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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 1,081 records · Page 60

Conversion of real-world aluminum scrap streams into high-performance Al–Mg–Si–Cu automotive alloys using shear assisted processing and extrusion

The conversion of post-consumer aluminum (Al) scrap into usable Al alloys without adding primary Al is challenging because of excess impurities. In this work, >99% post-consumer Twitch, used beverage cans (UBCs), and remelt scrap ingots (RSIs) were used as feedstock materials. As-cast and solution heat-treated feedstock billets were extruded using Shear Assisted Processing and Extrusion (ShAPE) at ~510°C, followed by press quenching. To explore the development of the microstructure, texture, and underlying mechanisms and how they contribute to the overall strengthening in as-extruded and artificially aged samples, scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) were used to collect microstructure and texture data. The enhanced strength and ductility were corroborated with the microstructural features and crystallographic texture. Simple shear $\textrm{A}/\bar{\textrm{A}}$, $\textrm{A}_1^*/\textrm{A} _2^*$ texture components along with weak $\textrm{C}$ and $\textrm{B}/\bar{\textrm{B}}$ texture components were formed during extrusion; the texture was strengthened after heat treatment. The refined second-phase particles helped to retain the deformed microstructure and texture. The contributions of dislocation and precipitate strengthening were maximized when billets were solution-heat-treated prior to extrusion. This is attributed to the formation of effective supersaturated solid solutions during the ShAPE process, which precipitate out during the peak age treatment. Overall, the highest yield strength of 305 MPa, ultimate tensile strength of 350 MPa, and elongation of 12% were achieved in artificially aged samples, which are comparable to those of Al 6082-T6.

Al alloy↗

Characterization of hot-pressed von Alpen type NASICON ceramic electrolytes

The Na-ion conducting solid electrolyte NASICON is a promising solid state electrolyte (SSE) for use in Na based electrochemical systems. The effects of particle morphology and synthesis of von Alpen type NASICON via hot-pressing were investigated. Spray dried particles were shown to improve mechanical and electrochemical properties. X-ray diffraction, scanning electron microscopy, impulse excitation measurements, Vickers hardness, and impedance spectroscopy were used to correlate relationships between phase purity, microstructure, mechanical properties, and electrochemical properties. Scanning electron microscopy showed the presence of a glass phase as between 19.08% and 28.23% area percentage and a ZrO 2 phase between 0.46% and 3.51% area percentage in the hot-pressed samples. Impulse excitation showed elastic modulus varying from 83.65 to 97.65 GPa. The first values of Poisson's ratio and shear modulus of NASICON are reported as between 0.23 and 0.26 and 33.87 to 38.79 GPa, respectively. Vickers hardness and fracture toughness measurements showed Vickers hardness ranging from 4.30 to 4.68 GPa and fracture toughness ranging from 1.05 to 1.09 MPa m ½ . Impedance spectroscopy showed grain conductivities ranging from 1.023 to 1.287 mS/cm, with grain boundary resistance percentages between 73.22 and 47.5%. Total conductivities ranged from 0.292 to 0.596 mS/cm, with 0.596 mS/cm being achieved at room temperature for the spray dried powders with lower grain boundary resistance percentages.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effect of post-deposition heat treatment on microstructure and mechanical properties of NASA HR-1 cold spray coatings

The primary goal of this work was to examine the impact of heat treatment on the evolution of microstructure and mechanical properties of NASA HR-1 cold spray coatings. Coatings were produced employing a high pressure cold spray system using N2 and He process gases and the effect of process gas and deposition temperature on the microstructure and mechanical properties of the coatings was examined. Microstructural characterization was performed using optical microscopy, scanning electron microscopy, micro X-ray computed tomography, and electron backscatter diffraction. NASA HR-1 coatings produced with He process gas exhibited improved plastic deformation and resulted in the lowest porosity compared to those deposited with N2 process gas. All coatings showed brittle failure with limited ductility in the as-deposited condition. Heat treatment of the NASA HR-1 cold spray coatings was performed at 550°C and 950°C for 1 h to improve the mechanical strength of the coatings. Heat treatment improved the particle bonding and enhanced the mechanical properties of the cold spray coatings. Heat treatment performed at 550°C resulted in higher mechanical strength of coatings, whereas the heat treatment performed at 950°C resulted in recrystallized microstructure and improved ductility of the coatings. However, heat treatment at 950°C resulted in forming the Eta (η) phase and Ni-Ti intermetallics in all the NASA HR-1 cold spray coatings. Here, the overall results suggest that using He as process gas contributed to reduced porosity and enhanced mechanical properties of the cold spray coatings.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Elasto-viscoplastic fast Fourier transform modeling framework for assessing microstructural effects on stress intensity factors characterizing fracture toughness

