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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 253 records · Page 14

Pore Structures in Detritusphere of Soils Under Switchgrass and Restored Prairie Vegetation Community

Root detritusphere, that is, the soil in the vicinity of decomposing root residues, plays an important role in soil microbial activity and C sequestration. Pore structure (size distributions and connectivity of soil pores) in the detritusphere serves as a major driver for these processes and, in turn, is influenced by the physical characteristics of both soil and roots. This study compared pore structure characteristics in the root detritusphere of soils of contrasting texture and mineralogy subjected to > 6 years of contrasting vegetation: monoculture switchgrass and polyculture prairie systems. Soil samples were collected from five experimental sites in the US Midwest representing three soil types. Soil texture and mineralogy were measured using a hydrometer and x-ray powder diffraction, respectively. The intact cores were scanned with x-ray computed micro-tomography to identify visible soil pores, biopores, and particulate organic matter (POM). We specifically focused on pore structure within the detritusphere around the POM of root origin. Results showed that the detritusphere of coarser textured soils, characterized by high sand and quartz contents, had lower porosity in the vicinity of POM compared with finer textured soils. POM vicinities in finer textured soils had high proportions of large (> 300 μm diameter) pores, and their pores were better connected than in the coarser soils. Lower porosity in the outer (> 1 mm) parts of the detritusphere of switchgrass than of prairie suggested soil compaction by roots, with the effect especially pronounced in the coarser soils. Here, the results demonstrated that soil texture and mineralogy played a major, while vegetation played a more modest, role in defining the pore structure in the root detritusphere.

54 ENVIRONMENTAL SCIENCES↗

Tailoring a 3D Covalent Organic Framework Toward Facile Functionalization

Three-dimensional covalent organic frameworks (3D COFs) are notably crystalline and stable, but their architectures and monomer structures make them difficult to functionalize. Here, a new strategy is presented to render COF-300 and other imine-linked frameworks amenable to facile functionalization in the last step of synthesis. By reducing the imine linkages to secondary amines and appending them with acetyl halide groups, the linkages are converted to electrophiles that can be readily reacted with nucleophilic guests. This route yields eight new COF-300 derivatives, bearing chloroacetyl, bromoacetyl, azide, cyano, amino, hydroxyl, methoxy, or thiomethyl groups appended to the inter-monomer linkages. The new materials are characterized through solid-state NMR, infrared spectroscopy, and powder X-ray diffraction, among other techniques, finding that the reported linkage transformations proceed to complete conversion while retaining the crystallinity of the materials. Microcrystal electron diffraction (microED) data are used to solve the evacuated structure of the amine-linked framework COF-300-AR for the first time, providing conclusive evidence of this framework's guest-induced phase change, along with the structure of the new framework COF-300-NH 2 . Finally, COF-300-NH 2 is shown to have significantly improved adsorption capacity for CO 2 and perfluoroalkyl substances (PFAS), highlighting the benefits of this synthetic strategy for the generation of customized adsorbents.

COF-300↗

Beyond the Surface: Non-Invasive Low-Field NMR Analysis of Microbially-Induced Calcium Carbonate Precipitation in Shale Fractures

Microbially-induced calcium carbonate precipitation (MICP) is a biological process in which microbially-produced urease enzymes convert urea and calcium into solid calcium carbonate (CaCO 3 ) deposits. MICP has been demonstrated to reduce permeability in shale fractures under elevated pressures, raising the possibility of applying this technology to enhance shale reservoir storage safety. For this and other applications to become a reality, non-invasive tools are needed to determine how effectively MICP seals shale fractures at subsurface temperatures. In this study, two different MICP strategies were tested on 2.54 cm diameter and 5.08 cm long shale cores with a single fracture at 60 °C. Flow-through, pulsed-flow MICP-treatment was repeatedly applied to Marcellus shale fractures with and without sand (“proppant”) until reaching approximately four orders of magnitude reduction in apparent permeability, while a single application of polymer-based “immersion” MICP-treatment was applied to an Eagle Ford shale fracture with proppant. Low-field nuclear magnetic resonance (LF-NMR) and X-Ray computed microtomography (micro-CT) techniques were used to assess the degree of biomineralization. With the flow-through approach, these tools revealed that while CaCO 3 precipitation occurred throughout the fracture, there was preferential precipitation around proppant. Without proppant, the same approach led to premature sealing at the inlet side of the core. In contrast, immersion MICP-treatment sealed off the fracture edges and showed less mineral precipitation overall. This study highlights the use of LF-NMR relaxometry in characterizing fracture sealing and can help guide NMR logging tools in subsurface remediation efforts.

