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DOE OSTI2023

Single and dual metal atom catalysts for enhanced singlet oxygen generation and oxygen reduction reaction

We demonstrate rational design of graphene-supported single and dual metal atom catalysts (SACs and DACs) for photocatalytic applications, such as singlet oxygen ( 1 O 2 ) sensitization and H 2 O 2 production. Here we combine density functional theory (DFT) and time-dependent DFT (TD-DFT) calculations with experimental verifications. We found a synergistic effect between triplet sensitization and triplet–triplet (Dexter) energy transfer; both play a role in the photocatalytic activity through the volcano plot of 3d transition metal SACs. More specifically, FeN 4 -SAC exhibits a low ISC energy gap (ΔE ISC ) of 0.039 eV, compared with 0.108 eV for FeNiN8-DACs, both possessing a high Bader charge transfer of 0.366 e- and 0.405 e-, respectively. Guided by these computational results, we synthesized a series of SACs and a DAC and confirmed their structures with scanning transmission electron microscopy (STEM) along with the X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine structure (EXAFS). We then confirm their band structures with low-energy inverse photoemission spectroscopy (LEIPS) and UV-vis-NIR. Subsequently, we synthesized the catalysts for the photooxygenation of anthracene and two-electron oxygen reduction reaction (ORR) to measure their photocatalytic activity. We found that H 2 O 2 production through the two-electron ORR competes with the 1 O 2 generation through Dexter energy transfer. FeN 4 -SAC demonstrates a high photooxygenation conversion of 86% and a high 1 O 2 quantum yield of 1.04, obtained from electron spin resonance (ESR) spectroscopy, with low H 2 O 2 production. In contrast, NiN 4 -SAC exhibits a low 1 O 2 generation and a high H 2 O 2 production mainly because of the high Gibbs free energy of the OOH* intermediate. In conclusion, this work proposes an effective DFT-guided strategy for designing SACs and DACs for various photocatalytic applications.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Large-volume centimeter-wave cavities for axion searches

The scan rate of an axion haloscope is proportional to the square of the cavity volume. In this paper, a new class of thin-shell cavities are proposed to search for axionic dark matter. These cavities feature active volume much larger (>20×) than that of a conventional cylindrical haloscope, comparable quality factor Q, and a similar frequency tuning range. Furthermore, full 3D numerical finite-element analyses have been used to show that the TM 010 eigenmodes are singly polarized throughout the volume of the cavity and can facilitate axion-photon conversion in uniform magnetic field produced by a superconducting solenoid. To mitigate spurious mode crowding and volume losses due to localization, a pre-amplification binary summing network will be used for coupling. Because of the favorable frequency-scaling, the new cavities are most suitable for centimeter-wavelength (~ 10–100 GHz), corresponding to the promising post-inflation axion production window. In this frequency range, the tight machining tolerances required for high-Q thin-shell cavities are achievable with standard machining techniques for near-infrared mirrors.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2024

3D Reconstruction of a High-Energy Diffraction Microscopy Sample Using Multi-modal Serial Sectioning with High-Precision EBSD and Surface Profilometry

High-energy diffraction microscopy (HEDM) combined with in situ mechanical testing is a powerful nondestructive technique for tracking the evolving microstructure within polycrystalline materials during deformation. This technique relies on a sophisticated analysis of X-ray diffraction patterns to produce a three-dimensional reconstruction of grains and other microstructural features within the interrogated volume. However, it is known that HEDM can fail to identify certain microstructural features, particularly smaller grains or twinned regions. Characterization of the identical sample volume using high-resolution surface-specific techniques, particularly electron backscatter diffraction (EBSD), can not only provide additional microstructure information about the interrogated volume but also highlight opportunities for improvement of the HEDM reconstruction algorithms. In this study, a sample fabricated from undeformed “low solvus, high refractory” nickel-based superalloy was scanned using HEDM. The volume interrogated by HEDM was then carefully characterized using a combination of surface-specific techniques, including epi-illumination optical microscopy, zero-tilt secondary and backscattered electron imaging, scanning white light interferometry, and high-precision EBSD. Custom data fusion protocols were developed to integrate and align the microstructure maps captured by these surface-specific techniques and HEDM. The raw and processed data from HEDM and serial sectioning have been made available via the Materials Data Facility (MDF) at https://doi.org/10.18126/4y0p-v604 for further investigation.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Sputter-Deposited Mo Thin Films: Multimodal Characterization of Structure, Surface Morphology, Density, Residual Stress, Electrical Resistivity, and Mechanical Response

