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NASA NTRS2011

An Experimental Study of Upward Burning Over Long Solid Fuels: Facility Development and Comparison

As NASA's mission evolves, new spacecraft and habitat environments necessitate expanded study of materials flammability. Most of the upward burning tests to date, including the NASA standard material screening method NASA-STD-6001, have been conducted in small chambers where the flame often terminates before a steady state flame is established. In real environments, the same limitations may not be present. The use of long fuel samples would allow the flames to proceed in an unhindered manner. In order to explore sample size and chamber size effects, two large chambers were developed at NASA GRC under the Flame Prevention, Detection and Suppression (FPDS) project. The first was an existing vacuum facility, VF-13, located at NASA John Glenn Research Center. This 6350 liter chamber could accommodate fuels sample lengths up to 2 m. However, operational costs and restricted accessibility limited the test program, so a second laboratory scale facility was developed in parallel. By stacking additional two chambers on top of an existing combustion chamber facility, this 81 liter Stacked-chamber facility could accommodate a 1.5 m sample length. The larger volume, more ideal environment of VF-13 was used to obtain baseline data for comparison with the stacked chamber facility. In this way, the stacked chamber facility was intended for long term testing, with VF-13 as the proving ground. Four different solid fuels (adding machine paper, poster paper, PMMA plates, and Nomex fabric) were tested with fuel sample lengths up to 2 m. For thin samples (papers) with widths up to 5 cm, the flame reached a steady state length, which demonstrates that flame length may be stabilized even when the edge effects are reduced. For the thick PMMA plates, flames reached lengths up to 70 cm but were highly energetic and restricted by oxygen depletion. Tests with the Nomex fabric confirmed that the cyclic flame phenomena, observed in small facility tests, continued over longer sample. New features were also observed at the higher oxygen/pressure conditions available in the large chamber. Comparison of flame behavior between the two facilities under identical conditions revealed disparities, both qualitative and quantitative. This suggests that, in certain ranges of controlling parameters, chamber size and shape could be one of the parameters that affect the material flammability. If this proves to be true, it may limit the applicability of existing flammability data.

Kleinhenz, Julie↗

DOE OSTI2022

Multi-lab study on the pure-gas permeation of commercial polysulfone (PSf) membranes: Measurement standards and best practices

Gas-separation membranes are a critical industrial component for a low-carbon and energy-efficient future. As a result, many researchers have been testing membrane materials over the past several decades. Unfortunately, almost all membrane-based testing systems are home-built, and there are no widely accepted material standards or testing protocols in the literature, making it challenging to accurately compare experimental results. Further, in this multi-lab study, ten independent laboratories collected high-pressure pure-gas permeation data for H 2 , O 2 , CH 4 , and N 2 in commercial polysulfone (PSf) films. Equipment information, testing procedures, and permeation data from all labs were collected to provide (1) accepted H 2 , O 2 , CH 4 , and N 2 permeability values at 35°C in PSf as a reference standard, (2) statistical analysis of lab-to-lab uncertainties in evaluating permeability, and (3) a list of best practices for sample preparation, equipment set-up, and permeation testing using constant-volume variable-pressure apparatuses. Results summarized in this work provide a reference standard and recommended testing protocols for pure-gas testing of membrane materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2012

Report of the Task Group 186 on model-based dose calculation methods in brachytherapy beyond the TG-43 formalism: Current status and recommendations for clinical implementation

