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NASA NTRS2020

Characterization of Cosmic Grain Analogs Formed at Low Temperature from Small Hydrocarbon Precursors in the NASA Ames COSmIC Facility

Here, we present the results of the first solid-phase ex situ analysis of cosmic grain analogs produced at low temperature (<200 K) in the NASA Ames COsmic SImulation Chamber (COSmIC) from small hydrocarbon precursors, methane (CH4) and acetylene (C2H2), seeded in an argon supersonic jet expansion and submitted to a plasma discharge. The plasma-induced chemical reactions, initiated between the precursor molecules and their atomic and molecular fragments, radicals and ions, produce larger molecules and eventually solid particles that are collected in situ under controlled conditions. Scanning electron microscopy (SEM) imaging was used to provide insight on the morphology and growth structure of the grains produced in COSmIC, and to investigate how the precursors used to produce the grains affect these parameters. This SEM study has shown that under identical experimental conditions with fixed physical and chemical parameters (precursor density, temperature, energy, and reaction time), heavier precursors in the initial mixture produce larger grains and in larger quantity, most likely as a result of a more complex chemistry: most of the grains produced in the Ar/CH4 (95:5) gas mixture ranged from 15 to 385 nm in diameter with an average density of 2.1 grains per sq.μm, while the grains produced in the Ar/C2H2 (95:5) gas mixture ranged from 40 to 650 nm with a density of 3.5 grains per sq.μm. Changes in the morphology were also observed, with grains produced from acetylene (C2H2) precursors tending to be more spherical than grains produced from methane (CH4) precursors. This change in morphology could be associated with different stages of growth formation at low temperature from a more "planar" growth at first, followed by coagulation into more spherical particles. This study demonstrates that the COSmIC experimental setup can be used to investigate carbon grain formation from small gas-phase molecular precursors at low temperature (<200 K), i.e., under a temperature regime that is representative of the dust condensation zone and outer region of circumstellar envelopes.

Ella Sciamma-O'Brien↗

DOE OSTI2018

Adverse Event Prediction Using Graph-Augmented Temporal Analysis (Final Report)

This report summarizes the work performed under the Sandia LDRD project "Adverse Event Prediction Using Graph-Augmented Temporal Analysis." The goal of the project was to develop a method for analyzing multiple time-series data streams to identify precursors providing advance warning of the potential occurrence of events of interest. The proposed approach combined temporal analysis of each data stream with reasoning about relationships between data streams using a geospatial-temporal semantic graph. This class of problems is relevant to several important topics of national interest. In the course of this work we developed new temporal analysis techniques, including temporal analysis using Markov Chain Monte Carlo techniques, temporal shift algorithms to refine forecasts, and a version of Ripley's K-function extended to support temporal precursor identification. This report summarizes the project's major accomplishments, and gathers the abstracts and references for the publication submissions and reports that were prepared as part of this work. We then describe work in progress that is not yet ready for publication.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2018

Adverse Event Prediction Using Graph-Augmented Temporal Analysis (Final Report)

This report summarizes the work performed under the Sandia LDRD project "Adverse Event Prediction Using Graph-Augmented Temporal Analysis." The goal of the project was to develop a method for analyzing multiple time-series data streams to identify precursors providing advance warning of the potential occurrence of events of interest. The proposed approach combined temporal analysis of each data stream with reasoning about relationships between data streams using a geospatial-temporal semantic graph. This class of problems is relevant to several important topics of national interest. In the course of this work we developed new temporal analysis techniques, including temporal analysis using Markov Chain Monte Carlo techniques, temporal shift algorithms to refine forecasts, and a version of Ripley's K-function extended to support temporal precursor identification. This report summarizes the project's major accomplishments, and gathers the abstracts and references for the publication sub-missions and reports that were prepared as part of this work. We then describe work in progress that is not yet ready for publication.

