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DOE OSTI2025

Towards Mitigating Electron Beam-Induced Damage in MOFs Using Low Dose Electron Microscopy for In-Situ Room-Temperature Measurements

Metal-Organic Frameworks (MOFs) have emerged as a versatile class of materials with applications in gas storage and separation, catalysis, and drug delivery [1]. Understanding their damage mechanisms in under various environmental conditions is crucial for optimizing performance and stability [2]. This study employs a combination of Length Structural Coherence (LSC) analysis in electron scattering and Electron Energy Loss Spectroscopy (EELS) to elucidate the damage mechanisms in two representative MOFs. MIL101(Fe), and MIL101(Cr). Here, the primary objective is to reveal structural and chemical changes that occur under electron beam irradiation in Scanning Transmission Electron Microscopy (STEM), both in the pristine state and during in-situ CO and CO 2 adsorption. By combining LSC in Radial Distribution Function (RDF) analysis with EELS, comprehensive insights into the nanoscale alterations are obtained and correlated to the electron dose rate.

dos Santos, Gabriel T. [Northwestern University, E↗

NASA NTRSDate not supplied

Europa Luminescence Microscope

The Europa Luminescence Microscope (ELM) is an automated fluorescence and dark-field mi-croscope designed to meet key objectives defined in the NASA Europa Lander Study Report, includ-ing the identification and characterization of morphological biosignatures. ELM’s heritage stems from a 2U cubesat fluorescence microscope, the Fluorescence Analysis for In-situ Research (FLAIR) im-ager, designed and built at NASA Ames Research Center, for the autonomous study of microbial bi-ology in low Earth orbit. For the ELM implementation, a sample is autonomously manipulated with a microfluidic system using in-line filter sets to capture successively smaller particles on 10, 1.0, and 0.1 µm pore-size filters for imaging. For darkfield imaging, ELM uses ultraviolet and visible light to image organic and inorganic structures with submicron resolution. The ability to detect structural and chemical biosignatures as small as 0.2 µm in size is achieved by imaging native fluorescence and us-ing fluorescence microscopy stains to identify key molecular and structural indicators of microbial life (proteins, lipids, nucleic acids). To excite fluorescence, ELM uses LEDs with wavelengths centered near 265, 370, 470, and 530 nm and five emission bands. The use of multiple excitation and emission wavelengths for native fluorescence imaging not only enables the detection of different molecular species, but also their rough classification. Excitation at 265 nm allows for the detection of smaller polyaromatic hydrocarbons (PAHs; 1-5 rings), aromatic amino acids, and proteins with little to no interference from mineral fluorescence, given proper emission band selection. 370 and 470 nm light excites increasingly larger PAH structures (e.g., coronene) and larger aromatic biomolecules that may be present (e.g., protective pigments). Similarly, inorganic fluorescence can be characterized and sep-arated from organic fluorescence, allowing the recognition and in some cases classification, of miner-als and other abiotic particles. ELM is based upon work supported by the NASA COLDTech and ICEE-2 programs.

Microscope↗

NASA NTRS2013

Coordinated in Situ Analyses of Organic Nanoglobules in the Sutter's Mill Meteorite

The Sutter's Mill meteorite is a newly fallen carbonaceous chondrite that was collected and curated quickly after its fall. Preliminary petrographic and isotopic investigations suggest affinities to the CM2 carbonaceous chondrites. The primitive nature of this meteorite and its rapid recovery provide an opportunity to investigate primordial solar system organic matter in a unique new sample. Here we report in-situ analyses of organic nanoglobules in the Sutter's Mill meteorite using UV fluorescence imaging, Fourier-transform infrared spectroscopy (FTIR), scanning transmission electron microscopy (STEM), NanoSIMS, and ultrafast two-step laser mass spectrometry (ultra-L2MS).

