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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 667 records · Page 37
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Oxidation mechanism in a refractory multiple-principal-element alloy at high temperature

Refractory multiple-principal-element alloys (RMPEAs) are promising structural materials to enable increased power efficiency in high-temperature oxidation environments, but the oxidation behavior and microstructures of the oxides, especially at the beginning of the oxidation, have received limited attention. Here, the oxidation mechanism in an equimolar W-Mo-Ta-Nb-V was investigated at 1300 °C and compared with the equimolar W-Mo-Ta-Nb alloy without V. The oxide scale on WMoTaNbV after 1 min exposure is shown to be composed of a degradation layer at the interface of the alloy/oxide, an initial oxide transition layer, followed by the main phase aggregate oxide layer, and an outermost oxide layer. At the early stage of oxidation, the absorption of oxygen by the RMPEA substrate forms a solid solution. Vanadium accelerates the initial degradation process as it forms VO. The initial oxidation-induced degradation of RMPEA follows a sequence governed by the free energy change accompanied by local element segregation. Liquid V-Mo oxides aggregate in the intermediate oxide layer. The inward growth of the oxide scale is controlled by the local composition changes, the orientation of the substrate, the crystal structure, and physical properties such as melting points of the oxides.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Microstructure-sensitive mechanical behavior of an additively manufactured psuedoelastic shape memory alloy

The additive manufacturing of shape memory alloys into complex geometries enables fabrication of advanced functional systems across a variety of fields and domains. This work presents results focused on the mechanical behavior of additively manufactured shape memory pseudoelastic NiTi. The deformation induced solid state phase transformation from austenite to martensite allows this system to accommodate large recoverable strains. This deformation behavior is fundamentally driven by crystal-scale transformation physics. Laser powder bed fusion processing reveals that the resulting microstructure, both grain morphology and crystallographic texture, is strongly dependent on the manufacturing processing history. Exhaustive mechanical testing demonstrates that these microstructural factors strongly impact both tensile and cyclic stress–strain behavior. Cyclic dissipative behavior, however, is similar across all tested microstructures following an initial transient period. Remarkably, analysis of spatial strain fields during tensile loading reveals two distinctly different localization “modes”. The first is initiation of localized deformation bands which continuously propagate through the tensile bar during loading. In the second mode localization is observed but lacks propagation; instead additional localization cites nucleate during subsequent loading. The latter phenomena is suspected to be driven by grain-scale deformation physics as the localized band morphologies coincide with grain morphologies. These phenomena strongly impact the resulting aggregate stress–strain behavior. Hence, manufacturers and designers of psuedoelastic functional components must at the very least consider the potential variability in properties when considering additive manufacturing processing. More ideally the process–structure–property relations can be used to further tailor and optimize final functional performance.

Additive manufacturing↗
DOE OSTI2018

A Novel Dual-Step Nucleation Pathway in Crystalline Solids under Neutron Irradiation

Innovations in nanostructuring of inorganic crystalline solids are often limited by prerequisite critical nucleation energy and solute supersaturation for formation of a phase. This research provides direct evidence supporting the viability of an unconventional irradiation-induced nanostructuring process, via transmission electron microscopy, that circumvents these preconditions. Using polymorphic silicon carbide (SiC) as a prototype, a surprising two-step nucleation route is demonstrated through which nanoscale distribution of the second phase is achieved by reaction of solutes with neutron irradiation-induced precursors. In the first step, nanoscale α–SiC precipitates in a β–SiC matrix unexpectedly nucleate heterogeneously at structural defects. This occurs at significantly lower temperatures compared with the usual β→α transition temperature. Subsequently, α–SiC precipitate acts as a surrogate template for its structural and compositional transition into a fission product precipitate, palladium silicide. These discoveries provide a modern view of irradiation engineering in polymorphic ceramics for advanced applications.