MICP↗

Oxygen Effects and Selective Oxidation of Group IV Alloying Additions in Group V-Based Refractory Multi-principal Element Alloys

Refractory multi-principal element alloys (RMPEAs) hold significant potential for advancing ultra-high-temperature technologies due to their remarkable strength retention under these conditions. However, the beneficial effects of alloying on microstructural evolution and mechanical properties are often obscured by the presence of interstitial alloying elements. The intricate interactions between substitutional alloying elements of Groups IV, V, and VI and interstitial content, whether intentional or incidental, remain poorly understood. In this study, we investigate the impact of dissolved oxygen on the microstructural evolution and stability of RMPEAs primarily composed of Group V elements, Nb and V, along with Group IV elements Ti, Zr, and Hf. We show that the strong affinity of oxygen for Group IV elements Zr and Hf leads to the internal precipitation of oxides during heat treatment, which competes with the homogenization of the as-cast dendritic microstructure. Here, we demonstrate that careful control and design of oxygen content and Group IV alloying additions are essential to minimize micro-segregation and prevent the detrimental precipitation of internal oxides. To address these challenges, we propose employing non-equilibrium solidification calculations to predict and optimize as-cast solidification structures, thereby reducing the reliance on homogenization processes.

Alloy design↗

Micromechanical and fatigue in situ synchrotron characterization of an additively manufactured superalloy with porosity

Additive manufacturing (AM) has the potential to transform component production, but its widespread adoption is constrained by defects, such as pores, that compromise structural integrity. Here, this study investigates the influence of porosity on the micromechanical and fatigue response of AM Inconel 718 (IN718), a widely used aerospace superalloy. One baseline specimen with minimal stochastic porosity and another intentionally seeded with lack of fusion (LOF) pores were examined using high-energy X-ray diffraction microscopy (HEDM) and micro-computed tomography during cyclic loading. Fatigue cracks in the LOF specimen initiated more frequently and at lower cycle counts than in the baseline specimen. The number fraction of fatigue cracks that grew was comparatively higher in the LOF specimen. Grain-level metrics, including stress and diffraction spot widths, were quantified using far-field HEDM. Across the thousands of grains detected in both specimens, the pores in the LOF specimen increased the variability of stress and spot width evolution in the azimuthal direction, the latter serving as a surrogate measure of plastic deformation. However, no correlations emerged between these metrics and grain proximity to fatigue crack initiation sites or pores, underscoring the limitations of grain-averaged metrics for predicting fatigue. Nonetheless, the rich dataset reported here provides a foundation for future modeling efforts.

High-energy X-ray diffraction microscopy↗

Discovery of nanopore filling by gypsum in wellbore cement exposed to 17 MPa CO 2 under geologic carbon storage conditions

Here, this study investigates the pore structure evolution of the reaction zones in wellbore cement samples exposed to a CO 2 -rich solution in equilibrium with 17 MPa supercritical CO 2 over 14 days. Through advanced characterization methods of field emission SEM, Quantitative Evaluation of Minerals by Scanning Electron Microscopy (QEMSCAN), and micro-CT, a new mechanism of CO 2 -cement reaction involving filling of nanopores in the interior of cement by gypsum was revealed. Gypsum was formed by the liberation of SO 4 2− from ettringite (AFt) and monosulfate (AFm) caused by a decrease in pH. Based on these experimental observations, a new CO 2 -cement reaction model that incorporates four distinct reaction zones is developed. This model provides a comprehensive framework for understanding the spatial and temporal distribution of minerals in cement due to high pressure CO 2 —cement reactions. This study demonstrates that the major damage induced by high pressure CO 2 alteration occurs in the most exterior region of the cement. The interior region of the cement maintains its integrity due to nanopore filling by gypsum.