Nakamura-Messenger, K.↗

NASA NTRS2013

Coordinated In Situ Analyses of Organic Nanoglobules in the Sutter's Mill Meteorite

The Sutter s Mill meteorite is a newly fallen carbonaceous chondrite that was collected and curated quickly after its fall [1]. Preliminary petrographic and isotopic investigations suggest affinities to the CM2 carbonaceous chondrites. The primitive nature of this meteorite and its rapid recovery provide an opportunity to investigate primordial solar system organic matter in a unique new sample. Organic matter in primitive meteorites and chondritic porous interplanetary dust particles (CP IDPs) is commonly enriched in D/H and N-15/N-14 relative to terrestrial values [2-4]. These anomalies are ascribed to the partial preservation of presolar cold molecular cloud material [2]. Some meteorites and IDPs contain gm-size inclusions with extreme H and N isotopic anomalies [3-5], possibly due to preserved primordial organic grains. The abundance and isotopic composition of C in Sutter's Mill were found to be similar to the Tagish Lake meteorite [6]. In the Tagish Lake meteorite, the principle carriers of large H and N isotopic anomalies are sub-micron hollow organic spherules known as organic nanoglobules [7]. Organic nanoglobules are commonly distributed among primitive meteorites [8, 9] and cometary samples [10]. Here we report in-situ analyses of organic nano-globules in the Sutter's Mill meteorite using UV fluorescence imaging, Fourier-transform infrared spectroscopy (FTIR), scanning transmission electron microscopy (STEM), NanoSIMS, and ultrafast two-step laser mass spectrometry (ultra-L2MS).

Nakamura--Messenger, K.↗

NASA NTRS2005

On the Origin of the Saturnian Satellite System: Did Iapetus Form In-Situ?

Current models of planet and satellite formation are marred by our lack of understanding regarding the turbulent state of accretion disks. According to the Rayleigh criterion, Keplerian disks are hydrodynamically stable. Indeed, it has been argued that a carefully designed Taylor Couette experiment shows stability in the case of positive radial gradients in specific angular momentum even for high Reynolds numbers [1], in agreement with numerical simulations which consistently show turbulence decay [2]. Other possible sources of turbulence may fail due to low ionization, may decay as the optical depth decreases due to dust coagulation, may involve unrealistic boundary conditions, or result in limited transport. The difficulty stems not only from the degree of turbulence, but also from the kind of turbulence, and whether it may be characterized by an alpha parameter.

Mosqueira, I.↗

DOE OSTI2026

TEM Approaches for Microstructure-Informed Prediction of Mechanical Properties in Structural Alloys

Predicting the mechanical performance of structural alloys from their evolving microstructure remains a major challenge in materials science, particularly for nuclear structural materials, where irradiation-induced defects span multiple types and length scales and interact through complex mechanisms. The dispersed barrier hardening (DBH) [1] and Friedel–Kroupa–Hirsch (FKH) [2,3] models have been widely used to evaluate the hardening contributions of individual obstacles and to estimate tensile strength from quantified microstructures; however, when multiple size-dependent obstacles coexist and evolve, predicting temperature-dependent tensile strength becomes significantly more complex, and a fully consistent hardening model is still lacking. Transmission electron microscopy (TEM) plays a central role in refining hardening models and enabling predictive assessments of tensile strength evolution by providing quantitative characterization of dislocations, irradiation-induced defects (e.g., dislocation loops and cavities), precipitates, and grain structure (Fig. 1.). These experimentally measured defect densities are incorporated into physically based hardening models with size- and shape- dependent obstacle strengths [4], using root-sum-square superposition for obstacles of comparable strength and linear superposition for dissimilar ones [5]. In addition, recent advances in TEM [6-8], including high-resolution imaging, 4D-STEM strain mapping, EDS/EELS elemental analysis, and flash-polishing-based TEM specimen preparation and extraction-replica methods (Fig. 2), further improve the accuracy of microstructural quantification. By comparison with prior studies as well as our own results, we show that when TEM-derived microstructural information is carefully integrated with physically grounded hardening models, yield strength (or irradiation-induced hardening) measured at room temperature can be predicted with good quantitative agreement across multiple alloy classes. In-situ TEM combined with high-temperature mechanical testing represents an important next step for refining hardening models by directly probing dislocation–obstacle interactions across varying irradiation doses and temperatures [9]. Because the barrier strength factor (α) depends on both temperature and obstacle size, it should not be treated as a constant fitting parameter; rather, it must be explicitly evaluated to achieve physically meaningful predictions of mechanical behaviour at operating temperatures. This presentation therefore discusses why all strengthening contributions (e.g., Peierls stress, solid-solution strengthening, voids, bubbles, dislocation loops, dislocation lines, and grain boundaries) must be considered collectively, why appropriate superposition methods are essential when obstacles possess different barrier strength factors, how hardness measurements can be meaningfully related to tensile properties, and how TEM-derived microstructural information can be systematically incorporated into hardening models. More broadly, it outlines a pathway toward microstructure-informed prediction of mechanical properties and supports the goal of establishing science-based tools for evaluating structural materials in extreme environments [10].

