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All sources NASA NTRS DOE OSTI

DOE OSTI2022

Understanding Fission Gas Bubble Distribution and Zirconium Redistribution in Neutron-irradiated U-Zr Metallic Fuel Using Machine Learning

U-10wt.% Zr (U-10Zr) based metallic fuel is the leading candidate for next-generation sodium cooled fast reactor in United States. Currently, Idaho National Laboratory (INL) has been the leading national laboratory for research, development, and demonstration (RD&D) on metallic fuel. Advanced post-irradiation characterization will help to understand fuel microstructure and property change during irradiation, benefiting fuel qualification for commercial application. Characterization capabilities ranging from sub-nanometer to micrometer, such as scanning electron microscopy (SEM), focused ion beam (FIB) sampling, transmission electron microscopy (TEM) characterization, and local thermal conductivity microscopy (TCM), have been utilized recently on irradiated U-10Zr fuel samples to gain a better understanding of nuclear fuel microstructure and property evolution inside a reactor. The FIB/SEM coupled with energy dispersive X-ray spectroscopy (EDS) can capture the essential information to achieve better understanding of fuel behaviors. Inside a nuclear reactor, the phase and microstructure of U-10Zr is constantly changing under neutron bombardment. For example, the gaseous fission product atoms have a limited solubility inside fuel matrix and tend to precipitate out in bubble form, which not only contribute to fuel thermal conductivity degradation but also provide a shortcut for movement of fission products, i.e. lanthanides. The resultant deposition of lanthanides at the cladding inner surface will potentially trigger a chemical reaction/interaction between nuclear fuel and cladding at reactor operational conditions, threatening fuel integrity and safety. FIB/SEM coupled with EDS can provide the fission bubble information as well as probe into phase separation or Zr redistribution, which is fundamental to predict the fuel performance. With high velocity image data generating method, such as FIB/SEM, an automatic way to extract the microstructural information quantitively can better serve the needs from post irradiation characterization. A trained machine learning model, named Decision Tree, is employed to generate a bubble classifier and to categorize bubbles into three categories: isolated bubble, connected without lanthanides, and connected with lanthanides bubbles[3]. This work presents a showcase of this approach on six regions of a fuel cross-section along the radial temperature gradient. We obtained distributions of bubble categories and porosity rates along the six regions. Moreover, a secondary phase U-Zr2 was determined and found on regions 5 and 6. The secondary phase fraction was increasing from 15.61% in region 5 to 34.79% in region 6 based on this approach . This quantitative data offers insights into the lanthanide migration and potentially thermal conductivity degradation. This information from machine learning will be fed into fuel design code for better prediction of fuel performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1998

Evidence of Microfossils in Carbonaceous Chondrites

Investigations have been carried out on freshly broken, internal surfaces of the Murchison, Efremovka and Orgueil carbonaceous chondrites using Scanning Electron Microscopes (SEM) in Russia and the Environmental Scanning Electron Microscope (ESEM) in the United States. These independent studies on different samples of the meteorites have resulted in the detection of numerous spherical and ellipsoidal bodies (some with spikes) similar to the forms of uncertain biogenicity that were designated "organized elements" by prior researchers. We have also encountered numerous complex biomorphic microstructures in these carbonaceous chondrites. Many of these complex bodies exhibit diverse characteristics reminiscent of microfossils of cyanobacteria such as we have investigated in ancient phosphorites and high carbon rocks (e.g. oil shales). Energy Dispersive Spectroscopy (EDS) analysis and 2D elemental maps shows enhanced carbon content in the bodies superimposed upon the elemental distributions characteristic of the chondritic matrix. The size, distribution, composition, and indications of cell walls, reproductive and life cycle developmental stages of these bodies are strongly suggestive of biology' These bodies appear to be mineralized and embedded within the meteorite matrix, and can not be attributed to recent surface contamination effects. Consequently, we have interpreted these in-situ microstructures to represent the lithified remains of prokaryotes and filamentous cyanobacteria. We also detected in Orgueil microstructures morphologically similar to fibrous kerite crystals. We present images of many biomorphic microstructures and possible microfossils found in the Murchison, Efremovka, and Orgueil chondrites and compare these forms with known microfossils from the Cambrian phosphate-rich rocks (phosphorites) of Khubsugul, Northern Mongolia.