42 ENGINEERING↗

NASA NTRS2020

Historical and Future Changes in Air Pollutants from CMIP6 Models

Poor air quality is currently responsible for large impacts on human health across the world. In addition, the air pollutants ozone (O3) and particulate matter less than 2.5 µm in diameter (PM2.5) are also radiatively active in the atmosphere and can influence Earth's climate. It is important to understand the effect of air quality and climate mitigation measures over the historical period and in different future scenarios to ascertain any impacts from air pollutants on both climate and human health. The Coupled Model Intercomparison Project Phase 6 (CMIP6) presents an opportunity to analyse the change in air pollutants simulated by the current generation of climate and Earth system models that include a representation of chemistry and aerosols (particulate matter). The shared socio-economic pathways (SSPs) used within CMIP6 encompass a wide range of trajectories in precursor emissions and climate change, allowing for an improved analysis of future changes to air pollutants. Firstly, we conduct an evaluation of the available CMIP6 models against surface observations of O3 and PM2.5. CMIP6 models consistently overestimate observed surface O3 concentrations across most regions and in most seasons by up to 16 ppb, with a large diversity in simulated values over Northern Hemisphere continental regions. Conversely, observed surface PM2.5 concentrations are consistently underestimated in CMIP6 models by up to 10 µg m−3, particularly for the Northern Hemisphere winter months, with the largest model diversity near natural emission source regions. The biases in CMIP6 models when compared to observations of O3 and PM2.5 are similar to those found in previous studies. Over the historical period (1850–2014) large increases in both surface O3 and PM2.5 are simulated by the CMIP6 models across all regions, particularly over the mid to late 20th century, when anthropogenic emissions increase markedly. Large regional historical changes are simulated for both pollutants across East and South Asia with an annual mean increase of up to 40 ppb for O3 and 12 µg m−3 for PM2.5. In future scenarios containing strong air quality and climate mitigation measures (ssp126), annual mean concentrations of air pollutants are substantially reduced across all regions by up to 15 ppb for O3 and 12 µg m−3 for PM2.5. However, for scenarios that encompass weak action on mitigating climate and reducing air pollutant emissions (ssp370), annual mean increases in both surface O3 (up 10 ppb) and PM2.5 (up to 8 µg m−3) are simulated across most regions, although, for regions like North America and Europe small reductions in PM2.5 are simulated due to the regional reduction in precursor emissions in this scenario. A comparison of simulated regional changes in both surface O3 and PM2.5 from individual CMIP6 models highlights important regional differences due to the simulated interaction of aerosols, chemistry, climate and natural emission sources within models. The projection of regional air pollutant concentrations from the latest climate and Earth system models used within CMIP6 shows that the particular future trajectory of climate and air quality mitigation measures could have important consequences for regional air quality, human health and near-term climate. Differences between individual models emphasise the importance of understanding how future Earth system feedbacks influence natural emission sources, e.g. response of biogenic emissions under climate change.

Air pollutants↗

DOE OSTI2015

Direct comparison of defect ensembles extracted from damage probability and raster scan measurements

The presented study addresses the characterization of nanometer sized defects acting as damage precursors in nanosecond laser pulse duration regime. Two approaches are used to extract distributions of localized damage precursors, namely, damage probability and damage density measurements. Testing is performed on uncoated and SiO{sub 2} monolayer film deposited fused silica substrate exposed with pulsed UV irradiation (355 nm, 4.8 ns). Then, a direct comparison of damage precursor ensembles obtained from both methods is carried out. Our analysis indicates apparent differences between both methods that are discussed in detail. Contamination by ablation products is identified as one of the key factors that influence damage density measurements.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2016

Deep eutectic solvent approach towards nickel/nickel nitride nanocomposites

Nickel nitride is an attractive material for a broad range of applications including catalysis. However preparations and especially those targeting nanoscale particles remain a major challenge. Herein, we report a wet-chemical approach to produce nickel/nickel nitride nanocomposites using deep eutectic solvents. A choline chloride/urea deep eutectic solvent was used as a reaction medium to form gels containing nickel acetate tetrahydrate. Heat treatment of the gel in inert atmosphere forms nanoparticles embedded within a nitrogen-doped carbon matrix. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) were used to understand the decomposition profile of the precursors and to select pyrolysis temperatures located in regions of thermal stability. X-ray diffraction (XRD) confirmed the presence of metallic nickel, whereas X-ray photoelectron spectroscopy (XPS) suggested the existence of a nickel nitride surface layer. According to transmission electron microscopy (TEM) analysis these mixed phase, possibly core-shell type nanoparticles, have very defined facets. Furthermore, these materials represent a unique opportunity to tune catalytic properties of nickel-based catalysts through control of their composition, surface structure, and morphology; in addition to employing potential benefits of a nitrogen-doped carbon support.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Photoluminescence of ZnO/C Nanocomposites Formed by the Sol-Gel Method

