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DOE OSTI2023

3D Visualization of Proteins within Metal–Organic Frameworks via Ferritin‐Enabled Electron Microscopy

Abstract Electron tomography holds great promise as a tool for investigating the 3D morphologies and internal structures of metal‐organic framework‐based protein biocomposites (protein@MOFs). Understanding the 3D spatial arrangement of proteins within protein@MOFs is paramount for developing synthetic methods to control their spatial localization and distribution patterns within the biocomposite crystals. In this study, the naturally occurring iron oxide mineral core of the protein horse spleen ferritin (Fn) is leveraged as a contrast agent to directly observe individual proteins once encapsulated into MOFs by electron microscopy techniques. This methodology couples scanning electron microscopy, transmission electron microscopy, and electron tomography to garner detailed 2D and 3D structural interpretations of where proteins spatially lie in Fn@MOF crystals, addressing the significant gaps in understanding how synthetic conditions relate to overall protein spatial localization and aggregation. These findings collectively reveal that adjusting the ligand‐to‐metal ratios, protein concentration, and the use of denaturing agents alters how proteins are arranged, localized, and aggregated within MOF crystals.

Chemistry↗

NASA NTRS2013

Crack Detection with Lamb Wave Wavenumber Analysis

In this work, we present our study of Lamb wave crack detection using wavenumber analysis. The aim is to demonstrate the application of wavenumber analysis to 3D Lamb wave data to enable damage detection. The 3D wavefields (including vx, vy and vz components) in time-space domain contain a wealth of information regarding the propagating waves in a damaged plate. For crack detection, three wavenumber analysis techniques are used: (i) two dimensional Fourier transform (2D-FT) which can transform the time-space wavefield into frequency-wavenumber representation while losing the spatial information; (ii) short space 2D-FT which can obtain the frequency-wavenumber spectra at various spatial locations, resulting in a space-frequency-wavenumber representation; (iii) local wavenumber analysis which can provide the distribution of the effective wavenumbers at different locations. All of these concepts are demonstrated through a numerical simulation example of an aluminum plate with a crack. The 3D elastodynamic finite integration technique (EFIT) was used to obtain the 3D wavefields, of which the vz (out-of-plane) wave component is compared with the experimental measurement obtained from a scanning laser Doppler vibrometer (SLDV) for verification purposes. The experimental and simulated results are found to be in close agreement. The application of wavenumber analysis on 3D EFIT simulation data shows the effectiveness of the analysis for crack detection. Keywords: : Lamb wave, crack detection, wavenumber analysis, EFIT modeling

Tian, Zhenhua↗

NASA NTRS2021

Residual Stresses Induced due to Curing of the Bulk Matrix in a Simplified Three-Dimensional (3D) Woven Repeating Unit Cell

It has been observed that 3D woven materials are highly susceptible to processes induced defects including tow misalignment, intratow and intertow cracking and/or voids. Adequate process modeling of 3D woven Polymer Matrix Composites (PMCs) is necessary to predict and estimate the effects of the manufacturing process on these defects. A preliminary step towards this is achieved with the commercial Finite Element Analysis (FEA) tool Abaqus complemented with written user subroutines to account for the effect of shrinkage and thermoelastic properties evolution as a function of the degree of cure of the bulk matrix phase in a 3D woven composite repeating unit cell (RUC). As a pathfinder, the process modeling framework is demonstrated on a simplified 3D woven RUC of an AS4/RIMR 135 system. Curing simulations are performed on the 3D woven RUC to observe the processing induced residual stresses. The results of the analysis show that high stress concentrations, present within the 3D intertow matrix bordering the binder tow, coincide with X-Ray computed tomography (X-Ray-CT) scan data depicting cracking in the same location

3D Woven↗

DOE OSTI2020

Influence of plasticizers on thermal and mechanical properties of biocomposite filaments made from lignin and polylactic acid for 3D printing