A large-strain elasto-viscoplastic fast Fourier transform (LS-EVPFFT) model with non-periodic (NP) velocity-based boundary conditions is adapted to simulate the sensitivity of stress intensity factors on microstructure for 304L stainless steel. The material was characterized via electron backscattered diffraction (EBSD) serial-sectioning to obtain a measured 3-D microstructural cell to perform simulations. The NP-LS-EVPFFT model, including the simulation setup and boundary conditions, was verified using a crystal plasticity finite element (CPFE) model. To this end, the generation of meshes of notched specimens was developed, which involved creating Python scripts for mesh “cutting” in Abaqus, and Sculpt scripts in Cubit for meshing of the measured microstructural cell processed with DREAM.3D. The complexity of the mesh preparation highlighted the advantages of the FFT-based model, which circumvents the mesh generation process. Given the efficiency of the FFT-based model, statistical distribution of stress intensity factors in function of crystal orientation at the crack tip, grain structure, and crystallographic texture surrounding the crack tip were predicted. Further, the distributions reveal about 10% variation of stress intensity factors with microstructure with the most significant sensitivity found to be the crystal orientation at the crack tip. The methodology developed in this work is discussed as a practical simulation tool for predicting the sensitivity of stress intensity factors on microstructural variability in metallic materials.

36 MATERIALS SCIENCE↗

Effect of substrate temperature on the growth of Nb 3 Sn film on Nb by multilayer sputtering

Here, we report on the fabrication of niobium tin (Nb 3 Sn) films by multilayer sequential sputtering on niobium at substrate temperatures ranging from room temperature to 250 °C. The multilayers were then annealed inside a separate vacuum furnace at 950 °C for 3 h. The material properties of the films were characterized by X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, atomic force microscopy, and transmission electron microscopy. The superconducting properties of the films were studied by four-point probe resistivity measurements from room temperature to below the superconducting critical temperature T c . The highest film T c was 17.76 K, obtained when the multilayers were deposited at room temperature. When the deposition temperature was raised to 250 °C, a significant reduction in voids was achieved while the film's T c was 17.58 K.

36 MATERIALS SCIENCE↗

Correlating results from high resolution EBSD with TEM- and ECCI-based dislocation microscopy: Approaching single dislocation sensitivity via noise reduction

High resolution electron backscatter diffraction (HREBSD), an SEM-based diffraction technique, may be used to measure the lattice distortion of a crystalline material and to infer the geometrically necessary dislocation content. Uncertainty in the image correlation process used to compare diffraction patterns leads to an uneven distribution of measurement noise in terms of the lattice distortion, which results in erroneous identification of dislocation type and density. This work presents a method of reducing noise in HREBSD dislocation measurements by removing the effect of the most problematic components of the measured distortion. The method is then validated by comparing with TEM analysis of dislocation pile-ups near a twin boundary in austenitic stainless steel and with ECCI analysis near a nano-indentation on a tantalum oligocrystal. Finally, the HREBSD dislocation microscopy technique is able to resolve individual dislocations visible in TEM and ECCI and correctly identify their Burgers vectors.

36 MATERIALS SCIENCE↗

A Quantitative Method for In Situ Pump-Beam Metrology in 4D Ultrafast Electron Microscopy

In this work, we report a method for measuring spot size and focusing conditions of the femtosecond (fs) excitation laser in situ at the specimen location in 4D ultrafast electron microscopy (UEM). The method makes use of threshold laser ablation behaviors of thin amorphous carbon membranes. For Gaussian beam profiles and for ablation threshold fluence values, we analytically derive expressions describing the relationship between ablated hole size and the actual laser spot size. Using these expressions, we developed experimental procedures for characterizing the shape and spot size of the pump beam at the specimen. We demonstrate the viability of the approach for incident excitation wavelengths of 343 nm and 515 nm, thus illustrating the applicability of the method to a range of optical wavelengths without modification. Further, we show that by measuring ablated hole size as a function of focusing condition, a full metrological characterization of the Gaussian beam propagation properties can be performed. Finally, we find good agreement for spot sizes determined with this method and with those determined by extrapolation from measurements taken outside the microscope column. Overall, this method is a simple, cost-effective means for accurate and precise determination of key pump-beam parameters in situ at the specimen location in UEM experiments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Post weld heat treatment and operating temperature effect on tribological behavior of laser cladded stellite 21 coating