The charge of Task Group 186 (TG-186) is to provide guidance for early adopters of model-based dose calculation algorithms (MBDCAs) for brachytherapy (BT) dose calculations to ensure practice uniformity. Contrary to external beam radiotherapy, heterogeneity correction algorithms have only recently been made available to the BT community. Yet, BT dose calculation accuracy is highly dependent on scatter conditions and photoelectric effect cross-sections relative to water. In specific situations, differences between the current water-based BT dose calculation formalism (TG-43) and MBDCAs can lead to differences in calculated doses exceeding a factor of 10. MBDCAs raise three major issues that are not addressed by current guidance documents: (1) MBDCA calculated doses are sensitive to the dose specification medium, resulting in energy-dependent differences between dose calculated to water in a homogeneous water geometry (TG-43), dose calculated to the local medium in the heterogeneous medium, and the intermediate scenario of dose calculated to a small volume of water in the heterogeneous medium. (2) MBDCA doses are sensitive to voxel-by-voxel interaction cross sections. Neither conventional single-energy CT nor ICRU/ICRP tissue composition compilations provide useful guidance for the task of assigning interaction cross sections to each voxel. (3) Since each patient-source-applicator combination is unique, having reference data for each possible combination to benchmark MBDCAs is an impractical strategy. Hence, a new commissioning process is required. TG-186 addresses in detail the above issues through the literature review and provides explicit recommendations based on the current state of knowledge. TG-43-based dose prescription and dose calculation remain in effect, with MBDCA dose reporting performed in parallel when available. In using MBDCAs, it is recommended that the radiation transport should be performed in the heterogeneous medium and, at minimum, the dose to the local medium be reported along with the TG-43 calculated doses. Assignments of voxel-by-voxel cross sections represent a particular challenge. Electron density information is readily extracted from CT imaging, but cannot be used to distinguish between different materials having the same density. Therefore, a recommendation is made to use a number of standardized materials to maintain uniformity across institutions. Sensitivity analysis shows that this recommendation offers increased accuracy over TG-43. MBDCA commissioning will share commonalities with current TG-43-based systems, but in addition there will be algorithm-specific tasks. Two levels of commissioning are recommended: reproducing TG-43 dose parameters and testing the advanced capabilities of MBDCAs. For validation of heterogeneity and scatter conditions, MBDCAs should mimic the 3D dose distributions from reference virtual geometries. Potential changes in BT dose prescriptions and MBDCA limitations are discussed. When data required for full MBDCA implementation are insufficient, interim recommendations are made and potential areas of research are identified. Application of TG-186 guidance should retain practice uniformity in transitioning from the TG-43 to the MBDCA approach.

61 RADIATION PROTECTION AND DOSIMETRY↗

NASA NTRS1974

Carbon composites in space vehicle structures

Recent developments in the technology of carbon or graphite filaments now provide the designer with greatly improved materials offering high specific strength and modulus. Besides these advantages are properties which are distinctly useful for space applications and which provide feasibility for missions not obtainable by other means. Current applications include major and secondary structures of communications satellites. A number of R & D projects are exploring carbon-fiber application to rocket engine motor cases, advanced antenna systems, and space shuttle components. Future system studies are being made, based on the successful application of carbon fibers for orbiting space telescope assemblies, orbital transfer vehicles, and very large deployable energy generation systems. Continued technology development is needed in analysis, material standards, and advanced structural concepts to exploit the full potential of carbon filaments in composite materials.

Mayer, N. J.↗

NASA NTRS2006

Lunar Regolith Simulant Materials: Recommendations for Standardization, Production, and Usage

Experience gained during the Apollo program demonstrated the need for extensive testing of surface systems in relevant environments, including regolith materials similar to those encountered on the lunar surface. As NASA embarks on a return to the Moon, it is clear that the current lunar sample inventory is not only insufficient to support lunar surface technology and system development, but its scientific value is too great to be consumed by destructive studies. Every effort must be made to utilize standard simulant materials, which will allow developers to reduce the cost, development, and operational risks to surface systems. The Lunar Regolith Simulant Materials Workshop held in Huntsville, AL, on January 24 26, 2005, identified the need for widely accepted standard reference lunar simulant materials to perform research and development of technologies required for lunar operations. The workshop also established a need for a common, traceable, and repeatable process regarding the standardization, characterization, and distribution of lunar simulants. This document presents recommendations for the standardization, production and usage of lunar regolith simulant materials.