Multimodal datasets of materials are rich sources of information which can be leveraged for expedited discovery of process–structure–property relationships and for designing materials with targeted structures and/or properties. For this data descriptor article, we provide a multimodal dataset of magnetron sputter-deposited molybdenum (Mo) thin films, which are used in a variety of industries including high temperature coatings, photovoltaics, and microelectronics. In this dataset we explored a process space consisting of 27 unique combinations of sputter power and Ar deposition pressure. Here, the phase, structure, surface morphology, and composition of the Mo thin films were characterized by x-ray diffraction, scanning electron microscopy, atomic force microscopy, and Rutherford backscattering spectrometry. Physical properties—namely, thickness, film stress and sheet resistance—were also measured to provide additional film characteristics and behaviors. Additionally, nanoindentation was utilized to obtain mechanical load-displacement data. The entire dataset consists of 2072 measurements including scalar values (e.g., film stress values), 2D linescans (e.g., x-ray diffractograms), and 3D imagery (e.g., atomic force microscopy images). An additional 1889 quantities, including film hardness, modulus, electrical resistivity, density, and surface roughness, were derived from the experimental datasets using traditional methods. Minimal analysis and discussion of the results are provided in this data descriptor article to limit the authors’ preconceived interpretations of the data. Overall, the data modalities are consistent with previous reports of refractory metal thin films, ensuring that a high-quality dataset was generated. The entirety of this data is committed to a public repository in the Materials Data Facility.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Effects of cyclic plasma heating on surface damage of micro-porous tungsten

The operating temperature window of solid tungsten (W) is dictated by its Ductile to Brittle Transition Temperature (DBTT) and re-crystallization temperature; roughly between 300-1300 °C. The brittleness of W at lower temperatures is exasperated when it undergoes recrystallization. We investigate here the thermal shock resistance of micro-porous W as a meta-material fabricated in a 3D open-cell network structure. We present experimental results for the effects of cyclic high-enthalpy arc-jet plasma on surface damage in three testing categories. Observed damage includes surface ablation of asperities, melting and solidification of W-fuzz on samples that have been exposed to a prior helium plasma, and micro-cracks at ligament triple junctions. Scanning electron microscope (SEM) observations show more micro-cracking on 54% and 23% foams compared to the 43% ones. In all tested samples, thermal expansion/contraction displacements were accommodated by ligament rotation and a network of micro-cracks. Furthermore, no large through-thickness crack were observed.

36 MATERIALS SCIENCE↗

NASA NTRS2001

Sources of Variability in the Stratospheric Column of Nitrogen Dioxide

Instruments such as the Global Ozone Monitoring Experiment (GOME, on the European Remote Sensing Satellite (ERS-2), launched 1995), the Scanning Imaging Absorption Spectrometer for Atmospheric Chartography (SCIAMACHY, on ENVISAT, to be launched July 2001) and the Ozone Monitoring Instrument (OMI on EOS Aura, to be launched 2003) make measurements of the total column of NO2. There is interest in separating the stratospheric and tropospheric contributions to the column, as the tropospheric column provides a measure of pollution. We are using a 3D chemistry and transport model driven by winds from the Goddard Space Flight Center Data Assimilation System to examine variability in the stratospheric NO2 column. Model results for NOx = NO + NO2 + 2N2O5 will be shown to compare well with sunset observations from the Halogen Occultation Experiment on the Upper Atmosphere Research Satellite, and to exhibit similar temporal and spatial dependence. Partitioning between NO, NO2, and N2O5 is also shown to compare well with observations. This good agreement supports the use of simulated fields in the stratosphere to derive the tropospheric column from the total column. Preliminary comparisons of the tropospheric column with model simulations for the troposphere will also be shown.

