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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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Microstructural Characterization of Felsite Fragments From the Apollo Next Generation Sample Analysis (ANGSA) Double Drive Tube 73001/73002

While the Moon’s surface is dominated by mafic igneous products formed through the crystallization of the lunar magma ocean, and the subsequent eruption of mare basalts – felsic magmatic fragments (variably referred to as felsites, granites, rhyolites or granophyres) have been identified from a number of Apollo samples (e.g. 12013[1], 14321[2], 15405[3] and 73215[4]). Magmatic edifices like the Gruithuisen Domes – silicic constructs sometimes found proximal to the basaltic mare provinces filling nearside basins, may represent a petrogenetic origin. However, this is, is complicated by the fact that they apparently predate mare volcanism (e.g. [5]). Additionally, crater-counting indicates that these silicic surface features also postdate radiogenic ages of Apollo felsites [6]. Various modes of felsic magmatism have been invoked to explain the presence of felsic lithologies on the Moon, including: 1) fractional crystallization and silicate liquid immiscibility; 2) partial melting of lunar crust through basaltic underplating; and 3) fractional crystallization of the mare parent magmas. Although these models are plausible, based on known Apollo samples and lunar meteorites, they are complicated by the lack of sample lithologies with intermediate composition between basaltic magmas and the felsic components, and the fact that partial melting of many crustal rock types on the Moon (e.g., anorthosite, troctolites) are unlikely to form granites. Along with other unique magmatic lithologies, new felsites have been identified within the < 1 mm size fractions of the ANGSA double drive core tube (73001/73002) from Apollo 17 station 3, sampling the light mantle landslide deposit from the South Massif [7]. These additional examples of lunar felsite will help us to better constrain the processes that lead to the formation of these evolved lithologies. To do this, we have employed a gambit of high-resolution scanning electron microscopy (SEM) and scanning transmission electron microscopy (TEM) analytical techniques, including electron backscatter diffraction (EBSD), cathodoluminescence and high-angle annular dark field (HAADF) imaging. These data provide unique insights into the felsite mineralogy and microstructures including the coexistence of quartz and tridymite in many of the fragments. In addition, these analyses provide petrological context and assist targeted in situ secondary ion mass spectrometry (SIMS) measurements of the U-Pb systematics of accessory minerals, and the volatile abundances and D/H ratios of apatite grains identified within the clasts.

lunar↗
DOE OSTI2022

TopTemp: Parsing Precipitate Structure from Temper Topology

Technological advances are in part enabled by the development of novel manufacturing processes that give rise to new materials or material property improvements. Development and evaluation of new manufacturing methodologies is labor-, time-, and resource-intensive expensive due to complex, poorly defined relationships between advanced manufacturing process parameters and the resulting microstructures. In this work, we present a topological representation of temper (heat-treatment) dependent material micro-structure, as captured by scanning electron microscopy, called TopTemp. We show that this topological representation is able to support temper classification of microstructures in a data limited setting, generalizes well to previously unseen samples, is robust to image perturbations, and captures domain interpretable features. The presented work outperforms conventional deep learning baselines and is a first step towards improving understanding of process parameters and resulting material properties.

Kassab, Lara↗
DOE OSTI2025

Mind the gap: Bridging the divide between AI aspirations and the reality of autonomous microscopy

What does materials science look like in the “Age of Artificial Intelligence?” Each material’s domain—synthesis, characterization, and modeling—has a different answer to this question, motivated by unique challenges and constraints. This work focuses on the tremendous potential of autonomous characterization within electron microscopy. We present our recent advancements in developing domain-aware, multimodal models for microscopy analysis capable of describing complex atomic systems. We then address the critical gap between the theoretical promise of autonomous microscopy and its current practical limitations, showcasing recent successes while highlighting the necessary developments to achieve robust, real-world autonomy.

