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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 343 records · Page 19
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Multidisciplinary studies with mutated HIV-1 capsid proteins reveal structural mechanisms of lattice stabilization

Abstract HIV-1 capsid (CA) stability is important for viral replication. E45A and P38A mutations enhance and reduce core stability, thus impairing infectivity. Second-site mutations R132T and T216I rescue infectivity. Capsid lattice stability was studied by solving seven crystal structures (in native background), including P38A, P38A/T216I, E45A, E45A/R132T CA, using molecular dynamics simulations of lattices, cryo-electron microscopy of assemblies, time-resolved imaging of uncoating, biophysical and biochemical characterization of assembly and stability. We report pronounced and subtle, short- and long-range rearrangements: (1) A38 destabilized hexamers by loosening interactions between flanking CA protomers in P38A but not P38A/T216I structures. (2) Two E45A structures showed unexpected stabilizing CA NTD -CA NTD inter-hexamer interactions, variable R18-ring pore sizes, and flipped N-terminal β-hairpin. (3) Altered conformations of E45A a α9-helices compared to WT, E45A/R132T, WT PF74 , WT Nup153 , and WT CPSF6 decreased PF74, CPSF6, and Nup153 binding, and was reversed in E45A/R132T. (4) An environmentally sensitive electrostatic repulsion between E45 and D51 affected lattice stability, flexibility, ion and water permeabilities, electrostatics, and recognition of host factors.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2021

Toward nonthermal control of excited quantum materials: framework and investigations by ultrafast electron scattering and imaging

Quantum material systems upon applying ultrashort laser pulses provide a rich platform to access excited material phases and their transformations that are not entirely like their equilibrium counterparts. The addressability and potential controls of metastable or long-trapped out-of-equilibrium phases have motivated interests both for the purposes of understanding the nonequilibrium physics and advancing the quantum technologies. Thus far, the dynamical spectroscopic probes eminently focus on microscopic electronic and phonon responses. For characterizing the long-range dynamics, such as order parameter fields and fluctuation effects, the ultrafast scattering probes offer direct sensitivity. Bridging the connections between the microscopic dynamics and macroscopic responses is central toward establishing the nonequilibrium physics behind the light-induced phases. Here, we present a path toward such understanding by cross-examining the structure factors associated with different dynamical states obtained from ultrafast electron scattering, imaging, and modeling. We give the basic theoretical framework on describing the non-equilibrium scattering problems and briefly describe how such framework relates to the out-of-equilibrium phenomena. We give effective models outlining the emergences of nonthermal critical points, hidden phases, and non-equilibrium relaxational responses from vacuum-suspended rare-earth tritellurides, tantalum disulfides thin films, and vanadium dioxide nanocrystalline materials upon light excitations.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2026

Collaborative R&D with REEL Solar Inc (REEL) to Understand and Overcome Performance Limitations in CdTe Solar Cells: Cooperative Research and Development (Final Report)

This CRADA will focus on processing, advanced characterization, and testing of photovoltaic materials and devices to understand and improve REEL CdTe solar technology. This will include examining process variations and different buffer, absorber, and contact layers from REEL and NLR to maximize performance. The unique and diverse advanced characterization tools at NLR, such as time-resolved photoluminescence, capacitance-voltage measurements, electron beam scattered diffraction, cathodoluminescence, electron microscopy, TOF-SIMS, and other measurements will be applied to characterize REEL processing to improve understanding and guide experimental directions. Accelerated stability and potential induced degradation tests will be used to analyze metastability, short-and-long term degradation, and improve bankability. A second and major thrust this period will be joint development of Si/CdTe tandem solar cells to overcome industry wide terrestrial solar efficiency limits with the two lowest cost and manufacturable solar materials today. This will include developing novel transparent back contacts that can be incorporated into tandem structures and other novel solar applications, detailed analysis of designs and configurations for CdTe/Si tandem modules, and prototyping REEL CdTe Technology with Si bottom cells in tandem structures.

