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DOE OSTI2021

Liquid crystalline behavior and photoluminescence of lanthanide decanoate nanoparticles synthesized by microwave radiation

Luminescent lanthanide decanoate nanoparticles (LnC 10 NPs; Ln = Pr, Nd, Sm, Eu, Gd, Er) with spherical morphology (<100 nm) have been synthesized via a facile microwave (MWV) method using Ln(NO 3 ) 3 ·xH 2 O, ethanol/water, and decanoic acid. These hybrid nanomaterials adopt a lamellar structure consisting of inorganic Ln 3+ layers separated by a decanoate anion bilayer and exhibit liquid crystalline (LC) phases during melting. The particle size, crystalline structure, and LC behavior were characterized using transmission electron microscopy (TEM), differential scanning calorimetry (DSC), and powder X-ray diffraction (ambient and heated). Thermal analysis indicated the formation of Smectic A LC phases by LnC 10 nanoparticles, with the smaller lanthanides (Ln = Sm, Gd, Er) displaying additional solid intermediate and Smectic C phases. The formation of LC phases by the smaller Ln 3+ suggests that these nanoscale materials have vastly different thermal properties than their bulk counterparts, which do not exhibit LC behavior. In this work, photoluminescence spectroscopy revealed the LnC 10 NPs to be highly optically active, producing strong visible emissions that corresponded to expected electronic transitions by the various Ln 3+ ions. Under long-wave UV irradiation (λ = 365 nm), bright visible luminescence was observed for colloidal suspensions of Nd, Sm, Eu, Gd, and ErC 10 NPs. To the best of the authors’ knowledge, this is the first reported synthesis of nanoscale metal alkanoates, the first report of liquid crystalline behavior by any decanoate of lanthanides smaller than Nd, and the first observation of strong visible luminescence by non-vitrified lanthanide alkanoates.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Simple Hybrid Sea Ice Nudging Method for Improving Control Over Partitioning of Sea Ice Concentration and Thickness

Abstract To assess the effect of ocean‐atmosphere coupling in the climate response to forced sea ice loss, the Polar Amplification Model Intercomparison Project protocol includes centennial coupled atmosphere‐ocean general circulation model simulations with imposed sea ice loss. The protocol, which specifies sea ice concentration and thickness distribution targets, does not prescribe a method for achieving them. Although different methods for imposing sea ice loss (or growth) in models have been documented, testing of the method‐dependence of the resulting climate responses has been limited. Achieving the targeted sea ice state has proven to be challenging using the so‐called ghost‐flux nudging method, which induces ice melt from below, as this method does not constrain the partitioning between thickness and concentration. We propose, describe and test a simple method that combines the advantages of direct sea ice nudging and ghost‐flux nudging. The hybrid nudging method better captures the partitioning between thickness and concentration while conserving total water content. We document how this novel sea ice constraining method reaches specific targets, enhances surface turbulent heat flux responses to sea ice loss, and induces tropospheric warming for both polar regions.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1998

Pristine Igneous Rocks and the Early Differentiation of Planetary Materials

Our studies are highly interdisciplinary, but are focused on the processes and products of early planetary and asteroidal differentiation, especially the genesis of the ancient lunar crust. Most of the accessible lunar crust consists of materials hybridized by impact-mixing. Rare pristine (unmixed) samples reflect the original genetic diversity of the early crust. We studied the relative importance of internally generated melt (including the putative magma ocean) versus large impact melts in early lunar magmatism, through both sample analysis and physical modeling. Other topics under investigation included: lunar and SNC (martian?) meteorites; igneous meteorites in general; impact breccias, especially metal-rich Apollo samples and polymict eucrites; effects of regolith/megaregolith insulation on thermal evolution and geochronology; and planetary bulk compositions and origins. We investigated the theoretical petrology of impact melts, especially those formed in large masses, such as the unejected parts of the melts of the largest lunar and terrestrial impact basins. We developed constraints on several key effects that variations in melting/displacement ratio (a strong function of both crater size and planetary g) have on impact melt petrology. Modeling results indicate that the impact melt-derived rock in the sampled, megaregolith part of the Moon is probably material that was ejected from deeper average levels than the non-impact-melted material (fragmental breccias and unbrecciated pristine rocks). In the largest lunar impacts, most of the impact melt is of mantle origin and avoids ejection from the crater, while most of the crust, and virtually all of the impact-melted crust, in the area of the crater is ejected. We investigated numerous extraordinary meteorites and Apollo rocks, emphasizing pristine rocks, siderophile and volatile trace elements, and the identification of primary partial melts, as opposed to partial cumulates. Apollo 15 sample 15434,28 is an extraodinarily large glass spherule, nearly if not entirely free of meteoritic contamination, and provides insight into the diversity of mare basalts in the Hadley-Apennine region. Apollo 14 sample 14434 is in many respects a new rock type, intermediate between nonmare gabbronorites and mare basalts. We helped to both plan and implement a consortium to study the Yamato-793605 SNC/martian meteorite.

