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All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Heterogeneous Polymer Dynamics Explored Using Static 1H NMR Spectra

NMR spectroscopy continues to provide important molecular level details of dynamics in different polymer materials, ranging from rubbers to highly crosslinked composites. It has been argued that thermoset polymers containing dynamic and chemical heterogeneities can be fully cured at temperatures well below the final glass transition temperature (Tg). In this paper, we described the use of static solid-state 1H NMR spectroscopy to measure the activation of different chain dynamics as a function of temperature. Near Tg, increasing polymer segmental chain fluctuations lead to dynamic averaging of the local homonuclear proton-proton (1H-1H) dipolar couplings, as reflected in the reduction of the NMR line shape second moment (M2) when motions are faster than the magnitude of the dipolar coupling. In general, for polymer systems, distributions in the dynamic correlation times are commonly expected. To help identify the limitations and pitfalls of M2 analyses, the impact of activation energy or, equivalently, correlation time distributions, on the analysis of 1H NMR M2 temperature variations is explored. It is shown by using normalized reference curves that the distributions in dynamic activation energies can be measured from the M2 temperature behavior. An example of the M2 analysis for a series of thermosetting polymers with systematically varied dynamic heterogeneity is presented and discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Quantifying the cooperative evolution of microphase segregation and nanostructural order in annealed polyurethanes of MDI-BDO-PTHF

Here, we quantify the relationship between microphase segregation and local structure development in thermoplastic polyurethanes. Samples were prepared with varying ratios of 4,40 -methylene diphenyl diisocyanate (MDI) and 1,4-butanediol (BDO) to polytetrahydrofuran (PTHF) and annealed at temperatures T a between RT–140 °C for 20 h each. Distinct populations of smaller and larger ordered domains are distinguished by pair distribution func tion analysis. The intermediate-range order of nanoscale hard domains in the paracrystalline state (form I) is directly extracted and characterized. The results suggest that form I of the MDI-BDO:PTHF system presents a conformational and packing order similar to the form III structure, typically obtained from stretching/annealing, but with limited spatial coherence of 3–7 nm. Heating above T g of the hard segments is necessary to achieve a substantial structural response from the annealing treatment. Increasing T a promotes purification of the soft phase via microphase segregation, coalescence of the hard blocks, and growth of paracrystalline phase, while a minority fraction of longer-range ordered domains left over from production remains relatively constant. We observe a composition-dependent decrease in the average nearest-neighbor dis tance that can be correlated with the greater number of C C, C N, and C O bonds with increased hard segment content. A non-linear deviation in the trend is observed to correlate with sample densification. The mechanical and thermal behavior of the samples is intimately tied to the segregation state.

processing-structure-properties↗
DOE OSTI2019

Origin of High Activity and Durability of Twisty Nanowire Alloy Catalysts under Oxygen Reduction and Fuel Cell Operating Conditions

The ability to control the surface composition and morphology of alloy catalysts is critical for achieving high activity and durability of catalysts for oxygen reduction reaction (ORR) and fuel cells. Here, this report describes an efficient surfactant-free synthesis route for producing a twisty nanowire (TNW) shaped platinum–iron (PtFe) alloy catalyst (denoted as PtFe TNWs) with controllable bimetallic compositions. PtFe TNWs with an optimal initial composition of ~24% Pt are shown to exhibit the highest mass activity (3.4 A/mg Pt , ~20 times higher than that of commercial Pt catalyst) and the highest durability (<2% loss of activity after 40000 cycles and <30% loss after 120000 cycles) among all PtFe-based nanocatalysts under ORR or fuel cell operating conditions reported so far. Using ex situ and in situ synchrotron X-ray diffraction coupled with atomic pair distribution function (PDF) analysis and 3D modeling, the PtFe TNWs are shown to exhibit mixed face-centered cubic (fcc)-body-centered cubic (bcc) alloy structure and a significant lattice strain. A striking finding is that the activity strongly depends on the composition of the as-synthesized catalysts and this dependence remains unchanged despite the evolution of the composition of the different catalysts and their lattice constants under ORR or fuel cell operating conditions. Notably, dealloying under fuel cell operating condition starts at phase-segregated domain sites leading to a final fcc alloy structure with subtle differences in surface morphology. Due to a subsequent realloying and the morphology of TNWs, the surface lattice strain observed with the as-synthesized catalysts is largely preserved. This strain and the particular facets exhibited by the TNWs are believed to be responsible for the observed activity and durability enhancements. These findings provide new insights into the correlation between the structure, activity, and durability of nanoalloy catalysts and are expected to energize the ongoing effort to develop highly active and durable low-Pt-content nanowire catalysts by controlling their alloy structure and morphology.