14 SOLAR ENERGY↗
DOE OSTI2023

Development and implementation of an in situ high-resolution isotopic microscope for measuring metabolic interactions in soil mesocosms (Final Report)

Many of our planet’s ecosystems rely on the activities of soil microbial communities. These microbes have significant and wide-ranging effects: they metabolize carbon and other nutrients, interact with plants and fungi, and perform other processes important to soil health. However, our ability to directly observe the enzymatic and metabolic activities of microbes within soil is currently limited, not only by the complexity of soil microbial communities themselves, but also by the lack of experimental tools to study them and their molecular interactions in situ. These challenges hinder our understanding of the life-sustaining processes of biomass decomposition and the manner in which it contributes to the movement of freed carbon within soil ecosystems. Here we aimed to develop a novel ultrahigh-resolution isotopic microscope that combines complementary imaging modalities to gain insights into metabolic cycling in soil. This final report covers both the portion of this work that was initially completed at the University of North Carolina at Chapel Hill from 2018 to 2019 (as award DE-SC0019012) and then from 2020 to 2022 (2023 in NCE) at the University of Massachusetts Chan Medical School. This goal was to build an integrated platform consisting of fluorescence microscopy, Raman microspectroscopy, and nanospray desorption electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry (nanoDESI-FTICR-MS) to directly investigate microbial activities and molecular transformations occurring in soil by exploiting the use of both fluorescent labels and stable isotope probing. Specifically, our instrument was conceived as integrating: (A) fluorescence detection to localize soil microbes, identify bacteria taking up polysaccharides, and monitor gene expression of enzymes involved in decomposition; (B) Raman microspectroscopy to determine which microbes incorporate decomposition products into their biomass, as well as which decomposers are metabolically active; and (C) nanoDESI-FTICR-MS imaging to spatially probe, in real-time, the metabolites in the surrounding area, which we expect will reveal the distributions of the products of the enzymatic breakdown of polysaccharides, as well as specialized metabolites acting as cell-cell signals between decomposers. To enable these measurements, we exploited fluorescence-based probes to map the microbes that are enzymatically active (per A) and utilized stable isotope-labeled substrates to visualize both the microbial and molecular fate of decomposed biomass (B and C, respectively). To accomplish our goal, we combined the expertise of a multidisciplinary group of scientists to pursue the construction of this microscope and to investigate scientific questions that would be facilitated by such a capability. We aimed to employ this spatially informative, high-resolution isotopic microscope to visualize the critical steps of biomass degradation and the molecular fate of other environmentally relevant substrates within soil mesocosms. Accordingly, this technology will enhance our understanding of the microbial and metabolic interactions occurring within soil communities that are relevant to carbon degradation and other soil processes. The instrument has been developed and housed at EMSL, where it will be available to the entire EMSL User Base, enabling a variety of related DOE-relevant systems to be interrogated in the future by diverse scientific research groups.

59 BASIC BIOLOGICAL SCIENCES↗
NASA NTRS1994

Quantitative 3-D imaging topogrammetry for telemedicine applications

The technology to reliably transmit high-resolution visual imagery over short to medium distances in real time has led to the serious considerations of the use of telemedicine, telepresence, and telerobotics in the delivery of health care. These concepts may involve, and evolve toward: consultation from remote expert teaching centers; diagnosis; triage; real-time remote advice to the surgeon; and real-time remote surgical instrument manipulation (telerobotics with virtual reality). Further extrapolation leads to teledesign and telereplication of spare surgical parts through quantitative teleimaging of 3-D surfaces tied to CAD/CAM devices and an artificially intelligent archival data base of 'normal' shapes. The ability to generate 'topogrames' or 3-D surface numerical tables of coordinate values capable of creating computer-generated virtual holographic-like displays, machine part replication, and statistical diagnostic shape assessment is critical to the progression of telemedicine. Any virtual reality simulation will remain in 'video-game' realm until realistic dimensional and spatial relational inputs from real measurements in vivo during surgeries are added to an ever-growing statistical data archive. The challenges of managing and interpreting this 3-D data base, which would include radiographic and surface quantitative data, are considerable. As technology drives toward dynamic and continuous 3-D surface measurements, presenting millions of X, Y, Z data points per second of flexing, stretching, moving human organs, the knowledge base and interpretive capabilities of 'brilliant robots' to work as a surgeon's tireless assistants becomes imaginable. The brilliant robot would 'see' what the surgeon sees--and more, for the robot could quantify its 3-D sensing and would 'see' in a wider spectral range than humans, and could zoom its 'eyes' from the macro world to long-distance microscopy. Unerring robot hands could rapidly perform machine-aided suturing with precision micro-sewing machines, splice neural connections with laser welds, micro-bore through constricted vessels, and computer combine ultrasound, microradiography, and 3-D mini-borescopes to quickly assess and trace vascular problems in situ. The spatial relationships between organs, robotic arms, and end-effector diagnostic, manipulative, and surgical instruments would be constantly monitored by the robot 'brain' using inputs from its multiple 3-D quantitative 'eyes' remote sensing, as well as by contact and proximity force measuring devices. Methods to create accurate and quantitative 3-D topograms at continuous video data rates are described.

