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DOE OSTI2022

Thermal conductivity of salvaged fused cast alumina used in the glass industry

Fused cast alumina (FCA) has been and continues to be used as a refractory material in energy intensive industries such as glass melting and chemical processing. In-service degradation due to high temperature exposure in harsh environment affects the designed furnace thermal profiles and energy consumption. Phase transformation may occur at the refractory hot face during glass melting altering the properties. Three FCA blocks recovered from industrial furnaces were investigated in this study. The as-received FCA consists primarily of a mixture of alpha (α) and beta (β) alumina that has a thermal conductivity value of 5–6 W/mK. The Hot Disk method was used to obtain thermal conductivity directly on the refractory blocks. At the hot face, a transformation from β to α alumina occurred and was confirmed by an X-ray diffraction study. Thermal conductivity measurements as a function of position also showed a clear transition from β to α alumina at both ends of a complete block with no voids. Thermal conductivity of the α alumina tripled compared to β alumina. This study provides important information of heat transfer and thermal conductivity evolution to refractory manufacturers and users.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Highly Loaded Sulfur Cathode, Coated Separator and Gel Electrolyte for High Rate Li-Sulfur Batteries

As one of DOE Battery 500 Seedling projects, Cornell University and EIC Labs investigated and developed i) highly loaded sulfur cathodes (> 3 mg/cm 2 ), ii) hybrid separators, and iii) gel ceramic electrolytes (GCE) to mitigate the low rate capability, shuttling effect and limited cycle life in high performance Li-Sulfur batteries. Scalable nanomanufacturing processes such as air-controlled electrospray (ACES) and gas-assisted electrospinning (GAES) have been utilized to develop directly deposited electrodes and polymer/ceramic hybrid separators. First, in the development of highly loaded cathodes, alternating layers of sulfur impregnated mesoporous carbon and graphene were fabricated via ACES and the resulting layered cathodes and coated separators exhibit higher capacity and capacity retention (about 1,000 mAh/g capacity with less than 0.02% fade/cycles) than single layer cathode or cathode prepared by conventional slurry cast. Alternating layer approach via ACES has been applied to high loading systems (3 - 5 mg S/cm 2 ), demonstrating the potential to increase sulfur utilization and capacity retention. We have also incorporated iron oxides (Fe 3 O 4 ) into S/mesoporous carbon/graphene cathodes to enhance sulfur utilization and mitigation of polysulfide shuttling. and the effect of Fe 3 O 4 in mesoporous carbon and Gr is highly pronounced at high C rates of 1C and 2C cycling performance. To further improve the cathodes at high rates, graphene nanoribbons (GNR) which can promote ion transport were incorporated in the cathode, resulting in 550 mAh/g at 5C/5C rates. Hybrid Li-ion/Li-S cathodes has also been explored to better engage unreacted polysulfides during charge/discharge. S/LFP hybrid cathodes offer higher sulfur utilization and enhanced rate capability, as well as higher areal loading. This study suggests inclusion of iron phosphide (Fe2P) which can chemically interact with polysulfides can further enhance sulfur utilization and mitigation of soluble polysulfides at high rates. Secondly, in the development of hybrid separators, we first employed graphene coating on the commercial polyolefin separators, which exhibits higher capability, better capacity retention and enhanced rate capability. To improve the rate capability with enhanced safety features such as thermal stability and nonflammability, we developed polymer/ceramic hybrids based on thermally stable polyimide (PI) and room temperature curable ceramic precursors such as organopolysilazane (OPSZ) or polysilsesquioxanes (PSSQ), which exhibit no shrinkages up to 300 ºC and non-flammability. To improve mechanical properties and electrochemical stability, polybenzimidazole (PBI) and alumina have been incorporated in polymer/ceramic hybrid separator, replacing PI and OPSZ/PSSQ, respectively. Finally, the gel ceramic electrolyte (GCE) based on ceramic cross linkers have been applied to make Li-S cells even safer and also to mitigate the polysulfide shuttling further. The resulting gel ceramic electrolyte offers improved capacity retention and rate capability, and also effectively mitigates polysulfide shuttling which was also confirmed by modeling. Inclusion of high ion conducting additives into GCE together with polymer/ceramic hybrid separators exhibit the higher ionic conductivity than liquid electrolyte with commercial polyolefin separator. We demonstrated that the developed highly loaded sulfur cathodes, polymer/ceramic hybrid separators and gel ceramic electrolyte can effectively mitigate the low rate capability, shuttling effect and limited cycle life in high performance Li-Sulfur batteries with improved safety.