Warren, Paul H.↗

DOE OSTI2020

A Complex Interplay between Nitric Oxide, Quorum Sensing, and the Unique Secondary Metabolite Tundrenone Constitutes the Hypoxia Response in Methylobacter

Methylobacter species, members of the Methylococcales, have recently emerged as some of the globally widespread, cosmopolitan species that play a key role in the environmental consumption of methane across gradients of dioxygen tensions. In this work, we approached the question of howMethylobacter copes with hypoxia, via laboratory manipulation. Through comparative transcriptomics of cultures grown under high dioxygen partial pressure versus cultures exposed to hypoxia, we identified a gene cluster encoding a hybrid cluster protein along with sensing and regulatory functions. Through mutant analysis, we demonstrated that this gene cluster is involved in the hypoxia stress response. Through additional transcriptomic analyses, we uncovered a complex interconnection between the NO-mediated stress response, quorum sensing, the secondary metabolite tundrenone, and methanol dehydrogenase functions. This novel and complex hypoxia stress response system is so far unique to Methylobacter species, and it may play a role in the environmental fitness of these organisms and in their cosmopolitan environmental distribution.Here, we describe a novel and complex hypoxia response system in a methanotrophic bacterium that involves modules of central carbon metabolism, denitrification, quorum sensing, and a secondary metabolite, tundrenone. This intricate stress response system, so far unique to Methylobacter species, may be responsible for the persistence and activity of these species across gradients of dioxygen tensions and for the cosmopolitan distribution of these organisms in freshwater and soil environments in the Northern Hemisphere, including the fast-melting permafrosts.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2021

Additively Manufactured Compliant Hybrid Gas Thrust Bearing for Supercritical Carbon Dioxide Turbomachinery: Design and Proof of Concept Testing

The following paper presents a new type of gas lubricated thrust bearing that utilizes additive manufacturing or also known as direct metal laser melting (DMLM) to fabricate the bearing. The motivation for the new bearing concept is derived from the need for highly efficient supercritical carbon dioxide (sCO2) turbomachinery in the mega-watt power range. The paper provides a review of existing gas thrust-bearing technology, outlines the need for the new DMLM concept, and discusses proof-of-concept testing results. The new concept combines hydrostatic pressurization with individual tilting pads that are flexibly mounted using hermetic squeeze film dampers (HSFD) in the bearing-pad support. This paper describes the thrust-bearing concept and discusses the final design approach. Proof-of-concept testing in air for a 6.8 in. (173 mm) outer diameter thrust gas bearing was performed; with thrust loading, up to 1500 lbs (6.67 kN) and a thrust runner speed of 10krpm (91 m/s tip speed). The experiments were performed with a bent shaft resulting in thrust runner axial vibration magnitudes of 2.9 mils (74 μm) p-p and dynamic thrust loads of 270 lbs (1.2 kN) p-p. In addition, force deflection characteristics and stiffness coefficients of the bearing system are presented for an inlet hydrostatic pressure of 380 psi (2.62 MPa). Results at 10 krpm show that the pad support architecture was able to sustain high levels of dynamic misalignment equaling 6 times the nominal film clearance while demonstrating a unit load-carrying capacity of 55 psi (0.34 Mpa). Gas-film force deflection tests portrayed nonlinear behavior like a hardening spring, while the bearing pad support stiffness was measured to be linear and independent of gas film thickness.

