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All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Electron Microscopy Transfer System to Protect Atmosphere‐Sensitive Materials for Scanning Electron Microscopy Characterization

Atmosphere- and/or moisture-sensitive materials can be challenging to characterize using electron microscopy techniques due to sample preparation workflows that generally require exposure to ambient conditions. Here, we describe a novel preparation method that uses aluminum foil in combination with a commercial cryo-EM transfer system to circumvent undesired exposure to the atmosphere. First, hygroscopic MgCl 2 was used as a model material, and prepared samples (both protected and unprotected) were placed in a controlled-humidity environment (> 80% relative humidity) for various exposure lengths (circa seconds to hours). Following this, the effectiveness of the sample preparation method was determined by comparing qualitative photos and quantitative X-ray diffraction patterns between the two sample subsets. The combined results of these experiments suggest that the outlined preparation method effectively protects MgCl 2 from atmospheric contamination compared to MgCl 2 samples that had no protective measures taken. Finally, the preparation method was utilized to protect a highly hygroscopic crystalline BaO thin film for characterization via scanning electron microscopy, thereby demonstrating a functional application of the outlined preparation technique and an additional use for the commercial cryo-EM transfer system beyond its intended application.

atmosphere-sensitive materials↗
DOE OSTI2026

Quasi‐Steady State Supersaturation: Do High Values Derived From ESCAPE Represent Real High Supersaturations and the Potential for Condensational Invigoration?

Deep convective clouds were intensively sampled during the Experiment of Sea Breeze Convection, Aerosols, Precipitation, and Environment (ESCAPE) with coordinated flights of the NRC Convair-580 and SPEC Learjet. A total of 219 updraft core segments were sampled over coastal Texas and Louisiana under diverse meteorological conditions. Median updraft properties included widths of ∼1 km, velocities of 4.8 m s −1 , droplet number concentrations of ∼400 cm −3 , and liquid water contents of 0.9 g m −3 . The limitations of using the quasi-steady state approximation to derive supersaturations were explored. Supersaturation (S QSS ) estimated from in situ observations under a quasi-steady state assumption averaged 0.4% but occasionally exceeded 2%, with values >1% (high supersaturations) identified as statistical outliers. Two case studies illustrated the conditions linked to high supersaturations. In a storm over the Gulf, median core S QSS reached 2.46% in the developing stage compared to 2.17% in the mature stage under similar thermodynamic conditions. In a storm over coastal Louisiana, S QSS peaked near 11% within a 13.7-m s −1 updraft, accompanied by predominantly supercooled liquid droplets at −13°C and exceptionally low diameter concentrations of 0.29 mm cm −3 . Bootstrap analysis of all sampled cores showed that high supersaturations are most probable in cold and mixed-phase regimes with moderate to strong updrafts and are strongly influenced by vertical velocity and droplet number concentrations. In conclusion, while extreme supersaturations (∼10%) were rare, their occurrence underscores the need for targeted multiplatform observations to resolve their spatiotemporal variability and assess their potential role in deep convective invigoration.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRSDate not supplied

The Scientific Significance of Potential Samples From the Jezero Crater Rim

The Mars 2020 Perseverance rover has been exploring Jezero crater, Mars to characterize the geology,assess the potential for rocks to represent ancient habitable environments and/or preserve biosignatures, and collect a suite of scientifically compelling samples for return to Earth (Farleyet al.,2020).Thus far, Perseverance has collected samples that represent the diversity of igneous materials encountered on the crater floor and a suite of aqueously deposited sedimentary rocks from the fanand margin units(Simon et al., 2023; Bosak et al., 2024). When the rover ascendsthe crater rimit will encounter rocktypesthat are not included in the current sample cache. These include rocks fromthe Noachian whose mineralogical, geochemical, and geochronological recordswould greatly expand our understanding of early Mars. Some of the exposures are understood to come from subsurface aquifers that may represent the most ancient potentially habitablesubsurfaceenvironmentson Mars(Ehlmann et al., 2024). Samples ofthese rocks will add uniquescientific value tothe sample cache and to the Mars sample returnprogramby addressing outstanding questions in Mars science including potential habitability and how the climate and the interior of the planet evolved through time.