Hoover, Richard B.↗

DOE OSTI2021

Impact of Controlled Storage Conditions on the Hydrolysis and Surface Morphology of Amorphous-UO 3

The hydration and morphological effects of amorphous (A)-UO 3 following storage under varying temperature and relative humidity have been investigated. This study provides valuable insight into U-oxide speciation following aging, the U-oxide quantitative morphological data set, and, overall, the characterization of nuclear material provenance. A-UO 3 was synthesized via the washed uranyl peroxide synthetic route and aged based on a 3-factor circumscribed central composite design of experiment. Target aging times include 2.57, 7.00, 14.0, 21.0, and 25.4 days, temperatures of 5.51, 15.0, 30.0, 45.0, and 54.5 °C, and relative humidities of 14.2, 30.0, 55.0, 80.0, and 95.8% were examined. Following aging, crystallographic changes were quantified via powder X-ray diffraction and an internal standard Rietveld refinement method was used to confirm the hydration of A-UO 3 to crystalline schoepite phases. The particle morphology from scanning electron microscopy images was quantified using both the Morphological Analysis of MAterials software and machine learning. Results from the machine learning were processed via agglomerative hierarchical clustering analysis to distinguish trends in morphological attributes from the aging study. Significantly hydrated samples were found to have a much larger, plate-like morphology in comparison to the unaged controls. Predictive modeling via a response surface methodology determined that while aging time, temperature, and relative humidity all have a quantifiable effect on A-UO 3 crystallographic and morphological changes, relative humidity has the most significant impact.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Performance of biochar assisted catalysts during hydroprocessing of non-edible vegetable oil: Effect of transition metal source on catalytic activity

Biochar-supported catalysts were developed from nickel (Ni) - and cobalt (Co)- nitrates and hydroxides and tested for the hydrotreatment of carinata oil. Nitrate-based (from water-soluble salts) and hydroxide-based (from water-insoluble salts) catalysts of Ni and Co were prepared via wetness impregnation and aqueous dispersion methods, respectively. The catalysts were characterized using various tools such as, confocal XRF, BET specific surface area analyzer, NH3-TPD, and SEM-EDS. Synchroton method showed nitrate-sourced metals were dispersed mostly in the pores while, the hydroxide-sourced metals were distributed mainly on the catalyst surface. C = C saturation and cracking of triglycerides, decarboxylation, and hydrogenation of aromatic structures appeared to be dominant on the hydroxides of transition metals, hence took place on catalyst surface. Methanation and dehydrogenation (thus aromatization), however, seemed to be a pore phenomenon, catalyzed more over nitrate-based catalysts. A reaction network was proposed based on chemical analysis of upgraded carinata oil and erucic acid model compound. Catalytic cracking followed by hydrotreatment performed better in terms of fuel properties than other approaches in this study.

Biochar catalysts↗

NASA NTRS2014

Pu'u Poli'ahu, Mauna Kea: A Possible Analog for the Hematite Bearing Layer Located in Gale Crater, Mars.

Hyperspectral data detected by the Compact Reconnaissance Imaging Spectrometer for Mars (CRISM) on board Mars Reconnaissance Orbiter (MRO) indicated the presence of a hematite bearing ridge on Mount Sharp situated in the Gale Crater, Mars. [Fraeman]. The presence of this mineral in high concentrations is indicative of possible aqueous origins. [Fraeman] In 2012, Curiosity Rover landed in Gale Crater on Mars. Curiosity's mission is to determine Mars' habitability and is equipped with an advanced suite of scientific instruments that are capable of conducting analyses on rocks and soil. The hematite bearing ridge on Mount Sharp is thought to be a good candidate of study for Curiosity. To better understand this type of terrain, the study of analog sites similar in geologic setting is of great importance. One site thought to be a comparable analog is a cinder cone called Pu'u Poli'ahu located on the summit of Mauna Kea, Hawaiʻi. Poli'ahu is unique among the tephra cones of Mauna Kea because it is thought to have formed in subaqueous conditions approximately 170,000 to 175,000 years ago. [Porter] Consequently located on the inner flanks of Poli'ahu is a rock outcrop that contains hematite. Samples were collected from the outcrop and characterized using the following instruments: Digital Microscope, Panalytical X‐ray diffraction (XRD), and scanning electron microscope (SEM). The initial preparation of the rocks involved documenting each sample by creating powdered samples, thick sections, and photo documentation.

