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DOE OSTI2020

Fiberboard Properties and Degradation Rates for Storage of 9975 Shipping Package in KAC (2020 Status Report)

Savannah River Site (SRS) stores plutonium materials within model 9975 shipping packages in the K-Area Complex (KAC). The 9975 shipping package consists of a 35 gallon stainless steel drum, Celotex fiberboard insulation, lead shield, and primary and secondary containment vessels. The 9975 shipping package design, performance, and analysis for safe transport of radioactive material are described in the Safety Analysis Report for Packaging (SARP). Celotex fiberboard provides three safety functions: thermal insulation to limit internal temperature during a fire, criticality control, and resistance to package crushing. The fiberboard material must retain its dimensions and density within certain ranges to provide the required impact resistance, criticality control, and fire resistance. The SRS Surveillance Program monitors material performance to establish a basis for service life and ensures the continued integrity of 9975 packages. Fiberboard samples, taken from multiple fiberboard assemblies fabricated from cane and softwood fiberboard, have been conditioning in elevated temperature environments since 2005. The samples are periodically examined to monitor thermal, mechanical, and physical properties, and assess degradation trends. Fiberboard properties of interest that are evaluated to demonstrate acceptable long-term performance include dimensional stability, density, compressive strength, thermal conductivity, and specific heat capacity. Duplicate samples from multiple package sources have been tested to identify the range of variability in fiberboard properties and degradation rates. Baseline and long-term testing of fiberboard material properties have been reported previously; reference 6 summarized experimental results of cane and softwood fiberboard through May 2019 and presented degradation models for the measured properties. This report presents the cumulative data collected through June 2020 and the corresponding updated aging models.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

Inactivation of Fluorescent Lipid Bilayers by Irradiation With 300 keV Electrons Using Liquid Cell Transmission Electron Microscopy

Liquid cell transmission electron microscopy allows for imaging of samples in a fully hydrated state at high resolution and has the potential for visualizing static or dynamic biological structures. However, the ionizing nature of the electron beam makes it difficult to discern real physiological dynamics from radiation induced artifacts within liquid cell samples. Electron flux thresholds for achieving high resolution structures from biological samples frozen in ice have been described extensively by the cryo-electron microscopy field, while electron flux thresholds which do not result in a functional change for biological samples within the hydrated environment of a transmission electron microscope liquid cell is less clear. Establishing these functional thresholds for biologically relevant samples is important for accurate interpretation of results from liquid cell experiments. Here we demonstrate the electron damage threshold of fluorescently tagged lipid bilayers by quantifying the change in fluorescence before and after electron exposure. We observe the reduction of fluorescent signal in bilayers by 25% after only 0.0005 e − /Å 2 and a reduction of over 90% after 0.01 e − /Å 2 . These results indicate that the loss of function occurs at irradiation thresholds far below a typical single high resolution (scanning) transmission electron microscopy image and orders of magnitude below fluxes used for preserving structural features with cryo-electron microscopy.

Moser, Trevor↗

NASA NTRS1971

Test and evaluation of Apollo 14 composite casting demonstration specimens and flight and control samples

The results of experiments 1, 2, and 10 of the Apollo 14 composite casting demonstration are discussed. The purpose of the demonstration, with regard to samples 1 and 2, was to obtain preliminary data on the liquid phase sintering process in a weightless environment. With regard to sample 10, the purpose was to obtain preliminary information on how to achieve uniform dispersion of dense particles on a metal matrix by employing shaking modes or forces in the system when the metal matrix is molten. Results of the demonstrations were interpreted in a quantitative and qualitative manner. For experiment 1 it was found that the tungsten particles were redistributed more uniformly in the flight sample than in the control sample. Experiment 2 results indicate that complete melting may not have occured and thus a high degree of significance cannot be associated with the qualitative results relating to particle redistribution data. The particle-matrix system of experiment 10 was found to be nonwetting.

Fabiniak, R. C.↗

NASA NTRS1993

Measured space environmental effects to LDEF during retrieval

Data gathered by the Interim Operational Contamination Monitor (IOCM) with regard to the effect of the space environment on the STS-32 Shuttle mission and on the Long Duration Exposure Facility (LDEF) are reported. IOCM measures the deposition of molecular and particulate contamination during all flight phases. It also measures the thermophysical properties of thermal control surfaces by calorimetry, the flux of the ambient atomic oxygen environment, the incident solar flux, and the absolute ambient pressure in the payload bay. The IOCM also provides a structure and sample holders for the exposure of passive material samples to the space environment. One of the more salient results from the STS-32 flight suggests that the LDEF emitted a large number of particulates after berthing into the Shuttle. The mission atomic oxygen fluence was also calculated. Although the fluence was low by normal standards, the Kapton (trademark) passive samples exhibited the onset of erosion. Orbital debris and micrometeoroid impacts also occurred during the retrieval mission. The average perforation diameter was approximately 1.25 micrometers. The largest perforation diameter was measured at 65 micrometers.