Engineering↗

NASA NTRSDate not supplied

On the Prediction of Surface Melt Over the Greenland Ice Sheet at NWP and S2S Timescales

Greenland surface melt “events” – encompassing large swaths of the ice sheet over approximately 4-10 day periods – have occurred with increasing frequency in the 21st Century. Surface processes are significant to the ice sheet’s overall contribution to sea level. In addition, the sudden onset of widespread surface melt produces hazardous conditions for researchers and for communities adjacent to the ice sheet. The mechanisms producing melt events, their associated large-scale forcing, and timescales of interest are highly variable and poorly understood. Here we examine the predictability of melt events in a numerical weather prediction system (NWP) and a subseasonal-to-seasonal system (S2S). The NASA Global Modeling and Assimilation Office forward processing (GMAO-FP) is an NWP system that incorporates an evolving, global hybrid 4D ensemble–variational (4DEnVar) data assimilation system and a state-of-the-art model that is run twice-daily with forecasts out to five and ten days. The GMAO S2S system is a hindcast-anomaly, coupled-model prediction system initialized with an atmospheric analysis, and in situ and satellite ocean data assimilation. Both systems represent ice sheet surface hydrology and snowpack processes. We examine the performance of the systems over the period 2018-2023, a span that includes approximately nine significant events, against analyses and satellite-derived melt extent. In addition to extent, we examine related conditions and their role in the melt forecast, including the onset of both omega and Rex atmospheric blocking patterns, sea surface temperatures, sea ice extent, water vapor transport, precipitation, and surface preconditioning. We further examine the tendency for false-alarm events in each system and assess reasons for the forecast performance. North Atlantic atmospheric blocking patterns leading to surface melt are well forecast by the NWP system out to around eight days, while the S2S system generally underestimates the magnitude of such events at monthly lead times. These systems suggest that while short term forecasts of ice sheet melt and melt events are relatively robust, S2S predictions of surface conditions are highly dependent on the ability of a coupled system to generate the short-term atmospheric conditions associated with surface melt events.

Richard Cullather↗

DOE OSTI2022

Effect of coaxial nozzle wear on catchment efficiency in direct energy deposition built components

Laser based Direct Energy Deposition (DED) systems using metallic powder feedstock are recognized as a promising manufacturing method for their ability to shorten production cycles and create complex part geometries. Components are built by generating a melt pool with a high-power laser beam while material is coaxially injected and left to solidify. An impediment to large scale use of DED lies in poor powder catchment efficiency, the condition in which a portion of injected powder escapes the melt pool resulting in a ratio of decreased printed material mass to mass of supplied feedstock. The wear state of a coaxial nozzle on a DED system within a hybrid manufacturing machine tool has been observed to decrease catchment efficiency over time. Herein this study investigates this effect by adapting flow visualization techniques to an in-situ process monitoring format, the implementation of a Computational Fluid Dynamics (CFD) simulation, and deposition testing. Nozzle geometric defects due to wear are identified and categorized, and the impact of nozzle tip wear, resulting in axial tip reduction, on powder catchment efficiency is proven by multiple calculation methods. A linear correlation between catchment efficiency and powder stream diameter is identified, causing a 15–20% loss in efficiency sustained over incremental nozzle tip reduction up to − 1 mm. These results provide a foundation for further study of wear effects and Zero defect manufacturing solutions for powder fed DED systems.

42 ENGINEERING↗

DOE OSTI2022

Transient Mesoscopic Immiscibility, Viscosity Anomaly, and High Internal Pressure at the Semiconductor–Metal Transition in Liquid Ga 2 Te 3

Gallium tellurides appear to be promising phase-change materials (PCMs) of the next generation for brain-inspired computing and reconfigurable optical metasurfaces. They are different from the benchmark PCMs because of sp 3 gallium hybridization in both cubic Ga 2 Te 3 and amorphous pulsed laser deposition (PLD) films. Liquid Ga 2 Te 3 also shows a viscosity η(T) anomaly just above melting when η(T) first increases and only then starts decreasing. We used high-energy X-ray diffraction to observe a transient mesoscopic immiscibility that suggested dense metallic liquid droplets in a semiconducting melt. The η(T) shape was consistent with this finding. A vanishing first sharp diffraction peak that also shifts to a higher Q indicates a high internal pressure in the metallic melt, which produces a remarkable asymmetry of the Ga–Te nearest neighbor distances and is reminiscent of high-pressure rhombohedral Ga 2 Te 3 . Finally, the observed phenomena provide a realistic scenario for a fast, multilevel SET–RESET response, which also unravels similar trends in the purported density-driven liquid polyamorphism of water, phosphorus, sulfur, and other materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1999