Lin, Yan-Ru [ORNL] (ORCID:0000000339991473)↗

NASA NTRSDate not supplied

Space Launch System Artemis I CubeSats: SmallSat Vanguards of Exploration, Science and Technology

When NASA’s Space Launch System (SLS) rocket launches in 2021 with the Orion crew vehicle, it will lay the foundation for NASA’s goal of landing the first woman and the next man on the Moon as part of the Artemis program. This first flight—Artemis I—will also mark a milestone for smallsats. Thirteen6U CubeSats are manifested on the Artemis I flight, the first fleet of CubeSats carried as a ride share opportunity to deep space.(NASA’s first CubeSats to deep space, the twin Mars Cube One [MarCO] spacecraft, were an integral part of the InSight Mars lander mission). The Artemis I CubeSat manifest represents a diverse collection of smallsats performing an array of science missions and technology demonstrations. Payloads from NASA, international partners, academia and industry will execute a variety of experiments. Several smallsats will perform lunar-focused missions that may return data that addresses Strategic Knowledge Gaps (SKGs) in the agency’s lunar exploration program. Indeed, the Artemis I CubeSats will be in the vanguard of the agency’s 21st-century lunar program. The Artemis I missions will produce data to support space radiation awareness,crewed landings and in-situ resource utilization, helping to support a sustained human lunar presence. Several of the Artemis I CubeSats are demonstrating new technologies, including propulsion capabilities. Among the Artemis I CubeSats are three selected through NASA’s Cube Quest Challenge, part of the Centennial Challenges program. These three missions will compete for prize money while meeting specific technical development goals. Payloads from the Japanese and Italian space agencies provide an early opportunity for international involvement in the Artemis program. Student involvement in almost half of the payloads allow STEM engagement with NASA’s Artemis program. The SLS Block 1 vehicle for the Artemis I flight is manufactured with several elements delivered to Kennedy Space Center (KSC) and being prepared for stacking and integration. The new-development of the program, the 212-footcore stage with its four RS-25 engines installed is currently at Stennis Space Center (SSC) for “green run” testing. Following the green run test campaign, the stage will ship to KSC, where it will be integrated with the rest of the vehicle, including the upper stage adapter, where the Artemis I smallsats will be housed.

Kimberly F Robinson↗

NASA NTRS1999

Fundamental Studies of Solidification in Microgravity Using Real-Time X-Ray Microscopy

This research applies a state of the art X-ray Transmission Microscope, XTM, to image (with resolutions up to 3 micrometers) the solidification of metallic or semiconductor alloys in real-time. We have successfully imaged in real-time: interfacial morphologies, phase growth, coalescence, incorporation of phases into the growing interface, and the solute boundary layer in the liquid at the solid-liquid interface. We have also measured true local growth rates and can evaluate segregation structures in the solid; a form of in-situ metallography. During this study, the growth of secondary phase fibers and lamellae from eutectic and monotectic alloys have been imaged during solidification, in real-time, for the first time in bulk metal alloys. Current high resolution X-ray sources and high contrast X-ray detectors have advanced to allow systematic study of solidification dynamics and the resulting microstructure. We have employed a state-of-the-art sub-micron source with acceleration voltages of 10-100 kV to image solidification of metals. One useful strength of the XTM stems from the manner an image is formed. The radiographic image is a shadow formed by x-ray photons that are not absorbed as they pass through the specimen. Composition gradients within the specimen cause variations in absorption of the flux such that the final image represents a spatial integral of composition (or thickness). The ability to image these features in real-time enables more fundamental and detailed understanding of solidification dynamics than has previously been possible. Hence, application of this technique towards microgravity experiments will allow rigorous testing of critical solidification models.