25 ENERGY STORAGE↗
NASA NTRS2011

Characterization of the as Manufactured Variability in a CVI SiC/SiC Woven Composite

The microstructure of a 2D woven ceramic matrix composite displays significant variability and irregularity. For example, a chemical vapor infiltrated (CVI) SiC/SiC composite exhibits significant amount of porosity arranged in irregular patterns. Furthermore, the fiber tows within a ply frequently have irregular shape and spacing, and the stacked plies are often misaligned and irregularly nested within each other. The goal of an ongoing project at NASA Glenn is to investigate the effects of the complex microstructure and its variability on the properties and the durability of the material. One key requirement for this effort is the development of methods to characterize the distribution in as-fabricated ceramic matrix composite (CMC) microstructures with the objective of correlating microstructural distribution parameters with mechanical performance. An initial task in this effort was to perform quantitative image analysis of polished cross sections of CVI SiC/SiC composite specimens. This analysis provided sample distributions of various microstructural composite features, including: inter-tow pore sizes and shapes, transverse sectioned tow sizes and shapes, and within ply tow spacing. This information can then be used to quantify the effect of extreme values of these features on the local stress state with the goal of determining the likelihood of matrix cracking at a given external load.

Bonacuse, Peter J.↗
DOE OSTI2021

Illustrated formalisms for total scattering data: a guide for new practitioners

The total scattering method is the simultaneous study of both the real- and reciprocal-space representations of diffraction data. While conventional Bragg-scattering analysis (employing methods such as Rietveld refinement) provides insight into the average structure of the material, pair distribution function (PDF) analysis allows for a more focused study of the local atomic arrangement of a material. Generically speaking, a PDF is generated by Fourier transforming the total measured reciprocal-space diffraction data (Bragg and diffuse) into a real-space representation. However, the details of the transformation employed and, by consequence, the resultant appearance and weighting of the real-space representation of the system can vary between different research communities. As the worldwide total scattering community continues to grow, these subtle differences in nomenclature and data representation have led to conflicting and confusing descriptions of how the PDF is defined and calculated. This paper provides a consistent derivation of many of these different forms of the PDF and the transformations required to bridge between them. Some general considerations and advice for total scattering practitioners in selecting and defining the appropriate choice of PDF in their own research are presented. This contribution aims to benefit people starting in the field or trying to compare their results with those of other researchers.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Disc dichotomy signature in the vertical distribution of [Mg/Fe] and the delayed gas infall scenario