Films of undoped zinc oxide (ZnO) and of ZnO/C nanocomposite were formed by the sol-gel method on glass substrates and on fiberglass using zinc acetate as a precursor and with the addition of zinc chloride respectively. Analysis of the photoluminescence spectra of ZnO/C films at high (N{sub 2}-laser) and low (HeCd-laser) excitation levels made it possible to establish the defining role of bound excitons in this process at 20–60 K, due to the presence of chlorine residues in the films. With the temperature raised to 300 K the role of recombination through the 1LO- and 2LO-phonon replicas of free exciton levels and impurity-defect levels begins to dominate in the photoluminescence of the ZnO/C films.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Coal-based graphene oxide-like materials: A comprehensive review

Coal is the most abundant energy and hydrocarbon resource in the United States which has been primarily used for power generation. With the increasing retirement of coal power plants and transition to a low-carbon emission economy, the future use of coal will likely shift to a feedstock source for production of valuable materials for different applications. In this review, the latest research reported on production of graphene-like materials in a powder form from coal is compiled and discussed. Here, this review includes: 1) brief background information on graphene and related materials (GRM); 2) relevant material, resource, economic, and socioeconomic information regarding suitability of coal as a potential feedstock for production of GRM; 3) a summary of common approaches for coal upgrading for preparation of more suitable precursors for production of GRM; 4) a compilation and analysis of the reported routes and methods for preparation of GRM from coal and coal derivatives; and 5) reported potential applications of coal-based GRM.

36 MATERIALS SCIENCE↗

NASA NTRS1975

Development of space stable thermal control coatings for use on large space vehicles

The development of a large scale manufacturing method for the production of a stable zinc orthotitanate pigment is studied, with emphasis placed on the comprehensive analysis of the properties and environmental stability of oxalate precursor zinc orthotitanate pigments and of the preparative conditions (time and temperature) leading to optimum properties and optical stability.

Gilligan, J. E.↗

NASA NTRS1994

Reactive Melt Infiltration of Silicon-Niobium Alloys in Microporous Carbons

Studies of the reactive melt infiltration of silicon-niobium alloys in microporous carbon preforms prepared by the pyrolysis of a polymer precursor have been carried out using modeling, Differential Thermal Analysis (DTA), and melt infiltration. Mercury porosimetry results indicate a very narrow pore size distribution with virtually all the porosity within the carbon preforms open to infiltrants. The morphology and amount of the residual phases (niobium disilicide and silicon) in the infiltrated material can be tailored according to requirements by careful control of the properties (pore size and pore volume) of the porous carbon preforms and alloy composition. The average room temperature four-point flexural strength of a reaction-formed silicon carbide material (made by the infiltration of medium pore size carbon preform with Si - 5 at. % Nb alloy) is 290 +/- 40 MPa (42 +/- 6 ksi) and the fracture toughness is 3.7 +/- 0.3 MPa square root of m. The flexural strength decreases at high temperatures due to relaxation of residual thermal stresses and the presence of free silicon in the material.

Singh, M.↗

NASA NTRS2005

An Automatic Phase-Change Detection Technique for Colloidal Hard Sphere Suspensions

Colloidal suspensions of monodisperse spheres are used as physical models of thermodynamic phase transitions and as precursors to photonic band gap materials. However, current image analysis techniques are not able to distinguish between densely packed phases within conventional microscope images, which are mainly characterized by degrees of randomness or order with similar grayscale value properties. Current techniques for identifying the phase boundaries involve manually identifying the phase transitions, which is very tedious and time consuming. We have developed an intelligent machine vision technique that automatically identifies colloidal phase boundaries. The algorithm utilizes intelligent image processing techniques that accurately identify and track phase changes vertically or horizontally for a sequence of colloidal hard sphere suspension images. This technique is readily adaptable to any imaging application where regions of interest are distinguished from the background by differing patterns of motion over time.

