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DOE OSTI2026

Automation of Laser Plasma Focused Ion Beam Microscopy for Next-Gen Energy Materials

Automation can revolutionize the use of ultrafast laser ablation and plasma-focused ion beam (PFIB) techniques for high-throughput, reproducible cross-sectioning and various sample preparation in materials characterization. As these methods become essential for analyzing complex energy materials and next-generation devices, efficient, standardized workflows are needed to minimize variability and enhance precision. This work highlights our advancements in developing automated processes for sample preparation that integrates machine learning, workflow optimization, and large-scale data acquisition to improve efficiency and scalability in applications such as electrolyzers, photovoltaic cells, and microelectronics. To streamline cross-sectioning and lamella fabrication, we have implemented fully automated workflows that standardize laser ablation and PFIB milling sequences. These workflows incorporate pre-programmed protocols for material removal, alignment, and thinning, reducing user intervention and ensuring consistency across different sample types. Machine learning algorithms further enhance automation by predicting optimal milling strategies and adapting parameters based on material properties and sectioning requirements. This approach significantly improves throughput while maintaining the structural integrity of prepared samples for high-resolution imaging and analysis, including transmission electron microscopy. Beyond sample preparation, our automation platform enables the acquisition of large, high-resolution datasets through serial sectioning, image alignment, and 3D reconstruction. These automated routines facilitate multi-scale characterization, capturing structural and compositional details from the nanoscale to the device level. By reducing variability and increasing efficiency, our automated approach enhances defect analysis, failure diagnostics, and process optimization, accelerating advancements in materials research and device engineering.

36 MATERIALS SCIENCE↗

NASA NTRS2017

NASA's In-Space Manufacturing Project: Materials and Manufacturing Process Development Update

The mission of NASA's In-Space Manufacturing (ISM) project is to identify, design, and implement on-demand, sustainable manufacturing solutions for fabrication, maintenance and repair during exploration missions. ISM has undertaken a phased strategy of incrementally increasing manufacturing capabilities to achieve this goal. The ISM project began with the development of the first 3D printer for the International Space Station. To date, the printer has completed two phases of flight operations. Results from phase I specimens indicated some differences in material properties between ground-processed and ISS-processed specimens, but results of follow-on analyses of these parts and a ground-based study with an equivalent printer strongly indicate that this variability is likely attributable to differences in manufacturing process settings between the ground and flight prints rather than microgravity effects on the fused deposition modeling (FDM) process. Analysis of phase II specimens from the 3D Printing in Zero G tech demo, which shed further light on the sources of material variability, will be presented. The ISM project has also developed a materials characterization plan for the Additive Manufacturing Facility, the follow-on commercial multimaterial 3D printing facility developed for ISS by Made in Space. This work will yield a suite of characteristic property values that can inform use of AMF by space system designers. Other project activities include development of an integrated 3D printer and recycler, known as the Refabricator, by Tethers Unlimited, which will be operational on ISS in 2018. The project also recently issued a broad area announcement for a multimaterial fabrication laboratory, which may include in-space manufacturing capabilities for metals, electronics, and polymeric materials, to be deployed on ISS in the 2022 timeframe.

Prater, Tracie↗

DOE OSTI2024

Development of ceria-supported metal-oxide (MO x /CeO 2 ) catalysts via a one-pot chemical vapor deposition (OP-CVD) technique: Structure and reverse water gas shift reaction study

Current synthesis techniques for metal oxide (MO x )-supported catalysts have certain limitations of undesired target loading, ineffective dispersion of active species over the surface, uncontrolled particle size of active species, and complicated synthesis steps. Here, we developed a one-pot chemical vapor deposition (OP-CVD) methodology; by using which a solid metal precursor forms a vapor in a controlled condition and gets supported over the surrounding matrix. The theoretical stability followed by experimental validation using TGA is crucial for selecting the metal precursors. Three simple steps viz. premixing, dispersion, and rapid fixation by calcination are involved in the catalyst development via the OP-CVD approach. This study solely focused on the synthesis of 3d transition MO x over ceria support. The physicochemical characterizations of the prepared catalysts were performed by XRD, ICP-OES, SEM-EDX, CO pulse chemisorption, XANES, and EXAFS analyses to understand the crystal structure of involved species, target metal loading, dispersion, and particle size and prove the feasibility and viability of OP-CVD. The prepared catalysts were further tested for reverse water gas shift (RWGS) reaction to link their structural information with activity. The RWGS reaction data showed that the CO activity and CO selectivity were metal - and metal precursor-dependent. Higher CO activity of > 0.1 mol/h g-cat was observed for Cu and Co-based catalysts, with CO selectivity of ~100 %. This study provides an opportunity to produce efficient supported catalysts in a convenient way, providing effective catalytic activity.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Development of a forced advection sampling technique (FAST) for quantification of methane emissions from orphaned wells