Douglass, Anne↗

NASA NTRS2019

Bounding Methods for Heterogeneous Lidar-derived Navigational Geofences

Safe Unmanned Aerial Vehicle (UAV) operations near the ground require navigation methods that avoid fixed obstacles such as buildings, power lines and trees. Aerial lidar surveys of ground structures are available with the precision and accuracy to geolocate obstacles, but the high volume of raw survey data can exceed the compute power of onboard processors and the rendering ability of ground-based flight planning maps. Representing ground structures with bounding polyhedra instead of point clouds greatly reduces the data size and can enable effective obstacle avoidance, as long as the bounding geometry envelopes the structures with high spatial fidelity. This report describes in detail four methods to compute bounding geometries of ground obstacles from lidar point clouds. The four methods are: 1) 2.5D Maximum Elevation Box, 2) 2.5D Ground Map Extrusion, 3) 3D Bounding Cylinder, and 4) 3D Bounding Box. The methods are applied to five point cloud datasets from lidar surveys of UAV flight research sites in Georgia and Virginia with an average point spacing that ranges from 0.1m to 0.6m. The methods are assessed using survey areas with geometrically heterogeneous ground structures: buildings, vegetation, power lines, and sub-meter structures such as road signs and guy wires. The 2.5D Maximum Elevation Box method is useful for simple structures. The 2.5D Ground Map Extrusion method efficiently encloses vegetation, but requires handdrawn ground footprints. The 3D Bounding Cylinder method excels at enclosing linear structures such as power lines and fences. The 3D Bounding Box method excels at enclosing planar structures such as buildings. The methods are compared on the basis of data compression and boundary fidelity on selected areas. The 2.5D methods yield the highest data compression but the polyhedra produced by them enclose significant amounts of empty space. Boundary fidelity is superior for the 3D methods, though this fidelity comes at the cost of a roughly thirtyfold lower data compression ratio than the 2.5D Maximum Elevation Box method. A mix of these output geometries is proposed for autonomous UAV navigation with limited on-board computing. Both the accuracy and spatial detail of emerging satellite-based survey technology lower than that of aerial lidar scanning survey technology. Sub-meter structures and thin linear structures are not reliably mapped at present by satellite-based surveys.

Moore, Andrew J.↗

DOE OSTI2025

Advanced Interactive 3D Visualization Tool for Customizable Analyses of Tomography Datasets in Material Science

Current methods for visualizing and analyzing 3D tomography datasets in materials science often lack the interactivity and depth required for detailed structural insights. This limitation restricts a researchers' ability to accurately interpret complex data, which is critical for advancing material innovations and understanding structural properties. To address this issue, we have developed a novel, web-based interactive 3D visualization and analysis tool from the Trame framework that offers customizable features to enhance data interpretability. The tool allows users to adjust parameters such as visible range, slice planes, data rotation, and layering, providing a more detailed and dynamic view of complex structures. Its user-friendly web interface increases the accessibility and ease of use for both novice and experienced researchers, to visualize large volumetric datasets. The tool supports a diverse range of data formats, making it versatile for various research applications. Unique capabilities include real-time data manipulation, automated feature detection, context-sensitive feedback, and real-time volume calculations and distributions per sliced region or layer, alongside the ability to quickly generate high-quality screenshots and videos for presentations and reports. These advancements offer a comprehensive solution for enhanced 3D data exploration, significantly improving the analysis process and communication of results in materials science.