Polylactic acid (PLA) and organosolv lignin were mixed at different ratios and extruded to obtain PLA-lignin composite filaments. PLA was replaced with lignin up to 20 wt%. Two plasticizers (polyethylene glycol (PEG) 2000 and struktol TR451) were added in varying concentrations to enhance the properties of PLA_L20 (20% lignin in PLA) composite filaments. Furthermore, the effect of lignin in PLA, and PEG, and struktol in PLA_L20 composites was investigated via tensile test, differential scanning calorimetry, thermogravimetric analysis, scanning electron microscopy, Fourier transform infrared spectroscopy of the filaments, and dynamic mechanical analysis of 3D printed samples. A 2 wt% PEG was able to enhance both tensile stress and elongation at maximum load of PLA_L20 composite by 19% and 35%, respectively, whereas struktol TR451 was able to improve elongation at maximum load by 24%.

3D printing↗

DOE OSTI2023

Temporally Stable Supramolecular Polymeric Salts Enabling High-Performance 3D All-Aromatic Polyimide Lattices

Vat photopolymerization (VP) Additive Manufacturing (AM), in which UV light is selectively applied to cure photo-active polymers into complex geometries with micron-scale resolution, has a limited selection of aliphatic thermoset materials that exhibit relatively poor thermal performance. Ring-opening dianhydrides with acrylate-containing nucleophiles yielded diacrylate ester-dicarboxylic acids that enabled photo-active polyimide (PI) precursors, termed polysalts, upon neutralization with an aromatic diamine in solution. In situ FTIR spectroscopy coupled with a solution and photo-rheological measurements revealed a previously unknown time-dependent instability of 4,4'-oxydianiline (ODA) polysalts due to an aza-Michael addition. Replacement of the electron-donating ether-containing diamine with an electron withdrawing sulfone-containing monomer, e.g., 4,4'-diaminodiphenyl sulfone (DDS), prohibited the aza-Michael addition of the aromatic amine to the activated acrylate double bond. Novel DDS polysalt photocurable solutions are similarly analyzed and validated long-term stability, which enabled reproducible printing of polyimide organogel intermediates. Subsequent VP AM afforded 3-dimensional (3D) structures of intricate complexity and excellent surface finish, as demonstrated with scanning electron microscopy. In addition, the novel PMDA-HEA/DDS solution enabled the production of the first beam latticed architecture comprised of all-aromatic polyimide. Finally, the versatility of a polysalt platform for multi-material printing is further demonstrated by printing parts with alternating polysalt compositions.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Exploration of Sn 70 Li 30 alloy as possible material for flowing liquid metal plasma facing components

As an advanced alternative to solid materials, Liquid Metals (LM) may offer more resilient and feasible Plasma Facing Components (PFCs). Particularly, regarding the unavoidable material erosion/degradation produced by particle/heat fluxes in future fusion devices where much longer duty cycles are expected. Furthermore, configurations that propose a flowing LM surface can add the advantage of a continuously fresh and clean layer facing the plasma. Although lithium is the most widely tested option, tin-lithium (SnLi) alloys have been proposed to attempt to combine the positive characteristics of both pure elements and ameliorate the specific issues of lithium. In this work, the potential use of Sn70Li30 alloy in such flowing concepts has been explored by addressing several preliminary and mandatory aspects for its utilization. Key issues such as wettability and compatibility of the alloy with relevant substrates have been studied in a multidisciplinary approach. The data obtained from deposited liquid tin-lithium droplets indicates approximate wetting temperatures of 360 °C, 390 °C and 405 °C for the fresh alloy on 316 stainless steel, molybdenum, and tungsten, respectively. However, the alloy contamination appeared to strongly affect the wetting characteristics of materials, increasing their wetting temperature by ~130 °C in the worst observed cases. Interestingly, in some instances, the instability of the liquid alloy surface was observed in the form of sudden gaseous ejection. The deposited droplets were posteriorly characterized in terms of absolute composition and depth profile by Inductively Coupled PlasmaOptical Emission Spectroscopy (ICP-OES) and Secondary Ion Mass Spectrometry (SIMS-ToF). Additionally, the nature and composition of the boundaries between the substrates and alloy microparticles was investigated by Scanning Electron Microscopy (SEM), Energy Dispersive X-Ray Spectroscopy (EDS), and 3D Laser microscopy. The overall results of this post-mortem characterization revealed that first signs of corrosion induced by both alloy elements (lithium-chromium association and iron-tin intermetallic mixing) were present on 316 stainless steel after short exposures (≤3 h) at temperatures lower than 550 °C. Conversely, molybdenum and tungsten showed good compatibility with the alloy in equivalent conditions. The global implications of these results are finally addressed, focusing on the future perspectives and the more viable scenarios for the eventual utilization of these alloys in flowing liquid metal configurations.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2020