Abstract. Orphaned wells, meaning unplugged and non-producing wells lacking responsible owners, pose a significant and undersampled environmental challenge due to their vast number and unknown associated emissions. We propose, develop and test an alternative method for estimating emissions from orphaned wells using a forced advection sampling technique (FAST) that can overcome many of the limitations in current methods (cost, accuracy, safety). In contrast to existing ambient Gaussian plume methods, our approach uses a fan-generated flow to force advection between the emission source and a point methane (CH4) sensor. The fan flow field is characterized using a colocated sonic anemometer to measure the 3D wind profile generated by the fan. Using time-series measurements of CH4 concentration and wind, a simple estimate of the CH4 emission rate of the source can be inferred. The method was calibrated using outdoor controlled-release experiments and then tested on four orphaned wells in Lufkin, TX, and Osage County, OK. Our results suggest that the FAST method can provide a low-cost, portable, fast and safe alternative to existing methods with reasonable estimates of orphaned well emissions over a range of leak rates below 40 g h−1 and within certain geometric and atmospheric constraints.

Dubey, Mohit L↗

DOE OSTI2026

3D Play Fairway Analysis for Examining of Superhot Reservoir Production Scenarios

The DEEPEN (DE-risking Exploration for geothermal Plays in magmatic ENvironments) project was a multi-laboratory, international effort to reduce uncertainty and improve resource characterization in superhot geothermal systems. Building on this foundation, this work advances open-source tools designed to lower the exploration risk and cost of superhot geothermal projects while promoting transparency, reproducibility, and efficiency in exploration workflows. These tools are being tested at two key sites: (1) the Nesjavellir Geothermal Area in Iceland, where the Icelandic Deep Drilling Project (IDDP) will drill its third well, and (2) Newberry Volcano in Oregon, USA, where Mazama Energy will pilot the first superhot enhanced geothermal system (EGS). A major outcome is the creation of a modular, open-source Python framework for play fairway analysis (PFA) in 2D and 3D, called geoPFA. The PFA workflow has been expanded to produce pseudo conceptual models, and will soon be refined to assess reservoir components through integration with the thermo-hydraulic-mechanical-chemical (THMC) simulator TReactMech, to enable iterative coupling between PFA and THMC models, improving characterization of superhot systems. All three of the Icelandic Deep Drilling Project's production scenarios were analyzed via this framework: (1) a superhot deep injection well paired with conventional production wells at Nesjavellir, (2) a superhot deep production well at Nesjavellir, and (3) superhot enhanced geothermal system at Newberry Volcano. This analysis provides useful insights around conceptual modeling of these production scenarios, helping to inform decisions around which scenario is best suited for which types of environments.

15 GEOTHERMAL ENERGY↗

DOE OSTI2026

3D Play Fairway Analysis for Examining of Superhot Drilling Production Scenarios: Preprint

15 GEOTHERMAL ENERGY↗

DOE OSTI2025

Using multimodal X-ray computed tomography to advance 3D petrography: A non-destructive investigation of olivine inside a carbonaceous chondrite