Altschuler, Bruce R.↗
DOE OSTI2025

Ultralow-temperature cryogenic transmission electron microscopy using a new helium flow cryostat stage

Advances in cryogenic electron microscopy have opened new avenues for probing quantum phenomena in correlated materials. This study reports the installation and performance of a new side-entry condenZero cryogenic cooling system for JEOL (Scanning) Transmission Electron Microscopes (S/TEM), utilizing compressed liquid helium (LHe) and designed for imaging and spectroscopy at ultra-low temperatures. The system includes an external dewar mounted on a vibration-damping stage and a pressurized, low-noise helium transfer line with a remotely controllable needle valve, ensuring stable and efficient LHe flow with minimal thermal and mechanical noise. Performance evaluation demonstrates a stable base temperature of 4.37 K measured using a Cernox bare chip sensor on the holder with temperature fluctuations within ±0.004 K. Complementary in-situ electron energy-loss spectroscopy (EELS) via aluminum bulk plasmon analysis was used to measure the local specimen temperature and validate cryogenic operation during experiments. The integration of cryogenic cooling with other microscopy techniques, including electron diffraction and Lorentz TEM, was demonstrated by resolving charge density wave (CDW) transitions in NbSe2 using electron diffraction, and imaging nanometric magnetic skyrmions in MnSi via Lorentz TEM. In conclusion, this platform provides reliable cryogenic operation below 7 K, establishing a low-drift route for direct visualization of electronic and magnetic phase transformations in quantum materials.

Charge density wave↗
DOE OSTI2022

The performance of additively manufactured Haynes 282 in supercritical CO 2

The use of supercritical carbon dioxide (sCO 2 ) as a working fluid is garnering interest in next generation power production systems due to the possibility of increased operational efficiencies and lower associated costs. Its implementation requires alloys with excellent high temperature strength and corrosion resistance, which makes Haynes 282® (H282) a suitable candidate. With increasing adoption of additive manufacturing (AM) in the energy industry, there is a need to investigate long-term sCO2 exposure on AM produced materials. Additively manufactured H282 (AM-H282) samples built using laser powder bed fusion in two different orientations were analyzed through imaging, gravimetric analysis, and room-temperature tensile testing before and after 1000-h exposure to CO 2 at 750 °C and 20 MPa. Performed imaging included observation of the sample surfaces and of the material bulk (cross sections) through means of Scanning Electron Microscopy (SEM) and optical microscopy. In comparison to wrought H282, it was found that the exposed material exhibited a similar Cr 2 O 3 oxide protective layer about 2 μm in thickness with additional top-surface TiO 2 oxide and carbon-rich precipitates. It was also similarly observed that internal oxidation was present but limited to a depth of 20 μm, and a 1–3 μm γ’ denuded region appeared to surround all internal and surface oxidation. Thermal aging effects were noted with the precipitation of needle-like structures in the γ/γ’ matrix and a coarsening of the γ’ precipitates from 28 nm to 73 nm. Mass measurements analyzing oxide precipitation revealed a larger increase compared to wrought, representing an approximate 20% difference. Tensile testing results showed similar behavior to wrought with a slight increase in yield strength and a large reduction in elongation in the exposed samples.

36 MATERIALS SCIENCE↗
DOE OSTI2022

The effects of microstructure on deformation twinning in Mg WE43

The interplay between microstructure and deformation twinning in a WE43-T6 Mg alloy under uniaxial compression was investigated using a combination of scanning electron microscopy with digital image correlation (SEM-DIC) and crystal plasticity finite element (CPFE) simulation. To improve understanding of the statistical characteristics of deformation twin formation, microstructural effects were characterized in over 1000 grains through metrics including the nominal Schmid Factor, grain size, geometric compatibility factor (m'), residual Burgers vector, and the strain accommodated by neighboring grains. There was a strong correlation between the nominal Schmid Factor and both twin activation and variant selection, but this was not fully deterministic. Deformation twinning also exhibited a strong dependence on existing slip and twinning in the neighboring grain and on the m' value. Within the range of grain sizes present in this condition, grain size was determined to have minimal effect on deformation twinning. Finally, statistical analysis of CPFE simulations was used to further investigate microstructural effects on twinning, and qualitatively captured the effect of the nominal Schmid Factor.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Ultrathin Boron Growth onto Nanodiamond Surfaces via Electrophilic Boron Precursors