2D materials↗
DOE OSTI2024

Phase Composition and Phase Transformation of Additively Manufactured Nickel Alloy 718 AM Bench Artifacts

Additive manufacturing (AM) technologies offer unprecedented design flexibility but are limited by a lack of understanding of the material microstructure formed under their extreme and transient processing conditions and its subsequent transformation during post-build processing. As part of the 2022 AM Bench Challenge, sponsored by the National Institute of Standards and Technology, this study focuses on the phase composition and phase evolution of AM nickel alloy 718, a nickel-based superalloy, to provide benchmark data essential for the validation of computational models for microstructural predictions. Here, we employed high-energy synchrotron X-ray diffraction, in situ synchrotron X-ray scattering, as well as high-resolution transmission electron microscopy for our analyses. The study uncovers critical aspects of the microstructure in its as-built state, its transformation during homogenization, and its phase evolution during subsequent aging heat treatment. Specifically, we identified secondary phases, monitored the dissolution and coarsening of microstructural elements, and observed the formation and stability of γ ’ and γ ” phases. The results provide the rigorous benchmark data required to understand the atomic and microstructural transformations of AM nickel alloy 718, thereby enhancing the reliability and applicability of AM models for predicting phase evolution and mechanical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2022

The effect of hardness on polymer-bonded pentaerythritol tetranitrate (PETN) explosive impact sensitivity

Handling sensitivity is an important property to assess when working with explosive samples and can be measured using a variety of tests, including drop-weight impact sensitivity. There exists a longstanding interest in the explosives community on the importance of measurable chemical, physical, and mechanical properties of explosives in impact sensitivity. However, most recent work in this area has explored chemical attributes rather than physical and mechanical properties of explosives. In this study, we measure hardness of explosive samples of pentaerythritol tetranitrate and Sylgard binder (XTX) during the curing process. The samples have been characterized for particle morphology through scanning electron microscopy and handling sensitivity through drop-weight impact testing. The relative importance of states of cure, methods of curing, morphology, and age of material are discussed. The data indicate that although there is a notable difference in morphology and mechanical properties for the samples as the polymer-bonded mixtures cure, the resulting changes to mechanical properties have a minimal effect on the sensitivity of the XTX.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Analysis of Interpretable Data Representations for 4D-STEM Using Unsupervised Learning

Abstract Understanding the structure of materials is crucial for engineering devices and materials with enhanced performance. Four-dimensional scanning transmission electron microscopy (4D-STEM) is capable of mapping nanometer-scale local crystallographic structure over micron-scale field of views. However, 4D-STEM datasets can contain tens of thousands of images from a wide variety of material structures, making it difficult to automate detection and classification of structures. Traditional automated analysis pipelines for 4D-STEM focus on supervised approaches, which require prior knowledge of the material structure and cannot describe anomalous or deviant structures. In this article, a pipeline for engineering 4D-STEM feature representations for unsupervised clustering using non-negative matrix factorization (NMF) is introduced. Each feature is evaluated using NMF and results are presented for both simulated and experimental data. It is shown that some data representations more reliably identify overlapping grains. Additionally, real space refinement is applied to identify spatially distinct sample regions, allowing for size and shape analysis to be performed. This work lays the foundation for improved analysis of nanoscale structural features in materials that deviate from expected crystallographic arrangement using 4D-STEM.

Bruefach, Alexandra (ORCID:0000000209323477)↗
DOE OSTI2021

Population balance modeling of polyurethane foam formation with pressure‐dependent growth kernel

Abstract Polyurethane foams are widely used materials often chosen for their useful characteristics such as low thermal conductivity, ease of application, and high strength‐to‐weight ratios. Computational models are needed to predict the dynamics of the flow and expansion, and the resulting material properties, to improve manufacturing processes. In this paper, a model for PMDI, a water‐blown polyurethane foam, is presented. By extending a kinetics‐based approach by adding bubble‐scale information via a population balance equation (PBE) using the quadrature method of moments, we can track bubble size distributions during foaming. We present results from a three‐dimensional computational fluid dynamics model using arbitrary Lagrangian–Eulerian interface tracking implemented in finite element software. The model compares favorably with experimental data, including dynamics, bubble distributions measured by both camera and diffusion wave spectroscopy, and post‐test bubble size from scanning electron microscopy and density measurements from x‐ray computed tomography.