Maag, Carl R.↗

NASA NTRS2003

From Global Reconnaissance to Sample Return: A Proposal for a Post-2009 Strategy to Follow the Water on Mars

Since the mid-1990's, the stated strategy of the Mars Exploration Program has been to Follow the Water. Although this strategy has been widely publicized, its degree of influence -- and the logic behind its current implementation (as reflected in mission planning, platform and instrument selection, and allocation of spacecraft resources) remains unclear. In response to this concern, we propose an integrated strategy for the post-2009 exploration of Mars that identifies the scientific objectives, rationale, sequence of missions, and specific investigations, that we believe provides the maximum possible science return by pursuing the most direct, cost-effective, and technically capable approach to following the water. This strategy is based on the orbital identification, high-resolution surface investigation, and ultimate sampling of the highest priority targets: near-surface liquid water and massive ground ice (potentially associated with the discharge of the outlflow channels or the relic of a former ocean). The analysis of such samples, in conjunction with the data acquired by the necessary precursor investigations (to identify the locations and characterize the environments of the optimum sampling sites), is expected to address a majority of the goals and high priority science objectives identified by MEPAG.

S M Clifford↗

NASA NTRS1992

Measured space environmental effects to LDEF during retrieval

On the STS-32 shuttle mission, a space flight experiment provided an understanding of the effects of the space environment on the Long Duration Exposure Facility (LDEF) from rendezvous with the shuttle until removal from the payload bay at the Orbiter Processing Facility (OPF) at KSC. The Interim Operational Contamination Monitor (IOCM) is an attached shuttle payload that has been used on two earlier flights (STS 51C and STS 28) to quantify the contamination deposited during the course of the mission. The IOCM can characterize by direct measurement, the deposition of molecular and particulate contamination during any phase of flight. In addition to these principal measurements, the IOCM actively measures the thermophysical properties of thermal control surfaces by calorimetry, the flux of the ambient atomic oxygen environment, the incident solar flux, and the absolute ambient pressure in the payload bay. The IOCM also provides a structure and sample holders for the exposure of passive material samples to the space environment, e.g. thermal cycling, atomic oxygen, and micrometeoroids and/or orbital debris, etc. One of the more salient results from the STS-32 flight suggests that the LDEF emitted a large number of particulates after berthing into the shuttle. The mission atomic oxygen fluence was also calculated. Although the fluence was low by normal standards, the Kapton passive samples exhibited the onset of erosion. Orbital debris and micrometeoroid impacts also occurred during the retrieval mission. The average perforation diameter was approximately 12.5 microns. The largest perforation diameter was measured at 65 microns.

Maag, Carl R.↗

NASA NTRS2006

Arcing in Leo and Geo Simulated Environments: Comparative Analysis

Comprehensive tests of two solar array samples in simulated Low Earth Orbit (LEO) and Geosynchronous Orbit (GEO) environments have demonstrated that the arc inception voltage was 2-3 times lower in the LEO plasma than in the GEO vacuum. Arc current pulse wave forms are also essentially different in these environments. Moreover, the wide variations of pulse forms do not allow introducing the definition of a "standard arc wave form" even in GEO conditions. Visual inspection of the samples after testing in a GEO environment revealed considerable damage on coverglass surfaces and interconnects. These harmful consequences can be explained by the discharge energy being one order of magnitude higher in vacuum than in background plasma. The tests also revealed a potential danger of powerful electrostatic discharges that could be initiated on the solar array surface of a satellite in GEO during the ignition of an arcjet thruster.

Vayner, Boris V.↗

NASA NTRS2019

Robotic Mars Sample Return and Earth entry vehicle concept development

NASA has studied potential Mars Sample Return over many decades, and the most recent Planetary Science Decadal Survey recommended making significant progress on this topic one of its highest priority goals. Recent inter-agency discussions and scientific support are lending credence to current Mars Sample Return planning activities, which notionally target launch of Sample Retrieval Lander and Earth Return Orbiter flight elements in 2026, and return of Martian samples to Earth in 2031. As part of the Mars Sample Return architecture under consideration, an Earth Entry Vehicle would perform the final phase by protecting the samples through severe entry environments using a 60-deg. sphere-cone flying on a passive/ballistic trajectory. The Earth Entry Vehicle design activities in particular are considering a variety of potential challenges, including: minimizing vehicle mass due to the need to travel to Mars and back to Earth, vehicle robustness to Micrometeroid and Orbital Debris impacts, capability to withstand severe entry environments while minimizing landing ellipse size, and providing impact load attenuation during a high-speed landing to meet Martian sample tube load limits and ensure sample containment in off-nominal scenarios. The present work provides a snapshot of current study work in progress, and highlights paths being taken to address these various design challenges for the conceptual Earth Entry Vehicle.