36 - MATERIALS SCIENCE↗

DOE OSTI2023

Residual strain orientation in rolled titanium determined with synchrotron X-ray Laue microdiffraction

Previously, synchrotron X-ray Laue microdiffraction has been used to measure the magnitudes of residual strain in materials. Recently the method was advanced to determine the orientation of the strain ellipsoid and applied to naturally deformed quartzites; however, the deformation history of these quartzites is ambiguous due to their natural origin. Here, in this study, synchrotron X-ray Laue microdiffraction (µXRD) is used to measure the residual strain for the first time in a sample with known stress history, rolled titanium. A deviatoric strain tensor is calculated from each Laue diffraction image collected with two µXRD scans of a rolled titanium sheet in different sample orientations. The principal strain axes are calculated using an eigen decomposition of the deviatoric strain tensors. The results show that the principal axis of compression is aligned with the normal direction of the titanium sheet, and the principal axis of extension is aligned with the rolling direction. Pole figures are used to represent the 3D distribution of residual strain axes.

36 MATERIALS SCIENCE↗

NASA NTRS2001

C-Coupon Studies of CMCS: Fracture Behavior and Microstructural Characterization

A curved beam 'C-coupon' was used to assess fracture behavior in a Sylramic(tm)/melt infiltration (MI) SiC matrix composite. Failure stresses and fracture mechanisms, as determined by optical and scanning electron microstructural analysis, are compared with finite element stress calculations to analyze failure modes. Material microstructure was found to have a strong influence on mechanical behavior. Fracture occurs in interlaminar tension (ILT), provided that the ratio of ILT to tensile strength for the material is less than the ratio of radial to hoop stresses for the C-coupon geometry. Utilization of 3D architectures to improve interlaminar strength requires significant development efforts to incorporate through thickness fibers in regions with high curvatures while maintaining uniform thickness, radius, and microstructure.

Hurwitz, Frances I.↗

NASA NTRS2002

Visions of our Planet's Atmosphere, Land & Oceans

The NASA/NOAA Electronic Theater presents Earth science observations and visualizations in a historical perspective. Fly in from outer space to South Africa, Cape Town and Johannesburg using NASA Terra MODIS data, Landsat data and 1m IKONOS "Spy Satellite" data. Zoom in to any place South Africa using Earth Viewer 3D from Keyhole Inc. and Landsat data at 30 m resolution. Go back to the early weather satellite images from the 1960s and see them contrasted with the latest US and international global satellite weather movies including hurricanes & "tornadoes". See the latest visualizations of spectacular images from NASA/NOAA remote sensing missions like Terra, GOES, TRMM, SeaWiFS, Landsat 7 including 1 - min GOES rapid scan image sequences of Nov 9th 2001 Midwest tornadic thunderstorms and have them explained. See how High-Definition Television (HDTV) is revolutionizing the way we present science to the public. See dust storms and flooding in Africa and smoke plumes from fires in Mexico. See visualizations featured on the covers of Newsweek, TIME, National Geographic, Popular Science & on National & International Network TV. New computer software tools allow us to roam & zoom through massive global images e.g. Landsat tours of the US, and Africa, showing desert and mountain geology as well as seasonal changes in vegetation. See animations of the north and south polar ice packs and with icebergs on the coasts of Greenland and off the coast of Antarctica. Spectacular new visualizations of the global land, atmosphere & oceans are shown. Listen to the pulse of our planet. See how land vegetation, ocean plankton, clouds and temperatures respond to the sun & seasons. See vortexes and currents in the global oceans that bring up the nutrients to feed tiny algae and draw the fish, whales and fisherman. See the how the ocean blooms in response to these currents and El Nino/La Nina climate changes. See the city lights, fishing fleets, gas flares and biomass burning of the Earth at night observed by the "night-vision" DMSP military satellite. The presentation will be made using the latest HDTV and video projection technology that is now done from a laptop computer through an entirely digital path.