McDowell, Mark↗

NASA NTRS2008

An Investigation of State-Space Model Fidelity for SSME Data

In previous studies, a variety of unsupervised anomaly detection techniques for anomaly detection were applied to SSME (Space Shuttle Main Engine) data. The observed results indicated that the identification of certain anomalies were specific to the algorithmic method under consideration. This is the reason why one of the follow-on goals of these previous investigations was to build an architecture to support the best capabilities of all algorithms. We appeal to that goal here by investigating a cascade, serial architecture for the best performing and most suitable candidates from previous studies. As a precursor to a formal ROC (Receiver Operating Characteristic) curve analysis for validation of resulting anomaly detection algorithms, our primary focus here is to investigate the model fidelity as measured by variants of the AIC (Akaike Information Criterion) for state-space based models. We show that placing constraints on a state-space model during or after the training of the model introduces a modest level of suboptimality. Furthermore, we compare the fidelity of all candidate models including those embodying the cascade, serial architecture. We make recommendations on the most suitable candidates for application to subsequent anomaly detection studies as measured by AIC-based criteria.

Martin, Rodney Alexander↗

DOE OSTI2016

Deposition kinetics and characterization of stable ionomers from hexamethyldisiloxane and methacrylic acid by plasma enhanced chemical vapor deposition

A novel ionomer of hexamethyldisiloxane and methacrylic acid was synthesized by plasma enhanced chemical vapor deposition (PECVD). The PECVD process, being solventless, allows mixing of monomers with very different solubilities, and for polymers formed at high deposition rates and with high structural stability (due to the high number of cross-links and covalent bonding to the substrate) to be obtained. A kinetic study over a large set of parameters was run with the aim of determining the optimal conditions for high stability and proton conductivity of the polymer layer. Copolymers with good stability over 6 months' time in air and water were obtained, as demonstrated by ellipsometry, X-Ray reflectivity, and FT-IR spectroscopy. Stable coatings showed also proton conductivity as high as 1.1 ± 0.1 mS cm{sup −1}. Chemical analysis showed that due to the high molecular weight of the chosen precursors, it was possible to keep the plasma energy-input-per-mass low. This allowed limited precursor fragmentation and the functional groups of both monomers to be retained during the plasma polymerization.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2016

Water-gas shift reaction on alumina-supported Pt-CeO x catalysts prepared by supercritical fluid deposition

Alumina-supported platinum catalysts, both with and without ceria, were prepared by supercritical fluid deposition and evaluated for activity for water-gas shift reaction. The organometallic precursor, platinum(II) acetylacetonate, was deposited from solution in supercritical carbon dioxide. Analysis of the catalysts by high resolution scanning transmission electron microscopy indicated that platinum was present in the form of highly dispersed metal nanoparticles. Pretreatment of the alumina-supported ceria in hydrogen prior to the deposition of the platinum precursor resulted in more platinum nucleated on ceria than non-pretreated alumina-supported ceria but varied in both particle size and structure. The ceria-containing catalyst that was not pretreated exhibited a more uniform particle size, and the Pt particles were encapsulated in crystalline ceria. Reaction rate measurements showed that the catalyst was more active for water-gas shift, with reaction rates per mass of platinum that exceeded most literature values for water-gas shift reaction on Pt-CeO x catalysts. The high activity was attributed to the significant fraction of platinum/ceria interfacial contact. We found that these results show the promise of supercritical fluid deposition as a scalable means of synthesizing highly active supported metal catalysts that offer efficient utilization of precious metals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRSDate not supplied