Context. Analysis of the Apache Point Observatory Galactic Evolution Experiment project (APOGEE) data suggests the existence of a clear distinction between two sequences of disc stars in the [α/Fe] versus [Fe/H] abundance ratio space, known as the high- and low-α sequence, respectively. This dichotomy also emerges from an analysis of the vertical distribution of the [α/Fe] abundance ratio. Aims. We aim to test whether the revised two-infall chemical evolution models designed to reproduce the low- and high-α sequences in the [α/Fe] versus [Fe/H] ratios in the solar neighbourhood are also capable of predicting the disc bimodality observed in the vertical distribution of [Mg/Fe] in APOGEE DR16 data. Methods. Along with the chemical composition of the simple stellar populations born at different Galactic times predicted by our reference chemical evolution models in the solar vicinity, we provide their maximum vertical height above the Galactic plane |zmax| computed assuming the relation between the vertical action and stellar age in APOGEE thin-disc stars. Result. The vertical distribution of the [Mg/Fe] abundance ratio predicted by the reference chemical evolution models is in agreement with that observed when combining the APOGEE DR16 data (chemical abundances) with the astroNN catalogue (stellar ages, orbital parameters) for stars younger than 8 Gyr (only low-α sequence stars). Including the high-α disc component, the dichotomy in the vertical [Mg/Fe] abundance distribution is reproduced considering the observational cut in the Galactic height of |z|< 2 kpc. However, our model predicts an overly flat (almost constant) growth of the maximum vertical height |zmax| quantity as a function of [Mg/Fe] for high-α objects in contrast with the median values from APOGEE data. Possible explanations for such a tension are that: (i) the APOGEE sample with |z|< 2 kpc is more likely than ours to be contaminated by halo stars, causing the median values to be kinematically hotter, and (ii) external perturbations – such as minor mergers – that the Milky Way experienced in the past could have heated up the disc, and the heating of the orbits cannot be modeled by only scattering processes. Assuming a disc dissection based on chemistry for APOGEE-DR16 stars (|z|< 2 kpc), the observed |zmax| distributions for high-α and low-α sequences are in good agreement with our model predictions if we consider the errors in the vertical action estimates in the calculation. Moreover, a better agreement between predicted and observed stellar distributions at different Galactic vertical heights is achieved if asteroseismic ages are included as a constraint in the best-fit model calculations. Conclusions. The signature of a delayed gas infall episode, which gives rise to a hiatus in the star formation history of the Galaxy, are imprinted both in the [Mg/Fe] versus [Fe/H] relation and in vertical distribution of [Mg/Fe] abundances in the solar vicinity.

79 ASTRONOMY AND ASTROPHYSICS↗
NASA NTRS1992

Project APEX: Advanced Phobos Exploration. Manned mission to the Martian moon Phobos

The manned exploration of Mars is a massive undertaking which requires careful consideration. A mission to the moon of Mars called Phobos as a prelude to manned landings on the Martian surface offers some advantages. One is that the energy requirements, in terms of delta 5, is only slightly higher than going to the Moon's surface. Another is that Phobos is a potential source of water and carbon which could be extracted and processed for life support and cryogenic propellants for use in future missions; thus, Phobos might serve as a base for extended Mars exploration or for exploration of the outer planets. The design of a vehicle for such a mission is the subject of our Aerospace System Design course this year. The materials and equipment needed for the processing plant would be delivered to Phobos in a prior unmanned mission. This study focuses on what it would take to send a crew to Phobos, set up the processing plant for extraction and storage of water and hydrocarbons, conduct scientific experiments, and return safely to Earth. The size, configuration, and subsystems of the vehicle are described in some detail. The spacecraft carries a crew of five and is launched from low Earth orbit in the year 2010. The outbound trajectory to Mars uses a gravitational assisted swing by of Venus and takes eight months to complete. The stay at Phobos is 60 days at which time the crew will be engaged in setting up the processing facility. The crew will then return to Earth orbit after a total mission duration of 656 days. Both stellar and solar observations will be conducted on both legs of the mission. The design of the spacecraft addresses human factors and life science; mission analysis and control; propulsion; power generation and distribution; thermal control; structural analysis; and planetary, solar, and stellar science. A 0.5 g artificial gravity is generated during transit by spinning about the lateral body axis. Nuclear thermal rockets using hydrogen as fuel are selected to reduce total launch mass and to shorten the duration of the mission. The nuclear systems also provide the primary electrical power via dual mode operation. The overall spacecraft length is 110 meters and the total mass departing from low Earth orbit is 900 metric tons.