Mars 2020↗
DOE OSTI2020

Preliminary Test Design and Plan for a Canister Deposition Field Demonstration

This report provides a high-level test plan for deploying three commercial 32PTH2 spent nuclear fuel (SNF) canisters inside NUHOMS Advanced Horizontal Storage Modules (AHSM) from Orano (formerly Transnuclear Inc.). The details contained in this report represent the best designs and approaches explored for testing as of this publication. Given the rapidly developing nature of this test program, some of these plans may change to accommodate new objectives or adapt in response to conflicting requirements. The goal of the testing is to collect highly defensible and detailed surface deposition measurements from the surface of dry storage systems in a marine coastal environment to guide chloride-induced stress corrosion crack (CISCC) research. To facilitate surface sampling, the otherwise highly prototypic dry storage systems will not contain SNF but rather will be electrically heated to mimic the thermal-hydraulic environment. Instrumentation throughout the canister, storage module, and environment will provide an extensive amount of information for the use of model validation. Manual sampling over a comprehensive portion of the canister surface at regular time intervals will offer a high-fidelity quantification of the conditions experienced in a harsh yet realistic environment.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2021

Status Update for the Canister Deposition Field Demonstration

This report updates the high-level test plan for evaluating surface deposition on three commercial 32PTH2 spent nuclear fuel (SNF) canisters inside NUTECH Horizontal Modular Storage (NUHOMS) Advanced Horizontal Storage Modules (AHSM) from Orano (formerly Transnuclear Inc.) and provides a description of the surface characterization activities that have been conducted to date. The details contained in this report represent the best designs and approaches explored for testing as of this publication. Given the rapidly developing nature of this test program, some of these plans may change to accommodate new objectives or requirements. The goal of the testing is to collect highly defensible and detailed surface deposition measurements from the surface of dry storage canisters in a marine coastal environment to guide chloride-induced stress corrosion crack (CISCC) research. To facilitate surface sampling, the otherwise highly prototypic dry storage systems will not contain SNF but rather will be electrically heated to mimic the thermal-hydraulic-environment. Instrumentation throughout the canister, storage module, and environment will provide an extensive amount of information for the use of model validation. Manual sampling over a comprehensive portion of the canister surface at regular time intervals will offer a high-fidelity quantification of the conditions experienced in a harsh yet realistic environment.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2021

Rapid estimation of photosynthetic leaf traits of tropical plants in diverse environmental conditions using reflectance spectroscopy

Tropical forests are one of the main carbon sinks on Earth, but the magnitude of CO 2 absorbed by tropical vegetation remains uncertain. Terrestrial biosphere models (TBMs) are commonly used to estimate the CO 2 absorbed by forests, but their performance is highly sensitive to the parameterization of processes that control leaf-level CO 2 exchange. Direct measurements of leaf respiratory and photosynthetic traits that determine vegetation CO 2 fluxes are critical, but traditional approaches are time-consuming. Reflectance spectroscopy can be a viable alternative for the estimation of these traits and, because data collection is markedly quicker than traditional gas exchange, the approach can enable the rapid assembly of large datasets. However, the application of spectroscopy to estimate photosynthetic traits across a wide range of tropical species, leaf ages and light environments has not been extensively studied. Here, we used leaf reflectance spectroscopy together with partial least-squares regression (PLSR) modeling to estimate leaf respiration ( R dark25 ), the maximum rate of carboxylation by the enzyme Rubisco ( V cmax25 ), the maximum rate of electron transport ( J max25 ), and the triose phosphate utilization rate ( T p25 ), all normalized to 25°C. We collected data from three tropical forest sites and included leaves from fifty-three species sampled at different leaf phenological stages and different leaf light environments. Our resulting spectra-trait models validated on randomly sampled data showed good predictive performance for V cmax25 , J max25 , T p25 and R dark25 (RMSE of 13, 20, 1.5 and 0.3 μmol m -2 s -1 , and R 2 of 0.74, 0.73, 0.64 and 0.58, respectively). The models showed similar performance when applied to leaves of species not included in the training dataset, illustrating that the approach is robust for capturing the main axes of trait variation in tropical species. We discuss the utility of the spectra-trait and traditional gas exchange approaches for enhancing tropical plant trait studies and improving the parameterization of TBMs.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS2026