36 MATERIALS SCIENCE↗
DOE OSTI2015

An Investigation of Catastrophic Failure in Solid-State Lamps Exposed to Harsh Environment Operational Conditions

Today’s lighting technology is steadily becoming more energy efficient and less toxic to the environment since the passing of the Energy Independence and Security Act of 2007 (EISA) [1]. EISA has mandated a higher energy efficiency standard for lighting products and the phase out of the common incandescent lamp. This has led lighting manufacturers to pursue solid-state lighting (SSL) technologies for consumer lighting applications. However, two major roadblocks are hindering the transition process to SSL lamps: cost and quality. In order to cut cost, manufactures are moving towards cheaper packaging materials and a variety of package architecture construction techniques which may potentially erode the quality of the lamp and reduce its survivability in everyday applications. Typically, SSL lamps are given product lifetimes of over twenty years based off of the IES TM-21-11 lighting standard which does not include moisture effects or large operational temperatures [2]. A group of recently released off-the-shelf lamps have undergone a steady-state temperature humidity bias life test of 85°C/85%RH (85/85) to investigate the reliability in harsh environment applications. The lack of accelerated test methods for lamps to assess reliability prior to introduction into the marketplace does not exist in literature. There is a need for SSL physics based models for the assessment and prediction of a lamp’s lifetime which is being spearheaded by the DOE [3]. In order to be fully accepted in the marketplace, SSL lamps must be able to perform similarly to incandescent lamps in these environments, as well as live up to the lifetime claims of manufacturers. A lamp’s package architecture must be designed with performance factors in mind, as well as address some of the known and published package related failure mechanisms, such as carbonization of the encapsulant material, delamination, encapsulant yellowing, lens cracking, and phosphor thermal quenching [4]. Each failure mechanism produces the similar failure mode of lumen degradation predominately due to two contributing factors: high junction temperature and moisture ingress. The current state-of-the-art has focused on individual areas of the lamp, such as the LED chip, substrate material, electrical driver design and thermal management techniques. [5] – [16] Looking at the lamp as a whole is a novel approach and has not been seen before in literature. This work followed the JEDEC standard JESD22-A101C of 85/85 with a one hour interval of applied voltage followed by a one hour interval of no applied voltage [17]. This test was performed continuously for each SSL lamp until it became nonoperational, i.e. did not turn on. Periodically, photometric measurements were taken following the IES LM-79-08 standard at room temperature using an integrating sphere, a spectrometer, and lighting software. The overall health of the SSL lamps was assed using the relative luminous flux (RLF), correlated color temperature (CCT) and the color difference (Δu'v') using the Euclidean distance of the CIE 1976 color space coordinates. Finally, a Weibull analysis was completed to compare the characteristic lifetime of the SSL lamp to the actual rated lifetime. An important result from this work shows that the rated lifetime does not come close to the actual lifetime when the SSL lamps are used in a harsh humid environment which is fairly common in outdoor applications across the U.S. Also, the photometric results are presented for the entire lifetime of each SSL lamp under test.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2023

Surface structure studies in 2D and 3D Nb resonators using GI-XRD

Superconductor radio frequency (SRF) Nb-resonators are a key element in the development of new generations of particle accelerators as well as in the fabrication of 3D circuit QED architecture for quantum computing. Nevertheless, Niobium is extremally reactive to light elements such as C, N, O and H, and therefore to the impurities ordering under special conditions, e.g., cryogenic temperatures. Since these resonators are put through a series of metallurgical and chemical processes, the number of impurities in the solid increases in tens of ppm. Upon operational conditions ~1.6 K, Nb become vulnerable to H atoms ordering, which leads to the nucleation of secondary phases such as Nb-hydrides. Thereupon to the energy dissipation and eventually to the superconductivity breakdown known as Q-disease and potentially High-Field Q-slope. In this contribution, we present a detailed structural analysis by high-energy grazing-incidence X-ray diffraction of specimens extracted from 3D Nb resonators to shed light on the kinetic formation of the resulting secondary phases and their crystal phase identification upon cooling and heating cycles. To our knowledge, this is the first study carried out in resonators samples using a light source, shallow angles and temperatures near ~4 K. Consequently, this work opens new routes to understand the chemical and phase composition, crystal and electronic structure of the Nb surface at temperatures near the operating conditions as a strategy to improve the physical and functional properties of Nb superconducting resonators.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2025

HPC for Optimizing Process Parameters to Control Material Evolution in Seamless Induction Hardening of Wind Turbine Main Shaft Bearings

