular fuel geometries. In conclusion, future work will focus on broader validation and refinement of the model’s treatment of different fuel alloys and cladding materials.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Anisotropic grain boundary area and energy distributions in tungsten

Describing microstructure evolution in tungsten requires a quantitative description of the anisotropic grain boundary energy. Here we present a grain boundary energy function for tungsten that specifies the energy of an arbitrary boundary given its five macroscopic crystallographic parameters. A comparison of measured grain boundary areas and the grain boundary energies given by the function at the Σ11, Σ17b, and Σ33a misorientations, which are problematic to determine by measurement or atomistic calculations, reveals inverse correlations that are similar to what have been observed in other metals.

36 MATERIALS SCIENCE↗

Unfaulting mechanisms of interstitial Frank loops in fluorite-structured ThO 2

Unfaulting of Frank loops in irradiated fluorite-structured oxides is of significance for understanding microstructural evolution. However, the mechanisms have not yet been directly observed. To this end, we utilize molecular dynamics to reveal the atomistic details related to the unfaulting process of interstitial Frank loops in ThO 2 , which involve a single pair or multiple pairs of co-propagating Shockley partials to annihilate the stacking faults. Here, we find that the unfaulting is achieved via a synchronous shear of the partial pairs to remove the extrinsic stacking fault in the cation sublattice and the intrinsic stacking fault in the anion sublattice. The high mobility of oxygen at the dislocation core may reduce the activation barriers of dislocation nucleation and migration. These findings provide a fundamental understanding of the transformation of faulted loops in irradiated ThO 2 , and could be transferable to other fluorite-structured oxides.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Carbon nanotube (CNT) reinforced 316L stainless steel composites made by laser powder bed fusion: Microstructure and wear response

Carbon nanotube (CNT) reinforced 316L stainless steel (SS) composites were fabricated by laser powder bed fusion (LPBF) additive manufacturing (AM). This study focuses on microstructure evolution, hardness, and wear behavior. The wear behavior for AM 316L SS and 1 wt% CNT/316L SS was studied by a dry sliding test under normal loads of 10, 15, and 25 N. The addition of CNT to 316L SS led to the change of solidification mode from cellular/columnar to dendritic growth, producing grain refinement. Nanoscale dendrites were observed. Although TEM characterization confirmed the existence of CNT in cell interior, most CNT were damaged, resulting in carbon material segregation along cellular/dendritic boundaries. The wear rate was found dramatically decreased due to the improved hardness. Compared to the adhesive and abrasive wear in AM 316L SS, the wear mechanism of CNT/316L composite was adhesion and oxidative wear. Furthermore, enhanced cellular/dendritic boundary strengthening by carbon segregation was the main strengthening mechanism of CNT/316L composite.

36 MATERIALS SCIENCE↗

Resolving atomic transport through iron oxide under irradiation using isotopic tracers

Structural materials in nuclear environments are exposed to complex and harsh conditions, including high temperatures, corrosive solutions, and irradiation. Material stability and likewise degradation are fundamentally controlled by atomic transport mechanisms. Here, we investigate the influence of radiation-induced, non-equilibrium point defect populations on mass transport within model oxide systems using isotopic tracers and atom probe tomography. An isotopically labelled hematite (a-Fe2O3) film was synthesized with 16O- and 18O-rich layers (>30nm and 10 nm, respectively) sequentially deposited via molecular beam epitaxy. One region of the film was proton irradiated to ~0.1 dpa at 450°C, and regions outside the beam spot provided a non-irradiated control of thermal annealing only. 3D APT was used to directly visualize the elemental and O-isotopic redistribution following both thermal and combined thermal and irradiation conditions. Complementary scanning transmission electron microscopy (STEM) was also employed to study the microstructural evolution. Error function fits of the 18O-concentration profiles enabled quantification of diffusion coefficients.

isotopic tracers, diffusion, proton irradiation, h↗

In Situ and Operando Morphology Study of Germanium-Selenium Alloy Anode for Li-ion Batteries