25 ENERGY STORAGE↗

NASA NTRS2009

Tensile Properties and Microstructure of Inconel 718 Fabricated with Electron Beam Freeform Fabrication (EBF(sup 3))

Electron beam freeform fabrication (EBF3) direct metal deposition processing was used to fabricate two Inconel 718 single-bead-width wall builds and one multiple-bead-width block build. Specimens were machined to evaluate microstructure and room temperature tensile properties. The tensile strength and yield strength of the as-deposited material from the wall and block builds were greater than those for conventional Inconel 718 castings but were less than those for conventional cold-rolled sheet. Ductility levels for the EBF3 material were similar to those for conventionally-processed sheet and castings. An unexpected result was that the modulus of the EBF3-deposited Inconel 718 was significantly lower than that of the conventional material. This low modulus may be associated with a preferred crystallographic orientation resultant from the deposition and rapid solidification process. A heat treatment with a high solution treatment temperature resulted in a recrystallized microstructure and an increased modulus. However, the modulus was not increased to the level that is expected for Inconel 718.

Bird, R. Keith↗

DOE OSTI2023

Influence of oxygen on performance of multi-principal element alloy as braze filler for Ni-base alloys

In manufacturing of multi-principal element alloys (MPEAs), the casting process is often a primary point of oxygen introduction to the material system, which was demonstrated by the laboratory scale button arc-melting process. Oxygen introduction raises concerns for the mechanical performance of these alloys if employed as structural materials alone or in engineering applications, such as serving as filler materials to enable joining of similar or dissimilar alloy pairs that are conventionally considered difficult to join. In this work, oxide inclusions in an as-cast off-equiatomic MnFeCoNiCu MPEA and Ni-base alloy braze joints made with this MPEA were evaluated by synchrotron x-ray diffraction mapping and electron microscopy. MnO was found to be prevalent throughout the cast MPEA and was chemically reduced during brazing by trace Al from the base material, Ni-base Alloy 600. Incomplete reaction of the MnO with Al, and some alternative reaction with Cr, left a mixture of MnO, Al 2 O 3 , and Cr 2 O 3 in the as-brazed joint, with the oxides concentrated near the braze centerline due to directional solidification. Further, in the braze joints, the non-oxide constituent phases detected were an FCC matrix and particles of Cr 23 C 6 , Cr 7 C 3 , and TiN which are all native to Alloy 600. The evolution of oxides within the brazed joints at elevated service temperatures of 600-800°C was also evaluated. While MnO and Al 2 O 3 were stable during high-temperature service, Cr 2 O 3 particles grew to several hundred microns, with dissolved oxygen in the MPEA providing a significant source for oxide growth. Comparing tensile performance of the as-brazed condition with post-service conditions showed that the evolution of oxide particles contributed to an increase in strength and decrease in ductility of the brazed joints. Evaluating particle morphologies among fracture surfaces of individual specimens demonstrated that large Cr 2 O 3 particles and continuous cluster networks of Al 2 O 3 were the features most detrimental to total elongation. Hence, unmitigated evolution of oxygen-containing species during brazing and service conditions is detrimental to the ductility of the brazed joints, which highlights the importance of oxygen control in initial manufacturing of MPEAs for engineering applications.

36 MATERIALS SCIENCE↗

NASA NTRS1977

The direct observation of solidification as a function of gravity level

A saturated solution of NH4Cl was solidified on earth at 1 g and in a suborbital rocket flight at .00001 g. In the 1 g experiments, macrosegregation caused by the gravitational acceleration was marked. Nucleation started at the cold walls after which dendrites and dendritic debris were swept into the center of the cuvette by convective fluid flow. Secondary dendrite arms were oriented toward the cold wall. When solidified in low g, only four nuclei grew to form the complete casting. There were no free floating crystals or visible dendrite remelting. The lack of fluid flow allowed symmetrical dendrite growth into the fluid.

Johnston, M. H.↗

DOE OSTI2020

Prospects for fundamental physics with LISA

In this paper, which is of programmatic rather than quantitative nature, we aim to further delineate and sharpen the future potential of the LISA mission in the area of fundamental physics. Given the very broad range of topics that might be relevant to LISA,we present here a sample of what we view as particularly promising fundamental physics directions. We organize these directions through a “science-first” approach that allows us to classify how LISA data can inform theoretical physics in a variety of areas. For each of these theoretical physics classes, we identify the sources that are currently expected to provide the principal contribution to our knowledge, and the areas that need further development. Overall, the classification presented here should not be thought of as cast in stone, but rather as a fluid framework that is amenable to change with the flow of new insights in theoretical physics.