Source record↗
DOE OSTI2023

ECAR-6599 Rev 0 PCAT Walls Temperature Distribution, Beryllium Inserts and Fuel-to-Fuel Gap Tolerance Analysis

This document reports the primary coolant system structures temperature distribution for the Primary Coolant Apparatus Test (PCAT) of the MARVEL microreactor. The temperature distributions have been calculated using the RELAP5-3D system code, using one-dimensional approximation, and considering radial heat losses, effects of thermal insulators, and hot spot factors. Sensitivities on the Be inserts dimensions tolerances and heater-to-heater pitch has been also performed, investigating the effects on the NaK and heater cartridge sheath temperatures.

21 - SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLAN↗
DOE OSTI2020

Distributed Solar Utility Tariff and Revenue Impact Analysis: A Guidebook for International Practitioners

Depending on a range of technical, economic, policy, regulatory, and market-related factors, the adoption of DPV may have a net positive or negative financial impact on utilities and ratepayers. This guidebook provides a methodological approach for quantifying the net financial impact of DPV on utilities (in the form of “net revenue losses”) and ratepayers (in the form of “net tariff impacts”). Written for technical staff at utilities, regulatory bodies, energy ministries, research institutes, and civil society organizations who wish to better understand the financial impacts of DPV in their jurisdiction, this guidebook can be used to inform important decisions regarding DPV compensation, tariff design, and regulatory cost allocations, among other aspects. It is focused exclusively on customer-sited DPV systems and adopts a primarily cost-based (as opposed to an equally valid value-based) perspective to understanding DPV financial impacts. The approach for calculating net revenue losses can be applied in nearly any utility jurisdiction, regardless of institutional arrangements, business models, or regulatory paradigms.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗
DOE OSTI2022

Fatty acid capped, metal oxo clusters as the smallest conceivable nanocrystal prototypes

Metal oxo clusters of the type M 6 O 4 (OH) 4 (OOCR) 12 (M = Zr or Hf) are valuable building blocks for materials science. Here, we synthesize a series of zirconium and hafnium oxo clusters with ligands that are typically used to stabilize oxide nanocrystals (fatty acids with long and/or branched chains). The fatty acid capped oxo clusters have a high solubility but do not crystallize, precluding traditional purification and single-crystal XRD analysis. We thus develop alternative purification strategies and we use X-ray total scattering and Pair Distribution Function (PDF) analysis as our main method to elucidate the structure of the cluster core. We identify the correct structure from a series of possible clusters (Zr3, Zr4, Zr6, Zr12, Zr10, and Zr26). Excellent refinements are only obtained when the ligands are part of the structure model. Further evidence for the cluster composition is provided by nuclear magnetic resonance (NMR), infrared spectroscopy (FTIR), thermogravimetry analysis (TGA), and mass spectrometry (MS). We find that hydrogen bonded carboxylic acid is an intrinsic part of the oxo cluster. Using our analytical tools, we elucidate the conversion from a Zr6 monomer to a Zr12 dimer (and vice versa), induced by carboxylate ligand exchange. Finally, we compare the catalytic performance of Zr12-oleate clusters with oleate capped, 5.5 nm zirconium oxide nanocrystals in the esterification of oleic acid with ethanol. The oxo clusters present a five times higher reaction rate, due to their higher surface area. Since the oxo clusters are the lower limit of downscaling oxide nanocrystals, we present them as appealing catalytic materials, and as atomically precise model systems. In addition, the lessons learned regarding PDF analysis are applicable to other areas of cluster science as well, from semiconductor and metal clusters, to polyoxometalates.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Uncertainty Quantification and Sensitivity Analysis of Nuclear Construction Cost Reduction Pathways