Selenium-doped germanium (GeSe) micrometersized particles have been reported with good cycling performance and rate capability due to a Li-Se-Ge network formed during the first lithiation that provides a Li-ion fast pathway. To understand the effect of the Li-Se-Ge network at a high cycling rate, we monitored the morphology change of both pure Ge and GeSe particles during cycling with an in situ/operando focused-ion beam-scanning electron microscope method. Our results showed that the proposed inactive Li-Se-Ge network can provide fast Li-ion transport and also buffer volume variation, resulting in homogeneous volume change and uniform microstructural evolution.

germanium↗

High-Temperature Neutron Diffraction Study of Vanadium and Vanadium–Niobium Null-Matrix Alloy for Spectrum Normalization

This study systematically evaluates a vanadium–niobium (V 94.1 Nb 5.9 ) null-matrix alloy as a reference material for neutron spectrum normalization and compares its performance with that of pure vanadium under identical experimental conditions. Neutron diffraction experiments are conducted on the VULCAN Engineering Materials Diffractometer at the Spallation Neutron Source, Oak Ridge National Laboratory, over a temperature range from room temperature to 1200 °C under vacuum. Pure vanadium exhibited distinct Bragg peaks across all temperatures, with its diffraction behavior influenced by both sample orientation and temperature. As the temperature increased, the diffraction peaks shifted to larger d-spacings and decreased in intensity, while spectral deviation near d ≈ 2.8 Å exceeded 10% at 1200 °C. In contrast, the V–Nb alloy produced a nearly featureless spectrum over the full d-spacing range, confirming near-complete cancellation of coherent scattering over the wide temperature range. Its spectra were insensitive to sample orientation, temperature, and microstructural evolution, with spectral deviation around d ≈ 2.8 Å exceeded 5% at 1200 °C. In conclusion, these results demonstrate that the V–Nb null-matrix alloy provides a thermally stable, efficient, and reliable normalization standard for time-of-flight diffractometers or other instrument where it is needed, enabling reduced data acquisition time and improved data quality in high-temperature neutron diffraction experiments.

Alloys↗

In Situ and Operando Observation of Zinc Moss Growth and Dissolution in Alkaline Electrolyte for Zinc–Air Batteries

As a promising battery technology, zinc–air batteries still face significant challenges, including the formation of a mossy structure on the zinc metal anode in alkaline electrolyte. Because a similar phenomenon also plagues lithium and sodium metal batteries, elucidating its mechanism has important implications for progress in energy storage. Herein, operando X-ray nanotomography was employed to visualize zinc moss growth and dissolution at the individual colony level. By tracking its microstructure evolution, zinc moss was found to display irreversible plating/stripping behavior. While zinc moss exhibits self-limiting growth and zinc deposition occurs mainly in its outer region, zinc dissolution is more uniformly distributed inside the moss colony upon stripping, leading to the formation of “dead” zinc and capacity loss. A direct correlation is established between the moss amount and zinc plating/stripping efficiency. Finally, results from this study offer new insights into mitigating the unstable zinc plating morphology and improving the cycle life of aqueous zinc–air batteries.

36 MATERIALS SCIENCE↗

Chemo-Mechanical Behavior and Stability of High-Loading Cathodes in Solid-State Batteries

Solid-state batteries can offer higher energy density and improved safety compared to lithium ion batteries, which use flammable liquid electrolytes. Increasing the ratio of cathode active materials in composite cathodes enhances the energy density and reduces manufacturing costs. Changes in the ratio of cathode active materials alter the microstructure and chemo-mechanical response of a cathode during operation. Understanding the relationship between composition, microstructure, and chemo-mechanical interactions is critical for optimizing solid-state cathodes. Here, in this study, we engineered composite cathodes with varying ratios of LiNi 0.8 Co 0.1 Mn 0.1 O 2 and Li 6 PS 5 Cl to systematically investigate the role of microstructural evolution in long-term chemo-mechanical transformations. Chemo-mechanical stresses resulting from the volume changes of the cathode active materials led to degradation mechanisms, such as fracture and interfacial delamination. Active material fracture and delamination led to underutilization of active material and significant capacity decay during cycling. Coatings that suppress active material-active material interactions during cycling may aid in suppressing the generation of local stress hotspots.