This study intends to investigate the feasibility of using laser cladding as a potential process to repair hot working tools by a hardfacing process. A Stellite 21 alloy coating was printed on a 350 maraging steel via laser cladding and the coating microstructure and tribological performance were characterized in as printed conditions and after heat treatment. Such a laser-processed coating showed a high integrity with little porosity and good bonding with the substrate. The Stellite coating produced substantially lower friction and a smoother contact area but had inferior wear resistance compared with the maraging steel substrate. Post process heat treatment at 650 °C for 20 h led to significant amount of strain-induced FCC to HCP phase transformation but had little improvement in wear resistance. Detailed materials characterization using X-ray diffraction and electron microscopy provided fundamental insights to the underlying mechanisms. This study opens the door for future R&D for tool surface repair by laser cladding.

36 MATERIALS SCIENCE↗

In-situ synchrotron X-ray diffraction investigation on deformation behavior of Nb/NiTi composite during pre-straining process

The mechanisms responsible for deformation behavior in Nb/NiTi composite during pre-straining were investigated systematically using in-situ synchrotron X-ray diffraction, transmission electron microscopy and tensile test. It is shown that upon loading, the composite experiences elastic elongation and slight plastic deformation of B19', B2 and β-Nb phases, together with the forward stress-induced martensitic (SIM) transformation from B2 to B19'. Upon unloading, the deformation mechanisms of the composite mainly involve elastic recovery of B19', B2 and β-Nb phases, compression deformation of β-Nb phase and incomplete B19'→B2 reverse SIM transformation. In the tensile loading-unloading procedure, besides the inherent elastic deformation and SIM transformation, the (001) compound twins in B19' martensite can also be conducive to the elastic deformation occurring in B19'-phase of the composite. Therefore, this composite can exhibit a large recoverable strain after unloading owing to the elastic deformation, and the partially reversible and consecutive SIM transformation together with the (001) compound twins.

36 MATERIALS SCIENCE↗

Cluster Analysis of Combined EDS and EBSD Data to Solve Ambiguous Phase Identifications

A common problem in analytical scanning electron microscopy (SEM) using electron backscatter diffraction (EBSD) is the differentiation of phases with distinct chemistry but the same or very similar crystal structure. X-ray energy dispersive spectroscopy (EDS) is useful to help differentiate these phases of similar crystal structures but different elemental makeups. However, open, automated, and unbiased methods of differentiating phases of similar EBSD responses based on their EDS response are lacking. This paper describes a simple data analytics-based method, using a combination of singular value decomposition and cluster analysis, to merge simultaneously acquired EDS + EBSD information and automatically determine phases from both their crystal and elemental data. I use hexagonal TiB 2 ceramic contaminated with multiple crystallographically ambiguous but chemically distinct cubic phases to illustrate the method. Code, in the form of a Python 3 Jupyter Notebook, and the necessary data to replicate the analysis are provided as Supplementary material.

47 OTHER INSTRUMENTATION↗

Argon Milling of Bulk and Post-FIB Specimens for Multi-Length Scale Analyses by EBSD, TEM, and APT under Controlled Environments

Correlative investigations involve structural characterization by transmission electron microscopy (TEM) combined with compositional analysis by atom probe tomography (APT) using the same specimen. A critical component of successful correlative analyses is specimen preparation; probing individual atoms requires a surface and subsurface with minimal defects, beginning with the bulk material through to the prepared specimen for TEM or APT analysis. Our previous work showed that low-energy concentrated ion beam Ar ion milling improves TEM [1] and APT [2,3] specimen quality by removing surface oxides and Ga damage caused by focused ion beam (FIB) preparation. Further enhancement in specimen quality of APT specimens is achieved in the established workflow under controlled environments, as shown in [4]. In this work, we present specimen preparation using Ar ion milling techniques not only for the APT specimen, but also the bulk sample for subsequent multi-length scale analyses by electron backscatter diffraction (EBSD), TEM, and APT under controlled environments. The removal of surface damage and oxidation, which is crucial for probing atomic layer specimens by broad and concentrated Ar ion beam milling techniques under controlled environments, is highlighted.