RockFlow: Fast Generation of Synthetic Source Rock Images Using Generative Flow Models

Image-based evaluation methods are a valuable tool for source rock characterization. The time and resources needed to obtain images has spurred development of machine-learning generative models to create synthetic images of pore structure and rock fabric from limited image data. While generative models have shown success, existing methods for generating 3D volumes from 2D training images are restricted to binary images and grayscale volume generation requires 3D training data. Shale characterization relies on 2D imaging techniques such as scanning electron microscopy (SEM), and grayscale values carry important information about porosity, kerogen content, and mineral composition of the shale. Here, we introduce RockFlow, a method based on generative flow models that creates grayscale volumes from 2D training data. We apply RockFlow to baseline binary micro-CT image volumes and compare performance to a previously proposed model. We also show the extension of our model to 2D grayscale data by generating grayscale image volumes from 2D SEM and dual modality nanoscale shale images. The results show that our method underestimates the porosity and surface area on the binary baseline datasets but is able to generate realistic grayscale image volumes for shales. With improved binary data preprocessing, we believe that our model is capable of generating synthetic porous media volumes for a very broad class of rocks from shale to carbonates to sandstone.

58 GEOSCIENCES↗

NASA NTRS1999

Hurricane Directional Wave Spectrum Spatial Variation in the Open Ocean

The sea surface directional wave spectrum was measured for the first time in all quadrants of a hurricane in open water using the NASA airborne scanning radar altimeter (SRA) carried aboard one of the NOAA WP-3D hurricane hunter aircraft at 1.5 km height. The SRA measures the energetic portion of the directional wave spectrum by generating a topographic map of the sea surface. At 8 Hz, the SRA sweeps a radar beam of 1 deg half-power width (two-way) across the aircraft ground track over a swath equal to 0. 8 of the aircraft height, simultaneously measuring the backscattered power at its 36 GHz (8.3 mm) operating frequency and the range to the sea surface at 64 positions. These slant ranges are multiplied by the cosine of the incidence angles to determine the vertical distances from the aircraft to the sea surface. Subtracting these distances from the aircraft height produces the sea surface elevation map. The sea surface topography is interpolated to a uniform grid, transformed by a two-dimensional FFT, and Doppler corrected. The data presented were acquired on 24 August 1998 when hurricane Bonnie was east of the Bahamas and moving slowly to the north. Wave heights up to 18 m were observed and the spatial variation of the wave field was dramatic. The dominant waves generally propagated at significant angles to the downwind direction and at times there were wave fields traveling at right angles to each other. The NOAA aircraft spent over five hours within 180 km of the hurricane Bonnie eye, and made five eye penetrations. A 2-minute animation of the directional wave spectrum spatial variation over this period will be shown.

Wright, C. W.↗

NASA NTRS1999

Hurricane Directional Wave Spectrum Spatial Variation at Landfall

On 26 August 1998, hurricane Bonnie was making landfall near Wilmington, NC. The NASA airborne scanning radar altimeter (SRA) carried aboard one of the NOAA WP-3D hurricane hunter aircraft at 2.2 km height documented the sea surface directional wave spectrum in the region between Charleston, SC and Cape Hatteras, NC. The aircraft ground track included both segments along the shoreline and Pamlico Sound as well as far offshore. An animation of the directional wave spectrum spatial variation at landfall will be presented and contrasted with the spatial variation when Bonnie was in the open ocean on 24 August 1998.