Ortiz, Weston↗
DOE OSTI2020

Deep Learning and Structural Imaging of Materials

Deep learning has had a transformative effect on numerous domains and is actively utilized by many scientists in data-intensive fields such as high-energy physics and cosmology. Materials science, and in particular, the structural imaging of materials with electrons and X-rays are projected to enter the age of scientific data torrents, positioning them as new application spaces for modern artificial intelligence. In this contribution, we provide a synopsis on the foundations and latest progress in deep learning and present an in-depth application of utilizing modern deep artificial neural networks in scanning transmission electron microscopy to extract structural material properties. We use this case study to expose the strengths of deep learning-based models and discuss their current limitations, in the process highlighting their potential use in other data-intensive structural imaging modalities.

Laanait, Nouamane↗
DOE OSTI2023

In Situ Ultra-Small- and Small-Angle X-ray Scattering Study of ZnO Nanoparticle Formation and Growth through Chemical Bath Deposition in the Presence of Polyvinylpyrrolidone

ZnO inverse opals combine the outstanding properties of the semiconductor ZnO with the high surface area of the open-porous framework, making them valuable photonic and catalysis support materials. One route to produce inverse opals is to mineralize the voids of close-packed polymer nanoparticle templates by chemical bath deposition (CBD) using a ZnO precursor solution, followed by template removal. To ensure synthesis control, the formation and growth of ZnO nanoparticles in a precursor solution containing the organic additive polyvinylpyrrolidone (PVP) was investigated by in situ ultra-small- and small-angle X-ray scattering (USAXS/SAXS). Before that, we studied the precursor solution by in-house SAXS at T = 25 °C, revealing the presence of a PVP network with semiflexible chain behavior. Heating the precursor solution to 58 °C or 63 °C initiates the formation of small ZnO nanoparticles that cluster together, as shown by complementary transmission electron microscopy images (TEM) taken after synthesis. The underlying kinetics of this process could be deciphered by quantitatively analyzing the USAXS/SAXS data considering the scattering contributions of particles, clusters, and the PVP network. A nearly quantitative description of both the nucleation and growth period could be achieved using the two-step Finke–Watzky model with slow, continuous nucleation followed by autocatalytic growth.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Micro- and nano-porosity of the active Alpine Fault zone, New Zealand

Porosity reduction in rocks from a fault core can cause elevated pore fluid pressures and consequently influence the recurrence time of earthquakes. We investigated the porosity distribution in the New Zealand's Alpine Fault core in samples recovered during the first phase of the Deep Fault Drilling Project (DFDP-1B) by using two-dimensional nanoscale and three-dimensional microscale imaging. Synchrotron X-ray microtomography-derived analyses of open pore spaces show total microscale porosities in the range of 0.1 %–0.24 %. These pores have mainly non-spherical, elongated, flat shapes and show subtle bipolar orientation. Scanning and transmission electron microscopy reveal the samples' microstructural organization, where nanoscale pores ornament grain boundaries of the gouge material, especially clay minerals. Our data imply that (i) the porosity of the fault core is very small and not connected; (ii) the distribution of clay minerals controls the shape and orientation of the associated pores; (iii) porosity was reduced due to pressure solution processes; and (iv) mineral precipitation in fluid-filled pores can affect the mechanical behavior of the Alpine Fault by decreasing the already critically low total porosity of the fault core, causing elevated pore fluid pressures and/or introducing weak mineral phases, and thus lowering the overall fault frictional strength. We conclude that the current state of very low porosity in the Alpine Fault core is likely to play a key role in the initiation of the next fault rupture.

58 GEOSCIENCES↗
NASA NTRS1975

Interaction of hydrogen chloride with alumina

The influence of outgas conditions and temperature on the adsorptive properties of two aluminas Alon-c and Al6sG were studied using adsorption isotherm measurements. Alon-C and Al6SG were characterized using X-ray powder diffraction, thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and BET nitrogen surface areas. Some of these techniques were applied to two other aluminas but no isotherm data was obtained. Isotherm data and techniques applied to each alumina are summarized in tabular form.

Bailey, R. R.↗
NASA NTRS1981

Experiment K-314: Fetal and neonatal rat bone and joint development following in Utero spaceflight

Infant rat limb specimens from Soviet and U.S. ground-based studies were examined by radiography, macrophotography, histologic sectioning and staining and scanning electron microscopy. A comparison was conducted between vivarium and flight-type diets suggesting that nutritional obesity may adversely affect pregnancy. Data were obtained on maturation of ossification centers, orientation of collagen fibers in bone, tendon and ligaments, joint surface texture and spatial relationships of bones of the hind limb. Computer reconstructions of the knee and hip show promise as a means of investigating the etiology of congenital hip dislocation.