Work proposed in this project focused on understanding the effect of martensitic transformation in the steel on the potential for cracking during seamless induction hardening (SIH) as a function of process conditions to allow the process to optimally scale up. Large-scale, three-dimensional phase-field simulations of martensitic transformation were performed using MEUMAPPS-SS (Microstructure Evolution Using Massively Parallel Phase-field Simulations – Solid State) code developed at Oak Ridge National Laboratory. The simulations were guided by location-specific thermal history generated by experimental measurements of time-temperature history generated at The Timken Company. The simulations were able to capture the morphological evolution of the martensite variants in an Fe-1.0C-1.5Cr steel based on the Nishiyama-Wasserman (NW) orientation relationship. The simulations were also able to quantify the stress-state at the interface between impinging martensite variants. The simulations indicated that the magnitude of the various stress and strain components were dependent on the sizes of the impinging plates with a reduction in these quantities with reduced plate size in agreement with experimental findings. The results obtained from the simulations will be used to guide the optimization of the alloy thermal conditions to eliminate quench cracking during SIH of bearing steels.

99 GENERAL AND MISCELLANEOUS↗
DOE OSTI2025

HPC for optimizing process parameters to control material evolution in seamless induction hardening of wind turbine main shaft bearings

Work proposed in this project focused on understanding the effect of martensitic transformation in the steel on the potential for cracking during seamless induction hardening (SIH) as a function of process conditions to allow the process to optimally scale up. Large-scale, three-dimensional phase-field simulations of martensitic transformation were performed using MEUMAPPS-SS (Microstructure Evolution Using Massively Parallel Phase-field Simulations – Solid State) code developed at Oak Ridge National Laboratory. The simulations were guided by location-specific thermal history generated by experimental measurements of time-temperature history generated at The Timken Company. The simulations were able to capture the morphological evolution of the martensite variants in an Fe-1.0C-1.5Cr steel based on the Nishiyama-Wasserman (NW) orientation relationship. The simulations were also able to quantify the stress-state at the interface between impinging martensite variants. The simulations indicated that the magnitude of the various stress and strain components were dependent on the sizes of the impinging plates with a reduction in these quantities with reduced plate size in agreement with experimental findings. The results obtained from the simulations will be used to guide the optimization of the alloy thermal conditions to eliminate quench cracking during SIH of bearing steels.

17 WIND ENERGY↗
DOE OSTI2016

Materials and methods for the preparation of nanocomposites

Disclosed herein is an isolable colloidal particle comprising a nanoparticle and an inorganic capping agent bound to the surface of the nanoparticle, a solution of the same, a method for making the same from a biphasic solvent mixture, and the formation of structures and solids from the isolable colloidal particle. The process can yield photovoltaic cells, piezoelectric crystals, thermoelectric layers, optoelectronic layers, light emitting diodes, ferroelectric layers, thin film transistors, floating gate memory devices, imaging devices, phase change layers, and sensor devices.

14 SOLAR ENERGY↗
DOE OSTI2018

Materials and methods for the preparation of nanocomposites

Disclosed herein is an isolable colloidal particle comprising a nanoparticle and an inorganic capping agent bound to the surface of the nanoparticle, a solution of the same, a method for making the same from a biphasic solvent mixture, and the formation of structures and solids from the isolable colloidal particle. The process can yield photovoltaic cells, piezoelectric crystals, thermoelectric layers, optoelectronic layers, light emitting diodes, ferroelectric layers, thin film transistors, floating gate memory devices, imaging devices, phase change layers, and sensor devices.

36 MATERIALS SCIENCE↗
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

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 OSTI2019

Direct Visualization of Drug–Polymer Phase Separation in Ritonavir–Copovidone Amorphous Solid Dispersions Using in situ Synchrotron X-ray Fluorescence Imaging of Thin Films