MoSi2-Base Structural Composite Passed Engine Test

The intermetallic compound molybdenum disilicide (MoSi2) is an attractive high-temperature structural material for advanced engine applications. It has excellent oxidation resistance, a high melting point, relatively low density, and high thermal conductivity; and it is easily machined. Past research at the NASA Lewis Research Center has resulted in the development of a hybrid composite consisting of a MoSi2 matrix reinforced with silicon nitride (Si3N4) particulate and silicon carbide (SiC) fibers. This composite has demonstrated attractive strength, toughness, thermal fatigue, and oxidation resistance, including resistance to "pest" oxidation. These properties attracted the interest of the Office of Naval Research and Pratt & Whitney, and a joint NASA/Navy/Pratt & Whitney effort was developed to continue to mature the MoSi2 composite technology. A turbine blade outer air seal, which was part of the Integrated High Performance Turbine Engine Technology (IHPTET) program, was chosen as a first component on which to focus.

Nathal, Michael V.↗

NASA NTRS2004

Study of Rapid-Regression Liquefying Hybrid Rocket Fuels

A report describes experiments directed toward the development of paraffin-based hybrid rocket fuels that burn at regression rates greater than those of conventional hybrid rocket fuels like hydroxyl-terminated butadiene. The basic approach followed in this development is to use materials such that a hydrodynamically unstable liquid layer forms on the melting surface of a burning fuel body. Entrainment of droplets from the liquid/gas interface can substantially increase the rate of fuel mass transfer, leading to surface regression faster than can be achieved using conventional fuels. The higher regression rate eliminates the need for the complex multi-port grain structures of conventional solid rocket fuels, making it possible to obtain acceptable performance from single-port structures. The high-regression-rate fuels contain no toxic or otherwise hazardous components and can be shipped commercially as non-hazardous commodities. Among the experiments performed on these fuels were scale-up tests using gaseous oxygen. The data from these tests were found to agree with data from small-scale, low-pressure and low-mass-flux laboratory tests and to confirm the expectation that these fuels would burn at high regression rates, chamber pressures, and mass fluxes representative of full-scale rocket motors.

Zilliac, Greg↗

NASA NTRS2004

Prepreg and Melt Infiltration Technology Developed for Affordable, Robust Manufacturing of Ceramic Matrix Composites

Affordable fiber-reinforced ceramic matrix composites with multifunctional properties are critically needed for high-temperature aerospace and space transportation applications. These materials have various applications in advanced high-efficiency and high-performance engines, airframe and propulsion components for next-generation launch vehicles, and components for land-based systems. A number of these applications require materials with specific functional characteristics: for example, thick component, hybrid layups for environmental durability and stress management, and self-healing and smart composite matrices. At present, with limited success and very high cost, traditional composite fabrication technologies have been utilized to manufacture some large, complex-shape components of these materials. However, many challenges still remain in developing affordable, robust, and flexible manufacturing technologies for large, complex-shape components with multifunctional properties. The prepreg and melt infiltration (PREMI) technology provides an affordable and robust manufacturing route for low-cost, large-scale production of multifunctional ceramic composite components.