Diamond as a templating substrate is largely unexplored, and the unique properties of diamond, including its large bandgap, thermal conductance, and lack of cytotoxicity, makes it versatile in emergent technologies in medicine and quantum sensing. Surface termination of an inert diamond substrate and its chemical reactivity are key in generating new bonds for nucleation and growth of an overlayer material. Oxidized high-pressure high temperature (HPHT) nanodiamonds (NDs) are largely terminated by alcohols that act as nucleophiles to initiate covalent bond formation when an electrophilic reactant is available. In this work, we demonstrate a templated synthesis of ultrathin boron on ND surfaces using trigonal boron compounds. Boron trichloride (BCl 3 ), boron tribromide (BBr 3 ), and borane (BH 3 ) were found to react with ND substrates at room temperature in inert conditions. BBr 3 and BCl 3 were highly reactive with the diamond surface, and sheet-like structures were produced and verified with electron microscopy. Surface-sensitive spectroscopies were used to probe the molecular and atomic structure of the ND constructs’ surface, and quantification showed the boron shell was less than 1 nm thick after 1–24 h reactions. Observation of the reaction supports a self-terminating mechanism, similar to atomic layer deposition growth, and is likely due to the quenching of alcohols on the diamond surface. X-ray absorption spectroscopy revealed that boron-termination generated midgap electronic states that were originally predicted by density functional theory (DFT) several years ago. DFT also predicted a negative electron surface, which has yet to be confirmed experimentally here. The boron-diamond nanostructures were found to aggregate in dichloromethane and were dispersed in various solvents and characterized with dynamic light scattering for future cell imaging or cancer therapy applications using boron neutron capture therapy (BNCT). The unique templating mechanism based on nucleophilic alcohols and electrophilic trigonal precursors allows for covalent bond formation and will be of interest to researchers using diamond for quantum sensing, additive manufacturing, BNCT, and potentially as an electron emitter.

36 MATERIALS SCIENCE↗
NASA NTRS2017

Field Exploration and Life Detection Sampling Through Planetary Analogue Sampling (FELDSPAR).

Exploration missions to Mars rely on rovers to perform analyses over small sampling areas; however, landing sites for these missions are selected based on large-scale, low-resolution remote data. The use of Earth analogue environments to estimate the multi-scale spatial distributions of key signatures of habitability can help ensure mission science goals are met. A main goal of FELDSPAR is to conduct field operations analogous to Mars sample return in its science, operations, and technology from landing site selection, to in-field sampling location selection, remote or stand-off analysis, in situ analysis, and home laboratory analysis. Lava fields and volcanic regions are relevant analogues to Martian landscapes due to desiccation, low nutrient availability, and temperature extremes. Operationally, many Icelandic lava fields are remote enough to require that field expeditions address several sampling constraints that are experienced in robotic exploration, including in situ and sample return missions. The Fimmvruhls lava field was formed by a basaltic effusive eruption associated with the 2010 Eyjafjallajkull eruption. Mlifellssandur is a recently deglaciated plain to the north of the Myrdalsjkull glacier. Holuhraun was formed by a 2014 fissure eruptions just north of the large Vatnajkull glacier. Dyngjusandur is an alluvial plain apparently kept barren by repeated mechanical weathering. Informed by our 2013 expedition, we collected samples in nested triangular grids every decade from the 10 cm scale to the 1 km scale (as permitted by the size of the site). Satellite imagery is available for older sites, and for Mlifellssandur, Holuhraun, and Dyngjusandur we obtained overhead imagery at 1 m to 200 m elevation. PanCam-style photographs were taken in the field by sampling personnel. In-field reflectance spectroscopy was also obtained with an ASD spectrometer in Dyngjusandur. All sites chosen were 'homogeneous' in apparent color, morphology, moisture, grain size, and reflectance spectra at all scales greater than 10 cm. Field lab assays were conducted to monitor microbial habitation, including ATP quantification, qPCR for fungal, bacterial, and archaeal DNA, and direct cell imaging using fluorescence microscopy. Home laboratory analyses include Raman spectroscopy and community sequencing. ATP appeared to be significantly more sensitive to small changes in sampling location than qPCR or fluorescence microscopy. Bacterial and archaeal DNA content were more consistent at the smaller scales, but similarly variable across more distant sites. Conversely, cell counts and fungal DNA content have significant local variation but appear relatively homogeneous over scales of 1 km. ATP, bacterial DNA, and archaeal DNA content were relatively well correlated at many spatial scales. While we have observed spatial variation at various scales and are beginning to observe how that variation fluctuates over time as biodiversity recovers after an eruption, we do not yet fully understand what parameters lead to the observed spatial variation. Home laboratory analyses will help us further understand the elemental and structural composition of the basaltic matrices, but further field analyses are vital for the understanding how temperature, moisture, incident radiation, and so forth influence the habitability of a microclimate.