Analysis of Historical International Space Station Logistical Mass Delivery

Crewed space exploration missions are extremely logistics dependent, as cargo requirements shape numerous program elements such as vehicle and habitat size. Logistics mass is the mass of items like food and clothing that are not a part of the vehicle or habitat, yet are required by the crew to complete the mission. Numerous studies, such as the Human Exploration Research Analog (HERA) and the Human Exploration Spacecraft Testbed for Integration and Advancement (HESTIA) 20-foot chamber analog, have been conceived to research the rates at which crews consume logistics mass. These analogs can simulate many aspects of life in space, including confinement, isolation, limited supplies, and, in certain experiments, the habitat pressure. However, some aspects of space exploration, such as the effects of low gravity and the use of space-based amenities, cannot currently be tested on the ground. In this paper, International Space Station (ISS) manifest data obtained through the National Aeronautics and Space Administration’s (NASA’s) Mission Integration Database Application System (MIDAS) portal is used as a precursor to space-based analogs. The objective of the analysis is determining the breakdown of logistics mass used in space exploration. This identifies potential areas of improvement and highlights the rates at which significant items are supplied, aiding in the weighing of alternative options such as utilizing in space manufacturing for supplies vs. manifesting spares, or cleaning clothing in flight vs. discarding it. Official flight manifests ranging a span of 878 days, just short of the three-year length of a potential human mission to Mars, were analyzed to find the rates at which astronauts consumed various logistics supplies. From this analysis we have found that contrary to our own hypothesis, ‘food’ was not the largest portion of the supplied mass. Instead, ‘Environmental Control and Life Support Systems’ (ECLSS) contributed 34% of the overall supplied mass, followed by ‘Science and Outfitting,’ which contributed 29%. Food totaled less than a quarter (21% of the resupplied mass, while other items of focus in mass reduction efforts such as ‘Hygiene’ (6%), ‘Clothing’ (3%), and ‘Operational Supplies’ (4%) each contributed less than a tenth of the supplied mass. This data suggests that by categorizing and analyzing the data based on an alternative taxonomy and analyzing the full supply manifests rather than handpicked items, we have revealed unexpectedly significant items which had not been previously tracked by exploration logistics efforts. For example, toilet hardware made up 4% of ECLSS mass, and laptop hardware and multi-tools each made up 10% of operational supplies mass. Additionally, the ‘Specialized Clothing’ subcategory containing fire protective equipment, coveralls, and penguin suits made up 15% of the overall clothing mass. By identifying these newly found significant items, we can create more realistic mass estimates for exploration missions and direct mass reduction efforts to new areas, potentially leading to lower future mission masses.

Logistics↗

DOE OSTI2019

A Polymer-Oriented Self-Assembly Strategy toward Mesoporous Metal Oxides with Ultrahigh Surface Areas

Mesoporous metal oxides (MMOs) have attracted comprehensive attention in many fields, including energy storage, catalysis, and separation. Current synthesis of MMOs mainly involve use of surfactants as templates to generate mesopores and organic reagents as solvents to hinder hydrolysis and condensation of inorganic precursors, which is adverse to adjusting the interactions between surfactants and inorganic precursors. The resulting products have uncontrollable pore structure, crystallinity, and relatively lower surface areas. Here, a facile and general polymer-oriented self-assembly strategy to synthesize a series of MMOs (e.g., TiO 2 , ZrO 2 , NbO 5 , Al 2 O 3 , Ta 2 O 5 , HfO 2 , and SnO 2 ) by using cationic polymers as porogens and metal alkoxides as metal oxide precursors in a robust aqueous synthesis system are reported. Nitrogen adsorption analysis and transmission electron microscopy confirm that the obtained MMOs have ultrahigh specific surface areas and large pore volumes (i.e., 733 m 2 g –1 and 0.485 cm 3 g –1 for mesoporous TiO 2 ). Moreover, the structural parameters (surface area, pore size, and pore volume) and crystallinity can be readily controlled by tuning the interactions between cationic polymers and precursors. The as-synthesized crystalline mesoporous TiO 2 exhibits promising performance in photocatalytic water splitting of hydrogen production and a high hydrogen production rate of 3.68 mol h –1 g –1 .