Walsh, E. J.↗

NASA NTRS2000

Hurricane Directional Wave Spectrum Spatial Variation in the Open Ocean and at Landfall

The sea surface directional wave spectrum was measured for the first time in all quadrants of a hurricane in open water using the NASA airborne scanning radar altimeter (SRA) carried aboard one of the NOAA WP-3D hurricane hunter aircraft at 1.5 km height. The SRA measures the energetic portion of the directional wave spectrum by generating a topographic map of the sea surface. At 8 Hz, the SRA sweeps a radar beam of 1' half-power width (two-way) across the aircraft ground track over a swath equal to 0.8 of the aircraft height, simultaneously measuring the backscattered power at its 36 GHz (8.3 mm) operating frequency and the range to the sea surface at 64 positions. These slant ranges are multiplied by the cosine of the off-nadir angles to determine the vertical distances from the aircraft to the sea surface. Subtracting these distances from the aircraft height produces the sea surface elevation map. The sea surface topography is interpolated to a uniform grid, transformed by a two dimensional FFT, and Doppler corrected. The open-ocean data were acquired on 24 August 1998 when hurricane Bonnie was east of the Bahamas and moving toward 330 deg at about 5 m/s. Individual waves up to 18 m height were observed and the spatial variation of the wave field was dramatic. The dominant waves generally propagated at significant angles to the downwind direction. At some positions there were three different wave fields of comparable energy crossing each other. The NOAA aircraft spent over five hours within 180 km of the eye, and made five eye penetrations. On 26 August 1998, the NOAA aircraft flew at 2.2 km height when hurricane Bonnie was making landfall near Wilmington, NC, documenting the directional wave spectrum in the region between Charleston, SC and Cape Hatteras, NC. The aircraft flight lines included segments near and along the shoreline as well as far offshore. Animations of the directional wave spectrum spatial variation along the aircraft tracks on the two flights will be presented using a 100: 1 time compression.

Walsh, Edward J.↗

NASA NTRS2000

Hurricane Directional Wave Spectrum Spatial Variation at Landfall

Walsh, Edward J.↗

NASA NTRS2000

Hurricane Directional Wave Spectrum Spatial Variation in the Open Ocean and at Landfall

The sea surface directional wave spectrum was measured for the first time in all quadrants of a hurricane in open water using the NASA airborne scanning radar altimeter (SRA) carried aboard one of the NOAA WP-3D hurricane hunter aircraft at 1.5 km height. The SRA measures the energetic portion of the directional wave spectrum by generating a topographic map of the sea surface. At 8 Hz, the SRA sweeps a radar beam of 1 E half-power width (two-way) across the aircraft ground track over a swath equal to 0.8 of the aircraft height, simultaneously measuring the backscattered power at its 36 GHz (8.3 mm) operating frequency and the range to the sea surface at 64 positions. These slant ranges are multiplied by the cosine of the incidence angles to determine the vertical distances from the aircraft to the sea surface. Subtracting these distances from the aircraft height produces the sea surface elevation map. The sea surface topography is interpolated to a uniform grid, transformed by a two-dimensional FFT, and Doppler corrected. The open-ocean data were acquired on 24 August 1998 when hurricane Bonnie was east of the Bahamas and moving slowly to the north. Individual waves with heights up to 18 m were observed and the spatial variation of the wave field was dramatic. The dominant waves generally propagated at significant angles to the downwind direction. At some positions there were three different wave fields of comparable energy crossing each other. The NOAA aircraft spent over five hours within 180 km of the hurricane Bonnie eye, and made five eye penetrations. A 3-minute animation of the directional wave spectrum spatial variation over this period will be shown as well as summary plots of the wave field spatial variation. On 26 August 1998, the NOAA aircraft flew at 2.2 km height when hurricane Bonnie was making landfall near Wilmington, NC, documenting the directional wave spectrum in the region between Charleston, SC and Cape Hatteras, NC. The aircraft ground track included both segments along the shoreline and Pamlico Sound as well as far offshore. An animation of the directional wave spectrum spatial variation at landfall will be presented and contrasted with the spatial variation when Bonnie was in the open ocean on 24 August 1998.