Field↗
DOE OSTI2023

Atomic-scale origin of the low grain-boundary resistance in perovskite solid electrolyte Li 0.375 Sr 0.4375 Ta 0.75 Zr 0.25 O 3

Oxide solid electrolytes (OSEs) have the potential to achieve improved safety and energy density for lithium-ion batteries, but their high grain-boundary (GB) resistance generally is a bottleneck. In the well-studied perovskite oxide solid electrolyte, Li 3x La 2/3-x TiO 3 (LLTO), the ionic conductivity of grain boundaries is about three orders of magnitude lower than that of the bulk. In contrast, the related Li 0.375 Sr 0.4375 Ta 0.75 Zr 0.25 O 3 (LSTZ0.75) perovskite exhibits low grain boundary resistance for reasons yet unknown. Here, we use aberration-corrected scanning transmission electron microscopy and spectroscopy, along with an active learning moment tensor potential, to reveal the atomic scale structure and composition of LSTZ0.75 grain boundaries. Vibrational electron energy loss spectroscopy is applied for the first time to reveal atomically resolved vibrations at grain boundaries of LSTZ0.75 and to characterize the otherwise unmeasurable Li distribution therein. We find that Li depletion, which is a major reason for the low grain boundary ionic conductivity of LLTO, is absent for the grain boundaries of LSTZ0.75. Instead, the low grain boundary resistivity of LSTZ0.75 is attributed to the formation of a nanoscale defective cubic perovskite interfacial structure that contained abundant vacancies. Our study provides new insights into the atomic scale mechanisms of low grain boundary resistivity.

25 ENERGY STORAGE↗
DOE OSTI2025

Exploring Domain-Wall Pinning in Ferroelectrics via Automated High-Throughput Atomic Force Microscopy

Domain-wall dynamics in ferroelectric materials are strongly position-dependent, since each polar interface is locked into a unique local microstructure. This necessitates spatially resolved studies of wall pinning using scanning-probe microscopy techniques. The pinning centers and pre-existing domain walls are usually sparse within the image plane, precluding the use of dense hyperspectral imaging modes and requiring time-consuming human experimentation. Here, a large-area epitaxial PbTiO 3 film on cubic KTaO 3 was investigated to quantify the electric-field-driven dynamics of the polar–strain domain structures using ML-controlled automated piezoresponse force microscopy. Analysis of 1500 switching events reveals that domain-wall displacement depends not only on field parameters but also on the local ferroelectric–ferroelastic configuration. For example, twin boundaries in polydomains regions, like a 1 – /c+ ∥ a 2 – /c – , stay pinned up to a certain level of bias magnitude and change only marginally as the bias increases from 20 to 30 V, whereas single-variant boundaries, like the a 2 + /c + ∥ a 2 – /c – stack, are already activated at 20 V. These statistics on the possible ferroelectric and ferroelastic wall orientations, together with the automated high-throughput AFM workflow, can be distilled into a predictive map that links domain configurations to pulse parameters. Here, this microstructure-specific rule set forms the foundation for the design of ferroelectric memories.