High construction costs have plagued recent nuclear projects and they hamper the widespread deployment of nuclear technology. The Nuclear Cost Reduction Tool is a plant economic framework that quantifies the impact that various plant design and construction attributes have on construction costs and cost overruns and shows the positive effects of learning over a series of deployments. However, a downside of the current model is that all model outputs and capabilities are deterministic. To provide a more comprehensive view, this study evaluated the impact of model parameter uncertainty through a sensitivity analysis applied to 18 model parameters. This approach quantified the impact of model uncertainty on the output variables of Net Overnight Capital Cost (Net OCC), Construction Duration (CD), and Levelized Cost of Electricity (LCOE). Monte Carlo analysis revealed uncertainty distributions for these variables, showing that absolute uncertainty decreases over a series of deployments. A local sensitivity analysis showed that even small parameter perturbations (5%) can have a significant impact on project execution, highlighting areas that could reduce costs by billions across an order book of plants. The results of this study have improved the understanding of the model and identified the most impactful model parameters and construction attributes.

Levelized Cost of Electricity↗
NASA NTRS1978

The McDonald Observatory lunar laser ranging project

A summary of the activities of the McDonald lunar laser ranging station at Fort Davis for the FY 77-78 fiscal year is presented. The lunar laser experiment uses the observatory 2.7m reflecting telescope on a thrice-per-day, 21-day-per-lunation schedule. Data are recorded on magnetic tapes and sent to the University of Texas at Austin where the data is processed. After processing, the data is distributed to interested analysis centers and later to the National Space Science Data Center where it is available for routine distribution. Detailed reports are published on the McDonald operations after every fourth lunation or approximately once every 115 days. These reports contain a day-by-day documentation of the ranging activity, detailed discussions of the equipment development efforts, and an abundance of other information as is needed to document and archive this important data type.

Silverberg, E. C.↗
NASA NTRS1985

Cosmogenic Mn-53 in meteorites

The distributions of the Mn-53 contents in 106 nonantarctic and 112 antarctic chondrites were analyzed. A correlation analysis of these distributions showed that the correlation coefficient is a maximum r sub max = 0.75 plus or minus 0.03) when the histogram for antarctic chondrites is displaced by 40 plus or minus 8 dpm kg-1Fe towards lower Mn-53 contents. The distribution of Mn-53 saturated contents in nonantarctic ordinary chondrites was investigated as a function of their radiation age (T). It is found that the Mn-53 average content is higher by (21 plus or minus 9)% in H-chondrites with radiation age T approximately 12 Myr than in thse with T 12 Myr. This effect can be attributed to the fact that a considerable proportion of H-chondrites with T 12 Myr originates from a comet or from the objects of Chiron like, with the orbits more inclined to the ecliptic plane and/or more extended, which caused their irradiation by cosmic rays of higher intensity.

Alexeev, V. A.↗
NASA NTRS2013

Cleaning Study of Genesis Sample 60487

The Genesis mission collected solar wind and brought it back to Earth in order to provide precise knowledge of solar isotopic and elemental compositions. The ions in the solar wind were stopped in the collectors at depths on the order of 10 to a few hundred nanometers. This shallow implantation layer is critical for scientific analysis of the composition of the solar wind and must be preserved throughout sample handling, cleaning, processing, distribution, preparation and analysis. Particles of Genesis wafers, brine from the Utah Testing Range and an organic film have deleterious effects on many of the high-resolution instruments that have been developed to analyze the implanted solar wind. We have conducted a correlative microscopic study of the efficacy of cleaning Genesis samples with megasonically activated ultrapure water and UV/ozone cleaning. Sample 60487, the study sample, is a piece of float-zone silicon from the B/C array approximately 4.995mm x 4.145 mm in size

Kuhlman, Kim R.↗
NASA NTRS2014

Cellulose Acetate Replica Cleaning Study of Genesis Non-Flight Sample 3CZ00327

The Genesis mission collected solar wind and brought it back to Earth in order to provide precise knowledge of solar isotopic and elemental compositions. The ions in the solar wind were stopped in the collectors at depths on the order of 10 to a few hundred nanometers. This shallow implantation layer is critical for scientific analysis of the composition of the solar wind and must be preserved throughout sample handling, cleaning, processing, distribution, preparation and analysis. We are working interactively with the community of scientists analyzing Genesis samples, using our unique laboratory facilities -- and, where needed, our unique cleaning techniques -- to significantly enhance the science return from the Genesis mission. This work is motivated by the need to understand the submicron contamination on the collectors in the Genesis payload as recovered from the crash site in the Utah desert, and -- perhaps more importantly -- how to remove it. That is, we are evaluating the effectiveness of the wet-chemical "cleaning" steps used by various investigators, to enable them to design improved methods of stripping terrestrial contamination from surfaces while still leaving the solar-wind signal intact.