Rocks form in three dimensions through time and studying them provides information from inside dynamic systems we cannot otherwise observe. Yet how we typically access the interior of the rocks themselves to gain that information may limit our understanding and influence how we reconstruct the processes that formed them. Here, we demonstrate combined non-destructive 3D X-ray imaging techniques that produce quantitative densitometric and crystallographic maps of entire individual grains inside a rock. Olivine grains throughout a sample of the carbonaceous chondrite Northwest Africa (NWA) 11346 were each characterized by size, shape, composition, zoning intensity, and crystallographic orientation. The addition of 3D crystallographic mapping to calibrated 3D densitometric analysis—used to calculate chemical composition—demonstrates a fully non-destructive petrographic method and provides unique insight. For instance, in our case, using crystallographic data to delineate individual grains and then measuring the 3D size, shape, and composition of each distinguishes variably reset relict grains from those later crystallized after a melting event. Intersection in a 2D slice could not have led to this interpretation because the integration of three-dimensional size, rounding, composition, location, and crystallographic orientation measured from each grain forms the key patterns. Multimodal laboratory X-ray imaging has strong potential to advance 3D petrography.

36 MATERIALS SCIENCE↗

DOE OSTI2025

3D-printed mirror-less helicity preserving metasurface “mirror” for THz applications

Stimulated by seminal works on generalized reflection and refraction laws, metasurfaces have evolved to a highly promising research direction, as they allow a multitude of different functionalities by optically thin wave-control elements/structures. Among them, structures functioning in the low THz regime are of extensive research interest, due to their high potential in communication and sensing applications. In this paper we propose a simple THz metasurface design that exhibits ideally perfect cross-polarized reflection for linear polarization and perfect helicity-preserving reflection with a geometric (Pancharatnam–Berry) phase for circular polarization, without the presence of any back-reflector. Numerical calculations demonstrating the structure response are justified by analytical models, which provide physical insights on this response. The designed metasurfaces are fabricated using the direct laser writing 3D-printing technology, metallized with electroless silver plating, and are characterized by THz time domain spectroscopy, with the experimental results validating the corresponding theoretical ones. Applications including beam steering and focusing, exploring the Pancharatnam–Berry phase, are also demonstrated numerically. Besides those applications, the helicity preserving mirror response of our metasurfaces can be valuable, among others, also in molecular chirality sensing applications, an issue that is also highlighted here.

3D-printed metasurfaces↗

DOE OSTI2026

3D printed water-stable Cd-doped Cs 4 MnBi 2 Cl 12 /polylactic acid perovskite/polymer composites for high-flux X-ray scintillation

Stable and efficient X-ray scintillators are crucial for medical diagnostics, industrial, and defense applications. However, conventional scintillator technologies face a trade-off between stability, optimal performance, and sustainability. Herein, we introduce 3D-printed Cs 4 MnBi 2 Cl 12 (Pero1) and Cs 4 Cd 0.68 Mn 0.32 Bi 2 Cl 12 (Pero2) perovskite microcrystals embedded within a polylactic acid (PLA) polymer composite as X-ray scintillators, combining efficiency, stability, and sustainability. The orange luminescent perovskite powder phosphors exhibited poor water stability, which was successfully addressed through incorporation into PLA via filament extrusion and fused deposition modeling (FDM) 3D printing. The resulting composite films demonstrated remarkable water stability while maintaining uniform orange emission throughout the polymer matrix, as confirmed by 3D topography scanning and X-ray fluorescence mapping. Structural characterization revealed minimal chemical interaction between the perovskite and PLA matrix, with the composites retaining their crystalline properties. The PLA-Pero2 composite exhibited superior optical properties, with a photoluminescence quantum yield of 47%, nearly 17 times higher than that of PLA-Pero1 (2.8%), attributed to the effective suppression of non-radiative decay pathways through Cd 2+ doping. Under hard X-ray irradiation at synchrotron beamlines, both composites exhibited excellent radioluminescence, with emission peaks at 605 nm, a linear response across a wide X-ray flux range, and remarkable radiation stability, showing less than 3% intensity degradation after 600 seconds of continuous high-dose exposure. The PLA-Pero2 composite achieved a spatial resolution of 5 line pairs per millimeter and a contrast ratio of 0.255. These performance metrics, combined with the polymer's biodegradability and scalability through additive manufacturing, position PLA-based composites as a more sustainable alternative to conventional petroleum-based polymer scintillators for next-generation medical imaging, radiation monitoring, and industrial radiography applications.