Curreri, Peter A.↗

NASA NTRSDate not supplied

NASA Lunabotics Robotic Mining Competition 10th Anniversary (2010-2019): Taxonomy and Technology Review

Space Mining for resources such as water ice, and regolith, which contain many elements in the form of metals, minerals, volatiles and other compounds, is a necessary step for In-Situ Space Resource Utilization (ISRU). One of the primary goals is to extract propellants from the regolith and water ice, such as oxygen and hydrogen which could then be used for in-space transportation. In addition, the space mining system can be used for various construction tasks that can benefit human and robotic exploration as well as scientific investigations based on excavated exposed topography, such as the side walls of trenches. The National Aeronautics & Space Administration (NASA) "Lunabotics" Robotic Mining Competition (RMC) is a university-level competition designed to engage and retain students in science, technology, engineering and mathematics (STEM). NASA has directly benefited from the competition by encouraging the development of innovative lunar excavation concepts from universities which has resulted in clever ideas and solutions which could be applied to an actual lunar excavation device or payload. The challenge is for students to design and build a remote controlled or autonomous excavator, called a "lunabot", which can collect and deposit a minimum of 10 kilograms of lunar simulant within 15 minutes. In recent years the goal has been changed to excavate a minimum of 1 kg of simulated icy regolith which is found under an overburden of regolith simulant. The complexities of the challenge include the abrasive characteristics of the lunar regolith simulant, the weight and size limitations of the lunabot, and the ability to control the lunabot from a remote-control center or operate it autonomously. This paper will present the results of the ten Lunabotics Robotic Mining Competitions held between May 2010 and May 2019. Each year over 50 university teams have attended, resulting in over 500 lunabot designs and subsequent prototypes. Over 6,000 university students have been part of the on-site competition at KSC. Even more students and the public were engaged via internet broadcasting and social networking media. The various designs have been cataloged and categorized here to provide information to future Lunabotics RMC mining robot designers and competitors. Categories will focus on both the mechanical design as well as the autonomy architecture/design. It is also expected to be of value for actual future space missions, as knowledge is gained from testing many innovative prototypes in simulated lunar regolith. A taxonomy of robotic excavator designs has been presented. In addition, the paper will discuss changes in learning paradigms occurring in the current generation of students, and how this competition leverages those changes to challenge students to develop skills in graduate level concepts and apply them. Examples of how this translates to hiring opportunities for commercial sponsors has also been discussed.

Robert P Mueller↗

NASA NTRSDate not supplied

Lunabotics Robotic Mining Competition for Universities

Space Mining for resources such as water ice, and regolith, which contain many elements in the form of metals, minerals, volatiles and other compounds, is a necessary step for In-Situ Space Resource Utilization (ISRU). One of the primary goals is to extract propellants from the regolith and water ice, such as oxygen and hydrogen which could then be used for in-space transportation. In addition, the space mining system can be used for various construction tasks that can benefit human and robotic exploration as well as scientific investigations based on excavated exposed topography, such as the side walls of trenches. The National Aeronautics & Space Administration (NASA) “Lunabotics” Robotic Mining Competition (RMC) is a university-level competition designed to engage and retain students in science, technology, engineering and mathematics (STEM). NASA has directly benefited from the competition by encouraging the development of innovative lunar excavation concepts from universities which has resulted in clever ideas and solutions which could be applied to an actual lunar excavation device or payload. The challenge is for students to design and build a remote controlled or autonomous 80 kg mass lightweight excavator, called a “lunabot”, which can collect and deposit a minimum of 10 kilograms of lunar simulant within 15 minutes. In recent years the goal has been changed to excavate a minimum of 1 kg of simulated icy regolith which is found under an overburden of regolith simulant. The complexities of the challenge include the abrasive characteristics of the lunar regolith simulant, the weight and size limitations of the lunabot, and the ability to control the lunabot from a remote mission control center or operate it autonomously. This presentation will summarize the results of the Lunabotics Robotic Mining Competitions held in May 2022. Each year, since 2010, over 50 university teams have attended, resulting in over 500 lunabot designs and subsequent prototypes. Over 6,000 university students have been part of the on-site competition at KSC, and many are employed in the space sector today with thriving careers. Even more students and the public were engaged via internet broadcasting and social networking media. Examples of how this translates to hiring opportunities for commercial sponsors will also be discussed. Overall, this competition has proven to be popular with multi-disciplinary university senior design classes and a valuable tool for NASA and academia in educating and inspiring the next generation of space engineers.