Singh, Mrityunjay↗

DOE OSTI2022

Synthesis of a 316L stainless steel-copper composite by laser melting

This paper demonstrates a laser melting method to produce a metal matrix composite with a higher thermal conductivity compared to 316 L stainless steel using a Jettable Cu ink. A novel canister was used to control the oxygen level during laser processing to emulate a hybrid inkjet-powder bed fusion technique for doping the stainless steel powder bed with Cu precursor ink. Here, the thermal conductivity of the composite was found to be 187% higher than that of 316 L stainless steel, while the microhardness decreased by 39%. Microstructural results show opportunities to further enhance the thermal conductivity and mechanical properties of the composite by eliminating interfacial cracking.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Modeling Time-Dependent Surrogates of Additive-Manufactured Nuclear Fuels Processes

Additive manufacturing (AM) technology is being increasingly adopted in a wide variety of application areas for its ability to rapidly produce, prototype, and customize designs. Recently, a hybrid AM technique was successfully developed at Idaho National Laboratory (INL) to manufacture nuclear fuels [1]. Despite the advantages, this AM technique needs optimization due to defects from a highly complex melting and sintering process. The complex metallurgical phenomena during AM processes are strongly related to parameters such as applied laser power, traveling speed, and scan style, which could lead to differences in density, residual stress, crystallographic texture, and mechanical properties. In addition, stochastic variations in laser energy interaction and associated multiscale/multiphysics phenomena cause variations in microstructure evolution and mechanical properties. Currently, researchers at INL are focusing on developing a comprehensive modeling framework, leveraging INL’s simulation tools MOOSE/MARMOT/BISON/RAVEN [2-4] to describe all steps of this AM process across multiple length scales. Although this advanced framework plays a critical role in enabling enhancements to traditional trial and error approaches for design and optimization of nuclear fuel materials, it remains computationally intense, limiting its use in sensitivity and optimization analysis. In this case, an accurate and inexpensive surrogate becomes an effective tool for providing a tractable approximation of the underlying underline physics. Surrogate models generally not based on the physics of a system are purely mathematical models used to capture the relationships between specific system inputs and outputs. Popular approaches, including neural networks [5], response surfaces [6], and subspace-based reduced order models [7], have been applied to a wide range of disciplines, such as nuclear reactor design, aerospace design and automotive design. In this summary, we employ advanced time-dependent surrogate models such as high-dimensional model representation (HDMR) [8] and physics-informed deep neural network (PINNs) [9] to accelerate the design and optimization of AM process.

42 ENGINEERING↗

DOE OSTI2026

Metal hybridization in dilute-alloy catalysts promotes sintering resistance by decreasing surface mobility

Dilute-metal-alloy nanoparticles exhibit enhanced catalytic performance compared with monometallic nanoparticles for many reactions. Anecdotal reports indicate that very dilute alloying can also slow the sintering rates of supported nanoparticles, although this has not been rigorously assessed and cannot be explained using bulk descriptors such as metal melting temperature. Here, in this study, we utilize methanol synthesis reactivity, microscopy and in situ spectroscopy measurements to demonstrate that 1 atom% Pt addition to ~1–2-nm-diameter Cu (Pt 1 Cu 100 ) nanoparticles supported on SiO 2 dramatically decreases their sintering rates. Minimal sintering of Pt 1 Cu 100 nanoparticles is observed during aging in H 2 up to 700 °C versus 500 °C for Cu nanoparticles. Scanning tunnelling microscopy reveals that the addition of 0.01 monolayer of Pt to a Cu(110) surface decreases the detachment rate of undercoordinated atoms, demonstrating that dilute dopants can locally decrease the rate of the first step in nanoparticle sintering. Density functional theory calculations quantify the stabilization and predict other sinter-resistant dilute alloys. We find that the degree of host–dopant d-state hybridization correlates with decreased surface mobility, providing a mechanistic framework for designing sinter-resistant catalysts.

Finzel, Jordan [Univ. of California, Santa Barbara↗

NASA NTRS2012

Formulation and Testing of Paraffin-Based Solid Fuels Containing Energetic Additives for Hybrid Rockets