Walsh, E. J.↗

NASA NTRS2001

Hurricane Directional Wave Spectrum Spatial Variation in the Open Ocean and at Landfall

The sea surface directional wave spectrum was measured for the first time in all quadrants of a hurricane in open water using the NASA scanning radar altimeter (SRA) carried aboard one of the NOAA WP-3D hurricane research aircraft at 1.5 kilometer height. The SRA measures the energetic portion of the directional wave spectrum by generating a topographic map of the sea surface. The data were acquired on 24 August 1998 when Hurricane Bonnie was 400 km east of Abaco Island, Bahamas. Individual waves with heights up to 19 meters were observed and the spatial variation of the wave field was dramatic. The dominant waves generally propagated at significant angles to the downwind direction. At one position, three different wave systems of comparable energy and wavelength crossed each other. The aircraft spent over five hours within 180 kilometers of the Hurricane Bonnie eye and made five eye penetrations. On 26 August 1998, the SRA at 2.2 kilometer height documented the directional wave spectrum in the region between Charleston, SC, and Cape Hatteras, NC, as Hurricane Bonnie was making landfall near Wilmington, NC. The storm was similar in size during the two flights, but the maximum speed in the NOAA Hurricane Research Division surface wind analysis was 15% lower prior to landfall (39 meters per second) than it had been in the open ocean (46 meters per second). This was compensated for by its faster movement prior to landfall (9.5 meters per second) than when it was encountered in the open ocean (5 meters per second), significantly increasing the effective fetch and duration of waves near the peak of the spectrum which propagated in the direction of the storm track. The open ocean wave height variation indicated that Hurricane Bonnie would have produced waves of 11 meters significant wave height on the shore northeast of Wilmington had it not been for the continental shelf. The bathymetry distributed the steepening and breaking process across the shelf so that the wavelength and wave height were reduced gradually as the shore was approached. The wave height 5 kilometers from shore was about 4 meters.

Walsh, E. J.↗

NASA NTRS2016

Primitive Liquid Water of the Solar System in an Aqueous Altered Carbonaceous Chondrite

Non-destructive 3D observations of the aqueous altered CM chondrite Sutter's Mill using scanning imaging x-ray microscopy (SIXM) showed that some of calcite and enstatite grains contain two-phase inclusion, which is most probably composed of liquid water and bubbles. This water should be primitive water responsible for aqueous alteration in an asteroid in the early solar system.

Tsuchiyama, A.↗

DOE OSTI2024

Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light Source

Geological samples are inherently multi-scale. Understanding their bulk physical and chemical properties requires characterization down to the nano-scale. A powerful technique to study the three-dimensional microstructure is X-ray tomography, but it lacks information about the chemistry of samples. To develop a methodology for measuring the multi-scale 3D microstructure of geological samples, correlative X-ray micro- and nanotomography were performed on two rocks followed by scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS) analysis. The study was performed in five steps: (i) micro X-ray tomography was performed on rock sample cores, (ii) samples for nanotomography were prepared using laser milling, (iii) nanotomography was performed on the milled sub-samples, (iv) samples were mounted and polished for SEM analysis and (v) SEM imaging and compositional mapping was performed on micro and nanotomography samples for complimentary information. Correlative study performed on samples of serpentine and basalt revealed multiscale 3D structures involving both solid mineral phases and pore networks. Significant differences in the volume fraction of pores and mineral phases were also observed dependent on the imaging spatial resolution employed. This highlights the necessity for the application of such a multiscale approach for the characterization of complex aggregates such as rocks. Information acquired from the chemical mapping of different phases was also helpful in segmentation of phases that did not exhibit significant contrast in X-ray imaging. Adoption of the protocol used in this study can be broadly applied to 3D imaging studies being performed at the Advanced Light Source and other user facilities.