Adams, M. E.↗

DOE OSTI2022

Characterizing how size distribution and concentration affect echogenicity of ultrasound contrast agents

Here, we investigated the effects of UCA gas bubble size distribution and concentration on the generated ultrasound echogenicity signal. Gas bubble size characterization using Coulter Counter and cryogenic-SEM revealed the hollow structure and rare presence of microbubbles >10 µm in a commercial UCA product, Lumason™. Volume-weighed size and concentration were observed to be more sensitive to changes in UCA bubble stability than number-weighted size and concentration. Size distribution measurements showed that the force (e.g., shaking/agitation energy) used to redisperse the sample did not affect the size distribution, concentration, or echogenicity of the UCA sample. The ultrasound backscattering coefficient (BSC) of size fractionated and serial diluted microbubbles showed that the echogenicity signal correlates most with UCA bubble concentration, especially volume-weighted concentration. Findings from this study may be used to support demonstrating the equivalence of a generic UCA product to the reference listed drug.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2020

The effects of heat treatment on the response of WE43 Mg alloy: crystal plasticity finite element simulation and SEM-DIC experiment

The present report addressed the effects of heat treatment on the mechanical response of a WE43 Mg alloy using an integrated framework of SEM-DIC experiment and CPFE simulation. Both macroscopic responses including yield strength, ultimate strength, ductility, and microscopic responses, including local displacement and strain maps, were experimentally investigated. The focus of this work is to use the CPFE simulation as an integrated computational tool to study the effects of heat treatment. The CPFE framework was evaluated using the local fields of displacement and strain obtained from the SEM-DIC experiment rather than the conventional scheme of using macroscopic responses at different loading directions. Subsequently, the information which is available using CPFE, such as the critical resolved shear stress (CRSS) and relative slip activity, was used to study the effects of heat treatment on the response of WE43 Mg alloy. The contributions of different strengthening mechanisms on the CRSS were addressed. The results show that effects of heat treatment can be captured using the predominant mechanisms of the grain size effect and the influence of precipitates. Finally, it has been shown that classical Hall-Petch in which one constant can capture the size effects, should be modified. To do so, each deformation mode should have a unique Hall-Petch constant, which are calculated here for the WE43 Mg alloy.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Reversible assembly of silica nanoparticles at water–hydrocarbon interfaces controlled by SDS surfactant

Achieving reversible and tunable assembly of silica nanoparticles at liquid–liquid interfaces is vital for a wide range of scientific and technological applications including sustainable subsurface energy applications, catalysis, drug delivery and material synthesis. In this study, we report the mechanisms controlling the assembly of silica nanoparticles (dia. 50 nm and 100 nm) at water–heptane and water–toluene interfaces using sodium dodecyl sulfate (SDS) surfactant with concentrations ranging from 0.001–0.1 wt% using operando ultrasmall/small-angle X-ray scattering, cryogenic scanning electron microscopy imaging and classical molecular dynamics simulations. The results show that the assembly of silica nanoparticles at water–hydrocarbon interfaces can be tuned by controlling the concentrations of SDS. Silica nanoparticles are found to: (a) dominate the interfaces in the absence of interfacial SDS molecules, (b) coexist with SDS at the interfaces at low surfactant concentration of 0.001 wt% and (c) migrate toward the aqueous phase at a high SDS concentration of 0.1 wt%. Energetic analyses suggest that the van der Waals and electrostatic interactions between silica nanoparticles and SDS surfactants increase with SDS concentration. However, the favorable van der Waals and electrostatic interactions between the silica nanoparticles and toluene or heptane decrease with increasing SDS concentration. As a result, the silica nanoparticles migrate away from the water–hydrocarbon interface and towards bulk water at higher SDS concentrations. These calibrated investigations reveal the mechanistic basis for tuning silica nanoparticle assembly at complex interfaces.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2022

Origin, parameters, and underlying deformation mechanisms of propagating deformation bands in irradiated 316L stainless steel