Sibille, L.↗

DOE OSTI2020

Improving Elemental Ratio Measurements on Uranyl Fluoride with NanoSIMS

Measurements on samples of calcined uranyl fluoride (UO 2 F 2 ) using Raman spectroscopy, electron microscopy with elemental analysis, and secondary ion mass spectrometry (SIMS) indicate four facts. First, UO 2 F 2 undergoes a previously unreported oxidation reaction beginning around 350 °C in air. The resulting oxidation compound is likely similar to U 3 O 8 /UO 3 , but presently represents a novel chemical species. Second, variations in F/U ratio across samples as measured by electron microscopy with x-ray spectroscopy correlate with variations in F/U ratio as measured with the NanoSIMS 50L instrument. Third, simple mixed powders of LaF 3 +U 3 O 8 are not sufficiently homogeneous to act as a high F+U content standard material. Fourth, additional method development for determining the bulk F/U ratio using an alternative technique is necessary to further develop analytical standards.

36 MATERIALS SCIENCE↗

NASA NTRS1994

Pyrolysis-gas chromatography/mass spectrometry analyses of biological particulates collected during recent space shuttle missions

Biological particulates collected on air filters during shuttle missions (STS-40 and STS-42) were identified using pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). A method was developed for identifying the atmospheric particles and their sources through the analysis of standard materials and the selection of "marker" compounds specific to the particle type. Pyrolysis spectra of biological standards were compared with those of airborne particles collected during two space shuttle missions; marker compounds present in the shuttle particle spectra were matched with those of the standards to identify the source of particles. Particles of 0,5--1-mm diameter and weighing as little as 40 micrograms could be identified using this technique. The Py-GC/MS method identified rat food and soilless plant-growth media as two sources of particles collected from the shuttle atmosphere during flight.

NASA Program Environmental Health↗

DOE OSTI2022

Design considerations for high entropy alloys in advanced nuclear applications

The demanding operating environments of advanced nuclear reactors require the development of new nuclear materials that can withstand their increased physical, chemical, thermal, and radiation-related challenges. High-entropy alloys (HEAs) have shown often-impressive mechanical, thermomechanical, and corrosion-resistant properties, and offer a massive, unexplored compositional space which allows for the targeted development of application-specific materials. Furthermore, although still in a nascent stage, research has shown that HEAs may exhibit unique irradiation tolerance, including reduced defect production and resistance to irradiation-induced swelling and hardening. The mechanisms behind this increased tolerance are not yet well-understood, although the HEA-specific attributes of a complex energy landscape, reduced thermal conductivity, and shift in defect migration energies and pathways provide promising explanations. Here this work assesses the current and future challenges faced by structural nuclear materials, identifying the specific applications in which HEAs may provide a competitive advantage compared to industry-standard materials with the aid of Ashby material selection maps. Considerations are provided for the design of future nuclear HEAs, including calculations of nuclear-relevant properties to assist in the initial down-selection of elements depending on application requirements (e.g., low neutron capture for in-core applications), narrowing the existing compositional space of HEAs to a manageable scope.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Ta compressibility to 20+ Mbar

Developing techniques for experimentally constraining equation of state (EOS) models for important programmatic materials under extreme conditions is vital for advancing our modeling and predictive capabilities. Tantalum is a frequently used standard material for both calibration and testing, and this report describes our work to both measure Ta compressibility to very high pressures and densities using the Ramp Compression Equation of State platform on the National Ignition Facility (NIF). Using a series of seven shots, increasing in peak pressure with each shot, we have made absolute measurements of the compressibility of Ta along the ramp compression path up to 2.3 TPa. Previous experimental measurements constrained the cold compressibility up to ~400 GPa, and there is a spread in the EOS models above that pressure. To improve communication and collaboration between the experimental team and the EOS development group, these new data, along with other experimental and theoretical constraints, were used to develop a Ta equation of state table, M73000. This report first describes the experimental measurements made at the NIF, and then discusses the construction of the EOS model. The ramp compression data can be found in tabular form in Appendix A. Appendix B contains some additional experimental details. In Appendix C we include some additional details on the EOS modeling. At the end of this document, we have attached a detailed report on the NIF ramp compression platform itself and in the main text referenced specific sections for additional details.