Assessing the Adhesion of Nanofibrous PVDF-HFP as Passive Thermal Control Coatings for the Extraterrestrial Storage of Cryogenic Propellants

Cryogenic propellant passive thermal management techniques in space are essential complements to active thermal management methods, helping reduce absolute dependence on the latter. Particularly, materials with superior optical properties (high solar reflectance and infrared emittance) would be beneficial for passive thermal control to reject most of the incident solar radiation and enhance thermal emission from the storage tank, leading to self-cooling. We developed a nanofibrous, porous passive thermal control material by electrospinning polyvinylidene fluoride-co-hexafluoropropylene (PVDF-HFP) co-polymer onto an aluminum foil substrate. The material exhibits a very high solar reflectance (>99%) and infrared emittance (~86%) when characterized in the ultraviolet-visible-near infrared and mid-infrared wavelengths. This study focuses on the adhesion of the nanofibrous PVDF-HFP to the substrate. We incorporated in-lab fabricated and commercial adhesives, under normal room conditions, between the nanofibers and the aluminum foil substrate to improve their adhesion. Some samples were also exposed to space-like conditions – vacuum and thermal cycling, to investigate their effects on the strengths of adhesives. Subsequently, adhesion peel tests were conducted on all the samples to assess the peel strengths of the bonds. Peel test strengths after space environment conditioning of the adhesives were generally higher than those observed in the pristine, unaged samples. The results are discussed in this study.

Chieloka Ibekwe↗
NASA NTRS2024

Space Environmental Exposure of the MISSE 9-15 Polymers and Composites Experiment 1-4 (PCE 1-4)

Spacecraft in low Earth orbit (LEO) are subjected to harsh environmental conditions, including radiation (cosmic rays, ultraviolet (UV), x-ray and charged particle radiation), micrometeoroids and orbital debris, temperature extremes, thermal cycling, and atomic oxygen (AO). These environmental exposures can result in erosion, embrittlement and optical property degradation of susceptible materials threatening spacecraft performance and durability. To increase our understanding of effects such as AO erosion and radiation induced embrittlement of spacecraft materials, NASA Glenn Research Center has developed a series of experiments that were flown as part of the Materials International Space Station Experiment (MISSE) missions on the exterior of the International Space Station (ISS). These experiments have provided critical space environmental durability data such as AO erosion data of polymers and composites, and radiation induced mechanical property degradation of spacecraft insulation materials, after long term space exposure. Recently, four Glenn experiments with 365 flight samples were flown on ISS’s MISSE-Flight Facility (MISSE-FF). These experiments are the Polymers and Composites Experiment-1 (PCE-1) flown as part of the MISSE-9 mission, the PCE-2 flown as part of the MISSE-10 mission, the PCE-3 flown as part of the MISSE-12 and MISSE-15 missions, and the PCE-4 flown as part of the MISSE-13 mission. This paper provides details on the space environment exposure of Glenn’s PCE 1-4 flight samples. Passive samples were flown in each flight orientation for post-flight AO fluence determination and on-orbit contamination analyses. Solar exposure estimates were computed by Aegis Aerospace, Inc. The environment exposure details include the total space vacuum duration, time on the MISSE-FF, the direct space exposure duration, the AO fluence and the computed mission Equivalent Sun Hours (ESH) solar exposure. Typical on-orbit temperatures are also provided along with a summary of analyses of PCE 1-4 contamination witness samples. Knowledge of the space environmental exposure of the PCE 1-4 flight samples is crucial for flight data interpretation.

Atomic oxygen↗
NASA NTRS1977

Voyager electronic parts radiation program, volume 1

The Voyager spacecraft is subject to radiation from external natural space, from radioisotope thermoelectric generators and heater units, and from the internal environment where penetrating electrons generate surface ionization effects in semiconductor devices. Methods for radiation hardening and tests for radiation sensitivity are described. Results of characterization testing and sample screening of over 200 semiconductor devices in a radiation environment are summarized.