54 ENVIRONMENTAL SCIENCES↗

Mapping the Microhardness of Al Matrix in U-7Mo/Al Dispersion Fuels at Medium and High Burn-up by in situ Nanoindentation

The mechanical degradation of the Al matrix in U-7Mo dispersion fuels was detected after irradiation in previous studies, but more details of the degradation mechanism are not clear yet to clarify the root cause. In this study, microhardness mapping in fresh and irradiated U-7Mo dispersion fuels coated with ZrN, with burn-up of 3.35 × 10 21 and 6.28 × 10 21 f/cm 3 , are measured to reveal the hardening of the Al matrix as a function of distance to fuel particles. Micro cubes were pulled by plasma focused ion beam scanning electron microscopy and tested by in situ nanoindenter with Berkovitch tip. Size effects are measured in medium and high burn-up samples. The higher burn-up specimen exhibits a more pronounced size effect when indent load is lower than 20 mN. Size effect correction models are also calculated by plots fitting, which predicts the true microhardness without size effect. Results shows that the hardness of the Al matrix near the ZrN coating has the highest value, then decreases moving away from the coating and become stable when the distance reaches ∼10 µm. The hardness starts increasing again getting closer to the next fuel particle, which makes the hardness distribution between two fuel particles to be “U” shape.

36 - MATERIALS SCIENCE↗

Soil pore characteristics and the fate of new switchgrass-derived carbon in switchgrass and prairie bioenergy cropping systems

Abstract Monoculture switchgrass and restored prairie are promising perennial feedstock sources for bioenergy production on the lands unsuitable for conventional agriculture. Such lands often display contrasting topography that influences soil characteristics and interactions between plant growth and soil C gains. This study aimed at elucidating the influences of topography and plant systems on the fate of C originated from switchgrass plants and on its relationships with soil pore characteristics. For that, switchgrass plants were grown in intact soil cores collected from two contrasting topographies, namely steep slopes and topographical depressions, in the fields in multi-year monoculture switchgrass and restored prairie vegetation. The 13 C pulse labeling allowed tracing the C of switchgrass origin, which X-ray computed micro-tomography enabled in-detail characterization of soil pore structure. In eroded slopes, the differences between the monoculture switchgrass and prairie in terms of total and microbial biomass C were greater than those in topographical depressions. While new switchgrass increased the CO 2 emission in depressions, it did not significantly affect the CO 2 emission in slopes. Pores of 18–90 µm Ø facilitated the accumulation of new C in soil, while > 150 µm Ø pores enhanced the mineralization of the new C. These findings suggest that polyculture prairie located in slopes can be particularly beneficial in facilitating soil C accrual and reduce C losses as CO 2 .