Amorphous solid dispersions (ASDs) are new formulations currently being used in pharmaceutical industry. The ASDs, in which amorphous drug and polymeric excipients are intimately mixed at a molecular level, exhibit dramatically enhanced solubility and dissolution characteristics relative to their crystalline drug counterparts. In the process of achieving an ever-increasing drug loading (DL), it is noticed however, that the drug release profile deteriorates significantly beyond a certain DL. As an example, a ritonavir-copovidone ASD achieves continuous and full drug release when DL ≤ 25 wt%. The release drops at 30 wt% and when DL > 30 wt% there is virtually no drug release, behaving like a pure amorphous drug. In this communication, the dissolution behavior of ASD thin films has been investigated by in situ synchrotron X-ray fluorescence (XRF) imaging to elucidate the mechanism for the unique change in extent of drug release as a function of DL. It is found that the drug release profile correlates well with the amorphous-amorphous phase separation (AAPS) onset. At a lower drug loading (up to 20 wt%), it takes more than 12 hours for AAPS to happen while in sharp contrast, it only needs less than 10 minutes for DL > 30 wt%. During AAPS amorphous drug accumulates on the surface of the film which prevents further dissolution from the interior of the ASD. The current study provides a mechanistic understanding of the confounding drug release profile of ASDs as a function of DL, and opens the door for studying drug-excipient (e.g. polymer, surfactant) interactions via XRF imaging in the future.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2019

Application of time-of-flight secondary ion mass spectrometry to the detection of surface intermediates during the first cycle of atomic layer deposition (ALD) of platinum on silica surfaces

Atomic layer deposition (ALD) has become the method of choice for many applications requiring the controlled growth of thin films on solid surfaces. Yet, the use of metalorganic precursors typical in these depositions adds significant complexity to the chemistry involved. Unfortunately, it is difficult to obtain direct information about the surface species that participate in the reaction mechanisms of ALD. Here we illustrate the value of using time-of-flight secondary ion mass spectrometry (ToF-SIMS) for this purpose. A specific example is provided, a study of the first cycle of deposition of platinum using trimethyl(methylcyclopentadienyl)platinum (IV), or MeCpPt(CH 3 ) 3, on silicon oxide surfaces. In previous investigations of this process, we have determined that the low reactivity of the MeCpPt(CH 3 ) 3 precursor, which hinders fast deposition, can be partially overcome by gas-phase electron-impact activation. What has not been clear is what chemical species form on the solid surface as a result of such activation. Here we show that the MeCp ligand is quite stable and that it remains intact and coordinated to the Pt atoms upon adsorption on the surface. It was also established that some of the methyl groups may remain bound to the Pt center: the main species detected on the silicon oxide surfaces were MeCpPt and MeCpPt(CH 3 ). On the other hand, it appears that no Pt intermediates without MeCp ligands are formed during this initial adsorption. Finally, O 2 treatment of these surfaces at elevated temperature to complete the first ALD cycle leads to the complete removal of all the organic ligands: no evidence for MeCp or methyl groups is seen in the ToF-SIMS traces from the final samples.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Scalable aqueous-phase fabrication of reduced graphene oxide nanofiltration membranes by an integrated roll-to-roll (R2R) process

Economic fractionation of multicomponent biomass-derived streams is a key challenge in biobased fuels and chemicals production. Kraft black liquor (BL) is generated at ~1 billion tons/yr globally from biomass pulping and contains ~15wt% total solids including lignin, hemicellulose fragments, and inorganics. Membrane-based BL concentration is attractive but challenged by low solute rejections and poor stability in BL, which combines alkaline pH (~13), high dissolved solids content (15+ wt%) and high temperature (70–85°C). Here we discuss the scaled fabrication and characterization of reduced graphene oxide (rGO) nanofiltration membranes by slot die coating on a roll-to-roll (R2R) with integrated vacuum filtration. Here, we obtain high-quality 90×30 cm rGO membranes (referred to as “R2R-rGO membranes” in this work) with ~100 nm average thickness supported on porous poly(ethersulfone) (PES) sheets, and an effective area of 2700cm 2 . We present characterizations of their microstructure and uniformity as mapped over large areas by scanning electron microscopy (SEM), ellipsometry, adhesion test and X-ray photoelectron spectroscopy (XPS). The constructed ellipsometry model for the rGO membrane/PES substrate composite was successfully applied to 48 different locations of the R2R-rGO membranes. The R2R-rGO membranes showed >98% lignin rejection with a steady state flux of ~12 LMH at 50bar in a 15.7wt% total solids (TS) kraft BL stream at 72°C and 2–3 gal/min crossflow rates. Slot die coating on a R2R platform with integrated vacuum filtration can enable rapid fabrication of high-quality GO membranes at scale without organic solvents or volatile organic compounds.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Epitaxial thin film growth of LiH using a liquid-Li atomic template