Kuhlman, K. R.↗
NASA NTRS1992

Effect of Index of Refraction on Radiation Characteristics in a Heated Absorbing, Emitting, and Scattering Layer

The index of refraction can considerably influence the temperature distribution and radiative heat flow in semitransparent materials such as some ceramics. For external radiant heating, the refractive index influences the amount of energy transmitted into the interior of the material. Emission within a material depends on the square of its refractive index, and hence this emission can be many times that for a biackbody radiating into a vacuum. Since radiation exiting through an interface into a vacuum cannot exceed that of a blackbody, there is extensive reflection at the internal surface of an interface, mostly by total internal reflection. This redistributes energy within the layer and tends to make its temperature distribution more uniform. The purpose of the present analysis is to show that, for radiative equilibrium in a gray layer with diffuse interfaces, the temperature distribution and radiative heat flux for any index of refraction can be obtained very simply from the results for an index of refraction of unity. For the situation studied here, the layer is subjected to external radiative heating incident on each of its surfaces. The material emits, absorbs, and isotropically scatters radiation. For simplicity the index of refraction is unity in the medium surrounding the layer. The surfaces of the layer are assumed diffuse. This is probably a reasonable approximation for a ceramic layer that has not been polished. When transmitted radiation or radiation emitted from the interior reaches the inner surface of an interface, the radiation is diffused and some of it thereby placed into angular directions for which there is total internal reflection. This provides a trapping effect for retaining energy within the layer and tends to equalize its temperature distribution. An analysis of temperature distributions in absorbing-emitting layers, including index of refraction effects, was developed by Gardon (1958) to predict cooling and heat treating of glass plates. The interfaces were optically smooth; the resulting specular reflections were computed from the Fresnel reflection laws. This provides a somewhat different behavior than for diffuse interfaces. A similar application was for heating that occurs in a window of a re-entry vehicle (Fowle et al., 1969). A number of recent papers (Rokhsaz and Dougherty, 1989; Ping and Lallemand, 1989; Crosbie and Shieh, 1990) further examined the effects of Fresnel boundary reflections and nonunity refractive index. Other examples of analyses of both steady and transient heat transfer to single or multiple plane layers (Amlin and Korpela, 1979; Tarshis et al., 1969) have used diffuse assumptions at the interfaces as in the present study

Siegel, R.↗
NASA NTRS2016

Catastrophic Impact of Silicon on Silicon: Unraveling the Genesis Impact Using Sample 61881

The Genesis mission collected solar wind and brought it back to Earth in order to provide precise knowledge of solar isotopic and elemental compositions. The ions in the solar wind were stopped in the collectors at depths on the order of 10 to a few hundred nanometers. This shallow implantation layer is critical for scientific analysis of the composition of the solar wind and must be preserved throughout sample handling, cleaning, processing, distribution, preparation and analysis. The current work is motivated by the need to understand the interaction of the Genesis payload with contamination during the crash in the Utah desert. Silicon contamination has been found to be notoriously difficult to remove from silicon samples despite multiple cleanings with multiple techniques. However, the question has been posed, "Does the silicon really need to be removed for large area analyses?." If the recalcitrant silicon contamination is all pure silicon from fractured collectors, only a very tiny fraction of that bulk material will contain solar wind, which could skew the analyses. This could be complicated if the silicon trapped other materials and/or gases as it impacted the surface.

Kuhlman, K. R.↗