Sabelman, E. E.↗
NASA NTRS1983

Particulate erosion mechanisms

Particulate damage and erosion of ductile metals are today plaguing design and field engineers in diverse fields of engineering and technology. It was found that too many models and theories were proposed leading to much speculation from debris analysis and failure mechanism postulations. Most theories of solid particle erosion are based on material removal models which do not fully represent the actual physical processes of material removal. The various mechanisms proposed thus far are: melting, low-cycle fatigue, extrusion, delamination, shear localization, adhesive material transfer, etc. The experimental data on different materials highlighting the observed failure modes of the deformation and cutting wear processes using optical and scanning electron microscopy are presented. The most important mechanisms proved from the experimental observations of the specimens exposed to both spherical and angular particles are addressed, and the validity of the earlier theories discussed. Both the initial stages of damage and advanced stages of erosion were studied to gain a fundamental understanding of the process.

Veerabhadrarao, P.↗
NASA NTRS2004

In Situ Location and Characterization of Carbon-bearing Phases in Carbonaceous Chondrites: Insights from Yamato 791198, a Weakly-altered CM2 Chondrite

Intense studies of carbonaceous chondrites have provided remarkable insights into the behavior of carbon during the earliest stages of our solar system. This research has demonstrated that carbonaceous meteorites contain a diverse array of organic compounds, whose origins are probably the result of multiple processes that occurred in different locations including interstellar space, the solar nebula and asteroidal parent bodies [1-3]. The most abundant organic carbon component in CI1 and CM2 carbonaceous chondrites is so-called macromolecular carbon, a high molecular weight material that has some affinities to terrestrial kerogen and constitutes approximately 60-70% of the organic material in these meteorites. Although recent studies e.g. [3] have radically improved our understanding of the structural and compositional characteristics of this material, a number of key questions remain to be addressed. In particular, our knowledge of where this macromolecular material is distributed at the fine-scale within carbonaceous chondrites is scant. [4] have shown that organic material is associated with phyllosilicate-rich matrix in CM chondrites, but the detailed mineralogical associations are not well-known. Over the past 2 years, we have begun to address this question by using energy filtered transmission electron microscopy (EFTEM) to locate carbon-bearing materials in situ, focusing specifically on the CM2s. To date we have reported data on the Murchison CM2 chondrite [5], a meteorite that has experienced a modest degree of aqueous alteration. To extend our observations to other CM2 chondrites, we have examined the occurrence of carbon-bearing phases in Yamato 791198. Our recent studies [5] have shown that Y-791198 is among the most weakly-altered CM chondrite currently known and hence is likely to preserve a quite primitive distribution of carbonaceous material. In this study, we present initial observations on the distribution of these materials in one fine-grained rim and compare them with our results from Murchison. Such information may provide important insights into the origins of the carbonaceous material and how it was distributed in nebular and perhaps presolar dust.

Brearley, Adrian J.↗
DOE OSTI2021

Enabling phase quantification of anhydrous cements via Raman imaging

The phase composition of Portland cements is typically determined using conventional techniques like X-ray Diffraction (XRD) Rietveld analysis, optical microscopy point counting, and electron microscopy. However, these techniques have several limitations that may affect their accuracy in certain sample-specific scenarios. Here, we report a highly accurate phase quantification of 11 different types of commercial, anhydrous cements using a new and complementary technique: Raman imaging. Specifically, for the 4 principal phases, composition from our extensive data (250,000 Raman spectra per sample, error < 0.71%) and those obtained from XRD Rietveld and supplier data have high coefficients of determination (R{sup 2} > 0.98, mean deviation <2%). Additionally, we also quantify 8 secondary phases present in cement clinkers (gypsum, anhydrite, bassanite, syngenite, dolomite, calcite, quartz, and portlandite) with a high degree of confidence, thereby demonstrating that Raman imaging is a highly versatile tool for anhydrous phase quantification in a broad variety of cements.