Corliss, James↗

DOE OSTI2022

Laser Surface Processing of Alloys for Corrosion Protection (Final Project Report of Marine Energy Seedling Project)

This is the final project report for the MHK Seedling project. The report describes use of laser surface processing (LSP) to modify the surface of test materials (Al, steel) and the corrosion testing performed on the resulting samples in different corrosion environments. Data shows that LSP improved the corrosion resistance of Al and steel used in this work relative to respective non-LSP samples. The data also showed that each material had a specific range of laser processing conditions where the beneficial effects of LSP (i.e. improvement in corrosion protection) were observed. Application of LSP to enable low-cost materials in marine environments, additional microstructural analysis and long-term testing are proposed to further develop this technology for marine renewable energy and systems.

36 MATERIALS SCIENCE↗

NASA NTRS1991

Measured space environmental effects to LDEF during retrieval

The Interim Operational Contamination Monitor (IOCM) is an attached shuttle payload to the Long Duration Exposure Facility (LDEF) that was used on 2 earlier flights to quantify the contamination deposited during the course of the missions. The IOCM can characterize by direct measurement the deposition of molecular and particulate contamination during any phase of flight. Also, the IOCM actively measures the optical property changes of thermal control surfaces by calorimetry, the flux of the ambient atomic oxygen environment, the incident solar flux, and the absolute ambient pressure in the payload bay. The IOCM also provides a structure and sample holders for the exposure of passive material samples to the space environment, e.g., thermal cycling, atomic oxygen, and micrometeoroids and/or debris. Some of the more salient results from the flight suggests that the payload bay was slightly contaminated during both the prelaunch phase of the mission and after the deployment of the SYNCOM IV payload. Measurements during the postflight phases, i.e., ferry flight and deintegration processing, show negligible to very low mass deposition. The results of the data are discussed in depth.

Maag, Carl R.↗

NASA NTRS2012

Glovebox for GeoLab Subsystem in HDU1-PEM

The GeoLab glovebox was designed to enable the preliminary examination, by astronauts, of geological samples collected from the surface of another planetary body. The collected information would then aid scientists in making decisions about sample curation and prioritization for return to Earth for study. This innovation was designed around a positive- pressure-enriched nitrogen environment glovebox to reduce sample handling contamination. The structure was custom-designed to fit in section H of NASA s Habitat Demonstration Unit 1 Pressurized Excursion Module (HDU1- PEM). In addition, the glovebox was designed to host analytical instruments in a way that prevents sample contamination.

Evans, Cynthia↗

DOE OSTI2020

The sensitive surface chemistry of Co-free, Ni-rich layered oxides: identifying experimental conditions that influence characterization results

Recent studies have suggested that Co-free, Ni-rich layered cathodes (e.g., doped LiNiO2) can provide promising battery performance for practical applications. However, these layered cathodes suffer from significant surface instability during various stages of the sample history, which generates inherent challenges for achieving stable battery performance and obtaining statistically representative characterization results. To reliably report the surface chemistry of these materials, delicate controls of stepwise sample preparation are required. In this study, we aim to reveal how the surface chemistry of LiNiO2 based materials changes with various environments, including human exhalation, sample storage, sample preparation, electrochemistry cycling, and surface doping. Our results demonstrate that the surface of these materials is highly reactive and prone to alter at various stages of sample handling and characterization. The sensitive surface could impact the interpretation of the surface chemical and structural information, including surface carbonate formation, transition metal reduction and dissolution, and surface reconstruction. Importantly, the heterogeneity of the surface degradation calls for a consolidation of nanoscale, high-resolution characterization, and ensemble-averaged methods in order to improve statistical representation. Furthermore, the doping chemistry can effectively mitigate the surface degradation and improve overall battery performance due to the enhanced surface oxygen retention. Our study highlights the necessity of strict measurements through complementary characterizations at multiple length scales to eliminate unintentional biased conclusions.