36 MATERIALS SCIENCE↗

Formation of Bimetallic Nanoparticles via Exsolution Using a Reducible Metal Oxide Capping Layer

Bimetallic nanoparticles are promising catalysts that can improve performance in heterogeneous catalysis and solid-state electrochemistry. Exsolution is a useful method for forming such nanoparticles; however, it is limited by the elements present within the host oxide lattice. Here, in this work, we develop and demonstrate a strategy to form bimetallic particles from La 0.5 Sr 0.5 Ti 0.94 Ni 0.06 O 3 (LSTN) exsolution and using a reducible SnO 2 capping layer, expanding the range of elements available for bimetallic nanoparticle formation. Using this capping layer strategy, we formed nickel–tin (Ni 0 –Sn 0 ) bimetallic nanoparticles via exsolution. We used in situ near-ambient pressure X-ray photoelectron spectroscopy to monitor surface chemical changes during exsolution, showing that first, SnO 2 volatilized. This SnO 2 loss exposed the perovskite surface of LSTN to reducing conditions, which induced Ni exsolution, and compounded with SnO 2 reduction led to the formation of bimetallic Ni 0 –Sn 0 particles. To evaluate the associated microstructural evolution, we measured grazing incidence small-angle X-ray scattering (GISAXS), which confirmed the loss of the SnO 2 capping layer, and scattering simulations suggested the formation of bimetallic particles. We confirmed the bimetallic nanoparticle composition and morphology by Auger spectroscopy and scanning transmission electron microscopy. The resulting bimetallic nanoparticles were smaller and more thermally stable than the monometallic Ni counterparts on LSTN. This capping layer and exsolution approach allow synthesizing multimetallic nanoparticles and can be applied to other reducible metal oxides and perovskite hosts, broadening the compositional space for advanced catalytic materials.

36 MATERIALS SCIENCE↗

Deep learning-based segmentation of lithium-ion battery microstructures enhanced by artificially generated electrodes

Accurate 3D representations of lithium-ion battery electrodes, in which the active particles, binder and pore phases are distinguished and labeled, can assist in understanding and ultimately improving battery performance. Here, we demonstrate a methodology for using deep-learning tools to achieve reliable segmentations of volumetric images of electrodes on which standard segmentation approaches fail due to insufficient contrast. We implement the 3D U-Net architecture for segmentation, and, to overcome the limitations of training data obtained experimentally through imaging, we show how synthetic learning data, consisting of realistic artificial electrode structures and their tomographic reconstructions, can be generated and used to enhance network performance. We apply our method to segment x-ray tomographic microscopy images of graphite-silicon composite electrodes and show it is accurate across standard metrics. We then apply it to obtain a statistically meaningful analysis of the microstructural evolution of the carbon-black and binder domain during battery operation.

25 ENERGY STORAGE↗

Electric-field control of the nucleation and motion of isolated three-fold polar vertices

Recently various topological polar structures have been discovered in oxide thin films. Despite the increasing evidence of their switchability under electrical and/or mechanical fields, the dynamic property of isolated ones, which is usually required for applications such as data storage, is still absent. Here, we show the controlled nucleation and motion of isolated three-fold vertices under an applied electric field. At the PbTiO 3 /SrRuO 3 interface, a two-unit-cell thick SrTiO 3 layer provides electrical boundary conditions for the formation of three-fold vertices. Utilizing the SrTiO 3 layer and in situ electrical testing system, we find that isolated three-fold vertices can move in a controllable and reversible manner with a velocity up to ~629 nm s -1 . Microstructural evolution of the nucleation and propagation of isolated three-fold vertices is further revealed by phase-field simulations. This work demonstrates the ability to electrically manipulate isolated three-fold vertices, shedding light on the dynamic property of isolated topological polar structures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