09 BIOMASS FUELS↗

Turbulence link to L-mode, I-mode, and H-mode confinement in the DIII-D tokamak

Understanding the physics of low-confinement (L-), improved-confinement (I-), and high-confinement (H-) modes is critical for fusion reactors. The finding herein reports observations of two types of turbulence coexisting near the L-mode edge, one magnetohydrodynamic (MHD)-like and another micro-tearing mode (MTM)-like, linked to the H-mode and I-mode confinement in the DIII-D tokamak. Ion-scale magnetic and density turbulence is measured using a Faraday-effect radial-interferometer-polarimeter and beam-emission-spectroscopy (BES). Broadband turbulence spectra of up to ~600 kHz are observed in two discharges where transitions between L-mode, I-mode, and H-mode occurs. Turbulence is found to be inversely correlated with confinement, meaning lower turbulence power at higher confinement. Distinctively, the high-frequency (HF, >~100 kHz) magnetic turbulence power changes by the most (55%) during transitions primarily involving energy confinement change, whereas the low-frequency (LF, <~100 kHz) magnetic and density turbulence power changes by the most (80%) during transitions primarily involving particle confinement change. The LF turbulence amplitude oscillates with and leads to deuterium-alpha emission oscillations before an H-mode. These results imply that HF turbulence mainly affects energy confinement whereas LF turbulence can affect particle confinement. The magnetic and density turbulence exhibits coherence up to 0.6 and cross-phase magnitude close to π/2 in most cases, suggesting they have a common origin in both the LF and HF ranges. BES suggests that LF turbulence resides at the edge (ρ = 0.95) and HF turbulence can be at the outer core (ρ = 0.8) or edge (ρ = 0.95). Comparisons of measurements, theory, and gyrokinetic simulations suggest that HF turbulence is MTM-like in all cases, whereas LF turbulence is more consistent with MHD-like modes and the exact instability might change during transitions—except that a drift-wave origin is possible in a low collisionality H-mode. These results suggest that the H-mode involves suppressed MHD-like turbulence, whereas the I-mode mitigates MTM-like turbulence along with largely unchanged MHD-like turbulence.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

3D Nanocrystallography and the Imperfect Molecular Lattice

Crystallographic analysis relies on the scattering of quanta from arrays of atoms that populate a repeating lattice. While large crystals built of lattices that appear ideal are sought after by crystallographers, imperfections are the norm for molecular crystals. Additionally, advanced X-ray and electron diffraction techniques, used for crystallography, have opened the possibility of interrogating micro- and nanoscale crystals, with edges only millions or even thousands of molecules long. These crystals exist in a size regime that approximates the lower bounds for traditional models of crystal nonuniformity and imperfection. Accordingly, data generated by diffraction from both X-rays and electrons show increased complexity and are more challenging to conventionally model. New approaches in serial crystallography and spatially resolved electron diffraction mapping are changing this paradigm by better accounting for variability within and between crystals. The intersection of these methods presents an opportunity for a more comprehensive understanding of the structure and properties of nanocrystalline materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Mt. Simon Sandstone - High Resolution CT

High resolution micro-computed tomography images of sandstone from the Mt. Simon formation at different depths. These images provide an insight into the pore structure of the Mt. Simon sandstone (e.g. for potential CO2 storage). This data set can be used to further study the formation as a whole..

CCS,CO2 Sequestration,Carbon Sequestration,Compute↗

Surface-Enhanced Raman Spectroscopy Combined with Multivariate Analysis for Fingerprinting Clinically Similar Fibromyalgia and Long COVID Syndromes

Fibromyalgia (FM) is a chronic central sensitivity syndrome characterized by augmented pain processing at diffuse body sites and presents as a multimorbid clinical condition. Long COVID (LC) is a heterogenous clinical syndrome that affects 10–20% of individuals following COVID-19 infection. FM and LC share similarities with regard to the pain and other clinical symptoms experienced, thereby posing a challenge for accurate diagnosis. This research explores the feasibility of using surface-enhanced Raman spectroscopy (SERS) combined with soft independent modelling of class analogies (SIMCAs) to develop classification models differentiating LC and FM. Venous blood samples were collected using two supports, dried bloodspot cards (DBS, n = 48 FM and n = 46 LC) and volumetric absorptive micro-sampling tips (VAMS, n = 39 FM and n = 39 LC). A semi-permeable membrane (10 kDa) was used to extract low molecular fraction (LMF) from the blood samples, and Raman spectra were acquired using SERS with gold nanoparticles (AuNPs). Soft independent modelling of class analogy (SIMCA) models developed with spectral data of blood samples collected in VAMS tips showed superior performance with a validation performance of 100% accuracy, sensitivity, and specificity, achieving an excellent classification accuracy of 0.86 area under the curve (AUC). Amide groups, aromatic and acidic amino acids were responsible for the discrimination patterns among FM and LC syndromes, emphasizing the findings from our previous studies. Overall, our results demonstrate the ability of AuNP SERS to identify unique metabolites that can be potentially used as spectral biomarkers to differentiate FM and LC.