3D Printing↗

NASA NTRS2016

Average Cross-Sectional Area of DebriSat Fragments Using Volumetrically Constructed 3D Representations

Debris fragments from the hypervelocity impact testing of DebriSat are being collected and characterized for use in updating existing satellite breakup models. One of the key parameters utilized in these models is the ballistic coefficient of the fragment which is directly related to its area‐to‐mass ratio. However, since the attitude of fragments varies during their orbital lifetime, it is customary to use the average cross‐sectional area in the calculation of the area‐to‐mass ratio. The average cross‐sectional area is defined as the average of the projected surface areas perpendicular to the direction of motion and has been shown to be equal to one‐fourth of the total surface area of a convex object. Unfortunately, numerous fragments obtained from the DebriSat experiment show significant concavity (i.e., shadowing) and thus we have explored alternate methods for computing the average cross‐sectional area of the fragments. An imaging system based on the volumetric reconstruction of a 3D object from multiple 2D photographs of the object was developed for use in determining the size characteristic (i.e., characteristics length) of the DebriSat fragments. For each fragment, the imaging system generates N number of images from varied azimuth and elevation angles and processes them using a space‐carving algorithm to construct a 3D point cloud of the fragment. This paper describes two approaches for calculating the average cross‐sectional area of debris fragments based on the 3D imager. Approach A utilizes the constructed 3D object to generate equally distributed cross‐sectional area projections and then averages them to determine the average cross‐sectional area. Approach B utilizes a weighted average of the area of the 2D photographs to directly compute the average cross‐sectional area. A comparison of the accuracy and computational needs of each approach is described as well as preliminary results of an analysis to determine the "optimal" number of images needed for the 3D imager to accurately measure the average cross sectional area of objects with known dimensions.

Scruggs, T.↗

NASA NTRS2011

NASA Tech Briefs, December 2011

Topics covered include: 1) SNE Industrial Fieldbus Interface; 2) Composite Thermal Switch; 3) XMOS XC-2 Development Board for Mechanical Control and Data Collection; 4) Receiver Gain Modulation Circuit; 5) NEXUS Scalable and Distributed Next-Generation Avionics Bus for Space Missions; 6) Digital Interface Board to Control Phase and Amplitude of Four Channels; 7) CoNNeCT Baseband Processor Module; 8) Cryogenic 160-GHz MMIC Heterodyne Receiver Module; 9) Ka-Band, Multi-Gigabit-Per-Second Transceiver; 10) All-Solid-State 2.45-to-2.78-THz Source; 11) Onboard Interferometric SAR Processor for the Ka-Band Radar Interferometer (KaRIn); 12) Space Environments Testbed; 13) High-Performance 3D Articulated Robot Display; 14) Athena; 15) In Situ Surface Characterization; 16) Ndarts; 17) Cryo-Etched Black Silicon for Use as Optical Black; 18) Advanced CO2 Removal and Reduction System; 19) Correcting Thermal Deformations in an Active Composite Reflector; 20) Umbilical Deployment Device; 21) Space Mirror Alignment System; 22) Thermionic Power Cell To Harness Heat Energies for Geothermal Applications; 23) Graph Theory Roots of Spatial Operators for Kinematics and Dynamics; 24) Spacesuit Soft Upper Torso Sizing Systems; 25) Radiation Protection Using Single-Wall Carbon Nanotube Derivatives; 26) PMA-PhyloChip DNA Microarray to Elucidate Viable Microbial Community Structure; 27) Lidar Luminance Quantizer; 28) Distributed Capacitive Sensor for Sample Mass Measurement; 29) Base Flow Model Validation; 30) Minimum Landing Error Powered-Descent Guidance for Planetary Missions; 31) Framework for Integrating Science Data Processing Algorithms Into Process Control Systems; 32) Time Synchronization and Distribution Mechanisms for Space Networks; 33) Local Estimators for Spacecraft Formation Flying; 34) Software-Defined Radio for Space-to-Space Communications; 35) Reflective Occultation Mask for Evaluation of Occulter Designs for Planet Finding; and 36) Molecular Adsorber Coating