automated scanning probe microscopy↗
DOE OSTI2025

Dynamic nanodomains dictate macroscopic properties in lead halide perovskites

Lead halide perovskites have emerged as promising materials for solar energy conversion and X-ray detection owing to their remarkable optoelectronic properties. However, the microscopic origins of their superior performance remain unclear. Here we show that low-symmetry dynamic nanodomains present in the high-symmetry average cubic phases, whose characteristics are dictated by the A-site cation, govern the macroscopic behaviour. We combine X-ray diffuse scattering, inelastic neutron spectroscopy, hyperspectral photoluminescence microscopy and machine-learning-assisted molecular dynamics simulations to directly correlate local nanoscale dynamics with macroscopic optoelectronic response. Our approach reveals that methylammonium-based perovskites form densely packed, anisotropic dynamic nanodomains with out-of-phase octahedral tilting, whereas formamidinium-based systems develop sparse, isotropic, spherical nanodomains with in-phase tilting, even when crystallography reveals cubic symmetry on average. We demonstrate that these sparsely distributed isotropic nanodomains present in formamidinium-based systems reduce electronic dynamic disorder, resulting in a beneficial optoelectronic response, thereby enhancing the performance of formamidinium-based lead halide perovskite devices. By elucidating the influence of the A-site cation on local dynamic nanodomains, and consequently, on the macroscopic properties, we propose leveraging this relationship to engineer the optoelectronic response of these materials, propelling further advancements in perovskite-based photovoltaics, optoelectronics and X-ray imaging.

Materials Science↗
DOE OSTI2023

Review of multi-faceted morphologic signatures of actinide process materials for nuclear forensic science

Particle morphology is an emerging signature that has the potential to identify the processing history of unknown nuclear materials. Using readily available scanning electron microscopes (SEM), the morphology of nearly any solid material can be measured within hours. Coupled with robust image analysis and classification methods, the morphological features can be quantified and support identification of the processing history of unknown nuclear materials. The viability of this signature depends on developing databases of morphological features, coupled with a rapid data analysis and accurate classification process. With developed reference methods, datasets, and throughputs, morphological analysis can be applied within days to (i) interdicted bulk nuclear materials (gram to kilogram quantities), and (ii) trace amounts of nuclear materials detected on swipes or environmental samples. In conclusion, this review aims to develop validated and verified analytical strategies for morphological analysis relevant to nuclear forensics.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Nondestructive ultrasonic characterization of a triple-weld-bead wire arc additively manufactured ER70S-6 S-curved wall

Understanding build-scale microstructural variation in wire arc additive manufacturing (WAAM) of low-carbon steels is essential for ensuring consistent structure–property relationships throughout large components. Conventional destructive characterization techniques, such as scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD), are time-intensive and limited to localized regions, making comprehensive evaluation of large WAAM structures challenging. In this study, a nondestructive ultrasonic approach was employed to characterize a 252 mm tall ER70S-6 S-curved WAAM wall produced using a triple-bead deposition strategy. Optical and SEM analysis revealed a repeating dual-region microstructure consisting of uniform polygonal ferrite at melt pool centers and heterogeneous ferrite with coarse and fine grains near melt pool boundaries, attributed to cyclic thermal conditions. Longitudinal ultrasonic backscatter imaging was used to evaluate the continuity of this periodicity along the full build height. The ultrasonic response exhibited a consistent repeating pattern that correlated with the observed layer-wise microstructural variation. X-ray computed tomography confirmed the absence of detectable porosity, indicating that ultrasonic contrast is primarily governed by grain morphology. Overall, the results indicate that longitudinal backscatter ultrasound is a promising nondestructive characterization technique for validating microstructural variations along the s-curved WAAM wall, with significant potential for microstructure optimization and process control.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Illuminating the Material World: Autonomous Microscopy to Understand Order, Disorder, and Everything In Between