36 MATERIALS SCIENCE↗

Homoleptic Uranium–Bis(acyl)phosphide Complexes

Here, the first uranium bis(acyl)phosphide (BAP) complexes were synthesized from the reaction between sodium bis(mesitoyl)phosphide (Na( mes BAP)) or sodium bis(2,4,6-triisopropylbenzoyl)phosphide (Na( tripp BAP)) and UI 3 (1,4-dioxane) 1.5 . Thermally stable, homoleptic BAP complexes were characterized by single-crystal X-ray diffraction and electron paramagnetic resonance (EPR) spectroscopy, when appropriate, for the elucidation of the electronic structure and bonding of these complexes. EPR spectroscopy revealed that the BAP ligands on the uranium center retain a significant amount of electron density. The EPR spectrum of the trivalent U( tripp BAP) 3 has a rhombic signal near g = 2 (g 1 = 2.03; g 2 = 2.01; and g 3 = 1.98) that is consistent with the EPR-observed unpaired electron being located in a molecular orbital that appears ligand-derived. However, upon warming the complex to room temperature, no resonance was observed, indicating the presence of uranium character.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Synthesis and Characterization of Isostructural Th(IV) and U(IV) Pyridine Dipyrrolide Complexes

A series of pyridine dipyrrolide actinide(IV) complexes, ( Mes PDP Ph )AnCl 2 (THF) and An( Mes PDP Ph ) 2 (An = U, Th, where ( Mes PDP Ph ) is the doubly deprotonated form of 2,6-bis(5-(2,4,6-trimethylphenyl)-3-phenyl-1H-pyrrol-2-yl)pyridine), have been prepared. Characterization of all four complexes has been performed through a combination of solid- and solution-state methods, including elemental analysis, single crystal X-ray diffraction, and electronic absorption and nuclear magnetic resonance spectroscopies. Collectively, these data confirm the formation of the mono- and bis-ligated species. Time-dependent density functional theory has been performed on all four An(IV) complexes, providing insight into the nature of electronic transitions that are observed in the electronic absorption spectra of these compounds. Room temperature, solution-state luminescence of the actinide complexes is presented. Both Th(IV) derivatives exhibit strong photoluminescence; in contrast, the U(IV) species are nonemissive.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Influence of Compositional Complexity on Amorphization Resistance of Swift Heavy Ion Irradiated Titanate Pyrochlores

Compositionally complex oxides have garnered attention recently for their potential technological applications in harsh environments such as thermal barrier coatings and nuclear waste forms. Therefore, their response to extreme conditions, including high temperature and intense irradiation fields, must be thoroughly investigated. Here, the structural evolution of two pyrochlore oxides with comparable cation size ratio, r A /r B , (Yb 0.2 Er 0.2 Dy 0.2 Tb 0.2 Gd 0.2 ) 2 Ti 2 O 7 and Ho 2 Ti 2 O 7 , was evaluated after irradiation with 946 MeV Au ions up to a fluence of 8 × 10 12 ions/cm2 using synchrotron X-ray diffraction, transmission electron microscopy, and Raman spectroscopy. The overall radiation response is comparable for both titanate oxides and is dominated by a loss of crystallinity. When compared to a series of conventional titanate pyrochlore compositions, the amorphous track diameter of (Yb 0.2 Er 0.2 Dy 0.2 Tb 0.2 Gd 0.2 ) 2 Ti 2 O 7 is slightly larger than that of Ho2Ti2O7 and more in line with the diameter of the endmember with the maximum A-site cation size (Gd 2 Ti 2 O 7 ). Density functional theory calculations suggest that this behavior may be linked to local lattice distortions and the associated energetics of cation antisite formation. TEM and Raman analyses show that a disordered, crystalline shell surrounds the amorphous ion tracks in (Yb 0.2 Er 0.2 Dy 0.2 Tb 0.2 Gd 0.2 ) 2 Ti 2 O 7 , and the corresponding short-range structure resembles a weberite-type atomic arrangement.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Radiation-Induced Changes in Single Crystal Calcite and Dolomite: Mineral Analogues of Light Water Reactor, Nuclear Power Plant Concrete Aggregates