Lüders-type propagating deformation bands were observed in specimens of irradiated 316L stainless steel samples removed from Spallation Neutron Source target vessels after service. Mechanical testing with digital image correlation (DIC) and in-situ tensile testing with scanning electron microscopy electron backscatter diffraction showed that the observed Lüders-type behavior was not related to the known transformation-induced plasticity or twinning-induced plasticity behavior. Instead, the phenomenon occurs at small local strain values before a significant amount of martensite or deformation twins appear in the microstructure. Microstructural analysis and in-situ mechanical test results suggest Lüders-type band formation and propagation were related to the appearance and evolution of defect-free channels—analogous to slip bands. A modified Swift equation with a Ludwigson-like component was offered to rationalize the phenomenon and model the strain-softening processes at small strain values. Finally, the results indicate complex microstructural processes and deformation mechanisms were active at small strain values and underline the benefits of advanced mechanical test approaches such as DIC.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Morphological Characterization of Uranyl Fluoride Particles via Atomic Force Microscopy

Uranium hexafluoride (UF 6 ) undergoes a rapid hydrolysis reaction when exposed to atmospheric water. In addition to producing hazardous HF gas, the hydrolysis reaction produces uranyl fluoride (UO 2 F 2 ), a radioactive solid phase particulate material. Because of the technological utility of UF 6 in the nuclear fuel cycle, understanding the transport properties of UO 2 F 2 aerosol produced via UF 6 hydrolysis is important for accident scenarios. Moreover, the fundamental chemical and physical properties of the UF 6 hydrolysis reaction are not completely understood. Recently, several experiments on the aerosol phase properties of UO 2 F 2 produced in this way have shown that under most relevant conditions, the particle size distribution (PSD) of UO 2 F 2 can be extremely small, approximately 3 to 5 nm, which is well below the threshold that can be routinely observed via scanning electron microscopy (SEM). Although readily observable in the aerosol phase, observation of nanometer-sized particles in the condensed phase (i.e. deposited on surfaces) remains a challenge. Here, in this study, we have used atomic force microscopy (AFM) to study the PSD and morphological characteristics of UO 2 F 2 deposited at low and high concentrations under different humidity conditions, a primary variable in the hydrolysis reaction. Here, we find strong agreement between PSD measured in the aerosol phase via scanning mobility particle sizing and PSD measured via AFM, with particle sizes peaked below 4 nm for low-humidity conditions. At higher humidity, the distribution is centered around 5 to 10 nm but extends up to 20 nm. These results are in stark contrast to previous measurements using SEM that show PSD on the order of 300- to 1000-nm particle sizes; moreover, these are the first direct measurements of individual particles of UO 2 F 2 having been produced via UF 6 hydrolysis deposited on surfaces. These measurements, therefore, open a new avenue for collecting and detecting UO 2 F 2 in the condensed phase and further refine the PSD, which is critical for environmental transport determinations.

Uranium hexafluoride↗

NASA NTRSDate not supplied

High Resolution Imaging and Analysis of Terrestrial Impact Glass: Amorphous Materials, Phyllosilicates and Everything in Between

Introduction: Impact cratering is one of the most ubiquitous geologic processes shaping the surface of all solid bodies in our solar system. Impacts are also a major source of clay minerals, poorly crystalline clay-like phases and amorphous (i.e., lacking long-range atomic order) materials on Earth and Mars. Phyllosilicates and amorphous materials have consistently formed a major component (~20-70 wt%) of every single drilled rock and soil sample in Gale Crater on Mars, as determined by the CheMin instrument on Curiosity. The origin of the amorphous component is speculative, but could be primary impact or volcanic-produced glass(es) deposited via aeolian or fluvial processes, secondary aqueous alteration products or chemical precipitates; it is likely to be a combination of all three possibilities. Efforts to determine the composition of these materials across the rover’s traverse through Gale Crater are ongoing. Naturally occurring amorphous phases are found in a variety of environments on Earth, and terrestrial analogue studies may help shed light on how they may have formed on Mars. Primary and altered impact glass are likely widespread on Mars and may have contributed to the amorphous component found throughout Gale Crater. In its pristine, unaltered state, impact glass (i.e., melt glass) is considered amorphous. However, truly unaltered glass is rarely preserved in crater fill impactites as it quickly alters in the post-impact environ-ment, commonly forming a mixture of hydrated aluminosilicate phases whose structures are not always discernable at the microscale (i.e., they may be amorphous or contain short-range order). These phases are part of an incredibly complex group of materials; differences in their composition and crystalline structure (or lack thereof) and genetic relationship to the more well-crystalline clay minerals are often only discernable at the nanoscale, beyond the resolution of traditional X-ray diffractometers (XRD) and scanning electron microscopes/microprobes (SEM/EPMA) alone. In this contribution, we summarize recent results from ongoing characterization of clay minerals, poorly crystalline clay-like phases, and amorphous materials preserved in altered terrestrial impact glass from the Chicxulub (~66 Ma) and Ries (~15 Ma) impact structures. This work has been performed using a combination of high-resolution transmission electron microscopy (HR-TEM), SEM, microprobe/EPMA, Raman spectroscopy and XRD.