Hasler, Arthur F.↗

NASA NTRS2002

Visions of our Planet's Atmosphere, Land and Oceans

Hasler, A. F.↗

NASA NTRS2006

Improved Hurricane Boundary Layer Observations with the Imaging Wind and Rain Airborne Profiler

During the NOAA/NESDIS 2005 Hurricane Season (HS2005) and the 2006 Winter Experiment, the University of Massachusetts (UMass) installed two instruments on the NOAA N42RF WP-3D research aircraft: the Imaging Wind and Rain Airborne Profiler (IWRAP) and the Simultaneous Frequency Microwave Radiometer (SFMR). IWRAP is a dual-band (C- and Ku), dual-polarized pencil-beam airborne radar that profiles the volume backscatter and Doppler velocity from rain and that also measures the ocean backscatter response. It simultaneously profiles along four separate incidence angles while conically scanning at 60 RPM. SFMR is a C-band nadir viewing radiometer that measures the emission from the ocean surface and intervening atmosphere simultaneously at six frequencies. It is designed to obtain the surface wind speed and the column average rain rate. Both instruments have previously been flown during the 2002, 2003 and 2004 hurricane seasons. For the HS2005, the IWRAP system was modified to implement a raw data acquisition system. The importance of the raw data system arises when trying to profile the atmosphere all the way down to the surface with a non-nadir looking radar system. With this particular geometry, problems arise mainly from the fact that both rain and ocean provide a return echo coincident in time through the antenna s main lobe. This paper shows how this limitation has been removed and presents initial results demonstrating its new capabilities to derive the atmospheric boundary layer (ABL) wind field within the inner core of hurricanes to much lower altitudes than the ones the original system was capable of, and to analyze the spectral response of the ocean backscatter and the rain under different wind and rain conditions.

tropical cyclones↗

DOE OSTI2024

In-situ digital image correlation and thermal monitoring in directed energy deposition

A method and a system for digital image correlation and thermal monitoring during directed energy deposition are provided. The method and the system include global off-axis 3D mapping of surfaces features at high frame rates using the natural surface roughness of the additive build. Infrared thermography is projected onto these surface features to record the thermo-mechanical history of the finished component. As set forth herein, the method and the system provide a low-cost solution to monitoring and optimizing the unique temporal artifacts induced by complex scan strategies.

Haley, James↗

NASA NTRS1995

Full resolution hologram-like autostereoscopic display

Under this program, Dimension Technologies Inc. (DTI) developed a prototype display that uses a proprietary illumination technique to create autostereoscopic hologram-like full resolution images on an LCD operating at 180 fps. The resulting 3D image possesses a resolution equal to that of the LCD along with properties normally associated with holograms, including change of perspective with observer position and lack of viewing position restrictions. Furthermore, this autostereoscopic technique eliminates the need to wear special glasses to achieve the parallax effect. Under the program a prototype display was developed which demonstrates the hologram-like full resolution concept. To implement such a system, DTI explored various concept designs and enabling technologies required to support those designs. Specifically required were: a parallax illumination system with sufficient brightness and control; an LCD with rapid address and pixel response; and an interface to an image generation system for creation of computer graphics. Of the possible parallax illumination system designs, we chose a design which utilizes an array of fluorescent lamps. This system creates six sets of illumination areas to be imaged behind an LCD. This controlled illumination array is interfaced to a lenticular lens assembly which images the light segments into thin vertical light lines to achieve the parallax effect. This light line formation is the foundation of DTI's autostereoscopic technique. The David Sarnoff Research Center (Sarnoff) was subcontracted to develop an LCD that would operate with a fast scan rate and pixel response. Sarnoff chose a surface mode cell technique and produced the world's first large area pi-cell active matrix TFT LCD. The device provided adequate performance to evaluate five different perspective stereo viewing zones. A Silicon Graphics' Iris Indigo system was used for image generation which allowed for static and dynamic multiple perspective image rendering. During the development of the prototype display, we identified many critical issues associated with implementing such a technology. Testing and evaluation enabled us to prove that this illumination technique provides autostereoscopic 3D multi perspective images with a wide range of view, smooth transition, and flickerless operation given suitable enabling technologies.