Lunabotics↗

NASA NTRSDate not supplied

NASA LUNABOTICS ROBOTIC MINING COMPETITION 10TH ANNIVERSARY (2010 â€“ 2019): TAXONOMY AND TECHNOLOGY REVIEW

Space Mining for resources such as water ice, and regolith, which contain many elements in the form of metals, minerals, volatiles and other compounds, is a necessary step for In-Situ Space Resource Utilization (ISRU). One of the primary goals is to extract propellants from the regolith and water ice, such as oxygen and hydrogen which could then be used for in-space transportation. In addition, the space mining system can be used for various construction tasks that can benefit human and robotic exploration as well as scientific investigations based on excavated exposed topography, such as the side walls of trenches. The National Aeronautics & Space Ad-ministration (NASA) Lunabotics Robotic Mining Competition (RMC) is a university-level competition designed to engage and retain students in science, technology, engineering and mathematics (STEM). NASA has directly benefited from the competition by encouraging the development of innovative lunar excavation concepts from universities which has resulted in clever ideas and solutions which could be applied to an actual lunar excavation device or payload. The challenge is for students to design and build a remote controlled or autonomous excavator, called a lunabot, that can collect and deposit a minimum of 10 kilograms of lunar simulant within 15 minutes. In recent years the goal has been changed to excavate a minimum of 1 kg of simulated icy regolith which is found under an over-burden of regolith simulant. The complexities of the challenge include the abrasive characteristics of the lunar simulant, the weight and size limitations of the lunabot, and the ability to control the lunabot from a remote control center. This paper will present the results of the 10 Lunabotics Robotic Mining Competitions held between May 2010 and May 2019. Each year over 50 university teams have attended, resulting in over 500 lunabot designs and subsequent prototypes. Over 5,000 university students have been part of the competition on-site at KSC. More students and the public were en-gaged via internet broadcasting and social net-working media. The various designs will be cataloged and categorized to provide information to future Lunabotics mining robot designers and competitors. It is also expected to be of value for actual future space missions, as knowledge is gained from testing many innovative prototypes in simulated lunar regoith. A taxonomy of robotic excavator designs will be presented.

Competition↗

DOE OSTI2026

Prelithiated SiO x /Graphite-NMC811 Cells: Capacity Loss, Impedance Rise and Hidden Degradation Pathways Revealed Using Three-Electrode Diagnostics

Electrodes containing SiO x /graphite (Gr) materials are attractive as anodes for high-energy lithium-ion batteries. However, their mechanical deformation, electrochemical response, and impedance evolution during long-term cycling are strongly coupled, complicating accurate diagnosis of performance fade mechanisms. In this work, the behavior of electrochemically prelithiated SiO x /Gr anodes paired with NMC811 cathodes is systematically investigated using techniques that include in-situ dilatometry, three-electrode electrochemistry, and multiscale post-cycling microscopy. The SiO x /Gr electrode exhibits a maximum expansion of 49% upon lithiation to 10 mV vs Li + /Li, with 84% of the expansion and 91% of the capacity being reversible. In full cells, relatively stable cycling with only 12% capacity fade over 500 cycles is observed. Three-electrode experiments reveal cell-level impedance growth, which is dominated by the NMC811 cathode: the SiO x /Gr anode exhibits minimal net impedance rise and an initial impedance decrease at low potentials. Despite this apparent electrochemical stability, cross-sectional SEM, PFIB tomography, and cryo-STEM reveal irreversible anode thickening caused by the accumulation of an inorganic-rich solid electrolyte interphase (SEI) permeating the anode bulk. Electrode potential-shift analysis further demonstrates that Li + ions released from lithium reservoirs in the prelithiated anode mask true lithium inventory loss during aging. These results demonstrate that low-expansion SiO x /Gr anodes can simultaneously exhibit favorable cycling and impedance metrics while undergoing substantial, hidden degradation, underscoring the importance of electrode-resolved diagnostics for evaluating prelithiated silicon-based anodes.