Stanley, A. G.↗
NASA NTRS1984

Effect of space exposure of some epoxy matrix composites on their thermal expansion and mechanical properties (A0138-8)

This experiment has three objectives. The first and main objective is to detect a possible variation in the coefficient of thermal expansion of composite samples during a 1-year exposure to the near-Earth orbital environment. A second objective is to detect a possible change in the mechanical integrity of composite products, both simple elements and honeycomb sandwich assemblies. A third objective is to compare the behavior of two epoxy resins commonly used in space structural production. The experimental approach is to passively expose samples of epoxy matrix composite materials to the space environment and to compare preflight and postflight measurements of mechanical properties. The experiment will be located in one of the three FRECOPA (French cooperative payload) boxes in a 12-in.-deep peripheral tray that contains nine other experiments from France. The FRECOPA box will protect the samples from contamination during the launch and reentry phases of the mission. The coefficients of thermal expansion are measured on Earth before and after space exposure.

Elberg, R.↗
NASA NTRS2004

The In-Space Soldering Investigation: Research Conducted on the International Space Station in Support of NASA's Exploration Initiative

Soldering is a well established joining and repair process that is of particular importance in the electronics industry. Still. internal solder joint defects such as porosity are prevalent and compromise desired properties such as electrical/thermal conductivity and fatigue strength. Soldering equipment resides aboard the International Space Station (ISS) and will likely accompany Exploration Missions during transit to, as well as on, the moon and Mars. Unfortunately, detrimental porosity appears to be enhanced in lower gravity environments. To this end, the In-Space Soldering Investigation (ISSI) is being conducted in the Microgravity Workbench Area (MWA) aboard the ISS as "Saturday Science" with the goal of promoting our understanding of joining techniques, shape equilibrium, wetting phenomena, and microstructural development in a microgravity environment. The work presented here will focus on direct observation of melting dynamics and shape determination in comparison to ground-based samples, with implications made to processing in other low-gravity environments. Unexpected convection effects, masked on Earth, will also be shown as well as the value of the ISS as a research platform in support of Exploration Missions.

Grugel, R. N.↗
NASA NTRS2006

The In-Space Soldering Investigation: To Date Analysis of Experiments Conducted on the International Space Station

Soldering is a well established joining and repair process that is of particular importance in the electronics industry. Still, internal solder joint defects such as porosity are prevalent and compromise desired properties such as electrical/thermal conductivity and fatigue strength. Soldering equipment resides aboard the International Space Station (ISS) and will likely accompany Exploration Missions during transit to, as well as on, the moon and Mars. Unfortunately, detrimental porosity appears to be enhanced in lower gravity environments. To this end, the In-Space Soldering Investigation (ISSI) is being conducted in the Microgravity Workbench Area (MWA) aboard the ISS as "Saturday Science" with the goal of promoting our understanding of joining techniques, shape equilibrium, wetting phenomena, and microstructural development in a microgravity environment. The work presented here will focus on direct observation of melting dynamics and shape determination in comparison to ground-based samples, with implications made to processing in other low-gravity environments. Unexpected convection effects, masked on Earth, will also be shown as well as the value of the ISS as a research platform in support of Exploration Missions.

Grugel, Richard N.↗
NASA NTRS1994

Surface characterization through shape oscillations of drops in microgravity and 1-g

The goal of these experiments is to determine the rheological properties of liquid drops of single or multiple components in the presence or absence of surface active materials by exciting drops into their quadrupole resonance and observing their free decay. The resulting data coupled with appropriate theory should give a better description of the physics of the underlying phenomena, providing a better foundation than earlier empirical results could. The space environment makes an idealized geometry available (spherical drops) so that theory and experiment can be properly compared, and allows a 'clean' environment, by which is meant an environment in which no solid surfaces come in contact with the drops during the test period. Moreover, by considering the oscillations of intentionally deformed drops in microgravity, a baseline is established for interpreting surface characterization experiments done on the ground by other groups and ours. Experiments performed on the United States Microgravity Laboratory Laboratory (USML-1) demonstrated that shape oscillation experiments could be performed over a wide parameter range, and with a variety of surfactant materials. Results, however, were compromised by an unexpected, slow drop tumbling, some problems with droplet injection, and the presence of bubbles in the drop samples. Nevertheless, initial data suggests that the space environment will be useful in providing baseline data that can serve to validate theory and permit quantitative materials characterization at 1-g.