36 MATERIALS SCIENCE↗
NASA NTRS1994

Nucleation, growth, and strain relaxation of lattice-mismatched 3-5 semiconductor epitaxial layers

We have investigated the early stages of evolution of highly strained 2-D InAs layers and 3-D InAs islands grown by metal-organic chemical vapor deposition (MOCVD) on (100) and (111)B GaAs substrates. The InAs epilayer/GaAs substrate combination has been chosen because the lattice-mismatch is severe (approximately 7.2 percent), yet these materials are otherwise very similar. By examining InAs-on-GaAs composites instead of the more common In(x)Ga(1-x)As alloy we remove an additional degree of freedom (x) and thereby simplify data interpretation. A matrix of experiments is described in which the MOCVD growth parameters - susceptor temperature, Thin flux, and AsH3 flux - have been varied over a wide range. Scanning electron microscopy, atomic force microscopy, transmission electron microscopy, and electron microprobe analysis have been employed to observe the thin film surface morphology. In the case of 3-D growth, we have extracted activation energies and power-dependent exponents that characterize the nucleation process. As a consequence, optimized growth conditions have been identified for depositing approximately 250 A thick (100) and (111)B oriented InAs layers with relatively smooth surfaces. Together with preliminary data on the strain relaxation of these layers, the above results on the evolution of thin InAs films indicate that the (111)B orientation is particularly promising for yielding lattice-mismatched films that are fully relaxed with only misfit dislocations at the epilayer/substrate interface.

Welser, R. E.↗
NASA NTRS1994

Nucleation, Growth, and Strain Relaxation of Lattice-Mismatched III-V Semiconductor Epitaxial Layers

We have investigated the early stages of evolution of highly strained 2-D InAs layers and 3-D InAs islands grown by metal-organic chemical vapor deposition (MOCVD) on (100) and (111) B GaAs substrates. The InAs epilayer / GaAs substrate combination has been chosen because the lattice-mismatch is severe (approx. 7.20%), yet these materials are otherwise very similar. By examining InAs-on-GaAs composites Instead of the more common In(x)Ga(1-x)As alloy, we remove an additional degree of freedom (x) and thereby simplify data interpretation. A matrix of experiments is described in which the MOCVD growth parameters -- susceptor temperature, TMIn flux, and AsH3 flux -- have been varied over a wide range. Scanning electron microscopy, atomic force microscopy, transmission electron microscopy, and electron microprobe analysis have been employed to observe the thin film surface morphology. In the case of 3-D growth, we have extracted activation energies and power-dependent exponents that characterize the nucleation process. As a consequence, optimized growth conditions have been identified for depositing approx. 250 A thick (100) and (111)B oriented InAs layers with relatively smooth surfaces. Together with preliminary data on the strain relaxation of these layers, the above results on the evolution of thin InAs films indicate that the (111)B orientation is particularly promising for yielding lattice-mismatched films that are fully relaxed with only misfit dislocations at the epilayer / substrate interface.

Welser, R. E.↗
DOE OSTI2020

Nanoconfinement of Molecular Magnesium Borohydride Captured in a Bipyridine-Functionalized Metal-Organic Framework

The lower limit of metal hydride nanoconfinement is demonstrated through the coordination of a molecular hydride species to binding sites inside the pores of a metal-organic framework (MOF). Magnesium borohydride, which has a high hydrogen capacity, is incorporated into the pores of UiO-67bpy (Zr6O4(OH)4(bpydc)6 with bpydc2- = 2,2'-bipyridine-5,5'- dicarboxylate) by solvent impregnation. The MOF retained its long-range order, and transmission electron microscopy and elemental mapping confirmed the retention of the crystal morphology and revealed a homogeneous distribution of the hydride within the MOF host. Notably, the B-, N-, and Mg-edge XAS data confirm the coordination of Mg(II) to the N atoms of the chelating bipyridine groups. In situ 11B MAS NMR studies helped elucidate the reaction mechanism and revealed that complete hydrogen release from Mg(BH4)2 occurs as low as 200 °C. Sieverts and thermogravimetric measurements indicate an increase in the rate of hydrogen release, with the onset of hydrogen desorption as low as 120 °C, which is approximately 150 °C lower than that of the bulk material. Furthermore, density functional theory calculations support the improved dehydrogenation properties and confirm the drastically lower activation energy for B-H bond dissociation.

Nanoconfinement, Metal Hydrides, Metal-Organic Fra↗