36 MATERIALS SCIENCE↗

DOE OSTI2018

Hyperspectral remote sensing of fire: state-of-the-art and future perspectives

We report that fire is a widespread Earth system process with important carbon and climate feedbacks. Multispectral remote sensing has enabled mapping of global spatiotemporal patterns of fire and fire effects, which has significantly improved our understanding of interactions between ecosystems, climate, humans and fire. With several upcoming spaceborne hyperspectral missions like the Environmental Mapping And Analysis Program (EnMAP), the Hyperspectral Infrared Imager (HyspIRI) and the Precursore Iperspettrale Della Missione Applicativa (PRISMA), we provide a review of the state-of-the-art and perspectives of hyperspectral remote sensing of fire. Hyperspectral remote sensing leverages information in many (often more than 100) narrow (smaller than 20 nm) spectrally contiguous bands, in contrast to multispectral remote sensing of few (up to 15) non-contiguous wider (greater than 20 nm) bands. To date, hyperspectral fire applications have primarily used airborne data in the visible to short-wave infrared region (VSWIR, 0.4 to 2.5 μm). This has resulted in detailed and accurate discrimination and quantification of fuel types and condition, fire temperatures and emissions, fire severity and vegetation recovery. Many of these applications use processing techniques that take advantage of the high spectral resolution and dimensionality such as advanced spectral mixture analysis. So far, hyperspectral VSWIR fire applications are based on a limited number of airborne acquisitions, yet techniques will approach maturity for larger scale application when spaceborne imagery becomes available. Recent innovations in airborne hyperspectral thermal (8 to 12 μm) remote sensing show potential to improve retrievals of temperature and emissions from active fires, yet these applications need more investigation over more fires to verify consistency over space and time, and overcome sensor saturation issues. Furthermore, hyperspectral information and structural data from, for example, light detection and ranging (LiDAR) sensors are highly complementary. Finally, their combined use has demonstrated advantages for fuel mapping, yet its potential for post-fire severity and combustion retrievals remains largely unexplored.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2003

Unveiling the Nature of Soft Gamma Repeaters and Magnetars

We briefly describe some results of our ongoing study of Soft Gamma Repeater (SGR) bursts with Rossi X-ray Timing Explorer (RXTE) satellite. We have detected evidence of cyclotron resonance absorption features from the SGR 1806-20 in the spectrum of a long, complex precursor that preceded a strong burst. The observation is made by the analysis of data from the RXTE. The features consist of a narrow 5.0 keV absorption line together with modulation near its second and third harmonics (at 11.2 keV and 17.5 keV respectively). The line features are transient and are detected in the harder radiation part of the precursor. The 5.0 keV feature is strong, with an equivalent width of approximately 500 eV and a narrow width of less than 0.4 keV. Interpreting the features as electron cyclotron lines in the context of accretion models leads to a large mass radius ratio (M/R greater than 0.3 M sun/km) that is inconsistent with neutron stars or that requires a low (5-7) x l0(exp 11)G magnetic field that is unlikely for SGRs. The line widths are also narrow compared with those of electron cyclotron resonances observed so far in X-ray pulsars. In the magnetar picture, the features are plausibly explained as ion cyclotron resonances in an ultra-strong magnetic field that have recently been predicted from magnetar candidates. In this view, the 5.0 keV feature is consistent with a proton cyclotron fundamental whose energy and width are close to model predictions. The line energy would correspond to a surface magnetic field of 1.0 x 10(exp 15)G for SGR 1806-20, in good agreement with that inferred from the spin-down measure in the source. Following the first evidence of proton cyclotron features from SGR 1806-20, we performed a comprehensive search of a large number of bursts from the source. We detected the 5 keV absorption feature in a variety of bursts, confirming our initial discovery and establishing the presence of the feature in the source s burst spectra. The line feature is well explained as proton cyclotron resonance in an ultra-strong magnetic field, offering a direct measurement of SGR 1806-20 s magnetic field (B approx. 10(exp l5)G) and a clear evidence of a magnetar. Together with the source's spin-down rate, the feature also provided the first measurement of the gravitational redshift, mass and radius of a magnetar.

Parke, William↗