25 ENERGY STORAGE↗

DOE OSTI2026

In-situ observations of cyclic deformation in an extruded Mg-2Nd-1Y-0.1Zr-0.1Ca alloy

In this study, the evolution of deformation mechanisms during cyclic loading in an extruded, solution-treated Mg–2Nd–1Y–0.1Zr–0.1Ca alloy was investigated using a combination of in-situ loading, scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), and focused ion beam (FIB) nanofabrication. The initial microstructure exhibited a random crystallographic texture with no preferred grain orientation. Flat, rectangular dog-bone specimens were subjected to load-controlled, fully reversed fatigue for 50 cycles, during which the same region was sequentially mapped to track microstructural changes. After 10 cycles of loading deformation twins were observed. During tensile reloading detwinning or narrowing of those twinned regions occurred. After 20 cycles, detwinning ceased and residual twins remained in the material. SEM imaging revealed numerous surface slip traces after cyclic loading. EBSD-assisted slip trace analysis identified the activation of prismatic and pyramidal < c+a> slip systems during low-cycle fatigue. Site-specific scanning transmission electron microscopy (STEM) further revealed that deformation was also accommodated by basal < a> slip and the dissociation of < c+a> dislocations. Center-of-symmetry (COS) analysis confirmed that the dissociation of < c+a> dislocations resulted in the formation of I₁ intrinsic stacking faults after cyclic loading. These findings provide new insights into the complex interplay of dislocation mechanisms governing fatigue deformation in rare-earth-containing Mg alloys.

Cyclic deformation↗

DOE OSTI2025

Develop an efficient and cost-effective novel anaerobic digestion system producing high purity of methane from diverse waste biomass

This project focuses on developing an advanced, intensified anaerobic digestion system aimed at transforming the treatment and conversion of organic wastes into valuable products, specifically renewable natural gas. The motivation for this research stems from the limitations of conventional anaerobic digestion technologies, which often face challenges such as long retention times, high operational costs, and incomplete organic material degradation. The new technology called Intensified Versatile Anaerobic Digestion (IVAD), is developed to address these challenges by incorporating innovative reactors and processes that enhance the overall efficiency and output of anaerobic digestion. The significance of this project lies in its potential to revolutionize waste management practices and waste biomass utilization. The IVAD system integrates a hyperthermophilic anaerobic acidification reactor, a hydrothermal treatment (HTT) unit, and both thermophilic and mesophilic methanogenic reactors. This combination enables a higher rate of organic breakdown and energy recovery, resulting in faster processing times, reduced reactor sizes, and lower operational costs compared to traditional systems. Key data include an increase in methane productivity to 1.18 m 3 /m 3 /day, a significant improvement compared to the baseline technology’s 0.64 m 3 /m 3 /day. Additionally, the IVAD system achieves a 45% reduction in levelized cost of energy (LCOE), down to $\$$10.04/MMBTU, and an energy return on investment (EROI) of 3.19, representing an 87% increase over baseline levels. Technical and economic analyses highlight that the IVAD system significantly reduces hydraulic retention time (HRT) and solid retention time (SRT). The HRT for the HTT reactor can be reduced from 1 hour to 0.5 hours, while decoupling SRT from HRT in the anaerobic acidification reactor (AAR) allows for further reductions. These design optimizations lead to smaller reactor volumes, cutting down equipment and construction costs. Despite these advancements, energy consumption remains comparable to conventional methods due to a novel heat recovery strategy, enhancing overall process productivity. The system also achieves in-situ CO 2 removal and ammonia stripping features, resulting in biogas with a methane purity level of 75%, and produces high-quality nitrogen fertilizer as an additional by-product. Public benefits of the IVAD system are substantial, contributing to sustainable waste management and renewable energy production. By providing a scalable solution that can be adopted by dairy farms and similar agricultural operations, the IVAD system helps reduce waste, produce renewable natural gas (RNG) suitable for transportation fuel, and generate fertilizer, supporting a circular economy. This project plays a role in achieving broader environmental objectives by mitigating greenhouse gas emissions and promoting energy independence. Additionally, it offers a pathway for farmers to lower operational costs while adopting practices that are both environmentally sustainable and economically advantageous.