Artificial intelligence (AI) holds immense promise for revolutionizing microscopy, yet its widespread adoption has been hindered by challenges ranging from user inexperience to limited model transferability and difficulties in operationalizing machine learning. This presentation showcases our approach to developing practical autonomy for materials discovery, aiming to accelerate the integration of AI into everyday microscopy workflows. As shown in Fig. 1, I will focus on three key areas: understanding order-disorder transitions, quantifying point defects, and achieving truly device-scale microscopy. First, I will demonstrate the power of multi-modal knowledge graphs for integrating diverse microscopy data. By combining imaging, spectroscopy, and diffraction data, these graphs provide a holistic view of material behavior, capturing the intricate relationships between different modalities [1,2]. I will present a case study on how these models illuminate the structural and chemical changes associated with irradiation in oxide thin films, revealing critical insights for designing materials for extreme environments like spaceflight and nuclear energy. Specifically, I will show how multi-modal analysis clarifies the evolution of order-disorder transitions under irradiation, a key factor influencing material performance in these applications. Next, I will address the challenge of quantifying point defects in 2D materials. We demonstrate the application of computer vision and transfer learning to accurately identify and classify various defect types, such as vacancies and substitutional atoms, and to quantify their concentrations. This information is crucial for understanding and tailoring the properties of 2D materials for applications in electronics, optoelectronics, and catalysis. For example, I will show how our models can characterize the topological distribution of point defects in MXene transition metal carbides, providing valuable insights for optimizing their performance in energy storage and separation science. Finally, I will discuss our progress toward autonomous device-scale microscopy [3,4]. We are fundamentally redesigning electron microscopes around the principles of machine reasoning, enabling automation beyond basic tasks like sample navigation and data acquisition to include sophisticated experimental design. This approach paves the way for truly reproducible and massively scaled analysis campaigns. I will emphasize the importance of autonomous microscopy platforms for high-throughput materials discovery and characterization, facilitating the rapid screening of materials for a broad range of applications and accelerating the development of next-generation technologies.

36 MATERIALS SCIENCE↗
NASA NTRS2000

Creep Properties of NiAl-1Hf Single Crystals Re-Investigated

NiAl-1Hf single crystals have been shown to be quite strong at 1027 C, with strength levels approaching those of advanced Ni-based superalloys. Initial testing, however, indicated that the properties might not be reproducible. Study of the 1027 C creep behavior of four different NiAl-1Hf single-crystal ingots subjected to several different heat treatments indicated that strength lies in a narrow band. Thus, we concluded that the mechanical properties are reproducible. Recent investigations of the intermetallic NiAl have confirmed that minor alloying additions combined with single-crystal growth technology can produce elevated temperature strength levels approaching those of Ni-based superalloys. For example, General Electric alloy AFN 12 {Ni-48.5(at.%) Al-0.5Hf-1Ti-0.05Ga} has a creep rupture strength equivalent to Rene 80 combined with a approximately 30-percent lower density, a fourfold improvement in thermal conductivity, and the ability to form a self-protective alumina scale in aggressive environments. Although the compositions of strong NiAl single crystals are relatively simple, the microstructures are complex and vary with the heat treatment and with small ingot-toingot variations in the alloy chemistry. In addition, initial testing suggested a strong dependence between microstructure and creep strength. If these observations were true, the ability to utilize NiAl single-crystal rotating components in turbine machinery could be severely limited. To investigate the possible limitations in the creep response of high-strength NiAl single crystals, the NASA Glenn Research Center at Lewis Field initiated an in depth investigation of the effect of heat treatment on the microstructure and subsequent 1027 C creep behavior of [001]-oriented NiAl-1Hf with a nominal chemistry of Ni-47.5Al-1Hf-0.5Si. This alloy was selected since four ingots, grown over a number of years and possessing slightly different compositions, were available for study. Specimens taken from the ingots were subjected to several heat treatment schedules, examined by transmission electron microscopy, and tested in both compression and tension. An example of the microstructure found in a [001]-oriented NiAl-1Hf specimen after a solution treatment at 1317 C for 50 hr followed by air cooling is illustrated in the image on the left, where the NiAl matrix contains a uniform distribution of nanometer-scale Gphase (Ni16Hf6Si7) precipitates. Other heat treating schedules produced microstructures with nanometer-sized G-phase cubes and plates or, in an extreme case, produced a microstructure with all the G-phase converted to Heusler (Ni2AlHf) particles. The results of 1027 C creep strength and strain rate testing are illustrated which summarizes data from tensile and compressive testing of samples cut from all four NiAl-1Hf ingots and subjected to a variety of heat treatment schedules. With one exception, all the strength values lie in a narrow band that spans six orders of magnitude in strain rate. The only factor that produced results outside of this band was the heat treatment schedule that dissolved all the G-phase and replaced it with Heusler precipitates. The results portrayed in this figure lead to the important practical conclusion that the elevated-temperature creep properties of NiAl-1Hf single crystals are reproducible and are not affected by small variations in alloy chemistry from ingot to ingot or by different initial distributions of G-phase in the heat-treated alloy. The only variable in this study that produced a significant and delerious effect on mechanical strength was a post-solution heat treatment that lead to the complete disappearance of the G-phase in favor of Heusler precipitates.

Whittenberger, J. Daniel↗