58 GEOSCIENCES↗

DOE OSTI2025

Shining light on nanoscale ‘vine-on-stick’ eutectic structures in the Al-Ce-Ni system

Multiphase eutectics often comprise entangled solid phases with nanoscale periodicity, making it difficult to unravel their 3D connectivity using conventional 2D techniques. Among such systems, the three-phase eutectic Al-Al 11 Ce 3 -Al 3 Ni stands out for its ultrafine (∼100 nm) interphase spacing and promising creep resistance, yet its microstructure remains relatively unexplored despite its potential for high-temperature applications. Here, we use scanning hard X-ray microscopy with an unprecedented ∼10 nm pixel size to resolve its 3D morphology. Reconstructions reveal a novel “vine-on-stick” motif, wherein Al 11 Ce 3 wraps around Al 3 Ni pillars. Analysis of phase tortuosities confirms that Al 11 Ce 3 exhibits more convoluted morphologies than Al 3 Ni. No orientation relationship was observed between the two intermetallics, suggesting that growth is controlled by local solute gradients rather than epitaxy. Fragmentation of intermetallics along their longitudinal axis suggests a Rayleigh-type breakup mechanism in solid state. The “vine-on-stick” pattern may generalize to other alloy systems with variable interfacial anisotropies and low mutual solubilities.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Validation of an integrated modeling framework for investigating 3D plasma responses in tokamak plasmas

As contemporary experimental tokamaks are pushed toward reactor-relevant operation, they provide essential testbeds for demonstrating and exploring ELM control strategies for deployment in future fusion pilot plants. Accurate predictions of full plasma responses are essential to guide and optimize these demonstrations. This paper introduces and validates an integrated modeling framework over a historical range of DIII-D operational space. The integrated modeling framework uses only scalar plasma parameters and optional reference boundary to self-consistently and flexibly scan through tokamak operational space and estimate the corresponding ELM-suppression relevant plasma response over 3D coil phase space. The framework generates tightly converged equilibria that satisfy a target set of plasma parameters (I p , β N , l i ), with kinetic profiles constrained by an EPED(NN)-computed pedestal and empirical core model. The plasma response of these modeled equilibria is calculated with GPEC. Validated against 55 distinct DIII-D equilibria, the framework consistently reproduces experimentally constrained equilibrium pressure, q, and other representative profiles using the time-varying information from only evolving scalar plasma parameters; plasma response validation is performed for the n=3 perturbation. In particular, the plasma response of a DIII-D discharge scanning q 95 in search of ELM suppression windows is quantitatively reproduced. By accurately reproducing experimental equilibria and plasma responses across wide parameter variation, the framework supports potential for synthetic parameter scans in key operational, stability, and plasma response dimensions to investigate RMP ELM-suppression experiments and inform predictive RMP scenario optimization.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2025

Scaling deep learning for material imaging with a pseudo 3D model for domain transfer

The recent introduction of deep learning methods for image processing has greatly advanced the characterization of materials using three-dimensional (3D) X-ray imaging techniques. However, deep learning models often have difficulty performing consistently across images owing to unavoidable variations in imaging conditions, which create inconsistencies even for the same material. As a result, networks must frequently be retrained for new datasets, limiting their applicability and generalization. Thus, it is critical to reduce the variations between images to enable a single model to process multiple datasets. Herein, we introduce P3T-Net, a pseudo-3D domain transfer network that transfers diverse 3D images into a uniform domain before processing using deep learning models. Remarkably, P3T-Net enables the reuse of previously trained networks for processing new images and considerably reduces the computational cost of transferring 3D images across domains. These unique capabilities were demonstrated in the following scenarios: (i) image enhancement of fast scans for geological rock and hydrogen fuel cells, (ii) enhancement of images to match the quality of multi-source imaging for lithium-ion batteries, (iii) accurate segmentation of images captured under different conditions, and (iv) tera-scale 3D transfer (10 11 voxels) on a single GPU. Overall, the proposed approach addresses cross-domain inconsistencies across various materials and conditions, thereby enabling more robust and generalizable deep learning solutions for a wide range of material imaging tasks.

25 ENERGY STORAGE↗