Two analogues of aggregates (calcite and dolomite) found in nuclear power plant (NPP) concrete have been neutron irradiated to fluences up to 2 × 10 20 n/cm 2 at 52 °C and 4 × 10 19 n/cm 2 at 95 °C (E > 0.1 MeV). X-ray diffraction studies showed that these aging conditions affected crystallography of both calcite and dolomite, with both showing a growth in their unit cells compared to that of the unirradiated samples. Only dolomite samples showed a continuous increase of its lattice parameters with the increase in irradiation. In calcites, the lattice growth with irradiation dissipated after a fluence of 5 × 10 18 n/cm 2 . Radiation-induced disordering of the crystal structure was observed in both materials, while a healing effect of irradiation temperature was mainly observed in calcites. Dislocation densities calculated by using XRD data also supported these observations. Insights made into the unit cells of both minerals by using Fourier synthesis showed that the Mg sites are more prone to the neutron irradiation than the Ca sites, resulting in larger radiation effects and higher disruption in the crystal structure of dolomite than that of calcite. Furthermore, other than the polycrystalline characteristics observed by using TEM, these minerals did not show complete amorphization or significant structural decomposition at the studied irradiation fluences.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Laser-Induced Enhancement of Acoustic Mode Quality Factor Revealed by Correlated Single-Particle Optical and Electron Microscopy

Acoustic modes in plasmonic nanostructures provide fundamental insights into their optomechanical behavior at the nanoscale, enabling emerging applications in plasmon-enhanced optomechanics, ultrasensitive sensing, and nanoscale energy transduction. Here we explore the modulation of acoustic phonon dynamics in lithographically fabricated gold nanodisks via laser-induced photothermal annealing. Using a correlated approach that utilizes both single-particle transient extinction spectroscopy and advanced electron microscopy, we directly link nanoscale structural transformations to changes in mechanical properties as probed through the coherence of the excited acoustic modes. Specifically, ultrafast pump–probe microscopy reveals an enhancement in the acoustic mode quality factor of annealed gold nanodisks, indicative of reduced damping and improved vibrational coherence. Structural characterization via scanning electron microscopy and electron backscatter diffraction confirms that photoinduced annealing results in smoother surface morphology and overall enhanced crystallinity. The improved crystalline order reduces defect and crystal boundary scattering, which we suggest as the reason underlying the lower quality factor before annealing. Furthermore, these findings demonstrate that targeted structural engineering at the nanoscale offers a powerful strategy for optimizing the optomechanical performance of plasmonic nanostructures, with broad implications for the design of next-generation nanophotonic and optomechanical systems.

Annealing (metallurgy)↗

Epitaxial Electrodeposition of Fe with Controlled In-Plane Variants for a Reversible Metal Anode in an Aqueous Electrolyte

The development of reversible metal anodes is a key challenge for advancing aqueous battery technologies, particularly for scalable and safe stationary energy storage applications. Here, in this study, we demonstrate a strategy to realize epitaxial electrodeposition of iron (Fe) on single-crystal copper (Cu) substrates in aqueous electrolytes. We compare the electrodeposition behavior of Fe on polycrystalline and single-crystalline Cu substrates, revealing that the latter enables highly uniform, dense, and crystallographically aligned Fe growth. Comprehensive electron backscatter diffraction (EBSD) and X-ray diffraction (XRD) analysis confirms the formation of Fe with specific out-of-plane and in-plane orientations, including well-defined rotational variants. Our findings highlight that epitaxial electrodeposition of Fe can suppress dendritic growth and significantly enhance Coulombic efficiency during plating/stripping cycles. This approach bridges fundamental crystallography with practical electrochemical performance, providing a pathway toward high-efficiency aqueous batteries utilizing Earth-abundant materials.

aqueous battery↗

Neptunium Pyridine Dipyrrolide Complexes

Two pyridine dipyrrolide neptunium(IV) complexes, ( Mes PDP Ph )NpCl 2 (THF) and Np( Mes PDP Ph ) 2 , where ( Mes PDP Ph ) 2– is the doubly deprotonated form of 2,6-bis(5-(2,4,6-trimethylphenyl)-3-phenyl-1H-pyrrol-2-yl)pyridine, have been prepared. Characterization of the complexes has been performed through a combination of solid- and solution-state methods, including single-crystal X-ray diffraction and electronic absorption and nuclear magnetic resonance spectroscopies. Collectively, these data confirm the formation of the mono- and bis-ligated species. Electrochemistry of a series of bis-ligated actinide complexes, An( Mes PDP Ph ) 2 (An = Th, U, Np), is presented.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