Source record↗

DOE OSTI2026

Strain mapping of three-dimensionally structured two-dimensional materials

Strain plays a crucial role in tuning materials’ properties, influencing their optical, electrical, and chemical performances. In two-dimensional (2D) materials, applied stress often induces out-of-plane deformation, resulting in a more intricate three-dimensional (3D) topography, where mapping the strain remains a challenge due to the limitations of conventional characterization techniques. In this work, we introduce BRIGHT (Bragg-Rod Informed, Gradient-based Height-mapping Technique), an integrated method for reconstructing both the topography and planar strain profile of 3D-structured 2D materials using nanobeam four-dimensional scanning transmission electron microscopy (4D-STEM). We apply BRIGHT to a MoS2-MoSe2 transition metal dichalcogenide (TMD) lateral heterojunctions exhibiting built-in strain and out-of-plane ripples and show that varying heterojunction widths lead to distinct surface morphologies and corresponding changes in the planar strain distribution. These results establish a foundation for more effective strain engineering in 2D materials by accounting for out-of-plane structural features, thereby enabling more precise control of strain-dependent properties.

Mireles, Adan [Rice Univ., Houston, TX (United Sta↗

NASA NTRS2006

Construction and Resource Utilization Explorer (CRUX): Implementing Instrument Suite Data Fusion to Characterize Regolith Hydrogen Resources

CRUX is a modular suite of geophysical and borehole instruments combined with display and decision support system (MapperDSS) tools to characterize regolith resources, surface conditions, and geotechnical properties. CRUX is a NASA-funded Technology Maturation Program effort to provide enabling technology for Lunar and Planetary Surface Operations (LPSO). The MapperDSS uses data fusion methods with CRUX instruments, and other available data and models, to provide regolith properties information needed for LPSO that cannot be determined otherwise. We demonstrate the data fusion method by showing how it might be applied to characterize the distribution and form of hydrogen using a selection of CRUX instruments: Borehole Neutron Probe and Thermal Evolved Gas Analyzer data as a function of depth help interpret Surface Neutron Probe data to generate 3D information. Secondary information from other instruments along with physical models improves the hydrogen distribution characterization, enabling information products for operational decision-making.

in situ resource utilization (ISRU)↗

DOE OSTI2026

Geology of the One Earth Energy Site

The One Earth Energy site is one of two sites in the Illinois Storage Corridor (ISC) project. The objectives of the ISC project is to accelerate commercial deployment of carbon capture utilization and storage at two individual sites and receive approvals for Underground Injection Control (UIC) Class VI permits for construction at each site. At the One Earth Energy site, an extensive data collection program was undertaken, which included the drilling of a test well (One Earth Energy #1 [OEE #1]), four 2D seismic lines, and a small 3D seismic survey. The OEE #1 well was drilled in 2022 and acquired extensive core, log, and testing data to characterize the subsurface geology of the site. Coring was focused on the storage interval, the Mt. Simon Sandstone, and the confining interval, the Eau Claire Formation. The core and log data were used to evaluate the sedimentology and sequence stratigraphy, as well as to develop the conceptual geologic model. This report includes the geological summaries of the Mt. Simon Sandstone and the Eau Claire Formation. The extensive analysis of the log data is included in the petrophysical section, showing ranges of porosity, estimated pore size, and the mineral content of selected zones in the well. The separate petrographic technical report entitled “Petrographic and Advanced Geologic Characterization Report on One Earth Energy #1 (API# 1211325373)”, report number DOE-UIUC-0031892-04, details thin section point-counting analysis that includes mineralogical and pore space analysis, including grain size analysis, annotated thin section photomicrographs, scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDS), and statistics of grain size analysis on Mt. Simon thin sections from OEE #1. The final OEE #1 well data to be included in this geology report is the routine core analysis of both whole core plugs and rotary sidewall core plugs. In addition to the OEE #1 well, four 2D seismic lines and a small 3D survey were acquired as part of the overall subsurface geological characterization. This geology report references the seismic interpretation report, entitled “One Earth Energy Site Seismic Interpretation Task 5.0”, report number DOE-UIUC-0031892-07. This report details the stratigraphic and structural interpretation of the 2D and 3D seismic data acquired at the One Earth Energy site. The 2D seismic data was acquired in 2019 and 2021, and the 3D survey was acquired in 2022. The objectives of the seismic programs were to contribute to the subsurface characterization of the Mt. Simon-Eau Claire Storage Complex by evaluating the continuity of potential storage reservoirs and containment intervals across the project area, and to determine if any geologic features are present that would increase containment risk to the proposed carbon storage project.