60 APPLIED LIFE SCIENCES↗

Fracture Behavior Considerations for the TRISO Particle Matrix

To assess whether matrix fracture would result in an unacceptable loss of containment or confinement in TRISO fuel particles, it is crucial to evaluate the micro-tensile strength, fracture toughness, and irradiation effects on matrix materials. Current data must be comprehensive and validated for modeling fractures under various conditions. Relevant material properties surrounding matrix fracture will be discussed during the presentation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Femto-second Laser’s Enabling New Length Scale Fabrications for Rapid Post Irradiation Examination of Materials: Concluding LDRD Project Poster

Mechanical testing campaigns are required to qualify materials for advanced reactor conditions, yet economical and safety limitations restrict the number of standardized mechanical tests that can be performed. Reducing the size of the sample is one approach to addressing these challenges and to accelerating testing. Previous research has shown that smaller mechanical test samples produce higher yield and ultimate stress values compared to values measured from standard sample sizes: the “smaller is stronger” effect. Specimens used in accelerated material testing campaigns must reflect bulk material performance to enable engineering scale material property measurement. The objective of this research project was to determine if engineering scale mechanical behavior—the yield stress—could be measured with micro-tensile test samples smaller than traditional standard testing geometries. The relationship between yield stress and sample size was explored with two different nuclear-relevant structural materials: Zircaloy-4 and tungsten. Mechanical testing of both metals demonstrated decreasing yield stress values with increasing sample gauge size across three different sizes. Yield stress values from the largest gauge size, fabricated with a femto-second laser ablation system, approach bulk material yield stress values reported in published literature. Preliminary analysis of the tungsten samples indicates the yield stress value depends on the grain characteristics within the gauge section, in addition to the gauge size. Accompanying modeling efforts, including response surface generation and crystal plasticity approaches, further demonstrated that the size of the sample gauge section alone cannot explain the change in yield stress values.

36 MATERIALS SCIENCE↗

Microtensile Specimen Analysis

No abstract, presentation is a review on AGR micro tensile specimen analysis for FY 2024.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Scalable Nanoimprint Manufacturing of Functional Multilayer Metasurface Devices

Optical metasurfaces, consisting of subwavelength-scale meta-atom arrays, hold great promise of overcoming the fundamental limitations of conventional optics. Due to their structural complexity, metasurfaces usually require high-resolution yet slow and expensive fabrication processes. Here, using a metasurface polarimetric imaging device as an example, the photonic structures and the Nanoimprint lithography (NIL) processes are designed, creating two separate NIL molds over a patterning area of > 20 mm2 with designed Moiré alignment markers by electron-beam writing, and further subsequently integrate silicon and aluminum metasurface structures on a chip. Uniquely, the silicon and aluminum metasurfaces are fabricated by using the nanolithography and 3D pattern-transfer capabilities of NIL, respectively, achieving nanometer-scale linewidth uniformity, sub-200 nm translational overlay accuracy, and <0.017 rotational alignment error while significantly reducing fabrication complexity and surface roughness. Here, the micro-sized multilayer metasurfaces have high circular polarization extinction ratios as large as ≈20 and ≈80 in blue and red wavelengths. Further, the metasurface chip-integrated CMOS imager demonstrates high accuracy in broad-band, full Stokes parameter analysis in the visible wavelength ranges and single-shot polarimetric imaging. This novel, NIL-based, multilayered nanomanufacturing approach is applicable to the scalable production of large-area functional structures for ultra-compact optic, electronic, and quantum devices.

36 MATERIALS SCIENCE↗