surface chemistry, Co-free Ni-rich cathodes, Istab↗

NASA NTRS2019

Cleanroom Contamination Identification Method Development

During fabrication, assembly, and testing of spacecraft and flight hardware it is vital to avoid contaminants that can cause degradation and could result in significant failure. Yet, there is no existing contamination monitoring method that provides the identity of airborne particles in a cleanroom facility. Knowing the particle identities, would allow scientists and engineers to determine the source of the contaminants and prevent setbacks before they occur or cause damage. Current cleanliness monitoring methods include airborne particle counters (APCs), fallout filters, and visual inspections. Particle counts from APCs are the primary metric used to define a cleanroom class and hence its level of cleanliness, but do not provide identification nor can they differentiate between large and small sizes of particles. In addition, using fallout filters is not a proactive, timely, or representative approach to cleanroom contamination monitoring because these samples are only retrieved after 30 days and are placed away from spacecraft processing to avoid interference with operations. In contrast, the forced air sampling method can collect a sample within an hour at any location required and provide results in less than a day. This system uses a cassette and filter sample medium to capture airborne particles which are then taken to a scanning electron microscope with energy dispersive spectroscopy (SEM/EDS) to identify and size the captured particles. Development of forced air sampling into an established laboratory capability will allow for fast sampling and routine identification of unknown contamination sources within the cleanroom. The test method development required market research for an air sampling cassette that increases sample collection efficiency and a filter with low enough background contamination to allow differentiation between a blank (control) and the collected sample. It was determined that a conductive black cassette and a polycarbonate filter were the best options. Conductive black cassettes, in comparison to the standard styrene, are manufactured using polypropylene filled with carbon. This makes the cassette conductive and minimizes the tendency of particles to stick to the wall of the cassette due to electrostatic force. In previous trials a mixed cellulose ester (MCE) filter was used to capture the contaminants, however the rougher surface of the filter contributed to entrapment of the particles within the filter structure and made it harder to identify the particles. In comparison, track etched polycarbonate filters have random cylindrical pores and a smooth surface which contributes to uniform sample distribution on the surface of the filter. Future work includes: testing the system using control samples to determine the efficiency and suitability of the medium, performing sample collection in various environments to establish ideal operating parameters and analyzing contaminant particles using SEM/EDS and assistant characterization techniques. Once fully developed, employing the forced air sampling method will help to prevent damage to spacecraft, avoid schedule delays, and allow for mission success.

Hernandez Melendez, Jailyn M.↗

DOE OSTI2020

Sample Identifiers and Metadata Reporting Format for Environmental Systems Science

The ESS-DIVE sample identifiers and metadata reporting format primarily follows the System for Earth Sample Registration (SESAR) Global Sample Number (IGSN) guide and template, with modifications to address Environmental Systems Science (ESS) sample needs and practicalities (IGSN-ESS). IGSNs are associated with standardized metadata to characterize a variety of different sample types (e.g. object type, material) and describe sample collection details (e.g. latitude, longitude, environmental context, date, collection method). Globally unique sample identifiers, particularly IGSNs, facilitate sample discovery, tracking, and reuse; they are especially useful when sample data is shared with collaborators, sent to different laboratories or user facilities for analyses, or distributed in different data files, datasets, and/or publications. To develop recommendations for multidisciplinary ecosystem and environmental sciences, we first conducted research on related sample standards and templates. We provide a comparison of existing sample reporting conventions, which includes mapping metadata elements across existing standards and Environment Ontology (ENVO) terms for sample object types and environmental materials. We worked with eight U.S. Department of Energy (DOE) funded projects, including those from Terrestrial Ecosystem Science and Subsurface Biogeochemical Research Scientific Focus Areas. Project scientists tested the process of registering samples for IGSNs and associated metadata in workflows for multidisciplinary ecosystem sciences. We provide modified IGSN metadata guidelines to account for needs of a variety of related biological and environmental samples. While generally following the IGSN core descriptive metadata schema, we provide recommendations for extending sample type terms, and connecting to related templates geared towards biodiversity (Darwin Core) and genomic (Minimum Information about any Sequence, MIxS) samples and specimens. ESS-DIVE recommends registering samples for IGSNs through SESAR, and we include instructions for registration using the IGSN-ESS guidelines. Our resulting sample reporting guidelines, template (IGSN-ESS), and identifier approach can be used by any researcher with sample data for ecosystem sciences.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2006

Ultrasonic/Sonic Driller/Corer (USDC) as a Subsurface Sampler and Sensors Platform for Planetary Exploration Applications