Impact crater↗

NASA NTRS2025

Thermochemical Stability of Ca2Yb8(SiO4)6O2 Apatite in Presence of Molten Calcium-Magnesium-AluminoSilicate (CMAS)

Thermochemical stability of ytterbium silicon oxyapatite Ca 2 Yb 8 (SiO 4 ) 6 O 2 (CYbS) in the presence of molten calcium-magnesium aluminosilicate (CMAS) has been investigated at elevated temperatures. CYbS apatite powder was synthesized from the constituent oxides via solid state reaction method. Hot pressed apatite substrates were exposed to molten CMAS at 1200, 1300, and 1400 °C for 1, 10, and 50 h. Development of phases in the interaction region of the heat-treated specimens was monitored using scanning electron microscopy, transmission electron microscopy, high angle annular dark field imaging, selected area electron diffraction and energy dispersive X-ray spectroscopy. Monoclinic cyclosilicate Ca 3 Yb 2 (Si 3 O 9 ) 2 formed from interaction of CYbS apatite with CaO in the CMAS melt at the apatite-CMAS reaction front and continued to nucleate and grow within the residual CMAS in diffusion couples annealed for 1-50 h at 1200 °C and those heat treated at 1300 °C for 1 h. Residual CMAS was Ca-depleted when cyclosilicate was present. Dendritic wollastonite CaSiO 3 was observed within the residual CMAS in couples annealed at 1200 and 1300 °C. Ingress of molten CMAS, because of its exponential decrease in viscosity, occurred through open pores and along the grain boundaries of the apatite substrates without any detectable chemical reaction at 1300 and 1400 °C. Results of this study indicate that Ca 2 Yb 8 (SiO 4 ) 6 O 2 apatite has the potential to mitigate the CMAS corrosion up to about 1200 °C but not at higher temperatures.

X-ray diffraction↗

NASA NTRSDate not supplied

Characterization of Novel Spacecraft Materials aboard the Materials International Space Station Experiment-Flight Facility (Preliminary Results)

This work will encompass the preflight characterization of 15 novel and heritage materials currently under observation on the Materials International Space Station Experiment-Flight Facility (MISSE-FF). MISSE-FF has been upgraded to perform active reflectance measurements of the materials. Images taken in RGB/IR colors are compared to results from an extensive ground testing campaign to obtain quantitative on-orbit material evolution data. Identical materials samples are to be flown on the ram, wake, and zenith faces of MISSE-FF, enabling deconvolution of the energetic electron, proton, atomic oxygen, and ultraviolet damage pathways. Energy deposition from the space environment leads to chemical changes in the material that in turn alter the optical properties. The same chemical damage that manifests as changes in optical reflectance and absorptance also leads to changes in myriad physical properties such as mechanical strength, electrical conductivity, and chemical reactivity. Therefore, flight materials are able to be characterized based on their unique reflectance spectra by comparing on-orbit measurements of optical reflectance with extensive terrestrial experiments, which help to correlate changes in reflectance with respect to changes in other material properties. The MISSE program has been a part of the International Space Station National Laboratory for many years and has been instrumental in understanding space weather modification of material properties. However, MISSE-FF has been limited to passive experiments with only pre/post flight material studies possible. In advance of the MISSE-16 experiment, the flight facility has received a major upgrade to provide daily spectral observations by way of a RGB/IR camera and a tunable light source. The MISSE-16 mission launched in February 2022 and carries 15 material samples for 6 months of the low Earth orbital exposure. Identical materials samples are to be flown on the ram, wake, and zenith faces of MISSE-FF, enabling deconvolution of the energetic electron, proton, atomic oxygen, and ultraviolet damage pathways. This paper discusses the MISSE-16 experiment, highlights the first use of the facility upgrades, and presents results from the extensive preflight material characterization that includes directional hemispherical reflectance, bidirectional reflectance, AFM, SEM, and electrical conductivity. Additionally, data showing the modification of these properties by ground-based exposure to space-like electron and atomic oxygen flux will be discussed. Finally, updates on deployment and initial check-out of the experiment on MISSE-FF will be presented. It is the ultimate goal of this program to provide validation for the development of ground based space weather simulation facilities and techniques.