Eichenlaub, Jesse B.↗

DOE OSTI2020

Depth Thermography: Noninvasive 3D Temperature Profiling Using Infrared Thermal Emission

Here, we introduce a technique based on infrared thermal emission, termed depth thermography, that can remotely measure the temperature distribution beneath the surface of certain objects. Depth thermography utilizes the thermal-emission spectrum in the semitransparent spectral region of the target object to extract its temperature as a function of depth, in contrast with conventional thermography, which uses the spectrally integrated thermally emitted power to measure the surface temperature. Coupled with two-dimensional imaging, for example using an infrared hyperspectral camera or scanning a single-pixel spectrometer, this technique can yield volumetric temperature distributions. Furthermore, we carried out a proof-of-concept experiment on an asymmetrically heated fused-silica window, extracting the temperature distribution throughout the sample. Depth thermography may enable noncontact volumetric temperature measurements of microscopic objects such as multilayer electronic devices or macroscopic volumes of liquids and gases, as well as simultaneous all-optical measurements of optical and thermal properties of materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2013

Terahertz Lasers Reveal Information for 3D Images

After taking off her shoes and jacket, she places them in a bin. She then takes her laptop out of its case and places it in a separate bin. As the items move through the x-ray machine, the woman waits for a sign from security personnel to pass through the metal detector. Today, she was lucky; she did not encounter any delays. The man behind her, however, was asked to step inside a large circular tube, raise his hands above his head, and have his whole body scanned. If you have ever witnessed a full-body scan at the airport, you may have witnessed terahertz imaging. Terahertz wavelengths are located between microwave and infrared on the electromagnetic spectrum. When exposed to these wavelengths, certain materials such as clothing, thin metal, sheet rock, and insulation become transparent. At airports, terahertz radiation can illuminate guns, knives, or explosives hidden underneath a passenger s clothing. At NASA s Kennedy Space Center, terahertz wavelengths have assisted in the inspection of materials like insulating foam on the external tanks of the now-retired space shuttle. "The foam we used on the external tank was a little denser than Styrofoam, but not much," says Robert Youngquist, a physicist at Kennedy. The problem, he explains, was that "we lost a space shuttle by having a chunk of foam fall off from the external fuel tank and hit the orbiter." To uncover any potential defects in the foam covering, such as voids or air pockets, that could keep the material from staying in place, NASA employed terahertz imaging to see through the foam. For many years, the technique ensured the integrity of the material on the external tanks.

Source record↗

DOE OSTI2026

Directing Assembly of Mesoscale Multi‐Shell Morphologies of DNA Origami Crystals

Nature builds hierarchically ordered materials, such as seashells, wood, and bones, through spatially and temporally regulated growth. Mimicking such a level of control in synthetic systems remains challenging, particularly in achieving multiscale organizations with prescribed nanoscale arrangements and desired material morphologies. In this study, we introduce a DNA-based self-assembly strategy for constructing diverse multi-shell mesoscale morphologies from nanoscale lattices, enabling prescribed structural, and compositional 3D material patterns. Using DNA origami frames as modular monomers, we direct anisotropic epitaxial growth through addressable DNA frame binding motifs and encapsulate nanoparticles (NPs) in desired 3D patterns. Sequential monomer addition under thermodynamically favorable conditions enables shell growth through heterogeneous nucleation while minimizing unwanted homogeneous nucleation. Here, we demonstrate that DNA-encoded addressability enables epitaxial shell growth along specific lattice directions, yielding crystals with multilayered mesoscale organization, including tube-like (sushi roll) and plate-like (macaron) morphologies. Shell-specific NP configurations and compositions are achieved through addressable and differentiated placement of NPs within each shell, as validated by small-angle x-ray scattering and cross-sectional scanning transmission electron microscopy. We further demonstrate addressable NP release and reveal that shells modulate release kinetics. Together, these findings establish a platform for fabricating DNA origami crystals with programmable mesoscale morphologies, nanoscale structure, composition, and transport properties.

3D patterning↗