We report on the synthesis of lithium hydride (LiH) epitaxial thin films through the hydrogenation of a Li melt, forming abrupt LiH/MgO interface. Experimental and first-principles molecular dynamics studies reveal a comprehensive microscopic picture of the crystallization processes, which sheds light on the fundamental atomistic growth processes that have remained unknown in the vapor-liquid-solid method. We found that the periodic structure that formed, because of the liquid-Li atoms at the film/MgO-substrate interface, serves as an atomic template for the epitaxial growth of LiH crystals. In contrast, films grown on the Al{sub 2}O{sub 3} substrates indicated polycrystalline films with a LiAlO{sub 2} secondary phase. These results and the proposed growth process provide insights into the preparation of other alkaline metal hydride thin films on oxides. Further, our investigations open the way to explore fundamental physics and chemistry of metal hydrides including possible phenomena that emerge at the heterointerfaces of metal hydrides.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Plasma enhanced atomic layer deposition of thin film Li 1+x Mn 2-x O 4 for realization of all solid-state 3D lithium-ion microbatteries

Here, the plasma enhanced atomic layer deposition (PEALD) process for MnO 2 was demonstrated, exhibiting self-limiting growth as well as stable composition and stable growth rate over a temperature window of 205–265 °C. The PEALD process for MnO 2 was combined with the thermal ALD process for LiOH to synthesize Li 1+x Mn 2-x O 4 thin film cathodes, where the stoichiometry was effectively controlled to allow for crystallization in the electrochemically active spinel phase. A 3D nanostructure consisting of an Li 1+x Mn 2-x O 4 cathode layer, ALD Li x Al y Si z O solid electrolyte, and SiGe nanowire anode was fabricated and characterized via TEM. The Li 1+x Mn 2-x O 4 thin films maintained 66% of the areal capacity upon a 100× increase in the rate (4–360 μ A cm -2 ) as well as 97% capacity retention over 100 cycles at ~5C. The ALD Li 1+x Mn 2-x O 4 thin films exhibited a volumetric capacity of 52 μ Ah cm -2 μ m -1 at a C-rate of ~0.5C and, coupled with the high operating voltage (4.0 V), offer some of best areal energy densities for ALD thin film cathodes, making it a viable material for integration with 3D lithium-ion microbatteries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Friction stir processing of an aluminum-magnesium alloy with pre-placing elemental titanium powder: In-situ formation of an Al{sub 3}Ti-reinforced nanocomposite and materials characterization

A fine-grained Al–Mg/Al{sub 3}Ti nanocomposite was fabricated by friction stir processing (FSP) of an aluminum-magnesium (AA5052) alloy with pre-placed titanium powder in the stirred zone. Microstructural evolutions and formation of intermetallic phases were analyzed by optical and electron microscopic techniques across the thickness section of the processed sheets. The microstructure of the nanocomposite consisted of a fine-grained aluminum matrix (1.5 µm), un-reacted titanium particles (<40 µm) and reinforcement particles of Al{sub 3}Ti (<100 nm) and Mg{sub 2}Si (<100 nm). Detailed microstructural analysis indicated solid-state interfacial reactions between the aluminum matrix and micro-sized titanium particles to form Al{sub 3}Ti intermetallic phase. The hard inclusions were then fractured and re-distributed in the metal matrix by the severe thermo-mechanical conditions imposed by FSP. Evaluation of mechanical properties by hardness measurement and uniaxial tensile test determined significant enhancement in the mechanical strength (by 2.5 order of magnetite) with a high ductility (~22%). Based on a dislocation-based model analysis, it was suggested that the strength enhancement was governed by grain refinement and the presence of hard inclusions (4 vol%) in the metal matrix. Fractographic studies also showed a ductile-brittle fracture mode for the nanocomposite compared with fully ductile rupture of the annealed alloy as well as the FSPed specimen without pre-placing titanium particles. - Highlights: • FSP was employed to fabricate in situ nanocomposite. • The AA5052 Al alloy with pre-placed micro-sized Ti particles were utilized. • The structural analysis was revealed that the in situ formation of Al{sub 3}Ti nanophase. • The SZ grain structure was refined by PSN and ZHP mechanisms during DRX. • Hardness and tensile strength were improved up to ~2.5 times with a good ductility.

36 MATERIALS SCIENCE↗