36 MATERIALS SCIENCE↗

DOE OSTI2020

An anisotropic viscoplasticity model for shale based on layered microstructure homogenization

Viscoplastic deformation of shale is frequently observed in many subsurface applications. Many studies have suggested that this viscoplastic behavior is anisotropic—specifically, transversely isotropic—and closely linked to the layered composite structure at the microscale. In this work, we develop a two-scale constitutive model for shale in which anisotropic viscoplastic behavior naturally emerges from semianalytical homogenization of a bilayer microstructure. The microstructure is modeled as a composite of soft layers, representing a ductile matrix formed by clay and organics, and hard layers, corresponding to a brittle matrix composed of stiff minerals. This layered microstructure renders the macroscopic behavior anisotropic, even when the individual layers are modeled with isotropic constitutive laws. Using a common correlation between clay and organic content and magnitude of creep, we apply a viscoplastic modified Cam-Clay plasticity model to the soft layers, while treating the hard layers as a linear elastic material to minimize the number of calibration parameters. We then describe the implementation of the proposed model in a standard material update subroutine. The model is validated with laboratory creep data on samples from three gas shale formations. We also demonstrate the computational behavior of the proposed model through simulation of time-dependent borehole closure in a shale formation with different bedding plane directions.

58 GEOSCIENCES↗

DOE OSTI2026

Understanding the structural and morphological effects of synthesis route on NpO 2

The availability of actinide standard materials for use in nuclear safeguard applications is critical, as is thorough characterization thereof. Although accurate trace element compositions and isotopic considerations are paramount for deployment of reference standards, structural characterization is also essential towards accurately describing the chemical form and potential matrix effects in candidate materials. Here, to this end, samples of NpO 2 were synthesized via a direct denitration (DD) method and probed with powder X-ray diffraction (PXRD), Raman spectroscopy, and scanning electron microscopy (SEM) for structural and morphological characterization and comparison with NpO 2 materials produced via modified direct denitration (MDD). PXRD confirmed the bulk identity of NpO 2 , and no additional phases were identified using this method. Analysis of Raman data collected using a 532 nm excitation wavelength indicates that samples are mostly phase pure; however, some variability in spectral features is observed. Analysis of additional spectroscopic data collected with a 785 nm excitation wavelength revealed variability in the relative intensity of spectral features. Raman spectroscopy indicates that the sample is primarily NpO 2 ; however, additional signals indicate possible structural disorder, oxidized species, or potential contributions from other Np phases. To further investigate the possibility of additional phase contributions within the sample of NpO 2 , Raman spectroscopic mapping was employed to examine the homogeneity of the sample produced via DD. From this analysis, we determined that despite variability in the intensity of Raman-active vibrational modes, consistent spectra are obtained throughout the area of the sample investigated. SEM images show aggregates with variable sizes and shapes, with rounded, primary particles possessing an average diameter of approximately 100 nm. Comparison of the results of these multimodal analyses to the literature indicates that the crystal chemical, spectroscopic, and microstructural properties of NpO 2 vary based on synthesis method, even if X-ray diffraction data indicate that the bulk phase is NpO 2 .

Direct denitration↗

DOE OSTI2019

Evaluation of In Silico Multifeature Libraries for Providing Evidence for the Presence of Small Molecules in Synthetic Blinded Samples

The current gold standard for unambiguous molecular identification in metabolomics analysis is comparing two or more orthogonal properties from the analysis of authentic reference materials (standards) to experimental data acquired in the same laboratory with the same analytical methods. This represents a significant limitation for comprehensive chemical identification of small molecules in complex samples. The process is time-consuming and costly, and the majority of molecules are not yet represented by standards. Thus, there is a need to assemble evidence for the presence of small molecules in complex samples through the use of libraries containing calculated chemical properties. To address this need, we developed a Multi-Attribute Matching Engine (MAME) and a library derived in-part from our in silico Chemical Library Engine (ISiCLE). Here, we describe an initial evaluation of these methods in a blinded analysis of synthetic chemical mixtures as part of the U.S. Environmental Protection Agency’s (EPA) Non-Targeted Analysis Collaborative Trial (ENTACT, Phase 1). For molecules in all mixtures, the initial blinded false negative rate (FNR), false discovery rate (FDR), and accuracy were 57%, 77%, and 91%, respectively. For high evidence scores, the FDR was 35%. After unblinding of the sample compositions, we optimized the scoring parameters to better exploit the available evidence, and increased the accuracy for molecules suspected as present. The final FNR, FDR, and accuracy were 67%, 53%, and 96%, respectively. For high evidence scores, the FDR was 10%. This study demonstrates that multi-attribute matching methods in conjunction with in silico libraries may one day enable reduced reliance on experimentally-derived libraries for building evidence for the presence of molecules in complex samples.