03 NATURAL GAS↗

DOE OSTI2025

Quantification of grain rotation in bulk nanostructured copper via in situ heating white beam synchrotron X-ray diffraction

Grain rotation during microstructural relaxation under heating is conventionally studied extensively through transmission electron microscopy and simulations. However, there is a shortage in examining grain rotations at larger length and volume scales in bulk materials. It is critical to understand the thermal stability of bulk nanostructured metals, since those enhanced mechanical properties have been well recognized. Here, this study aimed to employ a white beam microdiffraction X-ray technique under in situ heating from 300 K to 1073 K at 12 K/min on a nanostructured copper processed by high-pressure torsion, yielding an initial grain size of ∼260 nm before the heating. Evaluation across a wide range of temperatures reveals transition temperatures associated with microstructural relaxation processes. By tracking separate Laue diffraction peaks stemming from individual grains, changes in their orientations can be estimated and quantified. This approach becomes particularly effective when the number of grains within the probed volume is reasonably small. At temperatures above 940 K, about 7.5 % of Cu grains are rotating at speeds of ∼2 × 10 –3 °/s. The radial direction of the disk specimen is found to be the preferred direction of grain rotation, with the rotation axis along the shear direction. Further analysis found no correlation between peak intensity and peak size, related to grain sizes and deviatoric strain, respectively, with rotation conditions or speed. These findings demonstrate that the diffraction technique utilizing white beam X-rays is a complementary and novel characterization tool for understanding microstructural evolution, especially in grain rotations, of bulk crystalline materials.

Grain orientation↗

NASA NTRS2012

Long-Lasting Science Returns from the Apollo Heat Flow Experiments

The Apollo astronauts deployed geothermal heat flow instruments at landing sites 15 and 17 as part of the Apollo Lunar Surface Experiments Packages (ALSEP) in July 1971 and December 1972, respectively. These instruments continuously transmitted data to the Earth until September 1977. Four decades later, the data from the two Apollo sites remain the only set of in-situ heat flow measurements obtained on an extra-terrestrial body. Researchers continue to extract additional knowledge from this dataset by utilizing new analytical techniques and by synthesizing it with data from more recent lunar orbital missions such as the Lunar Reconnaissance Orbiter. In addition, lessons learned from the Apollo experiments help contemporary researchers in designing heat flow instruments for future missions to the Moon and other planetary bodies. For example, the data from both Apollo sites showed gradual warming trends in the subsurface from 1971 to 1977. The cause of this warming has been debated in recent years. It may have resulted from fluctuation in insolation associated with the 18.6-year-cycle precession of the Moon, or sudden changes in surface thermal environment/properties resulting from the installation of the instruments and the astronauts' activities. These types of reanalyses of the Apollo data have lead a panel of scientists to recommend that a heat flow probe carried on a future lunar mission reach 3 m into the subsurface, approx 0.6 m deeper than the depths reached by the Apollo 17 experiment. This presentation describes the authors current efforts for (1) restoring a part of the Apollo heat flow data that were left unprocessed by the original investigators and (2) designing a compact heat flow instrument for future robotic missions to the Moon. First, at the conclusion of the ALSEP program in 1977, heat flow data obtained at the two Apollo sites after December 1974 were left unprocessed and not properly archived through NASA. In the following decades, heat flow data from January 1975 through February 1976, as well as the metadata necessary for processing the data (the data reduction algorithm, instrument calibration data, etc.), were somehow lost. In 2010, we located 450 original master archival tapes of unprocessed data from all the ALSEP instruments for a period of April through June 1975 at the Washington National Records Center. We are currently extracting the heat flow data packets from these tapes and processing them. Second, on future lunar missions, heat flow probes will likely be deployed by a network of small robotic landers, as recommended by the latest Decadal Survey of the National Academy of Science. In such a scenario, the heat flow probe must be a compact system, and that precludes use of heavy excavation equipment such as a rotary drill for reaching the 3-m target depth. The new heat flow system under development uses a pneumatically driven penetrator. It utilizes a stem that winds out of a reel and pushes its conical tip into the regolith. Simultaneously, gas jets, emitted from the cone tip, loosen and blow away the soil. Lab experiments have demonstrated its effectiveness in lunar vacuum.