Apfel, Robert E.↗
NASA NTRS2005

Cutting Silica Aerogel for Particle Extraction

The detailed laboratory analyses of extraterrestrial particles have revolutionized our knowledge of planetary bodies in the last three decades. This knowledge of chemical composition, morphology, mineralogy, and isotopics of particles cannot be provided by remote sensing. In order to acquire these detail information in the laboratories, the samples need be intact, unmelted. Such intact capture of hypervelocity particles has been developed in 1996. Subsequently silica aerogel was introduced as the preferred medium for intact capturing of hypervelocity particles and later showed it to be particularly suitable for the space environment. STARDUST, the 4th NASA Discovery mission to capture samples from 81P/Wild 2 and contemporary interstellar dust, is the culmination of these new technologies. In early laboratory experiments of launching hypervelocity projectiles into aerogel, there was the need to cut aerogel to isolate or extract captured particles/tracks. This is especially challenging for space captures, since there will be many particles/tracks of wide ranging scales closely located, even collocated. It is critical to isolate and extract one particle without compromising its neighbors since the full significance of a particle is not known until it is extracted and analyzed. To date, three basic techniques have been explored: mechanical cutting, lasers cutting and ion beam milling. We report the current findings.

Tsou, P.↗
NASA NTRS1983

Spacecraft contamination environment; Proceedings of the Meeting, Arlington, VA, May 4-6, 1982

Aspects of IECM debriefing are considered, taking into account preliminary results of the induced environment contamination monitor measurements of STS-2, the humidity monitor and dew point hygrometer, the induced environment contamination monitor cascade impactor, the optical effects module and passive sample array, temperature-controlled quartz crystal microbalance measurements on STS-2, camera/photometer results, the mass spectrometer, and a summary regarding the induced environment contamination monitor/space transport system. Other subjects explored are related to contamination management and control, contamination/optical degradation, and contamination assessments and measurements. Attention is given to approaches for controlling contamination before launch, the coronagraph as the ultimate device to monitor orbiting particulates in the Space Transport System environment, and the contamination sensitivity of typical mirror coatings.

Maag, C. R.↗
DOE OSTI2021

ATHENA: A unique radiation environment platform at the National Ignition Facility

This paper describes the ATHENA platform, an energy tuning assembly, which was developed to spectrally shape the National Ignition Facility (NIF) deuterium–tritium fusion neutron source to a thermonuclear (fusion) plus prompt fission neutron spectrum with a capability to act as a short-pulse neutron source. This unique, otherwise inaccessible radiation environment complements existing experimental facilities and capabilities. Here, the flexible ATHENA irradiation positions were modeled using an ensemble of Monte Carlo simulations with stochastic sampling of the nuclear cross-sections to characterize the radiation environments and uncertainty for the platform. Validation of the internal neutron spectrum produced from fielding ATHENA at NIF occurred through neutron flux unfolding with 20 measured activation products.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
NASA NTRS2022