Nunez, Jamie↗

DOE OSTI2012

Quantifying and Addressing the DOE Material Reactivity Requirements with Analysis and Testing of Hydrogen Storage Materials & Systems

The objective of this project is to examine safety aspects of candidate hydrogen storage materials and systems being developed in the DOE Hydrogen Program. As a result of this effort, the general DOE safety target will be given useful meaning by establishing a link between the characteristics of new storage materials and the satisfaction of safety criteria. This will be accomplished through the development and application of formal risk analysis methods, standardized materials testing, chemical reactivity characterization, novel risk mitigation approaches and subscale system demonstration. The project also will collaborate with other DOE and international activities in materials based hydrogen storage safety to provide a larger, highly coordinated effort.

08 HYDROGEN↗

NASA NTRS1994

Associated with aerospace vehicles development of methodologies for the estimation of thermal properties

Thermal stress analyses are an important aspect in the development of aerospace vehicles at NASA-LaRC. These analyses require knowledge of the temperature distributions within the vehicle structures which consequently necessitates the need for accurate thermal property data. The overall goal of this ongoing research effort is to develop methodologies for the estimation of the thermal property data needed to describe the temperature responses of these complex structures. The research strategy undertaken utilizes a building block approach. The idea here is to first focus on the development of property estimation methodologies for relatively simple conditions, such as isotropic materials at constant temperatures, and then systematically modify the technique for the analysis of more and more complex systems, such as anisotropic multi-component systems. The estimation methodology utilized is a statistically based method which incorporates experimental data and a mathematical model of the system. Several aspects of this overall research effort were investigated during the time of the ASEE summer program. One important aspect involved the calibration of the estimation procedure for the estimation of the thermal properties through the thickness of a standard material. Transient experiments were conducted using a Pyrex standard at various temperatures, and then the thermal properties (thermal conductivity and volumetric heat capacity) were estimated at each temperature. Confidence regions for the estimated values were also determined. These results were then compared to documented values. Another set of experimental tests were conducted on carbon composite samples at different temperatures. Again, the thermal properties were estimated for each temperature, and the results were compared with values obtained using another technique. In both sets of experiments, a 10-15 percent off-set between the estimated values and the previously determined values was found. Another effort was related to the development of the experimental techniques. Initial experiments required a resistance heater placed between two samples. The design was modified such that the heater was placed on the surface of only one sample, as would be necessary in the analysis of built up structures. Experiments using the modified technique were conducted on the composite sample used previously at different temperatures. The results were within 5 percent of those found using two samples. Finally, an initial heat transfer analysis, including conduction, convection and radiation components, was completed on a titanium sandwich structural sample. Experiments utilizing this sample are currently being designed and will be used to first estimate the material's effective thermal conductivity and later to determine the properties associated with each individual heat transfer component.

Scott, Elaine P.↗

DOE OSTI2020

Combined Spatially Resolved Characterization of Antireflection and Antisoiling Coatings for PV Module Glass

Characterization of photovoltaic (PV) module materials throughout different stages of service life is crucial to understanding and improving the durability of these materials. Currently the large-scale of PV modules (>1 m 2 ) is imbalanced with the small-scale of most materials characterization tools (= 1 cm 2 ). Furthermore, understanding degradation mechanisms often requires a combination of multiple characterization techniques. Here, we present adaptations of three standard materials characterization techniques to enable mapping characterization over moderate sample areas (=25 cm 2 ). Contact angle, ellipsometry, and UV-Vis spectroscopy are each adapted and demonstrated on two representative samples: a commercial multi-functional coating for PV glass and an oxide combinatorial sample library. Best practices are discussed for adapting characterization techniques for large area mapping and combining mapping information from multiple techniques.