79 ASTRONOMY AND ASTROPHYSICS↗

NASA NTRS1986

Patterns of vegetation in the Owens Valley, California

Spectral characteristics of semi-arid shrub communities were examined using Airborne Imaging Spectrometer (AIS) data collected in the tree mode on 23 May 1985. Mesic sites with relatively high vegetation density and distinct zonation patterns exhibited greater spectral signature variations than sites with more xeric shrub communities. Spectral signature patterns were not directly related to vegetation density or physiognomy, although spatial maps derived from an 8-channel maximum likelihood classification were supported by photo-interpreted surface features. In AIS data, the principal detected effect of shrub vegetation on the alluvial fans is to lower reflectance across the spectrum. These results are similar to those reported during a period of minimal physiological activity in autumn, indicating that shadows cast by vegetation canopies are an important element of soil-vegetation interaction under conditions of relatively low canopy cover.

Ustin, S. L.↗

NASA NTRS1992

Microstructural development during directional solidification of peritectic alloys

Despite the widespread commercial use of peritectic alloys (e.g., steels, brass, bronze, intermetallic compounds, Co based superalloys and A3B type superconductors), the characterization of the microstructural development during directional solidification of peritectics has historically lagged behind similar efforts directed towards other types of binary invariant reactions such as eutectic or monotectic. A wide variety of possible microstructures has been shown to form in peritectics depending upon the imposed temperature gradient, G, the solidification velocity, V, as well as the presence or absence of convection in the melt. This has important technological implications since many commercially important alloys exhibit peritectics and processing methods such as casting and welding often involve widely changing conditions. It has been the aim of this project to examine, in a systematic fashion, both experimentally and theoretically, the influence of gravitationally driven convection on segregation and microstructural development during solidification in peritectic systems under terrestrial conditions. The scientific results of the project will be used to establish ground based data in support of a meaningful microgravity flight experiment.

Lograsso, Thomas A.↗

NASA NTRS1993

A study of metal-ceramic wettability in SiC-Al using dynamic melt infiltration of SiC

Pressure-assisted infiltration with a 2014 Al alloy of plain and Cu-coated single crystal platelets of alpha silicon carbide was used to study particulate wettability under dynamic conditions relevant to pressure casting of metal-matrix composites. The total penetration length of infiltrant metal in porous compacts was measured at the conclusion of solidification as a function of pressure, infiltration time, and SiC size for both plain and Cu-coated SiC. The experimental data were analyzed to obtain a threshold pressure for the effect of melt intrusion through SiC compacts. The threshold pressure was taken either directly as a measure of wettability or converted to an effective wetting angle using the Young-Laplace capillary equation. Cu coating resulted in partial but beneficial improvements in wettability as a result of its dissolution in the melt, compared to uncoated SiC.

Asthana, R.↗

NASA NTRS2022

Integrated Topographic Corrections Improve Forest Mapping Using Landsat Imagery

In mountainous environments, topography strongly affects the reflectance due to illumination effects and cast shadows, which introduce errors in land cover classifications. However, topographic correction is not routinely implemented in standard data pre-processing chains (e.g., Landsat Analysis Ready Data), and there is a lack of consensus whether topographic correction is necessary, and if so, how to conduct it. Furthermore, methods that correct simultaneously for atmospheric and topographic effects are becoming available, but they have not been compared directly. Our objects were to investigate (1) the effectiveness of two topographic correction approaches that integrate atmospheric and topographic correction, (2) improvements in classification accuracy when analyzing topographically corrected single-date imagery (14 July 2016 and 2 October 2016), versus a full Landsat time series from 2014 to 2016, and 3) improvements in classification accuracy when including additional terrain information (i.e., topographic slope, elevation, and aspect). We developed a physical based model and compared it with an enhanced C-correction, both of which integrate atmospheric and topographic correction. We compared classification accuracies with and without topographic correction using combinations of single-date imagery, image composites and spectral-temporal metrics generated from the full Landsat time series, and additional terrain information in the Caucasus Mountains. We found that both the enhanced C-correction and the physical model performed very well and largely eliminated the correlation (Pearson’s correlation coefficient r ranges from 0.06 to 0.24) between surface reflectance and illumination condition, but the physical model performed best (r ranges from 0.05 to 0.11). Both image composites, and spectral-temporal metrics generated from corrected imagery, resulted in significantly (p ≤ 0.05) higher classification accuracies and better forest classifications, especially for the mixed forests. Adding terrain information reduced classification error significantly, but not as much as topographic correction. In summary, topographic correction remains necessary, even when analyzing a full Landsat time series and including a digital elevation model in the classification. We recommend that topographic correction should be applied when analyzing Landsat satellite imagery in mountainous region for forest cover classification.