09 BIOMASS FUELS↗

DOE OSTI2025

Benchmark microgravity experiments and computations for 3D dendritic-array stability in directional solidification

In this study, we present a comprehensive quantitative analysis of stability bands for dendritic arrays during directional solidification of a transparent succinonitrile-0.46 wt % camphor alloy, spanning a broad range of pulling velocities. Taking advantage of the microgravity environment aboard the International Space Station where most convection effects are suppressed, we obtain unique measurements that quantify the stable primary spacing range of spatially extended three-dimensional dendritic array structures under purely diffusive growth conditions. Through carefully designed velocity jump experiments and detailed examination of sub-grain boundary dynamics, we characterize key instabilities, including elimination and tertiary branching, shedding new light on the mechanisms governing dynamic dendritic spacing selection in extended 3D arrays. Phase field simulations are performed to characterize the stability limits of dendritic array structures for quantitative comparison with the flight experiments. Although the simulations capture general trends, significant deviations are noted at the upper stability boundary, indicating the influence of additional, unexplored factors. These findings contribute to a deeper understanding of dendritic growth dynamics and offer valuable benchmark data that could aid in refining predictive models and improving control of dendritic microstructures in metallurgical applications.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Probing boron vacancy defects in hBN via single spin relaxometry

Spin defects in solids offer promising platforms for quantum sensing and memory due to their long coherence times and optical addressability. Here, we integrate a single nitrogen-vacancy (NV) center in diamond with scanning probe microscopy to detect, read out, and spatially map spin-based quantum sensors at the nanoscale. Using the boron vacancy ($V$$^{–}_{B}$) center in hexagonal boron nitride—an emerging two-dimensional spin system—as a model, we detect its electron spin resonance indirectly via changes in the spin relaxation time (T 1 ) of a nearby NV center, eliminating the need for optical excitation or fluorescence detection of the $V$$^{–}_{B}$. Cross-relaxation between NV and $V$$^{–}_{B}$ ensembles significantly reduces NV T1, enabling quantitative nanoscale mapping of defect densities beyond the optical diffraction limit and clear resolution of hyperfine splitting in isotopically enriched h 10 B 15 N. Our method demonstrates interactions between spin sensors in 3D and 2D materials, establishing NV centers as versatile probes for characterizing otherwise inaccessible spin defects.

Quantum metrology↗

DOE OSTI2024

Ultrasonic Characterization of Material Properties in Metal Components Additively Manufactured by Powder Bed Fusion

We present the methodology for using pulsed-echo ultrasound to characterize the properties of additively manufactured (AM) metal components and their response to changes in the fabrication settings. We show how to accurately characterize anisotropy in these properties and when such characterization can be performed noninvasively. Our approach, when applied to 3D-printed stainless steel samples, reveals a significant heterogeneity between the surface and internal properties of the AM part and the anisotropy in material properties in the build and transverse directions.

Walton, Kenneth↗

DOE OSTI2024

Characterization of Stress-Corrosion-Cracking in Plutonium-Bearing Storage Containers

Introduction • The Integrated Surveillance Program, under the Department of Energy, is responsible for the periodic surveillance of storage containers containing plutonium-bearing materials. • The container-packages are designed to isolate the materials for 50 to 100 years with minimal surveillance. • During monitoring, corrosion-pitting and stress-corrosion-cracking (SCC) has been identified in some of the inner-cans near the weld regions. • SCC through wall penetration would result in an undesired increased risk of leakage. • An investigation is in progress to identify and characterize corrosion events to determine the prevalence of corrosion features and the likelihood of a throughwall breach. • Here, we discuss the characterization efforts carried out by Scanning Electron Microscopy (SEM), including 3D-tomography by Focused Ion Beam (FIB) methods.

Perez, Emmanuel E.↗