Ryan Hoffman↗

DOE OSTI2026

Optical interference for the guidance of cryogenic focused ion beam milling beyond the axial diffraction limit

Cryogenic focused ion beam (Cryo-FIB) milling has become a standard step in the cryogenic electron tomography (Cryo-ET) workflow and is required to thin cells to electron-semitransparency. However, this destructive process removes the vast majority of the cellular material and raises a critical question: what thin section should be preserved for Cryo-ET analysis? Using a tri-coincident cryogenic FIB-SEM-LM system, we identify an interferometric optical response that can be used for targeting lamella production to fluorescently labeled structures with accuracy beyond the diffraction limit. Here we demonstrate this approach using synthetic samples of fluorescent beads embedded in micron-scale droplets of amorphous ice. We then apply the approach to capture virions inside host cells. Successful targeting is confirmed by Cryo-ET revealing clusters of virions in intracellular vesicles. The method does not require any fluorescent fiducials or axial registration and can be performed on any fluorescently labeled structure that is visible in widefield fluorescence microscopy.

Cryoelectron microscopy↗

DOE OSTI2022

Deformation twinning and detwinning in extruded Mg-4Al: In-situ experiment and crystal plasticity simulation

Deformation twinning and detwinning in extruded Mg-4Al were investigated using in-situ SEM-DIC experiments and crystal plasticity finite element (CPFE) simulation. In this study, the in-situ SEM-DIC method was used to provide a unique set of data including twin/detwin characteristics and twin area fraction in addition to strain maps. A statistical analysis of the activation of twin variants and twin area fraction during both twinning and detwinning was conducted. A strong correlation was found between twin growth/shrinkage and the Schmid Factor (SF) for individual twin variants Higher twin SF during loading and unloading led to higher twin growth and shrinkage, respectively. However, after the applied compressive strain was removed, the pattern of the twin area fractions of the residual twin variants versus their nominal SFs did not follow the trend observed at the maximum compressive strain. Using a systematic methodology and an advanced twin/detwin model, the PRISMS-Plasticity CPFE simulation was calibrated using experimentally determined stress versus strain and twin area fraction versus strain information. A comprehensive evaluation of the CPFE model was conducted to determine its ability to capture the statistics of twin variants activation and twin area fraction. CPFE accurately captured the statistical aspects of both twinning and detwinning. Finally, it also predicted the first dominant twin variant for 47.5% of the grains and at least one of the two dominant twin variants for 80% of the grains at maximum compressive strain.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Spatio-Kinetic Electronic Heterogeneity in MoS 2 Revealed by Ultrafast Electron Microscopy: Implications for Optoelectronics

There is broad interest in layered, two-dimensional (2D) semiconductors owing to their high optical absorption and ability to heterogeneously integrate with various substrates. In such layered semiconductors, mesoscopic imperfections, such as surface step edges, may affect charge carrier kinetics and device performance, but studying their effects on carrier transport with sufficient spatial and temporal resolution is a challenge. Using scanning ultrafast electron microscopy, we image the near-surface charge carrier kinetics with μm/ps spatiotemporal resolution in single-crystal MoS 2 samples with surface steps tens of nanometers in height. We find an approximately 3-fold increase in surface trap density near such surface steps compared to the uniform, flat surface regions. Despite the difference in trap state density, filling of the traps occurs over the same time scale (∼100 ps), but carrier recovery is much slower near the step compared to the uniform regions of the material. Furthermore, these results provide an approach to measure ultrafast dynamics and determine the required uniformity of layered materials depending on the speed limit constraints for specific applications.