Sample Materials Considerations for Curating and Processing Pristine MSR Samples

The perseverance rover is collecting and caching samples of Mars as part of the Mars 2020 mission, which represents the first leg of a multi-mission Mars Sample Return Campaign. The MSR Campaign is an international partnership that will result in delivery of the first martian samples to Earth that were not delivered through meteoritic infall. All meteorites, regardless of how they were handled from recovery to curation, have experienced uncontrolled entry and exposure to the terrestrial environment. Whilst meteorite deliveries are serendipitous, they are also unplanned events that require reactionary responses for recovery and curation. However, with the direct return of pristine astromaterials from another body, we are afforded the ability to design a facility in advance of sample delivery to keep those samples in a pristine (i.e., as returned) state for an indefinite period of time. Given that the curation and processing infrastructure needs to be made out of something, it is important to choose materials for the pristine curation environment that will optimize between the need to effectively process samples and the need to minimize contamination of the samples. The Johnson Space Center (JSC) has an optimized list of materials that have been used in previous sample return missions that includes 304/316 Stainless Steel, Teflon, and T6061 Aluminum (1). This set of materials are compatible with inorganic, organic, and biological cleanliness requirements and protocols. Furthermore, only these materials are permitted to come in contact with pristine samples. We note that JSC uses Neoprene and Hypalon for the gloves on their gloveboxes, but the glove material never comes in direct contact with the samples, only the approved materials. The MSR sample tubes will be made of Ti, so Ti may be an acceptable material for making tools, but the minor and trace element abundances of 304 and 316 stainless steel are well known and do not inhibit scientific investigations of metals, including HSE (2). More work is needed to determine whether the same is true for Ti alloys. In addition to defining the materials in the pristine environment, one must also choose whether the pristine environment will be under vacuum or under a specific atmospheric composition and pressure. Although JAXA has successfully implemented pristine curation vacuum chambers for their Hayabusa and Hayabusa2 samples (3), a vacuum environment is not appropriate for martian samples because it may drive deliquescence of mineral phases in the samples that are sensitive to pressure and relative humidity (4). Consequently, the pristine environment for the martian samples should be under an inert gas. It will be crucial to minimize the number of gases that come into direct contact with samples and these gases will need to be high purity and consistent throughout the pristine isolators. Samples at JSC are stored under high purity gaseous nitrogen (1). Dry N2 gas has not been a problem for N isotope studies for high-T release phases, but an additional inert atmosphere like Ar may be needed for samples where there is a particular concern about low-T release of N from bulk sample analysis. References: (1) McCubbin FM, et al. (2019) Space Science Reviews, 215, 1-81. (2) Day JMD, et al. (2018) Meteorit. Planet. Sci. 53:1283-1291. (3) Yada, T., et al., (2014). Meteorit. Planet. Sci. 49, 135-153. (4) Tosca NJ, et al. (2021). Astrobiology, in press, doi:10.1089/ast.2021.0115.

F M McCubbin↗
DOE OSTI2022

How galaxies populate halos in extreme density environments: An analysis of the halo occupation distribution in SDSS

Recent works have shown that the properties of galaxy populations in simulated dark matter halos vary with large-scale environments. These results suggest a variation in the halo occupation distribution (HOD) in extreme density environments since the dynamical and astrophysical conditions prevailing in these regions may significantly affect the formation and evolution of their halos and residing galaxies, influencing the mean number of satellite galaxies. To analyse these effects, we identify cosmic voids and future virialised structures (FVS) in the Sloan Digital Sky Server Data Release 12 (SDSS-DR12) and estimate the HOD within these super-structures using group catalogues as dark matter halo proxies. Our goal is to use observational galaxy data to characterise the HOD within cosmic voids and FVS, explore the different properties of these galaxies populations and compare them with the general results outside these super-structures. We use a publicly available observational galaxy catalogue with information on redshifts, positions, magnitudes and other astrophysical features to build a volume complete galaxy sample and identify cosmic voids and FVS. Using a publicly available galaxy group catalogue as a proxy to dark matter halos, we compute the HOD within both types of super-structures for different absolute magnitude thresholds. We also study the dependence on the results on the main void and FVS properties, density and volume. We also analysed the main characteristics of the stellar content of galaxies inside these extreme-density regions such as the mean stellar age and the galaxy light concentration index. In all cases, we compare the results with those derived from the Field sample, defined by objects outside both types of environments. Inside cosmic voids, we find a strong decrease in HOD concerning the Field results. In the most extreme cases, the mean number of satellites fall to ~ 50%. Inside FVS, the HOD shows a significant increase to the Field, with a ~ 40% excess in the mean number of satellites. These results are present for the different galaxy luminosity ranges explored. In both environments, the differences with respect to the Field increases for the extreme values of the density environments. However, we obtain no signs of variations related to intrinsic characteristics of the super-structures, indicating that the effects depend mainly on the density of the large-scale environment. In addition, we find that the cumulative distribution of the mean age of stars of the central galaxy also varies in the different regions, this suggests that the history of the formation of the dark matter halos may be different. Finally, we explore the HOD for the 25% youngest (oldest) galaxies, based on the mean age of their stars. We find that for the low-mass groups the youngest galaxies are only present inside voids and are generally central galaxies. On the other hand, for the high-mass groups the FVS environments show the same increase in the HOD concerning the Field as previously mentioned. We find that cosmic voids lack a significant fraction of galaxies with the oldest stellar population.

79 ASTRONOMY AND ASTROPHYSICS↗