Atmospheric correction↗

DOE OSTI2020

Solid state grain alignment of permanent magnets in near-final shape

Magnet microstructure manipulation in the solid state by controlled application of a sufficient stress in a direction during high temperature annealing in a single-phase region of heat-treatable magnet alloys, e.g., alnico-type magnets is followed by magnetic annealing and draw annealing to improve coercivity and saturation magnetization properties. The solid-state process can be termed highly controlled abnormal grain growth (hereafter AGG) and will make aligned sintered anisotropic magnets that meet or exceed the magnetic properties of cast versions of the same alloy types.

Anderson, Iver E.↗

DOE OSTI2022

Solid state grain alignment of permanent magnets in near-final shape

Anderson, Iver E.↗

NASA NTRS1996

Lubricous Deposit Formed In Situ Between Wearing Surfaces at High Temperatures

Many components of future aircraft will be constructed from novel high-temperature materials, such as superalloys and ceramic composites, to meet expected operating temperatures in excess of 300 C. There are no known liquid lubricants that can lubricate above 300 C without significant decomposition. Solid lubricants could be considered, but problems caused by the higher friction coefficients and wear rates of the solid lubricant film make this an undesirable approach. An alternative method of lubrication is currently being investigated: vapor phase lubrication. In vapor phase lubrication, an organic liquid (in our studies a thioether was used) is vaporized into a flowing air stream that is directed to sliding surfaces where lubrication is needed. The organic vapor reacts at the concentrated contact sliding area generating a lubricous deposit. This deposit has been characterized as a thin polymeric film that can provide effective lubrication at temperatures greater than 400 C. Initial tribological studies were conducted at the NASA Lewis Research Center and Cleveland State University with a high-temperature friction and wear tribometer. A cast iron rod was loaded (a 4-kg mass was used to generate a contact pressure of 1.2 MPa) against a reciprocating, cast iron plate at 500 C. This system was then lubricated with the vapor phase of thioether.

Source record↗

NASA NTRS2002

Mechanical stimulation improves tissue-engineered human skeletal muscle

Human bioartificial muscles (HBAMs) are tissue engineered by suspending muscle cells in collagen/MATRIGEL, casting in a silicone mold containing end attachment sites, and allowing the cells to differentiate for 8 to 16 days. The resulting HBAMs are representative of skeletal muscle in that they contain parallel arrays of postmitotic myofibers; however, they differ in many other morphological characteristics. To engineer improved HBAMs, i.e., more in vivo-like, we developed Mechanical Cell Stimulator (MCS) hardware to apply in vivo-like forces directly to the engineered tissue. A sensitive force transducer attached to the HBAM measured real-time, internally generated, as well as externally applied, forces. The muscle cells generated increasing internal forces during formation which were inhibitable with a cytoskeleton depolymerizer. Repetitive stretch/relaxation for 8 days increased the HBAM elasticity two- to threefold, mean myofiber diameter 12%, and myofiber area percent 40%. This system allows engineering of improved skeletal muscle analogs as well as a nondestructive method to determine passive force and viscoelastic properties of the resulting tissue.

Non-NASA Center↗

NASA NTRS2005

The Rio Tinto Basin, Spain: Mineralogy, Sedimentary Geobiology, and Implications for Interpretation of Outcrop Rocks at Meridiani Planum, Mars