SEM↗

DOE OSTI2023

Ice Cryo-Encapsulation Balloon (Project ICEBall) Field Campaign Report

The Ice Cryo-Encapsulation Balloon (ICEBall) field campaign was designed to sample the ice crystals that compose high-altitude cirrus with a passive device. The campaign made use of a new instrument, ICEBall, which is a balloon-borne ice crystal sampling system. The ice crystal sounding system is capable of measuring ice crystal concentration, temperature, atmospheric pressure, ice crystal habit, aerosol particle morphology, and residual composition. The 3-kg instrument is carried upwards at 5 m s-1 by a high-altitude balloon. The instrument can be cut down from the balloon at any altitude up to 20 km, and the apparatus returns to the surface by parachute. Basic measurements such as temperature and pressure are recorded onboard, and high-frequency Global Positioning System (GPS) records altitude and latitude/longitude. Ice crystal concentrations are measured through the use of a high-resolution video camera mounted on the device. Ice crystals are collected through an open aperture leading to insulated collection chambers cooled with dry ice. Upon exiting the top of the cloud system, the chamber aperture is closed, and the ~1 mm3 sample cell is magnetically sealed and isolated at -78 °C, ensuring that ice particles do not sublimate or grow after collection. Once the crystals are returned to the surface, they are double-sealed and immersed at liquid nitrogen temperature in “dry-cryo shippers” before being transported back to the laboratory. Dr. Magee’s laboratory at The College of New Jersey contains a cryo-stage scanning electron microscope (SEM), which was used to interrogate the crystals and aerosol particles. The main purpose of this pilot field campaign was to provide an unprecedented level of detail on the crystal habits and ice surface complexity in mid-latitude cirrus, which may help resolve issues associated with habit identification and classification in cirrus. The ICEBall campaign was originally scheduled to run from March 28 to April 18 of 2021 at the U.S. Department of Energy Atmospheric Radiation Measurement (ARM) Southern Great Plains observatory. The COVID-19 pandemic intervened and caused us to shift the dates of the experiment to October 16-November 6 of 2021. This period is also climatologically favorable for cirrus. The approximately six-month gap between our original field campaign dates and the actual dates afforded us the opportunity to build two new ICEBall payload instruments. These instruments were tested during an August 2021 trip to The College of New Jersey. During this field testing phase, we decided to launch the ICEBall payload upstream from the ARM SGP site with the goal of landing in the vicinity of the site. Our goal was to sample the ice crystals before the cirrus were advected over the remote-sensing instruments at the SGP site. The team assembled for the field campaign consisted of the Principle Investigator (PI) and Co-Principle Investigator (Co-PI) (Drs. Harrington and Magee), The Pennsylvania State University research scientist Dr. Alfred Moyle, and two graduate students (Ms. Marley Majetic and Gwenore Pokrifka). The team operated out of a house rented in Enid, Oklahoma. We successfully sampled seven cirrus cloud systems during the three-week field campaign (October 21, 23-26, 31, and November 1). This was a much higher success rate than either of the PIs anticipated (our goal was closer to sampling three or four cases). The balloon was typically launched from oil pads or farm fields northwest of Enid and the payload was typically retrieved somewhat north of the SGP site. We never landed directly at the SGP site, and so did not need regular access to the SGP facilities. Our greatest concern going into the field campaign was the longer-term storage of crystals in the -196°C cryo dry-shipper dewars and the subsequent transport across the country. We had tested storage and transport prior to the field campaign, but we had never stored crystals for a few weeks nor had we transported the dewars over long distances. To our great relief, the storage and transport worked flawlessly and we were able to image a large number of crystals from six of the seven cases. Working with the staff at the ARM SGP office was excellent. They not only helped us find the sources we needed for helium, liquid nitrogen, and other materials, but also helped with contacts within the Federal Aviation Administration (FAA) and Vance Air Force Base. One goal of our field project was to tie the in situ measurements of ice crystal habits to the radar signatures derived from the Ka-band ARM Zenith-pointing Radar (KAZR). Unfortunately KAZR was down for the duration of our experiment. However, the Ka-band Scanning ARM Cloud Radar (KASACR) was put into vertically pointing mode during the ICEBall campaign and those data, along with Doppler lidar measurements, have proved very useful.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2017