The search for existing or past life in the Universe is one of the most important objectives of NASA's mission. For this purpose, effective instruments that can sample and conduct in-situ astrobiology analysis are being developed. In support of this objective, a series of novel mechanisms that are driven by an Ultrasonic/Sonic actuator have been developed to probe and sample rocks, ice and soil. This mechanism is driven by an ultrasonic piezoelectric actuator that impacts a bit at sonic frequencies through the use of an intermediate free-mass. Ultrasonic/Sonic Driller/Corer (USDC) devices were made that can produce both core and powdered cuttings, operate as a sounder to emit elastic waves and serve as a platform for sensors. For planetary exploration, this mechanism has the important advantage of requiring low axial force, virtually no torque, and can be duty cycled for operation at low average power. The advantage of requiring low axial load allows overcoming a major limitation of planetary sampling in low gravity environments or when operating from lightweight robots and rovers. The ability to operate at duty cycling with low average power produces a minimum temperature rise allowing for control of the sample integrity and preventing damage to potential biological markers in the acquired sample. The development of the USDC is being pursued on various fronts ranging from analytical modeling to mechanisms improvements while considering a wide range of potential applications. While developing the analytical capability to predict and optimize its performance, efforts are made to enhance its capability to drill at higher power and high speed. Taking advantage of the fact that the bit does not require rotation, sensors (e.g., thermocouple and fiberoptics) were integrated into the bit to examine the borehole during drilling. The sounding effect of the drill was used to emit elastic waves in order to evaluate the surface characteristics of rocks. Since the USDC is driven by piezoelectric actuation mechanism it can designed to operate at extreme temperature environments from very cold as on Titan and Europa to very hot as on Venus. In this paper, a review of the latest development and applications of the USDC will be given.

sampling↗

NASA NTRS1980

An interactive modular design for computerized photometry in spectrochemical analysis

A general functional description of totally automatic photometry of emission spectra is not available for an operating environment in which the sample compositions and analysis procedures are low-volume and non-routine. The advantages of using an interactive approach to computer control in such an operating environment are demonstrated. This approach includes modular subroutines selected at multiple-option, menu-style decision points. This style of programming is used to trace elemental determinations, including the automated reading of spectrographic plates produced by a 3.4 m Ebert mount spectrograph using a dc-arc in an argon atmosphere. The simplified control logic and modular subroutine approach facilitates innovative research and program development, yet is easily adapted to routine tasks. Operator confidence and control are increased by the built-in options including degree of automation, amount of intermediate data printed out, amount of user prompting, and multidirectional decision points.

Bair, V. L.↗

DOE OSTI2024

Nonparametric Multiparticle Set Methods for Interpreting Environmental Samples

Collection and analysis of environmental samples is commonly used by a range of stakeholders in nuclear safeguards and security contexts. While the ubiquity of samples and their transport in the environment allow regular collection, developing and demonstrating methods for analyzing these samples is difficult. In this work, an environmental sample consists of a set of one or more individual particles. Recent advances in reactor simulation have allowed us to generate data that are more representative of real-world environmental samples, enabling statistically defensible method development and testing. The most notable of these advances is a drastic increase in the number of material depletion regions, which allows our simulations to capture the variation in isotopic composition seen at length scales consistent with environmental samples. Traditional approaches for handling multiparticle samples treat each particle in the sample individually, estimating the quantity of interest (e.g., core-average burnup) resulting from measurement and analysis of signatures (e.g., nuclide assays) from each individual particle. Individual estimates are then averaged to generate a single estimate of the quantity of interest over the entire sample. In this presentation, we introduce two novel approaches for interpreting environmental samples that comprise of multiple particles: (1) the Quantile-Quantile Comparator, which uses a multivariate generalization of quantile-quantile plots for comparing unknown statistical distributions, and (2) the Set Transformer, an attention-based neural network module designed to model interactions among elements (particles) in the input set (sample). Statistically representative sampling cannot be guaranteed as samples are passively collected and are beholden to what particles are available in the environment. These new analysis methods for set-input problems are expected to be more robust than traditional approaches to issues of sampling bias where particles are not uniformly distributed throughout regions of interest, as well as generally outperform traditional approaches by jointly considering all elements in the set. We will present results comparing the performance of traditional single particle approaches and the novel Quantile-Quantile Comparator and Set Transformer for interpretation of simulated environmental samples.

Phathanapirom, Birdy↗

NASA NTRS1966

Corrosion of metal samples rapidly measured

Corrosion of a large number of metal samples that have been exposed to controlled environment is accurately and rapidly measured. Wire samples of the metal are embedded in clear plastic and sectioned for microexamination. Unexposed wire can be included in the matrix as a reference.

Maskell, C. E.↗