Exploration by the NASA rover Opportunity has revealed sulfate- and hematite-rich sedimentary rocks exposed in craters and other surface features of Meridiani Planum, Mars. Modern, Holocene, and Plio-Pleistocene deposits of the Rio Tinto, southwestern Spain, provide at least a partial environmental analog to Meridiani Planum rocks, facilitating our understanding of Meridiani mineral precipitation and diagenesis, while informing considerations of martian astrobiology. Oxidation, thought to be biologically mediated, of pyritic ore bodies by groundwaters in the source area of the Rio Tinto generates headwaters enriched in sulfuric acid and ferric iron. Seasonal evaporation of river water drives precipitation of hydronium jarosite and schwertmannite, while (Mg,Al,Fe(sup 3+))-copiapite, coquimbite, gypsum, and other sulfate minerals precipitate nearby as efflorescences where locally variable source waters are brought to the surface by capillary action. During the wet season, hydrolysis of sulfate salts results in the precipitation of nanophase goethite. Holocene and Plio-Pleistocene terraces show increasing goethite crystallinity and then replacement of goethite with hematite through time. Hematite in Meridiani spherules also formed during diagenesis, although whether these replaced precursor goethite or precipitated directly from groundwaters is not known. The retention of jarosite and other soluble sulfate salts suggests that water limited the diagenesis of Meridiani rocks. Diverse prokaryotic and eukaryotic microorganisms inhabit acidic and seasonally dry Rio Tinto environments. Organic matter does not persist in Rio Tinto sediments, but biosignatures imparted to sedimentary rocks as macroscopic textures of coated microbial streamers, surface blisters formed by biogenic gas, and microfossils preserved as casts and molds in iron oxides help to shape strategies for astrobiological investigation of Meridiani outcrops.

Fernandez-Remolar, David C.↗

DOE OSTI2024

Theory-guided design of duplex-phase multi-principal-element alloys

Density-functional theory (DFT) is used to identify phase-equilibria in multi-principal-element and high-entropy alloys (MPEAs/HEAs), including duplex-phase and eutectic microstructures. Here, a combination of composition-dependent formation energy and electronic-structure-based ordering parameters were used to identify a transition from FCC to BCC favoring mixtures, and these predictions experimentally validated in the Al-Co-Cr-Cu-Fe-Ni system. A sharp crossover in lattice structure and dual-phase stability as a function of composition were predicted via DFT and validated experimentally. The impact of solidification kinetics and thermodynamic stability was explored experimentally using a range of techniques, from slow (castings) to rapid (laser remelting), which showed a decoupling of phase fraction from thermal history, i.e., phase fraction was found to be solidification rate-independent, enabling tuning of a multi-modal cell and grain size ranging from nanoscale through macroscale. Strength and ductility tradeoffs for select processing parameters were investigated via uniaxial tension and small-punch testing on specimens manufactured via powder-based additive manufacturing (directed-energy deposition). This work establishes a pathway for design and optimization of next-generation multiphase superalloys via tailoring of structural and chemical ordering in concentrated solid solutions.

36 MATERIALS SCIENCE↗

NASA NTRS2000

Global MHD Simulations of Space Plasma Environments: Heliosphere, Comets, Magnetospheres of Plants and Satellites

Magnetohydrodynamics (MHD) provides an approximate description of a great variety of processes in space physics. Accurate numerical solutions of the MHD equations are still a challenge, but in the past decade a number of robust methods have appeared. Once these techniques made the direct solution of MHD equations feasible, a number of global three-dimensional models were designed and applied to many space physics objects. The range of these objects is truly astonishing, including active galactic nuclei, the heliosphere, the solar corona, and the solar wind interaction with planets, satellites, and comets. Outside the realm of space physics, MHD theory has been applied to such diverse problems as laboratory plasmas and electromagnetic casting of liquid metals. In this paper we present a broad spectrum of models of different phenomena in space science developed in the recent years at the University of Michigan. Although the physical systems addressed by these models are different, they all use the MHD equations as a unifying basis.

Kabin, K.↗

NASA NTRS2006

Metallurgical Mechanisms Controlling Mechanical Properties of Aluminum Alloy 2219 Produced by Electron Beam Freeform Fabrication

The electron beam freeform fabrication (EBF3) layer-additive manufacturing process has been developed to directly fabricate complex geometry components. EBF3 introduces metal wire into a molten pool created on the surface of a substrate by a focused electron beam. Part geometry is achieved by translating the substrate with respect to the beam to build the part one layer at a time. Tensile properties demonstrated for electron beam deposited aluminum and titanium alloys are comparable to wrought products, although the microstructures of the deposits exhibit cast features. Understanding the metallurgical mechanisms controlling mechanical properties is essential to maximizing application of the EBF3 process. Tensile mechanical properties and microstructures were examined for aluminum alloy 2219 fabricated over a range of EBF3 process variables. Unique microstructures were observed within the deposited layers and at interlayer boundaries, which varied within the deposit height due to microstructural evolution associated with the complex thermal history experienced during subsequent layer deposition. Microstructures exhibited irregularly shaped grains with interior dendritic structures, described based on overall grain size, morphology, distribution, and dendrite spacing, and were correlated with deposition parameters. Fracture features were compared with microstructural elements to define fracture paths and aid in definition of basic processing-microstructure-property correlations.

Domack, Marcia S.↗