Validation of a Manually Oscillating Chair for In-The-Field Assessment of Dynamic Visual Acuity on Crewmembers Within Hours of Returning From Long-Duration Spaceflight

Long-duration spaceflight results in sensorimotor adaptations, which cause functional deficits during gravitational transitions, such as landing on a planetary surface after long-duration microgravity exposure. Both the vestibular system and the central nervous system are affected by gravitational transitions. These systems are responsible for coordinating head and eye movements via the vestibulo-ocular reflex (VOR) and go through an adaptation period upon exposure to microgravity. Consequently, they must also re-adapt to Earth's gravitational environment upon landing. This re-adaptation causes decrements in gaze control and dynamic visual acuity, with crewmembers reporting oscillopsia and blurred vision caused by retinal slip, or the inability to keep an image focused on their retina. This is thought to drive motion sickness symptoms experienced by most crewmembers following landing. Retinal slip can be estimated by dynamic visual acuity (DVA); visual acuity while in motion. Previously, DVA has been assessed in the laboratory where subjects walked at 6.4 km/hr on a motorized treadmill. Using this method, Peters et al. (2011) found that DVA is worsened in astronauts by an average of 0.75 eye-chart lines one day after landing. However, it is believed that re-adaptation occurs quickly and that DVA might be worse immediately upon re-exposure to a gravitational environment. Since many crewmembers are unable to walk safely upon landing, it was necessary to develop a method for replicating the vertical head movements associated with walking. In addition, the use of a chair to imitate the head displacement caused by walking isolates eye-head interactions without allowing for trunk and lower-body compensation, as seen with treadmill walking (Mulavara & Bloomberg 2003). Therefore, a modality for assessing DVA in the field within a few hours of landing was developed. In this study, we validated the ability of a manually operated oscillating chair to reproduce the oscillatory frequency of walking on a treadmill. Healthy non-astronaut subjects (n=14) participated in one test session and completed three static (seated) and three dynamic (walking/oscillated) visual acuity tests. DVA was assessed using a motorized treadmill, an automated oscillating chair, and a manually operated chair, both developed in the Neuroscience Laboratory at JSC. The automated chair was motor-driven and set to oscillate vertically at 2 Hz with a vertical displacement of +/- 5 cm to simulate vertical translation while walking. The manually operated chair was oscillated vertically by a test operator to the beat of a metronome at 120 beats/min (2 Hz) and a vertical displacement of approximately +/- 5 cm. As the subject was oscillated, they were asked to discern the direction gap of Landolt-C optotypes of varying sizes and verbally reported the direction while an operator recorded their response using a gamepad. Subjects were outfitted with accelerometers (sampling rate = 128 Hz) on their head, trunk and lumbar spine. A fast Fourier transform was performed on the vertical trunk acceleration to compare the peak and spread of the distribution of oscillation frequencies for each oscillating condition. The spread of the frequency distribution for the manual chair was not significantly different from either the treadmill or the automated chair. However, all three conditions had similar non-zero standard error values, suggesting a variance in head movement frequency which may affect DVA. The average oscillation frequency of the manual chair (1.85 Hz) was significantly different (α=0.05) from that of treadmill walking (2.24 Hz), but not significantly different from that of the automated chair (1.85 Hz) and all three conditions had small standard errors (SEM = 0.04, 0.06, and 0.08 Hz for manual, treadmill, and automated respectively). This implies that both chairs oscillate at a frequency below that of treadmill walking, but are comparable to each other and reproducible across sessions. Additionally, DVA scores did not vary significantly across conditions. The smaller spread values of the oscillating chairs' frequencies indicated mitigation of variation induced by locomotor strategies, which enables better examination of the issue of VOR adaptation. Furthermore, due to the deconditioned state of crewmembers in the initial hours after landing, it is easier to transport a manual bouncing chair into the field and safer to perform a vision test while seated in a chair versus walking on a treadmill. Therefore, the manually oscillating chair has been deemed to meet and exceed the DVA testing capabilities previously obtained by treadmill walking.

Kreutzberg, G. A.↗