Nagihara, S.↗

NASA NTRS2015

Pathfinder Lander Rover Recharge System, and MARCO POLO Controls and ACME Regolith Feed System Controls and Integration

This project stems from the Exploration, Research, and Technology Directorate (UB) Projects Division, and one of their main initiatives is the "Journey to Mars". Landing on the surface of Mars which is millions of miles away is an incredibly large challenge. The terrain is covered in boulders, deep canyons, volcanic mountains, and spotted with sand dunes. The robotic lander is a kind of spacecraft with multiple purposes. One purpose is to be the protective shell for the Martian rover and absorb the impact from the landing forces; another purpose is to be a place where the rovers can come back to, actively communicate with, and recharge their batteries from. Rovers have been instrumental to the Journey to Mars initiative. They have been performing key research on the terrain of the red planet, trying to unlock the mysteries of the land for over a decade. The rovers that will need charging will not all have the same kind of internal battery either. RASSOR batteries may differ from the PbAC batteries inside Red Rover's chassis. NASA has invested heavily in the exploration of the surface of Mars. A driving force behind further exploration is the need for a more efficient operation of Martian rovers. One way is to reduce the weight as much as possible to reduce power consumption given the same mission parameters. In order to reduce the mass of the rovers, power generation, communication, and sample analysis systems currently onboard Martian rovers can be moved to a stationary lander deck. Positioning these systems from the rover to the Lander deck allows a taskforce of smaller, lighter rovers to perform the same tasks currently performed by or planned for larger rovers. A major task in transferring these systems to a stationary lander deck is ensuring that power can be transferred to the rovers.

Internship↗

DOE OSTI2025

Inkless, dry printing nanographene via in-Situ Coordinated laser ablation and sintering processes

Printing carbon, such as graphene and other carbon structures, for flexible and printed electronics currently relies on either ink-based printing, laser-induced forward transfer (LIFT), or laser-induced graphitization (LIG) to convert carbon-rich precursor materials, such as polymers, to graphene-like carbon structures. Liquid inks contain toxic solvents, surfactants, and stabilizing additives that degrade electrical conductivity and require high-temperature post-processing. On the other hand, LIG is limited by the substrate. Here, this study introduces an additive manufacturing method for dry-printing carbon nanomaterials, ranging from amorphous carbon to crystalline graphene-like structures, on various substrates. The system utilizes laser ablation of a solid graphite target to create pure carbon nanoparticles in situ and on demand. An inert gas carries the nanoparticles onto the substrate, where they can be deposited either as amorphous structures or laser-sintered in real time to form various graphitic structures. The study of laser processing parameters, specifically fluence and pulse repetition frequency, revealed three unique regimes of nanostructure evolution that influence the morphological and electrical properties of these printed structures. Raman spectroscopy confirmed graphitization with a resistivity slightly higher than that of the bulk graphite target. The conductivity/resistivity could be tuned as a function of sintering laser power. Scanning transmission electron microscopy (STEM) revealed that turbostratic nanographene formed with an interlayer spacing of 0.40 nm. Despite ink-based printing methods, such as screen printing, inkjet printing (IJP), and aerosol jet printing (AJP), this eco-friendly and green manufacturing technique could eliminate toxic chemicals, reduce environmental impact, and enable single-step fabrication of carbon-based devices for applications in wearable sensors, energy storage, flexible electronics, and Internet of Things (IoT) devices.

Additive nanomanufacturing↗