Many approaches have been considered in an effort to improve the regression rate of solid fuels for hybrid rocket applications. One promising method is to use a fuel with a fast burning rate such as paraffin wax; however, additional performance increases to the fuel regression rate are necessary to make the fuel a viable candidate to replace current launch propulsion systems. The addition of energetic and/or nano-sized particles is one way to increase mass-burning rates of the solid fuels and increase the overall performance of the hybrid rocket motor.1,2 Several paraffin-based fuel grains with various energetic additives (e.g., lithium aluminum hydride (LiAlH4) have been cast in an attempt to improve regression rates. There are two major advantages to introducing LiAlH4 additive into the solid fuel matrix: 1) the increased characteristic velocity, 2) decreased dependency of Isp on oxidizer-to-fuel ratio. The testing and characterization of these solid-fuel grains have shown that continued work is necessary to eliminate unburned/unreacted fuel in downstream sections of the test apparatus.3 Changes to the fuel matrix include higher melting point wax and smaller energetic additive particles. The reduction in particle size through various methods can result in more homogeneous grain structure. The higher melting point wax can serve to reduce the melt-layer thickness, allowing the LiAlH4 particles to react closer to the burning surface, thus increasing the heat feedback rate and fuel regression rate. In addition to the formulation of LiAlH4 and paraffin wax solid-fuel grains, liquid additives of triethylaluminum and diisobutylaluminum hydride will be included in this study. Another promising fuel formulation consideration is to incorporate a small percentage of RDX as an additive to paraffin. A novel casting technique will be used by dissolving RDX in a solvent to crystallize the energetic additive. After dissolving the RDX in a solvent chosen for its compatibility with both paraffin and RDX, the mixture will be combined with the melted paraffin. With the melting point of the paraffin far below the decomposition temperature of the RDX, the solvent will be boiled off, leaving the crystallized RDX embedded in the paraffin. At low percentages of RDX additive and with crystallized RDX surrounded by paraffin, the fuel grains will remain inert, maintaining a key benefit of hybrids in the safety of the solid fuel.

Larson, Daniel B.↗

NASA NTRS1980

Fiber release characteristics of graphite hybrid composites

The paper considers different material concepts that can be fabricated of hybridized composites which demonstrate improved graphite fiber retention capability in a severe fire without significant reduction to the composite properties. More than 30 panels were fabricated for mechanical and fire tests, the details and results of which are presented. Methods of composite hybridization investigated included the addition of oxidation resistant fillers to the resin, mechanically interlocking the graphite fibers by the use of woven fabrics, and the addition of glass fibers and glass additives designed to melt and fuse the graphite fibers together. It is concluded that a woven fabric with a serving of glass around each graphite tow is by far the superior of those evaluated: not only is there a coalescing effect in each graphite layer, but there is also a definite adhesion of each layer to its neighbor.

Henshaw, J.↗

DOE OSTI2023

Environmental stability of additively manufactured siliconized silicon carbide for applications in hybrid energy systems

A key consideration for the successful operation of hybrid energy systems will be the environmental stability of materials used for their construction, particularly when experiencing service environments containing water vapor at high temperatures. Here, we report results from the characterization of siliconized silicon carbide (Si-SiC) prepared via binder jet additive manufacturing and reactive silicon melt infiltration after being exposed to environments representative of those in solid oxide fuel cell (SOFC) anodes, and to exhaust gases inside a microturbine operating on natural gas. In both cases, it was found that oxide scales formed on the surface and that these scales were dense, continuous, and well-bonded to the substrates, although there was evidence of transverse and longitudinal cracking most likely as a result of mismatches in the thermal expansion of the scale and the substrate. Measured values of the thickness of the oxide scale were compared to those predicted by parabolic oxidation kinetics of silicon, but the potential effects of silica volatilization induced by water vapor, and silica reduction when exposed to hydrogen are discussed. The overall results showed that the oxide scale is expected to be protective under the conditions of hybrid power generation systems.

36 MATERIALS SCIENCE↗

NASA NTRS2009

Modeling of Melt-Infiltrated SiC/SiC Composite Properties

The elastic properties of a two-dimensional five-harness melt-infiltrated silicon carbide fiber reinforced silicon carbide matrix (MI SiC/SiC) ceramic matrix composite (CMC) were predicted using several methods. Methods used in this analysis are multiscale laminate analysis, micromechanics-based woven composite analysis, a hybrid woven composite analysis, and two- and three-dimensional finite element analyses. The elastic properties predicted are in good agreement with each other as well as with the available measured data. However, the various methods differ from each other in three key areas: (1) the fidelity provided, (2) the efforts required for input data preparation, and (3) the computational resources required. Results also indicate that efficient methods are also able to provide a reasonable estimate of local stress fields.

Mital, Subodh K.↗