14 SOLAR ENERGY↗

NASA NTRS2017

Crack Growth Testing of an Aluminum Oxynitride (AlON) for International Space Station Kick Panes

The mechanical properties of an aluminum oxynitride supplied as ground beams and disks were measured using ASTM International (formerly American Society for Testing and Materials) standard test methods. The slow crack growth tests were complicated by a "short" finish that increased strength scatter. Refining of the finish by more material removal in the second stage of grinding or the use of uniaxial grinding as specified in ASTM C1499 might have avoided the issue. The structural design parameters are an elastic modulus of E = 319 GPa, Poisson's ratio of v = 0.26, a fracture toughness of KIvb(A) = 2.18 MPa/m, slow crack growth (SCG) parameter n = 36, and SCG parameter A = 1.96 x 10-11 m/s.(MPa/m)n. For a ground finish, the Weibull parameters are a mean modulus of m = 14.0 and characteristic strength of sigma theta = 250.2 MPa. The 2015 vintage material exhibits similar mechanical properties to a 2010 vintage billet. Indentation flaws were not sensitive to the inherent crack growth mechanisms of this material and produced misleading results.

strength↗

DOE OSTI2018

Preliminary assessment of stable nitrogen and oxygen isotopic composition of USGS51 and USGS52 nitrous oxide reference gases and perspectives on calibration needs

Rationale: Despite a long history and growing interest in isotopic analyses of N 2 O, there is a lack of isotopically characterized N 2 O isotopic reference materials (standards) to enable normalization and reporting of isotope-delta values. Here, in this paper we report the isotopic characterization of two pure N 2 O gas reference materials, USGS51 and USGS52, which are now available for laboratory calibration (https://isotopes.usgs.gov/lab/referencematerials.html). Methods: A total of 400 sealed borosilicate glass tubes of each N 2 O reference gas were prepared from a single gas filling of a high vacuum line. We demonstrated isotopic homogeneity via dual-inlet isotope-ratio mass spectrometry. Isotopic analyses of these reference materials were obtained from eight laboratories to evaluate interlaboratory variation and provide preliminary isotopic characterization of their δ 15 N, δ 18 O, δ 15 N α , δ 15 N β and site preference (S P ) values. Results: The isotopic homogeneity of both USGS51 and USGS52 was demonstrated by one-sigma standard deviations associated with the determinations of their δ 15 N, δ 18 O, δ 15 N α , δ 15 N β and S P values of 0.12 mUr or better. The one-sigma standard deviations of SP measurements of USGS51 and USGS52 reported by eight laboratories participating in the interlaboratory comparison were 1.27 and 1.78 mUr, respectively. Conclusions: The agreement of isotope-delta values obtained in the interlaboratory comparison was not sufficient to provide reliable accurate isotope measurement values for USGS51 and USGS52. Lastly, we propose that provisional values for the isotopic composition of USGS51 and USGS52 determined at the Tokyo Institute of Technology can be adopted for normalizing and reporting sample data until further refinements are achieved through additional calibration efforts.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2019

History of NASA's Determination of Offgassed Products (Test 7)

NASA's Determination of Offgassed Products (Test 7) from materials and assembled articles for spaceflight has evolved since the Apollo program for over 50 years to meet various habitable spacecraft nonmetallic programmatic requirements. Now mandated by NASA STD-6016A, Standard Materials and Processes Requirements for Spacecraft, all nonmetallic materials used in habitable flight compartments, with the exception of ceramics, metal oxides, inorganic glasses, and materials used in sealed containers, must meet the offgassing requirements in NASA-STD-6001B Test 7. This manuscript presents the history of Test 7, beginning with the Apollo spacecraft nonmetallic materials selection guidelines and test requirements in 1967, in which tests were performed in mostly oxygen atmospheres. It progresses through Skylab, Space Shuttle, International Space Station nonmetals testing, and acceptance requirements with milder test environments. This review of the history of Test 7 presents the reader with a perspective on the development and changes undergone since inception to the present. Related NASA standard tests (some now former, discontinued, combined, or supplemental) including Test 6, Odor Assessment, Test 16, Determination of Offgassed Products from Assembled Articles, and Test 12, Total Spacecraft Cabin Offgassing, are discussed in context

Greene, Benjamin↗